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advantages and features of the present invention and methods of accomplishing the same may be understood more readily by reference to the following detailed description of preferred embodiments and the accompanying drawings . the present invention may , however , be embodied in many different forms and should not be construed as being limited to the embodiments set forth herein . rather , these embodiments are provided so that this disclosure will be thorough and complete and will fully convey the concept of the invention to those skilled in the art , and the present invention will only be defined by the appended claims . thus , in some embodiments , well - known structures and devices are not shown in order not to obscure the description of the invention with unnecessary detail . like numbers refer to like elements throughout . in the drawings , the thickness of layers and regions are exaggerated for clarity . it will be understood that when an element or layer is referred to as being “ on ,” or “ connected to ” another element or layer , it can be directly on or connected to the other element or layer or intervening elements or layers may be present . in contrast , when an element is referred to as being “ directly on ” or “ directly connected to ” another element or layer , there are no intervening elements or layers present . as used herein , the term “ and / or ” includes any and all combinations of one or more of the associated listed items . spatially relative terms , such as “ below ,” “ beneath ,” “ lower ,” “ above ,” “ upper ,” and the like , may be used herein for ease of description to describe one element or feature &# 39 ; s relationship to another element ( s ) or feature ( s ) as illustrated in the figures . it will be understood that the spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures . embodiments described herein will be described referring to plan views and / or cross - sectional views by way of ideal schematic views of the invention . accordingly , the exemplary views may be modified depending on manufacturing technologies and / or tolerances . therefore , the embodiments of the invention are not limited to those shown in the views , but include modifications in configuration formed on the basis of manufacturing processes . therefore , regions exemplified in figures have schematic properties and shapes of regions shown in figures exemplify specific shapes of regions of elements and not limit aspects of the invention . hereinafter , embodiments of the present invention will be described with reference to the accompanying drawings . fig1 is a plan view of a display device according to an embodiment of the present invention . referring to fig1 , a display device according to an embodiment of the present invention may include a display panel 100 , a gate tape carrier package 200 , a gate integrated circuit 200 a , a data tape carrier package 300 , a data integrated circuit 300 a , a first printed circuit board 400 , a first connector 500 , a second printed circuit board 600 , a timing controller 600 a , a second connector 700 , and a flexible cable 800 . the display panel 100 is a panel that displays data . the display panel 100 may be a liquid crystal display ( lcd ) panel , an electrophoretic display panel , an organic light emitting display ( oled ) panel , a light emitting diode ( led ) panel , an inorganic electroluminescent ( el ) display panel , a field emission display ( fed ) panel , a surface - conduction electron - emitter display ( sed ) panel , a plasma display panel ( pdp ), or a cathode ray tube ( crt ) display panel . hereinafter , as a display device according to an embodiment of the present invention , a liquid crystal display is exemplified , and as a display panel 100 , an lcd panel is exemplified . however , the display device and the display panel 100 according to embodiments of the present invention are not limited thereto , and various types of display devices and display panels may be used . although not illustrated in the drawing , the display panel 100 may include a display region where an image is displayed and a non - display region where an image is not displayed . in an exemplary embodiment , the display region may be surrounded by the non - display region . for example , the display region may be a center region of the display panel 100 , and the non - display region may be an edge region of the display panel 100 . further , although not illustrated in the drawing , the display panel 100 may include a first substrate , a second substrate that faces the first substrate , and a liquid crystal layer interposed between the first substrate and the second substrate . the first substrate and the second substrate may be in a cuboidal shape . however , the shape of the first substrate and the second substrate is not limited thereto , but the first substrate and the second substrate may be manufactured in various shapes . further , between the first substrate and the second substrate , a sealing member , such as a sealant , may be arranged along the edge portions of the first substrate and the second substrate to attach and seal the first substrate and the second substrate . the gate tape carrier package ( tcp ) 200 may be connected to at least one side of the display panel 100 . in an exemplary embodiment , the gate tape carrier package 200 may be formed in the non - display region of the display panel 100 . further , the gate tape carrier package 200 may be positioned on two short sides of the display panel 100 , but is not limited thereto . the gate tape carrier package 200 may be positioned on one short side or long side of the display panel 100 . the gate tape carrier package 200 may include a flexible film . in an exemplary embodiment , such a flexible film may be made of a plastic material . a plurality of gate tape carrier packages 200 may be provided . the plurality of gate tape carrier package 200 may be arranged to be spaced apart from each other by a predetermined distance . in an exemplary embodiment illustrated in fig1 , four gate tape carrier packages 200 may be positioned on one short side , and four gate tape carrier packages 200 may be positioned on the other short side that is opposite to the one short side , but are not limited thereto . the gate integrated circuit 200 a may be mounted on the gate tape carrier package 200 . the gate integrated circuit 200 a may be connected to a plurality of gate lines ( not illustrated ) of the display panel 100 via the gate tape carrier package 200 . the gate integrate circuit 200 a may successively provide a scan signal of a gate high voltage to the plurality of gate lines . further , the gate integrated circuit 200 a may supply a gate low voltage to the plurality of gate lines in the remaining period except for a period when the gate high voltage is supplied . the data tape carrier package 300 may be connected to at least one side of the display panel 100 . in an exemplary embodiment , the data tape carrier package 300 may be formed in the non - display region of the display panel 100 . further , the data tape carrier package 300 may be positioned on one long side of the display panel 100 , but is not limited thereto . the data tape carrier package 300 may be positioned on two long sides or short sides of the display panel 100 . the data tape carrier package 300 may include a flexible film . in an exemplary embodiment , such a flexible film may be made of a plastic material . a plurality of data tape carrier packages 300 may be provided . the plurality of data tape carrier package 300 may be arranged to be spaced apart from each other by a predetermined distance . in an exemplary embodiment illustrated in fig1 , eight data tape carrier packages 300 may be positioned on one long side , but are not limited thereto . the data integrated circuit 300 a may be mounted on the data tape carrier package 300 . the data integrated circuit 300 a may be connected to a plurality of data lines ( not illustrated ) of the display panel 100 via the data tape carrier package 300 . the data integrate circuit 300 a may convert pixel data into an analog pixel signal and supply the analog pixel signal to the plurality of data lines . the first printed circuit board ( pcb ) 400 may be connected to the data tape carrier package 300 . in embodiments , one end of the data tape carrier package 300 may be connected to the display panel 100 , and the other end of the data tape carrier package 300 that faces the one side may be connected to the first printed circuit board 400 . the first printed circuit board 400 may be a source printed circuit board . the first printed circuit board 400 may supply a control signal that is output from the timing controller 600 a mounted on the second printed circuit board 600 to be described later to the data integrated circuit 300 a . a plurality of printed circuit boards 400 may be provided . in an exemplary embodiment , two first printed circuit boards 400 may be arranged along the long side of the display panel 100 , but are not limited thereto . in an exemplary embodiment illustrated in fig1 , the plurality of first printed circuit boards 400 may be connected to four data tape carrier packages 300 , respectively , but are not limited thereto . the first connector 500 may be connected to the first printed circuit board 400 . in an exemplary embodiment , the first connector 500 may be positioned on the other side of the first printed circuit board 400 that faces one side of the first printed circuit board 400 to which the gate tape carrier package 200 is connected . the first connector 500 may transfer a control signal that is output from the timing controller 600 a mounted on the second printed circuit board 600 to be described later to the first printed circuit board 400 . a plurality of first connectors 500 may be provided . in an exemplary embodiment , the plurality of first connectors 500 may be positioned on the plurality of first printed circuit boards 400 , respectively . in embodiments , the first connectors 500 and the first printed circuit boards 400 may have one - to - one correspondence relationship . the structure of a connection portion between the first printed circuit board 400 and the first connector 500 will be described in detail later . the second printed circuit board 600 may be connected to the first printed circuit board 400 . in embodiments , the second printed circuit board 600 may be connected to the first printed circuit board 400 through the flexible cable 800 to be described later . the second printed circuit board 600 may be a control printed circuit board . the second printed circuit board 600 may transfer a control signal that is output from the timing controller 600 a to be described later to the first connector 500 . one second printed circuit board 600 may be provided . in an exemplary embodiment , one second printed circuit board 600 may be connected to two first printed circuit boards 400 , but is not limited thereto . the timing controller 600 a may be mounted on the second printed circuit board 600 . the timing controller 600 a may output various kinds of control signals that are transferred to the display panel 100 to match the timing thereof . the control signals generated by the timing controller 600 a may be transferred to the data integrated circuit 300 a via the second printed circuit board 600 , the second connector 700 , the flexible cable 800 , the first connector 500 , the first printed circuit board 400 , and the data tape carrier package 300 . the second connector 700 may be connected to the second printed circuit board 600 . in an exemplary embodiment , the second connector 700 may be positioned on one side of the second printed circuit board 600 that faces the first printed circuit board 400 . the second connector 700 may transfer the control signals from the timing controller 600 a to be described later to the first connector 500 . a plurality of second connectors 700 may be provided . in an exemplary embodiment , the plurality of second connectors 700 may be positioned on one second printed circuit boards 600 . the plurality of second connectors 700 may correspond to the plurality of first connectors 500 , respectively . that is , the first connectors 500 and the second connectors 700 may have one - to - one correspondence relationship . the structure of a connection portion between the second printed circuit board 600 and the second connector 700 will be described in detail later . the flexible cable 800 may connect the first connector 500 and the second connector 700 to each other . in an exemplary embodiment , the flexible cable 800 may be a flat flex cable ( ffc ). the flexible cable 800 may have a structure in which insulating plastic surrounds a metal thin film . the flexible cable 800 may serve to transfer the control signal generated by the timing controller 600 a from the second connector 700 to the first connector 500 . hereinafter , the structure of the connection portion between the first printed circuit board 400 and the first connector 500 in accordance with embodiments will be described in detail with reference to fig2 to 5 . fig2 is an enlarged perspective view of a portion ii of fig1 , and fig3 is an enlarged plan view of a portion ii of fig1 . fig4 is an enlarged plan view of a portion iv of fig3 , and fig5 is a cross - sectional view taken along line v - v ′ of fig3 . referring to fig2 to 5 , the first printed circuit board 400 may include a first base member 410 , a plurality of first conductive features 430 , and a first adhesive layer 450 . in embodiments , the conductive features may include conductive tracks , conductive wires , conductive pads and other features formed on an insulator substrate for forming a printed circuit board . such conductive features may be provided by forming a conductive metal layer , for example , copper layer , on the insulation substrate and patterning the conductive metal layer to form a conductive pattern layer with the conductive features , but not limited thereto . the first base member 410 may be a base that forms the first printed circuit board 400 . the first base member 410 may include at least one first conductive layer 410 a and at least one first insulating layer 410 b . the first conductive layer 410 a may be made of a conductive material . in an exemplary embodiment , the first conductive layer 410 a may be a copper foil layer , but is not limited thereto . the first conductive layer 410 a may be made of various conductive materials that can transfer an electrical signal . in embodiments , the first conductive layer 410 a may include a ground of a circuit . the first insulating layer 410 b may be made of an insulating material . in an exemplary embodiment , the first insulating layer 410 b may be made of a resin that includes polyimide ( pi ), but is not limited thereto . the first insulating layer 410 b may be made of various insulating materials . the first base member 410 may include a plurality of first conductive layers 410 a and a plurality of first insulating layers 410 b . the plurality of first conductive layers 410 a and the plurality of first insulating layers 410 b may be alternately stacked . in an exemplary embodiment illustrated in fig2 to 5 , five first conductive layers 410 a and five insulating layers 410 b may be stacked , but are not limited thereto . that is , the first base member 410 may have a multilayer structure . although not illustrated in the drawing , at least one of the plurality of first insulating layers 410 b may include at least one via hole that connects the plurality of first conductive layers 410 a and the plurality of first conductive features 430 to each other . in embodiments , the printed circuit board may include a first region 10 a and a second region 20 a when viewed in a viewing direction perpendicular to a major surface of t 0 the base member . the second region 20 a is next to the first region 10 a . the first region 10 a may be a region where the first conductive layer 410 a is positioned . further , the first region 10 a may be a region where the plurality of first conductive features 430 are positioned . further , the first region 10 a may be a center region of the first base member 410 . the second region 20 a may be adjacent to the first region 10 a . the second region 20 a may be a region where the first conductive layer 410 a is not positioned . further , the second region 20 a may be a region where the plurality of first conductive features 430 are not positioned . further , the second region 20 a may be a part of an edge region of the first base member 410 . further , the second region 20 a may be a region where a part of the first connector 500 is arranged . in an exemplary embodiment , the second region 20 a may be a region that corresponds to a main body of the first connector 500 . in embodiments , the first connector 500 includes a plurality of conductive terminals each of which is attached to one of the corresponding conductive features 430 in the first region . as described above , the first conductive layer 410 a may be positioned only in the first region 10 a , and the first insulating layer 410 b may be positioned in both the first region 10 a and the second region 20 a . the plurality of first conductive features 430 may be positioned on the first base member 410 . specifically , the plurality of first conductive features 430 may be positioned on the first conductive layer 410 a . further , the plurality of first wiring pattern 430 may be positioned in the first region 10 a . further , the plurality of first conductive features 430 may not be positioned in the second region 20 a . further , the plurality of first conductive features 430 may be directly positioned on the first insulating layer 410 b . that is , the first insulating layer 410 b may be interposed between the plurality of first conductive features 430 and the first conductive layer 410 a . control signals that are transferred from the timing controller 600 a may be applied to the plurality of conductive features 430 . the plurality of first conductive features 430 may be made of a conductive material . in an exemplary embodiment , the plurality of first conductive features 430 may be made of the same material as the first conductive layer 410 a . the plurality of first conductive features 430 may have impedance of about 100 ohms . parts of the plurality of first conductive features 430 may be connected to the first connector 500 . in an exemplary embodiment illustrated in fig2 to 4 , four first conductive features 430 are connected to the first connector 500 , but are not limited thereto . the minimum width d 1 of each of the plurality of first conductive features 430 that are connected to the first connector 500 may be smaller than the minimum width d 2 of each of the plurality of first conductive features 430 that are not connected to the first connector 500 . in an exemplary embodiment , referring to fig4 , the minimum width d 1 of each of the plurality of first conductive features 430 that are connected to the first connector 500 may be about 0 . 8 mm to about 1 . 2 mm . preferably , the minimum width d 1 of each of the plurality of first conductive features 430 that are connected to the first connector 500 may be about 1 mm . the minimum width d 1 of each of the plurality of first conductive features 430 that are connected to the first connector 500 may be determined by the amount of increase of necessary inductance and the tolerance in a process of manufacturing the first printed circuit board 400 to be described later . further , the minimum width d 2 of each of the plurality of first conductive features 430 that are not connected to the first connector 500 may be about 1 . 2 mm to about 1 . 6 mm . the minimum width d 2 of each of the plurality of first conductive features 430 that are not connected to the first connector 500 may be preferably about 1 . 4 mm . the first adhesive layer 450 may be positioned on the first base member 410 . specifically , the first adhesive layer 450 may be positioned in the second region 20 a . further , the first adhesive layer 450 may be positioned on the same plane as the plurality of first conductive features 430 . further , the first adhesive layer 450 may be interposed between the first connector 500 and the first base member 410 . the first adhesive layer 450 may serve to fix the first connector 500 to the first base member 410 . the first adhesive layer 450 may be made of an adhesive resin that is generally used . the first adhesive layer 450 may be omitted according to circumstances . as described above , the main body of the first connector 500 may be arranged in the second region 20 a of the first base member 410 , on which the first conductive layer 410 a is not positioned , to be electrically connected to parts of the plurality of first conductive features 430 . hereinafter , the structure of the connection portion between the second printed circuit board 600 and the second connector 700 will be described in detail with reference to fig6 . fig6 is a cross - sectional view taken along lint vi - vi ′ of fig1 . referring to fig6 , a second printed circuit board 600 may include a second base member 610 , a plurality of second conductive features 630 , and a second adhesive layer 650 . the second base member 610 may include at least one second conductive layer 610 a and at least one second insulating layer 610 b . since the second conductive layer 610 a and the second insulating layer 610 b have substantially the same material and structure as the first conductive layer 410 a and the first insulating layer 410 b as described above , the detailed description thereof will be omitted . the second base member 610 may include a first region 10 b and a second region 20 b . since the first region 10 b and the second region 20 b mean substantially the same regions as the first region 10 a and the second region 20 a as described above , the detailed description thereof will be omitted . the plurality of second conductive features 630 may be positioned on the second base member 610 . since the plurality of second conductive features 630 have substantially the same material and structure as the plurality of first conductive features 430 as described above , the detailed description thereof will be omitted . the second adhesive layer 650 may be positioned on the second base member 610 . since the second adhesive layer 650 has substantially the same material and structure as the first adhesive layer 450 as described above , the detailed description thereof will be omitted . as described above , the connection structure between the first printed circuit board 400 and the first connector 500 may be substantially the same as the connection structure between the second printed circuit board 600 and the second connector 700 . according to an embodiment of the present invention as described above , the signal integrity characteristics of the display device can be improved by the connection structure between the first printed circuit board 400 and the first connector 500 and the connection structure between the second printed circuit board 600 and the second connector 700 . this will be described in detail with reference to fig7 to 10 . fig7 is a graph illustrating the results of measuring time domain reflectometry of the display device of fig1 , and fig8 is an enlarged graph of a portion viii of fig7 . fig9 is a graph illustrating the results of analyzing an s parameter of the display device of fig1 , and fig1 is an enlarged graph illustrating a portion x of fig9 . first , referring to fig7 and 8 , graph a of fig7 is a graph in the case where the first conductive layer 410 a and the second conductive layer 610 a exist not only in the first regions 10 a and 10 b but also in the second regions 20 a and 20 b , and the minimum width of the plurality of first conductive features 430 and the plurality of second conductive features 630 is constantly about 1 . 4 mm . on the other hand , a transition region tr of fig7 is a region that corresponds to the connection region between the first printed circuit board 400 and the first connector 500 and the connection region between the second printed circuit board 600 and the second connector 700 . that is , if the first conductive layer 410 a and the second conductive layer 610 a exist not only in the first regions 10 a and 10 b but also in the second regions 20 a and 20 b , and the minimum width of the plurality of first conductive features 430 and the plurality of second conductive features 630 is constantly about 1 . 4 mm ( graph a ), the impedance is excessively lowered in the transition region tr . referring to fig8 , the minimum point of the graph a is about 71 . 2979 ohms at about 1 . 4231 ns . such excessive impedance lowering may deteriorate the signal integrity characteristics . the excessive impedance lowering may be mainly caused by parasitic capacitance between the first connector 500 and the first conductive layer 410 a , parasitic capacitance between the second connector 700 and the second conductive layer 610 a , parasitic capacitance between the plurality of first conductive features 430 , and parasitic capacitance between the plurality of second conductive features 630 . accordingly , a method for decreasing the parasitic capacitance or increasing the inductance based on an impedance formula , z 0 = root ( l / c ) ( here , z 0 is the characteristic impedance , l is the inductance , and c is the capacitance ), may be considered . first , the first conductive layer 410 a of the lower portion of the main body of the first connector 500 and the second conductive layer 610 a of the lower portion of the main body of the second connector 700 may be removed ( graph b ). through this , if the first conductive layer 410 a of the lower portion of the main body of the first connector 500 and the second conductive layer 610 a of the lower portion of the main body of the second connector 700 are removed , the parasitic capacitance between the first connector 500 and the first conductive layer 410 a and the parasitic capacitance between the second connector 700 and the second conductive layer 610 a can be removed , and thus the impedance in the transition region tr can be prevented from being excessively decreased . referring to fig8 , the minimum point of the graph b is about 72 . 8754 ohms at about 1 . 4231 ns . that is , the impedance on the condition of graph b with respect to the condition of graph a is increased by about 1 . 57 ohms in the transition region tr . next , the minimum width of each of the plurality of first conductive features 430 connected to the first connector 500 and the minimum width of each of the plurality of second conductive features 630 connected to the second connector 700 may be decreased ( graph c ) simultaneously with the removal of the first conductive layer 410 a of the lower portion of the main body of the first connector 500 and the second conductive layer 610 a of the lower portion of the main body of the second connector 700 . as described above , if the minimum width of each of the plurality of first conductive features 430 connected to the first connector 500 and the minimum width of each of the plurality of second conductive features 630 connected to the second connector 700 are decreased , the distance between the plurality of first conductive features 430 connected to the first connector 500 and the distance between the plurality of second conductive features 630 connected to the first connector 500 can be increased , and thus the parasitic capacitance between the plurality of first conductive features 430 and the parasitic capacitance between the plurality of second conductive features 630 can be decreased . further , if the minimum width of each of the plurality of first conductive features 430 connected to the first connector 500 and the minimum width of each of the plurality of second conductive features 630 connected to the second connector 700 are decreased , the impedance in this portion is increased . accordingly , the impedance in the transition region tr can be prevented from being excessively decreased . referring to fig8 , the minimum point of the graph c is about 74 . 3948 ohms at about 1 . 4260 ns . that is , the impedance on the condition of graph c with respect to the condition of graph b is increased by about 1 . 52 ohms in the transition region tr . as a result , the impedance on the condition of graph c with respect to the condition of graph a is improved by about 3 . 09 ohms in the transition region tr . that is , the display device according to an embodiment of the present invention has superior signal integrity characteristics in the connection portion between the first printed circuit board 400 and the first connector 500 and the connection portion between the second printed circuit board 600 and the second connector 700 . next , fig9 and 10 are referred to . fig9 illustrates the results of measuring a forward transfer coefficient ( s 21 ) of an s parameter . the conditions of graphs d , e , and f of fig9 correspond to the conditions of graphs a , b , and c of fig7 , respectively . referring to fig1 , in the ultra - high speed driving of 6 gbps ( 3 ghz ), the minimum point of graph d is − 5 . 7691 db , the minimum point of graph e is − 4 . 5593 db , and the minimum point of graph f is − 4 . 4877 db . that is , in the ultra - high speed driving of 3 ghz , the s 21 characteristics on the condition of graph f with respect to the condition of graph d are improved by about 1 . 28 db . that is , the display device according to an embodiment of the present invention has superior signal integrity characteristics in the connection portion between the first printed circuit board 400 and the first connector 500 and the connection portion between the second printed circuit board 600 and the second connector 700 . on the other hand , although not illustrated in the drawing , as the results of testing the signal integrity characteristics through application of the condition of 6 gbps in a linear source , the eyeheight on the condition of graph c of fig7 ( or the condition of graph f of fig9 ) with respect to the condition of graph a of fig7 ( or the condition of graph d of fig9 ) is increased from about 317 mv to about 383 mv . that is , the eyeheight on the condition of graph c of fig7 ( or the condition of graph f of fig9 ) with respect to the condition of graph a of fig7 ( or the condition of graph d of fig9 ) is improved by about 66 mv ( about 21 %). that is , the display device according to an embodiment of the present invention has superior signal integrity characteristics in the connection portion between the first printed circuit board 400 and the first connector 500 and the connection portion between the second printed circuit board 600 and the second connector 700 . hereinafter , other embodiments of the present invention will be described . in other embodiments of the present invention , the structure of the first printed circuit boards 401 and 402 is substantially the same as the structure ( not illustrated ) of the second printed circuit boards , and thus explanation will be made to focus on the structure of the first printed circuit boards 401 and 402 . fig1 is a perspective view of a first printed circuit board 401 , a first connector 500 , and a flexible cable 800 of a display device according to another embodiment of the present invention , and fig1 is a plan view of the first printed circuit board 401 , the first connector 500 , and the flexible cable 800 of fig1 . for convenience in explanation , the same reference numerals are used for substantially the same elements as the elements illustrated in the drawings as described above , and the duplicate explanation thereof will be omitted . referring to fig1 and 12 , in a first base member 411 of the first printed circuit board 401 , the ranges of a first region 11 a and a second region 21 a may differ from each other . that is , the first region 11 a may mean a center region of the first base member 411 , and the second region 21 a may mean the whole edge region of the first base member 411 . that is , the second region 21 a may mean not only the region that corresponds to the first connector 500 but also the whole edge region of the first base member 411 . on the other hand , a plurality of first conductive features 431 may be positioned on the first region 11 a as described above or may be positioned on the second region 21 a as described above . here , since the range of the second region 21 a differs , an area occupied by a first adhesive layer 451 may also differ . fig1 is a perspective view of a first printed circuit board 402 , a first connector 500 , and a flexible cable 800 of a display device according to still another embodiment of the present invention . fig1 is a plan view of the first printed circuit board 402 , the first connector 500 , and the flexible cable 800 of fig1 , and fig1 is a cross - sectional view taken along line xv - xv ′ of fig1 . for convenience in explanation , the same reference numerals are used for substantially the same elements as the elements illustrated in the drawings as described above , and the duplicate explanation thereof will be omitted . referring to fig1 to 15 , in a first base member 412 of the first printed circuit board 402 , the ranges of a first region 12 a and a second region 22 a may differ from each other . that is , the first connector 500 may be arranged only on the second region 22 a , but may not be arranged on the first region 12 a . further , one side of a plurality of first conductive features 432 may be positioned on the first region 12 a , but the other side of the plurality of first conductive features 432 , which faces the one side , may be positioned on the second region 22 a . that is , the plurality of first conductive features 432 may be arranged to further project from an end portion of a first conductive layer 412 a . in other words , end portions of the plurality of first conductive features 432 may not overlap the first conductive layer 412 a , but may overlap a first insulating layer 412 b . on the other hand , a first adhesive layer 452 may be positioned on the second region 22 a as described above . fig1 to 19 are cross - sectional views of first printed circuit boards 403 , 404 , 405 , and 406 of display devices according to other embodiments of the present invention . for convenience in explanation , the same reference numerals are used for substantially the same elements as the elements illustrated in the drawings as described above , and the duplicate explanation thereof will be omitted . referring to fig1 to 19 , a plurality of first conductive layers 413 a , 414 a , 415 a , and 416 a may all exist on a first region 10 a . however , at least one of the plurality of first conductive layers 413 a , 414 a , 415 a , and 416 a may not exist on a second region 20 a . in an exemplary embodiment , at least one of the plurality of first conductive layers 413 a , 414 a , 415 a , and 416 a , which does not exist on the second region 20 a , may be adjacent to a first connector 500 . that is , it is most helpful in improving the signal integrity characteristics to remove all the first conductive layers 413 a , 414 a , 415 a , and 416 a from the second region 20 a on which the first connector 500 is arranged . however , even if only one of the plurality of first conductive layers 413 a , 414 a , 415 a , and 416 a that are adjacent to the first connector 500 is removed , the parasitic capacitance between the first connector 500 and the plurality of first conductive layers 413 a , 414 a , 415 a , and 416 a can be decreased to improve the signal integrity characteristics . here , as going from a structure ( see fig1 ) in which the first conductive layer 413 a that is most adjacent to the first connector 500 is removed from the second region 20 a to a structure ( see fig1 ) in which only the first conductive layer 416 a that is farthest apart from the first connector 500 remains , the parasitic capacitance between the first connector 500 and the plurality of first conductive layers 413 a , 414 a , 415 a , and 416 a can be decreased to improve the signal integrity characteristics . although preferred embodiments of the present invention have been described for illustrative purposes , those skilled in the art will appreciate that various modifications , additions and substitutions are possible , without departing from the scope and spirit of the invention as disclosed in the accompanying claims . | 6 |
the principles of the present invention are particularly useful when embodied in a chain - closing apparatus such as shown in fig1 generally indicated by the numeral 10 . the apparatus 10 generally comprises a stationary element - engaging block 11 fixedly mounted on a vertical support plate 12 , a movable element block 13 slidably mounted on the support plate 12 and vertically movable toward and away from the stationary element - engaging block 11 , a photoelectric sensor 14 disposed upstream of the stationary element - engaging block 11 and spanning the path of movement of a pair of continuous slide fastener stringers f to be processed on the apparatus 10 , for detecting a disengaged portion of each coupling element chain or an element - free space disposed adjacent to the disengaged portion of the chain , and a spreading roller 15 disposed between the sensor 14 and the stationary element - engaging block 11 for spreading the disengaged portion of the chain or the element - free space to thereby assure reliable space sensing by the sensor 14 . the stationary and movable element - engaging blocks 11 , 13 jointly constitute an element engaging block assembly 16 . as shown in fig8 a , the slide fastener stringers f to be processed on the apparatus 10 include a plurality of longitudinally spaced chains c of two rows of interengaged coupling elements having a plurality of element - free gaps or spaces g ( only one shown ) disposed between the chains c . each of the chains c has a bottom end stop b secured at one end ( bottom end ) thereof . before being processed on the apparatus 10 , a slider s is threaded on each chain c from the other end ( top end ) thereof through the adjacent element - free space g while a rear end of the slider s is facing away from the bottom end stop b of the preceding chain c . due to this threading of slider , the rows of coupling elements e of the chain c are separated or disengaged from the top ends thereof , as shown in fig8 b . the apparatus 10 of the present invention is also effectively operative to process a pair of slide fastener stringers f1 such as shown in fig9 a , 10a and 11a . the slide fastener stringers f1 are the same as the slide fastener stringers f of fig8 a with the exception that a bottom end stop is not mounted on each chain c of coupling elements . the chain c is therefore separable from either one or both ends as shown in fig9 b , 10b and 11b when a slider s is threaded on the chain c . as shown in fig3 the support plate 12 has a vertical guide groove 17 extending therethrough . the movable element - engaging block 13 includes , as shown in fig4 a horizontal guide groove 18 defined in its upper surface for constrictingly receiving the partly disengaged coupling element chains to close the same in the manner as described later . the guide groove 18 has a width slightly larger than the width of the chains c of interengaged coupling elements . the guide groove 18 includes a flared inlet portion 18a for easy entry of the coupling element chains c into the guide groove 18 . the movable element - engaging block 13 is secured by a pair of screws ( fig2 ) to a horizontal arm 19 of an l - shaped support bracket 20 slidably received in the vertical groove 17 in the support plate 12 . connected to the horizontal arm 19 is a piston rod 21 of an air cylinder 22 which is actuated to reciprocate the bracket 20 along the vertical guide groove 17 , thereby moving the movable element - engaging block 13 toward and away from the stationary element - engaging block 11 . the stationary element - engaging block 11 has an l - shape as shown in fig5 and includes a guide groove 23 which is defined in the underside of a horizontal arm 24 of the stationary element - engaging block 11 in confronting relation to the guide groove 18 in the movable element - engaging block 13 . the guide groove 23 has the same shape as the guide groove 18 and hence includes a flared inlet portion 23a . when the movable element - engaging block 13 is moved upwardly to its upper working position shown in fig6 the stationary and movable element - engaging blocks 11 , 13 jointly constitute the element - engaging block assembly 16 . the assembly 16 has a guide channel 16a formed jointly by the guide grooves 18 , 23 of the movable and stationary element - engaging blocks 13 , 11 so that it functions as a slide fastener slider for closing the partly disengaged coupling element chains c . the stationary element - engaging block 11 further includes a guide ridge 25 disposed centrally in and extending longitudinally through the guide groove 23 for restricting lateral movement or wobbling of the coupling element chains c as they pass through the guide channel 16a in the element - engaging block assembly 16 . the photoelectric sensor 16 is disposed between the element - engaging block assembly 16 and a tension roller 26 rotatably mounted on the vertical support plate 12 at a position upstream of the element - engaging block assembly 16 . the tension roller 26 is held in contact with the slider fastener stringers f to exert a tension on the latter while the fastener stringers f are fed along the path . the photoelectric sensor 14 includes a light projector 27 and a photoelectric cell 28 disposed on opposite side of the path of movement of the fastener stringers f in confronting relation to each other . the photoelectric cell 28 is connected , for energization and de - energization , in circuit with the cylinder 22 through a control unit 29 . when an element - free space g or a disengaged portion ea ( fig1 b ) of the coupling element chain c arrives at the photoelectric sensor 14 and opens the light beam path from the light projector 27 , the photoelectric cell 28 sends an electric signal to the control unit 29 which in turn sends an output signal to the cylinder 22 to cause the latter to extend its piston rod 21 . consequently , the movable element - engaging block 13 is moved upwardly toward the stationary element - engaging block 11 . when the slider s arrives at the photoelectric sensor 14 and blocks the light beam path from the light projector 27 , the photoelectric cell 28 sends an electric signal to the control unit 29 which at a predetermined interval of time after receipt of the electric signal , sends an output signal to the cylinder 22 to cause the latter to reverse its mode of operation . that is , the cylinder is de - energized to lower the movable element - engaging block 13 . the light beam projected from the light projector 27 may be a laser beam . the spreading roller 15 is rotatably mounted on a lower end of an inverted l - shaped lever 30 . the lever 30 is pivotably connected by a pin 31 to a vertical elongate member 32 secured by a pair of screws 33 , 33 to the stationary element - engaging block 11 . a compression coil spring 34 acts between the stationary element - engaging block 11 and the lever 30 to turn the latter about the pin 31 in the counterclockwise direction in fig1 thereby urging the spreading roller 15 downwards . the spreading roller 15 has a tapered outer peripheral edge 35 as shown in fig2 . designated by the numeral 36 ( fig1 ) is an idler roller for guiding the slide fastener stringers f as they are fed through the apparatus 10 by a non - illustrated feed means . the apparatus 10 of the foregoing construction operates as follows . the slide fastener stringers f , f shown in fig8 b are introduced into the apparatus 10 and fed longitudinally along the path at a first or high speed until an element - free space g between adjacent two chains c is detected by the photoelectric sensor 14 . during that time , the spring - biased spreading roller 15 is held in rolling engagement with two rows of interengaged coupling elements of the preceding chain c , and then is urged into the element - free space g under the force of the spring 34 , thereby spreading the element - free space g . with the element - free space g thus spread , detection of the same by the photoelectric sensor 14 can be achieved reliably . upon detection of the element - free space g , the photoelectric cell 28 of the sensor 14 sends an electric signal to the control unit 29 which in turn sends an output signal to the non - illustrated feed means to cause the same to operate in a different mode in which the slide fastener stringers f , f are fed at a second or low speed . at the same time , the control unit 29 sends an output signal to the air cylinder 22 to energize the same , whereupon the movable element - engaging block 13 is moved upwardly from a lower stand - by position of fig2 to an upper working position of fig6 . the stationary and movable element - engaging blocks 11 , 13 now constitute a element - engaging block assembly 16 which has the same function as a slide fastener slider . while the slide fastener stringer f , f are being continuously fed at the low spaced , a disengaged portion e of the next following chain c is introduced into the guide grooves 18 , 23 in the element - engaging block assembly 16 and then coupling elements of the disengaged chain portion e are brought into inter - digitating engagement with each other . as the slide fastener stringers f , f are further advanced , a slider s on the chain c arrives at the photoelectric sensor 14 and blocks the light beam path from the light projector 27 . the photoelectric cell 28 then sends an electric signal to the control unit 29 to cause it to set a time switch ( not shown ) in the control unit 29 . the control unit 29 , at a predetermined interval of time after setting of its time switch , sends an output signal to the air cylinder 22 to de - energize the same . that is , upon its de - energization , the cylinder 22 retracts its piston rod 21 to lower the movable element - engaging block 13 to its lower stand - by position shown in fig2 . at the same time , the control unit 29 also sends an output signal to the feed means to cause the same to reverse its mode of stringer feeding operation . the slide fastener stringers f , f are fed again at the high speed . the time interval is selected such that coupling engagement of the disengaged portion e of the chain c ( fig8 b ) continues after detection of the slider s by the sensor 14 until the chain c is fully closed , as shown in fig8 c after the slider s on the chain c has been detected by the photoelectric sensor 14 . as the slide fastener stringers f , f are further advanced after the full closure of the chain c , the slider s abuts against the spreading roller 15 , which then is urged upwardly against the force of the compression coil spring 34 ( fig7 ), and finally passes through the element - engaging block assembly 16 . thus , the foregoing cycle of operation of the apparatus 10 can be repeated automatically until all the partly separated coupling element chains c are closed . it appears that since individual slide fasteners produced by severing the slide fastener stringers f , f , at the element - free spaces g have respective fully closed coupling element chains c , they can be easily attached by sewing to the garment fabrics . in case where the slide fastener stringers f1 , f1 shown in fig1 b are to be closed , the chain - closing apparatus 10 operates in the same manner as it has done to close the slide fastener stringers f , f shown in fig8 b . when the slide fastener stringers f1 , f1 shown in fig1 b are to be closed , the cylinder 22 is energized to move the movable element - engaging block 13 toward its upper operating position ( fig6 ) upon arrival of a disengaged portion ea of the preceding coupling element chain c at the photoelectric sensor 14 . as the slide fastener stringer f1 , f1 are fed forwardly , the spreading roller 15 projects into the disengaged chain portion ea and spreads the same to assure reliable detection of the disengaged chain portion ea by the photoelectric sensor 14 . a continuous advancing movement of the slide fastener stringers f1 , f1 causes the disengaged portion ea of the preceding chain c and a disengaged portion e of the next following chain to be closed as they move through the guide channel 16a in the element - engaging block assembly 16 . other operational steps of the apparatus 10 are the same as the apparatus 10 has done in closing the slide fastener stringers f , f and f1 , f1 shown respectively in fig8 b and 9b and no description is necessary . the apparatus 10 of the present invention is also effectively operative to close the slide fastener stringers f1 , f1 in the manner as shown in fig1 b and 11c . in this instance , the cylinder 22 is actuated to lift the movable element - engaging block 13 upon expiration of a predetermined interval of time after detection by the senser 14 of a disengaged portion ea of the preceding coupling element chain c . the time interval is selected such that the disengaged chain portion ea has advanced beyond the element - engaging block assembly 16 after its detection by the sensor 14 . this selection of the time interval is achieved by a time switch of the control unit 29 . as the slide fastener stringers f1 , f1 are fed forwardly while the movable element - engaging block 13 is being held in the upper working position , the disengaged portion e of the next following chain c is closed , as shown in fig1 c . the disengaged portion ea of the preceding chain c still remains unclosed . obviously , many modefications and variations of the present invention are possible in the light of the above teachings . it is therefore to be understood that within the scope of the appended claims , the invention may be practiced otherwise than as specifically described . | 0 |
with reference to fig2 and 3 , the glass substrate or bottom plate 10 is provided with a layer 12 of photoresist and the top plate 16 is provided with a layer 14 of photoresist and the two components are adhered together to form the completed assembly . none of the figures is to scale so that the details of the miniaturized structure is readily apparent . in fig1 - 3 , the bottom plate 10 may be about 44 mm square and the thickness of each layer 12 and 14 may be 0 . 005 mm . in fig1 only the first layer 12 as applied to the bottom plate 10 is illustrated , for clarity . from fig1 then , it will be apparent that the layer 12 is patterned as indicated , to include the opposite side boundaries 17 and 18 and the intervening opposite side boundaries 20 and 22 . the widths of the boundaries 17 , 20 and 22 may be about 4 mm whereas the width of the side boundary 18 may be about 12 mm except in the region of the notch 24 where it is about 4 mm . extending from the opposite side boundary 17 and into the notch 24 are parallel legs 26 and 28 , each of about 1 mm in width and defining the bottom half of a channel 30 which is of about 2 mm in width . where the legs 26 and 28 enter the notch 24 , they define entrance passages 31 and 33 into the bottom halves of the chambers 50 and 52 , each of about 2 mm in width , and the ends of the legs are spaced from the bottom of the notch 24 by about 2 mm . in addition , the pattern includes the four annular pads 32 , 34 , 36 and 38 for holding adhesive , each having a central opening 40 for that purpose . the resist pads are about 4 mm in diameter and their exact positioning is not critical . the second layer 14 is identical to the first layer 12 except that it is formed on the top plate 16 , which is of lesser width than the bottom plate so that the legs 26 &# 39 ; and 28 &# 39 ; are shorter by about 2 mm than the corresponding legs 26 and 28 of the first layer 12 . corresponding portions of the two layers are referenced by primed numbers . the assembly is completed by registering the glass top plate 16 with its patterned resist layer 14 in position atop the bottom plate 10 with its patterned resist layer 12 so that the resist patterns are in registry , and effecting adhesion therebetween by means of spots of adhesive 48 which are received in the openings 40 . the steps of making the embodiment according to fig1 - 3 are as follows : 1 . prepare a master drawing by computer aided design of the film pattern according to fig1 . 3 . spin 1 / 4 milliliters / square inch shipley 1690 positive resist , vapor saturated with the solvents ( propylene methoxy glycol & amp ; xylene ) contained in the resist , followed by baking at 100 ° c . for 30 minutes , all in a dust - free ( particle - free ) environment . this applies to both layers . 4 . expose each thin resist film layer through the mask with a 275 watt mercury lamp unfiltered at a distance of 8 inches for 10 minutes and develop with shipley 455 potassium hydroxide developer spray applied at the rate of 10 cc per minute for 50 seconds at 500 rpm overlapping 5 seconds with distilled water rinse for 2 minutes . 5 . cure by hard baking at 140 ° c . for 30 minutes in a convection oven . 6 . place the samples on the ground plate between the electrodes of a parallel plate plasma system spaced one inch apart . evacuate the chamber to 1 micron . flush with helium at 500 millitorr for ten minutes . change the gas to tetrafluoromethane at 500 millitorr for one minute . excite the gas with a 100 watt rf source at 13 . 6 megahertz and maintain the plasma for 5 minutes . flush with helium . 7 . dispense adhesive dots ( about 10 nanoliter per dot ) into openings 40 of one resist pattern . 8 . place bottom plate into recessed vacuum fixture and register top plate thereon . place # 2 glass onto top plate to cover the vacuum recess and apply vacuum to press the top and bottom plates together . expose the assembly to uv light as above for 1 minute to cure the adhesive 48 . the process as above results in a unitary assembly which is the patterned resist disposed between the top and bottom glass plates as best seen in fig2 and 3 . the fluorinating plasma treatment as noted above conditions or alters the exposed glass surface of the bottom glass plate 10 and the exposed surfaces of the developed and cured resist respectively to make the glass surface more wettable ( increasing its surface energy ) while rendering the resist more hydrophobic ( decreasing it surface energy ). the volumes of the two chambers 50 and 52 on either side of the evaluation chamber 30 are more than sufficient to accommodate the volume of a biological sample deposited at the region indicated at 54 in fig3 so that the totality of the deposited sample is drawn into the capillary evaluation passage or chamber 30 and partially into the chambers 50 and 52 until meniscii are present at about the positions indicated at 56 , 58 and 60 in dotted lines in fig1 and 3 . this assures that very small surface areas of the liquid medium are exposed to ambient air and therefore to destructive evaporation . it also assures that the liquid phases of the contents of the chambers 30 , 50 and 52 are separated while the vapor phases thereof are connected across the top edges of the legs defining the chamber 30 therebetween , as indicated at 62 and 64 . it also assures that a rather precisely defined volume of the sample will almost immediately enter and fill the chamber 30 as an immobilized sample for study while the bulk of the applied sample will be drawn into and enter the chambers 50 and 52 somewhat more slowly but with the menisci forming at the positions as illustrated . the almost completely isolated sample for study in the chamber 30 is well protected against deterioration even at the body temperature ( almost 100 ° f .) at which the sample will be maintained for study . the embodiment according to fig4 - 6 is for the study of individual cells or cell cultures and includes means for nourishing or growing them . as will be evident from fig5 and 6 , substantially identically sized top and bottom glass plates 100 and 102 are provided with a single resist layer 104 in the case of the top plate 100 and with three layers 106 , 108 and 110 in the case of the bottom plate 102 . fig4 is a plan view of the bottom plate with its layers 106 , 108 and 110 . 1 . prepare a master drawing by computer aided design of the pattern of holes according to fig4 to make mask 1 which is transparent in the areas of the seven circles . prepare another master drawing of the pattern of the layer 110 in fig4 to make mask 2 . prepare still another master drawing of the pattern of the layer 108 in fig4 to make mask 3 . 2 . reduce the masters to provide masks 1 , 2 and 3 . 3 . spin 1 / 4 milliliters / square inch shipley 1690 positive resist , vapor saturated with the solvents ( propylene methoxy glycol & amp ; xylene ) contained in the resist , followed by baking at 100 ° c . for 30 minutes , all in a dust - free ( particle - free ) environment . this applies only to the bottom plate and its layer 106 . 4 . expose the thin resist film layer 106 through the mask 1 with a 275 watt mercury lamp unfiltered at a distance of 8 inches for 10 minutes and develop with shipley 455 potassium hydroxide developer spray applied at the rate of 10 cc per minute for 50 seconds at 500 rpm overlapping 5 seconds with distilled water rinse for 2 minutes . the layer 106 now is patterned with openings 118 , 120 , 122 and 124 as well as the openings 112 , 114 and 116 , all of which expose the glass plate 102 at this time . 5 . cure the patterned layer 106 by hard baking at 140 ° c . for 30 minutes in a convection oven . 6 . place the bottom plate with the patterned layer 106 in an evaporator ( polaron evaporator ) 10 inches away from a tungsten wire basket containing small quantity ( 1 mm diameter ) pure aluminum bead . evacuate to 1 micron and pass sufficient current through the basket to evaporate the aluminum onto the patterned layer 106 and the exposed portions of the plate 102 within the circles 112 , 114 , 116 , 118 , 120 , 122 and 124 7 . apply shipley 1375 positive resist as in 3 above to the entirety of the aluminum surface . 8 . expose the 1375 phoresist through mask 2 and develop as in 4 above , followed by etch in phosphoric - nitric acid aluminum etchant for 30 seconds followed by 2 minute distilled water rinse . dip in acetone followed by methanol and distilled water to remove the 1375 photoresist . the aluminum now covers only the area of the layer 110 , that is from the point 126 to the point 128 along the division line 130 , the upper half 132 of the circle or opening 112 , line 134 and so on through the upper circle halves 136 and 140 and the lines 138 and 142 and thence along the lines 144 , 146 and 148 . 9 . apply 1650 photoresist as in 3 above over the entire exposed surface . 10 . expose the 1650 through mask 3 and develop as in 4 above . 12 . drill four holes through the bottom plate as indicated for the holes 150 and 152 in fig6 . 13 . apply 1350 resist as in 3 to the bottom surface of the top plate and cure as in 5 to provide the layer 104 . 14 . place the top and bottoms plates on the ground electrode between the electrodes of a parallel plate plasma system spaced one inch apart . evacuate the chamber to 1 micron . flush with helium at 500 millitorr for ten minutes . change the gas to tetrafluoromethane at 500 millitorr for one minute . excite the gas with a 100 watt rf source at 13 . 6 megahertz and maintain the plasma for 5 minutes . flush with helium . when using the embodiment just described , the top plate is separated form the bottom plate in a sterile environment and an aliquot containing liquid medium and one or more cells is loaded to fill each of the wells or chambers within the layer 106 , one such chamber being indicated at 158 in fig5 . the top plate is then placed in position on the bottom plate and clamped or otherwise secured in position thereon . a source of gas such air mixed with 5 % carbon dioxide is connected to the opening through the bottom plate corresponding to the circle 124 and is exhausted through the glass plate opening corresponding to the circle 122 to circulate the gas through the gas perfusion chamber 154 . similarly , a source of cell culture media is connected to the glass plate opening 150 and exhausted through the opening 152 to circulate the liquid media through the nutrient or reagent chamber 156 . the cell culture chambers 158 must be of a size to accommodate the original cells in the aliquot plus any cells which will grow up from the original cells during the study . typically , these chambers may be 100 microns deep for egg cells or 20 microns deep for other types of animal cells . therefore , the layer 106 may vary in thickness in accord with its intended use . the diameter of these chamber depends upon the number of cells to be studied in each chamber , for example typically ranging between about 250 microns and 1 centimeter . the aluminum layer normally is about 100 angstrom units thick which will promote the wetting of the chamber 156 while allowing observations through the aluminum layer . the thickness of the layer 108 must be thin enough to impede the flow of gas into the chamber 156 and to impede the flow of media into the gas perfusion chamber 154 and blocking cells from escaping the culture chambers 158 . at the same time it must be thick enough to allow proper exchange of nutrients , and cell products between the chambers 158 and 156 and gases between the chambers 158 and 154 . typically , this thickness will range between 1 / 4 micron and 10 microns . the layer 104 is thin enough to provide good visibility into the cell chambers 158 and may be any material which is thin and hydrophobic . when miniaturized structures are formed of contiguous or adjacent materials desired to have significantly different surface energy levels , these surface energy levels are often compromised or altered from those desired and the desired characteristics cannot be restored by well known methods . in fact , well known methods when attempted tend to compromise the surface energy levels of the materials involved , usually altering the surface energy level of one material in the desired direction while having the opposite effect on the other . i have found , however , that the effect of attaining desired disparate surface energy levels can be obtained and that , furthermore , it can even be obtained simultaneously by a single treatment . specifically , as disclosed above , the desired effect can be accomplished by subjecting the miniaturized structural assembly to fluorinating plasmas in the absence of contaminant gases such as oxygen or water . i have also found that hydrogen plasmas , under the same conditions , are effective as well . in miniaturized structures as disclosed herein , surface energy levels as high as or greater than 100 dynes per centimeter as well as surface energy levels less than 30 dynes per centimeter are advantageous and are considered necessary and surface energy levels as high as 300 dynes per centimeter and as low as 5 dynes per centimeter may be highly desirable . in accord with this invention , surface energy levels of this nature have been simultaneously attained in structures smaller than 10 microns . in considering this invention , the above disclosure is intended to be illustrative only and the scope and coverage of the invention should be construed and determined by the following claims . | 1 |
within this application , both infra and supra , the following terms have the following meanings unless explicitly denoted otherwise : &# 34 ; inner &# 34 ; means toward the end of the invented fluffer nearest the tractor &# 39 ; s three - point hitch ; &# 34 ; outer &# 34 ; means away from the end of the invented fluffer furthest from the tractor &# 39 ; s three - point hitch ; &# 34 ; distal &# 34 ; means further from the three - point hitch ; &# 34 ; proximal &# 34 ; means closer to the three - point hitch ; &# 34 ; left &# 34 ; and &# 34 ; right &# 34 ; are used in reference to what would be considered left and right by an operator of the tractor while the operator is operating the tractor and facing forward ; &# 34 ; clockwise &# 34 ; is the direction that the pickup drum turns while the device is in use , as viewed from the left side of the device as attached to the tractor . the invented fluffer is a retractable hay and bean fluffer 100 . as shown in fig1 and fig2 the invented fluffer 100 comprises a pickup assembly 40 for fluffing hay and beans , the pickup assembly 40 is attached to and supported by a pickup frame 30 for holding the pickup assembly 40 above the surface of the ground , the pickup frame 30 is pivotally attached to a hitch attachment assembly 50 at a pivot , the hitch attachment assembly 50 attaches to a standard three - point hitch on the rear of a tractor 200 . a hydraulic ram 300 is attached at one end to the hitch attachment assembly 50 , and at the other end to the pickup frame 30 . preferably , a gauge wheel assembly 60 is pivotally attached to the pickup frame 30 for assisting in holding the pickup frame 30 and pickup assembly 40 above the surface of the ground . as shown in fig3 and 4 , the pickup assembly 40 further comprises a cylindrical pickup drum 42 having a plurality of perpendicularly extending tines 44 circumscribing the exterior surface of the drum 42 . this drum 42 is rotatably attached between an inner pickup attachment arm 22 and an outer pickup attachment arm 24 respectively at an inner drum attachment assembly 46 and an outer drum attachment assembly 48 of the pickup frame 30 . the tines 44 are preferably straight , however , other shaped tines 44 are also envisioned by the inventor . the tines 44 are spaced symmetrically in a concentric arrangement about the drum 42 . the tines are preferably of a plastic material , 8 &# 34 ; long , affixed in a rubber block , said tines being replaceable if broken . in the preferred embodiment , the pickup drum 42 is a premanufactured piece , called a rehn pickup . attached to the pickup assembly 40 , preferably at the inner and outer attachment assemblies 46 , 48 , is a set of stripper bars 18 extending in a mutually spaced relationship transverse to the rearward portion of the drum 42 . the stripper bars 18 are arranged and positioned to receive therebetween the tines 44 as the pickup drum 42 rotates . as the pickup drum 42 rotates in a clockwise direction , the stripper bars 18 serve to strip plant matter entangled within the tines 44 from the pickup drum 42 . as shown in fig5 and 6 , a standard hydraulic &# 34 ; orbit &# 34 ; motor 38 is attached to either the bottom surface of the outer extension arm 54 or the inner side of the drum pickup 42 . this hydraulic motor 38 is powered from the hydraulic system of the tractor 200 in the usual manner , and its speed is controlled by the operator of the tractor 200 operating a standard , hydraulic , flow control valve 36 connected into the hydraulic system of the tractor 200 , by the usual pressure hoses 35 . the hydraulic &# 34 ; orbit &# 34 ; motor 38 drives a first sprocket 80 that drives a chain that turns second sprocket 82 and a third sprocket 84 . the second sprocket 82 is attached to a rear shaft 70 extending beneath the stripper bars 18 the length of the pickup drum 42 , and the third sprocket 84 is attached to a front shaft 72 extending through the center of the pickup drum 42 . corresponding sprockets ( not shown ) are also located on the distal end of the pickup drum 42 where a second chain ( not shown ) extends between the second sprocket 82 and the third sprocket 84 . the motor 38 drives the first sprocket 80 that drives a chain turning the second sprockets 82 and the third sprockets 84 , thereby causing the rotation of the drum pickup 42 in a direction opposite the forward direction of travel of the tractor 200 . preferably , the operator is also able to rotate the drum pickup 42 in the same direction as the forward direction of travel of the tractor 200 to clear any plant matter entangled upon the drum 42 . as shown in fig3 and 4 , the drum 42 is rotatably attached between an inner pickup attachment arm 22 and an outer pickup attachment arm 24 respectively at an inner drum attachment assembly 46 and an outer drum attachment assembly 48 . the inner pickup attachment arm 22 , for support of the pickup assembly , extends at an upper end from the frame support bar 63 to the inner drum attachment assembly 46 at its lower end . the inner drum attachment assembly 46 further attaches to the proximal end of the pickup assembly 40 . the distal end of the outer extension arm 54 attaches to the inner pickup attachment arm 22 at a point near the inner drum attachment assembly &# 39 ; s attachment 46 to the drum pickup 42 . the outer pickup attachment arm 24 extends at an upper end from the bottom surface of the frame support bar 63 at near the distal end of the frame support bar 63 to the outer drum attachment assembly 48 at its lower end . the outer drum attachment assembly 48 further attaches to the distal end of the pickup assembly 40 . in the preferred embodiment of the invented fluffer , the pickup attachment arms 22 , 24 comprise steel tubing of two - inches by four - inches by one - quarter - inch size and 22 inches in length , and the drum attachment assemblies 46 , 48 comprise steel plates welded to the bottom of the pickup attachment arms 22 , 24 , said attachment assemblies 46 , 48 welded to the drum pickup 42 . attached to the outer pickup attachment arm 24 is the gauge wheel assembly 60 . in the preferred embodiment , the gauge wheel assembly 60 comprises a gauge wheel 66 pivotally attached to a gauge wheel arm 14 at a gauge wheel attachment 16 . the gauge wheel arm 14 then connects to the distal surface of the outer pickup attachment arm 24 . the gauge wheel 66 is premanufactured and standard to the industry . in the preferred embodiment of the invented fluffer 100 , the gauge wheel extension arm 14 comprises a piece of steel tubing of two - inches by four - inches by one - quarter - inch size , and the gauge wheel assembly 60 comprises a steel plate 12 welded to the proximal end of the gauge wheel extension arm 14 , said gauge wheel assembly 60 welded to the outer pickup attachment arm 24 . in the invented fluffer 100 , the frame support bar 63 comprises a straight piece running parallel to the pickup drum 42 . the frame support bar 63 attaches to the outer pickup attachment arm 24 near the distal end of the frame support bar 63 , and attaches to the inner pickup attachment arm 22 near the proximal end of the frame support bar 63 . such attachments are preferably on the bottom surface of the bar 63 . the frame support bar 63 also has an attachment 27 for receiving one end of a hydraulic ram 300 , such attachment 27 is ; preferably located upon and extends from the back side of the invented fluffer 100 , preferably on the bar 63 at a position between the spot directly above the center of the pickup drum 42 and the attachment between the bar 63 and the inner pickup attachment arm 22 . attachment of the ram ( not shown ) is done in the standard manner . use of such a hydraulic ram , allows the operator of the tractor - fluffer to move the invented fluffer 100 from a retracted , transport position to an extended , operational position . moving the invented fluffer 100 between such positions could be done by hand , but use of a mechanical means is preferred . the frame support bar 63 preferably comprises an 8 &# 39 ;- 11 &# 34 ; long piece of 5 inches by 5 inches by 0 . 25 inch steel tubing for the hay fluffer version , and a 13 &# 39 ;- 8 &# 34 ; long piece of 5 inches by 5 inches by 0 . 25 inch steel tubing for the bean fluffer version . the proximal end of the frame support bar 63 is pivotally attached to the distal end of the upper hitch support bar 62 at an upper pivot assembly 31 and a pivot locking pin 32 . the upper pivot assembly 31 comprises a top plate 33 , a bottom plate 34 , a pivot pin 32 , and a pivot pin hole 37 . the top plate 33 is a plate of steel mounted on the top surface of upper hitch support bar 62 , and the bottom plate 34 is a plate of steel mounted on the bottom surface of upper hitch support bar 62 , both plates extend distally from the upper hitch support bar 62 . a pivot pin hole 37 extends through the top plate 33 , the bottom plate 34 and the frame support bar 63 . the pivot pin 32 is able to be received into the pivot pin hole 37 , thereby allowing the frame support bar 63 to pivot in relation to the hitch attachment assembly 50 . this pivoting of the frame support bar 63 is assisted by the lower pivot assembly 55 . the lower pivot assembly 55 is located and aligned directly below the upper pivot assembly 31 . in the preferred embodiment , the lower pivot assembly 55 comprises an upper plate 56 , a lower plate 57 , a lower pivot pin 58 and a lower pivot pin hole 59 . the upper plate 56 is a steel plate mounted on the upper surface of the inner extension arm 52 . the lower plate 5 7 is a steel plate mounted on the lower surface of the inner extension arm 52 . both plates 56 , 57 extend distally from the distal end of the inner extension arm 52 . alternatively , the upper plate 56 and the lower plate 57 may be mounted on and extended from the distal surface of the inner extension arm 52 , as shown in fig3 and 6 . the lower pivot pin hole 59 extends through the upper plate 56 , the proximal end of the outer extension arm 54 and through the lower plate 57 . the lower pivot pin 58 is able to be received into the lower pivot pin hole 59 , thereby allowing the outer extension arm 54 and the pickup assembly 40 and the pickup frame 30 to pivot in relation to the hitch attachment assembly 50 . preferably , the outer extension arm 54 is 13 inches in length and comprises a 2 inches by 4 inches by 0 . 25 inch thick piece of steel tubing . the pivoting of the lower pivot assembly 55 cooperates with the pivoting of the upper pivot assembly 31 to allow the pickup frame 30 and the pickup assembly 40 to be swung within a horizontal plane from an extended , operational position to a retracted , transportation position . preferably , this pivoting allows the pickup frame 30 and the pickup assembly 40 to swing from a perpendicular position in relation to the tractor 200 , to a parallel position directly behind the tractor 200 . the inventor does envision that other methods of pivoting may also be used . for instance , having the pickup frame 30 and the pickup assembly 40 retract to behind the tractor 200 by pivoting within a vertical plane rather than the preferred horizontal plane . in the invented fluffer , the hitch attachment assembly 50 comprises three pairs of 3 - point hitch mounting plates 20 mounted on a hitch frame 51 comprising : an inner hitch support bar 69 , an outer hitch support bar 68 , a lower hitch support bar 64 , an upper hitch support bar 62 , and an inner extension arm 52 . the hitch attachment assembly 50 comprises the above parts , all welded or otherwise affixed together into a single piece . the pairs of 3 - point hitch mounting plates 20 used are standard 3 - point hitch mounts , each comprising spaced tabs or plates , each having a hole ( not shown ) for receiving a pin 21 , as shown in fig5 and 6 . the 3 - point hitch mounting plates 20 are spaced apart as the standard 3 - point hitches are , thus resulting in one pair of the plates 20 located near the proximal end of the lower hitch support bar 64 , one pair of the plates 20 located near the distal end of the lower hitch support bar 64 , and the third pair of plates 20 located on the upper hitch support bar 62 , generally equidistant from the upper hitch support bar &# 39 ; s 62 attachment to outer hitch support bar 68 and the upper hitch support bar &# 39 ; s 62 attachment to inner hitch support bar 69 . all three pairs of the plates 20 are located on the front side of the invented fluffer 100 . the preferred material for these plates 20 is steel and it is believed that the best mode of attachment is through welding the plates 20 to the bars 62 , 64 as discussed above . the 3 - point hitch 23 is attached to the present invention by first placing the hitch point , 23 near the hitch mounts 20 , then a hitch pin 21 is inserted through a hole in one plate of a first hitch mount 20 , through the hole in the first one of the hitch points 23 and then through a hole in the second plate of the first hitch mount 20 . this pin 21 is then fastened in the common manner . this process is repeated for the other two hitch points 23 and the other two hitch mounts 20 , thereby attaching the attachment 10 to the tractor 200 . the inner hitch support bar 69 further comprises a vertical piece attaching at a lower end to the upper surface of the distal end of the lower hitch support bar 64 . such an attachment is preferably a weld . the inner hitch support bar 69 then extends vertically to its attachment with is the bottom surface of the upper hitch support bar 62 . such an attachment is preferably a weld . the inner hitch support bar 69 preferably comprises a 16 inches long piece of 5 inches by 5 inches by 0 . 25 inch steel tubing . the outer hitch support bar 68 further comprises a vertical piece attaching at a lower end to the upper surface of the proximal end of the lower hitch support bar 64 . such an attachment is preferably a weld . the inner hitch support bar 69 then extends vertically to its attachment with the bottom surface of the proximal end of upper hitch support bar 62 . such an attachment is preferably a weld . the outer hitch support bar 68 preferably comprises a 16 inches long piece of 5 inches by 5 inches by 0 . 25 inch steel tubing . the lower hitch support bar 64 is a horizontal piece extending from the proximal end of the invention 100 to the inner extension arm 52 . the length of the lower hitch support bar 64 is preferably 48 inches . two pairs of 3 - point hitch mounting plates are located on the front surface of the lower hitch support bar 64 , one located a few inches proximally from the distal end of the lower hitch support bar 64 and the other located a few inches distally from the proximal end of the lower hitch support bar 64 . the lower hitch support bar 64 preferably comprises a piece of 5 inches by 5 inches by 0 . 25 inch steel tubing . the upper hitch support bar 62 is a horizontal piece extending from the proximal end of the invention 100 to the upper pivot assembly 31 . the length of the upper hitch support bar 62 is preferably five feet , six inches . a pair of 3 - point hitch mounting plates are located on the front surface of the bar 62 , preferably said plates are centered approximately 24 inches from the proximal end of the bar 62 . the upper hitch support bar 62 preferably comprises a piece of 5 inches by 5 inches by 0 . 25 inch steel tubing . the upper hitch support bar 62 also has an attachment 26 for receiving one end of a hydraulic ram 300 , such an attachment 26 is preferably located upon and extends from the back side of the fluffer , preferably at a location on the bar 62 between the upper 3 - point hitch plates 20 located on the bar 62 and the distal , lower 3 - point hitch plates 20 located near the distal end of the lower hitch support bar . attachment of the ram is done in the standard manner . use of such a hydraulic ram , allows the operator of the tractor - fluffer to move the fluffer from a retracted , transport position to an extended , operational position . the inner extension arm 52 is a horizontal piece extending from the distal end of the lower hitch support bar 64 to the lower pivot assembly 55 . as such , the inner extension arm 52 is preferably , approximately 21 . 5 inches long . the inner extension arm 52 preferably comprises a piece of 3 inches by 4 inches by 0 . 25 inch thick piece of steel tubing . a piece of angle iron serving as a hydraulic assembly attachment 28 is welded to the upper hitch support bar 62 for support of a standard , hydraulic , flow control valve 36 for controlling the speed of the pickup drum 42 . attachment of the valve 36 to the attachment 28 is done using the standard nuts and bolts . preferably , the distal surface of the outer hitch support bar 68 is a weight bracket 88 for the support of counterweights 89 to add balance the invented fluffer 100 when extended . differing sizes of the fluffers are envisioned . for instance , a bean fluffer , by necessity of the manner in which beans are harvested , needs to be longer than a hay fluffer , mainly due to the fact that hay is usually placed into windrows upon cutting . in manufacturing the invented fluffer to achieve these differing lengths only the frame support bar 63 and the pickup drum 42 need to be made of different lengths . for instance , one version of a hay fluffer would require a seven foot long pickup drum 42 attached beneath a frame support bar 63 of eight feet , eleven inches in length ; and one version of a bean fluffer would require a twelve - foot long pickup drum 42 attached beneath a thirteen feet , eight inches long frame support bar 63 . preferably the invented fluffer comprises an attachment for a tractor , however the invented fluffer may also comprise a drawn unit or even a self - propelled unit . the invented fluffer 100 is used by attaching the 3 - point hitch 23 of a tractor to the 3 - point hitch mounting plates 20 of the invented fluffer . preferably , the operator can tilt the top side of the invented fluffer 100 forward using the 3 - point hitch , thereby elevating the distal end of the fluffer 100 for safety reasons while the fluffer is in the retracted , transport position . as shown in fig5 the directions of rotation of various parts are shown when the invented fluffer 100 is in use . the greek letter a shows the direction of travel of the invented fluffer 100 and the tractor 200 . the greek letter β shows the direction the gauge wheel 66 would rotate . the greek letter γ shows the direction of the rotation of the drum pickup 42 . the invented fluffer 100 has two positions , a retracted , transport position and an extended , operation position . as shown in fig2 and 6 , the retracted , transport position is where the hydraulic ram ( not shown ) is moved into a shortened state , thereby swinging the pickup frame 30 and the pickup assembly 40 rearward in relation to the tractor 200 . this position is preferred for transportation due to the fact that the tractor - fluffer unit ; is at its narrowest . the invented fluffer 100 can alternatively be moved into a retracted , transport position by hand , without the use of a hydraulic ram . as shown in fig1 and 4 , the extended , operation position is the position that the fluffer 100 is in when in operation in the field fluffing beans or hay . if the invented fluffer 100 is in the retracted , transport position , a hydraulic ram is preferably used to move the pickup frame 30 and the pickup assembly 40 outward in relation to the tractor 200 . while it is preferred that the pickup frame 30 and the pickup assembly 40 be rotated to an angle that is perpendicular to the forward direction of travel of the tractor , other angles are possible , and may be necessary depending on the needs and wishes of the operator of the fluffer 100 . the fluffer 100 can be moved into the extended , operation position by hand , without the use of a hydraulic ram . it is also envisioned that a dual fluffer model ( not shown ) of the invented fluffer 100 may be manufactured . as such , an additional pickup frame 30 and an additional pickup assembly 40 would be mounted on the proximal end of the hitch attachment assembly 50 . the operator , would then be able to swing one of the fluffers 100 to the left of the tractor 200 and one of the fluffers 100 to the right of the tractor 200 , thereby allowing the operator to fluff a field in one - half the time required if only one fluffer pickup drum 42 was used . although this invention has been described above with reference to particular means , materials and embodiments , it is to be understood that the invention is not limited to these disclosed particulars , but extends instead to all equivalents within the scope of the following claims . | 0 |
the process of the present invention begins with the selection of an appropriate structural composition through which microchannels or nanochannels are desired . the well known terms microchannel and nanochannel are considered to be interchangeable for the purposes of describing the present invention , with the general understanding that nanochannels are generally considered to be smaller in diameter than microchannels . a ductile structure ( i . e ., body ) should be selected which is appropriate for the intended use in accordance with known criteria . glass and glassy compositions are especially suitable for making ductile structures such as tubes , for example . moreover , other amorphous and / or semi - crystalline compositions , such as certain polymers , may also be used . ductility — the property of being permanently deformed by tension without rupture — is a critical property of an appropriate structural composition in accordance with the present invention . the ductile structure must have the ability to be drawn from a given cross sectional size to a smaller cross sectional size . the appropriate ductile structure can be formed into one or more tubes , the interiors of which are referred to herein as macro - channels . inside and outside surfaces of the tube ( s ) can be , in terms of cross - sectional shape , the same or different , and can be annular , round ( circular ), triangular , rectangular , hexagonal , other polygonal , or any other shape that is suitable for holding or forming a desired shape during a drawing process . cross - sectional shape of the tube ( s ) is not critical to the invention , but may be significant for some particular end - use of the article . once appropriate ductile structure is selected , an appropriate salt composition ( hereinafter often referred to simply as salt ) is selected . an appropriate salt composition may include a single salt compound or a mixture of different salt compounds . it is preferable ( but not always necessary ) that a salt be selected such that the following four conditions are met : a . the melting temperature of the salt should be lower than the drawing temperature of the ductile structure . thus , when the ductile structure is drawn , the salt will flow with the ductile structure . b . the melting temperature of the salt should be higher than the fusing temperature of the ductile structure . thus , when the final bundle is fused , the salt maintains the shape of the channels and prevents collapse thereof . c . the ions in the salt should match the ions in the ductile structure or be inert with respect thereto so that any ion exchange between the ductile structure and the salt either does not alter the composition of the ductile structure , or any such alteration is not deleterious to the application for which the microchannel article is intended . d . the salt should be soluble in water or another solvent that does not dissolve or etch the ductile structure to any significant extent . e . any possible toxicity or other hazard of the salt or salt solution should be considered and mitigated in cases where such minimization would be prudent for safety and / or environmental purposes . at least one tube made of an appropriate ductile structure is loaded with an appropriate salt composition . the tube may be loaded with powdered or crystalline salt grains or the inside of the tube may be coated with a layer of salt which does not necessarily completely fill the tube . one can proceed with a bundle of salt - filled tubes . fig1 shows , as an example , bundle 10 of glass tubes 12 having hexagonal outside surfaces 14 and round inside surfaces defining macro - channels 16 , the invention not being limited to those particular shapes . the macro - channels 16 contain an appropriate salt composition 18 . drawing , bundling , and slicing preferably proceed as taught in the published patent applications referenced above . in the drawing process , the glass tubes are heated to the softening point and fused into a monolith . the salt is melted and the melted salt fills the tube , preventing collapse and minimizing the formation of collapsed and / or misshapen microchannels . drawing , bundling , and slicing can be repeated to produce a preform having the desired dimensions of the desired article are obtained . there are no limitations associated with dimensions of the article , including , for example , size , aspect ratio , number of channels , size of channels , and spacing of channels . fig2 shows the bundle of glass tubes after drawing and fusing into a preform 20 . the glass monolith 22 has well - formed , salt - filled microchannels 24 . the salt composition is subsequently dissolved by a solvent and removed from the preform . the preform can be simply immersed in water to dissolve the salt , leaving behind well - preserved channels having little or no collapsing or other distortion . the water may be heated and / or agitated ( by circulating , stirring or ultrasonication , for example ) to further promote the dissolution and removal of the salt . the water may also be forced through the channels in cases where the salt simply coats the inside of each channel . the resulting microchannel or nanochannel glass may be rinsed by forcing water through the channels to remove any remaining salt . fig3 shows an example of a microchannel glass 30 article made from a preform such as that shown in fig2 . the microchannel glass article 30 comprises a glass monolith 22 which defines a plurality of microchannels 26 . referring to fig4 , bundling can be accomplished by inserting a plurality of tubes 12 into a larger tube ( sheath ) 32 to form a sheathed bundle 40 . this can be especially beneficial for the final bundling step because it will generally result in an article having a thicker , more robust outer surface . glass tubes 12 have hexagonal outside surfaces 14 and round inside surfaces defining macro - channels 16 , the invention not being limited to those particular shapes . the macro - channels 16 contain an appropriate salt composition 18 . the sheath 32 can be comprised of the same ductile structure as the tubes 12 or a different composition . voids 42 created by shape mismatches can optionally be filled with filler rods 44 , can be comprised of the same ductile structure as the tubes 12 or a different composition . referring to fig5 , final bundling is generally followed by fusing to produce a monolithic preform 50 . the preform 50 comprises a monolith 34 with well - formed , salt - filled microchannels 24 . fig6 shows the microchannel glass article 60 after the salt has been removed . the microchannel glass article 60 comprises a glass monolith 34 which defines a plurality of microchannels 26 . a glass tube comprised of schott 8330 © glass ( similar to corning pyrex ©) was provided . the tube had a length of 1000 mm , an outside diameter of 25 mm , and an inside diameter of 3 mm . the tube was filled with powdered kcl and drawn at about 860 ° c . to form a fiber having an outside diameter of 0 . 7 mm . the fiber was cut into 650 mm lengths , bundled into a hexagonal bundle , and drawn again at 870 ° c . to form a second fiber having an outside diameter of 0 . 7 mm . the second fiber was cut into 200 mm lengths , bundled into a shott 8330 © tube ( sheath ) having a length of 600 mm , an outside diameter of 24 . 5 mm , and an inside diameter of 22 mm , and heated at 700 ° c . under vacuum to fuse the bundled tubes and sheath together to form a fused bundle . the fused bundle was allowed to cool and cut transversely to the drawing direction into to form a plurality of preforms of various lengths ranging from 0 . 1 cm to 5 cm . the preforms were immersed in distilled water to dissolve the salt , rinsed by forcing water through the channels , and dried to form microchannel glass . microchannel glass was made in accordance with example i with the exception that the salt composition comprised nacl and kcl such that the ratio of na to k was the same as that of the glass composition . using the method of the present invention , many advantages and benefits can be realized , including but not limited to the following : 1 . microchannel and / or nanochannel glass may be produced from commercial off the shelf materials , minimizing costs . 2 . the glass composition can be a chemically durable , lead free glass for which a matching , easily etched glass is not commercially available . 3 . the aspect ratio of the microchannels or nanochannels can be much higher because the dissolution rate of the salt can be high and the contrast in dissolution rate of the salt and glass can be extremely high . 4 . the preferred dissolution process utilizes water , a non - hazardous solvent , instead of hazardous acid required by prior methods . moreover , the process generates a non - hazardous salt solution that can be recycled and reused . 5 . the use of salt in accordance with the present invention is feasible at high temperatures that would be pernicious to organic filler materials . microchannel and nanochannel glass have many applications including detectors , filters , catalyst supports . while there has been shown and described what are at present considered the preferred embodiments of the invention , it will be obvious to those skilled in the art that various changes and modifications can be prepared therein without departing from the scope of the inventions defined by the appended claims . | 2 |
since the development for wireless and cable network has grown rapidly , the demand for higher transmission speed and bandwidth has also increased relatively . the present invention integrates both wireless and cable network communication system to enhance the signal transmission efficiency and also at the same time reduces the system complexity . the present invention can apply on integrated optical communication network , wireless communication network and wavelength - division multiplexing ( wdm ) system . please refer to fig1 for a diagram schematically showing the architecture of the present invention where dash line represents traveling path for electrical signal and thick line represents traveling path for optical signal . the present invention comprises an optical modulation device 10 which is used to receive on - off keying ( ook ) signal from cable network and radio frequency ( rf ) signal from wireless network , the optical modulation device 10 then modulates the ook signal and the rf signal to an optical signal and generates an output optical signal . in addition , the rf signal is in phase shift keying ( psk ) format such as binary phase shift keying ( bpsk ), quadrature phase shift keying ( qpsk ) or octal phase shift keying ( opsk ) and the source of optical signal is laser . the modulated output optical signal is then transmitted to an optical splitter 20 via an optical fiber transmission channel , and received by an optical receiving device 22 . the optical receiving device 22 can access the ook signal and rf signal from the output optical signal . the optical modulation device 10 further comprises two phase shifters 12 and 14 , a laser diode 16 and an electro - optic modulator ( mach - zehnder modulator ) 18 . the phase shifter 12 is responsible for receiving the rf signal and shifting the phase of the rf signal by 90 degrees and the phase shifter 14 is responsible for receiving the ook signal and shifting the phase of the ook signal by 90 degrees also . the laser diode 16 is used to generate an optical signal . the electro - optic modulator 18 is responsible of receiving the original ook signal and the ook signal from phase shifter 14 at one electrical receiving end , and receiving original rf signal and the rf signal from phase shifter 12 at another electrical receiving end . in addition , an optical receiving end of electro - optic modulator 18 is responsible for receiving the optical signal and bias the electro - optic modulator 18 to a v π / 2 position , so that it can effect the transmission characteristic of the optical signal , allowing optical signal to modulate with two signals received by the two electrical receiving ends ( ook and rf ) and generate an output optical signal to an optical fiber transmission channel . the optical receiving device 22 further comprises a low speed photo detector 28 and a high pass filter ( hpf ) 26 . the low speed photo detector 28 receives the output optical signal splitted from the optical splitter 20 and extracts the ook signal which can be used by optical fiber cable network 32 applications such as fiber - to - the - home ( ftth ) system . in addition , the present invention is compatible with existing optical receiving device at user ends , therefore , the users does not require any upgrade on their optical receiving devices . the high speed photo detector 24 receives the output optical signal splitted from the optical splitter 20 and output an electrical signal . the hpf 26 in combination with the high speed photo detector 24 can be used to receive the electrical signal and extract the rf signal , which can be used by wireless network 30 applications . the following will describe the procedure of the present invention in detail . at first , the optical modulation device 10 receives rf and ook signal , the rf signal will be received by the phase shifter 12 and having its phase shifted by 90 degrees and output to the electro - optic modulator 18 , similarly , the ook signal will be received by the phase shifter 14 and having its phase shifted by 90 degrees also and output to the electro - optic modulator 18 . the electro - optic modulator 18 has to electrical receiving ends and one optical receiving end , one electrical receiving end will receive one shifted rf signal and one un - shifted ook signal , the other electrical receiving end will receive one un - shifted rf signal and one shifted ook signal . the optical receiving end receives an optical signal generated by a laser diode 16 , and when the electro - optic modulator 18 &# 39 ; s bias is under v π / 2 state , the electro - optic modulator 18 can effect the transmission characteristic of the optical signal , allowing optical signal to modulate with two signals received by the two electrical receiving ends ( ook and rf ) and generate an output optical signal to an optical fiber transmission channel . after passing the optical fiber transmission channel , the output optical signal will be received by an optical splitter 20 and splitted into two signals . one of the two signals will be received by the low speed photo detector 28 and high speed photo detector 24 within the optical receiving device 22 , the high speed photo detector 24 combines with hpf 26 can allow low speed photo detector 28 to extract ook signal , which can be used by the optical fiber cable network 32 applications . in addition , after the high speed photo detector 24 receives the output optical signal , it will output an electrical signal ; hpf 26 will receive this electrical signal and extract the rf signal , which can be used by wireless network 30 applications . please refer to fig2 for another diagram schematically showing the architecture of the present invention where the optical receiving device 22 of the present invention is being substitute with alternating device . in this diagram , the optical receiving device 22 comprises a high speed photo detector 34 , a low speed photo detector 36 and a dc block 38 wherein the low speed photo detector 36 is combined with dc block 38 . the high speed photo detector 34 receives output optical signal splitted from the optical splitter 20 and extracts the rf signal from it , which can be used by wireless network 30 applications . whereas the low speed photo detector 36 receives output optical signal splitted from the optical splitter 20 and generates an electrical signal , which allows dc block 38 to receive this electrical signal and extract the ook signal from it , which can be further used by optical fiber cable network 32 applications . in order to proof the practicability of the present invention , please refer to fig3 for a diagram schematically showing the architecture of experimental system of the present invention . in this setup , it utilizes an ook signal from 1 . 25 g ( gb / s ) cable network and a psk signal from 625m ( mb / s ) wireless network as illustration . within the experimental system , the present invention can further install an optical filter 40 , an optical amplifier 42 and an optical filter 44 in order between the electro - optic modulator 18 and optical fiber transmission channel . the optical filter 40 will receive the output optical signal from the electro - optic modulator 18 and output the output optical signal after adjusting the output optical signal &# 39 ; s optical carrier power . as a result , when photo detect 46 and 48 receives the output optical signal , it will be in optimal condition . the optical amplifier 42 then receives and amplifies the output optical signal received from optical filter 40 and outputs the processed signal , allowing the signal strength of the output optical signal to attenuate slower within the optical fiber transmission channel . lastly , the optical filter 44 receives the output optical signal from the optical amplifier 42 and filter out noises within the output optical signal , the resulting output optical signal is transmitted to the optical fiber transmission channel . please refer to fig4 for a spectra diagram showing the output optical signal of the present invention after passing an optical filter . the electro - optic modulator 18 generates an output optical signal with one optical carrier , an ook modulated optical sideband , and one psk modulated optical sideband , as shown in fig4 . after transmission of optical fibers , only one optical coupler 20 is needed to separate the optical power for wireless and wired application . for wireless application , high speed photo receiver and a suitable rf band pass filter is used to receive the rf psk signals . the high speed photo receiver and the suitable rf band pass filter is a photo detector 48 and a band pass filter 52 respectively in fig3 . for baseband ( bb ) wired application , the optical carrier and psk optical sideband signal only contribute dc signals in bb . the dc terms can be easily removed using a dc block . the dc block is a dc block 50 in fig3 . only ook signals will be observed in bb . therefore , the present invention does not need a narrow band optical filter to separate the ook optical sidebands for different applications . please refer to fig3 and fig5 at the same time , the modulation method for the psk signal is phase shift modulation and modulation method for ook signal is amplitude modulation . in fig5 , it can be clearly seen that after applying phase shift modulation to the optical signal , the optical signal would not cause any signal at base band ( bb ) after the optical signal passed photo detector ; therefore , only the signal from amplitude modulation can be observed . as a result , the present invention can discern different signals from different channels by using different frequency band photo detector ; that is , the user does not require designing additional optical filters to discern signals from different channels . in addition , the electrical signal mentioned above is not limited to a single wavelength , which allows the present invention to apply on wavelength - division multiplexing systems . furthermore , the ook signal of the 1 . 25 gb / s cable network can be extracted by low speed photo detector 46 alone , and the psk signal of the 625 mb / s wireless network can be extracted by band pass filter 52 ( bpf ) alone . please refer to fig3 and fig6 at the same time , the experimental system of fig3 uses bit error rate tester ( bert ) 54 and 58 relatively to measure the bit error rate ( ber ) of the ook signal of the 1 . 25 gb / s cable network and the psk signal of the 625 mb / s wireless network after being reduced frequency by a mixer 60 . from fig6 , it can be seen that after both signal ( ook and psk ) passed the optical fiber transmission channel for over 25 kilometers , the power loss is lower than 0 . 5 db , which proofs that the present invention can overcome the obstacle of rf signal strength reduction caused by the optical fiber dispersion over long distance transmission . the present invention not only eliminates rf signal reduction caused by the optical fiber dispersion , it also allows user to discern rf signal from wireless network and ook signal from cable network without using any optical filters . the embodiments described above are only to exemplify the present invention but not to limit the scope of the present invention . therefore , any equivalent modification or variation according to the shapes , structures , characteristics and spirits discloses in the present invention is to be also included within the scope of the present invention . | 7 |
no claim of novelty is asserted for the sprinkler heads served by the present device but their construction and mode of operation are relevant to this invention and , therefore , they are discussed briefly hereinbelow . pendent - type : in fig1 - 7 there is shown a pendent - type sprinkler head 10 equipped with a threaded conduit 11 for conveying fluid from an overhead water supply ( not shown ) through a fluid - emitting orifice 12 , suspended beneath the sprinkler head housing 13 on a pair of guide rods one of which is shown as 14 in fig1 and 2 is a circular baffle plate 15 and a valve assembly 16 . said baffle plate receives the fluid emitted from orifice 12 and disperses the stream in a generally uniform pattern in finely divided form . in fig1 - 3 said guide rods are shown in a lowered position with the baffle plate 15 and valve assembly 16 in an activated or discharge mode , that is , positioned to receive the stream which flows from orifice 12 , whereas , fig4 - 7 show the guide rods in a raised position with the baffle plate and valve assembly in a non - discharge mode . the baffle plate 15 is serrated to distribute the stream evenly in all directions and there is secured to its topside a flat circular disc 17 upon which there is disposed a tacky film 18 for contacting the orifice 12 and obturating fluid flow when the baffle plate 15 and valve assembly 16 are in a non - discharge mode . the shut - off device for the pendent sprinkler head 10 is shown generally as 22 in fig1 - 7 . this device consists essentially of a hollow cylindrical body equipped at the bottom end with a hexagonal opening and at the top or opposing end with a contoured opening 24 and a cavity 27 for receiving the flange 19 of said sprinkler head and the sprinkler head housing 13 . the cavity sidewalls 31 extend downwardly for about half the length of said body and terminate in a flat base 25 which extends laterally to provide the circular space or cirque shown as 34 in fig2 and 6 . centrally disposed within said cavity is a circular projection 29 which extends upwardly from the base 25 to provide a support means for a flat circular seat identified as 26 in fig2 and 6 . the seat 26 is a tubular member fitted onto an accommodating segment of projection 29 for receiving baffle plate 15 and spherical segment 30 ( fig2 ) when the shutoff device 22 is impressed onto an activated sprinkler head 10 . the sidewalls 31 of the cavity 27 include opposing apertures in the form of horizontally disposed channel members 32 and 33 . when viewed externally these channel members may appear identical but a careful examination reveals that they lie on a bias to the extent shown in fig2 and this obliquity provides means for frictionally engaging the projection members 20 and 21 of flange 19 . when the shut - off device 22 is impressed onto an activated sprinkler head 10 and rotated in a clockwise manner . included in the sidewalls 31 of said cavity is a horizontally disposed pattern of vent holes . an activated sprinkler head 10 emits a liquid stream under some considerable pressure and the present invention allows an installer to abate this difficulty by providing within said sidewalls a plurality of apertures through which water can be diverted and released as the device is being installed . operation : the sprinkler heads served by the present invention are equipped with temperature - responsive films which retain the shut - off valve within the fluid - emitting orifice by adhesive means ; however , any exposure to incendiary temperatures , that is , temperatures in excess of about 105 ° c . will cause the adhesive to melt so that water pressure within the conduit 11 can expel the valve assembly and permit fluid to be discharged from orifice 12 . the fluid thus emitted comes into contact with the baffle plate 15 and directs the liquid stream evenly to adjacent areas in the form of a finely divided spray . the present device obturates fluid flow by returning the valve assembly 16 to the fluid - emitting orifice ( fig4 ). this shut - off stage is achieved by positioning the shut - off device 22 beneath the activated sprinkler head 10 in such manner that the cutout segments 35 and 36 are in registry with projection members 20 and 21 of flange 19 ( fig1 and 2 ). when registry is assured the device 22 is impressed upwardly onto the sprinkler head 10 as a result of which the tubular seat 26 contacts the underside of baffle plate 15 and brings the valve assembly 16 into shut - off engagement with the fluid - emitting orifice 12 ( fig4 and 5 ). locking is achieved by rotating the shut - off device 22 in a clockwise direction until projection members 20 and 21 are brought into frictional engagement with channel members 32 and 33 ( fig6 and 7 ). a sprinkler head 10 secured in this manner may be removed by simply rotating the shut - off device in a counterclockwise direction . alternatively , the shut - off device 22 may be left unattended without risk because it is fabricated from compositions which melt at incendiary temperatures . accordingly , any rise in temperature to critical levels , that is , temperatures in excess of about 105 ° c . will cause the shut - off device 22 to lose its hold and automatically return the sprinkler head to an activated mode . sidewall type : fig8 - 14 illustrate a shut - off device 52 for a sprinkler head of the sidewall type 40 . this sidewall sprinkler 40 is essentially identical in operation to the pendent - type sprinkler shown as 10 in fig1 - 7 except that the baffle plate 45 consists essentially of projecting fingers , guide rod 44 and a vertically disposed arcuate deflector 65 for directing water in a given direction . the shut - off device which serves this sidewall sprinkler head 40 is the hollow cylindrical body shown generally as 52 in fig8 - 14 . this device is characterized by a hexagonal orifice 53 at one end and includes at the opposite end a contoured circular orifice 54 for receiving the projecting members 50 and 51 of flange 49 . extending downwardly from orifice 54 is a cavity 57 defined by downwardly extending sidewalls 61 and the flat laterally extending base shown as 55 in fig9 and 13 . centrally disposed within said cavity and extending upwardly from the base 55 is a circular projection 59 which terminates in a flat support upon which there is secured the tubular seat identified as 56 in fig9 - 11 and 13 . the upwardly projecting member 59 is centrally disposed within the cavity 57 so that its sidewalls and the cavity sidewalls 61 combine to form a circular space or cirque 64 for receiving the deflector 67 of the sprinkler head 40 when the shut - off device is impressed onto an activated sprinkler head . included within the sidewalls of cavity 57 are apertures in the form of horizontally disposed channel members 62 and 63 which extend through the walls of the shut - off device 52 . these channel members are obliquely biased to provide means for frictionally engaging the projection members 50 and 51 of flange 49 when the shut - off device 52 is impressed onto an activated sprinkler head 40 and rotated in a clockwise direction . in fig9 only the obliquity of channel member 62 can be seen in the drawings but channel member 63 is identically disposed . operation : the shut - off device 52 is installed by aligning its cutout segments 65 and 66 with the projection members 51 and 51 of the sprinkler head flange 49 and impressing the former upwardly with a thrusting force greater than the pressure exerted by the liquid stream emitted from orifice 42 . the plurality of holes within the sidewalls of the device 52 provide a form of pressure release by allowing water entrapped within the cavity 57 to escape and thus facilitate the installation procedure . the upward thrust of the shut - off device 52 onto the sprinkler head 40 brings the underside of baffle plate 45 into engagement with tubular seat 56 and causes the valve assembly 46 and film 48 to engage the fluid emitting orifice 52 where it creates a seal against further fluid discharge . at this juncture the projection members 50 and 51 are in view and can be clearly seen through channel members 62 . once the shut - off device has been installed and the flow of liquid has been stanched the sprinkler head 40 is secured against inadvertent discharge by turning said device in a clockwise direction so as to bring projection members 50 and 51 of flange 49 into engagement with the biased segment of the channel members 62 and 63 ( fig1 and 14 ). a sprinkler head secured in this manner can be reactivated by rotating the shut - off device 52 in a counterclockwise direction and withdrawing same in a downward fashion . alternatively , the shut - off device 52 can be allowed to remain on the sprinkler head without jeopardy because the device is fabricated from thermoplastic compositions which melt at sprinkler activating temperatures so that in case of a fire emergency the shut - off device 52 will simply melt , separate and return the sprinkler head to an operable mode . this invention has been described by reference to precise embodiments but it will be appreciated by those skilled in the art that this invention is subject to various modifications and to the extent that those modifications would be obvious to one of ordinary skill they are considered as being within the scope of the appended claims . | 0 |
fig1 shows an embodiment in accordance with the invention of gan edge emitting laser structure 100 . substrate 105 is typically al 2 o 3 or sic with gan buffer layer 110 separating substrate 105 from n - gan layer 120 . refractory metal elog masks 130 is a layer that overlies n - gan layer 120 . refractory metal elog masks 130 may be made from ti , pt , w , re mo , cr , ni , pd or other suitable refractory metal . elog layers , n - gan layer 138 , n - algan lower cladding layer 140 , ingan separate confinement heterostructure layer 150 , ingan multiple quantum wells 160 , algan electron blocking layer 170 which prevents electron leakage , ingan separate confinement heterostructure layer 180 , p - type algan upper cladding layer 190 and p - type gan layer 195 overlie refractory metal elog mask 130 . n - metal contact 134 contacts refractory metal layer 130 to provide efficient current injection into active region 199 of gan edge emitting ridge waveguide laser structure 100 . p - metal contact 136 is positioned over p - type gan layer 195 . typically gan edge emitting laser structure 100 is made by taking substrate 105 , typically al 2 o 3 or sic and depositing gan buffer layer 110 over it to a typical thickness of about 30 nm . then planar n - type gan layer 120 is deposited over gan buffer layer 110 as shown in fig2 a . refractory metal elog mask 130 is deposited by sputtering or evaporation and patterned by chemically assisted ion beam etching ( caibe ) or reactive ion - etching ( rie ) over n - gan layer 120 . then elog growth is started using refractory metal elog mask 130 for growing n - gan layer 138 to a typical thickness of about 1 to about 2 μm ; n - algan lower cladding layer 140 has a typical thickness of about 1 μm ; active region 199 which comprises ingan separate confinement heterostructure layer 150 has a typical thickness of about 0 . 1 μm , ingan multiple quantum wells 160 , algan electron blocking layer 170 has a typical thickness of about 20 nm , and ingan separate confinement heterostructure layer 180 has a typical thickness of about 0 . 1 μm ( see fig1 ); p - type algan upper cladding layer 190 has a typical thickness of about 0 . 5 μm and p - type gan layer 195 has a typical thickness of about 0 . 1 μm . fig2 d shows etching typically by caibe or rie to make the typical wave guide structure by etching through p - type gan layer 195 and into p - type algan upper cladding layer 190 . a second etch by caibe or rie down to refractory metal layer 130 is performed as shown in fig2 e to provide a contact area for n - metal contact 134 . finally , n - metal contact 134 and p - metal contact 136 are deposited and annealed . fig3 shows an embodiment in accordance with the invention of gan vcsel laser structure 300 having elog n - and p - refractory metal masks with a lower dbr elog mask . substrate 305 is typically al 2 o 3 or sic with gan buffer layer 310 having a typical thickness of about 30 nm and separating substrate 305 from n - gan layer 315 with a typical thickness of about 1 μm to about 2 μm . lower dielectric distributed bragg reflector ( dbr ) 318 overlies gan buffer layer 310 . elog n - gan layer 320 with a typical thickness of about 3 μm overlies lower dielectric dbr 318 and n - refractory metal elog mask 330 is a layer that overlies elog n - gan layer 320 . n - refractory metal elog mask 330 may be made from ti , pt , w , re mo , cr , ni , pd or other suitable refractory metal . care must be taken to place n - refractory metal elog mask 330 at a null of the standing wave set up between lower dielectric dbr 318 and upper dielectric dbr 319 . n - refractory metal elog mask 330 typically has a thickness of about 50 nm or less . elog layer n - gan 340 with a typical thickness of about 1 μm to about 2 μm , ingan multiple quantum well active region 345 , p - algan layer 346 having a typical thickness of about 20 nm and p - gan layer 350 with a typical thickness of about 1 μm to about 2 μm overlie refractory metal elog mask 330 . p - refractory metal elog mask 321 is a layer that overlies p - gan layer 350 . care must be taken to place p - refractory metal elog mask 321 at a null of the standing wave set up between lower dielectric dbr 318 and upper dielectric dbr 319 . p - refractory metal elog mask 321 typically has a thickness of about 50 nm or less . p - doped refractory metal elog mask 321 may be made from ti , pt , w , re mo , cr , ni , pd or other suitable refractory metal . p - gan layer 360 with a typical thickness of about 1 μm to about 5 μm overlies p - doped refractory metal elog mask 321 and upper dielectric dbr 319 . n - metal contact 334 contacts n - refractory metal layer 330 and p - metal contact 336 contacts p - refractory metal layer 321 to provide efficient current injection into vcsel structure 300 . typically , gan vcsel structure 300 is made by taking substrate 305 , typically al 2 o 3 or sic and depositing gan buffer layer 310 to a typical thickness of about 30 nm over it . then planar n - type gan layer 315 is deposited to a thickness of about 1 μm to about 2 μm over gan buffer layer 310 as shown in fig4 a . lower dielectric dbr 318 is then deposited and patterned as shown in fig4 b . lower dielectric dbr 318 serves as an elog mask for elog of n - gan layer 320 having a typical thickness of about 3 μm and is shown in fig4 c . then n - refractory metal elog mask 330 is deposited and patterned as shown in fig4 d . with reference to fig4 e , n - refractory metal elog mask 330 is then used to elog grow n - type gan layer 340 having a typical thickness of about 1 μm to about 2 μm , ingan multiple quantum well active region 345 , p - type algan layer 346 with a typical thickness of about 20 nm and p - type gan layer 350 with a typical thickness of about 1 μm to about 2 μm . after growing p - doped gan layer 350 , p - refractory metal elog mask 321 is deposited on p - doped gan layer 350 and patterned as shown in fig4 f . elog of p - doped gan layer 360 is then performed to a typical thickness of about 1 μm to about 5 μm using p - refractory metal elog mask 321 as shown in fig4 g . upper dbr 319 is then deposited on p - doped gan layer 360 and etched as shown in fig4 h . finally , as shown in fig4 i , etches are performed down to refractory metal layers 321 and 330 where n - electrode 334 and p - electrode 335 are deposited , respectively . fig5 shows an embodiment in accordance with the invention of gan vcsel laser structure 500 having an elog p - refractory metal mask and using a lower dbr deposited on an n - gan layer after removal of the substrate by laser liftoff or other suitable technique . n - type gan layer 520 with a typical thickness of about 4 μm has n - contacts 534 attached on the bottom surface along with lower dbr 518 . ingan multiple quantum well active region 545 overlies n - type gan layer and is topped by algan layer 546 having a typical thickness of about 20 nm . p - type gan layer 547 having a typical thickness of about 0 . 2 μm to about 2 μm overlies algan layer 546 . p - refractory metal elog mask 535 is a layer that overlies p - type gan layer 547 and elog p - type gan layer 560 having a typical thickness of about 1 μm to about 4 μm overlies p - type gan layer 547 . care must be taken to place p - refractory metal elog mask 535 at a null of the standing wave set up between lower dielectric dbr 518 and upper dielectric dbr 519 . p - refractory metal elog mask 321 typically has a thickness of about 50 nm or less . upper dbr mirror 519 sits on elog p - type gan layer 560 and p - type electrodes 536 are attached to p - type refractory metal layer 535 . typically , gan vcsel structure 500 may be made by taking substrate 505 , typically al 2 o 3 or sic and depositing gan buffer layer 510 to a typical thickness of about 30 nm over it . planar growth is performed for n - type gan layer 520 having a typical thickness of about 4 μm , ingan multiple quantum well active region 545 , algan layer 546 having a typical thickness of about 20 nm and p - type gan layer 547 with a typical thickness of about 0 . 2 μm to 2 μm as shown in fig6 a . p - refractory metal elog mask 535 is deposited on p - type gan layer 547 and patterned as shown in fig6 b . then elog growth of p - gan layer 560 to a typical thickness of about 1 μm to about 4 μm is performed as shown in fig6 c . upper dbr 519 is deposited on p - gan layer 560 and patterned as shown in fig6 d . substrate 505 is subsequentally removed by laser liftoff leaving the vcsel structure shown in fig6 e . lower dbr 518 is deposited on the bottom of gan buffer layer 510 and patterned as shown in fig6 f . finally , an rie or caibe etch is performed through p - gan layer 560 down to p - refractory elog metal mask 535 to deposit p - type electrodes 536 and n - type electrodes 534 on the bottom of gan buffer layer 510 . | 7 |
fig1 a - 1c show a device for guiding and affixing an endoscope . this device comprises a guidance unit 1 , a clamp 2 with metal washers 5 mounted to its ends , a thrust washer 3 and an axially displaceable shell 4 . the guidance unit 1 is provided with a seat 6 for adapters . in this embodiment the seat 6 comprises an external thread corresponding to the plug of the most commonly used inspection aperture which closes a machine , whereby the device also may be used without an adapter . be it borne in mind that a variation of this embodiment calls for the seat 6 being the matching part of a bayonet or a quick - connect . this applies also to the illustrative embodiments described below of device and adapter . the seat 6 is part of the guidance unit 1 and its diameter is less than that of the next part of the guidance unit 1 . this produces an offset forming an axially facing rest surface 12 which extends toward the larger diameter and bounding the depth of threading . in the next part the guidance unit 1 comprises a knurled surface 13 and a fine thread 15 beyond a projection in its end part to seat the axially displaceable device 4 . the guidance unit 1 is provided with a cylindrical stepped bore , with the smaller bore 8 corresponding to the largest of the outer diameters of the applicable endoscopes and , following an abrupt transition , to a bore part 11 , corresponding to the outside diameter of the clamp 2 with its metal washers 5 , provision being made that the tolerances allow for play . the entire bore is burnished . the larger bore part 11 of the guidance unit 1 seats first the clamp 2 with its externally burnished metal washers 5 bonded or vulcanized to the ends of the clamp and then the thrust washer 3 . the clamp 2 comprises an elastomeric such as a rubber resistance to kerosene and oil , preferably an acrylonitrile butadiene rubber , and assumes the shape of a hollow cylinder . the inside diameter of the unstressed clamp 2 and of the metal washers 5 matches that of the bore 8 . the inside diameter of the clamp 2 inclusive the metal washers 5 may vary according to a predetermined offset in relation to the shore hardness of the clamp and the outside diameter of the endoscope being used , so that the clamps are characterized by different colors to display those deviations . a possible reducing part made of plastic matching the funnel - shaped endoscope insertion opening 9 of the axially displaceable device 4 and the inside diameter of the clamp 2 being used , is made with the same color as the clamp coding and may be slipped onto the axially displaceable device 4 . the thrust washer 3 is made of a sintered metal and its outside / inside diameters match those of the clamp 2 having the largest inside diameter . the thrust washer 3 is formed at its top and bottom sides with grooves 14 extending radially over the entire width but mutually offset by 90 °. the axially displaceable device 4 is provided at tis front with an inside thread 15 a matching thread 15 on the outside of the guide unit 1 and , by means of this thread , can be moved axially . a funnel - like part 9 at the end and tapering from the outside to the inside merges into a through - bore of the same inside diameter as that of the previously described parts 3 , 2 , 8 . the exit from this through - bore is at a burnished pressure surface 10 acting on the thrust washer 3 and of the same outside diameter . the outside diameter of the axially displaceable device is constant and has a knurled part 13 which corresponds to that of the guidance unit 1 . the surface is knurled over a restricted area . by shifting the device 4 on the thread of the guide unit 1 , and in a predetermined direction , the clamp 2 is compressed or relieved by means of the thrust washer 3 and thereby changes its inside diameter . an endoscope inserted through the funnel - like opening 9 of the axially displaceable device and through the subsequent borehole can be moved to - and - fro to locate the observation point while being guided with little diameter tolerance relative to the clamp 2 , or its enclosed by this clamp and hence fixed in place . the components of the above described device and adapter as well as those of the embodiment below shall be made of corrosion - proof materials or be provided with corrosion - proof coating such as eloxal [ anodized coating ]. fig2 a and 2b show another illustrative embodiment of the device of the invention for guiding and affixing an endoscope . the device consists of a guidance unit 16 with a seat 6 for the adapter , three spring guides 22 , the associated helical springs 23 , a clamp consisting of three segments 17 , two expansion springs 18 , three drive pins 19 , three guidance pins 21 and a fixation pin 24 . the guidance unit 16 comprises a through - bore . this through - bore 8 is cylindrical in the area of the adapter seat 6 , but then merges into a conical part 25 extending as far as the exit at the insertion side of the clamp . in this area too there is the largest outside diameter of the guidance unit 16 , said diameter being stepped toward the seat 6 for the adapter . bores 26 equidistant from the sealing surface and 120 ° apart start from this diameter , issuing ; in the burnished conical inner bores 25 . the end surface 27 between the largest diameter portion and the next stepped smaller diameter comprises blind holes 28 which are 120 ° apart . the rod - like spring guides 22 made of hardened steel are forced into these blind holes 28 . the helical springs 23 are compressed to move onto the spring guides 22 . that part of the guidance unit 16 formed by the smaller outside diameter comprises a groove 29 at its surface which is offset by 60 ° from one of the blind holes 28 . this groove extends from the end face 27 to nearly the beginning of the next step following the seat 6 for the adapters . at this site there is a through - bore 30 in the groove , issuing into the conical inner bore 25 and which serves in dismantling the fixation pin 24 of the axially displaceable device 20 . the equal segments 17 made of a non - metallic material form the clamp which in this case comprises a cylindrical borehole widening like a funnel at the endoscope insertion side . two annular grooves 31 inside the bores receive the annular expansion springs 18 consisting of leaf - spring steel the ends of which overlap even when the spring is maximally extended . the grooves 31 are such that the entire spring , including the overlapping parts of the expansion springs 18 are released in the grooves . on the outside the clamp is provided with a conical slope matching the conical inside bore 25 of the guidance unit 16 and by means of a step terminates in a cylindrical part . in clamp parts 17 are located boreholes 33 at 120 ° to each other and equidistant to the outer edge , namely one per segment center , which issue into the funnel - like exit of the clamp . longitudinal grooves 32 are present at the segment centers in the conical outer part of the clamp and at 120 ° to each other , the bottoms of said grooves being parallel to the cylindrical inner bore . the grooves 29 serve to guide the segments and match by their lengths the smallest / largest inside diameters of the clamp resulting from displacement . the clamp or its segments 17 with the expansion springs 18 are inserted into the conical part of the bore 25 of the guidance unit 16 . the guidance pins 21 are pressed so far into the bore 26 of the guidance unit 16 that some play remains relative to the bottom of the groove 32 in the segments 17 of the clamp . the grooves 32 are somewhat wider than the diameter of the guidance pins 21 such that the pins have some play and permit shifting the segments 17 . the axially displaceable device 20 comprises a continuous bore with offset inside diameters . at the endoscope insertion side that bore corresponds to the largest outside diameter of the guidance unit 16 ; at the adapter side , it corresponds to the stepped outside diameter in which grooves 29 of the guidance unit 16 are formed . the bores are made to fit with play and are burnished . the outside diameter of the axially displaceable device 20 is constant . the surface is provided with knurling 34 over a limited area . through - bores 37 parallel to the axis but mutually offset by 120 ° are present at the adapter side starting at the end face of the axially displaceable device 20 . the through - bores 37 serve to guide the spring guides 22 . axially toward the insertion end and offset by 60 ° relative to the end - face bores 37 there is a bore 36 from the surface which issues into the larger inside diameter section and receives the fixation pin 24 . another three bores 35 are present in the end part which are mutually offset by 120 ° and equidistant to the outer edge : they receive the drive pins 19 . the axially displaceable device 20 is moved over the guidance unit 16 . the spring guides 22 are provided with a matching rest with play in the bore 37 . the fixation pin 24 is pressed into the bore 36 to an extent that play remains relative to the bottom of the groove 29 in the guidance unit 16 . next the drive pins 19 are forced into the bores 35 of the axially displaceable device 20 and are received with play by the bores 33 of the segments 17 of the clamp . if now the axially displaceable device 20 is moved in a predetermined direction , it shall be secured against rotation by means of the groove 29 of the guidance unit 16 and the fixation pin 24 . the drive pins 19 transmit the relative motions of the axially displaceable device 20 by means of the bores 26 to the clamp segments 17 . when the device of the invention is affixed , with or without adapter , to an inspection aperture and when en endoscope with least or largest diameter is inserted into the funnel - like opening of the clamp segments 17 while the axially displaceable device 20 is fully withdrawn , the axially displaceable device 20 is moved forward by the holding pressure yielding and by the force of the helical springs 23 , then the clamp segments 17 are driven along , the inside diameter of the clamp is reduced and matches that of the endoscope which , with little diameter tolerance relative to the clamp , can be guided to move to - and - fro to locate the observation point . upon releasing the axially displaceable device 20 , the helical springs 23 apply a corresponding compression to the axially displaceable device 20 and thereby , by means of the drive pins 19 , to the clamp segments 17 which then enclose the endoscope with a corresponding force , fix it in its position and prevent shifting . fig3 and 5 show illustrative embodiments of adapter in accordance with the invention used in relation with the device for guiding and affixing an endoscope shown in fig1 a - 1c or 2a , 2b . fig3 is an embodiment in the form of one integral part and comprising both stepped diameters and a through - bore 8 . the largest diameter corresponds to the device of the invention shown in fig1 a - 1c or 2a , 2b and is constant over the length of the coupling for this device . the surface of this part is knurled . the next and offset part is such that it matches , in length and diameter , the particular vicinity of the inspection aperture , that is , the adapter of the present invention may assume several embodiment modes . the next stepped part is provided with a thread 39 corresponding to threads in the applicable inspection aperture . in this case as well as regarding the other embodiments , any design matching the particular inspection aperture is conceivable . the bore 40 in this part is cylindrical and extends next through the length of the central part in the form of a conically flaring bore 41 as far as the transition to the coupling shown here with an inside thread 42 . in this case the adapter is made of a high - strength , tough material for the application to the smallest inspection aperture together with the largest likely endoscope diameter . fig4 shows a further embodiment of an adapter of the invention . this adapter consists of a guidance housing 43 , a swivel - joint ball 44 , a fixating pin 45 and a cap means in the form of an axially displaceable device 46 . the guidance housing 43 comprises stepped outside diameters . the part with the smaller diameter on the inspection side is matched to the inspection apertures . the next adjacent part with a larger diameter is provided with a fine thread to seat the axially displaceable cap means device 46 . the conical bore 49a through the guidance housing 43 terminates by its smaller diameter in a burnished spherical socket 47 seating the swivel - joint ball 44 . four boreholes 48 offset from one another by 90 ° and equidistant from the edge start at the periphery and issue in the socket . fixating pins 45 are pressed into said boreholes 48 and slightly project into the spherical socket 47 . the swivel - joint ball 44 comprises a through - bore having an internal thread 42 or matching the coupling of the device of the invention of fig1 a - 1c or 2a , 2b . that part of the swivel - joint ball 44 which is received by the spherical socket 47 of the guidance housing 43 comprises four end - faced millings 58 mutually offset by 90 ° of maximum width and entered by the fixating pins 45 . the depth of the millings is such that a predetermined maximum adjustment angle of the swivel - joint ball 44 is determined by the fixating pins 45 of which one rests against the end of one of the grooves . the swivel - joint ball 44 is made of a wear - resistant material of low friction , or coated with it . the axially displaceable device 46 matches by its outside diameter that of the device of the invention shown in fig1 a - 1c or 2a , 2b and comprises a knurling 49 at its periphery over a restricted area . part of the through - bore is finely threaded so that the axially displaceable device 46 can be moved over the outside thread of the guidance housing 43 . following an undercut there is a burnished spherical socket 50 providing the matched bearing of the swivel - joint ball 44 to the spherical socket 47 of the guidance housing 43 , whereupon the through - bore issues at the end of the axially displaceable device 46 . if the axially displaceable device 46 is moved in either direction , the swivel - joint ball 44 may be moved or shall be fixed . in conjunction with the device of the invention of fig1 a - 1c or 2a , 2b being mounted at an inspection aperture , this device may be pivoted over a limited range , that is , a rigid endoscope will allow a wider field of inspection and furthermore the endoscope may be affixed to this area at a given pivot angle . fig5 shows an illustrative embodiment of the adapter of the invention which permits inspecting inside spaces through detached tube or pipe connections . the adapter consists of an elastic clasp 58 , connectors 52 , a coupling 53 and a fixating pin 54 . the coupling 53 is cylindrical and is provided with knurling at its surface over a limited area . the outside diameter corresponds to that of the device of the invention of fig1 a - 1c or 2a , 2b . the surface subtended by the inside diameter is fitted with threads 42 or is designed in relation to the coupling of the device of the invention of fig1 a - 1c or 2a , 2b . two mutually opposite blind - hole threads 55 extend in the axial direction and at 90 ° offset from them there is a bore 56 to receive the fixation pin 54 . the bore 56 and the fixation pin 54 are so matched that after the fixation pin 54 has been pressed - in , it shall project by the thickness of the sheetmetal of the elastic clasp 58 . the elastic clasp 58 is made of leaf - spring steel . the central part is matched to the outside diameter of the coupling element 53 and comprises boreholes 57 , 59 aligned with those of coupling 53 . the bores 57 comprise countersinks . the central bore 60 is somewhat larger than that of the coupling 53 . mutually opposite legs of the same width bu narrower than the central part start from this central part . the legs end are bent by about 225 °. the inward drawn part is shaped in such manner -- taking into account prestressing which may effect the sheetmetal thickness -- that the curvature of the tube surface matches that of the tube end serving as the inspection aperture . the elastic clasp 58 comprises punched numerals corresponding to the tube or pipe diameter for its application , i . e ., elastic clasps 58 for different pipe diameters can be connected by the connection elements 52 , two countersunk screws , with the coupling 53 . the invention of the adapter with the device of fig1 or 2 now can be slipped by its bent ends onto a pipe end serving as the inspection aperture until it areally rests with the elastic clasp 58 against the pipe end . the prestressed elastic clasp 58 applies sufficient pressure on the pipe surface so that the unit shall be firmly affixed . the bent ends are pulled apart against the spring force when the adapter shall be removed from the pipe and the unit then will be removed . | 6 |
fig2 and 3 show a structure of a system of the present embodiment . fig3 shows a section along a line x - y in fig2 . a vacuum container 110 comprises a gas feeding system 120 , an exhaust system 130 , an etching power source 140 , an agitating electric field system 150 and an agitating magnetic field system 160 . the gas feeding system 120 has a gas feeding port 121 for feeding reactive gas via a flow controller 122 . for the flow controller 122 , a mass - flow controller , a needle valve or the like is used . the reactive gas which has passed the gas feeding port 121 is blown out to a reaction space 170 via gas blowout pores 123 so that it spreads homogeneously in the space . the gas is rendered to diffuse within an anode 124 where the gas blowout pores 123 exist in order to blow out the gas homogeneously . in the exhaust system 130 , exhaust ports 131 disposed around a substrate 180 so that the reactive gas fed from the gas feeding system 120 is exhausted homogeneously to flow the gas homogeneously on the surface of the substrate 180 are connected with an exhaust flow control valve 132 for maintaining the reaction space 170 at an approximately constant pressure by controlling the flow of the gas exhausted via the exhaust ports 131 . for the exhaust flow control valve 132 , one which can vary a conductance such as a butterfly valve , a variable orifice , a needle valve or the like is used . the exhaust flow control valve 132 is connected with an exhaust pump 133 to pull out the gas . for the exhaust pump 133 , one which conforms to the very purpose thereof has to be selected considering a type of the gas used , a flow amount of the gas used , a reaction pressure , a corrosivity of the gas used , a background pressure and the like such as a turbo pump , a mechanical pump , a rotary pump , a screw pump or the like among various vacuum pumps . in the etching power source 140 , a cathode 141 which also plays a role of a supporting table of the substrate 180 is connected with a cathode power source 143 via a matching device 142 . for the cathode power source 143 , a high frequency power source of 13 . 56 mhz for example , a medium frequency power source of less than 1 mhz or a low frequency power source of less than 1 khz is used . the purpose of the every power source is to lead ions generated in the reaction space 170 to the surface of the substrate . the agitating electric field system 150 is provided with agitating electrodes 151 , i . e . four electrodes 151a , 151b , 151c and 151d in the present embodiment . each of the agitating electrodes 151 is connected with an agitating power source 152 via an amplifier 153 . while a power source in which the agitating power source 152 and the amplifier 153 are integrated may be used , the amplifier 153 is necessary in the present embodiment because a so - called function generator ( frequency generator ) is used to vary a frequency of the agitating power source 152 widely . for the agitating power source 152 , function generators 152a , 152b , 152c and 152d are used corresponding to the respective agitating electrodes 151 , i . e . the electrodes 151a , 151b , 151c and 151d . a frequency band of each of the function generators 152a through 152d was from 0 to 15 mhz . the amplifiers 153 also include amplifiers 153a , 153b , 152c and 153d corresponding to the respective electrodes 151a through 151d and the function generators 152a through 152d . a phase controller 154 for controlling a phase of each agitating power source 152 when a phase difference thereof needs to be related to each other is connected to the agitating power source 152 . that is , phase shifters 154a , 154b , 154c and 154d are connected to the function generators 152a through 152d , respectively . for the agitating magnetic field system 160 , magnets 161 , i . e . electromagnets 161a , 161b , 161c and 161d are used in the present embodiment . the reactive gas fed in from the gas feeding port 121 via the flow controller 122 is diffused within the anode 124 and is led into the reaction space 170 from the gas blowout pores 123 . the reactive gas reached from the reaction space 170 to the surface of the substrate 180 flows to the exhaust ports 131 . the reaction space 170 is maintained at a desirable pressure by controlling a conductance of the exhaust flow control valve 132 located between the exhaust pump 133 and the exhaust ports 131 . in the present embodiment , etching uniformity and shape were compared by using substrates on which 2 μm of a - si is formed on corning 7059 glasses of 150 mm × 150 mm × 1 mm , 200 mm × 200 mm × 1 . 1 mm , 350 mm × 350 mm × 1 . 1 mm and 500 mm × 500 mm × 1 . 1 mm as the substrate 180 . mixed gas of sf 6 and cl 2 was used as the reactive gas . the ratio of the gas was sf 6 / cl 2 = 2 / 8 to 10 / 0 . for the cathode 141 , four sizes of cathodes of 200 × 200 mm , 250 mm × 250 mm , 400 mm × 400 mm and 550 mm × 550 mm were used corresponding to the sizes of the substrates 180 used in the experiment . for the cathode power source 143 , an rf generator of 13 . 56 mhz and a medium frequency power source of 500 khz were used . the power of the power source was between 0 . 1 to 3 w / cm 2 and a distance between the cathode 141 and the anode 124 was fixed to 70 mm . for the exhaust system 130 , one having 1800 liters / s of exhaust rate was used in order to be able to regulate the reaction pressure of the vacuum container 110 of about 75 liters to 50 to 300 mtorr . a total flow amount of the gas including the reactive gas was about 500 to 2000 sccm . in the agitating electric field system 150 , each of the phase shifters 154a through 154d were controlled so that the phase of the neighboring electrodes 151a through 151d is shifted by 90 ° each . the function generators 152a through 152d were operated in 1 khz and 5 mhz . they were operated in 1 khz to check an effect for agitating ions within a plane and 5 mhz to check an effect for agitating electrons within the plane . a power for the agitation was 0 . 3 to 1 w / cm 2 . in the agitating magnetic field system 160 , static magnetic field and rotary magnetic field were generated by the electromagnets 161a through 161d so that while the field strength is 2000 gauss at the inner wall of the vacuum container 110 , it is reduced exponentially toward the middle of the container , thus having about 100 gauss in maximum on the substrate 180 . although the rotary magnetic field is effective more or less as a result , the static magnetic field is also effective considerably as compared to a case without it . accordingly , permanent magnets may be used instead of the electromagnets 161a through 161d when the static magnetic field will do , considering a size of the system and the like . the result of the experiment shows that the etching rate and etching shape are decided almost by the condition of the etching power source 140 and the ratio of the reactive gas and that no effect of the agitating electric field system 150 and the agitating magnetic field system 160 can be seen . when typical conditions for performing anisotropic etching were sf 6 = 1000 sccm , cl 2 = 250 scc m , 200 mtorr of pressure , 13 . 56 mhz of frequency of the cathode power source and 0 . 8 w / cm 2 of power , the etching rate of the a - si was 6200 å / min . in average . however , concerning to the etching uniformity , an effect of the agitating electric field system 150 and the agitating magnetic field system 160 could be seen . table 1 shows the effect as dispersion of the etching rates within the substrate plane . ______________________________________condition 150 mm sq . 200 mm sq . 350 mm sq . 500 mm sq . ______________________________________w / o ams ± 4 . 0 % ± 4 . 5 % ± 5 . 5 %. ± 7 . 3 % w / o aeswith ams ± 4 . 0 ± 4 . 5 ± 5 . 1 ± 6 . 5w / o aesw / o ams ± 4 . 0 ± 4 . 2 ± 4 . 4 ± 4 . 8with aesw / o aes ± 4 . 0 ± 4 . 2 ± 4 . 4 ± 4 . 5with aes______________________________________ the data in table 1 showing the dispersion of the etching rates within the substrate plane was obtained by controlling each of the phase shifters 154a through 154d so that the phase of the neighboring electrodes is shifted by 90 ° each and by setting the function generators 152a through 152d in 5 mhz in the agitating electric field system 150 . no desirable result could be obtained when the frequency was 1 khz because the chemical effect of the etching drops in the case of the mixed gas system because the type and mass of the ions differ significantly . a large effect could be obtained when a single system gas was used . as it is apparent from the result of the experiment , the effect of the agitating electric field system 150 is large . although no big difference can be seen with the substrate of 150 mm sq ., its effect becomes remarkable when the substrate is 200 mm sq . or more . when a si wafer of 2 inches in diameter on which mos transistors are mounted on the whole surface of a substrate of 500 mm sq . is placed , plasma is generated by using helium gas instead of the reactive gas of the present embodiment and a number of elements of the transistor insulation - broken down was counted by taking out the substrate , the number of broken elements is only about a half when the agitating electric field system 150 exists as compared to a case without it , showing that ion damage caused by the bias of the plasma density is small . while the system in which the flow of the gas is controlled precisely in the gas feeding system and the exhaust system has been used in the first embodiment , a system shown in fig4 and 5 is used in the second embodiment . fig5 shows a section along a line x - y in fig4 . a vacuum container 210 comprises a gas feeding system 220 , an exhaust system 230 , an etching power source 240 , an agitating electric field system 250 and an agitating magnetic field system 260 . the gas feeding system 220 has a gas feeding port 221 for feeding reactive gas via a flow controller 222 . for the flow controller 222 , a mass - flow controller , a needle valve or the like is used . the reactive gas which has passed the gas feeding port 221 is blown out to a reaction space 270 via gas blowout pores 223 . no particular process for blowing it out homogeneously is provided . in the exhaust system 230 , exhaust ports 231 disposed at the sides of a substrate 280 for exhausting the reactive gas fed from the gas feeding system 220 are connected with an exhaust flow control valve 232 for maintaining the reaction space 270 at an approximately constant pressure by controlling the flow of the gas exhausted via the exhaust ports 231 . although the exhaust ports can be provided around the substrate 280 so that the gas flows homogeneously on the surface of the substrate 280 , the exhaust ports are not provided around the substrate 280 in this second embodiment . for the exhaust flow control valve 232 , one which can vary a conductance such as a butterfly valve , a variable orifice , a needle valve or the like is used . the exhaust flow control valve 232 is connected with an exhaust pump 233 to pull out the gas . for the exhaust pump 233 , one which conforms to the very purpose thereof has to be selected considering a type of the gas used , a flow amount of the gas used , a reaction pressure , a corrosivity of the gas used , a background pressure and the like such as a turbo pump , a mechanical pump , a rotary pump , a screw pump or the like among various vacuum pumps . in the etching power source 240 , a cathode 241 which also plays a role of a supporting table of the substrate 280 is connected with a cathode power source 243 via a matching device 242 . for the cathode power source 243 , a high frequency power source of 13 . 56 mhz for example , a medium frequency power source of less than 1 mhz or a low frequency power source of less than 1 khz is used . the purpose of the every power source is to lead ions generated in the reaction space 270 to the surface of the substrate . the agitating electric field system 250 is provided with agitating electrodes 251 , i . e . four electrodes 251a , 251b , 251c and 251d in the present embodiment . each of the agitating electrodes 251 is connected with an agitating power source 252 via an amplifier 253 . while a power source in which the agitating power source 252 and the amplifier 253 are integrated may be used , the amplifier 253 is necessary in the present embodiment because a so - called function generator ( frequency generator ) is used to vary a frequency of the agitating power source 252 widely . for the agitating power sources 252 , function generators 252a , 252b , 252c and 252d are used corresponding to the respective agitating electrodes 251 , i . e . the electrodes 251a , 251b , 251c and 251d . a frequency band of each of the function generators 252a through 252d was from 0 to 15 mhz . the amplifiers 253 also include amplifiers 253a , 253b , 252c and 253d corresponding to the respective electrodes 251a through 251d and the function generators 252a through 252d . a phase controller 254 for controlling a phase of each agitating power source 252 when a phase difference thereof needs to be related to each other is connected to the agitating power source 252 . that is , phase shifters 254a , 254b , 254c and 254d are connected to the function generators 252a through 252d , respectively . for the agitating magnetic field system 260 , magnets 261 , i . e . electromagnets 261a , 261b , 261c and 261d are used in the present embodiment . the reactive gas fed in from the gas feeding port 221 via the flow controller 222 is diffused within the anode 224 and is led into the reaction space 270 from the gas blowout pores 223 . the reactive gas reached from the reaction space 270 to the surface of the substrate 280 flows to the exhaust ports 231 . the reaction space 270 is maintained at a desirable pressure by controlling a conductance of the exhaust flow control valve 232 located between the exhaust pump 233 and the exhaust ports 231 . in the present embodiment , etching uniformity and shape were compared by using substrates on which 2 μm of a - si is formed on corning 7059 glasses of 150 mm × 150 mm × 1 mm , 200 mm × 200 mm × 1 . 1 mm , 350 mm × 350 mm × 1 . 1 mm and 500 mm × 500 mm × 1 . 1 mm as the substrate 280 . mixed gas of sf 6 and cl 2 was used as the gas . the ratio of the gas was sf 6 / cl 2 = 2 / 8 to 10 / 0 . for the cathode 241 , four sizes of cathodes of 200 × 200 mm , 250 mm × 250 mm , 400 mm × 400 mm and 550 mm × 550 mm were used corresponding to the sizes of the substrates 280 used in the experiment . for the cathode power source 243 , an rf generator of 13 . 56 mhz and a medium frequency power source of 500 khz were used . the power of the power source was between 0 . 1 to 3 w / cm 2 and a distance between the cathode 241 and the anode 224 was fixed to 70 mm . for the exhaust system 230 , one having 1800 liters / s of exhaust rate was used in order to be able to regulate the reaction pressure of the vacuum container 210 of about 75 liters to 50 to 300 mtorr . a total flow amount of the gas including the reactive gas was about 500 to 2000 sccm . in the agitating electric field system 250 , each of the phase shifters 254a through 254d were controlled so that the phase of the neighboring electrodes 251a through 251d is shifted by 90 ° each . the function generators 252a through 252d were operated in 1 khz and 5 mhz . they were operated in 1 khz to check an effect for agitating ions within a plane and 5 mhz to check an effect for agitating electrons within the plane . a power for the agitation was 0 . 3 to 1 w / cm 2 . in the agitating magnetic field system 260 , static magnetic field and rotary magnetic field were generated by the electromagnets 261a through 261d so that while the field strength is 2000 gauss at the inner wall of the vacuum container 210 , it is reduced exponentially toward the middle of the container , thus having about 100 gauss in maximum on the substrate 280 . although the rotary magnetic field is effective more or less as a result , the static magnetic field is also effective considerably as compared to a case without it . accordingly , permanent magnets may be used instead of the electromagnets 261a through 261d when the static magnetic field will do , considering a size of the system and the like . the result of the experiment shows that the etching rate and etching shape are decided almost by the condition of the etching power source 240 and the ratio of the reactive gas and that no effect of the agitating electric field system 250 and the agitating magnetic field system 260 can be seen . when typical conditions for performing anisotropic etching were sf 6 = 1000 sccm , cl 2 = 250 scc m , 200 mtorr of pressure , 13 . 56 mhz of frequency of the cathode power source and 0 . 8 w / cm 2 of power , the etching rate of the a - si was 6000 a / min . in average . however , concerning to the etching uniformity , an effect of the agitating electric field system 250 and the agitating magnetic field system 260 could be seen . table 2 shows the effect as dispersion of etching rates within the substrate plane . ______________________________________condition 150 mm sq . 200 mm sq . 350 mm sq . 500 mm sq . ______________________________________w / o ams ± 7 . 0 % ± 13 . 0 % ± 24 . 2 % ± 36 . 4 % w / o aeswith ams ± 7 . 0 ± 12 . 5 ± 21 . 2 ± 32 . 0w / o aesw / o ams ± 6 . 9 ± 8 . 5 ± 11 . 1 ± 15 . 3with aesw / o aes ± 6 . 9 ± 8 . 3 ± 10 . 5 ± 15 . 0with aes______________________________________ the data in table 2 showing the dispersion of the etching rates within the substrate plane was obtained by controlling each of the phase shifters 254a through 254d so that the phase of the neighboring electrodes is shifted by 90 ° each and by setting the function generators 252a through 252d in 5 mhz in the agitating electric field system 250 . no desirable result could be obtained when the frequency was 1 khz because the chemical effect of the etching drops in the case of the mixed gas system because the type and mass of the ions differ significantly . a large effect could be obtained when a single system gas is used . as it is apparent from the result of the experiment , the effect of the agitating electric field system 250 is large . although no big difference can be seen with the substrate of 150 mm sq ., its effect becomes remarkable when the substrate is 200 mm sq . or more . however , although the effect of the agitating electric field is large in the case of the present embodiment in which the flow of the gas is not considered at all , the uniformity of the etching rate within the substrate exceeds ± 15 % within 500 mm sq . accordingly , it is actually necessary to control how to flow the gas by a certain degree . however , it is certain that the design margin of the system is wider when there is the agitating electric field system 250 when the size of the substrate and system increases . when a si wafer of 2 inches in diameter on which mos transistors are mounted on the whole surface of a substrate of 500 mm sq . is placed , plasma is generated by using helium gas instead of the reactive gas of the present embodiment and a number of elements of the transistor insulation - broken down was counted by taking out the substrate , the number of broken elements is only about a half when the agitating electric field system 250 exists as compared to a case without it , showing that ion damage caused by the bias of the plasma density is small . fig6 shows a third embodiment . while a vacuum container of the present embodiment is based on that of the first embodiment which is square as shown in fig2 it is pentagonal in the present embodiment . a vacuum container 310 comprises an agitating electric field system and agitating magnetic field system . it also comprises an etching power source , a gas feeding system and an exhaust system similarly to the first embodiment , although not shown . the gas feeding system has a gas feeding port for feeding reactive gas via a flow controller . for the flow controller , a mass - flow controller , a needle valve or the like is used . the reactive gas which has passed the gas feeding port is blown out to a reaction space via gas blowout pores so that it spreads homogeneously in the space . the gas is diffused within an anode where the gas blowout pores exist in order to blow it out homogeneously . in the exhaust system , exhaust ports disposed around a substrate for exhausting the reactive gas fed from the gas feeding system homogeneously to flow the gas homogeneously on the surface of the substrate are connected with an exhaust flow control valve for maintaining the reaction space at an approximately constant pressure by controlling the flow of the gas exhausted via the exhaust ports . for the exhaust flow control valve , one which can vary a conductance such as a butterfly valve , a variable orifice , a needle valve or the like is used . the exhaust flow control valve is connected with an exhaust pump to pull out the gas . for the exhaust pump , one which conforms to the very purpose thereof has to be selected considering a type of the gas used , a flow amount of the gas used , a reaction pressure , a corrosivity of the gas used , a background pressure and the like such as a turbo pump , a mechanical pump , a rotary pump , a screw pump or the like among various vacuum pumps . in the etching power source , a cathode 341 which also plays a role of a supporting table of the substrate 380 is connected with a cathode power source via a matching device . for the cathode power source , a high frequency power source of 13 . 56 mhz for example , a medium frequency power source of less than 1 mhz or a low frequency power source of less than 1 khz is used . the purpose of the every power source is to lead ions generated in the reaction space to the surface of the substrate . the agitating electric field system is provided with five agitating electrodes 351 in the present embodiment . the agitating electrodes 351 are connected with an agitating power source 352 via an amplifier 353 ( although only one set is shown in the figure , all of the five electrodes are connected with them ). while a power source in which the agitating power source 352 and the amplifier 353 are integrated may be used , the amplifier 353 is necessary in the present embodiment because a so - called function generator ( frequency generator ) is used to vary a frequency of the agitating power source 352 widely . for the agitating power sources 352 , function generators are used corresponding to the respective agitating electrodes 351 . a frequency band of each function generator was from 0 to 15 mhz . a phase controller 354 for controlling a phase of each agitating power source 352 when a phase difference thereof needs to be related to each other is connected to the agitating power source 352 . for the agitating magnetic field system , five magnets 361 are used as shown in figure in the present embodiment . the reactive gas fed in from the gas feeding port via the flow controller is diffused within the anode and is led into the reaction space from the gas blowout pores . the reactive gas reached from the reaction space to the surface of the substrate flows to the exhaust ports . the reaction space is maintained at a desirable pressure by controlling a conductance of the exhaust flow control valve located between the exhaust pump and the exhaust ports . in the present embodiment , etching uniformity and shape were compared by using si wafers on which 2 μm of al was formed and whose size were 6 inches , 8 inches and 12 inches in diameter as the substrate 380 . mixed gas of sicl 4 , cl 2 and bcl 3 was used as the gas . the ratio of the gas was sicl 4 / cl 2 / bcl 3 = 1 / 1 / 4 to 3 / 1 / 15 . for the cathode 341 , three cathodes of 180 mm , 230 mm and 350 mm in diameter were used corresponding to the sizes of the substrates 380 used in the experiment . for the cathode power source , an rf generator of 13 . 56 mhz and a medium frequency power source of 500 khz were used . the power of the power source was between 0 . 1 to 3 w / cm 2 and a distance between the cathode 341 and the anode 324 was fixed to 70 mm . for the exhaust system , one having 1800 liters / s of exhaust rate was used in order to be able to regulate the reaction pressure of the vacuum container 310 of about 50 liters to 50 to 300 mtorr . a total flow amount of the gas including the reactive gas was about 500 to 2000 sccm . as for the agitating electric field , each of the phase controllers 354 were controlled so that the phases of the neighboring electrodes are shifted by 72 ° each . the function generators were operated in 1 khz and 5 mhz . they were operated in 1 khz to check an effect for agitating ions within a plane and 5 mhz to check an effect for agitating electrons within the plane . a power for the agitation was 0 . 03 to 1 w / cm 2 . as for the agitating magnetic field , static magnetic field and rotary magnetic field were generated by the electromagnets 361 so that while the field strength is 2000 gauss at the inner wall of the vacuum container 310 , it is reduced exponentially toward the middle of the container , thus having about 100 gauss in maximum on the substrate 380 . although the rotary magnetic field is effective more or less as a result , the static magnetic field is also effective considerably as compared to a case without it . accordingly , permanent magnets may be used instead of the electromagnets when the static magnetic field will do , considering a size of the system and the like . the result of the experiment shows that the etching rate and etching shape are decided almost by the condition of the etching power source and the ratio of the reactive gas and that no effect of the agitating electric field system and the agitating magnetic field system can be seen . when typical conditions for performing anisotropic etching were sicl 4 = 80 sccm , cl 2 = 80 sccm , bcl 3 = 720 sccm , 100 mtorr of pressure , 13 . 56 mhz of frequency of the cathode power source and 0 . 8 w / cm 2 of power , the etching rate of al was 5000 å / min . in average . however , concerning to the etching uniformity , an effect of the agitating electric field system and the agitating magnetic field system could be seen . table 3 shows the effect as dispersion of etching rates within the substrate plane . ______________________________________condition 6 inches . o slashed . 8 inches . o slashed . 12 inches . o slashed . ______________________________________w / o ams ± 3 . 5 % ± 4 . 3 % ± 7 . 6 % w / o aeswith ams ± 3 . 5 ± 4 . 1 ± 7 . 4w / o aesw / o ams ± 3 . 4 ± 3 . 6 ± 4 . 8with aesw / o aes ± 3 . 4 ± 3 . 5 ± 4 . 5with aes______________________________________ the data in table 3 was obtained by controlling each of the phase shifters so that the phase of the neighboring electrodes is shifted by 72 ° each and by setting the function generators in 5 mhz for the agitating electric field system . a power of the agitating power source 352 was 0 . 5 w / cm 2 . no desirable result could be obtained when the frequency was 1 khz because the chemical effect of the etching drops in the case of the mixed gas system because the type and mass of the ions differ significantly . a large effect could be obtained when a single system gas is used . as it is apparent from the result of the experiment , the effect of the agitating electric field system is large . although no big difference can be seen with the substrate of 6 inches in diameter , its effect becomes remarkable when the substrate is 8 inches in diameter or more . when a si wafer on which mos transistors are mounted on the whole surface of a substrate of 12 inches in diameter is placed , plasma is generated by using helium gas instead of the reactive gas of the present embodiment and a number of elements of the transistor insulation - broken down was counted by taking out the substrate , the number of broken elements is only about a half when the agitating electric field exists as compared to a case without it , showing that ion damage caused by the bias of the plasma density is small . as it can be understood also from the present embodiment , the agitating electric field system brings about the effect regardless of a concrete number of the agitating electrodes so long as it is plural . it was found that the effect is remarkable especially when the substrate size is 8 inches or more in diameter . fig7 shows a schematic structure of an application to a multi - chamber , wherein a basic shape of a robot chamber 430 is square . the structure shown in fig7 comprises a loading chamber 410 , an unloading chamber 420 , the robot chambers 430 , an etching chamber 440 , an ashing chamber 450 , a treatment chamber 460 and film forming chamber 470 . each of the chambers is connected via a gate valve which can close / open communication with the other chamber . in the present embodiment , a process of patterning source and drain electrodes of a bottom gate type tft with etching stopper sinx on a glass substrate of 500 mm sq ., of performing a hydrogen treatment and of forming a - sinx film in the end as a protecting film was carried out . the substrate set in the loading chamber 410 was conveyed to the etching chamber 440 by a robot in the robot chamber 431 . in the etching chamber 440 where there is the inventive etching system equipped with the agitating electric field system , al which is the source and drain electrodes was etched by using the reactive gas of sicl 4 , cl 2 and bc1 3 . the etching conditions were set conforming to those of the third embodiment . after etching al , n - type a - si under al was continuously etched by using sf 6 and cl 2 gases and setting the conditions conforming to those of the first embodiment . after etching , the substrate was conveyed to the ashing chamber 450 to ash and remove photoresist by oxygen plasma . although the inventive system comprising the agitating electric field system might be used for the ashing , a normal parallel plate plasma reaction system was used because all the photoresist on the whole surface just needs to be removed . after ashing , the substrate was conveyed to the treatment chamber 460 to perform sputter cleaning by ar or the like when there exists residue of the photoresist or to perform plasma hydrogen treatment immediately when there is no residue . the hydrogen treatment was performed with conditions of 100 to 250 ° c . of substrate temperature , 200 to 800 sccm of hydrogen and 0 . 2 to 0 . 8 w / cm 2 of rf power . it was effective to use the inventive agitating electric field system for the hydrogen treatment and because it was a single system gas in particular , a low frequency power source was effective to use as the agitating power source . each of the phase shifters was controlled so that a phase of neighboring electrodes is shifted by 90 ° each and the function generator was operated in 1 khz . a power of the agitating power source was 0 . 5 w / cm 2 . it was also found here that it is effective to comprise the agitating electric field system also in the process other than etching . after finishing the treatment in the treatment chamber 460 , the substrate was conveyed to the film forming chamber 470 by a robot in the robot chamber 432 . sinx is formed as a protecting film in the film forming chamber 470 . forming conditions were 200 to 250 ° c . of substrate temperature , sih 4 / nh 3 / n 2 = 1 / 5 / 20 , 500 to 1500 sccm of total flow amount and 0 . 5 to 1 . 0 w / cm 2 of rf power . it was also effective to use the inventive agitating electric field system in the film forming chamber 470 and the rf generator was effective as the agitating power source . each of the phase shifters was controlled so that a phase of neighboring electrodes is shifted by 90 ° each and the function generator was operated in 5 mhz . a power of the agitating power source was 0 . 5 w / cm 2 . it was also found here that it is effective to comprise the agitating electric field system also in the process other than etching . the substrate was conveyed to the unloading chamber 420 after forming the film . fig8 shows a schematic structure of an application to a multi - chamber , wherein a basic shape of a robot chamber 530 is pentagonal . it comprises a loading and unloading chamber 510 , the robot chambers 530 , an etching chamber 540 , an ashing chamber 550 , a treatment chamber 560 and film forming chamber 570 . each of the chambers is connected via a gate valve which can close / open communication with the other chamber . in the present embodiment , a process of patterning top wires on a si wafer of 12 inches in diameter having a laminated structure , of performing a surface treatment and of forming an a - siox film as a protecting film in the end was carried out . the substrate set in the loading and unloading chamber 510 was conveyed to the etching chamber 540 by a robot in the robot chamber 530 . in the etching chamber 540 where there is the inventive etching system equipped with the agitating electric field system , al which is the wired electrode was etched by using the reactive gas of sicl 4 , cl 2 and bcl 3 . the etching conditions were set conforming to those of the third embodiment . after etching , the substrate was conveyed to the ashing chamber 550 to ash and remove photoresist by oxygen plasma . although the inventive system comprising the agitating electric field system might be used for the ashing , a normal parallel plate plasma reaction system was used because all the photoresist on the whole surface just needs to be removed . after ashing , the substrate was conveyed to the treatment chamber 560 to perform sputter cleaning by ar or the like when there exists residue of the photoresist or to perform plasma hydrogen treatment immediately when there is no residue . the hydrogen treatment was performed with conditions of 100 to 250 ° c . of substrate temperature , 200 to 800 sccm of hydrogen and 0 . 2 to 0 . 8 w / cm 2 of rf power . it was effective to use the inventive agitating electric field system for the hydrogen treatment and because it was a single system gas in particular , a low frequency power source was effective to use as the agitating power source . each of the phase shifters was controlled so that a phase of neighboring electrodes is shifted by 72 ° each and the function generator was operated in 1 khz . a power of the agitating power source was 0 . 5 w / cm 2 . it was found here that it is effective to comprise the agitating electric field system also in the process other than etching . after finishing the treatment in the treatment chamber 560 , the substrate was conveyed to the film forming chamber 570 by a robot in the robot chamber 530 . siox is formed as a protecting film in the film forming chamber 570 . forming conditions were 200 to 250 ° c . of substrate temperature , teos / o 2 = 1 / 10 , 500 to 1500 sccm of total flow amount and 0 . 5 to 1 . 0 w / cm 2 of rf power . it was also effective to use the inventive agitating electric field system in the film forming chamber 570 and the rf generator was effective as the agitating power source . each of the phase shifters was controlled so that a phase of neighboring electrodes is shifted by 72 ° each and the function generator was operated in 5 mhz . a power of the agitating power source was 0 . 5 w / cm 2 . it was found here that it is effective to comprise the agitating electric field system also in the process other than etching . the substrate was conveyed to the unloading chamber 520 after forming the film . fig9 shows a schematic structure of an application to a multi - chamber , wherein a shape of a robot chamber 630 is hexagonal . it comprises a loading chamber 610 , an unloading chamber 620 , the robot chambers 630 , an etching chamber 640 , an ashing chamber 650 , a treatment chamber 660 and film forming chamber 670 . each of the chambers is connected via a gate valve which can close / open communication with the other chamber . in the present embodiment , a process of patterning source and drain electrodes of a bottom gate type tft with etching stopper sinx on a glass substrate of 500 mm sq ., of performing a hydrogen treatment and of forming a - sinx film in the end as a protecting film was carried out . the substrate set in the loading chamber 610 was conveyed to the etching chamber 640 by a robot in the robot chamber 630 . in the etching chamber 640 where there is the inventive etching system equipped with the agitating electric field system , al which is the source and drain electrodes was etched by using the reactive gas of sicl 4 , cl 2 and bcl 3 . the etching conditions were set conforming to those of the third embodiment . after etching al , an n - type a - si under al was continuously etched by using sf 6 and cl 2 gases and setting the conditions conforming to those of the second embodiment . after etching , the substrate was conveyed to the ashing chamber 650 to ash and remove photoresist by oxygen plasma . although the inventive system comprising the agitating electric field system might be used for the ashing , a normal parallel plate plasma reaction system was used because all the photoresist on the whole surface just needs to be removed . after ashing , the substrate was conveyed to the treatment chamber 660 to perform sputter cleaning by ar or the like when there exists residue of the photoresist or to perform plasma hydrogen treatment immediately when there is no residue . the hydrogen treatment was performed with conditions of 100 to 250 ° c . of substrate temperature , 200 to 800 sccm of hydrogen and 0 . 2 to 0 . 8 w / cm 2 of rf power . it was effective to use the inventive agitating electric field system for the hydrogen treatment and because it was a single system gas in particular , a low frequency power source was effective to use as the agitating power source . each of the phase shifters was controlled so that a phase of neighboring electrodes is shifted by 60 ° each and the function generator was operated in 1 khz . a power of the agitating power source was 0 . 5 w / cm 2 . it was found here that it is effective to comprise the agitating electric field system also in the process other than etching . after finishing the treatment in the treatment chamber 660 , the substrate was conveyed to the film forming chamber 670 by the robot in the robot chamber 630 . sinx is formed as a protecting film in the film forming chamber 670 . film forming conditions were 200 to 250 ° c . of substrate temperature , sih 4 / nh 3 / n 2 = 1 / 5 / 20 , 500 to 1500 sccm of total flow amount and 0 . 5 to 1 . 0 w / cm 2 of rf power . it was also effective to use the inventive agitating electric field system in the film forming chamber 670 and the rf generator was effective as the agitating power source . each of the phase shifters was controlled so that a phase of neighboring electrodes is shifted by 60 ° each and the function generator was operated in 5 mhz . a power of the agitating power source was 0 . 5 w / cm 2 . it was found here that it is effective to comprise the agitating electric field system also in the process other than etching . the substrate was conveyed to the unloading chamber 620 after forming the film . as it is apparent from the above description , the uniformity of the etching rate is improved for a substrate of 8 inches or more by having the agitating electric field system in the rie type etching system as compared to the case without it . with the increase of size of the system , it can give a manufacturing margin with respect to precision control of gas flow in the system , thus allowing to create a small and light - weight system having a high maintainability . it can be also readily applied to a multi - chamber system . the same effect can be obtained in plasma treatments other than etching by having the agitating electric field system . while preferred embodiments have been described , variations thereto will occur to those skilled in the art within the scope of the present inventive concepts which are delineated by the following claims . | 7 |
the invention as summarized can be implemented using either ac ( 1 - or 3 - phase induction ) or dc motors . the lower cost and longer life of an ac motor based system makes it preferable as long the cost ( and complexity ) of the power conversion electronics associated with the ac drive are not excessive . by using an integrated approach to the power conversion and control system , this incremental cost can be minimized , and both approaches will be practical . fig1 shows a schematic diagram of a first preferred embodiment of the overall system . it is based on an ac drive and comprises of the following : i ) a solar photovoltaic ( pv ) panel ( s )/ array ( 100 ) that is the primary power source . ii ) a flow circuit / loop ( 500 ) incorporating a fluid prime mover (( 400 ), i . e . a pump for a liquid , though it may be a compressor , blower or fan for a gas ) for driving a fluid ( typically water , but it may be any liquid or gas ), one or more sensors ( 700 ) that provide flow rate data ( directly or indirectly ), as well as other fittings , valves ( 600 ), etc . that are typical of standard flow systems . note that only a small portion of the flow circuit / loop ( 500 ) is shown in the figure : it may be an open circuit for transferring fluid from one location to another or may be a closed loop for circulating a fluid within . iii ) a fixed output dc - dc converter ( 200 ) that takes solar power at varying voltages as the input and provides output power at a fixed dc voltage suitable for driving a motor . iv ) a variable frequency dc - ac converter ( 250 ) that converts the dc voltage output from the dc - dc converter to an ac voltage whose frequency can be adjusted based on a control parameter . v ) an ac motor ( 300 ) that receives power from the dc - ac converter ( 200 ) and drives the fluid in the flow circuit / loop ( 500 ) using the fluid prime mover ( 400 ). vi ) a comparator / control module ( 800 , shown here as part of the dc - ac converter ( 250 )) that implements a perturb - and - observe algorithm to control the frequency of the output of the dc - ac converter ( 250 ) by using flow data from sensor ( s ) ( 700 ) in the flow circuit / loop . vii ) a communication link ( 900 ) between the sensor ( s ) ( 700 ) and the comparator / control module ( 800 ) that allows them to communicate as required per ( vi ) above . this may be done via wired , wireless , optical or other means . the sensor ( s ) ( 700 ) used for the control function are particularly important in ensuring maximum power usage . in this invention , these are selected by noting that the pumping power ultimately determines the power demand from the source ( the solar array ( 100 )). this pumping power is related to the product of the flow rate and the pressure drop between the pump outlet and the pump inlet . however , since the flow rate is determined by the pumping pressure , maximum power usage can be attained by maximizing this pressure or the flow rate . thus the comparator can be designed to work on the output one or more of the following sensor / transducer types : a flow transducer / sensor that directly measures the flow rate a pressure transducer ( s )/ sensor ( s ) that measures a differential pressure that can be related to the flow rate a pressure transducer / sensor that measures the maximum system pressure at the pump outlet the configuration of the variable frequency dc - ac converter ( 250 ) is also important in ensuring that it meets the goals of the invention ( low cost , high reliability / life and good efficiency ). dc - ac converters or inverters are of three types , square wave , modified sine wave and pure sine wave . the first two are less expensive but provide ac power with high frequency harmonics that cannot be adequately filtered out over the entire speed range . these harmonics have an adverse effects on motor life ( as well as other electronics in the vicinity ), and a pure sine - wave inverter is therefore used in this preferred embodiment . fig1 b shows a overview / block diagram of the variable frequency dc - ac converter ( 250 ) incorporating a pure sine - wave inverter architecture . these inverters comprise high frequency switching networks ( 260 ) that change a constant voltage dc input to a time - varying output by controlling the timing and polarity via multiple switching processes . the switching networks are controlled via driver ( s ) ( 270 ) using output signals from pulse - wave - modulation ( pwm ) circuits ( 275 ). the output of the pwm modules are obtained by combining a reference sinusoidal signal ( i . e . the modulating waveform at the required frequency , e . g . 60 hz ) together with one or more high frequency carrier waves ( typically triangular pulses ) which are generated in a separate block ( s ) ( 280 ). suitable low pass filters ( 265 ) are used to remove unwanted high frequency harmonics from the output of the switching networks so that it corresponds closely to a pure - sine wave . all inverters incorporate a feedback loop ( 290 ) that utilize the reference / carrier wave generating circuits ( 280 ) to ensure that the frequency remains stable regardless of load ( and supply ) changes . this is done by comparing the output frequency with the frequency of the modulating signal and correcting for any error via suitable compensating signals sent to the pwm modules . in the preferred embodiment , an important modification is made to this feedback - compensation loop , i . e . it is coupled with the reference / carrier signals and the comparator / control module ( 800 ) so that the frequency can be adjusted as required during operation ( instead of it being maintained constant ). by combining frequency ( i . e . speed ) control with the dc - ac conversion , a separate variable speed ac drive is not required in the preferred embodiment . such drives are a significant cost adder so that ac motor powered systems are often more expensive than dc motor driven systems even though dc motors typically cost much more than comparable ac motors . this use of a direct dc - ac variable frequency ( 1 phase or 3 phase ) inverter is a particularly important feature of this preferred embodiment . an additional advantage of this approach is that the maximum allowable frequency for the reference signal ( and the corresponding carrier wave ) can be preset to match the maximum allowable speed for a specific design in order to provide a hard operating limit for the motor / pump if necessary . it is also important to note that ( iii ) and ( iv ) above , i . e . the dc - dc converter ( 200 ) and dc - ac converter ( 250 ) can be interchanged in an equivalent design . the alternative would be to implement the dc - ac conversion in the first step after which the ac voltage is changed ( using a transformer for example ) so that it is suitable for use with an ac motor . cost and conversion efficiency will determine the preferred approach . based on the above , the overall system functions using the “ perturb and observe algorithm ” to adjust the frequency of the output voltage of the dc - ac converter ( and thereby speed of the ac motor ) to maximize the flow rate , i . e . the sensor output . this is done as follows ( note that there are many variations of the p & amp ; o algorithm — this a typical approach that may be replaced by other equivalent implementations ): a . power from a solar pv array is supplied via the dc - dc converter to the dc - ac inverter . power from the inverter is supplied to the ac - motor / pump with the initial predetermined frequency ( corresponding to a low speed in the preferred embodiment ). b . sensor data related to flow ( i . e . flow rate or pressure or differential pressure as described above ) is supplied by the sensor ( s ), after suitable processing / conditioning ( e . g . averaging , noise - filtering ) if necessary , to the comparator / controller module . c ) the converter output frequency is adjusted by an small incremental value ( which will typically be a preset amount ) in a pre - selected “ positive ” direction . d ) sensor data is once again sent to an electronic comparator / controller module and compared with the previously sent value . ( i ) if the previously sent value is less than ( or “ equal to ”) the flow rate in ( d ), step ( c ) is repeated . ( ii ) if the previously sent value is greater than the flow rate in ( d ), this shows a lower power usage . in this case , step ( c ) is repeated , but in the reverse direction by a small incremental value , and this reverse direction is now set as the “ positive ” direction . steps ( c - e ) are now repeated on a continuous basis at preset time intervals with the latest value being replaced as the previous value at the end of every step . this will ensure that operating condition corresponds to the maximum flow and maximum power point . it is important to note that the same algorithm with minor changes can be used if the goal is to use a flow related set - point ( e . g . fixed flow rate , pressure , etc .) instead of the maximum flow condition . in this case , the set - point is used as a constraint for the maximum , and the set point ( instead of previous value ) is compared to measured value in step ( d ) above . fig2 shows a schematic diagram of a second preferred embodiment of the overall system . it is similar to the first preferred embodiment but is based on a dc drive , and comprises of the following : i ) a solar photovoltaic ( pv ) panel ( s )/ array ( 100 ) that is the primary power source . ii ) a flow circuit / loop ( 500 ) incorporating a fluid prime mover (( 400 ), i . e . a pump for a liquid , though it may be a compressor , blower or fan for a gas ) for driving a fluid ( typically water , but it may be any liquid or gas ), one or more sensors ( 700 ) that provide flow rate data ( directly or indirectly ), as well as other fittings , valves ( 600 ), etc . that are typical of standard flow systems . note that only a small portion of the flow circuit / loop ( 500 ) is shown in the figure : it may be an open circuit for transferring fluid from one location to another or may be a closed loop for circulating a fluid within . iii ) a variable output dc - dc converter ( 225 ) that takes solar power as the input and provides output power over a wide voltage range suitable for driving a dc motor . iv ) a dc motor ( 325 ) that receives power from the dc - dc converter ( 225 ) and drives the fluid in the flow circuit / loop ( 500 ) using the fluid prime mover ( 400 ). v ) a comparator / control module ( 800 ) that implements a perturb - and - observe algorithm to control the output voltage of the variable output dc - dc converter ( 225 ) by using flow data from sensor ( s ) ( 700 ) in the flow circuit / loop . vi ) a communication link ( 900 ) between the sensor ( s ) ( 700 ) and the comparator / control module ( 800 ) that allows them to communicate as required per ( vi ) above . this may be done via wired , wireless , optical or other means . the sensor ( s ) ( 700 ) used for the control function are similar to those used in the first preferred embodiment . however , the variable output dc - dc converter is different so that it is suited to dc - dc converter circuit designs . the focus here is on the a specific aspect of the dc - dc converter , viz . a feedback loop that is used to ensure that the converter provides a stable output voltage regardless of load ( and supply ) changes . in conventional designs , this loop is used to compare the output voltage of the converter with a reference ( constant ) voltage source , so that any deviations between the two can be corrected . in the preferred embodiment ( fig2 b ), an important modification is made to the feedback loop ( 235 ) used with the dc - dc converter block ( 230 ). in this case , the loop is coupled with ( or replaced by ) the comparator / control module ( 800 ) so that the reference voltage ( 240 ) can be adjusted as required during operation instead of it being maintained constant . more specifically , the output of the sensor is used together with a voltage divider / compensation circuit ( 245 ) to change the reference voltage , and thereby the output voltage and motor speed as required . the upper limit of the reference voltage can be set such that it corresponds to the upper operating limit for the pump , so that the overall design is simplified considerably . thus , a separate variable speed dc drive is not required and system costs are minimized . as in the first embodiment , the overall system functions using the “ perturb and observe algorithm ” to adjust the output voltage of the dc - dc converter ( i . e . the input voltage and speed of the dc motor ) to maximize the flow rate , i . e . the sensor output . this is done as follows : a . power from a solar pv array is supplied to the dc - dc converter . power from the dc - dc converter is supplied to the dc - motor / pump with the initial output voltage . b . sensor data related to flow ( i . e . flow rate or pressure or differential pressure as described above ), after suitable processing / conditioning if necessary , is supplied by the sensor ( s ) to the comparator / controller module . c ) the converter output is adjusted by an small incremental value ( which will typically be a preset amount ) in a pre - selected “ positive ” direction . d ) sensor data is once again sent to an electronic comparator / controller module and compared with the previously sent value . ( i ) if the flow rate in ( d ) is greater than ( or “ equal to ”) the previously sent value , step ( c ) is repeated . ( ii ) if the flow rate in ( d ) is less than the previously sent value , this shows a lower power usage . in this case , step ( c ) is repeated , but in the reverse direction by a small incremental value , and this reverse direction is now set as the “ positive ” direction . steps ( c - e ) are now repeated on a continuous basis at preset time intervals . this will ensure that operating condition corresponds to the maximum flow and maximum power point . as in the first embodiment , note that other similar / equivalent p & amp ; o algorithms and flow related set - points can be used . it is important to note that in both embodiments above , the controller can readily have additional functions for special operating conditions . for example , 1 . when a control valve is closed ( e . g . if a tank is full ), the flow rate ( or differential pressure in the flow line ) will become zero / very small . the comparator / controller can have the additional function to shut down the pump below a ( preset ) low flow rate / differential pressure . alternatively , since the pressure in the flow circuit will become high ( beyond the value for normal operating conditions ), the comparator / controller can have the additional function that shuts down the pump above a ( preset ) high pressure . 2 . if there is a flow line break leading to a major leak , the flow rate may become very high ( higher than values under normal operating conditions ). for this case , the controller can have an additional function set to shut of the motor / pump above a ( preset ) high flow rate . a number of other variations are to above embodiments are also possible . some examples are as follows : a . instead of solar power , the power source can be another similar source where the available power varies with time in an unpredictable ( or partially predictable , e . g . a renewable source such as wind , etc . without adequate storage ) manner . at the same time , the prime mover can be a compressor ( for a refrigerant or other gas ) used in a flow loop of a cooling , thermal energy storage or other system ( e . g . refrigeration , air conditioning , etc .) instead of a pump in a solar pumping system . b . in an ac motor / pump based system ( the first preferred embodiment ), the fixed voltage output dc - dc converter and the variable frequency dc - ac converter may be combined into a single dc - ac converter module together with the comparator / controller . alternatively , the different subsystems ( dc - dc conversion , dc - ac conversion , variable frequency ac - ac conversion ) may be combined / split in different modules if that is advantageous from a design , cost and use perspective . c . a similar approach to ( b ) is also be possible for the second preferred embodiment . the single variable output dc - dc converter can be replaced by two separate modules — a fixed output dc - dc converter ( as in present systems ) coupled with a secondary variable output dc - dc converter that works on the fixed output of the first . this is equivalent to the preferred embodiment , but may make for a more manufacturable and modular package . the comparator / controller may also be split from the variable output module . d . instead of using data from a single measurement for comparison at every stage , data from multiple measurements can be used after suitable averaging using an appropriate signal conditioning circuit . this can help achieve more smooth system operation . e . the incremental adjustment can be time - varying . various options are possible here , e . g . larger increments can be used when the relative change in flow rate is small , whereas smaller increments can be used when the measured change in flow rate is high . this should also lead to quicker and smoother system operations . f . the incremental adjustments can be done at varying time intervals instead of fixed time intervals . for example , when the relative change in flow rate is high , the time interval can be small ; in contrast , when the relative change in flow is small , the time interval can be high . this too should result in more smooth operation as above . g . periodic and / or flow dependent re - initializations to preset controller settings may be incorporated in the control algorithm to ensure that the system does not get constrained at a local minima condition . this can help ensure that maximum flow ( and power usage ) conditions are achieved even under non - design conditions , e . g . when a portion of the array becomes shaded . h . other parameters can also be used to supplement / complement the flow data , e . g the voltage input to the motor , motor temperature , etc . may be used as additional control parameters . this may be particularly useful as a secondary or backup control mode ( e . g . in case of primary sensor failure , motor protection , etc . )— note that voltage ( or motor speed ) control by itself , will not lead to maximum power usage conditions under all circumstances , and would not meet the goals of this invention . i . finally , it is important to reiterate that there are a number of variations to the p & amp ; o algorithm that has been described in the previous sections . these may be based on differences between consecutive measurements ( the difference between consecutive measurements will change from a positive to a negative value or vice - versa as one crosses the maxima — the sign change (+ ve /− ve ) can be used for control ), the slope of the flow rate v / s converter output function ( which will also change signs across a maxima ), etc . similarly , when a set point or constraint condition ( fixed flow , maximum allowable pressure , etc .) is imposed , an equivalent method would be to minimize the difference between the output and the constraint . thus , any of the alternative implementations of the p & amp ; o algorithms can be used in this invention as equivalent embodiments . details of the power source , the motor drive system / variable output power module , the sensor / transducer data collection , transmission and conditioning hardware and software , the control logic , flow loop architecture , etc . have not been described above since many variations are feasible based on prior art . thus , while the invention has been described and disclosed in various terms or certain embodiments , the scope of the invention is not intended to be , nor should it be deemed to be limited thereby , and such other modifications or embodiments as may be suggested by the teachings herein are particularly reserved especially as they fall within the breadth and scope of the claims here appended . | 7 |
fig1 is a flowchart of a method of acquiring semantic information of a word according to an embodiment of this invention . this method provides a method of acquiring semantic information of a keyword , as shown in fig1 , the method comprises : s 102 searching with a predetermined keyword to obtain articles related to the keyword ; s 104 : classifying the articles to determine related articles of each category ; s 106 : for at least one category , performing word segmentation on articles of this category , determining a sequence of words obtained as words in this category and using this category and its corresponding words as semantic information of the keyword . the semantic information acquisition method of the above embodiment comprises : searching and classifying articles ; performing word segmentation on articles of a category to obtain words of this category , and using a plurality of words of this category as semantic information of the keyword . the above semantic information acquisition method may effectively avoid the problem in the prior art , i . e ., only semantic information of english words may be acquired ; it is difficult to update thesauruses in time , causing that it is unable to acquire semantic information of words accurately based on thesauruses ; in addition , it is unable to realize the classification of semantic information according to category information . this method is particularly suitable for searching with keywords , searching in a large amount of articles and integrated processing of a large amount of related data information . as another embodiment , words in each of various categories obtained are used as semantic information of the keyword , to achieve a better representation of words corresponding to various meanings of the keyword . fig2 is a flowchart of a method of acquiring semantic information of a word according to another embodiment of this invention . as shown in fig2 , the method comprises : s 202 : searching with a predetermined keyword to obtain articles related to the keyword ; s 204 : classifying the articles to determine related articles of each category . herein , the categories may be determined according to a particular demand . s 206 to s 208 : for at least one category , performing word segmentation on articles of this category , removing stop words , obtaining co - occurrence words using a sliding window , calculating relationship strength between the co - occurrence words and the keyword , and using co - occurrence words having stronger relationship strength as the semantic information . as an alternative embodiment , words obtained after word segmentation , removing stop words or obtaining co - occurrence words described above may be used as semantic information . however , words obtained after all of these processes are most relevant words of the keyword . as a preferred embodiment , the method further comprises a process of counting the occurrence numbers of words that are determined as semantic information , such as counting the occurrence numbers of the co - occurrence words . the occurrence numbers of words that are determined as semantic information are also used as semantic information , the occurrence number being the number of times a word appears in all articles of a category . meanwhile , classification information may be used as semantic information of the keyword as well , in which case a category having a maximum number of articles obtained through searching is considered as a preferred category . in this manner , the most complete semantic information is obtained , including not only various categories and words in these categories , but also occurrence numbers of these words in various categories , and words having top occurrence numbers are prioritized words . this embodiment provides a keyword expansion method based on semantic information , comprising : ( 1 ) according to a keyword inputted by a user , acquiring at least one category of the keyword . according to the keyword inputted by the user , categories of the keyword and semantic information corresponding to various categories are obtained using the semantic information acquisition method described herein . at least one category in the semantic information is acquired . preferably , all categories of the keyword may be acquired , or some categories containing more articles among all of the categories may be acquired . herein , a specific setting or selection may be made by users according to particular demands . ( 2 ) determining the acquired category and words included in this category as expanded keywords of the keyword . herein , the number of words selected from each category may be specified as needed , such as 10 or 50 words . a search method based on the keyword expansion method described above , in which a keyword inputted by a user and determined expanded keywords of the keyword are used as search words to be searched simultaneously . as an alternative embodiment , a search method based on the keyword expansion method , wherein according to a keyword inputted by a user , expanded keywords of the keyword are displayed to the user as recommended keywords , so that the user may make a selection from complete semantic information . when displayed to the user , those expanded keywords are sorted in descending order of their occurrence numbers . the process of making a selection from complete semantic information comprises : searching with a word selected by the user as a search word separately ; or searching with a plurality of words selected by the user as search words to be searched simultaneously ; or searching with a plurality of words selected by the user and the keyword inputted by the user as search words to be searched simultaneously ; or searching with words included in a category selected by the user as search words to be searched simultaneously ; or searching with words included in a plurality of categories selected by the user as search words to be searched simultaneously . this embodiment provides a method of expanding multiple keywords inputted by a user , i . e ., a keyword expansion method based on semantic information , comprising : ( 1 ) according to a plurality of keywords inputted by a user , acquiring at least one category of each keyword . the category of the keyword may be determined using the semantic information acquisition method described herein . as an alternative embodiment , all categories or some preferred categories of each keyword may be acquired . in the case of repetitive categories , those repetitive categories are deduplicated and are prioritized to be displayed . ( 2 ) determining each category obtained and words included in the category as expanded keywords of this keyword . herein , different categories are aggregated together to obtain words included in those categories . the number of words included in each category may be selected or set according to particular needs . fig3 is a structural diagram of a device of acquiring semantic information of a keyword according to an embodiment of this invention . as shown in fig3 , the device of acquiring semantic information of a keyword comprises : a search unit 31 for searching with a predetermined keyword to obtain articles related to the keyword ; a classification unit 32 for classifying the articles to determine related articles of each category ; an acquisition unit 33 for , for at least one category , performing word segmentation on articles of this category and determining a plurality of words obtained as semantic information of the keyword in this category . as an alternative embodiment , the acquisition unit comprises : a stop word removing subunit 331 for removing stop words from the plurality of words ; an update subunit 332 for determining words obtained after removing stop words as updated semantic information . further , the acquisition unit further comprises : a co - occurrence word acquisition subunit 333 for obtaining co - occurrence words around the keyword and using the co - occurrence words as updated semantic information . further , the acquisition unit further comprises a relationship strength calculation subunit 334 for calculating relationship strength between the co - occurrence words and the keyword and using co - occurrence words having stronger relationship strength as updated semantic information . as an alternative embodiment , in the co - occurrence word acquisition subunit , the process of obtaining co - occurrence words around the keyword further comprises counting occurrence numbers of the co - occurrence words . the semantic information further comprises word occurrence number information , wherein the word occurrence number information represents the number of times a word appears in articles of a category . category information is also used as semantic information of the keyword . fig4 is a structural diagram of a keyword expansion system based on semantic information according to an embodiment of this invention . as shown in fig4 , the system comprises : a category acquisition unit 41 for according to a keyword inputted by a user , acquiring at least one category of the keyword ; in the category acquisition unit , through comparing the keyword inputted by the user and keywords used in the semantic information acquisition method , the category acquisition unit obtains at least one category corresponding to a matched keyword in the semantic information . as an alternative embodiment , all or some categories of the keyword may be acquired . a keyword expansion unit 42 for determining the acquired category and words included in this category as expanded keywords of the keyword . as an alternative embodiment , in the case of multiple keywords inputted by a user , a keyword expansion system based on semantic information is provided , comprising : a category acquisition unit for according to multiple keywords inputted by a user , acquiring at least one category of each keyword . as an alternative embodiment , all or some categories of each keyword may be acquired . in the case of repetitive categories , those repetitive categories are deduplicated and are prioritized to be displayed . a keyword expansion unit for determining the each of the acquired categories and words included in this category as expanded keywords of the keyword . a search system based on a keyword expansion method , comprising a search unit for using a keyword inputted by a user and expanded keywords determined for the keyword as search words to be searched simultaneously . in another embodiment , a search system based on a keyword expansion method , comprising : a recommendation unit for according to a keyword inputted by a user , displaying expanded keywords of the keyword to the user as recommended keywords to enable the user to make a selection from complete semantic information . in the recommendation unit , when displayed to the user , words in each category of the expanded keywords are sorted in descending order of their occurrence numbers . the following subunits are provided for enabling the user to make a selection from complete semantic information : a first subunit for searching with a word selected by the user as a search word separately ; a second subunit for searching with a plurality of words selected by the user as search words to be searched simultaneously ; a third subunit for searching with a plurality of words selected by the user and the keyword inputted by the user as search words to be searched simultaneously ; a fourth subunit for searching with words included in a category selected by the user as search words to be searched simultaneously ; a fifth subunit for searching with words included in a plurality of categories selected by the user as search words to be searched simultaneously . given a predetermined keyword “ apple ”, 200 articles related to “ apple ” are acquired through searching , which are then classified to different categories . the number of categories may be specified according to particular needs . for a project having many categories , some categories are prioritized to acquire words contained therein . a category including a few articles may be directly removed without acquiring articles included therein . in this embodiment , categories are food — 80 articles , electronics — 100 articles , entertainment product — 20 articles . word segmentation is performed on 100 articles in the category of electronics . a sequence of words is acquired . at this point , the semantic information of “ apple ” is : a sequence of words in the category of electronics . in order to improve relevance between the sequence of words obtained in embodiment 1 and keyword “ apple ”, after word segmentation performed on 100 articles in the category of electronics , stop words are removed to remove meaningless stop words . then co - occurrence words around a target word are obtained using a sliding window , and relationship strengths between the co - occurrence words and the keyword are calculated . those co - occurrence words having stronger relationship strength are determined as the selected words . herein , the number of the selected words may be specified according to practical needs , in general , about 30 to 50 words . words obtained after the above calculation is : “ apple mobile phone ”, “ apple computer ”, and “ ipad ”. in order to guarantee more complete information of this keyword “ apple ”, it is necessary to perform a similar process on articles in all of other categories , i . e ., food — 80 articles and entertainment product — 20 articles to acquire words in various categories . after the processing of all categories , the following semantic information is obtained : electronics : apple mobile phone , apple computer , ipad entertainment product : apple mobile phone , ipod , apple store in addition , in order to provide using degrees of various words , the number of times each word appears in all articles of a corresponding category is counted as part of the semantic information . for example : apple food : apple ( 500 ), apple - pear ( 320 ), fuji apple ( 200 ) electronics : apple mobile phone ( 400 ), apple computer ( 200 ), ipad ( 150 ) entertainment product : apple mobile phone ( 200 ), ipod ( 100 ), apple store ( 50 ) according to the semantic information acquisition method of embodiment 1 , after semantic information acquisition , when a user enters keyword “ apple ”, at least one category in the semantic information of “ apple ” is obtained . herein , in order to guarantee a high coverage rate , all categories are obtained . all categories and words included in these categories are used as expanded keywords . that is , expanded keywords of “ apple ” are : electronics : apple mobile phone , apple computer , ipad entertainment product : apple mobile phone , ipod , apple store when a user enters “ apple ” as a search word , all of above categories and words are used as search words to be searched , so that an improved search coverage degree is achieved for the keyword inputted by the user , which is helpful in obtaining search information including results required by the user . in addition to the semantic information of “ apple ” above , semantic information of “ lenovo ” is also established . when a user enters “ apple ” and “ lenovo ” at the same time , these two words are expanded respectively . first , all semantic information of each keyword is obtained respectively , and then is deduplicated and aggregated as expanded keywords . after these expansions have been displayed to the user , the user may make a selection from these expanded words . then , a search is performed using search words automatically generated according to the selection of the user , for example , searching with a word selected by the user as a search word ; or searching with multiple words selected by the user as search words ; or searching with multiple words selected by the user and the keyword inputted by the user as search words ; or searching with words included in a category selected by the user as search words ; or searching with words included in multiple categories selected by the user as search words . this embodiment provides a method of acquiring semantic information of a keyword . words may be exhibited as symbols according to arbitrary conventions . users use these symbols to indicate concepts , i . e ., semantic information given to the words . for the purpose of thorough understanding of a query , the acquisition of semantic information of each word becomes a very important precondition . with a method of text classification and word statistics , semantic expansion may be performed to achieve the effect of acquiring semantic information . the semantic information acquisition method of this embodiment comprises the following steps . step 1 : given a training corpus and a target word , herein the target word is a keyword , the semantic information of which will be acquired , acquiring articles including the target word through full text searching . these articles may be considered as a broader semantic range of this word . however , these articles have scrambled data and information contained therein , which may obscure valid information intensively . thereby , it is necessary to perform further processes on these articles . step 2 : classifying the selected articles using a text classifier . due to the significant dependence of words on their usage environment , and in terms of different meanings of a word , the dependence on its context , selected articles may be classified into a specified classification system according to different contextual characteristics . each article is labeled with a field or a category it belongs to . step 3 : sorting by descending order of the numbers of articles included in various categories . step 4 : after sorting , taking the first m categories to exclude trivial matters from the training corpus while remaining categories having significant context information , and prevent errors caused by the classifier . as to the value of m , the ratio of the number of articles associated with the given word to the number of all articles included in the m categories selected shall be greater than a specified threshold α , in order to guarantee that semantic information may be remained as much as possible according to the particular requirement of an application while excluding the trivial matters . empirically , the value of α is in a range from 80 % to 90 %. step 5 : after acquiring articles belonging to the first m categories and carrying context information of the target word , performing word segmentation on these articles and removing stop words to remove information having no semantic information from the text ; using a sliding window having a size of k , extracting all words included in the window around the position where the target word appears , and calculating relationship strength between the target word and these co - occurrence words using an algorithm for word - relationship statistics to obtain values of relationship strength between the target word and co - occurrence words semantically related to the target word . the size k of the sliding window controls the semantic radiation range of the word . empirically , the value of k is 6 . step 6 : sorting the set of co - occurrence words of the target word by descending order of their relationship strength values and according to article categories they belong to . that is , the first n co - occurrence words having relationship strength values arranged from high to low with the target word are obtained for each of the m categories . a set of word in each category is the semantic information of the target word in this category , identifying a unique and recognizable category of the target word . the sum of all semantic information is the comprehensive semantic information of the target word . because the object of the application is to obtain categories for parsing words contained in a sentence to be searched by a user , category information in the semantic information is important . step 7 : executing operations of step 1 to step 7 for each target word concerned to obtain a category each target word fits into and words belonging to this category as semantic information of the target word , so that a semantic information repository is established . on the basis of embodiment 12 , keyword expansion is performed to recommend search words for searching . with the semantic information obtained in embodiment 12 , based on a search word inputted by a user , a plurality of semantic information options are provided for the user to obtain more accurate meanings from the user and in turn a more accurate search result , particularly as follows . step 1 : the keyword inputted by the user is fed back to the semantic information repository to obtain semantic information of the keyword , that is , to obtain semantic information of all categories of this word through calculation in stage one . step 2 : because the semantic information of the target word inputted by the user comprises m categories or category terms , each category including n co - occurrence words , a semantic prompt is provided to the user in the form of words in m rows and n ′ columns ( n ′ is less than or equal to n ) as recommended search words . the user is asked to make a selection to semantically clarify the search condition . step 3 : after the user has selected one of the m rows or a word in this row , co - occurrence words in this category or words selected by the user are automatically added into search words of the user as expanded keywords for searching . with word “ apple ” as an example , how to obtain semantic information of a word and provide it to a user through search word recommendation will be illustrated below . step 1 : using a corpus well chosen from an internal journal database as a selected corpus resource , search word “ apple ” in the whole corpus through full text searching to obtain about 7000 articles in which word “ apple ” appears as basic data of subsequent semantic analysis . step 2 : classify the 70000 articles in a predetermined category system using a svm classifier to label each article with a category tag . step 3 : count the number of articles classified in each category to obtain statistic result . step 4 : it can be found through checking the classification result that most articles including word “ apple ” are classified into category “ science ” and category “ food ”, and only a relatively fewer number of articles are contained in other categories . thereby , the value of m is set to 2 for word “ apple ”, i . e ., the first two categories comprise above 80 % of the relevant articles . step 5 : perform word segmentation on all articles included in these two categories selected and remove stop words ; with a sliding window in a size of 6 and a word - relationship strength calculation algorithm for counting absolute occurrence frequencies of words , make a process on all words segmented from these articles to obtain two categories : category “ science ” and a vector of relevant co - occurrence words and their relationship strength values ; category “ food ” and a vector of relevant co - occurrence words and their relationship strength values . step 6 : sort the two vectors generated in the above step in descending order , and only take the first 20 words as actual semantic information of each category . semantic information of word “ apple ” consists of two categories , 20 words in each category and their absolute frequencies . step 1 : when a user enters “ apple ” as a search word , the system searches in an existed semantic information repository to obtain various semantic representations of “ apple ”. step 2 : word “ apple ” has two categories , the system cannot determine which category is desired by the user and forms two prompt lines from two categories “ science ” and “ food ” returned from the semantic information repository , on each line 5 words of total 20 words being provided as assistant selection information to enable the user to select a desired category accordingly . step 3 : if the user selects a category , the system submits total 20 co - occurrence words and their strength values to a search engine as recommended expansion of the search word provided by the user ; if the user selects a word in a category , the system submits this word to the search engine as recommended expansion of the search word . as an alternative embodiment , in addition to forming recommended search words based on semantic information , this method may also show a multi - dimensional search word interface to users in other manners . step 1 : the keyword inputted by the user is fed back to the semantic information repository to obtain semantic information of the keyword , that is , to obtain semantic information of all categories of this word through calculation in stage one , wherein the semantic information includes relationship strength values . step 2 : because the semantic information of the target word inputted by the user comprises m categories or category terms , each category including n co - occurrence words , a semantic prompt is provided to the user in the form of words in m rows and n ′ columns ( n ′ is less than or equal to n ) as recommended search words . the user is asked to make a selection to semantically clarify the search condition . a prompt box is provided in the form of a drop - down box including m rows , each row comprising n ′ words belonging to the same category . step 3 : after the user has selected one of the m rows or one or more words in a row , co - occurrence words in this category or words selected by the user are automatically added into search words of the user as expanded keywords for searching . this embodiment provides a specific example of the keyword expansion method . step 1 : when a user enters “ apple ” as a search word , the system searches in an existed semantic information repository to obtain various semantic representations of “ apple ”. step 2 : word “ apple ” has two categories , the system cannot determine which category is desired by the user and forms two prompt lines from two categories “ science ” and “ food ” returned from the semantic information repository , on each line 5 words of total 20 words being provided as assistant selection information to enable the user to select a desired category accordingly . all words on each row belong to the same category . step 3 : if the user selects a category , the system submits total 20 co - occurrence words and their strength values to a search engine as recommended expansion of the search word provided by the user ; if the user selects one or more words in a category , the system submits these words to the search engine as recommended expansion of the search word . obviously , the above embodiments are merely examples given for clear description , but not limitations of this invention . for those skilled in the art , other modifications or variations may be made based on the above description , which will not be and cannot be listed exhaustively herein . these apparent modifications or variations derived are still within the protection scope of this invention . this invention further provides one or more computer readable mediums having stored thereon computer - executable instructions that when executed by a computer perform a keyword expansion method , the method comprising : searching with a predetermined initial keyword to obtain current keywords ; using the current keywords obtained through searching as a basis of a next search , performing loop search through keyword iteration ; if a keyword error between keywords obtained in the current search and those keywords obtained in a previous search is less than a predetermined threshold , terminating the loop search process and using the keywords obtained in the current search as expanded keywords . this invention further provides one or more computer readable mediums having stored thereon computer - executable instructions that when executed by a computer perform a method of annotating a classified corpus described above . those skilled in the art should understand that the embodiments of this application can be provided as method , system or products of computer programs . therefore , this application can use the forms of entirely hardware embodiment , entirely software embodiment , or embodiment combining software and hardware . moreover , this application can use the form of the product of computer programs to be carried out on one or multiple storage media ( including but not limit to disk memory , cd - rom , optical memory etc .) comprising programming codes that can be executed by computers . this application is described with reference to the method , equipment ( system ) and the flow charts and / or block diagrams of computer program products according to the embodiments of the present invention . it should be understood that each flow and / or block in the flowchart and / or block diagrams as well as the combination of the flow and / or block in the flowchart and / or block diagram can be achieved through computer program commands such computer program commands can be provided to general computers , special - purpose computers , embedded processors or any other processors of programmable data processing equipment so as to generate a machine , so that a device for realizing one or multiple flows in the flow diagram and / or the functions specified in one block or multiple blocks of the block diagram is generated by the commands to be executed by computers or any other processors of the programmable data processing equipment . such computer program commands can also be stored in readable memory of computers which can lead computers or other programmable data processing equipment to working in a specific style so that the commands stored in the readable memory of computers generate the product of command device ; such command device can achieve one or multiple flows in the flowchart and / or the functions specified in one or multiple blocks of the block diagram . such computer program commands can also be loaded on computers or other programmable data processing equipment so as to carry out a series of operation steps on computers or other programmable equipment to generate the process to be achieved by computers , so that the commands to be executed by computers or other programmable equipment achieve the one or multiple flows in the flowchart and / or the functions specified in one block or multiple blocks of the block diagram . although preferred embodiments of this application are already described , once those skilled in the art understand basic creative concept , they can make additional modification and alteration for these embodiments . therefore , the appended claims are intended to be interpreted as encompassing preferred embodiments and all the modifications and alterations within the scope of this application . | 6 |
hereinafter , various embodiments of the invention will be described in detail with reference to the accompanying drawings . the invention can be modified in various forms and can have various embodiments . the embodiments are not intended for limiting the invention , but it should be understood that the invention includes all the modifications , equivalents , and replacements belonging to the spirit and the technical scope of the invention . in description of the invention with reference to the drawings , like constituents are referenced by like reference numerals . a moving image encoding device and a moving image decoding device according to the invention may be user terminals such as a personal computer , a notebook pc , a personal digital assistant , a portable multimedia player , a smart phone , a wireless communication terminal , and a tv or servers providing services . the moving image encoding device and the moving image decoding device may be apparatuses having a communication device such as a communication modem for communicating with various apparatuses or wireless or wired communication networks , a memory storing various programs and data for encoding and decoding an image , and a microprocessor performing the programs to perform operations and controls . fig1 is a block diagram illustrating a moving image encoding device according to an embodiment of the invention . the moving image encoding device 100 according to the embodiment of the invention includes an intra prediction module 110 , an inter prediction module 120 , a transform and quantization module 130 , an entropy encoding module 140 , an inverse quantization and inverse transform module 150 , a post - processing module 160 , a picture buffer 170 , a subtraction module 190 , and an addition module 195 . the intra prediction module 110 creates an intra prediction block using reconstructed pixels of a picture or slice to which a current block belongs . the intra prediction module 110 selects one of a predetermined number of intra prediction modes depending on the size of the current block to be prediction - encoded and creates a prediction block depending on the selected intra prediction mode . the inter prediction module 120 performs a motion estimation operation using reference pictures stored in the picture buffer 170 and determines reference picture indices and motion vectors for the motion estimation operation . then , the inter prediction module 120 creates an inter prediction block of the current block using the reference picture indices and the motion vectors . the transform and quantization module 130 transforms and quantizes a residual block of the prediction block created by the intra prediction module 110 or the inter prediction module 120 . the transform is performed using one - dimensional transform matrixes in the horizontal and vertical directions . the residual block for intra prediction is transformed using transform matrixes determined depending on the size of the transform block ( that is , the size of the residual block ) and the intra prediction mode . the residual block for inter prediction is transformed using predetermined transform matrixes . the transform and quantization module 130 quantizes the transform block using a quantization step size . the quantization step size can be changed by coding units equal to or larger than a predetermined size . the quantized transform block is supplied to the inverse quantization and inverse transform module 150 and the entropy encoding module 140 . the inverse quantization and inverse transform module 150 inversely quantizes the quantized transform block and inversely transform the inversely - quantized transform block to reconstruct the residual block . the addition module adds the residual block reconstructed by the inverse quantization and inverse transform module 150 and the prediction block from the intra prediction module 110 or the inter prediction module 120 to creates a reconstructed block . the post - processing module 160 serves to improve image quality of the reconstructed picture and includes a deblocking filter module 161 , an offset module 162 , and a loop filter module 163 . the deblocking filter module 161 adaptively applies a deblocking filter to boundaries of the prediction block and the transform block . the boundaries can be limited to boundaries of 8 × 8 grids . the deblocking filter module 161 determines the boundaries to be filtered , determines boundary strengths thereof , and determines whether the deblocking filter should be applied to the boundaries when the boundary strength is larger than 0 . when it is determined that the boundaries should be filtered , the deblocking filter module 161 selects a filter to be applied to the boundaries and filters the boundaries with the selected filter . the offset module 162 determines whether an offset should be applied by pictures or slices so as to reduce the distortion between a pixel in the image undergoing the deblocking filter module and a corresponding original pixel . alternatively , a slice is divided into plural offset areas and the offset type of each offset area can be determined . the offset type may include a predetermined number of edge offset types and band offset types . when the offset type is an edge offset type , the edge type to which each pixel belongs is determined and an offset corresponding thereto is applied . the edge type is determined on the basis of the distribution of two pixel values neighboring a current pixel . the loop filter module 163 adaptively loop - filters the reconstructed image on the basis of the comparison result of the reconstructed image undergoing the offset module 162 with the original image . it is determined whether the reconstructed image should be loop - filtered by coding units . the size and coefficients of the loop filter to be applied may changed by the coding units . information indicating whether the adaptively loop filter should be applied by coding units may be included in each slice header . in case of a chroma signal , it can be determined whether the adaptive loop filter should be applied by pictures . therefore , information indicating whether chroma components are filtered may be included in a slice header or a picture header . the picture buffer 170 receives post - processed image data from the post - processing module 160 and reconstructs and stores an image in the unit of pictures . the picture may be an image in the unit of frames or an image in the unit of fields . the entropy encoding module 140 entropy - encodes the quantization coefficient information quantized by the transform and quantization module 130 , the intra prediction information received from the intra prediction module 140 , the motion information received from the inter prediction unit 150 , and the like . the entropy encoding module 140 includes a scanning module 145 which is used to transform coefficients of the quantized transform block into one - dimensional quantization coefficients . the scanning module 145 determines a scanning type for transforming the coefficients of the quantized transform block into one - dimensional quantization coefficients . the scanning type may vary depending on a directional intra prediction mode and the size of a transform block . the quantization coefficients are scanned in the backward direction . when the quantized transform block is larger than a predetermined size , the transform coefficients are divided into plural sub blocks and are scanned . the scanning types applied to the transform coefficients of the sub blocks are the same . the scanning types applied to the sub blocks may be a zigzag scan or may be the same scanning types as applied to the transform coefficients of the sub blocks . fig2 is a block diagram illustrating a moving image decoding device 200 according to an embodiment of the invention . the moving image decoding device 200 according to the embodiment of the invention includes an entropy decoding module 210 , an inverse quantization module 220 , an inverse transform module 230 , an intra prediction module 240 , an inter prediction module 250 , a post - processing module 260 , a picture buffer 270 , and an addition module 280 . the entropy decoding module 210 decodes a received bit stream and separates the bit stream into intra prediction information , inter prediction information , quantization coefficient information , and the like therefrom . the entropy decoding module 210 supplies the decoded intra prediction information to the intra prediction module 240 and supplies the decoded inter prediction information to the inter prediction module 250 . the entropy decoding module 210 includes an inverse scanning module 215 for inversely scanning the decoded quantization coefficient information . the inverse scanning module 215 converts the quantization coefficient information into a two - dimensional quantization block . one of plural scanning types is selected for the conversion . the scanning type may vary depending on a directional intra prediction mode and the size of a transform block . the quantization coefficients are scanned in the backward direction . when the quantized transform block is larger than a predetermined size , the transform coefficients are divided into plural sub blocks and are scanned . the scanning types applied to the transform coefficients of the sub blocks are the same . the scanning types applied to the sub blocks may be a zigzag scan or may be the same scanning types as applied to the transform coefficients of the sub blocks . the inverse quantization module 220 determines a quantization step size predictor of a current coding unit and adds the determined quantization step size predictor to the received residual quantization step size to reconstruct the quantization step size of the current coding unit . the inverse quantization module 220 inversely quantizes the quantization block using the quantization step size and the inverse quantization matrix . the quantization matrix is determined depending on the size of the quantization block and the prediction mode . that is , the quantization matrix is selected on the basis of at least one of the prediction mode of the current block and the intra prediction modes for the quantization block having a predetermined size . the inverse transform module 230 inversely transforms the inversely - quantized transform block to reconstruct a residual block . the inverse transform matrix to be applied to the inverse quantization block can be determined depending on the prediction mode and the intra prediction mode . the addition module 280 adds the prediction block created by the intra prediction module 240 or the inter prediction module 250 to the residual block reconstructed by the inverse transform module 230 to create a reconstructed block . the intra prediction module 240 reconstructs the intra prediction mode of the current block on the basis of the intra prediction information received from the entropy decoding module 210 . then , the intra prediction module 240 creates a prediction block depending on the reconstructed intra prediction mode . the inter prediction module 250 reconstructs the reference picture index and the motion vector on the basis of the inter prediction information received from the entropy decoding module 210 . then , the inter prediction module 250 creates a prediction block of the current block using the reference picture index and the motion vector . when motion compensation with decimal prediction is applied , the selected interpolation filter is applied to create the prediction block . the operation of the post - processing module 260 is the same as the operation of the post - processing module 160 shown in fig1 and thus will not be described again . the picture buffer 270 stores the decoded image post - processed by the post - processing module 260 in the unit of pictures . fig3 is a diagram illustrating a method of creating an intra prediction block according to the embodiment of the invention . first , the intra prediction information from the received bit stream is entropy - decoded ( s 110 ). the intra prediction information includes the intra prediction mode group indicator and the prediction mode index . the intra prediction mode group indicator indicates whether the intra prediction mode of the current block belongs to an mpm group or a group other than the mpm group . the prediction mode index is information indicating a specific intra prediction mode in the intra prediction mode group indicated by the intra prediction mode group indicator . the intra prediction mode group indicator can be received in the form of unsigned integer . in this case , the intra prediction mode group indicator can be used without being entropy - decoded . alternatively , the intra prediction mode group indicator may be adaptively entropy - encoded depending on the type of a current slice . for example , the intra prediction mode group indicator may be entropy - encoded using contexts determined depending on the slice type . therefore , the intra prediction mode group indicator may be decoded using the contexts determined depending on the type of the current slice . the entropy - encoding method of the prediction mode index varies depending whether the intra prediction mode belongs to the mpm group or not . therefore , the prediction mode index is entropy - decoded using different methods . specifically , when the intra prediction mode group indicator represents that the intra prediction mode of the current block belongs to the mpm group , the prediction mode index is binarized in a truncated exp - golomb code manner or a truncated unary manner and is then entropy - encoded . therefore , after the binary information is acquired by performing the entropy decoding , the prediction mode index is reconstructed using the above - mentioned methods . when the intra prediction mode group indicator represents that the intra prediction mode of the current block does not belong to the mpm group , the prediction mode index can be binarized with a fixed length . therefore , after the binary information is acquired by performing the entropy decoding , the prediction mode index can be reconstructed . then , the mpm group is created using the intra prediction modes of the blocks neighboring the current block and then the intra prediction mode of the current block is reconstructed using the mpm group ( s 120 ). the mpm group includes three intra prediction modes . this will be described with reference to fig4 . fig4 is a diagram illustrating intra prediction modes according to an embodiment of the invention . ( 1 ) when the intra prediction modes of the top and left blocks of a current block are both present and are different from each other , the mpm group includes the two intra prediction modes and one additional intra prediction mode . when one of the two intra prediction modes is a dc mode and the other is not a planar mode , the additional intra prediction mode may be the planar mode . similarly , when one of the two intra prediction modes is the planar mode and the other is not the dc mode , the additional intra prediction mode may be the dc mode . when the two intra prediction modes are the dc mode and the planar mode , the additional intra prediction mode may be a vertical mode or a horizontal mode . when the two intra prediction modes are not the dc mode nor the planar mode , the additional intra prediction mode may be an intra prediction mode having directionality between the two intra prediction modes , or the dc mode or the planar mode . ( 2 ) when the intra prediction modes of the top and left blocks of the current block are both present and are equal to each other , the mpm group includes the intra prediction mode and two additional intra prediction modes . when the intra prediction mode is neither the dc mode nor the planar mode , the two additional intra prediction modes are set to two intra prediction modes neighboring the intra prediction mode . when the intra prediction mode is the dc mode , the two additional intra prediction modes may be the planar mode and the vertical mode . ( 3 ) when only one of the intra prediction modes of the top and left blocks of the current block is present , the mpm group includes the intra prediction mode and two additional intra prediction modes . the two additional intra prediction modes are determined depending on the intra prediction mode . ( 4 ) when the intra prediction modes of the top and left blocks of the current block are not present at all , the mpm group includes the dc mode , the planar mode , and the vertical mode . when the intra prediction mode group indicator indicates the mpm group , the intra prediction mode indicated by the prediction mode index is selected from the mpm group and the selected intra prediction mode is determined as the intra prediction mode of the current block . the intra prediction mode group indicator may be flag information representing whether the intra prediction mode of the current block belongs to the mpm group or a group other than the mpm group . when the intra prediction mode group indicator does not indicates the mpm group , the intra prediction module 240 determines the intra prediction mode indicated by the prediction mode index out of the intra prediction modes ( hereinafter , referred to as residual intra prediction modes ) other than the intra prediction modes belonging to the mpm group as the intra prediction mode of the current block . the prediction mode indices assigned to the residual intra prediction modes vary depending on the configuration of the mpm group . that is , the decoded prediction mode indices indicate indices of the residual intra prediction modes rearranged depending on the configuration of the mpm group . therefore , the intra prediction module 240 selects the intra prediction mode of the current block from the residual intra prediction modes depending on the decoded prediction mode index and the intra prediction modes belonging to the mpm group . specifically , the residual intra prediction modes of the current block are rearranged in the mode number order and the intra prediction mode corresponding to the received prediction mode index is selected as the intra prediction mode of the current block . in this case , the residual intra prediction modes may be rearranged , but the intra prediction mode of the current block may be determined by comparison of the intra prediction mode numbers belonging to the mpm group with the intra prediction mode index of the current block . this method can be applied to a case where mode number 2 is assigned to the dc mode of the non - directional modes , mode number 34 is assigned to the planar mode , and directional mode numbers are assigned to the other modes . however , since the probability of selecting the planar mode and the dc mode as the intra prediction mode of the current is higher than those of the other directional modes , a small mode number ( for example , mode number 0 ) is assigned to the planar mode and the above - mentioned method can be applied . in this case , the mode numbers of the other lower - ranked modes increase by 1 . alternatively , the lowest indices may be assigned to the non - directional modes . for example , when the intra prediction mode of the current block is the planar mode and the residual intra prediction modes include the planar mode , the intra prediction mode index may include 0 . for example , when the residual intra prediction modes include the planar mode and the dc mode , the intra prediction mode corresponding to the prediction mode index in a state where the planar mode , the dc mode , and the directional modes are arranged in this order may be set as the intra prediction mode of the current block . for example , mode number 0 and mode number 1 may be assigned to the planar mode the dc mode , respectively , or mode number 0 and mode number 1 may be assigned to the dc mode and the planar mode , respectively . in this case , the intra prediction mode index of the current block may be compared with the intra prediction mode numbers belonging to the mpm group to determine the intra prediction mode of the current block . then , the size of the prediction block is determined using information indicating the transform size of the current block ( s 130 ). when the size of the prediction block is equal to the size of the current block , the prediction block is created using the intra prediction mode of the current block and the reference pixels of the current block . the reference pixels are pixels reconstructed or created previously to the current block . when the size of the prediction block is smaller than the size of the current block , that is , when the current block can be divided into plural sub blocks and the intra prediction is performed thereon , the same intra prediction mode ( that is , the intra prediction mode of the current block ) is used to create the prediction block of each sub block . the prediction blocks of the second sub block or sub blocks subsequent thereto in the decoding order are created using the reconstructed pixels of the preceding sub blocks . therefore , after the prediction block , the residual block , and the reconstructed block are created in the units of sub blocks , the prediction block of the next sub block is created . then , it is determined whether the reference pixels of the block corresponding to the size of the prediction block are all valid ( s 140 ). the reference pixels are pixels which are previously decoded and reconstructed . when it is determined that at least one of the reference pixels is not valid , the reference pixel is created ( s 150 ). specifically , when it is determined that the reference pixels are not valid at all , the reference pixel values are replaced with values of 2 l - 1 . here , l represents the number of bits representing the gray scale of luma components . when valid reference pixels are present in only one direction with respect to the position of the invalid reference pixel , the closest reference pixel out of the valid reference pixels is copied to create the reference pixels . when valid reference pixels are present in both directions with respect to the position of the invalid reference pixel , the reference pixel located at the closest position in a predetermined direction can be copied or two closest reference pixels in both directions can be averaged to create the reference pixels . then , it is determined whether the reference pixels should be filtered ( s 160 ). the reference pixels are adaptively filtered depending on the reconstructed intra prediction mode and the size of the prediction block ( s 170 ). the reference pixels are not filtered when the intra prediction mode is the dc mode . when the intra prediction modes are the vertical mode and the horizontal mode , the intra prediction module 240 does not also filter the reference pixels . however , when the intra prediction modes are directional modes other than the vertical mode and the horizontal mode , the reference pixels are adaptively filtered depending on the intra prediction mode and the size of the prediction block . when the size of the prediction block is 4 × 4 , the reference pixels are not filtered for the purpose of a decrease in complexity regardless of the intra prediction mode . the filtering serves to smooth the variation in pixel value between reference pixels and uses a low - pass filter . the low - pass filter may be [ 1 , 2 , 1 ] which is a 3 - tap filter or [ 1 , 2 , 4 , 2 , 1 ] which is a 5 - tap filter . when the size of the prediction block ranges from 8 × 8 to 32 × 32 , the reference pixels are filtered in more intra prediction modes with an increase in the size of the prediction block . then , the prediction block is created depending on the intra prediction mode ( s 180 ). the reference pixels used for the prediction block may be pixels which are adaptively filtered depending on the size of the prediction block and the intra prediction mode . in the dc mode , the average values of n top reference pixels located at positions of ( x = 0 , . . . , n − 1 , y =− 1 ), m left reference pixels located at positions of ( x = 1 −, y = 0 , . . . , m − 1 ), and the corner pixel located at a position of ( x =− 1 , y =− 1 ) can be determined as the prediction pixels of the prediction block . however , the prediction pixels neighboring the reference pixels can be created using weighted average of the average value and the reference pixel neighboring the prediction pixel . in the planar mode , the prediction pixels can be created in the same was as in the dc mode . in the vertical mode , the reference pixels located in the vertical direction are set to the prediction pixels . however , the prediction pixel neighboring the left reference pixel can be created using the reference pixel located in the vertical direction and the variation between the left reference pixels . the variation represents the variation between the corner reference pixel and the left reference pixel neighboring the prediction pixel . in the horizontal mode , the prediction pixels can be created in the same way as in the vertical mode , except for the direction . fig5 is a block diagram illustrating an intra prediction block creating unit 300 according to the embodiment of the invention . the intra prediction block creating unit 300 according to the invention includes a parsing module 310 , a prediction mode decoding module 320 , a prediction block size determining module 330 , a reference pixel validity determining module 340 , a reference pixel creating module 350 , a reference pixel filtering module 360 , a prediction block creating module 370 . the parsing module 310 entropy - decodes a received bit stream to acquired intra prediction information and transform block size information . the intra prediction information includes an intra prediction mode group indicator and a prediction mode index . the intra prediction mode group indicator represents which of an mpm group and a group other than the mpm group the intra prediction mode of a current block belongs to . the prediction mode index is information representing a specific intra prediction mode in the intra prediction mode group indicated by the intra prediction mode group indicator . the method of entropy - decoding the intra prediction information is the same as in step s 110 of fig3 . the transform block size information includes at least one flag ( split_transform_flag ) which represents the transform block size and which is transmitted from an encoder . the prediction mode decoding module 320 creates an mpm group using the intra prediction modes of blocks neighboring a current block and reconstructs the intra prediction mode of the current block using the mpm group and the entropy - decoded intra prediction information . the mpm group includes three intra prediction modes . ( 1 ) when the intra prediction modes of the top and left blocks of a current block are both present and are different from each other , the mpm group includes the two intra prediction modes and one additional intra prediction mode . when one of the two intra prediction modes is a dc mode and the other is not a planar mode , the additional intra prediction mode may be the planar mode . similarly , when one of the two intra prediction modes is the planar mode and the other is not the dc mode , the additional intra prediction mode may be the dc mode . when the two intra prediction modes are the dc mode and the planar mode , the additional intra prediction mode may be a vertical mode or a horizontal mode . when the two intra prediction modes are not the dc mode nor the planar mode , the additional intra prediction mode may be an intra prediction mode having directionality between the two intra prediction modes , or the dc mode or the planar mode . ( 2 ) when the intra prediction modes of the top and left blocks of the current block are both present and are equal to each other , the mpm group includes the intra prediction mode and two additional intra prediction modes . when the intra prediction mode is neither the dc mode nor the planar mode , the two additional intra prediction modes are set to two intra prediction modes neighboring the intra prediction mode . when the intra prediction mode is the dc mode , the two additional intra prediction modes may be the planar mode and the vertical mode . ( 3 ) when only one of the intra prediction modes of the top and left blocks of the current block is present , the mpm group includes the intra prediction mode and two additional intra prediction modes . the two additional intra prediction modes are determined depending on the intra prediction mode . ( 4 ) when the intra prediction modes of the top and left blocks of the current block are not present at all , the mpm group includes the dc mode , the planar mode , and the vertical mode . when the intra prediction mode group indicator indicates the mpm group , the intra prediction mode indicated by the prediction mode index is selected from the mpm group and the selected intra prediction mode is determined as the intra prediction mode of the current block . the intra prediction mode group indicator may be flag information representing whether the intra prediction mode of the current block belongs to the mpm group or a group other than the mpm group . when the intra prediction mode group indicator does not indicates the mpm group , the intra prediction module 240 determines the intra prediction mode indicated by the prediction mode index out of the intra prediction modes ( hereinafter , referred to as residual intra prediction modes ) other than the intra prediction modes belonging to the mpm group as the intra prediction mode of the current block . the prediction mode indices assigned to the residual intra prediction modes vary depending on the configuration of the mpm group . that is , the decoded prediction mode indices indicate indices of the residual intra prediction modes rearranged depending on the configuration of the mpm group . therefore , the intra prediction module 240 selects the intra prediction mode of the current block from the residual intra prediction modes depending on the decoded prediction mode index and the intra prediction modes belonging to the mpm group . specifically , the residual intra prediction modes of the current block are rearranged in the mode number order and the intra prediction mode corresponding to the received prediction mode index is selected as the intra prediction mode of the current block . in this case , the residual intra prediction modes may be rearranged , but the intra prediction mode of the current block may be determined by comparison of the intra prediction mode numbers belonging to the mpm group with the intra prediction mode index of the current block . the mpm group constructing method can be applied to a case where mode number 2 is assigned to the dc mode of the non - directional modes , mode number 34 is assigned to the planar mode , and directional mode numbers are assigned to the other modes . however , since the probability of selecting the planar mode and the dc mode as the intra prediction mode of the current is higher than those of the other directional modes , a small mode number ( for example , mode number 0 ) is assigned to the planar mode and the above - mentioned method can be applied . in this case , the mode numbers of the other lower - ranked modes increase by 1 . alternatively , the lowest indices may be assigned to the non - directional modes . for example , when the intra prediction mode of the current block is the planar mode and the residual intra prediction modes include the planar mode , the intra prediction mode index may include 0 . for example , when the residual intra prediction modes include the planar mode and the dc mode , the intra prediction mode corresponding to the prediction mode index in a state where the planar mode , the dc mode , and the directional modes are arranged in this order may be set as the intra prediction mode of the current block . for example , mode number 0 and mode number 1 may be assigned to the planar mode the dc mode , respectively , or mode number 0 and mode number 1 may be assigned to the dc mode and the planar mode , respectively . in this case , the intra prediction mode index of the current block may be compared with the intra prediction mode numbers belonging to the mpm group to determine the intra prediction mode of the current block . the prediction block size determining module 330 determines the size of the prediction block of the current block using the block transform size . the size of the prediction block may have the size of the current block or the size of sub blocks of the current block . when the size of the prediction block is equal to the size of the current block , the prediction block is created using the intra prediction mode of the current block and the reference pixels of the current block . the reference pixels are pixels reconstructed or created previously to the current block . when the size of the prediction block is smaller than the size of the current block , that is , when the current block can be divided into plural sub blocks and the intra prediction is performed thereon , the same intra prediction mode ( that is , the intra prediction mode of the current block ) is used to create the prediction block of each sub block . the prediction blocks of the second sub block or sub blocks subsequent thereto in the decoding order are created using the reconstructed pixels of the preceding sub blocks . therefore , after the prediction block , the residual block , and the reconstructed block are created in the units of sub blocks , the prediction block of the next sub block is created . the reference pixel validity determining module 340 determines whether the reference pixels of the block corresponding to the size of the prediction block are all valid . the reference pixels are pixels which are previously decoded and reconstructed . when it is determined that at least one of the reference pixels is not valid , the reference pixel validity determining module 340 creates the reference pixel . specifically , when it is determined that the reference pixels are not valid at all , the reference pixel values are replaced with values of 2 l - 1 . here , l represents the number of bits representing the gray scale of luma components . when valid reference pixels are present in only one direction with respect to the position of the invalid reference pixel , the closest reference pixel out of the valid reference pixels is copied to create the reference pixels . when valid reference pixels are present in both directions with respect to the position of the invalid reference pixel , the reference pixel located at the closest position in a predetermined direction can be copied or two closest reference pixels in both directions can be averaged to create the reference pixels . the reference pixel filtering module 360 determines whether the reference pixels should be filtered . the reference pixels are adaptively filtered depending on the reconstructed intra prediction mode and the size of the prediction block . the reference pixels are not filtered when the intra prediction mode is the dc mode . when the intra prediction modes are the vertical mode and the horizontal mode , the intra prediction module 240 does not also filter the reference pixels . however , when the intra prediction modes are directional modes other than the vertical mode and the horizontal mode , the reference pixels are adaptively filtered depending on the intra prediction mode and the size of the prediction block . when the size of the prediction block is 4 × 4 , the reference pixels are not filtered for the purpose of a decrease in complexity regardless of the intra prediction mode . the filtering serves to smooth the variation in pixel value between reference pixels and uses a low - pass filter . the low - pass filter may be [ 1 , 2 , 1 ] which is a 3 - tap filter or [ 1 , 2 , 4 , 2 , 1 ] which is a 5 - tap filter . when the size of the prediction block ranges from 8 × 8 to 32 × 32 , the reference pixels are filtered in more intra prediction modes with an increase in the size of the prediction block . the prediction block creating module 370 creates the prediction block depending on the intra prediction mode . the reference pixels used for the prediction block may be pixels which are adaptively filtered depending on the size of the prediction block and the intra prediction mode . in the dc mode , the average values of n top reference pixels located at positions of ( x = 0 , . . . , n − 1 , y =− 1 ), m left reference pixels located at positions of ( x = 1 −, y = 0 , . . . , m − 1 ), and the corner pixel located at a position of ( x =− 1 , y =− 1 ) can be determined as the prediction pixels of the prediction block . however , the prediction pixels neighboring the reference pixels can be created using weighted average of the average value and the reference pixel neighboring the prediction pixel . in the planar mode , the prediction pixels can be created in the same was as in the dc mode . in the vertical mode , the reference pixels located in the vertical direction are set to the prediction pixels . however , each prediction pixel neighboring the left reference pixel can be created using the reference pixel located in the vertical direction and the variation between the left reference pixels . the variation represents the variation between the corner reference pixel and the left reference pixel neighboring the prediction pixel . in the horizontal mode , the prediction pixels can be created in the same way as in the vertical mode , except for the direction . fig6 is a block diagram illustrating a residual block reconstructing sequence according to the embodiment of the invention . a residual signal received in the unit of a current block or a sub block is decoded to create a two - dimensional quantization block ( s 210 ). the quantization block is inversely quantized using a quantization parameter ( s 220 ). the inversely - quantized block is inversely transformed to reconstruct a residual block ( s 230 ). fig7 is a block diagram illustrating a quantization parameter reconstructing sequence according to the embodiment of the invention . the quantization parameter reconstructing sequence can be performed by the inverse quantization unit 220 shown in fig2 . a minimum cu size ( hereinafter , referred to as a minimum quantization cu size ) enabling changing of the quantization parameter is reconstructed ( s 310 ). the minimum quantization cu size can be signaled using one of the following methods . in a first method , whether a qp should be changed in the unit of lcu or can be additionally changed in a sub cu thereof can be indicated using cu_qp_delta_enabled flag included in a sequence parameter set . when the value of cu_qp_delta_enabled flag is 1 , that is , when the changing of qp y in a cu smaller than the lcu is enabled , the minimum quantization cu size can be signaled using max_cu_qp_delta_depth included in a picture parameter set . in a second method , the minimum quantization cu size is signaled using one information piece ( cu_qp_delta_depth ) through joint coding instead of transmitting both cu_qp_delta_enabled flag and max_cu_qp_delta_depth . that is , information related to the minimum quantization cu size is not transmitted from the sequence parameter set , but the minimum quantization cu size is transmitted using cu_qp_delta_depth through the picture parameter set . accordingly , it is possible to reduce the number bits required to transmit the information on the minimum quantization cu size and to adaptively adjust the size enabling changing of the quantization parameter by pps , thereby improving encoding performance . a quantization parameter predictor is calculated on the basis of the minimum quantization cu size ( s 320 ). the quantization parameter predictor can be created using the left quantization parameter of the current cu and the top quantization parameter of the current cu . for example , the average value of the left quantization parameter and the top quantization parameter can be set as the quantization parameter predictor . the quantization parameter predictor and the received residual quantization parameter are added to reconstruct the quantization parameter ( s 330 ). when the current cu is equal to or larger than the minimum quantization cu size , the quantization parameter of the current cu is reconstructed . however , when the current cu is smaller than the minimum quantization cu size , plural cus included in the minimum quantization cu size have the same quantization parameter . while the invention has been described with reference to the embodiments , it will be able to be understood by those skilled in the art that the invention can be modified and changed in various forms without departing from the spirit and scope of the invention described in the appended claims . | 7 |
reference will now be made in detail to the present preferred embodiments of the invention , examples of which are illustrated in the accompanying drawings . wherever possible , the same reference numbers are used in the drawings and the description to refer to the same or like parts . fig2 a through 2d are cross - sectional views showing the progression of manufacturing steps in fabricating the lower electrode of a dram capacitor according to one preferred embodiment of this invention . first , as shown in fig2 a , a source / drain region 220 is formed in a substrate 210 using , for example , an ion implantation process . thereafter , a dielectric layer 230 of , for example , silicon dioxide , is formed over the substrate 210 . the dielectric layer 230 can be formed using tetraethoxy silane ( si ( oc 2 h 5 ) 4 ) as a gaseous reactant in a low - pressure chemical vapor deposition ( lpcvd ) process . next , photolithographic and etching processes are carried out to form a node contact opening 240 in the dielectric layer 230 . subsequently , another lpcvd process is carried out using silane ( sih 4 ) as a gaseous reactant to deposit silicon as well as dopants into the node contact opening 240 and over the dielectric layer 230 to form a polysilicon layer . hence , a conductive plug 260 is formed inside the node contact opening 240 and a doped polysilicon layer 250 a is formed over the dielectric layer 230 . since a polysilicon layer rather than an amorphous silicon layer is deposited , the rate of deposition at 600 ° c . is about 100 å / min . hence , if a polysilicon layer having a thickness of about 8000 å is required , only 1 . 33 hours are needed to complete the deposition process . compared with the original 16 hours needed to deposit amorphous silicon , this is a tremendous improvement . another advantage of depositing doped polysilicon rather than doped amorphous silicon is that a doped polysilicon layer has a higher electrical conductivity . in general , if the dimensions of a device are reduced without changing the material used to form the device , its electrical resistance , and hence its operating speed , will decrease as the cross - sectional area is reduced . therefore , replacing the doped amorphous silicon with doped polysilicon allows the electrical conductivity of the conductive plug 260 to increase . as shown in fig2 b , the polysilicon layer 250 a is patterned to form a lower electrode 250 b . as shown in fig2 c , an ion implantation operation is carried out by bombarding the surface of the doped polysilicon lower electrode 250 b with ions 270 so that the upper portion of the polysilicon structure is damaged . consequently , an amorphous layer 252 a is formed over the polysilicon layer , so that the lower electrode 280 a now comprises an inner core of polysilicon 250 c and a surface layer of amorphous silicon 252 a . the implantation 270 can be conducted using argon ( ar ) ions set to an energy level of between 150 and 200 kev and a concentration of about 3 × 10 14 atom / cm 2 , or using phosphorus ( p ) ions set to an energy level of between 250 and 300 kev and a concentration of about 5 × 10 14 atom / cm 2 , or using arsenic ( as ) ions set to an energy level of between 180 and 230 kev and a concentration of about 10 14 atom / cm 2 . furthermore , even nitrogen ( n ) ions or antimony ( sb ) ions can be used . if the ions used in the implantation are phosphorus , arsenic , or antimony , resistance at the surface of the lower electrode will be lowered even further . in addition , since the surface material of the lower electrode is transformed into an amorphous layer , the electric charge will be distributed more evenly and the probability of electrical discharge will be reduced . thus , the operating speed of the device will be increased . because the ions are highly energetic when they are implanted into the lower electrode 280 a , the energy can be utilized to break up the regular lattice structure of a doped polysilicon layer near the surface . therefore , crystalline polysilicon 250 b near the surface will be transformed into an amorphous silicon layer 252 a . yet the highly energetic ions are unable to penetrate into the deep interior of the lower electrode ; therefore , polysilicon 250 c will remain in the core of the lower electrode . next , as shown in fig2 d , a seeding operation is carried out , and then an annealing operation is conducted in a high vacuum at a temperature of between 550 ° c . and 570 ° c . therefore , hemispherical grain silicon ( hsg - si ) 290 is able to grow over the amorphous silicon layer 252 a of the lower electrode 280 a . consequently , the overall surface area of the lower electrode 280 b will increase to twice its original value . in fact , the lower electrode 280 b is now composed of the inner polysilicon layer 250 c and the outer amorphous silicon layer 252 b , the surface of which is coated with an hsg - si layer 290 . in summary , the advantages of using the method of this invention to fabricate the lower electrode of a dram capacitor include : 1 . since polysilicon rather than amorphous silicon is used to form the lower electrode , the time needed to fabricate the lower electrode is very much reduced . therefore , productivity can increase several times . 2 . since polysilicon instead of amorphous silicon forms the bulk of matter inside the lower electrode , the conductive plug has a lower electrical resistance . hence , the device has a higher operating speed . 3 . after the conversion of a surface layer of the lower electrode into an amorphous silicon layer through an ion implantation process , silicon atoms can move quite easily along the surface of the lower electrode . therefore , after the seeding operation , a uniform hsg - si layer can be readily formed over the surface of the lower electrode during the high vacuum healing operation . it will be apparent to those skilled in the art that various modifications and variations can be made to the structure of the present invention without departing from the scope or spirit of the invention . in view of the foregoing , it is intended that the present invention cover modifications and variations of this invention provided they fall within the scope of the following claims and their equivalents . | 7 |
the present invention is directed to semiconductor optical devices , and more specifically to method of manufacturing micro - and nanotubes and devices incorporating them . reference may be made below to specific elements , numbered in accordance with the attached figures . the discussion below should be taken to be exemplary in nature , and not as limiting of the scope of the present invention . the scope of the present invention is defined in the claims , and should not be considered as limited by the implementation details described below , which as one skilled in the art will appreciate , can be modified by replacing elements with equivalent functional elements . within the text below and the embodiments of manufacturing , use , etc contained within the term “ semiconductor tube ” has been used and refers to either a semiconductor tube or a semiconductor nanotube . similarly whilst reference is made primarily to gaas / inalgaas semiconductors for embodiments of the invention it would be understood by one skilled in the art that other semiconductor material systems may be employed without departing from the scope of the invention according to the optical wavelength of the devices being provided and the constraints of material processing , suitable sacrificial layers , material properties etc . such material systems may include binary , tertiary and quaternary semiconductors within the ingaassb , ingaasp , algaasp , cdznsete , and gaalassb material systems as well as silicon , germanium , and selenides of zn , mg , and cd . fig1 depicts schematics of manufacturing semiconductor tubes using a semiconductor manufacturing methodology with and without structured edges according to an embodiment of the invention . as shown in first deposited layer structure 150 to achieve a free - standing semiconductor tube , a u - shaped mesa is defined within a gaas layer 146 that sits atop a semiconductor epitaxial structure comprising alas 112 , ingaas 114 and gaas 146 layers which were deposited atop a gaas substrate 118 . a mesa was then defined by etching into the ingaas 114 layer , and one edge of the mesa the 112 alas layer , which will form a sacrificial layer , was also etched through . this edge of the mesa is used to define the starting edge of the rolled - up semiconductor tube . the self - rolling process is initiated with the selective removal of the alas 112 sacrificial layer using hf based solutions . as shown in partial etch structure 120 after a certain distance , the middle part of the semiconductor tube separates from the substrate and begins to curl , curled structure 126 , through the stress distribution within the now free layer . further etching in combination with the continuous rolling of the tube on the side pieces results in first free - standing semiconductor tube 165 , as depicted in first finished structure 150 . for example the ingaas / gaas bilayer heterostructure may be grown as a 50 nm alas layer on gaas substrates by molecular beam epitaxy and comprising a 20 nm in0 . 18ga0 . 82as layer with a 30 nm gaas layer . likewise in second deposited layer structure 110 to achieve a free - standing semiconductor tube , a u - shaped mesa is defined within a gaas layer 116 that sits atop a semiconductor epitaxial structure comprising alas 112 , ingaas 114 and gaas 116 layers which were deposited atop a gaas substrate 118 . a mesa was then defined by etching into the ingaas 114 layer , and one edge of the mesa the alas 112 layer , which will form a sacrificial layer , was also etched through . this edge of the mesa is used to define the starting edge of the rolled - up semiconductor tube . the self - rolling process is initiated with the selective removal of the alas 112 sacrificial layer using hf based solutions . as shown in partial etch structure 120 after a certain distance , the middle part of the semiconductor tube separates from the substrate and begins to curl , curled structure 126 , through the stress distribution within the now free layer . further etching in combination with the continuous rolling of the tube on the side pieces results in second free - standing semiconductor tube 135 , as depicted in second finished structure 130 . in second deposited layer structure 110 the gaas 146 layer is patterned with a predetermined profile 116 a on the inner region , which is evident on the outer surface of the free - standing semiconductor tube 135 . as will be evident below from discussions on the structure of the optical modes within such semiconductor tubes the predetermined profile 116 a can be tailored to adjust the resulting optical mode profile of the semiconductor tube providing a mechanism of tailoring such optical mode profile through the photolithography step defining the etched pattern of the gaas 146 layer . within another embodiment of the invention , not shown in fig1 , a reduction in the radiative loss of the optical modes through the substrate , the region between the two side pieces 116 b and 116 c of the u - shaped mesa is etched through the ingaas 114 , alas 112 and into the gaas substrate 118 . this etching for example being approximately 1 μm and increases the air gap between the central part of the semiconductor tube and the substrate . typically semiconductor tubes fabricated with this method have 1 or 2 revolutions corresponding to wall thicknesses of approximately 50 nm and 100 nm for the epitaxial structure defined supra . typical ; semiconductor tube diameters are approximately 5 μm to 6 μm and are predetermined by the strain of the pseudomorphic ingaas 114 layer and the subsequently gaas 116 layer with or without the quantum dot heterostructure . referring to fig2 there is depicted a schematic of the method showing the incorporation of quantum dots into the semiconductor tube according to an embodiment of the invention . accordingly in curl schematic 210 a quantum dot semiconductor structure is shown during the etching step . accordingly there is a similar structure to that described supra in respect of fig1 comprising an ingaas / gaas bilayer heterostructure 206 comprising a 50 nm alas layer 204 on gaas substrates by molecular beam epitaxy and comprising a 20 nm in0 . 18ga0 . 82as layer with a 30 nm gaas layer . embedded within the gaas matrix of the ingaas / gaas bilayer hetero structure 206 are one or two layers of in0 . 5ga0 . 5as quantum dot layers 205 . selective etching of the alas 204 layer causes the ingaas / gaas bilayer heterostructure 206 to being rolling - up into the semiconductor tube , due to the relaxation of strain . the tube diameter is determined by the bilayer thicknesses and compositions , and the number of rotations is controlled by the etching time . tube schematic 220 showing a single rotation of the ingaas / gaas bilayer heterostructure 206 thereby forming a cavity 208 within the resulting semiconductor tube . now referring to fig3 exemplary semiconductor epitaxial structures employed in forming semiconductor tubes according to embodiments of the invention are depicted . as shown first epitaxial structure 310 represents a structure such as described supra in respect of fig1 and 2 . according there is shown an ingaas / gaas bilayer heterostructure grown on a 50 nm alas 302 layer on n + gaas substrate 301 , for example by molecular beam epitaxy . the heterostructure consists of a 20 nm in0 . 18ga0 . 82as 303 layer and a 30 nm gaas layer 304 as well as two vertically coupled in0 . 5ga0 . 5as qd layers 305 embedded in the gaas matrix . accordingly first epitaxial structure 310 allows semiconductor tubes to be fabricated on gaas substrates for either direct integration into microwave , rf or electronic circuits formed on gaas or their removal and transfer to another substrate . second semiconductor structure 320 provides a variant of the structure that is compatible with forming ingaas / gaas semiconductor tubes on silicon wafers . accordingly there is shown the same ingaas / gaas bilayer heterostructure grown on a 50 nm alas 302 layer where the heterostructure consists of a 20 nm in0 . 18ga0 . 82as 303 layer and a 30 nm gaas layer 304 as well as two vertically coupled in0 . 5ga0 . 5as qd layers 305 embedded in the gaas matrix . however , now the alas 302 layer is grown atop a gaas layer 306 that has been grown on a silicon 307 substrate . in this manner the structures can be integrated with silicon electronics , including for example cmos . now referring to fig4 a depicts a transfer method for semiconductor tubes that can be employed with semiconductor tubes manufactured according to an embodiment of the invention . pseudomorphic ingaas / gaas quantum dot heterostructures were grown on gaas substrates , which consist of a 50 nm alas sacrificial layer 411 and 20 nm in0 . 18ga0 . 82as 414 b and 30 nm gaas layers 414 a . two in0 . 5ga0 . 5as quantum dot layers were embedded in the gaas matrix , not shown for clarity . the use of quantum dots can substantially reduce nonradiative recombination associated with the presence of surface defects , due to the three dimensional localization of carriers in the dots . as shown in pre - etch schematic 410 a strained u - shaped mesa was first defined by etching the gaas 414 a to the ingaas layer 414 b . the alas sacrificial layer 411 was also etched through at the starting edge of the rolled - up semiconductor tube . the self - rolling process was initiated with the selective etching of the alas sacrificial layer 411 using hydrofluoric acid based solutions due to the relaxation of strain in the ingaas / gaas bilayer . after a certain distance , the middle part of the tube is separated from the substrate and as a result , continuous rolling on the side pieces leads to freestanding semiconductor tubes 415 on gaas substrate 412 as illustrated in pre - release schematic 420 . it may be noted that the presence of a sinusoid corrugation at the inner edge of the mesa results in semiconductor tube ring resonators with an engineered geometry as will be discussed below . to achieve semiconductor tube ring resonators employing semiconductor tubes 415 on si substrate 416 , the thin alas sacrificial layer underlying the mesa is completely etched and the fully released quantum dot semiconductor tubes 415 are then registered on the gaas substrate 413 . subsequently , as shown in transfer schematic 430 the gaas substrate 413 is placed directly on top of the si substrate 416 with the presence of an appropriate solvent . when the gaas substrate 413 is removed , freestanding semiconductor tubes 415 preferentially stay on the si substrate 416 due to the gravitational force induced by the solvent in and around the tube . upon drying out the solvent the semiconductor tubes 415 are attached to the si wafer 416 by van der waals bonding as shown in final schematic 440 . referring to fig4 b there are depicted sem micrographs of semiconductor tubes manufactured according to embodiments of the invention such as described above in respect of fig1 through 4a . the scanning electron microscopy sem image of an ingaas / gaas quantum dot semiconductor tube fabricated on a gaas substrate is shown in first sem 450 , which is evidenced by the presence of an etched gaas mesa upon the formation of the semiconductor tube . second sem 460 shows a quantum dot semiconductor tube transferred on a clean si substrate that is free of any etched pattern . the sinusoidal geometry of the freestanding region of a quantum dot semiconductor tube on si can also be clearly identified , as illustrated in third sem 480 where rolled end 464 is shown along with the body 472 of the central region of the semiconductor tube and the sinusoidal edge of the gaas is shown by line 476 . such quantum dot semiconductor tube exhibit a diameter of approximately 5 . 2 μm and in this example the freestanding region 472 was formed by 2 . 5 revolutions , thereby yielding wall thicknesses of approximately 100 μm and 150 μm for the regions with 2 and 3 revolutions respectively . the air gap between the semiconductor tube and si substrate , determined by the etching time , is estimated to be approximately 0 . 3 μm . the substrate - on - substrate transfer technique allows for the achievement of semiconductor tube ring resonators on si with extremely smooth surface and excellent structural properties that is not possible using either of the dry - printing or solution - casting based processes of the prior art . for 2 . 5 rotations the etching process removed approximately of 21 μm of alas such that where the semiconductor tube is formed and employed on the same substrate without any transfer an region of approximately 25 μm would be devoid of device elements to provide the region for the deposition of the epitaxial structure that would be subsequently rolled up during the etching step . now referring to fig5 a there is depicted a method of manufacturing a gaas / inalas semiconductor tube within a gaas electrical circuit for electrical injection of carriers to provide a semiconductor optical source according to an embodiment of the invention . the electrically injected device heterostructure , shown in pre - etching schematic 500 a is very similar to the ingaas / gaas bilayer hetero structure described above in respect of fig1 through 4b except that the top gaas 540 and the strained ingaas 530 layers are doped with si and be respectively . self - organized ingaas quantum dot layers are incorporated in the gaas 540 layer as the gain media , but are not shown for clarity . the epitaxial structure further including the alas 520 sacrificial layer between the ingaas 530 and the substrate 510 and an n - metal contact formed in n - metal 550 . during the fabrication process , a u - shaped mesa was first defined using standard photolithography and wet etching techniques , followed by the deposition of the n - metal 550 layer on the end of the mesa and the two side - pieces of the mesa . the free - standing rolled - up semiconductor tube structure 570 was then fabricated by etching the alas 520 layer . subsequently , su - 8 580 , an epoxy based negative photoresist providing a passivation and planarization layer with a thickness of approximately 4 μm to 5 μm , was spin coated onto the wafer . next a p - metal contact was formed in p - metal 590 that was deposited in regions of the free - standing rolled - up semiconductor tube structure 570 where the su - 8 580 is selectively removed , as illustrated interconnected tube schematic 500 b . referring to perspective view 500 c there is shown an alternative embodiment of the structure prior to etching wherein the region between the two sidepieces of the u - shaped mesa was etched to approximately 1 μm deep , with the sidewalls protected by a thin ( approximately 0 . 1 μm ) sinx layer . the trench 5000 providing increased separation of the fabricated semiconductor tube from the substrate . now referring to fig5 b there is depicted an optical micrograph of a semiconductor tube and electrical interconnects manufactured according to the method of fig5 a . the optical micrograph of the electrically injected rolled - up semiconductor tube device clearly depicts the free - standing semiconductor tube 570 , p - metal 590 contact , and the n - metal 550 contact . an sem image of the p - metal contact and the free - standing semiconductor tube region is shown in the inset to the right . accordingly in this design , electrons and holes are injected directly from the supporting side - pieces and the top surface of the free - standing semiconductor tube respectively . the radiative recombination of charge carriers in the quantum dot active region leads to the emission of photons , which can be largely confined in the micro - tube ring resonator formed by the semiconductor tube 570 . referring to fig6 a there are depicted micrographs of semiconductor tubes manufactured according to embodiments of the invention . first image 610 being a scanning electron microscopy ( sem ) image of a single - walled ingaas qd semiconductor tube with approximately 1 . 2 turns wherein the etched gaas , rolled - up semiconductor tube ( semiconductor tube ), and unetched region are easily identified . cathodoluminescence monochromatic analysis of the structures has shown that the ingaas / gaas quantum dot ( qd ) semiconductor tube is highly uniform and bright compared with the as - grown qd layer , suggesting a significant improvement of the qd optical quality . second image 620 shows a scanning electron microscopy image of a semiconductor tube wherein the etched gaas , formed semiconductor tube , and unetched region are easily identified . third image 630 shows in detail a semiconductor tube transferred according to the process described above in respect of fig4 a showing that the excellent structural properties of the semiconductor tube are maintained . fourth image 640 shows an ingaas / gaas quantum dot semiconductor tube onto si substrate . each of third and fourth images showing the engineered edge profile of the mesa prior to rolling - up that the inventors have identified as allowing precisely tailored optical modes to be achieved . now referring to fig6 b there are micrographs of semiconductor tubes manufactured according to embodiments of the invention . in fifth image 650 the controlled surface geometry of the semiconductor tube is evident where the surface geometry is directly related to the corrugations introduced at the inner edge of the u - shaped mesa . as described supra reduction in radiative losses through the substrate can be achieved when the region between the two side pieces of the u - shaped mesa is etched to approximately 1 μm before the tube formation , thereby increasing the air gap between the central part of the tube and the substrate . this is shown in sixth image where the deeper trench is evident as the central dark region against the lighter surrounding substrate and semiconductor tube . seventh image 670 shows a semiconductor tube transferred onto a si substrate using the newly developed substrate - on - substrate transfer technique described in respect of fig4 a showing the ingaas / gaas qd semiconductor tube after transfer without degradation of the semiconductor tube or the sinusoidal corrugation resulting from the inner edge of the u - shaped mesa being formed with an engineered geometry . the measured tube diameter , shown in the inset of seventh image 670 is approximately 5 . 2 μm . finally in eighth image 680 an sem image of a free - standing ingaas / gaas quantum dot semiconductor tube semiconductor tube is shown wherein the center part of the semiconductor tube is directly over an etched region of the target substrate to reduce any radiative loss through the substrate . it is also evident in this image that the rolled - up structure has broken so that the edges have layers of decreasing width wherein the material not lifted from the substrate is shown as remaining triangular region . referring to fig7 there is depicted an sem micrograph of a semiconductor tube manufactured according to an embodiment of the invention wherein the etched gaas buffer layer 710 , partially rolled - up semiconductor tube 740 , etched region 720 where the alas sacrificial layer has been etched away and unetched region 730 where the alas sacrificial layer has yet to be etched away where in the ingaas / gaas bilayer is still planar . as shown in the enlarged sem the end of the semiconductor tube is shown with an inner diameter of approximately 5 . 2 μm which is in excellent agreement with the calculated values using continuum mechanical models as will be evident in the results presented below . within the preceding descriptions of manufacturing semiconductor tubes according to embodiments of the invention the semiconductor tube comprises an ingaas / gaas bilayer heterostructure with quantum dots formed in one or two in0 . 5ga0 . 5as qd layers . the inventors have demonstrated self - organized quantum dots in strained - layer epitaxy of iii - v semiconductors , wherein the coherently strained and nearly defect - free quantum dots are formed in the stranski - krastanow growth mode . both molecular beam epitaxy ( mbe ) and metal organic chemical vapor deposition ( mocvd ) have been utilized for the fabrication of self - organized quantum dot heterostructures . in the stranski - krastanow growth mode , the transition from a layer - by - layer growth to the formation of three - dimensional islands is governed by the interplay between the interface energy and strain energy . the critical layer thickness , corresponding to the onset of island formation , being largely determined by the lattice mismatch . above the critical layer thickness , elastic strain relaxation occurs via the formation of coherently strained , defect - free islands . examples of self - organized qd structures on gaas and si layers see z . mi et al in “ iii - v compound semiconductor nanostructures on silicon : epitaxial growth , properties , and applications in light emitting diodes and lasers ” ( j . nanophotonics , vol . 3 , 031602 , 2009 ), p . bhattacharya et al in “ quantum dot lasers : from promise to high - performance devices ” ( j . cryst . growth , 311 , pp 1625 - 1631 , 2009 ), and z . mi et al in “ high performance quantum dot lasers and integrated optoelectronics on si ” ( proc . ieee , vol . 97 , no . 7 , pp 1239 - 1249 ). now referring to fig8 a and 8b there is depicted the origin of the optical mode structure within a semiconductor tube fabricated according to an embodiment of the invention . the unique emission characteristics of a semiconductor tube with quantum dots can be analyzed , if as an approximation , in the simplest case , the semiconductor tube ring structure is considered as a planar dielectric waveguide with periodic boundary conditions . illustrated in fig8 a is an sem image of a semiconductor tube as well as the equivalent waveguide model , wherein the outside edge ( or the surface corrugation ) of the semiconductor tube corresponds to the tapered region of the waveguide . z and l directions , shown in the waveguide model in fig8 a , correspond to the tube axial direction and the direction around the tube circumference , respectively . using this model , effective refractive index , neff ( z ), for photons propagating along the l direction , averaged over the length of the waveguide ( or the circumference of the semiconductor tube ). as a result , neff ( z ) is directly related to the size and shape of the tapered region . since the confined optical modes in a single walled semiconductor tube ring resonator is linearly polarized , with the electric field parallel to the tube wall ( the z axis ), then it is possible to derive the eigenmode distributions of the equivalent two - dimensional waveguide . from the scalar helmholtz equation ( 1 ) below . where e ( l , z ) is the electrical field distribution and k is the vacuum wave vector . utilizing e ( l , z )= φ ( z ) e iβl , where z is the transverse field distribution along the z direction and β is the propagation constant along the l direction , we can obtain equation ( 2 ) for the transverse optical modes from equation 1 . for any given wavelength , discrete eigenvalues of equation ( 2 ), i . e ., p = 0 , 1 , 2 , 3 , . . . , can be calculated , which correspond to various transverse modes supported by the waveguide . therefore , dispersion properties of the equivalent planar dielectric waveguide can be obtained by solving equation ( 2 ) over a wide wavelength range . dispersion curves ( p versus photon energy ) for the first three transverse modes ( p = 0 , 1 , and 2 ) are shown in the upper graph 800 a of fig8 b ( solid lines ). in this calculation , the tapered region is approximated as a parabolic shape . the cavity eigenmodes are subsequently determined from the intersections between these dispersion curves and the curves describing the azimuthal resonances ( dashed lines ), i . e . β = 2π × m / l , where l is the circumference of the semiconductor tube and m is the azimuthal mode number . shown in fig8 b , it can be seen that the calculated results are in excellent agreement with the measured values which are shown in the measured spectrum 800 b in fig8 b . now referring to fig9 there are shown simulation results for semiconductor tubes according to embodiments of the invention . first simulation 910 and second simulation 920 show optical resonance mode profiles , calculated by the finite - difference time domain method , for both an ideal ring resonator ( first simulation 910 ) and a rolled - up semiconductor tube device ( second simulation 920 ) with the same diameter ( approximately 5 μm ) and wall thickness ( approximately 50 nm ). it is seen that , while photons are well confined in an ideal ring resonator , strong light scattering occurs at the inside and outside edges of a rolled - up semiconductor tube device . the light scattering effect and , consequently , the q - factors of the optical cavities , depend strongly on the number of revolutions of the semiconductor tube . q - factors between approximately 6 , 000 and approximately 40 , 000 have been calculated for rolled - up semiconductor tube ring resonators with 1 and 4 revolutions , corresponding to wall thicknesses of approximately 50 nm and 200 nm respectively . evidently , rolled - up semiconductor tube devices offer the distinct advantages of directional emission as well as controlled output coupling efficiency , which are often difficult to realize in conventional micro - and nanoscale semiconductor optical cavities . also shown in fig9 are third simulation 930 and model 940 . the confined optical mode , from finite - difference time domain method , shown as azimuthal mode profile for photons ( m = 37 ) confined in a rolled - up tube with a diameter of approximately 5 . 6 μm and wall thickness of 100 nm is shown in third simulation 930 . it is seen that coherent emission from rolled - up semiconductor tube is predominantly determined by the photon scattering occurred at the inside edge . the calculated q - factor is & gt ; 14 , 000 , which is primarily limited by the optical scattering at the inside and outside edges and , in practice , any irregularities on the surface of the tube as well . this unique phenomenon is enormously important for achieving micro - and nanoscale lasers with controlled emission direction and output efficiency that are generally difficult to realize using photonic crystal , microdisk , and toroidal based optical cavities . the optical resonance modes in rolled - up semiconductor tube are also strongly influenced by the presence of surface corrugations . the first two axial field distributions associated with each azimuthal optical mode confined in the rolled - up semiconductor tube are schematically shown in model 940 , which explains the observed higher order modes near the dominant azimuthal modes in the emission spectra presented in fig1 to 16 below . as shown within the semiconductor tube 944 are first longitudinal mode 942 and second longitudinal mode 946 . it is also evident that control of the lasing modes can possibly be achieved in rolled - up micro - and nanotube lasers by varying the semiconductor tube surface geometry . the mode competition amongst various azimuthal modes may not be significant , since these modes are separated by approximately 20 mev , which is larger than the homogeneous linewidth of a single dot ( approximately 10 - 15 mev ) at room temperature . however , strong mode competition for the various axial modes associated with the same azimuthal mode number is expected to occur , due to their small ( approximately 2 - 6 mev ) separation in energy . referring to fig1 depicts simulation results for semiconductor tubes according to embodiments of the invention for a rolled - up semiconductor tube with a small wall thickness ( approximately 75 nm ), again by finite - difference time - domain methods . it was found that tm modes , with an electric field parallel to the tube wall , can be established as optical resonance modes . the calculated tm mode profiles with and without the presence of a gaas substrate are shown in first and second simulations 1010 and 1020 respectively . radiative losses through the substrate , evident in first simulation 1010 , are identified to be the primary cause for the observed small q factor of semiconductor tubes with small air gaps to the substrate . it is further calculated that significantly improved q factors , & gt ; 5000 , can be readily achieved in free - standing qd semiconductor tube resonators . although an ideal cylindrical resonator consists of a regular sequence of resonance modes , the observed single optical mode of a semiconductor tube is explained by the spiral asymmetry and other imperfections in the semiconductor tube formation . as shown in second simulation 1020 wherein the gaas substrate separation from the semiconductor tube has been increased , e . g . by etching this region of the substrate prior to rolling - up the semiconductor tube , see perspective view 500 c and trench 5000 . now referring to fig1 depicts optical emission spectra for semiconductor tubes according to embodiments of the invention . first emission spectrum 1110 depicts cathodoluminescence ( cl ) measurements for an ingaas / gaas qd semiconductor tube ring resonator taken directly from the qd semiconductor tube resonator at 100 k and is also compared with that of the as - grown qd layer ( inset of first emission spectrum 1110 ). an optical resonance mode at approximately 1020 nm can be observed , proving , for the first time , that a rolled - up semiconductor tube , with an average wall thickness of approximately 75 nm , can serve as an optical ring resonator . the emission linewidth is approximately 5 nm , corresponding to a cavity q factor of 204 . it may also be noted that , with the reduced strain distribution in the semiconductor tubes , there is a small red shift ( approximately 10 mev ) in the qd signal . second emission spectrum 1120 depicts for a rolled - up quantum dot semiconductor tubes with an engineered surface geometry where a raman spectrum for these semiconductor tubes is shown , wherein peaks associated with the ingaas and gaas layers , and the si substrate can be clearly identified third emission spectrum 1130 depicts the emission of a freestanding quantum dot semiconductor tube with the presence of corrugations at an excitation power of approximately 30 μw at room temperature is shown . this detailed view of the eigenmodes associated with azimuthal mode number m = 29 is shown with the axial mode numbers ( p ) identified . the two non - degenerate modes associated with p = 0 are induced by the inside and outer side edges around the tube . additionally , associated with each azimuthal mode m is a group of optical resonance modes with different axial field distributions , which are directly related to light localization along the tube axis due to the presence of corrugations . evidently , by varying the tube geometry , an exact tailoring of the 3 - dimensionally confined optical modes can be achieved . a minimum intrinsic linewidth of approximately 0 . 4 nm is derived for these structures , corresponding to a q - factor of ˜ 3 , 000 . it is important to note that such a relatively high q - factor is achieved in a single wall semiconductor structure , with a wall thickness of merely 50 nm . now referring to fig1 there are shown first to fourth optical emission spectra 1210 through 1240 respectively are shown . considering initially first and second optical emission spectra 1210 and 1220 respectively the emission characteristics of a free - standing ingaas / gaas quantum dot semiconductor tube optical ring resonator on gaas was studied using micro - photoluminescence measurements . in these measurements the semiconductor tube with ingaas / gaas bilayer heterostructure with approximately 2 . 5 revolutions , therefore with wall thicknesses varying from approximately 100 nm to approximately 150 nm the sample was mounted on a cryostat with continuous liquid nitrogen flow and cooled to 77 k . a semiconductor laser , with an emission wavelength of 641 nm was focused onto the free - standing region of the semiconductor tube using an objective ( 100 ×, na = 0 . 7 ). the emitted light was collected by the same objective , analyzed by a spectrometer , and detected by a liquid nitrogen cooled ingaas detector and lock - in amplifier . in this measurement scheme , both the excitation and signal collection are located at the same spot . the emission characteristic measured at a pump power of 22 μw is shown in first optical emission spectrum 1010 showing sharp optical resonant modes , spaced apart by approximately 14 mev . it should also be noted that the presence of the inside and outside edges leads to non - degenerate optical modes , illustrated in second optical emission spectrum 1220 . an intrinsic q factor of approximately 3 , 000 was derived for the structure . analysis using finite - difference time domain methods determined that the observed optical modes are tm polarized , with an electric field parallel to the semiconductor tube wall . in third and fourth optical emission spectra 1230 and 1240 respectively the emission characteristic of 3 - dimensionally confined ingaas / gaas quantum dot semiconductor optical ring resonators transferred onto si substrates are presented . the measurement scheme was identical to that described above in respect of first and second optical emission spectra 1210 and 1220 respectively . the photoluminescence spectrum measured from the free - standing quantum dot semiconductor tube is shown in third optical emission spectrum 1230 , which exhibits five dominant optical eigenmodes , curve 1240 a . photoluminescence emission directly from the as grown quantum dot ensemble is also shown for comparison with second curve 1240 b . referring to fourth optical emission spectrum 1140 which is an expansion of a region of third optical emission spectrum 1130 between 1090 nm and 1120 nm axial optical modes can also be observed which are related to the engineered shape of the semiconductor tube optical ring resonator . these measurements being taken with a pump power of 15 μw at 77k . both the axial and radial modes are therefore illustrated in the fourth optical emission spectrum 1240 . referring to fig1 there are depicted first to third optical emission spectra 1310 to 1330 respectively for semiconductor tubes according to embodiments of the invention . the emission characteristics of an ingaas / gaas bilayer heterostructure with quantum dots are shown using micro - photoluminescence spectroscopy at 293k . shown in first optical emission spectrum 1310 the emission spectrum of semiconductor tube resonators with a wall thickness of approximately 250 nm under a pump power of approximately 30 μw is shown wherein six sharp optical resonant modes , equally separated by approximately 16 mev , can be clearly identified . by reducing the tube wall thickness to approximately 100 nm , the observed spectral eigenmodes related to light localization along the tube axis were observed with an intrinsic linewidth of approximately 0 . 6 nm , corresponding to a q - factor of ˜ 2 , 000 . this being depicted in second optical emission spectrum 1320 . similarly emission characteristics of ingaas / gaas qd semiconductor tubes at 77k are shown in third optical emission spectrum 1330 for a pump power of 32 μw . six groups of sharp optical resonant modes , corresponding to orders 39 to 44 are evident , with the dominant modes of each group spaced apart by approximately 20 . 5 mev . emission from the as - grown qd layers is also shown for comparison . additionally , associated with each azimuthal mode is a group of at least five spectral eigenmodes , separated by approximately 3 - 4 mev , which are directly related to light localization along the tube axis due to the presence of surface corrugations now referring to fig1 there are depicted first to third optical emission spectra 1410 to 1430 respectively demonstrating the variations of spectra with wall thickness . again free - standing ingaas / gaas quantum dot semiconductor tube ring resonators were measured using micro - photoluminescence spectroscopy at room temperature wherein the devices were excited with a he — ne laser beam ( λ = 632 . 8 nm ) through a 60 × objective lens . light emitted from the semiconductor tube was collected by the same objective , analyzed by a high - resolution spectrometer with lock - in amplification , and detected using a liquid nitrogen cooled ingaas detector . in these spectra the semiconductor tube devices exhibit diameters of approximately 5 - 6 μm and have wall thicknesses varying from approximately 50 nm to 200 nm and exhibit an engineered surface geometry , which can be approximated as a parabolic shape . the measured emission spectra of semiconductor tubes with wall thicknesses of approximately 50 nm , 100 nm , and 200 nm are shown in first to third optical emission spectra 1410 to 1430 respectively evident that the emission spectra are characterized by several groups of sharp optical resonance modes , which are denoted by associated azimuthal and axial mode numbers ( m , p ), due to photon confinement around the circumference and axial directions of the tube , respectively . the energy separations between the adjacent azimuthal modes are approximately 24 , 21 and 19 mev , and the energy separations between the adjacent axial modes are approximately 7 , 4 and 2 - 3 mev , for semiconductor tubes with wall thicknesses of approximately 50 nm , 100 nm , and 200 nm , respectively . the dependence of emission characteristics of semiconductor tube ring resonators on the surface geometry can be explained by an equivalent planar waveguide model with periodic boundary conditions . in this model , the unique surface geometry of the semiconductor tube can be modeled by a tapered region in the dielectric waveguide . details about this model are described above . in this analysis , the axial optical field distribution φ ( z ) can be derived from the equation ( 3 ) below . where z represents the tube axial direction , k is the vacuum wave vector , and β is the propagation constant along the tube circumference . neff ( z ) is the effective refractive index averaged over the circumference of the tube , which is directly related to the tube surface geometry . for a given wave vector k , discrete eigenvalues of β , i . e ., βp ( k ) ( p = 0 , 1 , 2 , 3 . . . ), can be obtained by solving equation ( 3 ) analytically or numerically . in addition , the optical resonance modes satisfy the azimuthal phase matching condition , described by , βl = 2πm where l is the circumference of the semiconductor tube and m is azimuthal mode number . 16 , 20 , 22 , etc for example . the eigenenergy of each optical resonance mode can then be derived from the above equations . the optical mode numbers ( m , p ), shown in first to third optical emission spectra 1410 to 1430 were obtained from this model . detailed studies further confirm that these calculations agree well with the experimental results . now referring to fig1 there are depicted first and second optical emission spectra 1510 and 1520 for semiconductor tubes according to embodiments of the invention and the i - v curve 1530 for an electrically injected optical semiconductor tube emitter . first and second optical emission spectra 1510 and 1520 representing room temperature lasing in rolled - up ingaas / gaas quantum dot semiconductor tube ring cavities , with a diameter of approximately 5 μm and wall thickness of approximately 125 nm , representing 2 . 5 revolutions . first and second optical emission spectra 1510 and 1520 being measured below ( approximately 3 μw ) and above the threshold ( approximately 25 μw ) respectively . the dominant lasing wavelengths are 1193 . 6 nm , 1216 . 5 nm and 1240 . 7 nm , with the corresponding azimuthal mode numbers of 39 , 38 and 37 respectively . referring to i - v curve 1530 the integrated intensity of the emission peak at 1240 . 7 nm as a function of the absorbed pump power by the semiconductor tube is plotted . an ultralow threshold of approximately 4 μw is estimated . variation of spectral linewidth versus optical pump power is shown in the inset of third optical emission spectrum 1530 . with the increase of pump power , a linewidth reduction from approximately 0 . 6 - 0 . 8 nm to approximately 0 . 4 - 0 . 5 nm is observed , which agrees well with the measured threshold , further confirming lasing from the semiconductor tube cavity . a small increase of the spectral linewidth at higher pump power is also evident , possibly due to heating effect . other lasing modes exhibit similar characteristics . fig1 depicts the variation in optical emission for semiconductor tubes according to embodiments of the invention showing the impact of the profile of the end of the semiconductor “ sheet ” that is rolled up . as above a bilayer heterostructure ingaas / gaas qd semiconductor tube ring resonator was investigated using micro - photoluminescence spectroscopy at 300 k with he — ne laser excitation ( 632 . 8 nm ) to optically excite the device through a 60 ( 0 . 8 na ) objective lens . the spectrally resolved emission is detected by an ingaas detector with lock - in amplification . in regions of the semiconductor tube that are attached to the substrate , a broad emission spectrum is generally observed , shown as the dotted line 1640 in first spectrum 1610 . the absence of any optical resonance modes is largely due to radiative loss through the substrate . a typical emission spectrum measured from the free - standing region of such a semiconductor tube is shown as the solid line 1630 in first spectrum 1610 . this spectrum being characterised by a sequence of regularly spaced optical resonance modes superimposed on a broad ingaas / gaas qd emission spectrum the pump power was 27 mw . these resonance modes , arising from photons confined around the periphery of the semiconductor tube by total internal reflection , are separated by approximately 19 . 5 mev . the corresponding azimuthal numbers ( m = 38 to 45 ) were derived from modeling the semiconductor tube as being of diameter approximately 6 μm and 2 . 4 revolutions . the relatively small q - factor ( approximately 350 ) is attributed to the poor optical confinement provided by the random surface roughness along the tube axial direction . first insert 1615 shows an sem of the semiconductor tube . a significantly different emission spectra , however , is observed in freestanding semiconductor tubes with an engineered surface geometry , see second insert 1625 in second spectra 1620 . first to third emission spectra 1650 to 1670 being measured at pump powers of 27 μw , 12 μw , and 8 μw respectively at 300k . the optical resonance mode distribution for the semiconductor tube employed in first spectrum 1620 is also shown ( dotted curve 1680 ) for comparison . careful examination reveals that there are eight groups of eigenmodes , with the lowest energy mode in each group approximately aligned to the modes non - structured design . additionally , each group of resonance modes consists of four sharp peaks , separated by approximately 3 - 5 mev , which are directly related to the strong photon confinement along the tube axial direction by the intentionally introduced corrugations on the tube surface , evident in second insert 1625 . the resulting axial field dispersion also implies that the wave vector of each confined photon is not only determined by the azimuthal mode number ( m ) but also directly related to an additional axial mode number ( p ), thereby leading to different eigen energies . the minimum intrinsic linewidth of 0 . 5 mev at room temperature was established , which corresponds to a maximum q - factor of approximately 2000 . further improvement in the q - factor may be achieved by optimising the optical confinement along the tube axial direction . referring to fig1 there is depicted an i - v plot 1710 for an electrically injected optical semiconductor tube emitter and the polarization behaviour of an optically pumped semiconductor tube according to embodiments of the invention . with the p - contact placed directly near the device active region , the device resistance and heating effect can be drastically reduced . in spite of the presence of metal contacts on the tube surface , optical resonance modes were clearly observed under optical pumping in first spectrum 1720 . the polarization properties of the coherent emission from semiconductor are plotted in polarization plot 1730 . for photons circulating around the periphery of the tube , electric fields of the te and tm modes are defined as parallel and normal to the tube surface , respectively . the polarization measurements were performed by inserting a linear polarizer in the optical beam path . the semiconductor tube and polarizer were carefully aligned such that 0 ° and 90 ° correspond to te and tm polarizations , respectively . the peak intensity was then recorded by varying the polarization angle . plotted in polarization plot 1730 is the intensity of the lasing mode at 1240 . 7 nm as a function of the polarization angle . it is seen that the laser emission is primarily te polarized . this observation is also consistent with recent theoretical and experimental studies that only te optical modes , with an electric field parallel to the tube surface , can be supported by a rolled - up semiconductor tube ring resonator with a relatively thin wall ( approximately 40 nm to 200 nm ). referring to fig1 there is depicted the emission spectrum for a semiconductor tube transferred to a silica substrate . as with previous analysis the emission characteristics of semiconductor tube devices transferred on a fiber facet were studied by micro - photoluminescence spectroscopy at room temperature with optical pumping using a he — ne laser at 632 . 8 nm with an absorbed pump power of 20 μw was obtained . the associated azimuthal mode number ( m ) and eigenmodes ( p ) for each resonance mode are identified against these optical resonances in the graph . the semiconductor tube was positioned according to the technique reported by zhaobing tian et al in “ controlled transfer of single rolled - up ingaas — gaas quantum dot microtube ring resonator using optical fiber abrupt tapers ” ( ieee photonics tech . lett ., vol . 22 ( 5 ), pp 311 - 313 ) that as a low stress method demonstrates that the semiconductor tubes are manufactured with low internal stress . the method exploits optical fiber abrupt tapers , made by a fusion splicer machine , which are inserted into each end of the semiconductor tube as the tube diameter φ is larger than the size of the taper tip . the very small contact area between the free - standing semiconductor tube devices and their initial gaas substrate means that the surface tension is much smaller , compared to conventional planar devices . consequently , detaching the semiconductor tube devices from the host substrate can be achieved without introducing any structural defects and / or mechanical distortion and controllably transferred using either one or two fiber tapers and precisely positioned on a foreign substrate . the energy separations for the dominant modes between two adjacent groups and for the two adjacent modes within the same group are approximately 26 and 7 . 5 mev , respectively , which agree well with our calculations . the measured spectral linewidths are approximately 1 nm , corresponding to a q factor of approximately 1100 . the intrinsic - factor may be significantly higher , due to the presence of two non - degenerate modes induced by the inside and outside edges around the tube and can be further improved by optimizing the design and fabrication process . the emission characteristics of quantum - dot semiconductor tubes transferred on the cleaved facet of a fiber are nearly identical , in terms of both the mode profiles and light intensity , to those of similar quantum - dot semiconductor tube devices fabricated directly on gaas substrates , which further confirms the present fiber taper assisted transfer technique is suitable for achieving high - quality micro - and nanotube - based optical cavities on a foreign substrate . finally , it is important to note that emission from the rolled - up tube cavity devices can also be directly coupled to the optical fiber , with the coupling efficiency precisely determined by the vertical separation , or the number of revolutions of the semiconductor tube sidepieces . with the development of the fiber taper assisted transfer technique , it is also expected that nearly defect - free iii - v micro - and nanotube - based nanophotonic devices can be readily achieved on any foreign substrate . more importantly , it provides a viable approach for the monolithic integration of high - performance iii - v semiconductor micro - and nanoscale lasers with si waveguides and other nanophotonic devices on cmos chips for example . referring to fig1 there is depicted a detector assembly 1900 for an optical photodetector according to an embodiment of the invention . as such there shown a semiconductor tube fabricated according to an embodiment of the invention described above either in - situ or transferred using the fiber taper transfer process . considering the scenario that the semiconductor tube 1960 being disposed upon unetched region 1940 , the etched region 1930 being to the left and upon which are deposited first and second electrodes 1920 and 1910 that connect to photodetector leads 1950 and 1970 respectively . these photodetector leads 1950 and 1970 respectively are each connected to one rolled end of the semiconductor tube 1960 , such as described supra in respect of fig5 a and 5b . accordingly a potential difference exists between photodetector leads 1950 and 1970 such that the semiconductor tube 1960 is reverse biased . an optical fiber , for example corning smf - 28 which is a singlemode optical fiber 1980 with an approximately 8 μm core , is positioned laterally with respect to the semiconductor tube 1960 . the singlemode optical fiber 1980 being positioned within a groove , i . e . v - groove on silicon or u - groove on gaas so that the core is vertically aligned with the semiconductor tube 1960 . accordingly optical signals emitted from the singlemode optical fiber 1980 are coupled to the photodetector , formed by reverse biased semiconductor tube 1960 , and the generated photocurrent coupled to electronic circuitry within the integrated circuit of which detector assembly 1900 forms part . it would be evident that microwave / rf optical systems may exploit gaas electronics as well as 10 gb / s , 20 gb / s , and 40 gb / s telecommunications systems whilst data communications and lower speed telecommunication up to about 10 gb / s may exploit silicon electronics . for example the photodetector may form directly part of a circuit with an fet amplifier . it would also be evident to one skilled in the art that the semiconductor tube 1960 may through the use of multiple quantum well structures and quantum dots be implemented as an avalanche photodiode . additionally whilst the biasing of the photodetector has been described as being along the longitudinal axis of the photodetector it would be apparent that a metallization on the upper surface of the film prior to rolling up may be provided such that a the potential may be provided axially through the thickness of the semiconductor tube wall , particularly when the quantum structures are sandwiched between the inner and outer walls . now referring to fig2 depicts schematics of manufacturing semiconductor tubes with metalized inner surfaces and for fabricating a capacitor according to an embodiment of the invention . referring to first schematic 2010 there is shown a rolling process part - way through processing . accordingly there are shown a substrate 2016 upon which have been deposited sacrificial layer 2014 , tube layers 2018 and an upper layer 2012 . accordingly as the sacrificial layer 2014 is etched away the film 2015 comprising tube layers 2018 and upper layer 2012 curls due to the stress distribution within the layers . as etching proceeds as shown in second schematic 2020 the process has continued and now the rolled - up tube has an inner wall that is now completely “ coated ” with the upper layer 2012 . upper layer 2012 may for example be a metal , such as tungsten or copper , an oxide , a polymer , or an organic receptor . where the upper layer 2012 is a metal the resultant semiconductor tubes may provided novel catalytic environments for chemical reactions or the cracking of water through electrolysis with tungsten / copper surfaces for trapping the generated hydrogen and oxygen . where an oxide is employed one option is titanium oxide for the photolytic cracking of water wherein the walls of the semiconductor tubes are either transparent to the required wavelength of the solar spectrum or due to their low thickness provide relatively low absorption . alternatively tungsten oxide may , through its material properties varying with the present of nitrous oxide , hydrogen sulphide , ethanol , carbon monoxide , ammonia and ozone , provide for a change in the optical properties of the semiconductor tubes that may form the basis for sensing devices . likewise polymer and organic receptor materials may provide a means of implementing sensors as the very high q optical cavities would be easily impacted by small changes in the overall optical cavity that would vary when the refractive index shifted from bonding of antigens to an organic receptor for example . also shown in fig2 is a cross - section of a semiconductor tube capacitor implemented according to an embodiment of the invention . accordingly once the semiconductor tube has been rolled up an oxide 2022 and metallization 2024 are patterned onto the semiconductor tube . accordingly through appropriate design of the metallization 2024 and oxide 2022 a thin film variable capacitor may be implemented without the requirements for high resolution photolithography with very high surface geometry as for example is evident in the work of w . m . farnworth et al in u . s . pat . no . 7 , 081 , 385 entitled “ nanotube semiconductor devices and methods of making the same ” wherein the nanotubes were formed vertically upon the substrate . in contrast the nanotubes provided according to embodiments of the invention may be a few microns , tens of microns , or hundreds of microns long and yet all be of consistent diameter such that planar processing in the subsequent stages is the same for all devices irrespective of the tube length , unlike farnworth . also through the unique properties of the semiconductor tubes it may serve as a dielectric material and hence form a capacitor , and it may equally serve as a semiconductor material and form a transistor channel within the same device . further , the consistency of such nanotubes formed by a simple planar deposition / lithography process prior to their rolling - up will result in improved reproducibility of the characteristics of the devices both device - device , die - to - die , and wafer - to - wafer . referring to fig2 there is depicted a schematic for manufacturing semiconductor tubes with high density according to an embodiment of the invention . accordingly in first schematic 2110 an epitaxial structure 2130 has been formed on the substrate 2115 and comprises first to third sacrificial layers 2112 a through 2112 c respectively and first to third bilayer heterostructure qd layers 2114 a through 2114 c respectively that are alternating within the epitaxial structure 2130 . processing of the epitaxial structure 2130 provides within each of the first to third bilayer hetero structure qd layers 2114 a through 2114 c respectively the mesa and patterned edges for the film prior to rolling up . now , as shown etching of the sacrificial layer proceeds to etch each of the first to third sacrificial layers 2112 a through 2112 c respectively such that the first to third bilayer heterostructure qd layers 2114 a through 2114 c respectively begin to curl . now looking at second schematic 2120 this process has proceeded to the point that each first to third bilayer heterostructure qd layers 2114 a through 2114 c respectively has curled completely once to form first to third semiconductor tubes 2125 a through 2125 c are formed . it would be evident to one skilled in the art that using an epitaxial structure such as epitaxial structure 2130 allows the density of the semiconductor tubes to be increased within the finished device . it would also be evident that each of the first to third bilayer heterostructure qd layers 2114 a through 2114 c respectively may be the same or implemented with a different epitaxial structure so that adjacent tubes exhibit different optical properties . for example three adjacent tubes may be provided that emit in the red , green , and blue wavelength regions to form a pixel within a display , or as with sharp quattron four emitter colors including an additional yellow . accordingly as all “ red ” emitters are formed from the same layer in the epitaxial stack they will have improved uniformity . it would be evident that the above referenced process may also be applied to other materials such as lead zirconium titanate ( pzt ), lanthanum doped lead zirconium titanate ( plzt ) and other ceramics in thin film form to exploit their piezoelectric and ferroelectric properties to yield electrically tunable structures , such as adjusting the diameter of the resonator for example . the above - described embodiments of the present invention are intended to be examples only . alterations , modifications and variations may be effected to the particular embodiments by those of skill in the art without departing from the scope of the invention , which is defined solely by the claims appended hereto . | 7 |
any polysaccharide which is susceptible to hydroxyalkylation is suitable for this reaction . in general , polysaccharides useful in this process include any polymers of simple sugars ( monosaccharides ), for example , starches and cellulose compounds . polysaccharides useful in this invention include those described in hendrickson et al ., organic chemistry , 3d ed ., pp . 989 - 994 , mcgraw - hill , inc . ( new york ), 1970 ( incorporated herein by reference ). polysaccharides useful in this process include those which contain repeating units corresponding to the formula ## str1 ## polysaccharides useful in this process include substituted polysaccharides such as substituted starches and substituted cellulose , for example , methyl - substituted cellulose and ethyl - substituted cellulose . alkylene carbonates useful in this invention include those which correspond to the formula ## str2 ## wherein ( r ) 2 is separately in each occurrence hydrogen , c 1 - 20 hydrocarbyl or c 1 - 20 hydrocarbyl - substituted , with one or more of the following : a halo , hydroxyl , cyano , nitro , thioalkyl , alkoxy , aryloxy , aralkoxy , carbonyldioxyalkyl , carbonyldioxyaryl , carbonyldioxyaralkyl , alkoxycarbonyl , aryloxycarbonyl , alkylcarbonyl , arylcarbonyl , aralkylcarbonyl , alkylsulfinyl , arylsulfinyl , aralkylsulfinyl , alkylsulfonyl , arylsulfonyl or aralkylsulfonyl group . r is preferably hydrogen , a c 1 - 20 alkyl , a c 1 - 20 alkenyl or a c 1 - 20 haloalkyl group ; more preferably hydrogen , a c 1 - 3 alkyl , a c 1 - 3 haloalkyl or a c 1 - 3 alkenyl group ; even more preferably hydrogen or methyl ; and most preferably hydrogen . preferable alkylene carbonates include ethylene carbonate , propylene carbonate , butylene carbonate , vinylene carbonate and phenylene carbonate . more preferred are ethylene carbonate and propylene carbonate , with ethylene carbonate being most preferred . if the polysaccharide is unsubstituted , it is hydroxyalkylated at the 2 position . the following formula demonstrates the common numbering system for a saccharide unit ## str3 ## such products contain saccharide units which correspond to the formula ## str4 ## in the embodiment wherein the polysaccharide is substituted , generally the substituent is on the oxygen attached to the 2 carbon . the product of the reaction with alkylene carbonate in the presence of a quaternary ammonium halide is a cross - linked polysaccharide . the polysaccharides are linked by carbonate ether units ## str5 ## the carbonate moiety reacts with the hydroxyl on one saccharide unit , while the ether portion reacts with a hydroxyl unit on another saccharide unit . the cross - linking of two saccharide units can be represented by the following formula ## str6 ## wherein r is as defined above and r 2 is a c 1 - 20 hydrocarbyl group . r 2 is preferably c 1 - 10 alkyl , most preferably methyl or ethyl . the cross - linked product can be converted to the 4 - hydroxyalkyl polysaccharide by treatment with base as will be described hereinafter . in the process of this invention , the polysaccharides are dispersed in the alkylene carbonates . preferably between 1 and 30 percent by weight of the polysaccharides are dispersed in between 70 and 99 weight percent alkylene carbonate , with between about 5 and 15 weight percent of polysaccharide in between about 85 to 95 weight percent of an alkylene carbonate being most preferred . the catalysts for this reaction are quaternary ammonium halides . preferred catalysts are tetraalkylammonium halides . preferred halides are chlorides and bromides . examples of preferred tetraalkylammonium halides include tetramethylammonium chloride , tetramethylammonium bromide , tetraethylammonium chloride , tetraethylammonium bromide , hexadecyl trimethylammonium chloride , hexadecyl trimethylammonium bromide , tetrabutylammonium bromide , tetrabutylammonium chloride , tetrapropylammonium bromide , tetrapropylammonium chloride , trioctyl methylammonium bromide , trioctyl methylammonium chloride , hexyltriethylammonium bromide , hexyltriethylammonium chloride , octyltriethylammonium bromide , octyltriethylammonium chloride , decyltriethylammonium chloride , decyltriethylammonium bromide , dodecyltriethylammonium chloride , dodecyltriethylammonium bromide , hexadecyltriethylammonium bromide and hexadecyltriethylammonium chloride . generally any amount of catalyst which results in catalysis of the reaction described herein is suitable . preferable amounts of catalyst are between about 0 . 5 and 10 . 0 percent by weight of the reactants , with between about 2 and 5 percent by weight being most preferred . this process can be run at any temperature at which the reaction proceeds . preferable temperatures are between 80 ° c . and 140 ° c . below 80 ° c . the reaction rate is extremely slow , above 140 ° c . decomposition of the reactants and products takes place . more preferable temperatures are between about 110 ° c . and 140 ° c . this process is generally run at atmospheric pressures , although subatmospheric and superatmospheric pressures would be suitable . it may be desirable to run the reaction in an inert gas atmosphere , such as nitrogen or argon , as some of the reactants may be air sensitive . this process results in the hydroxyalkylation of up to about 40 percent of the saccharide units . the hydroxyalkylated polysaccharide can be separated from the alkylene carbonate and soluble catalyst by filtration . residual alkylene carbonate can be removed from the product by washing the product with an alkanol or ketone , such as methanol or acetone . the alkylene carbonate and catalyst can be recycled once the hydroxyalkylated polysaccharide has been filtered out . in the embodiment wherein the polysaccharide is substituted , a cross - linked product is prepared by the process described instead of the hydroxyalkylated product . the cross - linking occurs between the hydroxyl moieties on the 4 position of the saccharide units . such cross - linked products can be converted to hydroxyalkylated polysaccharides by treating them with an aqueous solution of base . preferably , the aqueous solution contains at least 5 percent by weight of base , most preferably between 5 and 15 percent by weight of base . preferable bases include alkali metal hydroxides , alkaline earth metal hydroxides , alkali metal carbonates and alkaline earth metal carbonates . a sufficient amount of the aqueous base solution to decompose the carbonate ether moieties which link the saccharide units is used . preferably between about 10 and 20 , weight percent of the aqueous base solution is used . upon treatment with base , the carbon dioxide is evolved . cessation of evolution of carbon dioxide indicates completion of the reaction . co 2 is eliminated from the carbonate - ether linkage between the saccharide units and the ether unit is retained on the saccharide unit to which it was attached during cross - linking so that such saccharide unit is hydroxyalkylated . substituted polysaccharides are generally water - soluble . the cross - linked substituted polysaccharides are water - insoluble and the hydroxyalkylated - substituted polysaccharides are water - soluble . the conversion of cross - linked polysaccharides to hydroxyalkylated polysaccharides can be done at any temperature at which the reaction proceeds . preferable temperatures are between about 40 ° c . and 80 ° c ., preferably between 50 ° c . and 60 ° c . the following examples are included for the purpose of illustrating the invention and do not limit the scope of the invention and claims . all parts and percentages are by weight unless specified otherwise . to a three - neck round - bottom flask is added 5 g of douglas pearl ® corn starch , 50 g of ethylene carbonate and 2 . 75 g of tetraethylammonium bromide ( 5 percent load by weight ). the reagents are stirred under nitrogen for three hours at elevated temperatures . upon completion of the reaction , the starch is removed from the ethylene carbonate by filtration , the solid cake is rinsed with acetone or remove any residual ethylene carbonate and dried . analysis for degree of substitution is done using a modified zeisel gas chromatographic method . the experiment is run at temperatures of 50 ° c ., 80 ° c ., 100 ° c . and 140 ° c . the table demonstrates the degree of substitution after three hours . table______________________________________example temperature degree of substitution______________________________________1 50 ° c . 02 80 ° c . 0 . 0943 100 ° c . 0 . 184 140 ° c . 0 . 31______________________________________ the table demonstrates that the degree of hydroxyalkylation increases with temperature . it is further demonstrated that at 50 ° c ., no detectable hydroxyalkylation is detected . | 2 |
the present invention is directed to a secure network interface unit ( sniu ), which is utilized to control communications between a user such as a computer host and a network . the sniu intercepts internet protocol ( ip ) datagrams as they are transmitted between the user and the network . the sniu determines whether each datagram from the user is releasable to the network and if and how it should be encrypted . the sniu decrypts each datagram from the network and determines whether it is releasable to the user . when a sniu releases a datagram from a lower classification user or network to a higher classification user or network ( i . e ., a write up ), the datagram is used to predict the expected response . when a datagram is received from the higher classification user or network , the sniu compares the datagram to the response which was predicted during the write up and , only if they match , releases it ( i . e ., allows the write down ) to the lower classification user or network . the sniu implements a custom trusted session protocol ( tsp ) to establish associations ( described later ) prior to permitting any communication between a user and a network . the tsp authenticates users , exchanges security parameters between snius , and establishes encryption keys for an association . this method of providing security allows existing network assets and existing network protocols to continue to be used , thereby avoiding the need to replace an installed network base for implementation of the multi - level security system . the connected host or user equipment and the network backbone are therefore not required to be secure ( trusted ). the sniu according to the present invention can be configured in a number of different embodiments depending on the particular physical locations and forms of implementation . these embodiments include a standalone hardware sniu (“ guard ”) and a software sniu (“ companion ”). the hardware embodiment of the sniu is implemented as a stand alone hardware device . such a configuration is desirable , since the guard sniu is highly trusted . the guard sniu is configured to be inserted between existing hosts and a network . the sniu is transparent to the host , and any legacy system or application software running on the host . the guard sniu provides protection for any host connected to an ip based network . there is no requirement that the attached host computers run a trusted operating system . the guard sniu provides a trusted boundary between the protected hosts and the unprotected network . protected means that the connection is with another known sniu ( a unique digital signature identifies the sniu ), the messages are confidential ( encrypted ) and unaltered ( cryptographic residues validate the packet ). the software embodiment of the sniu is implemented primarily as a software function resident in and executed from the host machine . the only hardware required is a commercially available cryptographic card ( e . g ., a fortezza card ) which plugs into the host computer &# 39 ; s pcmcia card reader , for example . such a configuration is desirable , since the companion sniu is designed to be installed in - existing portable computers , which avoids the additional cost of additional hardware required by a guard sniu . the companion sniu provides the same network security features as the stand alone sniu when the host computer is connected to home enterprise &# 39 ; s network . the software sniu also extends that same level of security across the internet ( or any other unprotected network ) when the user is on the road and is remotely communicating with the enterprise network or other remotely located computer devices including a similar companion sniu . the companion sniu provides all of the functionality and security of the guard sniu as well as complete interperability with these devices . the software comprising the companion sniu is based on the same software utilized in the guard sniu . the user of the companion sniu however , assumes an acceptable risk in exchange for not requiring additional hardware required by a guard sniu , which cannot be circumvented or corrupted via attacks originating from external hardware . by providing reasonable software protection ( not allowing unauthorized personnel physical access ) and software protection ( anti - virus protection ), a companion sniu can be utilized providing the user with an acceptable level of risk . if the user is confident that the software comprising the companion sniu is not circumvented or modified , then he can enjoy the same degree of confidence as the user of a guard sniu device . referring to fig1 , there is shown an example of a multi - level security ( mls ) system in accordance with the present invention . this system 10 incorporates the various embodiments of the snius ( guards and companions ) in order to provide mls for computer networks such as the internet . for example , the guard devices 14 , 16 which are hardware embodiments of the sniu are coupled between computer networks 34 , 36 , 38 providing inter - network security . additional guard devices 12 , 18 are coupled between users such as computer hosts 28 and 30 , and the respective networks 34 and 38 . the software embodiment of the sniu are implemented as companions within computer hosts 24 , 26 , which provides network security without requiring additional hardware . the auditors 20 , 22 are also guard snius which are configured to communicate directly with the other snius ( guards and companions ) to log audit events and potentially signal alarms . the above described system 10 enables secured , and non - secured users such as a web site 40 , to communicate with each other without the danger of compromising security . during operation , the snius included in the above described system 10 communicate with each other thereby creating a global security perimeter for end - to - end communications and wherein the network may be individually secure or non - secure without compromising security of communications within the global security perimeter . the sniu devices in accordance with the present invention may implement a number of security policies suitable to the circumstances of a given network environment . the major policy areas are : discretionary access control ; mandatory access control ; object reuse ; labeling ; identification and authentication ; audit ; denial of service detection ; data type integrity ; cascading control ; and covert channel use detection . discretionary access control is a means of restricting access to objects ( data files ) based on the identity ( and need to know ) of the user , process , and / or group to which the user belongs . it may be used to control access to user interface ports based on the identity of the user . for a single - user computer unit , this mechanism may be implemented in the sniu , whereas for a multi - user host , the dac control may be implemented at the host machine . discretionary access control may also be implemented as discretionary dialog addressing , wherein the addressing of all communications originated by a user is defined , and for user discretionary access denial , wherein a user may refuse to accept a communication from another user . mandatory access control is a means of restricting access to objects based on the sensitivity ( as represented by a classification label ) of the information contained in the objects , and the formal authorization ( i . e ., clearance ) of the user to access information of such sensitivity . for example , it may be implemented as dialog lattice - based access control , wherein access requires a correct classification level , integrity level , and compartment authorization , dialog data - type access control , wherein correct data type authorization is required for access , and cascade protection , wherein controls are provided to prevent unauthorized access by cascading user access levels in the network . object reuse is the reassignment and reuse of a storage medium ( e . g ., page frame , disk sector , magnetic tape ) that once contained one or more objects to be secured from unauthorized access . to be secured , reused , and assigned to a new subject , storage media must contain no residual data from the object previously contained in the media . object reuse protection may be implemented by port reuse protection , session reuse protection , dialog reuse protection , and / or association reuse protection . labeling requires that each object within the network be labeled as to its current level of operation , classification , or accreditation range . labeling may be provided in the following ways : user session security labeling , wherein each user session is labeled as to the classification of the information being passed over it ; dialog labeling , wherein each dialog is labeled as to the classification and type of the information being passed over it ; and host accreditation range , wherein each host with access to the secured network is given an accreditation range , and information passing to or from the host must be labeled within the accreditation range . identification is a process that enables recognition of an entity by the system , generally by the use of unique user names . authentication is a process of verifying the identity of a user , device , or other entity in the network . these processes may be implemented in the following ways : user identification ; user authentication ; dialog source authentication , wherein - the source of all communication paths is authenticated at the receiving sniu before communication is allowed ; sniu source authentication , wherein the source sniu is authenticated before data is accepted for delivery ; and administrator authentication , wherein an administrator is authenticated before being allowed access to the security manager functions . an audit trail provides a chronological record of system activities that is sufficient to enable the review of an operation , a procedure , or an event . an audit trail may be implemented via a user session audit , a dialog audit , an association audit , an administrator audit , and / or a variance detection , wherein audit trails are analyzed for variance from normal procedures . denial of service is defined as any action or series of actions that prevent any part of a system from functioning in accordance with its intended purpose . this includes any action that causes unauthorized destruction , modification , or delay of service . the detection of a denial of service may be implemented for the following conditions : user session automatic termination , such as when unauthorized access has been attempted ; user machine denial of service detection , such as detection of a lack of activity on a user machine ; dialog denial of service detection ; association denial of service detection , such as detection of a lack of activity between snius ; and / or data corruption detection , such as when an incorrect acceptance level is exceeded . covert channel use is a communications channel that allows two cooperating processes to transfer information in a manner that violates the system &# 39 ; s security policies . detection of covert channel use may be implemented , for example , by delay of service detection , such as monitoring for unusual delays in message reception , or dialog sequence error detection , such as monitoring for message block sequence errors . referring to fig2 , a block diagram of the companion sniu installed in a computer host is shown . the companion sniu 44 is implemented as a software function within a host computer 42 . the sniu 42 interfaces with the communications stack of the host computer 58 in order to send and receive messages over the ethernet or token ring cable 74 . the communications stack 58 is a typical osi model including a physical 72 , data link layer 70 , network layer 68 , transport layer 66 , session layer 64 , presentation layer 62 and application layer 60 . the network layer 68 includes an arp / rarp module which is utilized to process address resolution protocol ( arp ) and reverse address resolution protocol ( rarp ). as can be seen from fig2 , the sniu 44 is installed such that it is transparent to other high order software . the main modules of the sniu include a host / network interface 46 , session manager 48 , audit manager 52 , association manager 54 and fortezza api 56 . the primary data structures included in the sniu are the association table , sym_key table , certificate table , waiting queue and schedule table . these data structures are described later in the description of the protocol . the host / network interface 46 provides the interfacing between the sniu 44 and communications stack 58 . the fortezza api 56 is a driver for the card reader 8 included in the host computer 42 . the card reader 8 is adapted to receive a fortezza card which is a pcmcia card configured to perform integrity and authenticating functions , for example . the fortezza card performs the integrity function by encrypting messages leaving the sniu 44 and decrypting incoming messages . the authentication function is accomplished by the fortezza card generating and reading digital signatures which are unique to each sniu . the fortezza card includes a private key to generate the digital signature and a public key to read the signatures . the other sniu modules will be described in conjunction with data flow diagram of fig3 . referring to fig3 , there is shown a data flow diagram for the software sniu . when the host computer communicates with another computer over a network , the communications protocol stack within the computer processes the data to be transmitted . if a user on the computer is transmitting a file to another computer , the user may select the file to send by interacting with application layers software . the display which the user sees is controlled by presentation layer software . session layer software checks the users permission codes to determine if the user has access to the file . transport layer software prepares internet protocol datagrams containing blocks of file data and determines that the transmitted file data is properly received and acknowledged or is re - transmitted . the host / network interface 46 is utilized to intercept the data packets transmitted between the network and data link layers 68 , 70 . the interface 46 is utilized to format the data packets into an appropriate format depending on whether the data packet is incoming or out going . the interface 46 accomplishes this by removing the hardware address header when it receives a data packet and re - applies the same header when the packet is released ( even if the underlying ip address header was changed ). since the interface in the software sniu 46 does not handle arp and rarp message for the host computer , it can be smaller than the one utilized in the hardware sniu . the arp / rarp module included in the network layer 68 performs this function . when the untrusted host / network interface 46 completes re - assembling an ip datagram from a host computer , the datagram is passed to the trusted computing base ( tcb ) of the sniu for processing . the tcb is the collection of hardware and software which can be trusted to enforce the security policy . in the sniu guard the trusted scheduler software module controls the hardware which controls access to memory and guarantees that ip datagrams are not passed directly from the host - side host / network interface module to the network - side host / network interface module or vice versa . rather each ip datagram is passed to the snius other trusted software modules ( message parser , association manager , session manager , etc .) which determine if the ip datagram is allowed to pass through the sniu and if it is encrypted / decrypted . in a sniu companion the hardware is controlled by the host &# 39 ; s operating system software and not the sniu &# 39 ; s scheduler module . therefore , the sniu companion is inherently not as trust worthy as the sniu guard even though most of the software is identical . the message parser 50 b is the first module in the tcb which processes an ip datagram received from the host computer . the message parser 50 b checks the association table 76 and determines whether or not an association already exists for sending the datagram to its destination . if no association exists , the datagram is stored on the waiting queue and the association manager 54 is called to establish an association between this sniu and the sniu closest to the destination host . if an association does exist , the session manager 48 is called to encrypt the datagram , check security rules , and send the encrypted protected user datagram ( pod ) to the peer sniu . when the association manager 54 is called , it prepares two messages to initiate the association establishment process . the first message is an association request message which contains the originating host computer level and this sniu &# 39 ; s certificate ( containing it &# 39 ; s public signature key ). this message is passed to the fortezza api 56 which controls . the fortezza card which signs the message with this sniu &# 39 ; s private signature key . the second message is a message intended to evoke a response from the destination computer , (“ ping ”), such as an icmp echo request message which will be returned to this sniu if it is received by the destination host . both messages are passed to the network - side host / network interface module 46 to be transmitted to the destination host . if another sniu exists on the network between the originating sniu and the destination host , the messages are first processed by the sniu &# 39 ; s receiving port &# 39 ; s host / network interface 46 which reassembles the messages and passes them to the trusted software . the message parser module 50 b passes the association request message to the association manager 54 module and deletes the ping . the association manager 54 passes the message to the fortezza api 56 which verifies the digital signature . if not valid , the audit manager 52 is called to generate an audit event message to log the error . if the signature is valid , the association manager 54 saves a copy of the received association request message in the waiting queue , adds this sniu &# 39 ; s certificate to the message , calls the fortezza api 56 to sign the message , generates a new ping , and passes both messages to the host / network interface module 46 to transmit the messages to the destination host . if the messages are received by any other sniu &# 39 ; s before reaching the destination host , this process is repeated by each sniu . if the destination host computer does not contain the companion sniu software , the host &# 39 ; s communications protocol stack software automatically responds to the message intended to evoke a response from it , for example it converts the ping message to a reply message ( icmp echo reply ) and returns it to the sniu which sent it . however , the destination host does not contain any software which can process the association request message ; so it is ignored ( i . e ., deleted ). if the destination host computer does contain companion sniu software , the host &# 39 ; s data link layer software converts the stream of bits from the physical layer into packets which are passed to the companion &# 39 ; s host / network interface module 46 . the hardware address headers are stripped off of the packets and saved ; and the packets are re - assemble into ip datagrams which are passed to the message parser 50 b . the ping message is ignored ; and the association request message is passed to the fortezza api 56 to have the signature verified . if valid , the message is passed to the association manager module 54 which saves the originating host and sniu data and generates an association grant message . this message contains the sniu &# 39 ; s ip address ( which is the same as the destination host &# 39 ; s ), the sniu &# 39 ; s certificate , the host &# 39 ; s security level , and sealer keys for the originating sniu and the previous intermediate sniu ( if there was one ). the sealer keys ( a . k . a . message encryption keys ) are explained elsewhere . the fortezza api 56 is then called to sign the message which is passed to the host / network interface module 46 . the association grant message is converted from an ip datagram to network packets and passed back to the host &# 39 ; s hardware packet drivers ( in the data link layer ) for transmission back to the originating host . any intermediate sniu &# 39 ; s which receive the association grant message process the message up through the communications stack protocol layers and which calls the message parser 50 b to process the message . the signature on the message is verified by the fortezza api 56 and audited via the audit manager 52 if not valid . otherwise , the validated message is processed by the association manager 54 module which removes and saves one of the sealer keys ( a . k . a . a release key ) which will be used by this sniu and the previous sniu ( which generated the key ) to authenticate pud messages exchanged via this association in the future . the fortezza api 56 is called to generate and wrap another sealer key to be shared with the next sniu in the association path . the new key and this sniu &# 39 ; s certificate are appended to the message . the fortezza api 56 aligns the message . the host / network interface 46 transmits the message on its way back to the originating sniu . the originating sniu re - assembles the association grant message via the physical , data link 70 , and network layers 68 as previously described . the signature is validated and audited if necessary . if valid , the association manager 56 uses the fortezza api to unwrap the sealer key ( s ). if two keys are in the received message , the bottom key is a release key to be shared with the first intermediate sniu ; and the top key is an association key to be shared with the peer sniu ( which granted the association ). if there is only one key , it is the association key which is shared with the peer sniu ; and the association path does not contain any intermediate snius . once the keys are stored and the association table 76 is updated , the association is established and the session manager 48 is called to transmit the original user datagram which was stored in the waiting queue prior to issuing the association request message . the session manager 48 enforces the security policy , determines whether ip datagrams received from host computers can be transmitted via the network to their destination host , encapsulates these user datagrams in puds using the sealer keys for the appropriate association . the security policy is enforced by comparing the security levels of the host and destination . if the security level of the destination is at least as great as that of the host computer , the session manager checks the association table and identified the appropriate peer sniu and sealer key ( s ). the user datagram is encrypted by the fortezza api 56 using the association key . if the association contains any intermediate snius , the fortezza api 56 calculates a message authorization code using the release key . the session manager 48 creates a pud addressed from this sniu to the peer sniu , encloses the encrypted user datagram , appends the message authorization code ( if any ), and passes the new datagram to the host / network interface module 46 on the network - side of the sniu . the datagram is broken into packets and transmitted as previously described . if an intermediate sniu receives the pud , the data is passed through the data link layer software 70 to the network layer where the re - assembled datagram is passed to the session manager 48 . the source ip address is to identify the release key which is shared with the previous sniu . the fortezza api 56 uses the release key to verify the message authorization code . if not valid , the session manager 48 deletes the datagram and calls the audit manager 52 to generate an audit event message . if the code is valid , it removes the code from the datagram , and uses the destination ip address to identify the release key shared with the next sniu . the fortezza api 56 generates a new message authorization code . the session manager 48 appends the new code and passes the datagram to the opposite port &# 39 ; s host network interface module . when the peer sniu ( i . e ., the destination ip address ) received the pud and it has been reassembled into a datagram , the message parser 50 b passes the datagram to the session manager 48 . the source ip address is used to identify the corresponding association key . the fortezza api 56 decrypts the original user datagram . the session manager checks the message authorization code and the security levels of the source and destination hosts . if the code is valid ( i . e ., the message was not modified during transmission over the network ) and the security levels match , the decrypted datagram is passed to the host / network interface 46 to be released to the destination host . if either is not correct , the audit manager 52 is called . to establish trust between pairs of snius , within an internet protocol ( ip ) based network , the present sniu uses associations . an association is a sharing of trusted information developed within the sniu on an as needed basis . the sniu discovers the trusted information it needs , when it needs it . there is no need for pre - positioned network configuration data . the sniu uses custom messages and existing protocols to determine the existence of other snius and hosts , and maintains that information , each called an association , as long as it is needed and unchanged . the snius establish an association which provides a trusted communications path for a period of variable duration between the snius . while an association is open , the two snius use the association &# 39 ; s security parameters to make security decisions for each internet protocol ( ip ) packet of information exchanged . when a host behind a sniu attempts to communicate with someone else over the network , the sniu transmits an association request message and a message intended to evoke a response from a destination which is not a sniu according to the present invention (“ ping ” message ), to the destination . the association request message is used to identify other snius in the communications path . each sniu which receives the association request message authenticates the message , sends it and a new ping on to the destination . the sniu which receives the reply message to the ping is the terminating sniu ( i . e ., closest to the destination ) in the potential association &# 39 ; s communications path . this sniu determines if the association should be permitted , i . e ., would not violate the global or local security policy . the terminating sniu creates an association grant message , inserts its security parameters , and sends it back to the originating sniu . when the originating sniu receives the association grant message , it authenticates the message . address resolution protocol ( arp ) allows a host to find the hardware address of another host on the same network , given its ip address . the host broadcasts an arp . request message which contains its hardware and ip addresses and the ip address of the target host . the target host ( or an intermediate gateway ) returns to the requesting host an arp response message which contains the hardware address of the target host ( or the gateway ). reverse address resolution protocol ( rarp ) allows a host which only knows its hardware address to obtain an ip address from the network . the host broadcasts a rarp request which contains its hardware address and a server on the network , returns a rarp response containing an ip address assigned to the requester &# 39 ; s hardware address . all arp and rarp messages have the same format and are contained within the frame data area of a single ethernet frame ( they are not ip datagrams ). according to douglas e . corner , the format is as follows : protocol type is set to 0800 hex to indicate ip addresses hlen ( hardware address length ) is set to 06 hex bytes plen ( protocol address length ) is set to 04 hex bytes operation is set to 0001 hex for an arp request message 0002 hex for an arp response message 0003 hex for a rarp request message 0004 hex for a rarp response message sender &# 39 ; s ha contains the sender &# 39 ; s 48 bit ethernet hardware address . sender &# 39 ; s ip contains the sender &# 39 ; s 32 bit ip address target &# 39 ; s ha contains the target &# 39 ; s 48 bit ethernet hardware address target &# 39 ; s ip contains the target &# 39 ; s 32 bit ip address when a host broadcasts a request message , it fills in all of the data and the target &# 39 ; s hardware address field is set to 000000 hex if an arp , or the sender &# 39 ; s and target &# 39 ; s ip address fields are set to 0000 hex if a rarp . when the target machine responds , it fills in the missing address and changes the operation field to indicate a response message . during an arp , the target machine swaps the sender &# 39 ; s and target &# 39 ; s addresses so that the sender &# 39 ; s address fields contains its addresses and the target &# 39 ; s address fields contains the original requesting host &# 39 ; s addresses . during a rarp , the server stores its addresses in the sender &# 39 ; s address fields and returns the response to the original sender &# 39 ; s hardware address . arp request : if an arp request message is received on a sniu &# 39 ; s port a , the untrusted software in port a &# 39 ; s memory segment determines if the sender &# 39 ; s ip address is in port a &# 39 ; s arp cache . if not , it creates a new entry in the arp cache and inserts the sender &# 39 ; s hardware and ip addresses . otherwise , the sender &# 39 ; s hardware address is copied into the entry ( overwriting any previous address ); and packets ( if any ) waiting to be sent to the sender &# 39 ; s ip address are transmitted . if the target &# 39 ; s ip address is in port a &# 39 ; s address list ( i . e ., a list of ip addresses which are reachable from port b ), the untrusted software returns an arp response message swapping the sender &# 39 ; s and target &# 39 ; s addresses and inserting port a &# 39 ; s ethernet hardware address into the sender &# 39 ; s ha field . in either case , the untrusted software passes the arp request to the trusted computing base ( tcb ). the tcb checks port b &# 39 ; s address list for the sender &# 39 ; s ip . if the sender &# 39 ; s ip is not in port b &# 39 ; s address list , the tcb determines whether the sender &# 39 ; s ip is releasable to port b ; and if releasable , inserts it into port b &# 39 ; s address list . secondly , the tcb determines whether a proxy arp request should be broadcast from port b . if an arp response message was not returned by port a , and the target &# 39 ; s ip address is not in port a &# 39 ; s arp cache , and the sender &# 39 ; s ip is releasable to port b . the tcb creates a proxy arp request message the tcb inserts port b &# 39 ; s hardware and ip addresses in the sender &# 39 ; s address fields , copies the target &# 39 ; s ip address from the original arp request into the target &# 39 ; s ip field , and signals port b &# 39 ; s untrusted software to broadcast the message . each time the tcb releases a proxy arp request , it creates an anticipated message in the form of a proxy arp response message which contains the original sender &# 39 ; s addresses in the target &# 39 ; s fields , the target &# 39 ; s ip address in the sender &# 39 ; s ip field , and port a &# 39 ; s hardware address in the sender &# 39 ; s ha field . this message is saved in the anticipated message list for port a and will be released to port a &# 39 ; s untrusted software for transmission if the anticipated arp response message is received on port b . note that releasability may involve the tcb modulating arp requests from a high network to a low network in order to not exceed the 100 bits per second covert channel bandwidth requirement . arp response : if an arp response message is received on a sniu &# 39 ; s port a , the untrusted software in port a &# 39 ; s memory segment determines if the sender &# 39 ; s ip address is in port a &# 39 ; s arp cache . if not , it creates a new entry in the arp cache and inserts the sender &# 39 ; s hardware and ip addresses . otherwise , the sender &# 39 ; s hardware address is copied into the entry ( overwriting any previous address ); and packets ( if any ) waiting to be sent to the sender &# 39 ; s ip address are transmitted . finally , the untrusted software passes the arp response to the tcb . the tcb checks port b &# 39 ; s address list for the sender &# 39 ; s ip . if the sender &# 39 ; s ip is not in port b &# 39 ; s address list , the tcb determines whether the sender &# 39 ; s ip is releasable to port b ; and if releasable , inserts it into port b &# 39 ; s address list . secondly , the tcb checks the anticipated message list for port ( b and determines whether the arp response was due to a proxy arp request made for a request originally received on port b . if the sender &# 39 ; s ip matches an entry in the anticipated message list and the message is releasable to port b . the tcb signals port b &# 39 ; s untrusted software to create a proxy arp response message identical to the anticipated message , and removes the message from the anticipated message list for port b . rarp request : if a rarp request message is received on a sniu &# 39 ; s port a , the untrusted software in port a &# 39 ; s memory segment checks a flag to determine if the sniu was initialized to act as a rarp server for the network attached to port a . if not , the received message is ignored . otherwise , the untrusted software passes the rarp request to the tcb . the tcb determines whether the rarp request can be released to port b . if releasable , it creates a proxy rarp request message copying the target &# 39 ; s ha from the received message and inserting port b &# 39 ; s addresses in the sender &# 39 ; s ha and ip fields , passes the proxy rarp request message to port b &# 39 ; s untrusted software for broadcast , and creates an anticipated message in the form of a proxy rarp response message . the tcb copies the original target &# 39 ; s ha , inserts port a &# 39 ; s hardware address in the sender &# 39 ; s ha , and saves it in the anticipated message list for port a . rarp response : if a rarp response message is received on a sniu &# 39 ; s port a , the untrusted software in port a &# 39 ; s memory segment determines if the sender &# 39 ; s ip address is in port a &# 39 ; s arp cache . if not , it creates a new entry in the arp cache and inserts the sender &# 39 ; s hardware and ip addresses . otherwise , the sender &# 39 ; s hardware address is copied into the entry ( overwriting any previous address ); and packets ( if any ) waiting to be sent to the sender &# 39 ; s ip address are transmitted . finally , the untrusted software inserts the targets ip into port a &# 39 ; s address list and passes the rarp response to the tcb . the tcb checks port b &# 39 ; s address list for the sender &# 39 ; s ip . if the sender &# 39 ; s ip is not in port b &# 39 ; s address list , the tcb determines whether the sender &# 39 ; s ip is releasable to port b ; and if releasable , inserts it into port b &# 39 ; s address list . secondly , the tcb determines whether the target &# 39 ; s ip is releasable to port b . if releasable , the tcb creates a new entry in port b &# 39 ; s arp cache and inserts the target &# 39 ; s ha and ip . the tcb uses the . targets ha to find the appropriate proxy rarp response message in port b &# 39 ; s anticipated message list and copies the target &# 39 ; s ip and sender &# 39 ; s ip into the anticipated message signals port b &# 39 ; s untrusted software to create a proxy rarp response message identical to the anticipated message and removes the message from the anticipated message list for port b . dragonfly units ( e . g ., snius and companions ) establish associations in order to authenticate each other , exchange security parameters , and establish a trusted session for communication dragonfly uses a combination of custom messages and standard icmp echo request and echo reply messages to identify dragonfly units between source and destination hosts on a network and establish a trusted communications path . once the path and an association between two snius has been established , user datagrams are encapsulated in custom dragonfly messages called protected user datagrams for secure transmission between the two snius . this collection of messages to establish and utilize associations is — referred to as the dragonfly trusted session protocol ( tsp ). when a host behind a sniu attempts to communicate with someone else over the network , the sniu stores the datagram from the host in a waiting queue and transmits an association request message and an icmp echo request to the intended destination . the association request message is used to identify other dragonfly units in the communications path and to carry the originating sniu &# 39 ; s security parameters . the sniu inserts the originating host &# 39 ; s security level , appends its certificate , and signs the message . the icmp echo request message contains a flag which indicates that it came from a sniu . this message is referred to as a dragonfly ping message . each dragonfly unit which receives the association request message authenticates the message , saves a copy of the message , appends its certificate , signs the message , sends it on to the destination , and sends a new dragonfly ping message to the destination . when a sniu receives a dragonfly ping message from another sniu , the message is discarded and not passed through to the destination . when a destination host receives an association request message , it does not recognize the dragonfly custom protocol ; so it discards the message . however , the destination host does recognize the dragonfly ping message as an icmp echo request message ; so it returns an icmp echo reply message . therefore , a sniu only receives an icmp echo reply if and only if no other sniu exists between the sniu which sent the dragonfly ping message ( an icmp echo request ) and the destination host . the sniu which receives the icmp echo reply message is the terminating sniu ( i . e ., closest to the destination ) in the potential association &# 39 ; s communications path . this sniu determines if the association should be permitted ( i . e ., would not violate the security policy ). if permitted , the sniu grants the association , generates an encryption key for the association , and encrypts the key using the originating sniu &# 39 ; s public key ( from its certificate ). if the saved copy of the association request message contained an intermediate sniu &# 39 ; s certificate , the sniu also generates a release key and encrypts it using the intermediate sniu &# 39 ; s public key . the terminating sniu creates an association grant message , stores the encrypted key ( s ), inserts the destination host &# 39 ; s security level , appends its certificate , signs the message , and sends it onto the originating sniu . each intermediate sniu ( if any exist ) which receives the association grant message authenticates the previous sniu &# 39 ; s signature , extracts the release key , generates a new release key for the next sniu , encrypts the key using the public key ( from the certificate in the saved copy of the association request message ) of the next sniu , removes the previous intermediate sniu &# 39 ; s certificate and signature , appends its own certificate and signature , and sends the message on the return path . when the originating sniu receives the association grant message it authenticates the message and extracts the key ( s ). once association is granted , the originating sniu fetches the originating host &# 39 ; s datagram from the waiting queue and prepares to send it to the terminating sniu in the newly established association . the sniu uses the association key to encrypt the datagram for privacy and store it and the encryption residue into a new datagram from the originating sniu to the terminating sniu . if the association contains intermediate snius , the originating sniu uses the release key to calculate a second encryption residue and appends it to the datagram . finally , the sniu transmits the protected user datagram to the peer sniu in the association . when the protected user datagram is received by an intermediate sniu ( if any in the path ), the intermediate sniu fetches the release key corresponding to the previous sniu and uses the release key to validate the datagram . if valid , the sniu removes the release key residue from the datagram and checks to determine whether there are more intermediate snius in the path before reaching the terminating sniu . if another intermediate sniu exists , the release key corresponding to the next intermediate sniu is used to calculate a new release residue which is appended to the datagram . in either case , the datagram is sent on its way out the opposite the opposite port from which it was received . when the terminating sniu receives the protected user datagram , it uses the association key corresponding to the originating sniu to decrypt and validate the datagram . if the source and destination hosts are at the same security level ( i . e ., a write - equal situation ), the decrypted datagram is sent out the opposite port to the destination host . if the source host has a lower security level than the destination ( i . e ., a write - up situation ), the sniu predicts the response from the destination and saves it before sending the decrypted datagram to the destination host . if the source host has a higher security level than the destination ( i . e ., a write - down situation ), the received datagram ( i . e ., a response to a previous datagram from the lower level host ) was predicted by the sniu which sent the protected datagram . therefore , this sniu is assured that the classification of the received datagram is dominated by the lower level destination host ; so the datagram is released to the destination . if a sniu receives a user datagram from a native host which would be a write - down to the destination host and no predicted datagram is found , the received datagram is erased and the attempted write down is audited . there are three tables which are used to process in - coming and out - going messages ; the association table , the symmetric key table ( sym_key ), and the certificate table . each sniu has two association tables one for each port each entry contains data corresponding to a particular source or destination address . the sym_key table contains data corresponding to a particular message encryption key ( mek ) which could be used as a release key or an association key . the certificate table contains recently received certificates from other snius . each table consists of a linked list of tokens in which the data for an entry in the table is stored in a token . the tokens for each table have a unique data structure and are linked together in ‘ free ’ lists during initialization . when a new entry is made in one of the tables , a token is removed from the free list for that table &# 39 ; s tokens , the data for the new entry is inserted in the appropriate fields of the token , and the token is linked at the top of the table . when an entry is removed from a table , the ‘ previous ’ and ‘ next ’ tokens are linked , the data fields in the token are cleared , and the token is linked at the bottom of the appropriate free list . whenever the data in an entry is used , the token is removed from the table and relinked at the top of the table . in this way , the oldest ( i . e ., least used ) entry is at the bottom of the able . if a new entry is needed and the free list is empty , the bottom token is removed from the table , the data fields are cleared , the new entry &# 39 ; s data is inserted , and the token is linked at the top of the table . in addition , when a sniu removes the bottom ( oldest unused ) token in the sym_key table , it also removes every token in the association table which pointed to the removed key . a sniu does not terminate an association when a certificate , key , or association table entry is removed because many valid entries using the same association could still exist . where : next is a pointer to the next token in the table or list previous is a pointer to the previous token in the table or list ip address is the ip address of the source / destination peer sniu ip address is the address of the other terminating sniu for the association association key pointer points to the association mek in the sym_key table release key pointer points to the release mek in the sym_key table assoc - type is set to 0001 hex for “ pending ” 0002 hex for “ host ” ( i . e ., the entry is for a host destination ) 0003 hex for “ sniu ” ( i . e ., the entry is for a sniu destination ) 0004 hex for “ native host ” ( i . e ., no peer sniu ) 0005 hex for “ audit catcher ” use to validate release key residue ) 0002 hex for “ out ” ( i . e ., use to add release key residue ) 0003 hex for “ both ” security - level indicates the security level — of the source / destination ac - client indicates if the source / destination is an audit catcher client a token for the sym_key table has the following data structure : where : next is a pointer to the next token in the table or list previous is a pointer to the previous token in the table of list distinguished name is the 128 byte name in certificate from the other sniu using this key mek is the 12 byte wrapped key ( association or release ) shared with the another sniu certificate pointer points to the other sniu &# 39 ; s certificate in the certificate table index is a fortezza card key register index which indicates if and where the key is loaded ( 1 - 9 are valid key register indexes , 0 indicates that the key is not loaded on the fortezza ) spare is an unused byte to keep addressing on 32 - bit boundary any message ( ip datagram ) which is generated or modified by a dragonfly unit contains a dragonfly message flag in the last four bytes of the datagram . the first byte is the message type field ; the second byte is the message format field ; and the third and fourth bytes are the dragonfly flag . note that all dragonfly message types are signed except for dragonfly ping and protected user datagram ( pud ) messages . note that a pud uses mek residues for integrity and authentication . message type : 51 . audit event 52 . audit catcher list 53 . audit catcher check - in 54 . audit mask 55 . host unknown 56 . association request 57 . association grant 58 . association denial ( currently not implemented ) 59 . association unknown 60 . protected user datagram 61 . receipt 62 . certificate revocation list 63 . dragonfly ping 64 . sniu initialization 65 . association established 66 . release key unknown message format : 46 . signed type i ( source sniu &# 39 ; s certificate and signature ) 47 . signed type 2 ( source and intermediate sniu &# 39 ; s certificates and signature ) 48 . pud type i ( association mek residue ) pud type 2 ( association mek and release mek residues ) dragonfly flag : dfdf hex the waiting queue is used to store ip datagrams for potential future processing based upon some anticipated vent . for every entry made in the waiting queue , a corresponding entry is made in the schedule table . the schedule table is used to automatically process entries in the waiting queue if they have not been processed within some pre - determined amount of time ( i . e ., the anticipated event does not occur ). the schedule table entry contains a time - out field ( which is set to the current time plus some reasonable delta representing the maximum waiting period ) and a function pointer ( which indicates which subroutine should be called if time expires before the waiting queue entry is processed ). the schedule table is checked in the main executive loop of the tcb ; expired entries are removed ; and the corresponding datagrams in the waiting queue are processed by the designated subroutine . for example , when a sniu receives a user datagram from a native host which is destined for another host for which there is no existing association , the sniu stores the user datagram in the waiting queue and transmits an association request message . when the association grant message is received , the user datagram is removed from the waiting queue , the corresponding schedule table entry is deleted , and the user datagram is encrypted and sent to the peer sniu of the association . if an association grant message is never received , the schedule table entry expires which calls a subroutine to delete the user datagram from the waiting queue . another example is when sniu sends an audit event message to an audit catcher . the transmitted datagram is stored in the waiting queue . when the receipt message is received from the audit catcher , the original audit event datagram is removed from the waiting queue and the corresponding schedule table entry is deleted . if the schedule table entry expires , the designated subroutine is called which re - transmits the audit event message stored in the waiting queue and a new entry is made in the schedule table . message encryption keys ( meks ) are generated during the association establishment process ( previously ) described ) and are exchanged via the association grant message . when a sniu generates an mek it simultaneously generates an initialization vector ( iv ). when a sniu exchanges an mek with another sniu , it generates a random number , ra , which is required to encrypt ( i . e ., wrap ) the mek . the key exchange algorithm is designed so that only the sending and receiving snius can decrypt the mek and use it . the sender wraps the mek for transmission using the destination &# 39 ; s public key , ra , rb ( which is always set = 1 ), and the sender &# 39 ; s private key . ivs which were generated with release keys are transmitted in the clear with the wrapped mek in the association grant message . ivs which were generated with association keys are ignored . the recipient unwraps the key using its private key , ra , rb , and the sending sniu &# 39 ; s public key . once unwrapped , the safe exchange is complete . each sniu re - wraps the mek using its storage key ( ks ), stores the mek and the iv ( if the mek is a release key ) in the sym_key table , stores the pointer to the mek in the association table and stores the distinguished name ( of the other sniu sharing this mek ) in the sym_key key table entry . message encryption keys ( meks ) are used as association and release keys to provide confidentiality , integrity and authentication of user datagrams during an association between two snius . ivs are used to initialize the feedback loop in the skipjack encryption algorithm for most modes of operation . encrypting identical data using the same mek , but different ivs , will produce different ciphertext . in fact , the fortezza card requires the user to generate a new iv for each encryption event in order to assure that each message looks different when encrypted . when a sniu encrypts a user datagram it first generates a new iv for the association key , encrypts the datagram , appends the encryption residue for integrity and authentication purposes , and appends the new iv . if the association involves intermediate snius , the sniu does a second encryption operation ( on the new ciphertext , residue , and iv ) using the release key and release key iv . the release key iv is never changed since the encrypted data is always guaranteed to be unique even if the original datagram was not . the release key residue is appended to the protected user datagram . the completed protected user datagram is transmitted . when a sniu receives an ip datagram it checks the destination address in the header and determines if it is the intended recipient . then , it checks the last four bytes of the ip datagram for the dragonfly message flag and determines the type and format of the received message . when a sniu receives an ip datagram which is addressed to it , the message should be one of the following types of dragonfly formatted messages . if it is not , the sniu will audit the event . the only exceptions are icmp echo request messages which are processed by the receiving port &# 39 ; s untrusted software and not passed to the trusted computing base . 51 . audit event : if the sniu is not configured to be an audit catcher , it will audit the event sending the source ip address of the , received message to its primary audit catcher . if the sniu is configured to be an audit catcher , it verifies the signature on the message , increments its received audit event sequence number , generates a time - stamp , and prints the sequence number , time - stamp , source ip address , and ascii character string from the message . once the event has been recorded , the audit catcher sniu generates a receipt message ( copies the audit event counter from the received message and inserts it in the message number field ) and sends it . 52 . audit catcher list : the sniu verifies the signature on the message , stores the new list of audit catchers in the configuration table , generates a sniu initialization message , generates a receipt message , and updates the audit catcher check - in message stored in the waiting queue . 53 . audit catcher check - in : if the sniu is not configured to be an audit catcher , it will audit the event sending the source ip address of the received message to its primary audit catcher . if the sniu is configured to be an audit catcher , it verifies the signature on the message , generates a time - stamp , prints the time - stamp and source ip address , and compares the audit mask in the received message with the current mask . if they do not match , the current audit mask is sent to the sniu which just checked - in . note that the period between check - ins is a parameter in each sniu &# 39 ; s configuration data . the audit catcher does not return a receipt message in any case . 54 . audit mask : the sniu verifies the signature on the message , stores the new audit mask in the configuration table and the audit catcher check - in message stored in the waiting queue , generates a receipt message , and audits the event ( in case someone else other than the audit catcher is distributing new audit masks ). 55 . host unknown : when a sniu receives a valid protected user datagram , but cannot find the destination &# 39 ; s association table entry , it sends a host unknown message back to the originating sniu and audits the event . the originating sniu verifies the signature on the received host unknown message , extracts the original destination host &# 39 ; s ip , removes the host &# 39 ; s entry from its association table and audits the event it does not remove the peer sniu &# 39 ; s entry nor entries from the sym key key table as they might be supporting other associations . 56 . association request : this message should only be sent to native hosts and intercepted by snius ; but a sniu should never be the destination . 57 . association grant : the sniu verifies the signature in the datagram and updates the receiving port &# 39 ; s association table entries for the peer sniu and host destination . the sniu determines if an entry exists for the peer sniu . if not the sniu creates a new entry for the peer sniu and marks the association type as ‘ sniu ’. in either case , the sniu extracts and unwraps the association mek ( and release mek if needed ), stores the re - wrapped key ( s ) in the sym_key table ( being careful to over - write the old keys without changing the pointers to the keys if some already existed ), and marks the release key type as ‘ out ’ ( if a release key exists ). if the received message indicates that existing release keys are to be used , the sniu searches the association table for ‘ sniu ’ type entries and checks the dn of each sym_key key table entry identified via the release key pointer . the sniu compares that dn with the dn in the bottom certificate in the received message . if a match is found , the release key pointer is copied to the association table entry for the peer sniu of this new association . if no match can be found , the sniu generates a release key unknown message . this message is generated by modifying the received association grant message . the destination address ( its ip ) is swapped with the peer sniu &# 39 ; s address ( i . e ., the association granting sniu &# 39 ; s ip in the data section of the datagram . the previous sniu &# 39 ; s certificate is replaced with this sniu &# 39 ; s certificate so the previous sniu can wrap the new release key and return to this sniu in the association grant message . the signature at the bottom is removed . the message number is changed from 58 to 66 . the new message is signed and sent back to the previous sniu in the path . finally , the association type field of the peer sniu &# 39 ; s entry in the association table is changed back to ‘ pending ’. if a release key unknown message is transmitted , the sniu waits for the new release key in another association grant message before continuing . if the peer sniu &# 39 ; s association table entry is complete , the sniu finds the entry for the destination host , changes the association type from ‘ pending ’ to ‘ host ’, inserts the peer sniu &# 39 ; s ip copies the association and release key pointers and release key type from the peer sniu &# 39 ; s entry , and copies the destination host = s security level from the received message . once the receiving port &# 39 ; s association table has been updated , the sniu finds the original host &# 39 ; s user datagram in the waiting queue , removes the corresponding entry from the schedule table , and compares the source and destination security levels to determine it the user datagram can be sent to the destination . if the source &# 39 ; s security level is dominated by ( i . e ., less than or equal to ) the destination &# 39 ; s security level , the sniu creates a protected user datagram ( pud ). the sniu sets the destination to the peer sniu &# 39 ; s ip , sets the protocol type to indicate a dragonfly message , uses the association key to encrypt the entire received datagram and prefixed source host &# 39 ; s security level , inserts the ciphertext and iv , appends the association residue , generates and inserts a release residue ( if the destination host &# 39 ; s association table entry contains a pointer to a release key ), appends the appropriate dragonfly message flag , and sends the datagram . if the source host is not dominated by the destination ( i . e ., a potential write - down ), the attempted write - down is audited . this procedure is repeated for each entry in the waiting queue which is intended for the same destination . 59 . association unknown : a sniu sends an association unknown message ( and generates audit notices ) when a protected user datagram or association exists message is received and a corresponding association table entry does not exist . the message is sent back to the source sniu and contains the destination sniu &# 39 ; s ip address . when a sniu receives an association unknown message , it deletes every entry in the association table in which the peer sniu &# 39 ; s ip matches the returned destination sniu ip . subsequent user datagrams from the same host sent to the same destination will initiate an association request to re - establish the association . 60 . protected user datagram ( pud ): the sniu uses the source ip to find the peer sniu &# 39 ; s entry in the receiving port &# 39 ; s association table and retrieve the association key to decrypt and validate the received datagram . if the decryption residue does not match , the event is audited . otherwise , the sniu uses the destination host &# 39 ; s ip to find the appropriate entry in the opposite port &# 39 ; s association table , retrieves the destination host &# 39 ; s security level , and compares it to the security level in the received datagram . if a write - up situation , the sniu generates an anticipated message . however , regardless of the relative security levels , the decrypted and validated user datagram is sent to the destination host . if the decrypted and validated datagram is a broadcast message , the sniu compares the security level of the received datagram and the security level of the opposite port . if the security level of the opposite port dominates that of the datagram , the sniu releases the datagram out the opposite port . if a terminating sniu receives a pud and cannot find the peer sniu &# 39 ; s entry in the association table , the sniu returns an association unknown message ( containing this sniu &# 39 ; s ip ) and audits the event . if the receiving sniu validates the residue but cannot deliver the user datagram because it cannot fund the destination host in the association table , then the sniu returns a host unknown message ( containing the destination host &# 39 ; s ip ) to the originating sniu and audits the event . 61 . receipt : a receipt message is sent by an audit catcher to a sniu for a sniu initialization or an audit event message . the sniu uses the message number in the received datagram to locate the saved copy of the original message in the waiting queue and remove it and the corresponding schedule table entry . if the original message was a sniu initialization message , the sniu locates the association table entry for the audit catcher and changes the association type from ‘ pending ’ to ‘ audit catcher ’. if time expires in the schedule table entry before the receipt message is received the sniu will retransmit the original message . if no receipt is received after tbd attempts , the sniu will switch to the next audit catcher in its list . if all audit catchers are attempted without success , the sniu will check a configuration parameter to determine whether to continue without audit or halt . snius issue receipt messages to the source for audit catcher list , audit mask , and certificate revocation list messages . when the source receives a receipt , it uses the returned message number to remove the copy of the message from the waiting queue and the corresponding schedule table entry . refer to the section above . “ waiting queue and schedule table ”, for more details . 62 . certificate revocation list : if a certificate revocation list ( crl ) is received the sniu returns a receipt to the source and checks the sym_key table far any keys which were received from ( or sent to ) another sniu with a revoked certificate . for each entry which contains the distinguished name ( dn ) of a revoked certificate the sniu deletes the certificate from the certificate table ( if it is still there ), deletes the sym_key key table entry , and deletes every entry in the association table which pointed to the key . note that deleting a table entry means to unlink the token from the table , clear the token &# 39 ; s memory , and re - link the token in the token &# 39 ; s free list . 63 . dragonfly ping : this message can only be received by a sniu which is the terminating sniu in an association ( i . e ., the closest sniu to the destination host ). this sniu originally transmitted a dragonfly ping message ( in the form of an icmp echo request ) along with an association request message to some unknown destination which converted the echo request to an echo reply , returned it , and ignored the association request message ( which could only be processed by another sniu ). upon receiving this message the sniu checks the originating sniu ip in the data section of the received message to determine if it is the only sniu in the association ( i . e ., the only sniu between the originating host and the destination host ). if it was the originator , the sniu uses the source ip address to find the destination &# 39 ; s entry in the association table , changes the association type from ‘ pending ’ to ‘ native host ’, sets the security level to that port &# 39 ; s security level , finds the original host &# 39 ; s user datagram in the waiting queue , removes the corresponding entry from the schedule table , and compares the source and destination security levels to determine if the user datagram can be sent to the destination . if the comparison indicates a write - up situation , the sniu generates and saves an anticipated message and releases the original datagram to the destination port . if a write - down situation , the sniu deletes the datagram and audits the attempted write - down . if a write - equal , the datagram is released to the destination port . this procedure is repeated for each entry in the waiting queue which is intended for the same destination . if this sniu was not also the originating sniu , the originating sniu &# 39 ; s and originating host &# 39 ; s ip addresses in the data section of the received echo reply are used to identify the peer sniu &# 39 ; s entry in the association table and fetch the association request message which was saved in the waiting queue ( and delete the corresponding entry from the schedule table ). then the sniu creates or updates three association table entries . first , it creates an entry ( if it doesn &# 39 ; t already exist ) in the receiving port &# 39 ; s association table for the original destination host ( using the source ip from the received datagram header ), marks the association type as ‘ native host ’ and stores the receiving port &# 39 ; s security level in the security level field . second , it updates the entry in the opposite port &# 39 ; s association table for the peer sniu . if the peer sniu &# 39 ; s entry is already complete ( i . e ., the association type field is marked as ‘ sniu ’), the sniu verifies that the dn in the sym_key table entry for the association key is still valid and returns an association exists message ( containing the original destination host &# 39 ; s ip and security level ) instead of an association grant message to the peer sniu . if the dn or the certificate has changed , the sniu deletes all entries in the association table which refer to this entry as the peer sniu and then continues as if this was the first association with this peer sniu and over - writes the old data . if the peer sniu entry in the association table is incomplete ( i . e ., the association type field is marked as ‘ pending ’), the sniu continues to fill in the missing data as follows . if the release key type is marked ‘ out ’ or ‘ both ’, then the association path contains at least one intermediate sniu ; therefore , the sniu must extract the peer sniu &# 39 ; s certificate from the association request message and store it in the certificate table . if a certificate with this dn already exists , but is not identical , then the sniu must locate and delete all other sym_key key table and association table entries referencing this certificate . in either case , the sniu stores the pointer to the certificate the dn in a sym key table entry , and stores the pointer to the sym_key key table entry in the association key pointer field of the association table entry . if there aren &# 39 ; t any intermediate snius , the pointer in the release key pointer field is copied to the association key pointer field ; and the release key pointer field is cleared . in either case , the association type is changed from ‘ pending ’ to ‘ sniu ’. the sniu generates the association key and stores the key in the sym_key key table entry . if a release key is needed for an intermediate sniu , the sniu must determine if a release key associated with the intermediate sniu &# 39 ; s certificate &# 39 ; s dn already exists . the sniu uses the release key pointer in each entry with association type ‘ sniu ’ in the association table to locate the sym_key key table entry of every release key . if a match is found the pointer to that sym_key key table entry is copied . otherwise , a new release key is generated and stored . the third association table entry is for the originating host . it &# 39 ; s ip and security level are in the data portion of the association request message . the security level is copied to the entry , the association type is marked as ‘ host ’, and the rest of the data is copied from the peer sniu entry . once the association table entries are updated , an association grant message is generated . the sniu stores the source address from the association request message ( i . e ., the association originating sniu &# 39 ; s ip ) in the destination address and stores the destination host &# 39 ; s ip in the source address ( a little ip spoofing ). the sniu fills in the data section by storing its ip , the destination host &# 39 ; s security level , the association key data ( wrapped key and ra ), and if necessary , the release key data ( the wrapped key , ra and iv ). if a release key for the first intermediate sniu on the return path existed previously to establishing this association , the sniu sets a flag ( instead of storing the release key in the message ) to instruct the intermediate sniu to use the existing release key . the dragonfly message flag is inserted at the bottom marking the type as association grant and the format as signed type i to indicate only one certificate . the message is signed and sent ; and the event is audited . 64 . sniu initialization : this message is sent by a sniu to it &# 39 ; s primary audit catcher during the sniu &# 39 ; s initialization to determine whether the audit catcher is ready to support the sniu . depending upon a configuration parameter , the sniu may not allow any other message processing until a receipt message is received from the audit catcher . upon receiving this message , the audit catcher verifies the signature on the message , makes an entry in its receiving port &# 39 ; s association table using the source ip , marks the association type as ‘ sniu ’, returns a receipt message , and compares the audit mask in the received message with the current mask . if they do not match , the current audit mask is sent to the sniu in an audit mask message . 65 . association exists : if a sniu receives an association request message , determines that it is the terminating sniu , and that it already has an existing association with the requesting sniu ; the terminating sniu will return an association exists — message , instead of an association grant message . when a sniu receives an association exists message , it verifies the signature on the message and checks the receiving port b association table for an entry for the source sniu . if the source ( i . e ., peer ) sniu entry exists , this sniu uses the destination host &# 39 ; s ip address in the message to update ( or create , if necessary ) the destination host &# 39 ; s association table entry . it changes the association type from ‘ pending ’ to ‘ host ’, copies the mek pointers from the peer &# 39 ; s sniu entry , and copies the security level from the received message . once the association table has been updated , the sniu locates the user datagram ( which was stored in the waiting queue until the association was established ) and processes the datagram for transmittal the same as if a normal association grant message had been received ( see description above ). if an entry cannot be found in the association table for the source sniu , then this sniu will return an association unknown message to the source sniu . the message will contain this sniu &# 39 ; s ip address to indicate which association needs to be deleted . then the sniu will locate the original host &# 39 ; s datagram saved to the waiting queue , reset its time - out value in the schedule table , and schedule a new event ( after some tbd seconds delay ) to regenerate a new association request message . 66 . release key unknown : a sniu may receive an association grant message with a flag set to indicate that an existing release key should be used . however , if the sniu cannot locate the release key , it sends a release unknown key message back to the previous sniu requesting it to generate a new release key . this message is generated by modifying the received association grant message . the destination address ( the association originating sniu &# 39 ; s ip ) is swapped with the terminating sniu &# 39 ; s address ( i . e ., the association granting sniu &# 39 ; s ip ) in the data section of the datagram . the previous sniu &# 39 ; s certificate is replaced with this sniu &# 39 ; s certificate so the previous sniu can wrap the new release key and return it to this sniu in the association grant message . the signature at the bottom is removed . the message number is changed from 58 to 66 , and the new message is signed and sent back to the previous sniu in the path . note that this message is addressed to the terminating sniu which generated the original association grant message . however , this message is intended for the previous sniu in the new a association &# 39 ; s path . therefore , if the first sniu to receive this message is an intermediate sniu , it should process the message and not send it on to the terminating sniu . if a sniu receives a release key unknown message and it is the destination , the sniu must be the terminating sniu which granted the association . the sniu verifies the signature on the message , swaps the destination address ( its ip ) with the peer sniu address ( the association originating sniu &# 39 ; s ip ) in the data section , uses the new destination address to locate the peer sniu &# 39 ; s entry in the receiving port &# 39 ; s association table , removes the certificate from the message , and compares the dn in the certificate ’ with the dn in the sym_key table entry indicated via the peer sniu &# 39 ; s release key pointer . if the dn does not match , the sniu audits the error and over - writes the dn entry with the dn from the certificate . in either case , the sniu stores the certificate in the certificate table ( over - writing the old one if a certificate with the same dn already exists ), generates a new release key , over - writes the old release key in the sym_key key table with the new release key ( ks - wrapped ), wraps the key using the public key from the received certificate , stores the wrapped release key in the message , changes the message number from 66 back to 58 , stores its certificate in the message , signs and sends it . broadcast : various messages ( non - dragonfly ) are broadcast to every device on a network . when a broadcast message is received , the sniu creates a . protected user datagram ( containing the received broadcast message and the security level of the port on which the message was received ) for every peer sniu to the opposite port &# 39 ; s association table and sends them . when a sniu receives an ip datagram which is not addressed to it , the message should be one of the following types of dragonfly formatted messages . if it is not , the sniu will assume the ip datagram is from a native host . audit event : the sniu verifies the signature on the message and releases the message out the opposite port . 52 . audit catcher list : the sniu verifies the signature on the message and releases the message out the opposite port . 53 . audit catcher check - in : the sniu verifies the signature on the message and releases the message out the opposite port . 54 . audit mask : the sniu verifies the signature on the message and releases the message out the opposite port . 55 . host unknown : the sniu verifies the signature on the message and releases the message out the opposite port . 56 . association request : when a sniu receives an association request , it validates the signature at the bottom of the message and checks the receiving port &# 39 ; s association table for an entry with the originating sniu &# 39 ; s ip address . if it cannot find an entry , it creates one , marks the association type as ‘ pending ’, stores the previous sniu ’ certificate in the certificate table , updates the sym_key table entry for the distinguished name ( dn ), stores the pointer to the sym_key table entry in the release key pointer field in the association table entry , and store a copy of the received message in the waiting queue ( and makes a corresponding entry in the schedule table if a certificate with this dn already exists , but is not identical then the sniu must locate and delete all other sym_key table and association table entries referencing this certificate . if the previous sniu was an intermediate sniu ( i . e ., the message format field of the dragonfly message flag is ‘ signed type 2 ’), this sniu marks the release key type field as ‘ out ’ and removes the previous sniu &# 39 ; s certificate and signature . in either case , this sniu appends its certificate and signature and sends the message out other port . it does not make any entry in the out - going port &# 39 ; s association table . finally , the sniu creates and sends a dragonfly ping message ( in the form of an icmp echo request ) to the destination host . the sniu stores the originating sniu and originating host &# 39 ; s ip addresses in the datagram and sets the dragonfly flag , but does not sign the message . 57 . association grant : the sniu validates the signature at the bottom of the received datagram and if not correct deletes the datagram and audits the event . otherwise , since it is not the destination , the sniu is an intermediate sniu somewhere in the path between the two peer snius . the sniu creates an entry ( if one doesn &# 39 ; t already exist ) in the receiving port &# 39 ; s association table for the ip of the terminating sniu which granted the association ( in the data section of the association grant message ), marks the association type as ‘ sniu ’, marks the release key type as ‘ m ’ ( if the format is ‘ signed type 1 ’) or ‘ both ’ ( if the format is ‘ signed type 2 ’), extracts the release key data ( i . e ., the wrapped mek , ra and iv ), unwraps and stores the release key in the sym_key table , stores the release key iv in the same sym_key table entry , stores the pointer to the release key in the association table , stores the certificate in the certificate table , and stores the pointer to the certificate and the dn in the sym_key table entry . if a certificate with this dn already exists , but is not identical , then the sniu must locate and delete all other sym_key table and association table entries referencing this certificate . if the received message contains a flag indicating that an appropriate release key already exists , the sniu uses the release key pointer in every other ‘ sniu ’ type entry in the association table and compares the dns of the certificates associated with the release keys . if a match is found , the pointer to the matching sym_key table entry is copied to the new association table entry . if no match is found , the sniu generates a release key unknown message . this message is generated by modifying the received association grant message . the destination address ( i . e ., the association originating sniu &# 39 ; s ip ) is swapped with the peer sniu &# 39 ; s address ( i . e ., the association granting sniu &# 39 ; s ip ) in the data section of the datagram . the previous sniu &# 39 ; s certificate is replaced with this sniu &# 39 ; s certificate so the previous sniu can wrap the new release key and return it to this sniu in the association grant message . the signature at the bottom is removed . the message number is changed from 58 to 66 . the new message is signed and sent back to the previous sniu in the path . finally , the association type field of the terminating sniu &# 39 ; s entry in the association table is changed back to ‘ pending ’. if a release key unknown message is transmitted , the sniu waits for the new release key in another association grant message before continuing . next , the sniu uses the destination ip address in the header of the received association grant message to find the destination &# 39 ; s entry in the opposite port &# 39 ; s association table . if the association type is ‘ pending ’, the sniu determines whether an existing release should be used or if a new one should be generated . the sniu uses the release key pointer to fetch the saved certificate of the next sniu and compares its dn with the dn associated with the other release keys identified via the release key pointers in other ‘ sniu ’ type entries . if a match is found , the pointer to the release key &# 39 ; s entry in the sym_key table is copied to the new association table entry . if a match is not found , the sniu generates new release key data ( an mek , ra , and iv ) and stores the wrapped mek and iv in the sym_key key table entry . in either case , the sniu changes the association type to ‘ sniu ’. if the release key type is ‘ null ’ the sniu changes it to ‘ in ’; otherwise , it is marked as ‘ both ’. the sniu uses the original destination host &# 39 ; s ip ( the source ip in the header of the association grant message ) and the original sniu &# 39 ; s ip ( i . e ., the destination ip in the header of the association grant message ) to locate the association request message which was saved in the waiting queue and delete it and the corresponding entry in the schedule table . finally , the sniu rebuilds the association grant message to send on to the destination . the sniu copies the received datagram up to and including the association key data and the certificate of the sniu which originated the association grant message , inserts its certificate and the release key data ( or a flag indicating to use an existing release key ), and signs and sends the datagram . 59 . association unknown : the sniu verifies the signature on the message and releases the message out the opposite port . 60 . protected user datagram : the sniu uses the source ip address to find the appropriate entry in the receiving port &# 39 ; s association table , fetches the release key , and verifies the release key residue . if the release residue is not correct the datagram is delete and the event audited . otherwise , the sniu uses the destination ip address to find the appropriate entry in the opposite port &# 39 ; s association table , fetches the release key , generates the new release residue , overwrites the old release residue , and sends the datagram on in to the destination . 61 . receipt : the sniu verifies the signature on the message and releases the message out the opposite port . 62 . certificate revocation list : the sniu verifies the signature on the message and releases the message out the opposite port . 63 . dragonfly ping : the sniu ignores ( i . e ., deletes ) the icmp echo request and does nothing else . it should also receive an association request message which it will process ( see description above ). note that if the datagram is a standard icmp echo request ( i . e ., no dragonfly flag ), it is treated as any other native host message ( see description below ). 64 . sniu initialization : the sniu verifies the signature on the message and releases the message out the opposite port . 65 . association exists : when an intermediate sniu receives this message , it verifies the signature on the message and verifies that it has entries for both the source and destination ip addresses ( i . e ., the two peer snius of the association ) in the appropriate ports &# 39 ; association tables . if everything is verified , the message is released out the opposite port . if either peer . sniu &# 39 ; s entry cannot be found in the association table , then this sniu will return an association unknown message to the source sniu . the message will contain the destination sniu &# 39 ; s ip address to indicate which association needs to be deleted . in any case , the sniu uses the association originating sniu &# 39 ; s and the host destination &# 39 ; s addresses in the association exists message to locate and delete the association request message which was saved in the waiting queue ( and the appropriate schedule table entry ). 66 . release key unknown : a sniu may receive an association grant message with a flag set to indicate that an existing release key should be used . however , if the sniu cannot locate the release key , it sends a release key unknown message back to the previous sniu requesting it to generate a new release key . this message is generated by modifying the received association grant message . the destination address ( the association originating sniu &# 39 ; s ip ) is swapped with the terminating sniu &# 39 ; s address ( i . e ., the association granting sniu &# 39 ; s ip ) in the data section of the datagram . the previous sniu &# 39 ; s certificate is replaced with this sniu &# 39 ; s certificate so the previous sniu can wrap the new release key and return it to this sniu in the association grant message . the signature at the bottom is removed . the message is changed from 58 to 66 , and the new message is signed and sent back to the previous sniu in the path . note that this message is addressed to the terminating sniu which generated the original association grant message . however , this message is intended for the previous sniu in the new association &# 39 ; s path . therefore , if the first sniu to receive the message is an intermediate sniu , it should process the message and not send it on to the terminating sniu . if a sniu receives a release key unknown message and it is not the destination , the sniu must be an intermediate sniu somewhere in the middle of the association &# 39 ; s path . the sniu verifies the signature on the message , swaps the destination address ( the association granting sniu &# 39 ; s ip ) with the per sniu address ( the association originating sniu &# 39 ; s ip ) in the data section , uses the new destination address to locate the peer sniu &# 39 ; s entry in the receiving port &# 39 ; s association table , removes the bottom certificate from the message , and compares the dn in the certificate with the dn in the sym_key key table entry indicated via the peer sniu &# 39 ; s release key pointer . if the dn does not match , the sniu audits the error and over - writes the dn entry with the dn from the certificate . in either case , the sniu stores the certificate in the certificate table ( over - writing the old one if a certificate with the same dn already exists ), generates a new release key , over - writes the old release key in the sym_key key table with the new release key ( ks wrapped ), wraps the key using the public key from the received certificate , stores the wrapped release key in the message , changes the message number from 66 back to 58 , stores its certificate in the m . message , signs and sends it . native host message : when a sniu receives a user datagram from a native host , the sniu creates an entry ( if one doesn &# 39 ; t already exist ) in the receiving port &# 39 ; s association table for the source host &# 39 ; s ip , marks the association type as ‘ native host ’, sets he security level to the receiving port &# 39 ; s security level , and checks the opposite port &# 39 ; s association table for the destination &# 39 ; s ip address . if an entry does not already exist for the destination the sniu creates a new entry , marks the association type as ‘ pending ’, stores the received datagram in the waiting queue , makes a corresponding entry in the schedule table , creates an association request message and sends it . next , the sniu creates and sends a dragonfly ping to the destination host . the sniu stores the originating sniu and originating host &# 39 ; s ip addresses in the datagram and sets the dragonfly fly but does not sign the message . if an association table entry exists for the destination and the association type is ‘ pending ’, the sniu stores the e received datagram in the e waiting queue , linking it to other datagrams for the same destination . if an association table entry exists for the destination and the association type is ‘ host ’, the sniu compares the source host &# 39 ; s security level to the destination host &# 39 ; s security level . if the source &# 39 ; s security level is dominated by ( i . e ., less than or equal to ) the destination &# 39 ; s , the sniu creates a protected user datagram ( pud ). the sniu sets the destination to the peer sniu &# 39 ; s ip , sets the protocol type to indicate a dragonfly message , uses the association key to encrypt the entire received datagram , inserts the ciphertext and iv , appends the association residue , generates and inserts a release residue ( if the association table entry contains a pointer to a release key ), appends the appropriate dragonfly message flag , and sends the datagram . if the source host is not dominated by the destination ( i . e ., a potential write - down ), the sniu determines if this datagram was anticipated . if a matching datagram was predicted , the anticipated datagram is transformed into a pud ( as described above ) and sent . if an anticipated message is not found the attempted write - down is audited . if an association table entry exists for the destination and the association type is any other bona fide type ( i . e ., ‘ native host ’, ‘ sniu ’ or ‘ audit catcher ’, the sniu compares the source and destination ports &# 39 ; security levels to determine if the datagram can be allowed to proceed . if the comparison indicates a write - up situation , the sniu generates and saves an anticipated message and releases the original datagram to the destination port . if a write - down situation , the sniu determines if the datagram was predicted and sends the anticipated message or audits as previously described . if a write - equal , the datagram is released to the destination port . the following example is intended to provide a further illustration of a preferred embodiment of a sequence of operations according to the present invention . this sequence of operations is applicable to communications from a first user utilizing a sniu to a second user , also utilizing a sniu , sent over an unsecured network . the first user transmits an original message intended for the second user utilizing said network . a first guard sniu intercepts the original message . the first guard sniu then transmits an association request message intended for another sniu and a ping message intended for the second user . if the second user receives these messages , and is not utilizing a companion sniu , it will ignore the association request message intended for another sniu and respond to the ping message intended for it . when the first sniu receives the ping response from the second user , it will determine that it is the “ closest ” sniu to the second user , and decide whether transmitting the “ original ” message to the second sniu will violate network security parameters . if it will not , then the first sniu will simply forward the “ original ” message to the second user . if transmitting the “ original ” message to the second user will violate security parameters , then the “ original ” message will not be transmitted to the second user , and this event will be audited . when a second sniu receives the association request message intended for another sniu and the ping message intended for the second user which were transmitted by the first sniu , it ignores the ping message intended for the second user , and logs the association request message intended for another sniu . it likewise then transmits another association request message intended for another sniu and another ping message intended for the second user . if another sniu intercepts the second association request message intended for another sniu and the second ping message intended for the second user , it will perform the same before mentioned steps of the second sniu . accordingly , an unlimited number of snius can be interspaced between the first and second snius in the present invention , as each interspaced sniu will log the association request message received , ignore the ping message received , and further transmit another association request message , and another ping message . when the second user receives the association request message intended for another sniu and the retransmitted ping message intended for it , if not utilizing a companion sniu , it will again ignore the association request message intended for another sniu and respond to the ping message intended for it . when a sniu receives the ping response from the second user , it will determine that it is the “ closest ” sniu to the second user . upon this determination it will now respond to the association request message transmitted from the first sniu which it logged , with an association grant message . this association grant message includes necessary information for enforcing the network security policy , such as mandatory access control information ( i . e . the security level of the second user , and encryption key affiliated with the second sniu ). upon receipt of the association grant message transmitted by the second sniu , the first sniu can now determine whether allowing the “ original ” message to be transmitted to the second user will violate any of the network security policies , as the first sniu now has the security data required to make that decision . if the transmission of the “ original ” message will not violate the network security policy , then using the encryption key included in the association grant message , the first sniu will transmit the encrypted “ original ” message to the second sniu . upon receipt thereof , the second sniu will decrypt the encrypted “ original ” message and may again determine whether allowing the “ original ” message to proceed to the second user will violate network security parameters ( i . e . discretionary access control ). if it will not , the second sniu can now transmit the “ original ” message to the second user . when using the term “ closest ,” in this manner , it is to be understood that “ closest ” refers to that sniu which is to be associated or affiliated with the second user . if the first user is utilizing a companion sniu , then that companion can be seen to perform the steps of the first sniu in the above example . if the second user is utilizing a companion sniu , then that companion can be seen to perform the steps of the second sniu . it is to be understood that the embodiments described herein are merely exemplary of the principles of the invention , and that a person skilled in the art may make many variations and modifications without departing from the spirit and scope of the invention . all such variations and modifications are intended to be included within the scope of the invention as defined in the appended claims . | 7 |
referring now to fig1 there is shown a shell 10 of a preferred embodiment of the present invention , upon which is disposed a wheel 12 of an automobile and a cross - link 14 of an anti - skid tire chain 16 . in accordance with the principles of the present invention , the width of shell 10 is less than the length of the cross - links 14 of the size of tire chain which the shell 10 and a substantially similar mating shell ( see fig3 ) are adapted to contain . ( this last statement should not be construed as indicating that a different size of shell is required for every size of tire chain . to the contrary , it is a feature of the present invention that very few , perhaps three , sizes of shell embodying the present invention will accommodate all of the sizes of tire chains commonly fitted to standard highway vehicles in the united states .) as further seen in fig1 shell 10 is provided with a channel 22 adapted to completely contain one of the cross - links 14 of a tire chain when shell 10 is being used to facilitate the mounting of the tire chain . a further feature of the shell 10 of the present invention is the provision of a plurality of transverse ribs 24 , 26 ( fig1 ) which engage the outer face of vehicle tire 12 as the vehicle is being driven onto or off of ramp 10 , thereby tending to prevent slippage between the ramp 10 and the vehicle tire 12 . as best seen in fig1 the upper plane surfaces 28 , 30 of shell 10 are slightly sloped inwardly toward channel 22 , thus tending to maintain the vehicle tire 12 ( and the wheel upon which it is mounted ) in place on ramp 10 , and tending to maintain the vehicle in place on the roadway while the tire chain is being applied with the aid of shell 10 . while the shell 10 of the present invention and its use in mounting a tire chain upon a motor vehicle is being described without reference to its mating shell , which coacts with it to contain a pair of tire chains when those tire chains are not mounted on the vehicle , it is to be understood that the present invention contemplates the simultaneous use of shell 10 and its mating shell in mounting a pair of tire chains on a vehicle , the rear tires , and wheels , of the vehicle being simultaneously driven onto shell 10 and its mating shell . as further seen in fig1 a pair of flanges 32 , 34 are provided at the ends of shell 10 . as best seen in fig3 the mating shell is also provided with a pair of such flanges . flange 34 is provided with a hole 36 adapted to accommodate a fastener by means of which shell 10 and its mating shell are fastened together while a pair of tire chains is stored therein . flange 32 is provided with a similar hole 38 ( not shown in fig1 ). holes 36 and 38 are symmetrically located at the plane of symmetry of shell 10 , so that when a substantially identical shell is mated in open - face - to - open - face relation with shell 10 the holes in their end flanges will be in registration , to receive a pair of fasteners for fastening the mating shells together . in accordance with a particular feature of the present invention , no protrusions , such as integral fasteners or the like , which extend through the plane of the open face 40 of shell 10 are provided . it was recognized in the making of the present invention , that such protrusions would act as points of stress concentration when the shell was disposed on a hard surface ( e . g ., a concrete roadway ) and was bearing the weight of a vehicle , thus tending to rupture the shell . going now to fig2 there is seen shell 10 in a position inverted with respect to the position shown in fig1 . in fig2 it may be seen that shell 10 defines within itself three pockets or cavities 42 , 44 , and 46 . the two larger pockets 42 , 44 are of such a size as to each be capable of containing one tire chain of the largest size with which the shell 10 is adapted to cooperate ( it is not contemplated that such a maximum size tire chain will necessarily be entirely contained within a pocket 42 , 44 , but rather that such a maximum size tire chain can be easily piled in one of the pockets 42 , 44 , without spilling onto or projecting above open mating face 40 .) in addition to the tire chain receiving pockets 42 , 44 , shell 10 is also provided with a smaller central pocket 46 , wherein may be stored tire chain hardware , such as spare links and spare tire chain clips . going now to fig3 there is shown the cross - sectional configuration of a shell 10 embodying the preferred form of the present invention . it is to be particularly noted that , in accordance with the principles of the present invention , the small storage pocket 46 is defined by two side walls 50 , 51 , and a bottom wall 52 . it is to be further noted that the inner side walls of the chain receiving pockets 42 , 44 consist of said small pocket sidewalls 50 , 51 and also additional side members 53 , 54 ; all of said wall members 50 , 51 , 52 , 53 , 54 being integral , and the side wall members 53 , 54 being integral with the aforementioned plane bottom surfaces 28 , 30 . by this construction an integral strengthening bridge is provided , whereby shell 10 may be made as light as possible consistent with two such shells being capable of supporting the full weight of the rear end of the motor vehicle while tire chains are being mounted on the rear wheels thereof . going now to fig4 there is shown a pair of shells 10 , described hereinabove , which are fastened in open - face - to - open - face relation for containing a pair of tire chains and associated hardware . these two shells 10 are fastened together by means of bolts 56 , 58 coacting with nuts 60 , 62 , each nut if desired , being of the type incorporating a device for resiliently engaging the material through which it passes , in this case the flanges 32 , 34 , whereby to prevent the working loose of these nuts due to vibration . it is to be understood that the particular arrangement of nuts 60 , 62 and bolts 56 , 58 illustrated and described hereinabove are not the only means by which a pair of shells 10 of the present invention may be fastened together for containing a pair of tire chains . for instance , a belt or strap having a friction buckle ( sometimes called a &# 34 ; bookstrap &# 34 ;) may be passed through both of the channels 22 when a pair of shells 10 is in face - to - face relation , and drawn tight , the shells thereby being maintained in face - to - face relation for storing a pair of tire chains . other fastening arrangements will be provided by those having ordinary skill in the art without the exercise of invention . it is to kept in mind , however , that in accordance with one aspect of the present invention no protrusions are to project from the mating faces 40 of the shells 10 . it will now be seen that the objects set forth above , among those made apparent from the preceding description , are efficiently attained , and since certain changes may be made in the above construction without departing from the scope of the present invention , it is intended that all matter contained in the above description or shown in the accompanying drawings shall be interpreted as illustrative only , and not in a limiting sense . it is also to be understood that the following claims are intended to cover all of the generic and specific features of the invention herein described , and all statements of the scope of the invention which , as a matter of language , might be said to fall therebetween . | 1 |
this invention is further explained with the following first to third embodiments , which are however not intended to restrict the scope of this invention . for example , the first sub - patterns and / or the second sub - patterns of a photoresist pattern for forming a chessboard - type microlens may have shapes other than those shown in fig8 a - 8b . fig2 schematically illustrates the microlens array formed in the second case of the first embodiment and the paths of the incident lights at the array center and the array edge respectively . the microlens array formed in the first embodiment can be called a cushion - type microlens array , which is characterized in that each microlens therein has different curvatures between the x or y direction and the diagonal direction . as shown in fig2 , in the second case of the first embodiment , the height of the microlens 200 decreases from the array center toward the array edge , and the curvature of the same also decreases from the array center toward the array edge , so that the focal length of the same increases from the array center toward the array edge . since the incident angle of the incident light increases from the array center toward the array edge ( 16 b & gt ; 16 a ), all incident light passing the microlenses 200 from the array center to the array edge can be focused at the photosensitizing plane 110 . fig3 schematically illustrates the microlens array formed in the second embodiment and the paths of the incident lights at the array center and the array edge respectively . the microlens array formed in the second embodiment can be called a continuous - type microlens array , as described in u . s . patent application ser . no . 11 / 970 , 936 filed on jan . 8 , 2008 , being characterized in that any two neighboring microlenses therein are connected with each other and each microlens has substantially the same curvature in the vertical cross - sectional views of all directions . any two neighboring photoresist patterns among the photoresist patterns as the precursor of the continuous - type microlenses are connected with or close to each other , so that any two neighboring microlenses are connected with each other . as shown in fig3 , any two neighboring microlenses 300 are connected with each other . the heights of the microlenses 300 are substantially the same , but the curvature of the same decreases from the array center toward the array edge , so that the focal length of the same increases from the array center toward the array edge . since the incident angle of the incident light increases from the array center toward the array edge ( 16 b & gt ; 16 a ), all incident light passing the microlenses 300 from the array center to the array edge can be focused at the photosensitizing plane 110 . in the first embodiment of this invention concerning the cushion - type microlens array , microlenses are formed by reflowing a plurality of separate photoresist patterns previously formed on the planarization layer . the top view of each photoresist pattern has a substantially square shape , so that each microlens has different curvatures in the x or y direction and the diagonal direction . referring to fig4 a and the iv - iv ′ cross - sectional view in fig4 b , in the first case of the first embodiment , all the photoresist patterns 400 with a substantially square shape in the top view have the same height , but the area thereof increases from the array center to the array edge , so that the distance between two neighboring photoresist patterns 400 decreases from the array center to the array edge . because the photoresist patterns 400 have the same height and the area thereof increases from the array center to the array edge , the microlenses 410 formed from the photoresist patterns 400 have the same height , and the curvature thereof decreases from the array center toward the array edge so that the focal length thereof increases from the array center toward the edge . since the incident angle of the incident light also increases from the array center toward the array edge , all incident light passing the microlenses 410 from the array center to the array edge can be focused at the photosensitizing plane . moreover , for the distance between two neighboring photoresist patterns 400 decreases from the array center to the array edge 110 , any two neighboring microlenses 410 apart from the array center by a distance larger than a certain value are connected with each other , and the thickness of the connection part gradually increases toward the array edge . referring to fig5 a and the v - v ′ cross - sectional view in fig5 b , in the second case of the first embodiment , all the photoresist patterns 500 have the same area , but the height thereof decreases from the array center to the array edge , so that the height and the curvature of the microlenses 200 formed from the photoresist patterns 500 decrease from the array center toward the array edge and the focal length increases from the array center toward the array edge . in the second case of the first embodiment , the height decrease of the photoresist patterns 500 from the array center toward the array edge may be achieved by increasing the transparency of the photomask patterns defining the photoresist patterns 500 from the array center toward the array edge . the transparency increase may be achieved by including a transparent portion and an opaque portion in each photomask pattern and making the area proportion of the transparent portion in the photomask pattern increases from the array center toward the array edge . the area proportion of the transparent portion in a photomask pattern may be varied with the methods shown in fig6 a - 6b . referring to fig6 a , each photomask pattern 602 includes an opaque portion 604 constituted of a plurality of block opaque regions , and a transparent portion 606 constituted of a plurality of transparent line regions between the block opaque regions . the number of the transparent line regions of the photomask patterns 602 increases from the array center toward the edge , so that the area proportion of the transparent portion 606 in the photomask pattern 602 increases from the array center toward the array edge and the transparency of the photomask pattern 602 increases from the array center toward the array edge . referring to fig6 b , each photomask pattern 612 includes an opaque portion 614 , and a transparent portion 616 constituted of a plurality of transparent dot regions in the opaque portion 614 . the number of the transparent dot regions in the photomask patterns 612 increases from the array center toward the edge , so that the area proportion of the transparent portion 616 in the photomask pattern 612 increases from the array center toward the edge and the transparency of the photomask pattern 612 increases from the array center toward the array edge . on the other hand , in the second embodiment of this invention concerning the continuous - type microlens array , the photomask pattern for defining a microlens may have a transparency distribution where the transparency increases from the center of the photomask pattern toward the edge of the same . such a transparency distribution may be made by disposing certain concentric transparent scattering rings . three examples of the photomask patterns with transparent scattering rings are shown in fig7 a - 7b . referring to fig7 a , as compared to the edge photomask pattern 702 , the central photomask pattern 702 additionally has two smaller transparent scattering rings 706 , while the widths of the opaque portion 704 between the common transparent scattering rings 706 of them are substantially the same , so that the transparency increase rate from the center of the edge photomask pattern 702 toward the edge of the same is lower than that from the center of the central photomask pattern 702 toward the edge of the same . hence , as compared with the case of the central photomask pattern 702 , the center - to - edge height difference of the photoresist pattern 708 defined by the edge photomask pattern 702 is smaller , so that the curvature of the corresponding microlens 300 is smaller . the variation of the curvature of the microlenses 300 from the array center to the array edge can be controlled by adjusting the number and widths of the additional smaller transparent scattering rings 706 . referring to fig7 b , the central opaque portions 714 of the photomask patterns 712 from the array center to the array edge have the same diameter d 1 , while the width of the transparent scattering rings 716 decreases from the array center to the array edge ( w 1 ′& lt ; w 1 ) and the width of the annular opaque portions 714 between the scattering rings 716 increases from the array center to the edge . thereby , the closer a photomask pattern 712 is to the array edge , the lower the transparency increase rate from its center to its edge . thus , the self center - to - edge height difference of the photomask pattern 718 decreases from the array center to the edge , so that the curvature of the microlenses 300 formed from the photoresist patterns 718 by thermal reflow decreases from the array center to the edge . meanwhile , the height of the connection portion between two neighboring photomask patterns 718 increases from the array center to the array edge . referring to fig7 c , the central opaque portions 724 of the photomask patterns 722 from the array center to the array edge have the same diameter d 1 and the widths of the transparent scattering rings 726 are not varied , but the width of the annular opaque portions 724 between the scattering rings 726 increases from the array center to the edge ( d 2 ′& gt ; d 2 , d 3 ′& gt ; d 3 ). thereby , the closer a photomask pattern 722 is to the array edge , the lower the transparency increase rate from its center to edge . thus , the self center - to - edge height difference of the photomask pattern 728 decreases from the array center to the array edge , so that the curvature of the microlenses 300 formed from the photoresist patterns 728 by thermal reflow decreases from the array center to the edge . meanwhile , the height of the connection portion between two neighboring photomask patterns 728 increases from the array center to the array edge . fig8 a and 8b schematically illustrate the variations of the photoresist patterns as the precursor of the microlenses from the array center toward the edge according to two examples of the third embodiment of this invention . the microlens formed in this embodiment can be called a chessboard - type microlens , which typically includes two first sub - microlenses arranged diagonally and two second sub - microlenses arranged diagonally . the shapes of the first and the second sub - microlenses before the thermal reflow , i . e ., the shapes of the first and second sub - photoresist patterns as the precursors of the first and the second sub - microlenses , are different in the top view . to make all incident light passing the microlenses from the array center to the array edge be focused at the photosensitizing plane , the focal length of such chessboard - type have to be increased from the array center to the edge . this may be achieved by increasing the area of the first or second sub - photoresist pattern from the array center to the array edge . referring to fig8 a , a photoresist pattern 800 as the precursor of a chessboard - type microlens includes two first sub - patterns 802 arranged diagonally and two second sub - patterns 804 arranged diagonally . the first sub - patterns 802 are formed in a first lithography process , the second sub - patterns 804 are formed in a second lithography process , and the first sub - patterns 802 overlap with the second sub - patterns 804 . in the top view , a first sub - pattern 802 has a substantially circular shape , and a second sub - patterns 804 substantially has an octangular shape corresponding to a square shape that is cut at four corners thereof . in the example of fig8 a , the focal length of the chessboard - type microlenses is increased from the array center to the array edge in the following manner . the center - to - center distance between the two first sub - patterns 802 and that between the two second sub - patterns 804 in any photoresist pattern 800 are fixed . meanwhile , the radius of the substantially circular first sub - pattern 802 is increased from the array center to the array edge ( r ′& gt ; r ), so that the area of the first sub - pattern 802 increases from the array center to the array edge . in the example of fig8 b , the focal length of the chessboard - type microlenses is increased from the array center to the array edge in the following manner . the center - to - center distance between the two first sub - patterns 812 and that between the two second sub - patterns 814 in any photoresist pattern 810 are fixed . meanwhile , the area of the cut corners of the square shape corresponding to the second sub - pattern 814 is decreased from the array center to the array edge ( 2 d ′ 2 & lt ; 2 d 2 ), so that the area of the second sub - pattern 814 increases from the array center to the array edge . since the focal length of the microlenses formed in this invention increases from the center to the edge of the image sensor while the incident angle of the incident light increases from the center to the edge of the image sensor , all incident light from the center to the edge of the image sensor can be focused at the photosensitizing plane . thus , the sensitivity of the photosensitizing devices can be uniformized , so that the distortion in image recording can be reduced as compared to the prior art . this invention has been disclosed above in the preferred embodiments , but is not limited to those . it is known to persons skilled in the art that some modifications and innovations may be made without departing from the spirit and scope of this invention . hence , the scope of this invention should be defined by the following claims . | 7 |
the expression functional group of the said polyfunctional molecule is understood here to refer to a group capable of establishing a covalent bond with the solid support . amine , hydroxyl , carboxyl , aldehyde , thiol and phosphate groups are mentioned in particular as functional groups . when the linker arm contains a very reactive group such as a terminal phosphate group at its end which is not linked to the primer , it is not necessary for the polyfunctional molecule to contain a large number of functional groups . however , the said polyfunctional molecule preferably contains at least five , more preferably at least ten , functional groups . in an advantageous embodiment of the invention , the said polyfunctional molecule comprises a polymer fragment . preferably , each monomer unit of the said polymer fragment contains at least one functional group . in this case , an increase in the size of the linker arm , that is to say the polymer , is reflected by an increase in the number of potential sites for terminal binding of the primer and allows the elongation yield to be increased , this being although the overall level of binding of the primer to the solid support remains constant . preferably , the polymer fragment added to the 5 ′ end of the said primer contains more than 5 monomers , more preferably more than 10 monomers , in particular up to 50 monomers . advantageously , the said polymer fragment according to the invention comprises a homopolynucleotide fragment or a fragment of a polynucleotide analog . the term “ polynucleotide analog ” is understood here to refer to a polymer whose monomer units are joined by a phosphodiester linkage similar to the phosphodiester linkage of natural polynucleotides . in other words , it is a polymer in which the nucleoside residues of the nucleotide monomers are replaced with non - nucleoside residues , in particular aliphatic residues . mention is made in particular of the polymer fragments of formula ( i ) below : in which r is an aliphatic residue , in particular of from 2 to 20 carbon atoms , such as an alkylene residue , r containing at least one functional group according to the invention , and n is an integer from 2 to 50 in particular . preferably , the polymer fragment of polynucleotide - analog type according to the invention contains several reactive groups grafted onto each monomer , in particular amine or hydroxyl groups , and in this case n may more particularly be between 2 and 10 only . when the linker arm consists of a homopolynucleotide fragment , it preferably contains more than 5 nucleotides , more preferably more than 10 nucleotides , in particular up to 50 nucleotides . the polynucleotide analogs according to the invention may be obtained by synthetic methods similar to the methods for synthesizing dna , in particular by automated synthesis on a solid support . indeed , these polymer fragments may be obtained by condensation of monomer synthons which are suited to the processes of nucleotide synthesis involving the use of phosphoramidite synthon &# 39 ; s , that is to say a synthon containing , in a conventional manner , two terminal oh groups , one of which is protected by a dimethoxytrityl ( dmtr ) group and the other by a phosphoramidite group . the polymer fragment of polynucleotide - analog type corresponds in this case to the condensation of synthons similar to the standard nucleotide synthons in which the divalent nucleoside residue at 5 ′ and 3 ′ is replaced by an aliphatic residue , in particular an alkylene residue . more particularly , in order to obtain the polynucleotide analog polymer fragments of formula ( i ), it is possible to use phosphoramidite synthons of formula : thus , when the linker arm is a polynucleotide fragment or polynucleotide analog , the linker arm or the primer conjugated to the linker arm may advantageously be prepared directly by nucleotide - type synthesis , the said conjugate being subsequently coupled to the solid support according to the invention . the polymer fragment , in particular homopolynucleotide or polynucleotide analog , may be a branched fragment , that is to say one containing several branches . this type of fragment may be obtained using a monomer which may serge as a base for condensation with several monomers on the same synthon . mention is made in particular of the following phosphoramidite synthon ( ref . 5250 - 1 from clontech ): which may be used in the synthetic process of the automated dna synthesis type and may condense with two monomers in parallel . advantageously , the said polymer and in particular the homopolynucleotide fragment or polynucleotide analog placed between the solid support and the primer contains , at its end which is not linked to the primer , a reactive terminal functional group which may establish a covalent bond with the solid support . a hydroxyl group or an amine and , more preferably , a phosphate group are mentioned in particular as the said reactive terminal functional group of the polymer fragment . the use of a terminal phosphate group is particularly recommended when the linker arm is a poly - t . in the absence of phosphate group , a poly - a or poly - c linker arm is more effective . the methods of automated dna synthesis on a solid support make it possible chemically to phosphorylate the terminal 5 ′ end of large amounts of oligonucleotides . it is therefore possible , by these methods , to prepare linker arms of homopolynucleotide type or polynucleotide - analog type or conjugates of these linker arms and of the primer , which are phosphorylated at the 5 ′ end of the linker arm . according to the invention , the solid support consists of functionalized organic or inorganic polymer . according to the present invention , certain characteristics of the solid support are advantageous for being able to elongate an oligonucleotide primer bound to a solid support as a product of amplification . firstly , this solid support must be heat - resistant , that is to say capable of withstanding the high temperatures of pcr ( 100 ° c .) and must be of good heat conductance . it must be functionalized , that is to say contain chemical functions , in order to allow the stable binding of an oligonucleotide primer to the solid support . this primer / solid support bonding must also withstand high temperatures . this is why , according to the present invention , covalent bonding is preferred . the taq polymerase or other enzyme responsible for the elongation should not be inhibited by the components of the support . lastly , such a support should have optical properties which allow calorimetric or fluorescent detection with no background noise . a transparent support is preferred since it allows the use of reading equipment of any type . types of plastic which have great resistance to high temperatures are thus preferably used . plastics based in particular on heat - resistant modified polystyrene , on styrene / acrylonitrile copolymer , on polycarbonate , on polypropylene or on glass are mentioned in particular . solid plastic supports functionalized by uv treatment in order to induce the appearance of nh 2 functional groups may be used ( ref . 1 ). however , according to the present invention , the solid support may be a polyfunctionalized support , that is to say one containing a multiplicity of functional groups , in particular aldehyde , carboxyl , amine , hydroxyl or thiol , which promote the establishment of a stable covalent bond with the linker arm consisting of the said polyfunctional molecule linked to the primer . plastic supports which have been treated by corona treatment or gamma - irradiation in order to induce the appearance of a multiplicity of functional groups are appropriately used . this type of treatment is simple and avoids the use of chemical reagents for functionalization . polycarbonate or a styrene / acrylonitrile copolymer which are functionalized , inter alia , by corona treatment or gamma - radiation are used in particular as preferred heat - resistant support . methods for the covalent bonding of oligonucleotides to solid supports functionalized by means of a terminal functional group of the oligonucleotide are known ( ref . 1 to 5 ). however , according to the invention , the homopolynucleotide fragments may be bound to the solid support via the natural functional groups , in particular amine and hydroxyl of the nucleotide bases themselves , or via a terminal functional group , in particular phosphate . similarly , the fragments of polynucleotide - analog type may also be bound to the solid support via a terminal group or one of the functional groups , in particular amine or hydroxyl , which are substituted on the monomers . this coupling between the functional groups of the linker arm , in particular of the homopolynucleotide fragment or polynucleotide analog , and the functional groups of the support may take place by chemical coupling in the presence of conventional activating agents . in particular , chemical coupling to a polyfunctional support is carried out in the presence of an activating agent of carbodiimide type , such as edc . the subject of the present invention is also a process for immobilizing a primer on a solid phase , this primer being useful in carrying out an amplification process according to the present invention , characterized in that covalent coupling is carried out between the said functionalized support and the said polyfunctional molecule linked to the 5 ′ end of the said primer . the solid support may be the inner surface of the pcr reaction container , or a solid component which is introduced into the container before the reaction , such as beads . the inner surfaces of microtitration microplate wells or of assay tubes are mentioned in particular as solid support . the preferred format is the microplate format . the reason for this is that its widespread use and all the already - existing apparatus around this format allow it to be automated quickly and readily . two types of microplate are commonly used . the first is of standard type with flat - bottomed cylindrical cupules . the second does not contain cylindrical cupules as above , but wells in the form of a small , flat - bottomed truncated tube . this form of tube allows ready adaptation to the thermal cycler and allows excellent thermal conductance . the subject of the present invention is also a process for immobilizing a primer on a solid phase , this primer being useful in carrying out an amplification process according to the present invention , characterized in that covalent coupling is carried out between the said functionalized support and the said polyfunctional molecule linked to the 5 ′ end of the said primer . solid - phase amplification allows amplification and detection to be carried out on the same support . the amplification product elongated on the solid surface may be detected in different ways . the double - strand bound to the support may be detected either by revealing a label incorporated during the pcr , in particular by means of a second labeled primer , or via the use of an ethidium bromide , yoyo , toto or popo type intercalating agent ( molecular probes ref . 6 to 8 ). after denaturation , the single strand specifically bound to the solid support may also be detected by a labeled probe . the detection consists , for example , in hybridizing a biotinylated oligonucleotide probe which specifically recognizes the amplification product elongated on the plate . a streptavidin / alkaline phosphatase conjugate recognizes the biotin species of the hybridized probe and , after dephosphorylation of a substrate , generates a calorimetric or fluorescent product . the mode of binding of the primer according to the present invention is a determining factor for the elongation . this is because if the primer has a linker arm according to the invention , the elongation yield may be increased 15 - fold depending on the type of arm , whereas the level of binding remains constant irrespective of the linker arm . the amount of primer present in solution in the amplification reaction also plays an important role as regards the elongation yield . in order to have an optimum yield for elongation of the bound primer , an unequilibrated pcr is used ( ref . 9 ). during the pcr , the primer bound to the solid support ( primer a ) is also present in solution but in lower amount , in particular 8 to 16 times less than the other amplification primer ( primer x ). the amplification takes place in two steps ; the amplification is first exponential until the primer a in solution is depleted , the primers a bound to the solid support are next elongated , and the amplification then becomes arithmetic . the first step makes it possible to have a large number of copies and thus allows more effective elongation on the solid support . the amount of primer placed in solution is critical since it determines the moment at which the arithmetic amplification commences . an amount of about 5 to 10 pmol for the primer x and from 8 to 16 times less for the primer a gives good elongation yields . the amplification process according to the present invention affords a real improvement when compared with the usual diagnostic techniques using pcr , be it for infectious or genetic diseases . moreover , since the process according to the invention makes it possible to attach specifically a single strand to the solid phase , it may also be advantageous for sequencing , especially when large amounts need to be sequenced and when a simplification of the procedures and automation prove to be essential . other characteristics and advantages of the present invention will become apparent in the light of the detailed embodiment which follows . fig2 represents the binding yield in pm of the primer as a function of different linker arms . fig3 represents the levels of elongation in fluorescence units as a function of different linker arms . fig5 represents the influence of the size of the linker arm on the level of elongation . fig6 represents the influence of various chemical functions of the linker arm on the level of elongation . the process according to the invention was applied on an hla - drb model ( ref . 10 and 11 ). m13 clones carrying a 280 bp insert corresponding to the amplification product were used as target . this hla - drb model made it possible to demonstrate the important parameters involved in the elongation and to study most particularly the problem of specificity of this technique . linker arms comprising polymer fragments of the polynucleotide - analog type were also used ( fig6 ): the arm — nh 2 * corresponds here to an aminoalkyl arm introduced via the unilink ® amino modifier synthon from clontech , of formula : the arm — 5t - 5 nh 2 * corresponds to the successive condensation of 5 t nucleotides and then 5 unilink ® synthons in a phosphoramidite - type synthesis . the condensation of unilink ® synthons led to a polynucleotide - analog fragment with alkylamine residues grafted onto the monomers . ( teg ) 3 * corresponds to the condensation of the synthon from glen research ( ref : 10 - 1909 x ) of formula : ( teg ) 3 *− ph is obtained by 5 ′- terminal phosphorylation of the conjugate a —( teg ) 3 * according to the phosphoramidite synthesis . two types of polyfunctionalized heat - resistant support supplied by the company nunc were used to evaluate the various linker arms . type i is a heat - resistant modified polystyrene and type ii is a styrene / acrylonitrile copolymer . they are in a microplate format and are cycled in a thermocycler supplied by nunc . these plastic supports were functionalized by a corona treatment or gamma - irradiation , which consists conventionally in sending electric discharges into a chamber with controlled atmosphere and at fixed pressure . this functionalization allows the plastic support to be made capable of binding the oligonucleotide primers . this treatment causes functional groups of amine , alcohol , aldehyde , ketone , carboxylic acid , thiol , etc . type to appear at the surface of the plastic , these groups reacting chemically with the oligonucleotide to form a stable bond . although very heat - resistant , the types of bonds formed are , however , at the present time poorly understood . the chemical coupling is carried out in the presence of an activating agent according to the following procedure . 10 to 100 pmol of oligonucleotides are placed for binding per well in the presence of 10 to 50 mm final ethyl carbodiimide ( edc ) and 10 to 50 mm final n - methylimidazole , ph 7 , in a final volume of 100 μl . the plates are incubated for 5 to 15 hours at 50 ° c . and then washed 4 times with 0 . 4 n naoh solution and 0 . 25 % tween 20 , heated to 50 ° c . the elongation takes place in a final volume of 50 μl per well . 15 to 100 ng of the target dna are amplified in a mixture comprising 1x pcr buffer ii ( perkin elmer ), 0 . 25 mm mgcl 2 ( sigma ), 200 μm 2 datp , dctp , dgtp , dttp ( pharmacia ), 80 ng of primer x ( ccgctgcactgtgaagctct ) seq id no : 2 and 10 ng of primer a with or without linker and 1 . 2 units of taq polymerase ( perkin elmer ). the primer x is found in solution only , whereas the primer a is bound to the solid support and in solution . the amplification takes place on a thermocycler adapted to the microplate format , using the following method : fig1 represents the various steps of the solid - phase pcr . after amplification , the amplification products elongated on the solid phase are denatured . the wells are emptied and then washed 3 times with 0 . 4 m sodium hydroxide for 10 min . two types of detection were used . a semi - quantitative enzymic detection and a quantitative radioactive detection . the enzymic detection is performed as described in the literature ( 9 ). in this method , after denaturation , 1 pm of biotinylated probe complementary to a region of the strand elongated on the solid support is hybridized . the hybrid is revealed by a streptavidin / alkalyne phosphatase conjugate which converts a substrate into a chemiluminescent or fluorescent calorimetric product . for the radioactive detection , a 32 p - labeled probe is hybridized on the strand elongated on the solid support and the radioactivity is counted in a β counter . the binding capacity of the primer on the solid support was quantified by binding radioactively 5 ′- kinased primers and made it possible to show that the type i bound about 1 pm of primer per well , whereas the type ii bound 0 . 2 pm . fig2 represents the binding capacity of the primer to two microplate supports as a function of the various types of linker arm . for a given type of support , the binding capacity does not vary significantly as a function of the arms used . on the other hand , the elongation yield varies enormously as a function of the linker arm employed . the results are presented in fig3 and 5 , which represent the levels of elongation of the supports as a function of the various arms used . the influence of the arm attached to the primer is a determining factor for the elongation yield , which may be increased 15 - fold depending on the type of linker used , the level of binding remaining constant . the poly - a and poly - c fragments are more effective than the poly - t fragments . indeed , for linker arms of the same size , they give stronger signals for the elongation . the addition of a phosphate group always improves the elongation yield and this increase is more appreciable with the poly - t linker arm than with the poly - a or poly - c linker arms . the elongation was quantified indirectly by hybridization of radioactive probes complementary to the part elongated by pcr . the level of hybridization was verified by hybridizing radioactive probes to wells containing a known amount of bound primers . the level of elongation varies according to the type of linker arm used , between 2 fm and 38 fm or between 1 fm and 17 fm for type i and type ii respectively . these results are presented in fig4 . the presence of several functional groups in the linker arm makes it possible to increase the level of elongation of the primer bound to the solid support . thus , as shown in fig6 a 45 % increase is noted when 10 t is inserted between the primer and a terminal phosphate group . similarly , the addition of a phosphate function to a ( teg ) 3 * linker arm makes it possible to increase the signal by 40 % and 350 % relative to the primer alone without linker arm . the same phenomenon is observed when a 5t5nh 2 * arm is used ; the level of elongation is increased by 110 % relative to an nh 2 * arm . the use of several different chemical functions thus makes it possible to promote the elongation of the primer on the solid phase by increasing the types of terminal linkages . the amount of oligonucleotides elongated is , in fact , very low relative to the amount bound to the support . despite this low amount , signal - to - noise ratios of about 30 are achieved with the enzymic detection technique described , which is entirely sufficient for a diagnostic application . | 2 |
referring now to the drawings fig1 - 10 , wherein similar parts of the invention are identified by like reference numerals , there is seen in fig1 a plan view of a stringed instrument such as the depicted electric guitar employing the disclosed compound musical instrument string configuration and support system 10 . the compound musical instrument string configuration and support system 10 , while illustrated as an electric guitar 12 , is equally adaptable for inclusion on any stringed instrument . consequently , inclusion on any type of stringed instrument is anticipated by this patent application . most stringed instruments such as the guitar 12 consist of a lower body unit 14 and a neck 16 portion on which string tensioners 26 are mounted for adjusting the instrument tone . on a guitar 12 , the neck 16 features a plurality of frets 18 used as a means to locate the users fingers on the neck to produce different notes when the strings are depressed to the neck 16 . electronic pickups 20 and volume controls 22 are unique to electric instruments only . as shown , the compound instrument strings 24 are gripped on the distal ends on the conventional tensioners 26 and translate over the string height adjustment mechanism 28 then over the frets 18 to the electronic pickups 20 and over the bridge unit 30 to be held by the string retainer 32 b . the string height adjustment mechanism 28 , while desirable in the preferred mode of the device , could be an option . a means to strengthen the neck 16 and body 14 engagement to maintain an inline planar engagement of the neck and body when the stings are tensioned is provided in the depicted device as at least one buttress element 34 extending from the upper portion of the neck 36 to the guitar lower body 14 . two buttress elements 34 are shown . while those skilled in the are will no doubt realize that steel or other reinforcements may be built into the neck 16 and body 14 as a reinforcement means to maintain the inline planar engagement between the two when the strings 24 are tensioned , such reinforcement conventionally adds structure and considerable size to the neck 16 . this increase in size results in a neck 16 that is much more difficult for the user to play . consequently one and preferably two buttresses 34 allow the neck 16 to be sized small for easy play and still provide great strength to the instrument and maintain the neck 16 aligned with the body 14 when the strings are tensioned , and keep the strings in line raised position over the length of the neck and body . fig2 depicts a section through the side of the guitar 12 using the preferred embodiment of the compound musical instrument string configuration and support system 10 further illustrating the guitar 12 with the lower body unit 14 and a neck 16 with a plurality of frets 18 and the electronic pickups 20 and volume controls 22 . in used as a guitar , the compound instrument strings 24 are both attached or gripped on the conventional tensioners 26 at their distal ends , and translate over the string height adjustment mechanism 28 , then over the frets 18 down the guitar neck 16 to the electronic pickups 20 and over the bridge unit 30 to be held by the string retainer 32 b . this section clarifies the thin cross section 38 required of the guitar neck 16 when the buttress elements 34 are incorporated into the design of the musical instrument . fig3 depicts a cross section through the guitar neck 16 of the guitar 12 using the preferred embodiment of the compound musical instrument string configuration and support system 10 illustrating the relief &# 39 ; s 40 in the buttress elements 34 to add clearance in the areas 42 for the players hands to pass through . also shown in fig3 , is the metal reinforcement 41 which might be used instead of the preferred buttresses 34 as a means to strengthen the neck and body engagement . fig4 shows a section through a single compound instrument string 24 over a single fret 18 in a fret board 44 on the guitar neck 16 . the compound instrument string 24 consists of a first or left leg 46 and a second or right leg 48 doubled back and engaged by the means of a soft flexible polymer or rubber material 50 . the clearance 52 of the compound instrument string 24 over the fret 18 is maintained by a means to adjust the clearance of the compound string 24 over the fret in the form of a string height adjustment mechanism 28 allowing for a lower overall height 54 of the compound instrument string 24 . fig5 depicts a perspective view of the string height adjustment mechanism 26 consisting of a mounting plate 56 holding a central shaft 58 and a plurality of height adjustment bushings 60 separated by spacers 62 and held in place by the means of set screws 64 . fig6 and fig7 depict sections through the string height adjustment mechanism 28 in the raised position with a clearance of 52 a and in the lowered position with a clearance of 52 b with the compound instrument string 24 passing through the locating slot 66 . fig8 depicts a perspective view of the bridge unit 30 of the compound musical instrument string configuration and support system 10 showing central shaft 68 with a locking nut 70 and two of the low friction bearings 72 and a thin spacer washer 74 exploded away from a mounting plate 76 . the soft flexible polymer or rubber material 50 provides a means to slidably engage the left leg 46 with the right leg 48 of the compound instrument string 24 and is terminated prior to the left leg 46 and the right leg 48 being divided by the thin spacer washer 74 . the separation of the left leg 46 and the right leg 48 at the bridge unit 30 is essential for the left leg 46 to go below the low friction bearing 78 on the string retainer 32 a or 32 b . additionally shown in fig8 is a rigid clip or grommet 79 adjacent to the bridge unit 30 of the instrument . one or more of these rigid clips or grommets 79 can be attached to the compound instruments strings 24 . this coupling means may be used separately or in combination on the compound musical instrument string configuration and support system 10 . the slidable yet fixed coupling of the two legs in series insures that they vibrate at the same frequency with each other yet slip past each other when tensioned if need be . fig9 depicts a perspective view of the alternate embodiment of a means to rotationally engage the end of the string 24 in the form of the string retainer 32 b of the compound musical instrument string configuration and support system 10 with a central shaft 80 with a lock nut 82 exploded away from the retainer 32 b mounting plate 83 with a polarity of spacers 84 separating the low friction bearings 78 . the left leg 46 of the compound instrument string 24 goes below the low friction bearing 78 to double back and become the right leg 48 while staying in alignment with the thin spacer washer 74 of the bridge unit 30 . fig1 depicts a perspective view of another preferred embodiment of the string retainer 32 a of the compound musical instrument string configuration and support system 10 with two stanchions 85 attached to a mounting plate 86 with the compound instrument string 24 doubling back around a low friction bearings 88 on each side that is held in place with mounting screw 90 and spacers 92 on either side . the compound musical instrument string configuration and support system 10 shown in the drawings and described in detail herein disclose arrangements of elements of particular construction and configuration for illustrating preferred and alternate embodiments of structure and method of operation of the present invention . it is to be understood , however , that elements of different construction and configuration and other arrangements thereof other than those illustrated and described may be employed for providing a compound musical instrument string configuration and support system 10 in accordance with the spirit of this invention , and such changes , alternations and modifications as would occur to those skilled in the art are considered to be within the scope of this invention as broadly defined in the appended claims . further , the purpose of the foregoing abstract is to enable the u . s . patent and trademark office and the public generally and especially the scientists , engineers and practitioners in the art who are not familiar with patent or legal terms or phraseology , to determine quickly from a cursory inspection the nature and essence of the technical disclosure of the application . the abstract is neither intended to define the invention of the application , which is measured by the claims , nor is it intended to be limiting as to the scope of the invention in any way . | 6 |
applicants specifically incorporate the entire content of all cited references in this disclosure . further , when an amount , concentration , or other value or parameter is given as either a range , preferred range , or a list of upper preferable values and lower preferable values , this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value , regardless of whether ranges are separately disclosed . where a range of numerical values is recited herein , unless otherwise stated , the range is intended to include the endpoints thereof , and all integers and fractions within the range . it is not intended that the scope of the invention be limited to the specific values recited when defining a range . the key design element is the use of phosphoserine or phosphothreonine , preferably phosphoserine , as an inducible mimic of a structurally significant glutamic acid or aspartic acid residue , preferably a glutamic acid residue . by “ structurally significant ” is meant that the glutamic acid or aspartic acid residue plays an important role in the secondary , tertiary , and / or quaternary structure of a peptide . phosphoserine and glutamic acid are approximately isosteric anions , suggesting that the replacement of glutamic acid with phosphoserine would generate a motif that would bind metal in a phosphorylation - dependent manner ( see , e . g ., fig2 ). indeed , glutamic acid is commonly used as a mimic of phosphoserine [ 6 ]. here , applicants employed an inverse approach , in which phosphoserine , but not serine , mimics the electrostatic and lewis base properties of glutamic acid . in one embodiment , a designed phosphorylation - dependent protein domain ( a ) exhibits complete structural switching upon phosphorylation ; ( b ) includes a protein kinase recognition sequence ; ( c ) comprises a modular motif that is compatible with different protein kinase recognition sequences ; ( d ) includes a fluorescent reporter element for readout ; and ( e ) consists entirely of canonical amino acids , to enable its use as a genetically encoded phosphorylation - dependent protein tag and as a building block in the design of larger phosphorylation - dependent protein architectures . this strategy can be applied , in one embodiment , to the design of phosphorylation - dependent ef hand domains . the term “ ef hand ” refers to a protein domain containing a simple calcium - binding motif in which the metal is bound by five side chain groups and one main carbonyl ( see fig1 ). ef hand proteins , such as , for example , calmodulin , undergo a significant conformational change to a well - folded helix - loop - helix structure upon calcium binding [ 7 - 9 ]. due to similar electronics and ionic radii of calcium and lanthanides , ef hands effectively coordinate lanthanides [ 10 - 16 ], thereby endowing the ef hand with the luminescent , magnetic , and hydrolytic properties of lanthanides [ 17 - 20 ]. the ef hand motif accommodates a wide range of residues at most positions . in contrast , residue 12 of the ef hand is nearly invariantly glutamic acid , which binds the metal in a bidentate manner . replacement of glutamic acid with phosphoserine generates a motif that binds metal in a phosphorylation - dependent manner ( see fig2 ). non - phosphorylated serine is a poor glutamic acid mimic and should poorly bind metal ; in contrast , serine phosphorylation should lead to a tight protein - metal complex . critically , residues n - terminal and c - terminal to residue 12 are poorly conserved across ef hand proteins , and thus may be tuned to incorporate the recognition sequence of a protein serine / threonine kinase of interest [ 21 ]. in other embodiments of the ef - hand , glutamic acid or aspartic acid residues bind from different positions , including residue 9 , residue 16 , or from a different position in the tertiary or quaternary quaternary structure of the protein [ 46 - 47 ]. in one aspect , an inducible ef hand domain can be defined by the following formula : x 1 x 2 dx 3 x 4 x 5 dx 6 wx 7 x 8 x 9 x 10 x 11 x 12 x 13 x 14 x 15 x 16 ( i ) x 3 is any amino acid , preferably k , a , or l ; x 4 is any amino acid , preferably n or d ; x 6 is any amino acid , preferably g or r x 7 is any amino acid , preferably i or r ; x 8 is any amino acid , preferably d , r , s , or t ; x 9 is any amino acid , preferably a , r , k , p , or f ; x 10 is an optionally present amino acid , preferably a , r , g , or l , provided that , when x 8 is not s or t , x 10 is present ; x 11 is an optionally present amino acid , preferably s , t , or r , provided that , when x 8 is not s or t , x 11 is present and is s or t ; x 12 is an optionally present amino acid , preferably l , p , i , k , or f ; x 13 is an optionally present amino acid , preferably k , a , i , r , g , or l ; x 14 is an optionally present amino acid , preferably a , r , or p ; x 15 is an optionally present amino acid , preferably k ; x 16 is an optionally present amino acid , preferably a . for formula i , standard polypeptide abbreviations for amino acid residues are used , as shown in table 1 . the ef hand domain can have the amino acid sequence set forth in seq id no : 1 , seq id no : 3 , seq id no : 5 , seq id no : 8 , seq id no : 9 , seq id no : 10 seq id no : 11 , seq id no : 12 , seq id no : 13 , seq id no : 14 , seq id no : 15 , seq id no : 16 , seq id no : 17 , seq id no : 18 , seq id no : 19 , seq id no : 20 , seq id no : 21 , seq id no : 22 , seq id no : 23 , seq id no : 24 , seq id no : 25 , seq id no : 26 , seq id no : 27 , seq id no : 28 , seq id no : 29 , seq id no : 30 , seq id no : 31 , seq id no : 32 , seq id no : 33 , seq id no : 34 , seq id no : 35 , seq id no : 36 , seq id no : 37 , seq id no : 38 , or seq id no : 39 ; can have the amino acid sequence set forth in seq id no : 2 , seq id no : 4 , or seq id no : 6 ( when the serine residue is phosphorylated ); or can have the amino acid sequence set forth in seq id no : 40 or seq id no : 41 wherein the serine at amino acid residue number 16 is phosphorylated . effectiveness of inducible ef domains can be optimized through electrostatic balance of the ef domain between the n - terminal and c - terminal region . for example , modification of an ef hand domain to accommodate a consensus pka recognition sequence in the c - terminal region of the ef hand typically changes the electrostatic balance of the ef hand domain towards a positive charge due mainly to the change of neutral or negatively - charge amino acids to positive ones ( especially to arginines ). by electrostatically balancing the inducible ef hand domain through the modification of n - terminal amino acids to negatively - charged amino acids or through the addition of negatively - charged amino acids n - terminal of the ef hand domain , inducible functioning as described herein is increased as compared to electrostatically unbalanced ef hand domains . in embodiments where expressibility in cells is desired , the amino acids of the protein kinase - inducible domain can be canonical . this flexibility in domain composition is advantageous over known kinase assays where detectability of kinase activity is dependent on the use of non - canonical and / or synthetic amino acids that cannot be produced via a cell - based expression system . the protein kinase - inducible domains disclosed herein , however , can readily be produced via any expression as would be known to one of ordinary skill in the art . of course , non - canonical and / or synthetic amino acids can be utilized in the connection with the presently disclosed protein - kinase inducible domains in embodiments where cellular expressibility is not needed or undesired . provided that a proper kinase recognition sequence is present in the phosphorylation - dependent protein domain , any serine / threonine kinase should be functional in connection with the disclosed phosphorylation - dependent protein domains . exemplary serine / threonine kinases include protein kinase a , protein kinase c , protein kinase g , calmodulin - dependent protein kinases ( e . g ., camki , ii , iii , iv , v ), casein kinases ( e . g ., cki , ii ), cyclin - dependent kinases ( e . g ., cdk1 - 12 ), jun n - terminal kinases ( e . g ., jnk1 - 14 ), map kinases ( e . g ., erk , p38 , raf , ask ), myosin light chain kinase , akt / protein kinase bs ( e . g ., akt1 - 3 ), g protein - coupled receptor kinases ( e . g ., grk1 - 7 ), glycogen synthase kinases ( e . g ., gsk1 - 5 ), p21 - activated kinases ( e . g ., pak1 - 7 ), serum - and glucocorticoid - induced kinases ( e . g ., sgk1 - 3 ), 14 - 3 - 3 proteins ( e . g ., 14 - 3 - 3α , β , γ , δ , ε , ζ ), amp kinases ( e . g ., ampk1 - 2 ), aurora a kinase , aurora b kinase , checkpoint kinases ( e . g ., chk1 - 4 ), cytosolic protamine kinase , nemo - like kinase , nima - related kinases ( e . g ., nek1 - 12 ), phosphoinositide - dependent protein kinases ( e . g ., pdk1 - 4 ), pim kinases ( e . g ., pim1 - 6 ), receptor interacting protein kinases ( e . g ., ripk1 - 5 ), rho - associated kinase ( e . g ., rock1 - 3 ), s6 kinases ( e . g ., p70 s6 kinase , rsk1 - 6 ), ste family kinases ( e . g ., stk1 - 6 ), thousand and one amino acid protein kinases ( e . g ., tao1 - 3 ), zip kinase . one of ordinary skill in the art can readily identify the recognition sequences for the aforementioned serine / threonine kinases and can thus incorporate said sequences into the phosphorylation - dependent protein domains disclosed herein to provide the desired serine / threonine kinase specificity . it is also contemplated that protein phosphatase - inducible domains are within the scope of the present disclosure . useful protein phosphatases include , for example , pp1 , pp2a - d , pp3 , pp4 , pp5 , pp6 . one of ordinary skill in the art can readily identify the recognition sequences for the aforementioned protein phosphatases and can thus incorporate said sequences into the phosphorylation - dependent protein domains disclosed herein to provide the desired protein phosphatase specificity . in addition to ef hand domains , other protein kinase - inducible and / or protein phosphatase - inducible domains are also possible so long as the domain contains a structurally significant glutamic acid or aspartic acid residue . for example , a zinc finger domain can be redesigned to bind terbium or other lanthanide metals , with metal binding by aspartic acid or glutamic acid residues . replacement of one or more of these aspartic acid or glutamic acid residues with phosphoserine or phosphothreonine . this domain may function as a protein kinase - inducible and / or protein phosphatase - inducible domain . a phosphorylation - dependent protein domain comprising a glutamic acid or aspartic acid residue replaced with a serine or threonine residue can be produced by any technique known in the art to synthesize polypeptides . techniques for chemical synthesis of polypeptides are well known in the art ( see , e . g ., [ 22 ]). examples of techniques for biochemical synthesis involving the introduction of a nucleic acid into a cell and expression of nucleic acids are also well known in the art ( see , e . g ., [ 23 - 24 ]). another exemplary technique , described in u . s . pat . no . 5 , 304 , 489 , incorporated herein by reference , is the use of transgenic mammals having mammary gland - targeted mutations which result in the production and secretion of synthesized peptides in the milk of the transgenic mammal . a further aspect is for isolated nucleotide sequences which encode amino acid sequences comprising the phosphorylation - dependent protein domains described herein . because of “ codon degeneracy ”, i . e ., divergence in the genetic code permitting variation of the nucleotide sequence without affecting the amino acid sequence of an encoded polypeptide , the present disclosure thus relates to any nucleotide sequence that encodes an amino acid sequence comprising , consisting essentially of , or consisting of a phosphorylation - dependent protein domain described herein , for example as set forth in the amino acid sequences disclosed herein . the skilled artisan is well aware of the “ codon - bias ” exhibited by a specific host cell in usage of nucleotide codons to specify a given amino acid . therefore , when synthesizing a gene for improved expression in a host cell , it is desirable to design the gene such that its frequency of codon usage approaches the frequency of preferred codon usage of the host cell . also contemplated are isolated nucleotide sequences complementary to the nucleotide sequences which encode the phosphorylation - dependent protein domains described herein . expression of a nucleotide sequence may be accomplished by first constructing a chimeric gene in which a coding region is operably linked to at least one promoter capable of directing expression of the gene . for convenience , the chimeric gene may comprise promoter sequences and translation leader sequences derived from the same genes . 3 ′ non - coding sequences encoding transcription termination signals should also be provided . the instant chimeric gene may also comprise one or more introns in order to facilitate gene expression . a plasmid vector comprising the instant chimeric gene can then be constructed . the choice of plasmid vector is dependent upon the method that will be used to transfect host cells . the skilled artisan is well aware of the genetic elements that must be present on the plasmid vector in order to successfully transform , select , and propagate host cells containing the chimeric gene . the skilled artisan will also recognize that different independent transformation events will result in different levels and patterns of expression ( see , e . g ., [ 25 - 26 ]), and thus that multiple events must be screened in order to obtain lines displaying the desired expression level and pattern . such screening may be accomplished by southern analysis of dna , northern analysis of mrna expression , western analysis of protein expression , or phenotypic analysis . for some applications , it may be useful to direct the amino acid sequence comprising , consisting essentially of , or consisting of a phosphorylation - dependent protein domain to different cellular compartments or to facilitate its secretion from the cell . therefore , the chimeric gene described above may be further supplemented by altering the coding sequences to encode the amino acid sequence comprising , consisting essentially of , or consisting of a phosphorylation - dependent protein domain with appropriate intracellular targeting sequences such as transit sequences [ 27 ], signal sequences or sequences encoding endoplasmic reticulum localization [ 28 ], or nuclear localization signals [ 29 ] added and / or with targeting sequences that are already present removed . while the references cited give examples of each of these , the list is not exhaustive and , thus , other targeting signals of utility may be useful in connection with the present disclosure . in one embodiment , the kinase - inducible domain peptides disclosed herein comprise an expressible sequence , potentially enabling their use as genetically encoded tags of protein kinase activity . in one aspect , the design comprises an ef hand consensus sequence , a tryptophan at residue 9 of formula ( i ) to sensitize lanthanide luminescence , and a recognition sequence of a serine / threonine kinase . the ef hand domain can , e . g ., have the amino acid sequence set forth in seq id no : 1 , seq id no : 3 , seq id no : 5 , seq id no : 8 , seq id no : 9 , seq id no : 10 seq id no : 11 , seq id no : 12 , seq id no : 13 , seq id no : 14 , seq id no : 15 , seq id no : 16 , seq id no : 17 , seq id no : 18 , seq id no : 19 , seq id no : 20 , seq id no : 21 , seq id no : 22 , seq id no : 23 , seq id no : 24 , seq id no : 25 , seq id no : 26 , seq id no : 27 , seq id no : 28 , seq id no : 29 , seq id no : 30 , seq id no : 31 , seq id no : 32 , seq id no : 33 , seq id no : 34 , seq id no : 35 , seq id no : 36 , seq id no : 37 , seq id no : 38 , seq id no : 39 , seq id no : 40 , or seq id no : 41 . the sequences , including several sequences in series , can be incorporated as an n - terminal or c - terminal extension to an encoded protein sequence , on a plasmid or stably incorporated into a host genome . in one example , the sequence is incorporated as a fusion protein as a c - terminal sequence on glutathione s - transferase . in another example , the sequence is incorporated as a fusion protein as a c - terminal sequence on green fluorescence protein . in another example , the sequence is incorporated as a fusion protein with c - jun , to enable subcellular targeting of the protein kinase - inducible domain . according to another aspect , methods of screening for kinase activity are provided . one method of identifying protein kinase activity relates to a cell - based assay comprising ( a ) providing a host cell with a polypeptide comprising a protein kinase - inducible domain having a structurally significant glutamic acid or aspartic acid residue replaced with a serine or threonine residue ; and ( b ) identifying protein kinase activity by detecting phosphorylation of the replaced serine or threonine residue . in one embodiment , the host cell is transfected with a polynucleotide encoding the polypeptide comprising a protein kinase - inducible domain having a structurally significant glutamic acid or aspartic acid residue replaced with a serine or threonine residue . transfection methods are well known to those of ordinary skill in the art . in another embodiment , the polypeptide comprising a protein kinase - inducible domain having a structurally significant glutamic acid or aspartic acid residue replaced with a serine or threonine residue is inserted into the host cell by any method as known in the art , e . g ., by injection or liposomal delivery . the host cell can be , for example , of mammalian origin , preferably of human origin . suitable methods of kinase activity detection are disclosed elsewhere herein . additionally , other kinase activity detection methods are well known to those of ordinary skill in the art . cell - based methods of screening for phosphatase activity are also provided . one method of identifying protein phosphatase activity comprises ( a ) providing a host cell with a polypeptide comprising a protein phosphatase - inducible domain having a structurally significant glutamic acid or aspartic acid residue replaced with a phosphoserine or phosphothreonine residue ; and ( b ) identifying protein phosphatase activity by detecting dephosphorylation of the replaced phosphoserine or phosphothreonine residue . cell - free assays can also be utilized to identify kinase or phosphatase activity . one aspect thus relates to a method of identifying protein kinase activity comprising : ( a ) providing a polypeptide comprising a protein kinase - inducible domain having a structurally significant glutamic acid or aspartic acid residue replaced with a serine or threonine residue ; ( b ) contacting the polypeptide of ( a ) with a suspected protein kinase ; and ( c ) detecting phosphorylation of the serine or threonine residue of the polypeptide of ( a ). another aspect relates to a method of identifying protein phosphatase activity comprising : ( a ) providing a polypeptide comprising a protein kinase - inducible domain having a structurally significant glutamic acid or aspartic acid residue replaced with a phosphoserine or phosphothreonine residue ; ( b ) contacting the polypeptide of ( a ) with a suspected protein phosphatase ; and ( c ) detecting dephosphorylation of the serine or threonine residue of the polypeptide of ( a ). another aspect is for screening assays used to identify inhibitors of kinase or phosphatase activity . one embodiment is for a cell - based assay comprising ( a ) providing a host cell with a polypeptide comprising a protein kinase - inducible domain having a structurally significant glutamic acid or aspartic acid residue replaced with a serine or threonine residue ; ( b ) introducing into the host cell a test compound ; ( c ) activating in the host cell a protein kinase which recognizes the protein kinase - inducible domain ; and ( d ) measuring the phosphorylation of the replaced serine or threonine residue ; whereby inhibition of phosphorylation of the replaced serine or threonine residue is indicative of the test compound being a protein kinase inhibitor . cell - based assays for identifying phosphatase inhibitors are also provided . one embodiment is for a method of screening for a protein phosphatase inhibitor comprising : ( a ) providing a host cell with a polypeptide comprising a protein phosphatase - inducible domain having a structurally significant glutamic acid or aspartic acid residue replaced with a phosphoserine or phosphothreonine residue ; ( b ) introducing into the host cell a test compound ; ( c ) activating in the host cell a protein phosphatase which recognizes the protein phosphatase - inducible domain ; and ( d ) measuring the phosphorylation of the replaced phosphoserine or phosphothreonine residue ; whereby inhibition of dephosphorylation of the replaced phosphoserine or phosphothreonine residue is indicative of the test compound being a protein phosphatase inhibitor . alternatively , cell - free assays can be used to identify kinase or phosphatase inhibitors . one embodiment is for a method of screening for a protein kinase inhibitor comprising : ( a ) providing a polypeptide comprising a protein kinase - inducible domain having a structurally significant glutamic acid or aspartic acid residue replaced with a serine or threonine residue ; ( b ) contacting the polypeptide of ( a ) with : ( 1 ) a protein kinase having a kinase recognition domain on polypeptide of ( a ) and ( 2 ) a test compound suspected of being a kinase inhibitor ; and ( c ) detecting phosphorylation of the serine or threonine residue of the polypeptide of ( a ), whereby inhibition of phosphorylation of the replaced serine or threonine residue is indicative of the test compound being a protein kinase inhibitor . another embodiment is for a method of screening for a protein phosphatase inhibitor comprising : ( a ) providing a polypeptide comprising a protein kinase - inducible domain having a structurally significant glutamic acid or aspartic acid residue replaced with a phosphoserine or phosphothreonine residue ; ( b ) contacting the polypeptide of ( a ) with : ( 1 ) a protein phosphatase having a phosphatase recognition domain on polypeptide of ( a ) and ( 2 ) a test compound suspected of being a phosphatase inhibitor ; and ( c ) detecting phosphorylation of the phosphoserine or phosphothreonine residue of the polypeptide of ( a ), whereby inhibition of dephosphorylation of the replaced phosphoserine or phosphothreonine residue is indicative of the test compound being a protein phosphatase inhibitor . in some embodiments , identification of kinase or phosphatase inhibitors can be accomplished through the use of high - throughput screening assays to screen large number of compounds . another aspect pertains to novel inhibitors identified by the above - described screening assays . accordingly , it is within the scope of this disclosure to use as a kinase or phosphatase inhibitor a compound identified herein . protein kinase - inducible domains and / or protein phosphatase - inducible domains bind other metals , including the other lanthanide metals , the metal gadolinium is used in magnetic resonance imaging . the binding of ligands to gadolinium changes the imaging properties of the gadolinium . binding of gadolinium to peptides and proteins can be assessed by magnetic resonance imaging [ 48 ]. protein kinase - inducible domains and / or protein phosphatase - inducible domains can be used for imaging of kinase activity and / or phosphatase activity by magnetic resonance imaging . all of the compositions and methods disclosed and claimed herein can be made and executed without undue experimentation in light of the present disclosure . it will be apparent to those of skill in the art that variations may be applied to the compositions and methods and in the steps or in the sequence of steps of the method described herein without departing from the concept , spirit , and scope of the invention . more specifically , it will be apparent that certain agents which are chemically or biologically related may be substituted for the agents described herein while the same or similar results would be achieved . all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the spirit , scope , and concept of the invention as defined by the appended claims . the present invention is further defined in the following examples . it should be understood that these examples are given by way of illustration only . from the above discussion and these examples , one skilled in the art can ascertain the preferred features of this invention , and without departing from the spirit and scope thereof , can make various changes and modifications of the invention to adapt it to various uses and conditions . amino acids and resins for peptide synthesis were purchased from novabiochem . hbtu was purchased from senn chemicals . diisopropylethylamine ( dipea ) was purchased from aldrich . dimethyl formamide ( dmf ), methylene chloride , and trifluoroacetic acid ( tfa ) were purchased from acros . other compounds were purchased from acros unless otherwise indicated . peptide synthesis was carried out on a rainin ps3 automated peptide synthesizer . peptide stock solutions were prepared in ultrapure water purified by a millipore synergy 185 water purification system with a simpak ® 2 cartridge . peptide concentrations were determined by uvnis based on tryptophan absorbance ( ε = 5690 m − 1 cm − 1 at 280 nm in water ) on a perkinelmer lambda 25 spectrometer . peptide stock solutions were stored at − 10 ° c . postsynthetic modification reactions were performed in capped disposable fritted columns ( image molding ). all compounds were used as purchased with no additional purification . terbium ( iii ) chloride stocks were freshly prepared from hexahydrate salts ( aldrich ). 500 mm hepes buffer ph 7 . 8 was prepared from hepes ( acros ) and adjusted to ph 7 . 8 with a 1 m naoh solution . nacl ( 1 m ) and cacl 2 ( 1 m ) solutions were prepared from the corresponding salts ( acros ). peptides were synthesized using standard fmoc solid phase peptide synthesis with rink amide resin ( 0 . 25 mmol ). the resin was swelled in dmf ( 5 min ) prior to the start of the synthesis . amino acid couplings were performed using fmoc amino acids ( 1 mmol , 4 equiv ) and hbtu ( 1 mmol , 4 equiv ). the following steps were used for each cycle of peptide synthesis : ( 1 ) removal of the fmoc group with 20 % piperidine in dmf , 3 × 5 min ; ( 2 ) resin wash ( dmf , 5 × 1 min ); ( 3 ) amide coupling ( amino acid , hbtu and 0 . 05 m dipea in dmf , 50 min ); ( 4 ) resin wash ( dmf , 3 × 1 min ). trityl - protected serine was incorporated at the phosphorylation site to allow for site - specific phosphorylation . after addition of the final residue , the n - terminal fmoc group was removed ( 20 % piperidine in dmf , 3 × 5 mins ) and the amino terminus acetylated ( 10 % acetic anhydride in pyridine , 5 mins ). the resin was washed with dmf ( 6 ×) and ch 2 cl 2 ( 3 ×). non - phosphorylated peptides were subjected to cleavage from resin and deprotection for 3 h ( tfa : thioanisole : ethanedithiol : phenol : water , 84 : 4 : 4 : 4 : 4 ). the solutions were concentrated by evaporation under nitrogen and the peptides were precipitated with ether . the precipitate was dissolved in water , the resulting solution was filtered , and the peptides was purified by reverse phase hplc ( vydac semipreparative c18 , 10 × 250 mm , 5 μm particle size , 300 å pore ) using a linear gradient of 0 - 40 % buffer b ( 80 % mecn , 20 % h 2 o , 0 . 05 % tfa ) in buffer a ( 98 % h 2 o , 2 % mecn , 0 . 06 % tfa ) over 60 minutes . peptides were purified to homogeneity , as indicated by the presence of a single peak on reinjection on analytical hplc ( microsorb mv c18 , 4 . 6 × 250 mm , 3 - 5 μm particle size , 100 å pore ). peptides were characterized by esi - ms ( negative icon mode ) on an lcq advantage ( finnigan ) mass spectrometer . peptides were chemically phosphorylated on resin by the following procedure : ( 1 ) deprotection of the trityl group with 2 % tfa / 5 % triethylsilane ( tes )/ 93 % ch 2 cl 2 , 3 × 1 min , or until the flow - through solution was clear ; ( 2 ) phosphorylation was performed under nitrogen by addition to the resin of tetrazole ( 1 . 35 mmol ; 3 ml of 3 % tetrazole solution in mecn ) ( transgenomics ) and o , o - dibenzyl - n , n - diisopropylphosphoramidite ( 500 μl , 1 . 52 mmol ) ( fluka ), and allowed to react for 3 h with gentle mixing on a barnstead - thermoline labquake rotary shaker . the solution was removed and the resin washed with dmf ( 3 ×) and ch 2 cl 2 ( 3 ×); ( 3 ) oxidation was performed with t - butyl hydroperoxide ( 2 ml of a 3 m solution in ch 2 cl 2 ) and allowed to react with mixing for 30 mins . the solution was removed and the resin washed with dmf ( 3 ×), meoh ( 3 ×), and ether ( 3 ×). the phosphorylated peptides were purified and characterized as described above for non - phosphorylated peptides . fluorescence spectra were collected on a photon technology international fluorescence spectrometer model qm - 3 / 2003 with a cw source and a hamamatsu r928 pmt . all experiments were conducted with an excitation wavelength of 280 nm . 6 nm excitation and emission slit widths were used unless otherwise indicated . all spectra were acquired at room temperature , collecting data every 1 nm with a scan rate of 1 nm per second . at least 3 independent binding titrations were conducted for each peptide . all spectra are uncorrected and have not been normalized , and only representative ( median ), non - averaged spectra are shown , unless otherwise indicated . all fluorescence experiments were conducted using a 495 nm highpass filter ( model 495fg03 - 25 am - 53074 ; andover corporation , andover , n . h .) on the emission monochromator . peptide solutions were prepared by dilution of stock solutions into 5 mm hepes buffer ( ph 7 . 8 ) with 100 mm nacl . spectra were acquired in 10 mm quartz fluorescence cells ( starna ). tb 3 + titrations were conducted by dilution of a tb 3 + solution into a peptide solution as described above . each individual emission spectrum represents an independently prepared solution of peptide and metal . the tb 3 + emission band at 544 nm was used to evaluate metal binding . a series of kinase - inducible domain ( pkid ) peptides were synthesized which comprised an ef hand consensus sequence , a tryptophan at residue 7 to sensitize lanthanide emission , and the recognition sequence of a kinase important in intracellular signaling ( see fig1 ). as initial targets , applicants synthesized peptides containing the minimal recognition sequences , which include basic or helix - breaking residues that could potentially disrupt lanthanide binding and include residues n - terminal and c - terminal to the target serine , provide a significant test of the generality of the design . protein kinase a ( pka ) and pka reaction buffer were purchased from new england biolabs . pka reaction mixtures were prepared to a final volume of 25 μl as follows : stock solutions were mixed to yield final concentrations of 2 . 4 mm atp ( 6 μl of 10 mm atp ( alexis biochemicals )), 1 . 2 × pka buffer ( 3 μl of 10 × buffer ), and 240 μm non - phosphorylated pkid - pka ( 16 μl of a 370 μm stock solution ). after incubation at 30 ° c . for 5 min , 1 . 5 μl of pka enzyme solution ( 3 . 75 units ) was added to start the reaction . after 12 - 22 hours , the reaction mixture was analyzed by hplc , fluorescence , and esi - ms ( see fig3 and table 2 ). the kinase reaction mixtures ( 25 μl , 240 μm peptide ) were diluted with 1 ml of a solution containing 5 mm hepes buffer ( ph 7 . 8 ) 100 mm nacl and 50 μm tb 3 + and analyzed by fluorescence ( see fig4 d ) as described previously , except that 10 nm slit widths were used . fluorescence emission spectra revealed that the non - phosphorylated peptides bound tb 3 + poorly ( see fig4 ), displaying very weak terbium luminescence , consistent with the critical role of the glu12 in metal binding . in contrast , all phosphorylated peptides displayed strong fluorescence emission in the presence of tb 3 + , indicating the formation of a phosphopeptide - metal complex . notably , the fluorescence change upon phosphorylation by protein kinase a ( see fig4 d ) was similar to that observed in non - expressible kinase sensors , and was significantly greater than that of any expressible kinase sensor ( for a recent review , see [ 30 ]; for leading references see [ 31 - 45 ]). phosphorylation of pkid - pka by protein kinase a in hela nuclear extract protein kinase a ( pka ) and pka reaction buffer were purchased from new england biolabs . in vitro transcription grade helascribe ® nuclear extract was purchased from promega ( storage buffer : 40 mm tris - hcl ( ph 7 . 8 at 25 ° c . ), 25 % glycerol , 0 . 1 m kcl , 0 . 2 mm edta , 0 . 5 mm pmsf , 0 . 5 mm dtt ). reaction mixtures were prepared to a final volume of 25 μl as follows : stock solutions were mixed to yield final concentrations of 5 mm atp ( 7 . 5 μl of 20 mm atp ( alexis biochemicals )), 1 . 2 mg / ml hela nuclear extract ( 2 μl of helascribe ® hela nuclear extract ( 13 . 8 mg / ml )), 1 . 2 × pka buffer ( 3 μl of 10 × buffer ), and 500 μm non - phosphorylated pkid - pka . after incubation at 30 ° c . for 5 min , 3 μl of pka enzyme solution ( 7 . 6 units ) was added to start the reaction . after specified reaction times , the reaction mixture was analyzed by fluorescence ( see fig5 , left ). the kinase reaction mixtures ( 25 μl , 500 μm peptide ) were diluted with 200 μl of a solution containing 5 mm hepes buffer ( ph 7 . 8 ), 100 mm nacl and 100 μm tb 3 + and analyzed by fluorescence as described previously , using 10 nm slit widths . the fluorescence spectra were background corrected . each time point represents an independent experiment . data represent the average of three independent trials for each time point . error bars indicate standard error . phosphorylation of pkid - pka in hela nuclear extract in the absence of added kinase was also examined . reaction mixtures were prepared as described previously to a final volume of 25 μl , but protein kinase a was not added . after addition of atp and incubation for the indicated times , the reaction mixtures ( 25 μl , 500 μm peptide ) were diluted with 200 μl of a solution containing 5 nm hepes buffer ( ph 7 . 8 ), 100 mm nacl and 100 μm tb 3 + and analyzed by fluorescence as described previously . pkid - pka was phosphorylated by endogenous kinase present within the hela extracts to approximately 10 % conversion as determined by fluorescence and hplc ( see fig5 , right ). kinase specificity for protein kinase - inducible domain peptides was examined by incubation of protein kinase a with pkid - pka , pkid - pkc and pkid - erk . experiments were conducted with 2 . 4 mm atp ( 3 μl of freshly prepared 20 mm atp ), pka buffer ( 3 μl of 10 × buffer ), and peptide ( 200 μm ) with water in 25 μl final reaction volume . after incubation at 35 ° c . for 5 min , pka enzyme solution ( 1 μl , 2 . 5 units ) was added to start the reaction . after 12 - 14 hrs at 35 ° c ., the reaction mixture was analyzed by fluorescence , hplc and esi - ms . the kinase reaction mixtures were analyzed by fluorescence by diluting the reaction mixture with 1 ml of a solution containing 5 mm hepes buffer ( ph 7 . 8 ), 100 mm nacl , and 50 μm tb 3 + , and the resulting solution analyzed by fluorescence . fluorescence experiments were conducted with 10 nm slit widths and a 495 nm highpass filter on the emission monochromator . fluorescence data ( fig7 ) represent the average of four independent trials . error bars indicate standard error . the solutions used for the fluorescence analysis were analyzed by hplc to quantify the extent of peptide phosphorylation . pkid - pka was enzymatically phosphorylated to & gt ; 95 % conversion in 12 hrs by pka ( fig8 ), while under identical conditions pkid - erk ( fig9 ) and pkid - pkc ( fig1 ) showed no evidence of phosphorylation . experiments with different peptides were conducted in parallel to assure that the enzyme activity was comparable for enzymatic reactions with different peptides . to determine dissociation constants for tb 3 + - peptide complexes , titrations were conducted in solutions of 5 mm hepes ( ph 7 . 8 ) and 100 mm nacl , with 10 nm emission and excitation slit widths . all fluorescence experiments were conducted using a 495 nm highpass filter ( model 495fg03 - 25 am - 53074 ; andover corporation , andover , n . h .) on the emission monochromator . all tbcl 3 solutions were standardized by titration with a standard solution of edta ( 1 mm ) in the presence of xylenol orange indicator ( 10 μm ) and sodium acetate buffer ( ph 6 . 0 , 10 mm ). 500 μl of the 1 mm tb 3 + stock solution was diluted to 1 ml to make a 0 . 5 mm solution and edta ( 1 mm ) was added ( approximately 500 μl ) until the end point was reached ( see fig1 - 13 ). the solutions were prepared as serial dilutions of tb 3 + , from 3 . 3 μm to 450 μm tb 3 + , and the fluorescence emission scan of each solution was acquired . data points at the emission maximum of 544 nm were plotted against tb 3 + concentration to calculate the final k d . data points indicate the average of at least three independent titrations . error bars indicate standard error . the data were fit to equation ( 1 ) using a non - linear least squares fitting algorithm ( kaleidagraph version 3 . 6 , synergy software ), where q = fluorescence , q o = fluorescence of the apopeptide , q c = fluorescence of peptide - metal complex , m t = total metal concentration , k d = dissociation constant and p t = total peptide concentration ( 10 μm ). dissociation constants in the presence of 2 mm mg 2 + or 100 μm ca 2 + were measured for pkid - pka peptides to study the effect of these metals on tb 3 + - peptide complex formation . q = q o + ( q c - q o ) [ ( m t + k d + p t ) - ( m t + p t + k d ) 2 - 4 ( p t m t ) ] 2 p t ( 1 ) see table 3 for dissociation constants for peptide - tb 3 + complexes in aqueous solutions of 5 mm hepes ( ph 7 . 8 ) and 100 mm nacl ( ps indicates phosphoserine ). dissociation constants of the non - phosphorylated peptides were calculated by defining the maximum fluorescence of the non - phosphorylated peptide - tb 3 + complex as equal to the maximum fluorescence of the phosphorylated peptide - tb 3 + complex : q c ( non - phosphorylated peptide )= q c ( phosphorylated peptide ), with q c = the calculated fluorescence of the fully bonded phosphopeptide - tb 3 + complex . although the assumption of similar maximum fluorescence intensities of the tb 3 + complexes of the non - phosphorylated and phosphorylated peptides may not be valid , it provides a measure of relative tb 3 + fluorescence of the phosphorylated and non - phosphorylated peptides . competition experiments were used to confirm site - specific lanthanide binding and to address whether pkid peptides are a general phosphorylation - dependent lanthanide - binding motif . in order to determine whether tb 3 + binding is site - specific , competition experiments were performed with ho 3 + . ho 3 + solutions were prepared from hydrates of the chloride salts in ultrapure water . the phosphorylated pkid - pkc peptide was tested for ho 3 + binding by addition of aliquots of ho 3 + to a solution containing 10 μm phosphorylated pkid - pkc and 10 μm tb 3 + . pkid - tb 3 + - ho 3 + solutions were allowed to equilibrate for 2 minutes . fluorescence experiments were conducted using a 495 nm highpass filter ( model 495fg03 - 25 am - 53074 ; andover corporation , andover , n . h .) on the emission monochromator and 8 nm slit widths . ho 3 + binding to the peptide is observed as a loss of tb 3 + luminescence consistent with formation of a pkid - pkc - ho 3 + complex , as is seen in fig1 . tb 3 + binding of pkid - pka peptides in the presence of 2 mm mg 2 + tb 3 + binding experiments with the pkid - pka peptides were conducted in the presence of 2 mm mg 2 + to measure the effect of cellular concentrations of mg 2 + on peptide - tb 3 + complex stability . in the presence of 2 mm mg 2 + , the k d for phosphorylated pkid - pka decreased slightly ( 1 . 3 - fold ). see fig1 . in contrast , tb 3 + binding was not observed for the non - phosphorylated peptide pkid - pka in the presence of mg 2 + . tight peptide - tb 3 + complex formation is dependent on phosphorylation and is not affected by 2 mm mg 2 + . tb 3 + binding of pkid - pka peptides in the presence of 100 μm ca 2 + the binding of tb 3 + to phosphorylated pkid - pka in the presence of 100 μm ca 2 + was examined . the fluorescence emission spectra of 10 μm phosphorylated pkid - pka were analyzed in the absence and presence of 100 μm ca 2 + . samples were prepared and spectra were collected as described previously , using 10 nm slit widths . the dissociation constant of the phosphopeptide - tb 3 + complex did not significantly change in the presence of 100 μm ca 2 + ( see fig1 ). metal binding to phosphorylated pkid - pka was examined by circular dichroism ( cd ). cd spectra were collected at 25 ° c . on a jasco j - 810 spectropolarimeter in a 2 mm quartz cell ( starna ) with 100 μm phosphorylated pkid - pka in h 2 o with 10 mm hepes ( ph 7 . 8 ) and 10 mm nacl in the absence and presence of 500 μm tb 3 + or 500 μm la 3 + . data were collected every 1 nm with an averaging time of 4 s , 2 accumulations , and a 2 nm bandwidth . error bars are shown and indicate standard error . data represent the average of three independent trials . see fig1 . metal binding was further characterized by nmr . nmr samples of phosphorylated pkid - pkc were prepared as 1 - 1 . 5 mm peptide solutions containing 10 mm deuterated acetate buffer ( ph 6 . 1 ), 1 . 5 mm tsp [ d4 ] ( icn biomedicals ), 100 mm nacl , and 10 % d 2 o and 90 % h 2 o in a total volume of 400 μl . nmr experiments were conducted in the absence of metal , in the presence of two paramagnetic metals , tb 3 + ( fig1 ) and ce 3 + ( fig1 ), and in the presence of the diamagnetic metal la 3 + ( fig2 ) to evaluate changes due to metal - phosphopeptide complex formation . all metals were used as the metal ( iii ) chloride salts . nmr spectra were collected on a brüker avc 600 mhz nmr spectrometer equipped with a triple - resonance cryoprobe . 1 - d spectra and tocsy spectra were collected with water suppression using a watergate w5 pulse sequence with gradients ( bruker pulse programs zggpw5 and mlevgpphw5 , respectively ). 1 h - 15 n hsqc experiments were conducted with watergate water suppression ( brüker pulse program hsqcfpf3gpphwg ). 1 - d spectra were collected with a sweep width of 7183 hz , 8192 data points , and a relaxation delay of 3 s . tocsy spectra were acquired with sweep widths of 7183 hz in t 1 and t 2 , with 600 × 2048 complex data points , 2 scans per t 1 increment , and a relaxation delay of 2 s . 1 h - 15 n hsqc experiments were conducted using the peptides with natural abundance 15 n , with sweep widths of 1824 hz in t 1 and 5387 hz in t 2 , with 80 × 1024 complex data points , 128 - 192 scans per t 1 increment , and a relaxation delay of 2 s ( see fig2 ). addition of paramagnetic tb 3 + to phosphorylated pkid - pkc resulted in the disappearance of most signals , consistent with pkid - pkc - tb 3 + complex formation and tb 3 + - induced paramagnetic relaxation . 1 h - 15 n hsqc spectra ( see fig2 , fig2 ) of phosphorylated pkid - pkc in the absence and in the presence of diamagnetic la 3 + indicated that the metal induced significant changes in chemical shifts , particularly for metal - binding residues , consistent with peptide - metal complex formation . signarvic r s & amp ; degrado w f , j . mol . biol . 334 : 1 - 12 ( 2003 ). siedlecka m et al ., proc . natl . acad . sci . usa 96 : 903 - 08 ( 1999 ). kovacic r t et al ., j . am . chem . soc . 125 : 6656 - 62 ( 2003 ). lee v h l , “ peptide and protein drug delivery ”, new york , n . y ., m . dekker ( 1990 ). ausubel f m et al ., “ current protocols in molecular biology ”, john wiley ( 1987 - 1998 ). sambrook j et al ., “ molecular cloning , a laboratory manual ”, 2d edition , cold spring harbor laboratory press ( 1989 ). almeida e r p et al ., mol . gen . genet . 218 : 78 - 86 ( 1989 ). chrispeels m j , annu . rev . plant physiol . plant mol . biol . 42 : 21 - 53 ( 1991 ). wright d et al ., proc . natl . acad . sci . usa 78 : 6048 - 50 ( 1981 ). cotton g j & amp ; muir t w , chem . biol . 7 : 253 - 61 ( 2000 ). zhang j et al ., proc . natl . acad . sci . usa 98 : 14997 - 15002 ( 2001 ). ting a y et al ., proc . natl . acad . sci . usa 98 : 15003 - 08 ( 2001 ). chen c a et al ., j . am . chem . soc . 124 : 3840 - 41 ( 2002 ). veldhuyzen w f et al ., j . am . chem . soc . 125 : 13358 - 59 ( 2003 ). shults m d & amp ; imperiali b , j . am . chem . soc . 125 : 14248 - 49 ( 2003 ). wang q & amp ; lawrence d s , j . am . chem . soc . 127 : 7684 - 85 ( 2005 ) rigden d j & amp ; galperin m y , j . mol . biol . 343 : 971 - 84 ( 2004 ) | 2 |
the present invention will be better understood when the design of the prior art is first discussed . referring now to fig1 - 3 , two mine landing orientations are shown in fig1 . the first position &# 34 ; a &# 34 ; of the mine is shown with the round cover 10 of the mine disposed in an &# 34 ; up &# 34 ; position relative to ground surface 11 . the second position &# 34 ; b &# 34 ; is shown with the flat cover 12 in an &# 34 ; up &# 34 ; position . the primary mode explosive train of the prior art comprises a microdetonator 14 , located in microdetonator housing counterbore 15 , transversely disposed in housing body member 16 . microdetonator 14 is axially aligned with the input side 18 of transfer lead charge 20 and communicates therewith through microdetonator body housing orfice 22 and axially aligned tubular transfer lead housing input orifice 24 . transfer lead charge 20 is transversely positioned in transfer lead charge housing 26 which is in turn fixedly attached to transfer lead charge tubular member 28 , located in body housing central bore 29 , by groove pin 30 . transfer lead charge 20 output communicates with the input sides 32 and 34 of two mdf angularly positioned booster charges 32 &# 39 ; and 34 &# 39 ;. booster charges 32 &# 39 ; and 34 &# 39 ; communicate with the output side 36 of transfer lead charge 20 through selector chamber 38 , housing blow hole 40 and transfer lead tubular housing output orifice 42 . in operation of the prior art shown in fig1 - 3 , the mine cover that is &# 34 ; up &# 34 ; has to be ejected from a miznay - schardin dished liner plate located in the mine , not shown , in order for the mine to have maximum terminal effect against the target . an interrupter ball member 44 located in selector chamber 38 drops by gravity toward the ground surface 11 covering the input side of lower mdf booster 34 &# 39 ; of fig2 or 32 &# 39 ; of fig3 . the selected mdf booster initiates removal of either covers 10 or 12 by igniting either fuze 46 and 48 respectively leading to an ejection charge , not shown , attached to covers 10 or 12 . the above sequence is initiated when microdetonator 14 is electrically activated by a target sensing means located in the mine and which is not shown in the drawing . the microdetonator 14 initiates transfer lead charge 20 which blasts into the selector chamber 38 firing the microdetonator booster 32 &# 39 ; or 34 &# 39 ; uncovered by the ball 44 to eject either the upper cover 10 or 12 . the problem with the prior art design , shown in fig2 and 3 , was the extremely low order of reliability for the reason previously aforementioned . the distance designated by the letter &# 34 ; θ &# 34 ; is between the output side 36 of the transfer lead charge 20 and the input side 32 of the mdf booster 32 &# 39 ; and 34 &# 39 ; has been determined as being excessive and a contributing factor to poor reliability . referring now to the present invention as illustrated by fig4 and 5 the primary mode explosive train comprises a dual chamber mild detonating fuze housing 50 transversely fixedly disposed in a second transverse counterbore hole 52 of body housing member 54 . a pair of parallel aligned first and second mdf boosters 56 and 58 respectively are positioned one above each other in booster bores 57 and 59 in a rear section of the mdf housing 50 . a stepped interrupted disc member 60 has larger diameter section 62 slidably positioned in chamber slot 64 . the small diameter section 66 protrudes through chamber slot 64 and is slidably guided thereby while positioned in housing blow hole 68 . an elongated transfer lead charge 70 is positioned in transverse lead housing 26 so that it is in axial alignment with housing blowhole 68 and body housing orifice 22 , and microdetonator 14 . the output side of microdetonator 14 , located in a first transverse counterbore 15 , communicates with the input side 72 via body housing orifice 22 and input orifice 24 of the transfer lead charge tubular member 28 . transfer lead charge housing 26 is fixedly connected to the transfer lead charge tubular member 28 by thru groove pin 30 . lead charge tubular member 28 is proximately disposed in body housing central bore 29 so that output orifice 42 is axially aligned with housing blow hole 68 . in operation when the mine lands on the ground the stepped interrupter 60 drops by gravity toward the ground , covering the booster charge 58 and uncovering the upper booster charge 56 . when the microdetonator 14 is electrically signaled by a target sensing device located in the mine , and not shown , the microdetonator 14 initiates the elongated transfer lead charge 70 which in turn blasts through the output orifice 42 of tubular lead housing 28 and housing blow hole 68 into the selector chamber slot 68 , firing the upper mdf booster charge 56 uncovered by interrupter 60 through a reduced standoff gap θ &# 39 ;. booster 56 causes ejection of round mine cover 10 , shown in position &# 34 ; a &# 34 ; of fig1 by igniting ejection charge lighting fuze 46 . the lower mdf booster 58 of fig4 is adequately covered by the flat stepped interrupter 60 and consequently will not be initiated . fig5 shows the operation of the interrupter 60 when the mine &# 39 ; s landing orientation is as shown in position &# 34 ; b &# 34 ; of fig1 . under the latter condition the mdf booster 58 is uncovered and the mdf booster 56 is covered . the firing of upper mdf booster 58 by the transfer lead charge 70 in this instance ignites ejection charge lighting fuze 48 ejecting the flat mine cover 12 . the gap θ &# 39 ; between the output side 74 and the input side of the selected mdf booster 56 or 58 has been substantially reduced in the present design of fig4 and 5 to significantly improve the reliability of the directional fuze selector apparatus by providing a more direct path for the transfer lead charge blast through the dual chamber slot 64 and housing blow hole 68 into the input side 76 of the selected mdf booster 56 or 58 . the reliability of the present invention is also improved by the flat stepped interrupter disc member 60 by providing a more positive cover for the unselected mdf booster charge . while there has been described and illustrated specific embodiments of the invention , it will be obvious that various changes , modifications and additions can be made herein without departing from the field of the invention which should by limited only by the scope of the appended claims . | 5 |
referring now to fig1 , an apparatus for treating surfaces of wafer - shaped articles according to a first embodiment of the invention comprises an outer process chamber 1 , which is preferably made of aluminum coated with pfa ( perfluoroalkoxy ) resin . the chamber in this embodiment has a main cylindrical wall 10 , a lower part 12 and an upper part 15 . from upper part 15 there extends a narrower cylindrical wall 34 , which is closed by a lid 36 . a rotary chuck 30 is disposed in the upper part of chamber 1 , and surrounded by the cylindrical wall 34 . rotary chuck 30 rotatably supports a wafer w during use of the apparatus . the rotary chuck 30 incorporates a rotary drive comprising ring gear 38 , which engages and drives a plurality of eccentrically movable gripping members for selectively contacting and releasing the peripheral edge of a wafer w . in this embodiment , the rotary chuck 30 is a ring rotor provided adjacent to the interior surface of the cylindrical wall 34 . a stator 32 is provided opposite the ring rotor adjacent the outer surface of the cylindrical wall 34 . the rotor 30 and stator 32 serve as a motor by which the ring rotor 30 ( and thereby a supported wafer w ) may be rotated through an active magnetic bearing . for example , the stator 32 can comprise a plurality of electromagnetic coils or windings that may be actively controlled to rotatably drive the rotary chuck 30 through corresponding permanent magnets provided on the rotor . axial and radial bearing of the rotary chuck 30 may be accomplished also by active control of the stator or by permanent magnets . thus , the rotary chuck 30 may be levitated and rotatably driven free from mechanical contact . alternatively , the rotor may be held by a passive bearing where the magnets of the rotor are held by corresponding high - temperature - superconducting magnets ( hts - magnets ) that are circumferentially arranged on an outer rotor outside the chamber . with this alternative embodiment each magnet of the ring rotor is pinned to its corresponding hts - magnet of the outer rotor . therefore the inner rotor makes the same movement as the outer rotor without being physically connected . the lid 36 is of an improved design , and comprises an upper plate 50 formed from a composite fiber - reinforced material and a lower plate 60 that faces into the process chamber and is formed from a chemically - resistant plastic , which in this embodiment is ectfe . sandwiched between the upper plate 50 and lower plate 60 in this embodiment is a stainless steel plate 70 ( see fig3 ). as can be seen in fig3 , the lid 36 may further include an electrical heating layer 62 for heating the lower plate 60 to a temperature that prevents condensation of process vapors from occurring on the surface of plate 60 that faces into the process chamber . electrical heating layer 62 is preferably a silicone rubber heater . spacer plate 64 serves to maintain the heater layer 62 pressed into contact with lower plate 60 , as does the annular spacer 66 , which latter element is preferably formed from stainless steel . lid 36 may be secured to the process chamber by bolts ( not shown ) that pass through bores 58 . referring now to fig4 - 7 , the lower plate 60 of lid 36 is formed with a radially inwardly extending annular groove 65 that opens on the periphery of plate 60 . a ring 66 is fitted in the opening of that groove 65 , to form an annular chamber . upper openings in the plate 60 communicate with the annular chamber , and receive nozzles 54 that are attached to a gas supply so as to supply purge gas into the annular chamber . preferably there are at least three such nozzles 54 . purge gas exits the annular chamber through a much larger number of much smaller outlets 67 that extend from the annular chamber and open on the lower surface of lower plate 60 , which is a surface that faces inwardly of the closed process chamber when the lid is in place . as shown in fig6 , there are 120 outlets 67 in this embodiment , although the number of such outlets can of course be varied as desired to create a target gas flow profile . first additional gas outlets 63 also open on the lower surface of lower plate 60 , but are positioned radially inwardly of the annular chamber . outlets 63 are supplied by separate gas nozzles 57 . second additional gas outlets 67 also open on the lower surface of lower plate 60 , and , like the first additional outlets 63 , are positioned radially inwardly of the annular chamber . these second additional gas outlets 63 are likewise supplied by separate gas nozzles 59 . with reference to fig6 , it can be seen that the outlets 63 are moreover oriented so as to generate a rotating gas flow beneath said lid . in particular , the three outlets 63 together generate a flow of purge gas that rotates in a generally clockwise direction , as indicated by the circular arrow in fig6 . on the other hand , the stator 32 and rotor 30 operate to rotate the chuck in a counter - clockwise direction . the opposite directions of rotation as between the chuck and the flow of purge gas through outlets 63 has been found to provide an especially thorough and efficient purging of the chuck ambient within the closed process chamber , especially in the region above the wafer w . that effect can be further improved by the provision of the second additional outlets 69 , which direct their flow of purge gas radially outwardly of the lower plate 60 , yet are also positioned inwardly of the annular chamber formed in plate 60 . simulations were performed to compare the performance of the lid design as described herein with the purge ring of the commonly - owned copending application u . s . pub . no . 2013 / 0134128 . for wafers of 300 mm diameter rotated at speeds of 350 or 400 rpm , it was found that flow patterns of purge gas having improved velocity and uniformity could be obtained with the present design despite specifying much lower total flow rates of purge gas . for example , with total flow rate of gaseous nitrogen of 40 liters per minute ( lpm ) or 75 lpm , the flow pattern was improved in relation to the previous design at flow rates of 120 lpm . in the present design , a flow rate of 40 lpm is obtained by specifying 25 lpm flow through the outlets 67 and 15 lpm flow through the additional outlets 63 , 69 , and a flow rate of 75 lpm is obtained by specifying 50 lpm flow through the outlets 67 and 25 lpm flow through the additional outlets 63 , 69 . with reference to fig1 and 2 , it will be noted that the wafer w in the foregoing embodiments hangs downwardly from the rotary chuck 30 , supported by the gripping members 40 , such that fluids supplied through inlet 56 would impinge upon the upwardly facing surface of the wafer w . in case wafer 30 is a semiconductor wafer , for example of 300 mm or 450 mm diameter , the upwardly facing side of wafer w could be either the device side or the obverse side of the wafer w , which is determined by how the wafer is positioned on the rotary chuck 30 , which in turn is dictated by the particular process being performed within the chamber 1 . the apparatus of fig1 further comprises an interior cover 2 , which is movable relative to the process chamber 1 . interior cover 2 is shown in fig1 in its first , or open , position , in which the rotary chuck 30 is in communication with the outer cylindrical wall 10 of chamber 1 . cover 2 in this embodiment is generally cup - shaped , comprising a base 20 surrounded by an upstanding cylindrical wall 21 . cover 2 furthermore comprises a hollow shaft 22 supporting the base 20 , and traversing the lower wall 14 of the chamber 1 . hollow shaft 22 is surrounded by a boss 12 formed in the main chamber 1 , and these elements are connected via a dynamic seal that permits the hollow shaft 22 to be displaced relative to the boss 12 while maintaining a gas - tight seal with the chamber 1 . at the top of cylindrical wall 21 there is attached an annular deflector member 24 , which carries on its upwardly - facing surface a gasket 26 . cover 2 preferably comprises a fluid medium inlet 28 traversing the base 20 , so that process fluids and rinsing liquid may be introduced into the chamber onto the downwardly facing surface of wafer w . cover 2 furthermore includes a process liquid discharge opening 23 , which opens into a discharge pipe 25 . whereas pipe 25 is rigidly mounted to base 20 of cover 2 , it traverses the bottom wall 14 of chamber 1 via a dynamic seal 17 so that the pipe may slide axially relative to the bottom wall 14 while maintaining a gas - tight seal . an exhaust opening 16 traverses the wall 10 of chamber 1 , and is connected to a suitable exhaust conduit . the position depicted in fig1 corresponds to loading or unloading of a wafer w . in particular , a wafer w can be loaded onto the rotary chuck 30 either through the lid 36 , or , more preferably , through a side door ( not shown ) in the chamber wall 10 . however , when the lid 36 is in position and when any side door has been closed , the chamber 1 is gas - tight and able to maintain a defined internal pressure . in fig2 , the interior cover 2 has been moved to its second , or closed , position , which corresponds to processing of a wafer w . that is , after a wafer w is loaded onto rotary chuck 30 , the cover 2 is moved upwardly relative to chamber 1 , by a suitable motor ( not shown ) acting upon the hollow shaft 22 . the upward movement of the interior cover 2 continues until the deflector member 24 comes into contact with the interior surface of the upper part 15 of chamber 1 . in particular , the gasket 26 carried by deflector 24 seals against the underside of upper part 15 , whereas the gasket 18 carried by the upper part 15 seals against the upper surface of deflector 24 . when the interior cover 2 reaches its second position as depicted in fig2 , there is thus created a second chamber 48 within the closed process chamber 1 . inner chamber 48 is moreover sealed in a gas tight manner from the remainder of the chamber 1 . moreover , the chamber 48 is preferably separately vented from the remainder of chamber 1 , which is achieved in this embodiment by the provision of the exhaust port 46 opening into the chamber 48 , independently from the exhaust port 16 that serves the chamber 1 in general , and the remainder of the chamber 1 in the fig2 configuration . during processing of a wafer , processing fluids may be directed through medium inlets 56 and / or 28 to a rotating wafer w in order to perform various processes , such as etching , cleaning , rinsing , and any other desired surface treatment of the wafer undergoing processing . provision of the inner chamber 48 within the overall process chamber 1 thus enhances the safety of environmentally closed chambers by permitting the gases and liquids used for wafer processing to be better isolated from the exterior environment of the process chamber , and reduces the risk of process gas , chemical fumes , hot vapor such as vaporized isopropyl alcohol , ozone and the like being released to the tool environment . it will be understood that the foregoing description and specific embodiments shown herein are merely illustrative of the invention and the principles thereof , and that modifications and additions may be easily made by those skilled in the art without departing from the spirit and scope of the invention , which is therefore understood to be limited only by the scope of the appended claims . | 7 |
a large , self - contained burn - in bath unit incorporating the invention hereof is indicated generally by the reference character 20 . the unit comprises a generally rectangular box - like cabinet 22 mounted on casters 24 for ease of movement of the unit in such as a laboratory . electrical connection of the unit 20 is by cord 26 to a suitable electrical power supply connection . cabinet 22 comprises sheet metal walls mounted on an internal frame . a ventilating screen 28 is mounted on the cabinet front wall 29 to facilitate ventilation of the mechanical refrigeration unit contained in the cabinet . an upper housing 30 encloses control circuits and mounts indicators of the status and condition of the unit input knobs and switches also can be mounted on upper housing 30 . a top wall 32 of the cabinet comprises a segmented cover 34 and a surround portion 36 peripheral of the cover 34 in its closed position . interior of cabinet 22 a heat exchange tank 38 defines a rectangular burn - in chamber 40 that is generally open to the top and that can be closed by cover 34 . tank 38 contains a quantity of liquid heat exchange medium 42 and a plurality of circuit card carrying racks with one rack 44 carrying of plurality of circuit cards 46 being shown . a side wall 48 of the tank 38 includes a plurality of openings 50 for ventilation of the chamber space 52 above the medium 42 . thus arranged , a technician can approach the unit from the front , raise the cover 34 and install or remove circuit cards 46 from a rack 44 in the burn - in bath chamber 40 . controls and indicators of the burn - in procedure are available on the front of the control housing 30 and the unit can be moved on the casters 24 to suitable locations in a laboratory or testing facility . once connected to a source of electrical power by cord 26 , the unit 20 is self - contained . interior of cabinet 22 are additional systems that operate to effect a desired burn - in procedure in fig2 tank 38 is connected to a main liquid medium heating and cooling system 54 by conduits 56 and 58 . the main liquid medium heating and cooling system provides three functions first , this system raises the temperature of the liquid medium to the desired elevated temperature at which the burn - in procedure is to be effected , this being accomplished by a heating element contained therein . second , this system removes additional heat dissipated into the heat exchange medium by the operating semiconductor devices during the burn - in procedure , and third , serves to cool the liquid medium to ambient temperature at the termination of a burn - in procedure . this system thus serves as a temperature controller of the unit a portion of the liquid medium returning to the tank 38 in conduit 58 is carried by conduit 60 to a filter 62 and back to tank 38 through a conduit 64 . filter 62 serves to clean the liquid heat exchange medium by removing solid particulate and chemical contaminants introduced into the chamber or produced therein during the burn - in procedure . although not shown in this block diagram , the filtration system includes a weir assembly interior of tank 38 that facilitates filtration of the heat exchange medium . a vapor recovery system 66 comprises a vapor recovery condensor 68 and a liquid water separator 70 . gases including air , water vapor and medium vapor are exhausted from the tank 38 to the condensor 68 through duct 72 . these gases , less the condensed water and medium vapors , are fed back to the tank in duct 74 . the object of this recovery system 66 is conserving the supply of the expensive heat exchange medium . the liquid condensed water vapor and liquid condensed medium vapor are intermixed when condensed in the condensor 68 and are fed through duct 76 to liquid water separator 70 . there the intermixed liquids are allowed to rest for the liquid water to separate from and rise above the liquid medium as a result of the liquid medium having a greater specific gravity than water and the water being insoluble in the medium . the liquid water then is removed through schematically illustrated duct 78 while the expensive and recovered liquid medium is returned to the tank by duct 80 . in fig3 there is shown a structure , somewhat idealized , embodying the systems illustrated in block form in fig2 . referring also to fig6 and 7 , tank 38 has a rear wall 90 , two side walls 48 and 94 , a bottom wall 96 and a front wall 98 . tank 38 thus defines the burn - in chamber 40 that is closed on five sides by tank walls and is open to the top to be closed by cover 34 . cover 34 has five segments 34a through 34e that individually can be raised and lowered over the chamber 40 hinged at the rear wall 90 of the tank . the cover segments are arranged to be aligned with the racks and circuit cards carried by the racks for access to individual racks by raising individual cover segments . thus cover segment 34c is aligned directly above rack 42c carrying cards 46c while cover segment 34d is arranged aligned above rack 42d carrying cards 46d . burn - in chamber 40 contains in substantially its bottom half , the liquid heat exchange medium 42 previously generally described to be the fluorinert perfluorinated hydrocarbons manufactured by the 3m corporation . in particular , the heat exchange medium has a specific heat greater than air , a specific gravity greater than liquid water and a boiling point or temperature greater than the elevated temperature at which the burn - in procedure is to be effected . the upper half or space 52 of chamber 40 is filled with ambient gases that can include water vapor and especially during a burn - in procedure can include fluorinert medium vapor . the fluorinert medium has a low evaporation rate at room temperature that increases markedly at the elevated temperature of a burn - in procedure . during a burn - in procedure , the racks 44 are in the lowered position to place their circuit cards 46 and the carried semiconductor devices in the medium 42 in the bottom half 100 of the chamber 40 . before and after testing , the racks 44 hold the cards 46 in the top half space 52 of the chamber . the movements of the racks 44 are by means such as a hydraulic or pneumatic cylinder 101 connected with shaft 102 which in turn carries the racks 44 . shaft 102 then is vertically movable into and out of the pneumatic or hydraulic cylinder 101 . the main liquid heating and cooling system 54 comprises a structure arranged adjacent the tank side wall 94 and bottom wall 96 . in particular , the heating and cooling system 54 comprises a pump assembly 110 and a heating and cooling tube assembly 112 . in operation , the pump assembly 110 moves the liquid medium from the lower half 100 of burn - in chamber 40 through horizontally extending conduit 56 , vertically extending conduit 114 , horizontally arranged tube 116 of tube assembly 112 and then in a reverse direction therethrough and lastly through vertical riser pipes 58a through 58d back into the lower half 100 of chamber 40 , the flow being indicated by the arrows in the described conduits , tubes and pipes . referring also to fig4 and 5 , pump assembly 110 includes an impeller 120 carried at one end of a driven shaft 122 extending downward into substantially the length of conduit 114 with the impeller arranged adjacent tube 116 a bearing and baffle 124 are mounted inside the conduit 114 to stabilize the driven shaft 122 and to prevent up flow of liquid medium into the top half of conduit 114 . the other end of driven shaft 122 extends above the top end of conduit 114 and carries thereon a driven pulley 126 . a fixed length belt 128 connects the driven pulley 126 to a drive pulley 130 that is . carried at the end of a drive shaft 132 of an electric motor 134 . the medium 42 changes its viscosity with a change in its temperature and , therefore , the impeller 120 needs to be driven at a particular desired speed when the medium is at room ambient temperature and at a different speed when the medium is at the elevated temperature for effecting the burn - in procedure . to attain this result with the constant speed electric motor 134 , the pump assembly 110 includes a structure for varying the effective diameter of the drive pulley 130 while using a fixed length pulley belt 128 . the function is effected through use of a lever arm and lead screw and nut arrangement varying the distance between the drive shaft 132 and the driven shaft 122 and using a spring actuated mechanism to vary the effective diameter of the pulley 130 that engages the fixed length belt 128 . in particular , electric motor 134 is mounted on a mounting plate that is in turn mounted on a rotatable pivot shaft 138 pivot shaft 138 is mounted on a horizontal support plate 140 by means of a sleeve bearing 142 . plate 140 is clamped on the vertically extending tube 114 by a clamp portion 144 and clamp bolts 146 . the pivot shaft 138 passes downwardly through plate 140 and below plate 140 is connected to one end 148 of a lever arm 150 . the other end 152 of lever arm 150 is connected to a lead nut 154 threaded onto a lead screw 156 mounted below the plate 140 by a pair of brackets 158 lead screw 156 is mounted by brackets 158 for rotation around its longitudinal axis and is driven in such rotation by a stepping motor 160 mounted on support plate 140 by suitable bracket means 162 . in operation , stepping motor 160 rotates the lead screw 156 to move the lead nut 154 and lever arm end 152 to a selected position . this rotates or pivots the pivot shaft 138 to move the motor and its drive shaft 132 to a selected position on an arc around the pivot shaft 138 , selecting a particular distance between the center of the drive shaft 132 and the center of the driven shaft 122 a spring mechanism 164 mounted on the drive pulley 130 varies the effective diameter of drive pulley 130 engaging belt 128 to accommodate the fixed length belt 128 operating with different distances between the drive and driven shafts . in fig4 the solid lines indicate the position of the lever arm 150 , and motor 134 in one position while the dashed or broken lines indicate the positions of these same structures at another selected position . thus , by incrementally stepping the stepping motor 160 , variable speed rotation of the impeller driven shaft 122 can be obtained from a constant speed electric motor 134 this accommodates the varying pump requirements for the variable viscosity medium 42 without resorting to a variable speed drive motor and control device . referring now to fig3 , and 7 , tube assembly 112 provides the desired heating and cooling of the liquid heat exchange medium to raise the temperature of the medium to the elevated temperature , remove energy dissipated into the medium by the operating semiconductor devices and cool the medium to ambient temperature . assembly 112 comprises the earlier mentioned outer , horizontal tube 116 that is connected in fluid communication with the bottom end of vertically extending conduit 114 . outer tube 116 contains wholly therein an inner pipe 170 and a baffle 172 . pipe 170 rests on the bottom of the interior surface of outer tube 116 and can be held in position thereat , at least in part , by said baffle 172 . baffle 172 closes the space between the interior surfaces of horizontal tube 116 and pipe 170 so that liquid medium entering horizontal tube 116 can pass only into the interior of inner pipe 170 . the tube assembly 112 further comprises a cooling coil 174 that extends into one end of the tube 116 and into substantially the entire length of inner pipe 170 . the cooling coil in the preferred embodiment is the evaporator coil of a mechanical refrigeration unit and is intended to remove energy from the liquid medium as the liquid medium passes thereacross . while only one loop of the cooling coil 174 is shown for clarity of the drawing , plural coils can be inserted therein . in any event , the inner pipe 170 is arranged relative to the cooling coil 174 to contain the liquid medium in close contact with the cooling coil to obtain a maximum heat transfer . in this arrangement the medium 40 passes over and across coil 174 in inner pipe 170 in a first direction . the liquid medium that exits the inner pipe 170 empties into a space 176 interior of the outer tube 116 and reverses its flow to a second direction opposite the first direction within outer tube 116 to flow to the riser conduits 58 therefrom the medium flows back into the burn - in chamber 40 . the flow and counterflow of medium in one direction in inner pipe 170 and a second direction in outer tube 116 contributes to reduction in cabinet space required to effect the desired cooling and return of the medium to the tank at a plurality of locations . baffle 172 prevents the return of cooled medium back into the entrance to inner pipe 170 . outer tube 116 is closed at both ends 178 and 180 to contain the liquid medium therein with the cooling coil 174 entering the outer tube 116 through the end 178 . a portion of the liquid medium discharged into space 176 interior of horizontal tube 116 passes into conduit 60 and therefrom flows through filter 62 and conduit 64 back to chamber 40 . the flow through conduit 60 in the preferred embodiment is approximately 10 % of the liquid medium discharging into space 176 so that there is a constant filtering of the medium from the tank 38 . the filter 62 is intended to remove particulate foreign matter such as scale , solder particles , dirt and all types of foreign substances that are carried by the medium , aids in removing moisture from the liquid medium , and also removes acids , sludge and varnish from the medium . this is important for long term operation of the unit 20 for maximum efficiency . tube assembly 112 further comprises a heater element 182 , shown in fig3 that extends into space 176 . heater element 182 is any electrical heating device desired , such as a cartridge or coil heater , and functions to raise the temperature of the liquid medium 42 passing thereover to the desired elevated temperature for the burn - in procedure . thereafter the heating element 82 is not used because the semiconductor devices under test are sufficient to maintain the medium at the elevated temperature , with removal of excess energy by the cooling coil 174 . the arrows in fig3 and 6 indicate the flow of liquid medium from chamber 40 through conduit 56 , through vertically extending conduit 114 passed impeller 120 into outer tube 116 and contained pipe 170 , therein across cooling coil 174 , into space 176 and therefrom by counterflow in outer tube 116 to the vertical riser pipes 58 and back into chamber 40 . the return of medium to the main burn - in chamber at a plurality of locations effects an agitation or turbulence of the medium therein that is beneficial in mixing the medium in the chamber to achieve a homogeneous temperature throughout the bath medium . this achieves precise control of the elevated temperature at which the burn - in procedure is effected for closely following the calculated burn - in time requirements the agitation of the bath medium also is aided by the return of cooled medium to the bottom of the chamber and the removal of medium for cooling from the side of the burn - in chamber . this causes a flow of the medium across the cards carrying the semiconductor devices , also maintaining the semiconductor devices at the desired elevated temperature . thus , the function of the main liquid medium heating and cooling system is to elevate the temperature of the heat exchange medium to the desired temperature at which the burn - in procedure is to be effected , and to maintain the medium at that desired temperature through removal of the heat energy produced by the semiconductor devices into the cooling coil arrangement . at the end of the test , the cooling coil arrangement can be used to reduce the temperature of the liquid medium to ambient or room temperature . referring now specifically to fig3 and 9 , the vapor recovery system 66 provides recovery of the vapors of the expensive heat exchange medium . without this or a like recovery system , all of the medium would be lost in a short time through evaporation . system 66 comprises the vapor recovery condensor 68 located below the tank 38 , the liquid water separator 70 located to one side of the tank 38 and an exhaust manifold 190 and a feed manifold 192 located at the top side margins of tank 38 . exhaust ducts 194 provide for movement of gases from the upper space 52 of burn - in chamber 40 into the exhaust manifold 190 and feed ducts 196 provide for movement of gases from feed manifold 192 into the upper space 52 of chamber 40 . in operation , the gases in the upper space 52 of chamber 40 , which gases include water vapor and vapors of the liquid medium , are pulled by a fan assembly 198 , shown in fig8 and 9 , through the exhaust ducts 194 and into the exhaust manifold 190 . there , any of the medium vapors that have joined with the water vapor to form hydrofluoric acid are removed and any remaining water vapor picks up metal ions and is made conductive . therefrom the gases are pushed by the fan assembly down through duct 72 into the vapor recovery condensor 68 . vapor recovery condensor 68 comprises a box - like outer container 200 completely enclosing expansion coil 202 of a mechanical refrigeration device . the gases and vapors from duct 72 pass over the expansion coil 202 and included water vapors and medium vapors are condensed thereon the condensed water and medium vapors , now in intermixed liquid stage , drip off the bottom of the expansion coil into the bottom of the container 200 to form a pool 204 of intermixed liquid water and liquid medium . the remaining stripped gases exit from the vapor recovery condensor 68 through return duct 74 into feed manifold 192 wherefrom they are fed into the upper space 52 of chamber 40 through the feed ducts 196 opening through wall 48 at openings 50 . thereafter the stripped gases pass through the length of the chamber 40 between walls 48 and 94 back to the exhaust ducts 194 picking up vapors to complete one cycle . gases passing from the feed ducts to the exhaust ducts are used to advantage to remove liquid medium from semiconductor devices 47 carried on cards 46 that are raised to the upper position by the rack 44 . while most of the liquid medium drips off of the cards while they are held in the upper space 52 , the gases that pass across the semiconductor devices and cards aid in evaporating residual quantities of medium to &# 34 ; dry &# 34 ; the cards . this can be helpful in draining and &# 34 ; drying &# 34 ; a rack of cards before removal of the cards and devices from burn - in chamber 40 while the other racks of card carried semiconductor devices remain submerged in the liquid medium undergoing the burn - in procedure in such a situation , after the cards are &# 34 ; dry &# 34 ; of medium , only one segment of the cover need be raised to gain access to the cards . referring specifically to fig8 and 9 , the exhaust manifold 190 comprises an outer cylindrical housing 210 closed at one end by a plate 212 and at the other end by the fan assembly 198 . the exhaust ducts 194 extend horizontally from the side wall 94 of tank 38 and are bent at a 90 ° angle to meet the cylindrical housing 210 vertically . the exhaust ducts 194 thus place the interior 214 of the cylindrical housing in gaseous fluid communication with the burn - in chamber 40 interior tank 38 . mounted interior of cylindrical housing 210 by the plate 212 and an internal baffle 216 , are means 218 for removing acids from the gases exhausted from the chamber 40 into the interior 214 of exhaust manifold 190 . these means 218 comprise a pair of cylindrical members 220 and 222 concentrically mounted one within the other to form annular space 224 that is filled with an acid absorbing material 226 . this material 226 can be such as soda - sorb or other acid absorbing materials a drain pipe 228 extends downwardly from the bottom of cylindrical housing 210 to carry any liquids that have condensed in the exhaust manifold such as liquid water and liquid medium to the duct 72 earlier described . a space 230 interior of cylindrical member 222 is in gaseous fluid communication through an opening 232 in baffle 216 with impeller 236 of the fan assembly 198 . the impeller 236 is driven by a motor 238 through a belt 240 and a driven shaft 242 . the impeller 236 is mounted in a space 244 opening to the duct 72 earlier described . in operation the impeller 236 of the fan assembly 198 withdraws gases from the opening 232 into space 244 and forces them into duct 72 . this in turn draws gases including water vapor and medium vapor from the upper space 52 of chamber 40 through the exhaust duct 194 to the interior 214 of the cylindrical housing 210 . therefrom the gases pass through fine openings ( not shown ) in the cylindrical member 220 into close contact with the acid absorbing material 226 in the annular space 224 . this removes hydrofluoric acid vapors . the remaining gases and vapors pass through additional fine openings ( not shown ) in the inner cylindrical member 222 and into the space 230 interior of the cylindrical member 222 . therefrom these gases pass into the opening 232 , and are moved by the impeller 236 into the duct 72 . also referring to fig1 , impeller 236 comprises a circular disc of solid material that has a plurality of radially extending openings 246 machined or drilled therein . when rotated by motor 238 , impeller 236 centrifically moves gases and vapors radially outwardly from its center into space 244 . this provides an inexpensive piece part impeller that can be replaced easily upon excessive wear caused by any unabsorbed hydrofluoric acid that may pass through the acid absorbing means . the feed manifold 192 comprises a cylindrical housing 250 closed at both ends with the interior thereof in gaseous fluid communication with the chamber 40 through the feed ducts 196 . the feed manifold 192 performs the function of roughly equalizing the flow of gases from duct 74 into the several feed ducts 196 to chamber 40 . turning now to fig3 and 12 , the liquid water separator 70 receives intermixed liquid water and liquid medium from conduit 76 by way of pump 260 from pool 204 in the vapor recovery condensor 68 . the liquid water separator 70 feeds separated liquid medium back to chamber 40 through conduit 80 by way of pump 262 . conduit 80 returns the liquid medium to the tank 38 and chamber 40 well above the top surface of the liquid medium 42 to prevent a siphoning of the liquid medium back into the liquid water separator 70 . the purpose of separator 70 is to separate the liquid medium from the liquid water so that the expensive liquid medium can be reused in the burn - in chamber 40 . it is desired to remove the liquid water to prevent formation in the bath of hydrofluoric acid that can corrode the tank , racks , cards and semiconductor devices . liquid water separator 70 comprises an upstanding cylindrical housing 254 closed at its top by a cover 266 and at its bottom by a base 268 and having a pair of depending cylindrical tubes 270 and 272 , which are closed at their bottom ends by bases 274 and 276 . housing 264 defines a substantially cylindrical separator chamber 278 that is in fluid communication with a well 271 interior of depending tube 270 and a well 280 interior of the depending tube 272 a diffuser material 282 such as a rolled web of stainless steel mesh is installed in the well 280 of the tube 272 for a purpose to be described presently . liquid water separator 70 further comprises a pair of electrodes 282 and 284 each connected to a bridge circuit 286 by conductor leads 288 and 290 . the electrodes 282 and 284 extend radially through the wall of the housing 264 at a certain level so that their tips 292 and 294 are in fluid communication with any liquids or gases in the separator chamber 278 interior of the housing 264 . in operation , and initially , the interior of the housing and the two depending tubes are filled only with bath liquid medium and are void of any liquid water . when the burn - in procedure commences , quantities of liquid intermixed water and medium will be pumped up from pool 204 through conduit 76 into well 280 and therefrom into chamber 278 . the liquid entering chamber 278 from the well 280 of tube 272 will do so in a substantially planar flow , because the mesh material 282 has greatly diffused the stream of flow resulting from the liquid entering from conduit 76 . this prevents any turbulence or agitation of the intermixed liquids in chamber 278 so that the liquid water can rest and separate from the liquid medium and rise to float above the liquid medium at the top of chamber 278 . suitable controls ( not shown ) are provided so that chamber 278 remains substantially filled with liquid . during the course of the burn - in procedure , the liquid water separating from the intermixed liquids in the bottom of chamber 278 will increase in volume from the top of chamber 278 downwardly . when the interface 296 between the liquid water 298 and the liquid medium 42 touches both of the tips 292 and 294 of the electrodes 282 and 284 , an electrical signal can be conducted through the liquid water because it is conductive , the conductivity resulting from the water vapors passing through the acid absorbing material 226 in the exhaust manifold 190 . no electrical signal passes between the electrodes 282 and 284 while they are submerged in only the liquid medium because the liquid medium is non - conductive . the electrical signal flowing between the two electrodes causes a change in the balance of a bridge circuit 286 and an indicator is activated so that the operator may manually removed the liquid water from the liquid water separator 70 with such as a syringe . this is performed by lifting the cover 266 from the housing 264 for manual removal of the liquid water 298 . alternatively , the liquid water can be removed automatically through the conduit 78 schematically illustrated in fig2 . the flow of intermixed liquid into the liquid water separator 70 is minimal and provides for the liquid substantially to rest in chamber 278 for the lighter specific density liquid water to rise and float above the heavier specific density heat exchange medium . this separation of the liquid water from the liquid medium aids in reducing the quantity of hydrofluoric acid formed in the tank 38 , increasing the life of the tank and related pipes , ducts and conduits . while the well 280 serves to contain the diffuser means 282 , the well 271 serves another , equally important purpose . there is a substantial distance between the outlet port 300 in the bottom of well 271 through base 274 and the level of the two electrode tips 292 and 294 indicated by the water / medium interface 296 . this distance in separator chamber 278 and well 271 forms a long stable column of mainly liquid medium that , due to the differences in specific gravities , strongly urges any intermixed liquid water to separate , rise above and float on the medium . this urging is greatest at the bottom of well 271 adjacent outlet port 300 and results in medium containing the least amount or concentration of intermixed liquid water first being removed from the bottom of well 271 and separator 70 . this effect also occurs adjacent inlet port 302 in the base 276 of well 280 but the separated liquid heat exchange medium has to rise into separator chamber 278 before it can be removed through outlet port 300 . referring first to fig3 but also to fig1 and 14 , the filtration system includes a weir assembly 303 located in burn - in chamber 40 adjacent port 304 through which medium 100 flows from chamber 40 into conduit 56 . weir assembly 303 intentionally blocks clear flow of medium 100 into port 304 to channel solid , particulate contaminants that float on top of medium to port 304 and eventually to filter element 62 where they are trapped for later removal from the system . weir assembly 303 thus forms a turbulence box 305 into which the top layer of medium cascades from over the weir to agitate the floating contaminants into suspension for delivery to the fliter element 62 . referring also to fig1 and 14 , weir assembly 303 comprises a pair of plates , being a fixed lower plate 306 and an movable upper plate 307 . a leaf spring 308 attached to upper plate 307 acts to maintain upper plate 307 in a desired position . plates 306 and 307 mount in tracks 310 and 312 that are secured to heat exchanger tank walls 90 and 98 by such as spot welding . lower plate 304 rides in slot 314 between rails 316 and 318 of each track and plate 307 rides in slot 320 between rails 318 and 322 of each trade leaf springs 308 are secured to upper plate 307 at area 324 by such as spot welding and engage against rails 322 to press the upper plate 307 against rail 318 to maintain it in position . tracks 310 and 312 and plates 306 and 307 are dimensioned to prevent leakage of the medium 100 into turbulence box 305 , which is formed of weir assembly 303 , and heat exchanger tank front wall 90 , end wall 94 , bottom wall 96 and back wall 98 . the bottom edge 326 of lower plate 306 intentionally is set by screws 327 slightly spaced from bottom wall 96 to provide a passage for medium 100 therethrough into the bottom of turbulence box 305 . this assures a continuous , but minimal flow of medium 100 to port 304 and the main heating and cooling in the event the level of the medium in chamber 10 falls below the top edge 328 of upper plate 307 and cannot otherwise flow to port 304 . this can occur normally when the system is first being heated and the volume of the cold medium 100 is minimal . when the temperature and volume of medium 100 increases to operating range , the upper plate 307 is manually adjusted to locate the top edge 328 thereof approximately one half to one quarter inch below the top surface 330 of the medium 100 . this establishes a flow of the top layer 334 of medium 100 , which carries solid , particulate contaminants floating thereon , from the bath to the turbulence box . there , the contaminants are agitated and mixed with the medium 100 to be carried by the medium through port 304 and conduit 56 to the filter element for removal from the medium . this agitation and mixing is facilitated by the medium falling over the top edge 328 of movable upper plate 307 into turbulence box 305 . this flow of the top layer 332 of medium 100 maintains the top surface 330 clean and free of contaminants and debris . the burn - in procedure effecting unit 20 thus provides a structure that aids an operator in placing semiconductor devices in the tank burn - in chamber for the procedure and removing the devices after completion of the procedure . the unit includes special provisions for maintaining the heat exchange bath medium at the desired , elevated temperature for effecting the procedure precisely and for re - cycling evaporated medium into the bath . moisture , in the form of liquid water and water vapor , is removed substantially to protect the unit components from the attack of hydrofluoric acid that can form from interaction of the moisture and heat exchange medium . an included filter removes from the liquid medium particulate matter , chemical contaminants and moisture . all of this is provided in a unit that is self - contained after connection to an electrical power source and that has a burn - in chamber capable of effecting the procedure on production quantities of semiconductor devices . while the invention has been described with reference to a preferred embodiment , it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the broader aspects of the invention . it is intended that broad claims not specifying details of a particular embodiment disclosed herein as the best mode contemplated for carrying out the invention should not be limited to such details generally , while specific claimed details of the invention constitute important specific aspects of the invention , in appropriate instances even the specific claims involved should be construed in light of the doctrine of equivalents . | 1 |
now , the present invention will be described hereinafter with reference to embodiments shown in the accompanying drawings . fig2 shows an embodiment of a roof structure according to the present invention which is assembled according to procedures described hereinafter . in fig2 reference numeral 74 designates a roof support member , on which purlins 36 are mounted . supported on the purlins 36 are common rafters 34 each comprising a channel member of a c - shape in section . the common rafters 34 may be formed into any other suitable shape such as a hat shape in section , a shape provided with a step , or the like . on the common rafters 34 are arranged a plurality of roof boards 30 which are connected to one another in order from a purlin 76 constituting a ridge side rising support means to an eaves side . the roof structure also includes a backing member 32 comprising an excelsior board arranged under each of the roof boards 30 . the roof board 30 , as shown in fig2 may be formed by subjecting a lengthwise steel sheet of a predetermined width , to which baking finish for rust prevention was applied , to a shaping treatment using a suitable forming machine , so that it may have a flat surface section 80 , an upper side or ridge side connection 72 formed at one end 82 of the flat surface section 80 and a lower side or eaves side connection 66 formed at the other end 84 thereof . the so - shaped steel sheet is then cut into roof boards of a required width . the ridge side connection 72 and eaves side connection 66 of each of the roof boards 30 are constructed to be engaged with each other . also , each of the roof boards 30 , as clearly shown in fig5 is provided with a rising portion 86 which upwardly extends from the one end 82 of the flat surface section 80 to the ridge side connection 72 and a falling section 88 which downwardly extends from the other end 84 of the flat surface section 80 to the eaves side connection 66 and is adapted to be abutted against a rising section 86 of a lower adjacent roof board 30 in a manner to form a flat vertical surface together . such construction of the roof board allows rainwater to downwardly flow along the so - formed vertical surface to prevent it from entering through an engagement between the ridge side connection 72 of the lower side one of each adjacent two roof boards 30 and the eaves side connection 66 of the upper side roof board 30 , so that waterproofness of the engagement may be more efficiently improved . uppermost one of a plurality of the roof boards 30 connected together in order from the ridge side to the eaves side , as shown in fig4 is held at the ridge side connection 72 on a holding member 90 fixed on a vertical surface 92 of the purline or ridge side rising support means 76 utilizing any suitable means such as screws , welding or the like . the ridge side connection 72 and holding member 90 are covered with a water seal member 94 to prevent rainwater from entering through the ridge side connection 72 of the uppermost roof board 30 into the roof structure . the eaves side connection 66 of the uppermost roof board 30 , as shown in fig5 is engagedly connected to the ridge side connection 72 of the lower adjacent roof board 30 through a fixture 38 fixed on the common rafter 34 at a position on the eaves side beyond the eaves side connection 66 of the uppermost roof board 30 . between the lower adjacent roof board 30 and the common rafter 34 is inserted a backing member or excelsior board 32 in such a manner that a ridge side end 96 thereof is abutted against the fixture 38 . the fixture 38 , as shown in fig6 is integrally formed into a substantially c shape to have a base section 100 adapted to be mounted on the common rafter 34 , a holding section 102 vertically extending from the base section 100 and a support section 104 extending substantially in parallel with the base section 100 and in substantially the same direction as the base section 100 from the holding section 102 . the support section 104 is formed at a free end portion 108 thereof into a substantially c - shape . in the illustrated embodiment , the c - shape end portion 108 of the support section 104 is connected through an obliquely downwardly and outwardly extending portion to the support section . also , the fixture 38 is formed to have an internal space 106 sufficient to cause the insertion of the ridge side connection 72 of the lower side roof board 30 into the eaves side connection 66 of the upper adjacent roof board 30 and the holding of the former with respect to the latter to be readily carried out . the so - constructed fixture 38 is fixed on the common rafter 34 subsequent to the arrangement of the backing member or excelsior board 32 under the roof board 30 , so that the holding section 102 may be abutted against an eaves side end 98 of the upper adjacent excelsior board 32 and the support section 104 supports thereon the other end portion 84 of the upper adjacent roof board 30 . also , the free end 108 of the support section 104 of the fixture 38 , as described above , is downwardly bend into a substantially l - shape , resulting in the free end 108 being fixedly engaged with the eaves side connection 66 of the roof board 30 . also , in the illustrated embodiment , the base section 100 of the fixture 38 is formed at an eaves side end 110 thereof with a pair of mounting holes 112 and correspondingly the common rafter 34 is previously provided with a pair of raised projections 114 , so that the mounting and positioning of the fixture 38 with respect the common rafter 34 may be carried out by fitting the raised projections 114 in the mounting holes 112 and then bending the raised projections 114 as shown in fig5 . further , in the illustrated embodiment , the fixture 38 is so constructed that the eaves side end 110 of the base section 100 outwardly projects from the free end 108 of the support section 104 to cause the fixture to be fixed on the common rafter at a position on the eaves side beyond an engagement between the ridge side connection of the lower side roof board and the eaves side connection of the upper side roof board . such construction of the fixture 38 causes the fixture mounted on the common rafter 34 to exhibit satisfied strength . the fixing of the fixture 38 onto the common rafter 34 may be carried out in a manner different from the foregoing . for example , in a simple roof wherein backing members such as veneered woods are directly mounted on purlins without using any common rafter , the fixture 38 may be fixed directly on the backing member by means of screws , nails or the like . also , in a roof in which concrete support members are directly laid on a roof frame , the fixture 38 may be fixed directly on the concrete support member . now , the manner of assembling of the roof structure will be described with reference to fig7 to 13 . first , as shown in fig7 the holding member 90 is fixedly mounted on the vertical surface 92 of the ridge side rising support means 76 by means of screws or the like , and then the uppermost roof board 30 is securely held at the ridge side connection 72 on the holding member 90 as shown in fig8 . subsequently , the backing member or excelsior board 32 is inserted between the uppermost roof board 30 and the common rafter 34 from the eaves side as shown in fig9 and then the fixture 38 is positioned and fixed on the common rafter 34 in a manner to be abutted at the holding section 102 against the eaves side end 98 of the excelsior board 32 as shown in fig1 , so that the excelsior board 32 may be held in position . concurrently , the eaves side end portion 84 of the uppermost roof board 30 is held on the fixture 38 . thereafter , as shown in fig1 , the ridge side connection 72 of the lower adjacent roof board 30 is engagedly inserted in the eaves side connection 66 of the uppermost roof board 30 supported on the fixture 38 and then the lower adjacent excelsior board 32 is interposedly arranged between the lower adjacent roof board 30 and the common rafter 34 and fixed in place by a lower adjacent fixture 38 . such procedures are repeated in turn , so that a plurality of the roof boards 30 may be connected to one another in turn from the ridge side to the eaves side and mounted on the common rafters . the engagement between each adjacent two of the roof boards , as shown in fig1 , is made by inserting the ridge side connection 72 of the lower side roof board 30 in the eaves side connection 66 of the upper side roof board 30 supported on the fixture 38 and carrying out the rotation and drawing of the ridge side connection 72 of the lower side roof board as indicated at dashed lines and two - dot chain lines , respectively . such engagement can be smoothly performed because the internal space 106 of the fixture 38 is sufficient to facilitate the operation . in the embodiment described above , the fixture 38 is fixedly engaged with the eaves side connection 66 of the corresponding roof board 30 . however , it , as shown in fig1 , may be engaged with the ridge side connection 72 of the lower adjacent roof board 30 . also , in the illustrated embodiment , the mounting of the fixture 38 with respect to the common rafter 34 is carried out by inserting the raised projections 114 into the mounting holes 112 and bending the raised projections 114 . however , it may be practiced using any other suitable means such as screws , rivets or the like . fig1 shows a modification of the embodiment described above , in which a fixture 38 is used in a roof structure assembled without using a backing member or excelsior board and fixed on the common rafter 34 by means of nails . the remaining of the modification of fig1 may be constructed in a manner similar to the embodiment described above . the fixture of the present invention , so long as roof boards each is adapted to be engaged with the free end 108 of the fixture , is capable of connecting the roof boards to one another in order from the ridge side to the eaves side , even when the roof boards are originally made to be connected from the eaves side to the ridge side . thus , it will be noted that the present invention is effectively applicable to conventional roof boards . as can be seen from the foregoing , the illustrated embodiment is so constructed that a plurality of the roof boards are connected to one another in turn from the ridge side to the eaves side and mounted through common rafters on purlins , and the fixture securely holds therein the eaves side connection and ridge side connection of each adjacent two of the roof boards which have engaged with each other . also , the fixture holds the eaves side end of the backing member inserted under the roof board . accordingly , the illustrated embodiment not only facilitates the transfer of the roof boards but causes the assembling operation to be readily carried out without requiring scaffolding and injuring the roof boards irrespective of a steep slant , as compared to the prior art in which roof boards are connected to one another from the eaves side to the ridge side . also , the fixture is formed to have an sufficient internal space , so that the assembling operation may be more smoothly and efficiently accomplished . furthermore , the illustrated embodiment can be practiced without skill and at low costs . also , in the illustrated embodiment , the fixture is fixed on the common rafter at a position on the eaves side beyond the eaves side connection of the corresponding roof board , resulting in the strength of the fixture mounted on the common rafter being highly increased to a degree sufficient to bear force of blowing - up wind which is to peel the fixture together with the roof board from the common rafter , so that the roof structure may be rigidly constructed . fig1 shows another embodiment of a roof structure according to the present invention . in the embodiment shown in fig1 a plurality of roof boards 30 are connected to one another in turn from a ridge side to an eaves side while being securely mounted in turn through backing members 32 on common rafters 34 of a hat shape in section perpendicularly fixed at a predetermined slant on purlins or c - shaped channel members 36 formed of iron , by means of fixtures 38 securely mounted on the common rafters 34 which serve to fix the roof boards 30 and backing members 32 with respect to the common rafters 34 . the fixture 38 may be formed by subjecting a galvanized sheet of a large thickness to pressing . the fixture 38 , as shown in fig1 , is formed into a substantially c - shape so as to comprise a base section 40 formed with an engagement recess 42 , a first support section 44 formed to horizontally extend from the base section 40 with a step 46 being defined therebetween , an outward projection section 48 formed at a distal end of the first support section 44 , a first stopper section 50 formed to upwardly extend from the projection section 48 , a second support section 52 formed to inwardly horizontally extend from the first stopper section 50 , a second stopper section 54 formed to upwardly extend from the second support section 52 , a third support section 56 formed to inwardly horizontally extend from the second stopper section 54 , and a bent end section 58 downwardly extending from the third support section 56 and formed into a substantially u - shape . in the illustrated embodiment , the base section 40 is formed to outwardly project from the bent end section 58 , as shown in fig1 . the fixture 38 constructed as described above , as shown in fig1 , is held on a common rafter 34 through a pair of pawls 60a and 60b formed by raising a part of the common rafter 34 and fixed thereon by securely engaging the pawls 60a and 60b with the engagement recess 42 of the base section 40 and the projection section 48 by caulking , respectively . with respect to the fixture 38 fixed on the common rafter 34 in such a manner , lower one of each adjacent two backing members 32 is inserted at a ridge side end portion 62 thereof between the first and second support sections 44 and 52 of the fixture 38 to abut a ridge side end against the first stopper section 50 and the upper side backing member 32 is supported at an eaves side end portion 64 thereof on the second support section 52 and abutted at an eaves side end thereof against the second stopper section 54 . further , each of the roof boards 30 is so constructed that an eaves side connection 66 is inwardly bent at an end section 68 thereof to surround the bent end section 58 of the fixture 38 and the inwardly bent end portion 68 of the eaves side connection 66 is fitted in an outer end portion 70 of a ridge side connection 72 of the lower adjacent roof board 30 . fig1 shows a modification of the roof structure shown in fig1 to 17 . in the embodiment shown in fig1 to 17 , as described above , the eaves side connection 66 of the roof board 30 is adapted to engagedly surround the bent end section 58 of the fixture 38 . although this effectively prevents the lifting of the roof board 30 due to force of blowing - up wind ; the upper side one of each adjacent two roof boards 30 is apt to be moved at the eaves side connection toward the eaves side as indicated at two - dot chain lines in fig1 , for example , when a worker is on the roof board ; because a gap l is formed between the eaves side connection 66 of the roof board 30 and the bent end section 58 of the fixture 38 . this occasionally fails to provide the roof structure with rigidity and waterproofness . the modification of fig1 is for the purpose of eliminating such a disadvantage of the embodiment shown in fig1 to 17 . the embodiment shown in fig1 is constructed in such a manner that each of roof boards 30 is provided at an intermediate region of an inwardly bent end section 68 of an eaves side connection 66 thereof with a stepped engagement portion 120 having a rising surface , so that a fixture 38 may be engagedly abutted at a bent end section 58 thereof against the stepped engagement portion 120 . such construction effectively prevents an upper side one of adjacent two roof boards 30 from being moved toward an eaves side with respect to a ridge side roof board thereof because the upper side roof board can be securely held with respect to the lower side roof board due to the secure engagement between the bent end section 58 of the fixture 38 and the stepped engagement portion 120 of the eaves side connection 66 of the upper side or ridge side roof board 30 . the remaining of the modification of fig1 may be constructed in substantially the same manner as the roof structure shown in fig1 to 17 . fig1 to 22 each show a modification of the roof structure shown in fig1 , wherein the manner of abutment between a bent end section 58 of a fixture 38 and a stepped engagement 120 formed at an inwardly bent end section 68 of an eaves side connection 66 of a roof board 30 is modified . more particularly , the modification shown in fig1 is so constructed that a bent end section 58 of a fixture 38 is formed into an l - shape and a stepped engagement portion 120 of an inwardly bent end section 68 of an eaves side connection 66 is formed into a substantially inverted u - shape . in the modification of fig2 , a bent end section 58 of a fixture 38 comprises a downwardly obliquely extending portion and an l - shaped portion connected thereto , and a stepped engagement portion 120 of an inwardly bent end section 68 of an eaves side connection 66 is formed to be obliquely upwardly projected toward the bent end section 58 . the modification shown in fig2 is constructed in such a manner that a bent end section 58 is formed to downwardly extend from a third support section 56 and a stepped engagement portion 120 is formed into a triangle shape to securely interpose a distal end of the bent end section 58 between a falling section 88 and the stepped engagement portion 120 . the modification of fig2 is so constructed that a bent end section 58 comprises an obliquely downwardly and outwardly extending portion and a downwardly extending portion connected thereto and a stepped engagement portion 120 is provided in proximity to the a falling section 88 to securely interpose a lower end of the downwardly extending portion of the bent end section 58 between the falling section 88 and the stepped engagement portion 120 . it will be noted that each of the modifications likewise effectively prevents an upper side one of adjacent two roof boards 30 from being moved toward an eaves side with respect to a ridge side roof board thereof . it is a matter of course that the illustrated embodiment is not limited to the above description . the fixture and roof board in the roof structure of the illustrated embodiment may be modified in other different manners depending upon workability required . as can be seen from the foregoing , in the roof structure of the modification shown in fig1 , a plurality of the roof boards are connected to one another in turn from the ridge side to the eaves side and mounted on a roof support means in turn by means of the fixtures . also , the fixtures each are constructed to be engagedly abutted at the bent end section thereof against the stepped engagement portion formed at the inwardly bent end section of the eaves side connection of the roof board . accordingly , the roof structure of the embodiment can be readily assembled as compared with the conventional one assembled by connecting roof boards to one another in turn from the eaves side to the ridge side . also , the roof structure of the embodiment effectively prevents the looseness and movement of the roof board toward to the eaves side . it will thus be seen that the objects set forth above , among those made apparent from the preceding description , are efficiently attained and , since certain changes may be made in the above construction without departing from the spirit and scope of the invention , it is intended that all matter contained in the above description or shown in the accompanying drawings shall be interpreted as illustrative and not in a limiting sense . it is also to be understood that the following claims are intended to cover all of the generic and specific features of the invention herein described and all statements of the scope of the invention which , as a matter of language , might be said to fall therebetween . | 4 |
turning now to the single figure , there is illustrated a portion of an internal combustion engine 1 having a schematically indicated exhaust gas system 2 , a portion 3 of which is shown enlarged . the internal combustion engine has an induction tube 5 , the inlet of which includes a carburetor 6 which supplies the engine with an operational fuel - air mixture through the induction manifold 7 . in known manner , the carburetor has an air funnel 8 and downstream thereof an arbitarily settable throttle butterfly valve 9 . a float chamber 10 supplies fuel in the vicinity of the narrowest portion of the air funnel 8 in proportion to the air flow rate through the induction tube . fuel is supplied to the float chamber by a fuel pump 12 from a fuel supply container 13 through a fuel supply line 14 . the carburetor 6 includes a bypass air channel 16 which branches off from the induction tube upstream of the air funnel 8 and which returns to the induction tube downstream of the throttle valve 9 . the flow cross section of the bypass channel can be varied by means of an adjustment screw 17 . the air bypass channel is of the type commonly supplied in carburetors of modern construction and serves to adjust the idling of the engine . it may be disposed as illustrated , i . e ., as a bypass around the throttle valve 9 and the air funnel 8 or as a bypass only of the throttle valve . terminating in the bypass air channel is a fuel line 19 which branches off from the main fuel supply line 14 and which contains a fuel metering valve 21 . the flow through the fuel line 19 is controlled by an equal pressure control valve 22 which is disposed between the fuel metering valve 21 and the terminus of the line 19 in the bypass channel 16 . the equal pressure valve 22 has a firmly clamped elastic diaphragm 23 which divides the valve into a pressure chamber 24 and a control chamber 25 . the fuel line 19 terminates in the pressure chamber 24 . the portion of the fuel line 19 leading to the bypass channel 16 enters the pressure chamber 24 at right angles and its terminus is embodied as a valve seat 26 which cooperates with the diaphragm 23 to form a valve . a short line 28 connects the control chamber 25 with a pressure control chamber 29 of a differential pressure valve 31 . the closure member of the latter is a firmly clamped elastic diaphragm 32 which separates the pressure control chamber 29 from a working chamber 33 which is coupled to the fuel line 14 . a relief line 36 extends into the working chamber 33 and meets the diaphragm at right angles where its terminus is thus controlled by the position of the diaphragm 32 . from this point , the relief line 36 leads to the pressure control chamber 29 which is pressure - relieved through a throttle bore 39 and a return line 40 leading to the fuel container 13 . entering the control pressure chamber 29 in pressure sealed manner is an actuating rod 43 , one end of which is coupled to the diaphragm 32 and the other end of which is engaged by a first spring 45 having a progressively increasing force characteristic and which is supported on a diaphragm 46 . the opposite side of the diaphragm 46 encloses a vacuum chamber 47 which is coupled via channel 48 with the induction tube 5 downstream of the throttle valve 9 . if the actuating rod is guided with free tolerance , a throttle bore 39 may be dispensed with . the vacuum chamber 47 also contains a second spring 49 disposed between the diaphragm and the opposite side of the chamber . the metering valve 21 in the fuel line 19 is an electromagnetic valve acting as a switching valve having an &# 34 ; on &# 34 ; and an &# 34 ; off &# 34 ; position . a controller 52 actuates the valve 21 via a line 51 and the controller receives its information from an rpm transducer 54 , of known construction , which senses the rotational speed of the engine , for example at the crankshaft , and also , for example , by a known oxygen sensor 55 disposed within the portion 3 of the exhaust gas system 2 . when the internal combustion engine is running , the fuel pump 12 supplies fuel from the container 13 to the float chamber 10 of the carburetor 6 . in known manner , the carburetor produces a fuel - air mixture of predetermined composition and delivers it to the induction tube 5 of the engine . the amount of mixture is set by the position of the throttle valve . in addition hereto , an amount of fuel controlled by the metering valve 21 is supplied through the fuel line 19 to the bypass air channel and hence into the induction tube . this additional fuel quantity is also taken from the fuel line 14 and its magnitude depends on the opening flow cross section of the metering valve , the opening duration of which , together with the pressure difference across it , determines the fuel flow through that line . the pressure difference across the metering valve 21 is determined by the fuel pressure prevailing upstream of the valve in the line 19 and by the controlled pressure in the pressure chamber 24 of the equal pressure valve 22 . the pressure upstream of the metering valve is the same as the pressure in the working chamber 33 of the differential pressure valve and also equal to the fuel pressure generated by the fuel pump 12 in the line 14 . the pressure in the chamber 24 of the equal pressure valve 22 , however , is determined by the pressure prevailing in the control pressure chamber 25 . as sonn as the pressure in the chamber 24 exceeds that in the chamber 25 , the diaphragm 23 opens the valve seat 26 so that fuel may flow through the valve 21 and the fuel line 19 . in order to function in this manner , the pressure in the control chamber 25 must be lower than the pressure in the fuel supply line 14 and it is determined by the differential pressure valve 31 . if the force acting on the diaphragm 32 is assumed to be constant , the diaphragm 32 will open the relief line 36 as soon as the pressure in the control pressure chamber 29 has fallen below a value which is less than the pressure prevailing in the work chamber 33 due to the continuous flow of fuel through the throttle bore 39 back to the storage container 13 . the magnitude of the pressure difference is determined by the force which acts on the diaphragm 32 . however , as soon as the relief line 36 is opened , a larger amount of fuel flows into the control pressure chamber 29 so that the pressure there again reaches the previously adjusted value . accordingly , the control chamber 29 may be provided with a pressure which is less than the pressure in the chamber 33 or the pressure upstream of the metering valve 21 by a definite amount . the pressure in the chamber 24 of the equal pressure valve is the same as that in the pressure chamber 29 or in the control pressure chamber 25 . this insures that the same pressure difference always obtains across the free flow cross section of the metering valve . this pressure difference , however , may also be varied in dependence on the pressure in the induction tube 5 by changing the force which acts on the diaphragm 32 , i . e ., by changing the bias on the diaphragm . for this purpose , the diaphragm 46 in the vacuum chamber 47 is displaced in proportion to the induction tube pressure and against the force of the second spring . this produces a displacement which is proportional to the induction tube pressure and which changes the bias of the first spring 45 . this spring preferably has a progressive force characteristic so that the force of this spring becomes proportional to the square of the induction tube pressure and is transmitted to the diaphragm 32 . it is this force to which the pressure difference between the pressure in the working chamber 33 and that of the control pressure chamber 29 is proportional . accordingly , the pressure difference adjusted across the metering cross section of the fuel metering valve 21 is proportional to the square of the induction tube pressure . in order to insure satisfactory and rapid action of the various elements , the communicating lines between the control pressure chamber 25 and the pressure chamber 29 as well as between the working chamber 33 and the upstream side of the metering valve 21 are kept as short as possible so as to reduce throttling effects and thereby to prevent large deviations of the pressures at the metering valve from the pressure difference set by the differential pressure valve . as already mentioned , the metering valve is actuated by a control device 52 . the latter causes cyclic actuation of the valve by means of control pulses of variable width and of rpm - dependent frequency . an rpm transducer 54 senses the prevailing engine speed . the variation of the pulse width takes place in dependence on an operational parameter , for example the exhaust gas composition . for this purpose , the control device 52 receives signals from a per se known oxygen sensor 55 which responds to different oxygen partial pressures and which generates an abrupt signal in the transition from an excess of oxygen to a shortage of oxygen in the exhaust gas at a point where the air factor λ = 1 . in known manner , the pulse width of the fuel control pulses generated by the control device 52 is changed on the basis of the oxygen sensor signal . the above - described apparatus provides fuel into the induction tube in direct proportion to the air flow rate through the induction tube . this will be understood from the consideration that the aspirated air flow rate is proportional to the induction tube pressure and to the engine speed ( rpm ). however , the flow cross section of the metering valve 21 is also made proportional to the engine rpm . this is done by providing valve - opening control pulses at an rpm - dependent frequency , with the pulse width assumed constant for the time being . in the same manner in which the aspirated air quantity is proportional to the induction tube pressure , the pressure difference at the fuel metering cross section is such that its square root is proportional to the induction tube pressure . this is done , as described , by varying the force exerted on the diaphragm 32 of the differential pressure valve 31 . thus , the fuel quantity which is provided in proportion to the aspirated air flow rate can be influenced in accordance with the magnitude of an operational variable of the engine by changing the width of the control pulses in a multiplicative manner . in the present exemplary embodiment , this is done by using the oxygen sensor output voltage . however , the process could be performed by using other operational parameters , which have an influence on the exhaust gas composition . this could be , for example , in particular , the control variable of a per se known control process based on engine speed fluctuations . if the rpm signal is superimposed on the processed signal of , for example , the oxygen sensor , a continuous analog adjustment of the flow cross section at the fuel metering valve 21 may also be performed with a similar result . furthermore , the entire fuel supply of the engine may take place solely by means of the fuel metering valve 21 . advantageously , the fuel line 19 terminates in a bypass channel 16 associated with the carburetor 6 . in this way , even relatively low flow rates result in high air speeds which guarantee adequate preparation of the fuel in the fuel - air mixture . the apparatus described here can be adapted in simple manner as a supplementary device to an already existing carburetor system . it offers a wide control domain and a high degree of effectiveness in all load and speed regions of the engine . the foregoing relates to preferred exemplary embodiments of the invention , it being understood that other embodiments and variants are possible within the spirit and scope of the invention . | 5 |
referring now to the drawings wherein like reference numerals are used throughout the various views to designate like parts and , more particulary , to fig1 according to this figure , a scaffold generally designated by the reference numeral 10 includes a plurality of spaced posts 11 joined by conventional transverse elements , customary corner joints , and railing bars 16 . rectangular scaffold platforms 12 . 1 , 12 . 2 , forming two scaffold panels a , b are suspended , in a conventional manner , by drop in claw means 13 accommodated in upwardly open u - shaped supporting span members 14 extending between adjacent support posts 11 , with the posts 11 each being provided with conventional support feet 15 . as shown in fig1 the two scaffold panels a , b are set up at a mutual angle of 90 ° and are provided in this case , for example , with only one scaffold platform deck . the corner zone c must be bridged and comprises diagonally extending railing bars 16 as well as a corner platform section 117 including along one rim thereof a drop - in edge 18 with drop - in claws 13 , by which the corner platforms section 117 is suspended in this marginal zone in the upwardly open u - shaped supporting cross - pieces 14 . in the embodiment of fig2 a simple corner platform section 17 , suited for bridging corner zones of up to 45 °, is made of a uniform , slip - proof sheet - metal part and is cut to size in such a way that the corner platform section 17 includes , along a drop - in edge 18 thereof , the conventional width dimension gb of a customary scaffold platform panel width . in a first zone , the corner platform section 17 is defined along the side by lateral sections 19 . 1 and 19 . 2 adjoining at a right angle . the lateral section 19 . 2 has such a length between adjacent posts 11 . 1 , 11 . 2 that the lateral section 19 . 2 still extends to the scaffold platform 12 . 2 . at that location , the lateral section 19 . 2 has a supporting edge generally designated by the reference numeral 20 cut at an angle of 45 °. the supporting edge , as shown most clearly in fig8 is provided with an obliquely downwardly beveled marginal leg 21 resulting in a free spacing h at the bottom , so that the corner platform section 17 lies above the lower transverse connecting tube 22 of the posts 11 of a frame once the lateral section 19 . 2 has been suspended in place . the fourth boundary edge 23 ( fig2 ) extends from an outer corner point 24 of the supporting edge 20 to a corner point 25 of the lateral section 19 . 1 . in this arrangement , the position is chosen so that the post 11 . 3 is not impeded by the boundary edge even in different swiveling positions , when the angles become smaller . thus , relatively large angles , as well as minimally small angles can be readily bridged by means of a simple sheet - metal part that has been suitably cut to size and is somewhat beveled . the outer rims formed by the lateral section 19 . 1 and by the boundary edge 23 can be provided with an upwardly projecting , beveled leg ( not shown ) functioning as an edge board to prevent lateral slippage . as shown in fig5 the a corner platform section 117 may include a drop - in zone generally designated by the reference numeral 26 and include a platform plate 27 having a thickness of , for example , 3 - 5 mm . the drop - in zone 26 is provided at a rim 28 forming the drop - in edge 18 with a supporting leg 29 bent downwardly at a right angle . drop - in claws 13 are welded in place forwardly of the supporting leg 29 at an end face thereof , with the drop - in claws 13 being adapted to rest on upper , rounded edges 14 . 1 of the u - shaped supporting span members 14 . the supporting leg 29 has such a length that it exhibits at the bottom an outwardly projecting , being again bent into the horizontal , outwardly projecting lift - preventing leg 30 , with a position and length of the lift - preventing leg 30 being dimensioned to that the lift - preventing leg 30 lies , when dropped in obliquely from the top , in its final horizontal position by several millimeters below the bottom edge of the upwardly open u - shaped supporting span member 14 , as shown in fig5 thereby preventing corner platform section 117 from tipping . like arrangements are provided on all corner platform sections to permit dropping in and to prevent lifting off and tipping . in contrast to the corner platform section 17 according to fig2 the corner platform section 117 &# 39 ; of fig3 and 4 has a somewhat different contour line and is suitable for bridging larger angles of up to 90 ° while nevertheless permitting bridging of small angular ranges . in the arrangement of fig3 and 4 , a lateral section 19 . 2 &# 39 ; is positioned at an angle a of 135 ° so that the lateral section 19 . 2 &# 39 ; extends , in case of all scaffolds under consideration , just barely beyond the support posts 11 , even if two support posts are standing side - by - side . the supporting edge 20 with its edge leg 21 here extends with respect to the drop - in edge 18 at an angle of 90 ° and is arranged to be positioned farther outwardly so that this edge 20 rests on the scaffold platform 12 . 2 lying around the corner . furthermore , a boundary edge 23 &# 39 ; is here ex - tended in a straight line at a precise angle of 45 ° so that an outermost corner point 125 is located in such a way that the associated supports 11 , together with their attachments lying in the corresponding plane , can just barely be swung past . the boundary edge 23 &# 39 ; is provided with an upwardly bent border leg 35 of the type of an edge board and , in a zone of the boundary edge 23 , provided with border legs 35 , is followed , without border legs , by a linear section 36 swung further inwardly and associated with a pivotable member 37 . the pivotable member 37 permits , as shown in fig3 and 4 , a varying angular position for an optimum bridging of the remainder of the marginal zone because , for example , in case of angular positions of merely 45 ° according to fig4 the linear section 36 lies centrally on the surface . the pivotable member 37 has an upwardly projecting border leg 38 and is articulated , lying therebelow , with the aid of a continuously extending joint 39 , to the floor plate 27 , as shown in fig3 - 5 . in the embodiment of fig6 and 7 , frame scaffolds are provided having respectively two posts 11 . 1 and 11 . 2 , as in fig2 . however , the structure , position , and function are identical , and the two usage positions at 45 ° and at 90 ° are illustrated with the respective swivel position of the pivotable member 37 , where it can be seen even more clearly how the border leg 38 adjoins with its end 38 . 1 the actual edge board 40 of the primary scaffold . in fig9 a version similar to fig3 and 4 , a pivotable member 41 has a greater length and lies with a point of articulation 42 directly at the outer corner of the drop - in edge 18 . a sliding joint 43 with a slotted hole having the shape of a divided circle secures the connection . for certain constructions and angular ranges , such a solution may be expedient . a scaffold corner platform section generally designated by the reference numeral 47 in fig1 - 14 differs from the scaffold corner platform section described hereinabove in that the scaffold corner platform section 47 is composed of two circular 12 segments or components 50 . 1 , 50 . 2 of sheet metal superimposed in an overlapping zone 49 , with the two circular segments or components 50 . 1 and 50 . 2 respectively having an externally located drop - in edge 48 . 1 , 48 . 2 and supporting legs 29 , 29 . 2 . both supporting legs 29 , 29 . 2 have drop - in claws 13 fitting with the scaffold system and mounted in a suitable arrangement . the supporting leg 29 of the larger component 50 . 1 includes a lift - preventing leg 30 and is suspended in place in the same manner as described hereinabove . the supporting leg 29 . 2 is constructed without lift - preventing legs so that the corner platform section 47 can be swung or pivoted inwardly in a manner described hereinabove and can rest on both sides on the drop - in claws 13 on the edges 14 . 1 of the u - shaped supporting span members 14 . the two circular segments or components 50 . 1 , 50 . 2 each terminate in an outer boundary 51 . 1 , 51 . 2 extending in the shape of a divided circle , with a center of the divided circles being a center 52 of the corner supporting post 11 . 4 as shown most clearly in fig1 and 11 . in this scaffolding , the pivoting action when setting up at non - linear facades or the like takes place in each case about the center 52 of the supporting post 11 . 4 between two scaffold panels and thereby the corner arrangement is built up so that the corner platform section 47 can be fittingly suspended in place . when employing scaffoldings wherein two supporting posts , or the posts of two frames , are in close juxtaposition , a suitable center in their proximity is to be defined for fashioning the corner platform section . concentrically to the center 52 , a slotted hole 53 having the shape of a divided circle extends in the component 50 . 1 , with the slotted hole 53 extending to approximately the drop - in edge 48 . 1 and approximately the internal boundary 51 . 3 as shown most clearly in fig1 and 11 . a retaining pin generally designated by the reference numeral 54 passes through the slotted hole 53 , with the slotted hole 53 being curved in the manner of a partial circle . a rounded head 55 of the retaining pin 54 rests , through the interposition of an adequately large washer 56 , above rims of the slotted hole 53 on a surface of the circular segment or component 50 . 1 . a simple through hole or passage 58 is arranged in the sheet metal of the other circular segment or component 50 . 2 lying there below . a shank 57 of the retaining pin 54 extends through the through hole or passage 58 , with the entire arrangement being mounted on an underside with a washer 59 . 1 firmly braced against a shoulder and with a nut 59 . by virtue of this arrangement , a flexurally rigid connection is obtained between the two circular segments or components 50 . 1 and 50 . 01 in the inner end zone of the corner platform section 47 which can nevertheless be pivoted about the center 52 through an arc . the external , slidable and flexurally rigid connection is formed together with a border leg generally designated by the reference numeral 60 of the corner platform section 47 . for this purpose , border legs 60 . 1 and 60 . 2 , respectively , are formed , projecting upwardly , at both components 50 . 1 and 50 . 2 in the external zone , of a height corresponding to the remaining scaffolding and safety ; as is also shown in fig1 and 14 . in this arrangement , the component 50 . 2 lying at the bottom is provided with an externally located border leg 60 . 2 equipped at the top with overlapping legs 61 . 1 and 61 . 2 holding the sliding joint together and extending to the inside of the inwardly located border leg 60 . 1 from above . in order to obtain a readily operable sliding joint , supporting nubs 62 . 2 are embossed which project from the surface toward the border leg 60 . 1 so that two point - like contact sites are produced . the two overlapping legs 61 . 1 and 61 . 2 lie at a small angular spacing , as shown especially in fig1 , so that they both still engage securely at the border leg 60 . 1 even in the smallest overlapping range 49 . if the corner platform section 47 is further swiveled together due to a larger or smaller angle between the scaffold panels , as is possible up to the final position illustrated in fig1 , then the supporting nubs 62 . 2 are entirely within the neighboring zone of the drop - in edge 48 . 1 . in this position , the component 50 . 1 located on top is swung so far over the component 50 . 2 that its outer end 63 comes to lie above the scaffold platforms 12 . 2 of the adjoining panel , as shown in fig1 . this arrangement , which seems somewhat more 5 complicated in structure , provides readily surveyable supporting conditions , but requires a firm , flexurally rigid connection among the components which is safely slidable over a long period of time so that this connection can meet the needs in the rough realm of the 10 building trade over many years . for this reason , the arrangement does not employ the principle of support on the neighboring scaffold platform . this arrangement displays a clear edge board boundary which in all cases extends past the linear corner railing and always has a border leg arrangement which is continuous over the entire length . in the embodiment of fig1 and 16 shows a corner platform section generally designated by the reference numeral 67 essentially corresponds to the corner platform section 117 of fig6 with respect to its configuration ; however , in place of the drop - in claws 13 of the embodiment of fig6 this arrangement includes drop - in eyes 68 mounted at a spacing 69 to the supporting leg 29 . 3 of the corner platform section 67 along one edge , as is customary , for example , by welding , screws , or by rivets . the drop - in eyes 68 have vertical passage bores engaged by vertical retaining pins 70 fastened by , for example , welding on the outside to the supporting cross - pieces 71 at a suitable spacing . the supporting cross - pieces 71 are attached to posts 11 . 5 of a scaffold support in the neighboring panel , this support being fashioned , for example , in the shape of a frame . also the remaining scaffold platforms are mounted to retaining pins 70 by drop - in eyes . this type of mounting is provided for the corner platform section generally designated by the reference numeral 67 only on one drop - in edge . such mounting can also be provided identically at the second drop - in edge in a corner platform section having the configuration according to fig1 - 14 . as shown in fig1 , the scaffold floor 12 . 3 is retained by identical drop - in eyes 68 . a round , horizontally extending cross connection tube 73 pertains to the supporting structure of the scaffold and usually establishes the connection of the posts in their lower region for the formation of frames . the cross connection tube 73 serves simultaneously as a securing means against lifting off . the bottom plate 27 of the corner platform section 67 extends , exactly as has been described in connection with fig8 over this cross connection tube 73 . the other embodiments of corner platform sections can likewise be equipped with like drop - in eyes or other connecting means for the respective scaffolding . the connecting means or suspension means for connecting the corner platform part with the supporting span members 14 or the like can also have other shapes and can be designed as differently shaped hooks or eyes or as beads , prisms , or other drop - in shapes . they can also be designed as double claws , double hooks , double beads , or double prisms or the like as are usually employed for scaffold systems and which correspond to the receiving area and the cooperating fastening means , which ensure that the applied forces are supported and lifting up is prevented , for example , by transverse components , which after assembly are located so close to the suspension means that the latter can no longer be lifted out of the secured position of use . for example , as shown in fig1 , suspension double prisms generally designated by the reference numeral 75 can be fastened to supporting legs 29 , with the prisms 75 being formed , for example , from a multiple bent sheet metal section . the suspension double prism 75 is designed to be symmetrical to horizontal center 76 and has on each side , a depression 77 . 1 or 77 . 2 , with the depression 77 . 1 being designed as a suspension depression for resting on edge 14 . 1 of a u - shaped supporting span member 14 . downwardly projecting securing part 78 . 1 has a roughly triangular shape , with a lower edge 82 thereof being located at a distance 83 below the edge 14 . 1 of the support span member 14 . outer limiting wall 79 is vertical and blends with an upper securing part 78 . 2 which is likewise roughly triangular in shape . then , as shown in fig1 , only a small space 80 is left with respect to the transverse connecting tube 81 , with the transverse connecting tube 81 lying between the posts ( not shown ) and preventing , as can be seen , the suspension double prism 75 from being lifted out of the locking position because space 80 is much smaller than the distance 83 . the locking action also operates on the one side shown here of lift - preventing leg 30 . as can be seen , corner platform parts of any of the embodiments mentioned can also be fitted with suspension means known of themselves , as in fig1 . | 4 |
the present invention is more particularly described in the following examples that are intended as illustrative only since numerous modifications and variations therein will be apparent to those skilled in the art . various embodiments of the invention are now described in detail . referring to fig1 , the phase measurement calibrating method based on the lcs principle in accordance with the present invention is illustrated as follows : the phase measurement calibrating method adopts single - emission and single - receiving double light paths , the light wave emitter generates respectively the internal and external light path beam , and the receiver receives respectively the internal and reflected external light path beam and then compares them . by eliminating a fundamental reference caused by the phase drift , the phase difference is right for phase compensation and phase calibration . in the step 101 , the light wave emitter generates the light wave which arrives at the tested target through the first lcs , and a part of the light wave is reflected by the tested target before received by the receiver , as the external light path beam of the measurement system , wherein the light wave is generated by modulating high - frequency oscillation signal . in the step 102 , a part of the light wave is passing through the second lcs before being received by the receiver at the time as a part of the light wave is through the first lcs , wherein the light wave is as the internal light path beam for fundamental reference of the system phase measurement , which is generated by modulating high - frequency oscillation signal . in the step 103 , the receiver compares phases of the internal and external light path beam received respectively to output phase shift for eliminating a fundamental reference . in the embodiment of the invention , the internal and external light path beams could be mixed with mixing signals , wherein the mixing signals could be the same high - frequency oscillation signal , or the same frequency and phase signal with a stable phase difference . in the embodiment of the invention , both internal and external light path beams are laser . in the embodiment of the invention , the receiver could receive either the internal light path beam or the external light path beam at first , wherein the receiver could be light emitting diode , light emitting triode , apd , optoelectronic multiplier , or the like . fig2 is a schematic diagram of the double - emission and single - receiving phase measurement calibrating device based on the lcs principle in accordance with the present invention , in order to illustrate conveniently , this drawing only discloses information related to the embodiment of the invention , a high - frequency oscillation signal is modulated into the light wave , the light wave arrives at the tested target through the first lcs , as the external light path beam ; and at the same time a part of the light wave is reflected by the first lcs and then passes through the second lcs , as the internal light path beam . the optoelectronic converter respectively coverts the internal and external light path beams for outputting to the phase discriminator , then the phase discriminator compares phases of the internal and external light path beam received respectively to output phase shift for eliminating a fundamental reference . in the embodiment of the invention , the light wave emitter includes a clock generator , a modulator module circuit and a light source , wherein the driver drives the light - emitter to emit light , the light wave emitter of the present invention could be laser diode ( ld ), light emitting diode ( led ) and other light - emitting element . both the first and second lcs includes a driving circuit , lcs , and an assistant optical element , wherein the assistant optical element help to make the first and second lcs in a closed system as a whole . the lcs could be crystal optoelectronic switch or other electro - optic switch . in the embodiment of the invention , both the first and second lcs are directed to the optoelectronic converter , so that the light wave straight reaches the optoelectronic converter . there may be a reflector between the second lcs and the optoelectronic converter in order to change the light path , that is convenient to be received by the optoelectronic converter . otherwise , there could be optical signal transmission lines connecting the second lcs and the optoelectronic converter , and the optical signal transmission lines maybe optical fiber or light line . the optoelectronic converter could be light emitting diode , light emitting triode , apd , optoelectronic multiplier , or the like . the optoelectronic converter could receive either the internal light path beam or the external light path beam at first . fig3 shows one phase measurement calibrating device based on the lcs principle comprising : the oscillator , the light wave emitter , the first lcs , the second lcs , the optoelectronic converter , the high - frequency amplifier , the mixer , the low - frequency amplifier , and the phase discriminator . in order to illustrate conveniently , fig3 only discloses information related to the embodiment of the invention . the oscillator generates a first and second high - frequency oscillation signal of the same frequency and phase , and the light wave emitter receives the first high - frequency oscillation signal and modulates into light wave , then emits as optical signal . the optical signal arrives at the tested target through the first lcs , and then is reflected by the tested target , and the optoelectronic converter receives reflected optical signal , as external light path beam . the external light path beam is converted to electronic signal as high - frequency signal . the high - frequency amplifier amplifies and outputs the electronic signal from the optoelectronic converter . then the mixer mixes the high - frequency amplified signal with the second high - frequency oscillation signal . the mixed signals are amplified by the high - frequency amplifier after being into the phase discriminator . at the same time , a part of the light wave is reflected by the first lcs and then passes through the second lcs , as the internal light path beam , then the phase discriminator discriminates respectively the internal and external light path beam to output phase shift for eliminating a fundamental reference . in the embodiment of the invention , the oscillator could be crystal , crystal oscillator , phase - locked loops ( pll ), direct digital frequency synthesis ( dds ), or other frequency generator and circuit . in the embodiment of the invention , the mixer could be analog multiplier , down - conversion mixer , or other electric mixer , such as light emitting diode , light emitting triode , apd , optoelectronic multiplier , and as the like , i . e ., s9717 hamamatsu , ad230 and ad500 silicon sensor . in the embodiment of the invention , the optoelectronic converter and the mixer could be instead of the receiver which can meet the two functions of the optoelectronic converter and the mixer simultaneously , such as s9717 hamamatsu , ad230 and ad500 silicon sensor . the receiver could be light emitting diode , light emitting triode , apd , and pmt as the like , for example , s9717 hamamatsu , ad230 and ad500 silicon sensor . in the embodiment of the invention , the high - frequency amplifier is used for receiving and amplifying the high - frequency signal , while the low - frequency amplifier is used for amplifying the low - frequency mixed signal . the high - frequency amplifier is expensive as compared to the low - frequency amplifier . both the high - frequency amplifier and the low - frequency amplifier may be not adopted , or one of them may be not adopted , in the condition that other elements of the circuit have good properties . the high - frequency amplifier could not utilized if the receiver would instead the optoelectronic converter and the mixer , and then the receiver is straight connecting the low - frequency amplifier , which will makes cost down . fig4 shows the second embodiment of the invention . the phase measurement calibrating device includes the oscillator , the light wave emitter , the first lcs , the second lcs , the low - frequency amplifier and the phase discriminator . in order to illustrate conveniently , fig4 only discloses information related to the embodiment of the invention . the phase measurement calibrating device is further including an optoelectronic mixer used for respectively receiving internal and external light path beams , wherein the external light path beam is reflected by the tested target , then the internal and external light path beams are respectively mixed with mixing signal for outputting . in this embodiment of the invention , the optoelectronic mixer is instead of the optoelectronic converter and the mixer , such as s9717 hamamatsu , ad230 and ad500 silicon sensor . referring to fig5 - 7 , the structure of the phase measurement calibrating device based on the lcs principle includes pll and driving circuit , which drive the light wave emitter to generate light wave by the high - frequency oscillation signal , a part of the light wave passes through the first lcs as the external light path beam when a part of the light wave is reflected by the first lcs simultaneously . the reflected light wave is through the second lcs as the internal path light wave . the internal and external light path beams are respectively received by a receiver , and then are into a bias circuit . the internal and external light path beams mix with a high - frequency mixing signal from pll and implement optoelectronic conversion . then the internal and external light path beams are amplified by the low - frequency amplifier for outputting to the phase discriminator . at the end the phase discriminator compares phases of the internal and external light path beam received respectively to output phase shift for eliminating a fundamental reference . in the embodiment of the invention , the light wave emitter generates light wave to through the first lcs and aims to the receiver , so the light wave arrives at the receiver directly . referring to fig6 , there might be a reflector group between the second lcs and the receiver to change the light path , that is benefit for receiving . referring to fig7 , there may be optical signal transmission lines connecting the second lcs with the receiver , and the optical signal transmission line could be optical fiber , light line , or other optical element . in these embodiments of the invention , the first lcs is used to put throughout off the external light path beam , and the light wave emitter generates light wave , and a part of the light wave is through the first lcs to reach the receiver directly . any embodiment as shown in fig8 - 10 has the same function as the embodiment as shown in fig5 , wherein the position of the first lcs or the second lcs has changed . referring to fig8 , there is a beam - splitter added in transmission path of the external light path beam in order to divide internal light path beam from the external light path beam . the first lcs is used to put throughout off the external light path beam . fig9 shows that the internal light path beam is reflected by the reflector and then through the second lcs , the second lcs is used to put throughout off the internal light path beam . fig1 shows that the second lcs is disposed in the back of optical signal transmission line to put throughout off the internal light path beam . according to the above embodiments , the position of the first lcs in transmission path of the external light path beam can be changed in order to put throughout off the external light path beam , and the position of the second lcs in transmission path of the internal light path beam can be changed in order to put throughout off the internal light path beam . the single - emission and single - receiving phase measurement calibrating device based on the lcs principle , as shown in fig5 and fig8 , is used for calibrating measuring device , such as continuous phase - laser measuring distance device and pulse laser phase - laser measuring distance device . and the phase measurement calibrating device combining with the measuring device can implement phase compensation due to the influence of environmental factors . in the embodiments of the invention , control circuit could be adopted to put throughout off the internal or external light path beam instead of the mechanical switch , and the control circuit makes the response time short , and there is short interval up to millisecond level between the receiving of the internal and external light path beam , so that the environment is thought to keep the same during circuit switching and the circuit doesn &# 39 ; t influenced to obtain good measurement accuracy . the single - emission and single - receiving phase measurement calibrating device has short interval up to millisecond level , which removes the influence of common mode between apd and ld , so the measurement accuracy is higher than the way adopts double apds or double lds . referring to fig1 - 13 , the phase measurement calibrating device based on the lcs principle is comprising of the light wave emitter 1 , the optoelectronic converter , the first lcs , the second lcs , the phase discriminator , the mixer , the receiver , the oscillator , and the amplifier , all of which are mounted on a base . a lens 2 is on the front of the light wave emitter 1 , and the first lcs is on the front of the lens , when the light wave arrives at the tested target through the first lcs . the light wave reflected by the tested target passes through a receiving lens 5 mounted on the base . the receiver is on the back of the receiving lens 5 , and there is another lens 6 disposed on the front of the receiver 7 . the second lcs is disposed between the first lcs 3 and the receiver 7 . the phase discriminator adopts fourier transform to compute phase . ti &# 39 ; s single - chip msp430 or silicon lab &# 39 ; s single - chip c8051 or other equivalent chip can be chosen as microprocessor with integrated analog - to - digital converter . either the mixer or the optoelectronic converter could be s9717 hamamatsu , ad230 or ad500 silicon sensor . the receiver consists of the mixer and the optoelectronic converter , and the receiver could be s9717 hamamatsu , ad230 , or ad500 silicon sensor . the oscillator could be ti &# 39 ; s cdce925 pll , or fujitsu &# 39 ; s mb15 pll . the amplifier could be ti &# 39 ; opa354 , ti &# 39 ; opa357 , or adi &# 39 ; s ad8065 . the light wave emitter receives the first high - frequency oscillation signal and modulates into light wave , then a part of the light wave reaches the tested target through the first lcs as external light path beam ; when a part of the light wave is reflected by the first lcs and then passes through the second lcs , as internal light path beam . the optoelectronic converter receives the external and internal light path beam and then converts them into electronic signals for output and the phase discriminator receives the internal and external light path beam respectively and then compares phases of the internal and external light path beam to output phase shift for eliminating a fundamental reference . in the embodiment of the invention , both the first and second lcs are directed to the optoelectronic converter , so that the light wave straight reaches the optoelectronic converter . there might be one or more reflectors between the second lcs and the optoelectronic converter in order to change the light path , that is convenient for the light path to be received by the optoelectronic converter . otherwise , there could be optical signal transmission lines connecting the second lcs and the optoelectronic converter , and the optical signal transmission lines may be optical fiber or light line . the embodiments were chosen and described in order to explain the principles of the invention and their practical application so as to enable others skilled in the art to utilize the invention and various embodiments and with various modifications as are suited to the particular use contemplated . alternative embodiments will become apparent to those skilled in the art to which the present invention pertains without departing from its spirit and scope . accordingly , the scope of the present invention is defined by the appended claims rather than the foregoing description and the exemplary embodiments described therein . | 6 |
the present application discloses a novel method for inducing band - gap shifting as well as for fine band - gap tuning in iii - v semiconductor material microstructures . the microstructures of primary interest are quantum - well - based active devices , such as lasers , detectors , amplifies , modulators , etc . other non -( iii - v ) material microstructures , which comprise quantum wells ( qw ), e . g ., si / sige or cdte / insb , are of interest as well . by way of example , and in accordance with the present invention , a qw material 10 to be tuned is first irradiated with an uv beam 12 and then subjected to thermal annealing in furnace 14 ( fig1 a ). the irradiation can be realized with a pulsed laser , such as excimer or high - harmonic ir laser , or a continuous radiation from an uv lamp ( e . g ., an excimer lamp ). the advantage in using an excimer laser is that it can process relatively large areas is one step , similarly to the area coverage achieved by the excimer - based photolithography technique . the purpose of the irradiation is to : a ) introduce defects at the sample surface or in the sub - surface region ; b ) modify the surface of the sample in such a way that it can act either as a source or sink of defects that are activated during thermal annealing the important feature of this method is that the “ defect reservoir ” 16 created by the uv radiation is localized within a shallow depth from the surface , for example , 100 nm or less and typically 20 nm or less . also , in addition to the ability to fabricate a defect - rich layer near the surface of the irradiated sample , the uv process can be used to induce chemical changes and / or the growth of a thin film on top of the processed sample . the composition of such film can be chosen to achieve the maximum intermixing effect . the selective irradiation of the sample is obtained either by scanning a focused laser beam , or by projecting suitable patterns using a mask technique ( projection or contact ). following uv irradiation procedure , the sample is thermally annealed ( fig1 b , 1d or 1 e ) in order to realize a defect - mediated process of intermixing between atoms at the quantum well - barrier heterointerface . during this step , the intermixing of the well and barrier material takes place as a result of a defect - mediated diffusion . the important feature of this process is that the diffusion occurs at temperatures that are too low to induce any changes in areas that had not been exposed to the uv radiation . as a result of the intermixing the shape of the quantum well layers is modified , which results in a change of their ground state energy levels ( band - gap structure ). the extent of the intermixing and modification of the band - gap structure is controlled by both the composition of the uv - formed thin film and / or concentration of defects on top of the processed sample . the process of intermixing can be achieved is several steps consisting of uw irradiation and thermal annealing , which makes it possible to realize a fine band - gap tuning . both the process of uv irradiation and thermal annealing can be carried out in the same chamber , without changing the position of the sample , until the required parameters of band - gap shifting have been achieved . the sample discussed in fig1 was grown by chemical beam epitaxy . it includes 5 quantum wells of ingaas that are embedded between ingaasp barrier layers . other qw - based semiconductor laser materials that could be processed with this technique include : algaas / gaas , algaas / ingaas , algainp / gaas . in addition , si / sige qw material could also be processed with this technique . uv irradiation was carried out with a krf excimer laser ( λ = 248 nm ) delivering 30 ns pulses . pulse energy ( fluence ) at the sample surface was about 100 mj / cm 2 . the results shown in fig2 concern the photoluminescence measured at room temperature from the uv irradiated sample ( fig2 a ) and from the same sample following 10 sec rta at 750 ° c . two sites , which can be seen in fig2 b , were irradiated with 500 and 1000 pulses ( site 1 and 2 , respectively ). the irradiation was carried out using a laser mask projection technique , which offers a significant advantage over other techniques applied for selective area intermixing , such as ion implantation ( the need of a mask being in physical contact with the sample ) or oxide layer ( the surface of the sample has to be patterned with the oxide ). it can be seen that the uv irradiation alone does not introduce any changes detectable with the photoluminescence mapping ( fig2 a ). most of the 5 × 6 mm sample is characterized by the quantum well signal at λ = 1505 nm . the sample is affected only to a minor extent following a 10 sec annealing at 750 ° c ., with the majority of the background quantum well signal located at λ = 1499 nm ( fig2 b ). however , two blue - shifted areas , each approximately 2 . 0 × 1 . 5 mm , of the intermixed material can clearly be seen in this figure . the 500 ( site 1 ) and 1000 ( site 2 ) pulse areas are characterized by the quantum well signal at 1476 and 1449 nm , respectively . at this stage , the sample could be annealed for the second time in a rta apparatus , as indicated in fig1 b , or selected areas could be annealed with an ir laser , as indicated in fig1 d . the use of an ir laser for fine tuning makes possible the realization of intermixing in selective areas without affecting each other . one skilled in the art may therefore increase the demand for a material with band - gap shifted regions that are far beyond limits possible with other technologies . an important aspect of the novel tuning method is that the whole process of band - gap tuning can be realized with the “ laser only ” approach . this is schematically illustrated by the step a - e in fig1 . the novel approach exemplified above simplifies the whole procedure of band - gap tuning , allows for the application of a more efficient in - situ diagnostics , leading to a more efficient , precise and , potentially , less expensive process . the invention also allows the processing of industrial size semiconductor wafers 3 inch diameter and more . it is to be understood that the above description is intended to be illustrative , and not restrictive . many other embodiments will be apparent to those skilled in the art . | 7 |
the steering lock shown in fig1 a comprises an electric motor 10 furnished with an output shaft forming a worm 15 , a gearwheel 20 engaged on the worm 15 , and a bolt 30 mounted slidingly , these various elements being placed in a housing not shown . the gearwheel 20 is mounted so as to rotate about a shaft 21 which extends perpendicularly to the output shaft of the motor 10 such that the output shaft of the motor is indistinguishable in the geometric plane of the wheel . the wheel 20 has a first face 22 , turned toward a steering column not shown , which is furnished with a cam 23 in a disk portion which interacts with the bolt . accordingly , the bolt 30 has , in addition to a main bar 31 , a lateral appendage 32 capable of being interposed , at its first end 33 , onto the path of the cam 23 when the latter pivots with the gearwheel 20 . the lateral appendage 32 is pushed against the cam 23 under the effect of the return spring 40 which returns the bolt 30 to the locked position . this interaction of the lateral appendage 32 of the bolt 30 with the cam 23 therefore has the effect of bringing the main bar 31 closer to an outer ring gear 50 of the steering column . in an alternative embodiment not shown , the cam 23 is replaced by a gradient . the steering lock also comprises a control unit advantageously implemented in the form of an electronic circuit placed in the housing . in addition to implementing the control of the electric motor 10 , the control unit also takes account of the information supplied by an indexation device . this indexation device makes it possible to inform the motorized control unit that the gearwheel has reached a position allowing the main bar 31 of the bolt to carry out the locking and the unlocking . in response to this information , the control unit commands the stopping of the motor . this indexation device essentially comprises a movable indexer 60 interacting with two sensors not shown of which one is used for detecting the position called the unlocked position and the other for the detection of the position called the locked position . the position called the unlocked position is illustrated in fig3 a and corresponds to a position in which the main bar 31 of the bolt 30 is at a distance from the outer ring gear of the steering column . as can be seen also in fig3 b and 3 c , the ring gear 50 of the column consists of grooves 51 surrounded on either side by teeth 52 . the locking of the column takes place when the main bar 31 of the bolt 30 is at the bottom of a groove 51 , resting against an interstice of the ring gear 50 , thus preventing the ring gear 50 and hence the column from rotating . in certain conditions , although the gearwheel has reached the position called the locked position , the main bar 31 of the bolt 30 may be resting on a tooth 52 of the ring gear 50 . this position is called the rtl ( ready to lock ) position . specifically , in this position , the column can be rotated . however , as is conventional , if the steering wheel connected to the column is operated , a brief angular travel of the latter will have the effect of placing a groove 51 in line with the main bar 31 of the bolt 30 so as to allow the latter to fit into this groove 51 . this fitting will take place with the aid of the return spring 40 of the bolt . the movable indexer 60 advantageously consists of a bar extending longitudinally parallel to the sliding axis of the bolt 30 , a first end 61 of the movable indexer 60 pressing on the cam 23 of the gearwheel 20 . the movable indexer 60 is held , at its first end 61 , pressing on the cam 23 by a return spring 62 , advantageously placed on the second end of the movable indexer 60 . it is also on this second end that a magnet 63 is placed . in this case , the two indexation sensors are of the hall effect or reed switch type . in an alternative embodiment , a boss is placed on the second end of the indexer 60 , and the two magnetic sensors are replaced by mechanical commutators . thus configured , the movable index 60 will , under the rotary action of the gearwheel 20 , follow the contour of the cam 23 and move in a direction parallel to the sliding direction of the bolt 30 . in one advantageous embodiment , notably for requirements of compactness , the movable indexer 60 is placed so as to slide freely in a groove 34 arranged on the lateral appendage 32 of the bolt 30 . starting from an unlocked position illustrated in fig1 a and 2 a , and to reach a locked position illustrated in fig1 b and 2 b or fig1 c and 2 c , the gearwheel 20 will turn in the clockwise direction . the end 33 of the lateral appendage 32 of the bolt 30 and the end 61 of the movable indexer will both initially follow the contour of the cam 23 and respectively drive the bolt 30 and the movable indexer 60 to slide parallel in the same direction . as illustrated in fig1 c and 2 c , because the movable indexer 60 slides freely in the groove 34 arranged on the lateral appendage 32 of the bolt 30 , the movable indexer 60 can reach the locked position while the bar 31 is in the rtl ( ready to lock ) position , the motor will then receive a stop instruction via one of the sensors of the indexation device . in one advantageous embodiment , the steering - column lock is an element of forming a module for motorized assistance to the rotation of the steering column . incorporating the steering lock in a module for motorized assistance to the pivoting of the steering column provides an advantage in terms of safety since the steering lock is then in a particularly low portion of the steering column , at a particularly great distance from the instrument panel where a thief by predilection takes action and in a particularly inaccessible portion of the vehicle . as illustrated in fig3 , in this case the motorized assistance module comprises an assistance motor 70 which is oriented such that its output shaft 75 extends parallel to the steering column . the output shaft 75 of the motor 70 has peripheral gear teeth which mesh with a ring gear 50 surrounding the steering column in order to rotate the latter . the ring gear 50 is advantageously the ring gear in which the bolt engages such that only one ring gear is used for both functions of driving and immobilizing , further reducing the space requirement necessary for the implementation of the assistance module described . advantageously , the steering lock and the assistance motor are placed radially opposite with respect to the steering column , such that the bolt and the output shaft 75 of the assistance motor do not interfere . the motorized assistance module advantageously comprises one and the same electronic control unit for the assistance of pivoting and for controlling the immobilization of the column , which ensures that no assistance control is applied to the assistance motor when the steering lock is in the locked position . due to the fact that the steering - column lock , in this instance referenced 71 , is a portion of the module for motorized assistance to the rotation of the steering column , the control unit that is common to the motorized assistance and the locking of the steering column is advantageously fitted with a control logic applying a slight rotational movement of the steering column when it simultaneously controls a driving force to unlock the bolt . thus , by this slight movement , any frictional retention is removed between the bolt and the steering column , for example between the bolt and a lateral edge of a tooth of the ring gear 50 and the bolt slides reliably each time the vehicle is switched on . the control unit is advantageously implemented in the form of an electronic circuit placed in a common housing 80 of the assistance motor 70 and of the steering lock 71 . the electronic circuit is advantageously positioned outside the housing specific to the steering lock . in addition to implementing the control of the steering lock via this control unit notably in this instance takes account of the position of the bolt which is indicated to it by the receipt of output signals from the indexer positioning sensors as described above . naturally , many modifications can be made to the invention without departing from the context of the latter . | 8 |
the following description of the preferred embodiment is merely exemplary in nature and is in no way intended to limit the invention , its application , or uses . referencing fig1 , a passenger compartment 10 of a golf car 12 is shown . the passenger compartment 10 includes a seat 14 , a floor 16 , and a dash panel 18 , steering wheel 20 , a brake pedal 22 , and an accelerator pedal 24 . a non - skid floor mat 30 , designed in accordance with the principles of the present invention , covers the floor 16 of the passenger compartment 10 . with particular reference to fig2 , 3 and 3 a , the non - skid floor mat 30 will be discussed in detail . the non - skid floor mat 30 is formed of an elastomeric material 32 having an outer perimeter 34 shaped to conform with the floor 16 of the passenger compartment 10 . the floor mate 30 has the advantages of which are discussed in further detail herein below , but may also be formed of alternate materials . the non - skid floor mat 30 may include a steering wheel aperture 36 , a brake pedal aperture 38 , and an accelerator pedal aperture 40 . a series of attachment apertures 42 are positioned about the perimeter 34 for enabling fixed attachment of the non - skid floor mat 30 to the floor 16 . the non - skid floor mat 30 further includes a first section 44 having a flat surface 46 and a second section 48 having a flat surface 50 with a plurality of protrusions , or nibs 52 , extending upward therefrom . it is anticipated , however , that the flat surfaces 46 , 50 are textured of either or both of the first and second sections 44 , 48 may be rough , or otherwise textured . as best seen in fig3 a , the nibs 52 are generally semi - spherical in form with a sufficient radius . however , it is anticipated that the nibs 52 may take any one of a number of forms including , but not limited to , conical , frusto - conical , pyramid , truncated , cylindrical and the like at the bottom . as discussed in further detail below , each nib 52 is formed to fit within recesses of a soft spike . with particular reference to fig4 through 6 , a typical soft spike 60 of a golf shoe is shown engaging the nibs 52 of the non - skid floor mat 30 . soft spike 60 described herein is one of a number of soft spike configurations known in the art . the soft spike 60 generally includes a conical body 62 having a threaded post 64 extending upward therefrom , for threaded attachment with a golf shoe sole 66 . a series of ribs 68 extend downward from a conical face 70 of the soft spike 60 , thereby forming recesses 72 . as the soft spike 60 contacts the non - skid floor mat 30 , the nibs 52 are received into the recesses 72 of the soft spike 60 , as seen in fig5 and 6 , and as shown in phantom in fig4 . in this manner , the non - skid floor mat 30 provides traction for the soft spikes 60 , promoting passenger safety and comfort . it should further be noted that application of sufficient downward force through the soft spike 60 ( e . g . when passenger is standing ) enables the ribs 68 to contact the flat surface 50 between the nibs 52 concurrent to the nibs 52 engaging the recesses 72 . in this manner , improved traction is provided . as discussed briefly above , the nibs 52 are preferably semi - spherical in form for efficiently fitting within the recesses 72 . however , it is anticipated that other forms of the nibs 52 would suffice to fit within the recesses 72 for providing traction . for example , as shown in fig6 , partially frusto - conical nibs 52 are one possibility . more importantly , however , the size and spacing of the nibs 52 must be appropriate for enabling sufficient engagement between the nibs 52 and soft spike 60 , provide clearance to prevent a tripping hazard , and providing clearance for cleanability . additionally , spacing of the nibs 52 must be appropriate to enable hard spikes ( not shown ) to contact the flat surface 50 . in this manner , the non - skid floor mat 30 provides traction for both hard spike and soft spike golf shoes . to that end , the nibs 52 have a center - to center distance no greater than 0 . 80 inches . the center - to - center distance ensures that at least two nibs 52 , and optionally four nibs 52 , engage the recesses 72 of the soft spike 60 . additionally , the center - to - center distance ensures that a hard spike may pass between the nibs 52 for contacting the flat surface 50 , as well as enabling easy cleaning of the non - skid floor mat 30 . for example , if the nibs 52 were positioned too close together it would be difficult to remove dirt and debris deposited therebetween . further , the nibs 52 preferably have a height within the range of 0 . 12 to 0 . 19 inches . this height range ensures that there is adequate engagement between the soft spike recesses 72 and the nibs 52 . if the nibs 52 are too low , the non - skid floor mat 30 would fail to provide adequate traction . on the other hand , if the nibs 52 are too high , a soft spike may not move smoothly over the enon 0 skid floor mater 30 . similarly to the center - to - center distance , the height of the nibs 52 influences the cleanability of the non - skid floor mat 30 . if the nibs 52 are too high , removal of dirt and debris from between the nibs 52 is hindered . both the height and spacing of the nibs 52 are limited to prevent grabbing of the passenger &# 39 ; s golf shoe . as mentioned above , the non - skid floor mat 30 is formed using an elastomer component . the elastomeric material 32 provides toughness and wear resistance to extend the service life of the non - skid floor mat 30 . as an elastomer , the non - skid floor mat 30 is resilient and deformable for enabling improved traction . in the case of a hard spike , the tip of the hard spike may engage the flat surface 50 between the nibs , thereby gripping the non - skid floor mat 30 to provide traction for the passenger . if , however , the hard spike contacts a nib 52 , the hard spike can similarly project into the nib 52 , providing traction regardless of whether direct contact with the flat surface 50 is achieved . with regard to a typical soft spike 60 , as the recesses 72 engage the nibs 52 , the nibs 52 are able to slightly deform under the applied force of the passenger , thereby increasing the contact surface between the soft spikes 60 and the nibs 52 , thus increasing the traction . additionally , nib deformation enables the soft spike 60 to engage the nibs 52 and concurrently contact the flat surface 50 . the description of the invention is merely exemplary in nature and , thus , variations that do not depart from the gist of the invention are intended to be within the scope of the invention . such variations are not to be regarded as a departure from the spirit and scope of the invention . | 8 |
turning now to the drawings , and referring first to fig1 , an exemplary welding system is illustrated as including a power supply 10 and a wire feeder 12 coupled to one another via conductors or conduits 14 . in the illustrated embodiment the power supply 10 is separate from the wire feeder 12 , such that the wire feeder may be positioned at some distance from the power supply near a welding location . however , it should be understood that the wire feeder , in some implementations , may be integral with the power supply . in such cases , the conduits 14 would be internal to the system . in embodiments in which the wire feeder is separate from the power supply , terminals are typically provided on the power supply and on the wire feeder to allow the conductors or conduits to be coupled to the systems so as to allow for power and gas to be provided to the wire feeder from the power supply , and to allow data to be exchanged between the two devices . the system is designed to provide wire , power and shielding gas to a welding torch 16 . as will be appreciated by those skilled in the art , the welding torch may be of many different types , and typically allows for the feed of a welding wire and gas to a location adjacent to a workpiece 18 where a weld is to be formed to join two or more pieces of metal . a second conductor is typically run to the welding workpiece so as to complete an electrical circuit between the power supply and the workpiece . the system is designed to allow for data settings to be selected by the operator , particularly via an operator interface 20 provided on the power supply . the operator interface will typically be incorporated into a front faceplate of the power supply , and may allow for selection of settings such as the weld process , the type of wire to be used , voltage and current settings , and so forth . in particular , the system is designed to allow for mig welding with various steels , aluminums , or other welding wire that is channeled through the torch . these weld settings are communicated to control circuitry 22 within the power supply . the control circuitry , described in greater detail below , operates to control generation of welding power output that is applied to the welding wire for carrying out the desired welding operation . in certain presently contemplated embodiments , for example , the control circuitry may be adapted to regulate a suitable mig welding regime . the control circuitry is thus coupled to power conversion circuitry 24 . this power conversion circuitry is adapted to create the output power , such as pulsed pulsed waveforms that will ultimately be applied to the welding wire at the torch . various power conversion circuits may be employed , including choppers , boost circuitry , buck circuitry , inverters , converters , and so forth . the configuration of such circuitry may be of types generally known in the art in and of itself the power conversion circuitry 24 is coupled to a source of electrical power as indicated by arrow 26 . the power applied to the power conversion circuitry 24 may originate in the power grid , although other sources of power may also be used , such as power generated by an engine - driven generator , batteries , fuel cells or other alternative sources . finally , the power supply illustrated in fig1 includes interface circuitry 28 designed to allow the control circuitry 22 to exchange signals with the wire feeder 12 . the wire feeder 12 includes complimentary interface circuitry 30 that is coupled to the interface circuitry 28 . in some embodiments , multi - pin interfaces may be provided on both components and a multi - conductor cable run between the interface circuitry to allow for such information as wire feed speeds , processes , selected currents , voltages or power levels , and so forth to be set on either the power supply 10 , the wire feeder 12 , or both . the wire feeder 12 also includes control circuitry 32 coupled to the interface circuitry 30 . as described more fully below , the control circuitry 32 allows for wire feed speeds to be controlled in accordance with operator selections , and permits these settings to be fed back to the power supply via the interface circuitry . the control circuitry 32 is coupled to an operator interface 34 on the wire feeder that allows selection of one or more welding parameters , particularly wire feed speed . the operator interface may also allow for selection of such weld parameters as the process , the type of wire utilized , current , voltage or power settings , and so forth . the control circuitry 32 is also coupled to gas control valving 36 which regulates the flow of shielding gas to the torch . in general , such gas is provided at the time of welding , and may be turned on immediately preceding the weld and for a short time following the weld . the gas applied to the gas control valving 36 is typically provided in the form of pressurized bottles , as represented by reference numeral 38 . the wire feeder 12 includes components for feeding wire to the welding torch and thereby to the welding application , under the control of control circuitry 36 . for example , one or more spools of welding wire 40 are housed in the wire feeder . welding wire 42 is unspooled from the spools and is progressively fed to the torch . the spool may be associated with a clutch 44 that disengages the spool when wire is to be fed to the torch . the clutch may also be regulated to maintain a minimum friction level to avoid free spinning of the spool . a feed motor 46 is provided that engages with feed rollers 48 to push wire from the wire feeder towards the torch . in practice , one of the rollers 48 is mechanically coupled to the motor and is rotated by the motor to drive the wire from the wire feeder , while the mating roller is biased towards the wire to maintain good contact between the two rollers and the wire . some systems may include multiple rollers of this type . finally , a tachometer 50 may be provided for detecting the speed of the motor 46 , the rollers 48 , or any other associated component so as to provide an indication of the actual wire feed speed . signals from the tachometer are fed back to the control circuitry 36 , such as for calibration as described below . it should be noted that other system arrangements and input schemes may also be implemented . for example , the welding wire may be fed from a bulk storage container ( e . g ., a drum ) or from one or more spools outside of the wire feeder . similarly , the wire may be fed from a “ spool gun ” in which the spool is mounted on or near the welding torch . as noted herein , the wire feed speed settings may be input via the operator input 34 on the wire feeder or on the operator interface 20 of the power supply , or both . in systems having wire feed speed adjustments on the welding torch , this may be the input used for the setting . power from the power supply is applied to the wire , typically by means of a welding cable 52 in a conventional manner . similarly , shielding gas is fed through the wire feeder and the welding cable 52 . during welding operations , the wire is advanced through the welding cable jacket towards the torch 16 . within the torch , an additional pull motor 54 may be provided with an associated drive roller , particularly for aluminum alloy welding wires . the motor 54 is regulated to provide the desired wire feed speed as described more fully below . a trigger switch 56 on the torch provides a signal that is fed back to the wire feeder and therefrom back to the power supply to enable the welding process to be started and stopped by the operator . that is , upon depression of the trigger switch , gas flow is begun , wire is advanced , power is applied to the welding cable 52 and through the torch to the advancing welding wire . finally , a workpiece cable and clamp 58 allow for closing an electrical circuit from the power supply through the welding torch , the electrode ( wire ), and the workpiece for maintaining the welding arc during operation . it should be noted throughout the present discussion that while the wire feed speed may be “ set ” by the operator , the actual speed commanded by the control circuitry will typically vary during welding for many reasons . for example , automated algorithms for “ run in ” ( initial feed of wire for arc initiation ) may use speeds derived from the set speed . similarly , various ramped increases and decreases in wire feed speed may be commanded during welding . other welding processes may call for “ cratering ” phases in which wire feed speed is altered to fill depressions following a weld . still further , in pulsed welding regimes , the wire feed speed may be altered periodically or cyclically . it should also be noted , while the above discussion relates generally to manual welding processes , the system of fig1 may also be designed for automated processes . that is , the system components may be associated with various automated equipment for supporting and moving the welding torch , and for initiating , executing and terminating welds . in many applications this would be made by the intermediary of a robot that would be programmed to go to an initial location of a weld , perform the weld , and back away to a rest or home position , or move to the position of a subsequent weld . in both manual and automated welding , moreover , information may be available and collected on various workpieces , welds within any workpiece , and this information may be stored along with weld parameters , such as voltages , currents , wire feed speeds , and as described below , stickout of the electrode . fig2 is a partially broken away view of a portion of a welding torch during a welding operation . the welding torch , indicated generally by reference numeral 60 will typically include a gas nozzle 62 through which shielding gas is channeled during welding . within the nozzle a contact tip 64 supports the welding electrode or wire 66 and transmits electric current to the electrode for supporting the welding arc . during the welding operation , a welding arc is established between the workpiece 18 and the wire electrode 66 , and the wire electrode 66 is continuously advanced at a desired wire feed speed as indicated by arrow 68 . at the same time , as the weld advances , the torch ( and / or workpiece ) is displaced along the direction of the weld as indicated by arrow 70 . to permit distancing the nozzle and contact tip from the progressing weld , a stickout length 72 will typically be afforded , either by manual positioning of the torch ( and / or workpiece ) or by an automated setting of a robotic apparatus . in either case the torch may be positioned more or less close to the workpiece , such that the electrode stickout length 72 may change . in general , welders and welding engineers designing automated systems will prefer some optimal length of welding electrode to provide the desired penetration , arc heating , melting of the electrode , and so forth . the present techniques allow for determining the stickout length of the electrode , and at least one of monitoring the stickout or controlling system components based upon the stickout . fig3 illustrates a similar torch with the wire electrode retracted . in certain embodiments of the present techniques , the stickout may be controlled to allow for determination of stickout following a welding operation , and retraction of the electrode following the welding operation as indicated by reference numeral 74 . in certain applications , the desired at - rest stickout 76 may be controlled by reference to the stickout following the welding operation . for example , in some implementations , the electrode may be retracted to approximately the level of the nozzle front extremity or slightly within the nozzle to reduce the potential for touching or otherwise contacting the electrode between welding operations . fig4 illustrates exemplary steps in a process for determining the stickout length . the process indicated generally by reference numeral 78 , begins with measuring current , as indicated by reference numeral 80 . the current measured at step 80 will typically be the welding current , and will be measured by a current sensor associated with at least one of the welding torch , the wirefeeder , and the welding power supply . such current measurements are commonly made for various monitoring and control operations . in the present context , however , the current measurement is used to compute stickout as described below . current measurements are typically made periodically during the welding operation , and many such current measurements are made at pre - determined intervals under the control of processing circuitry as described below . at step 82 , then , based upon these current measurements , a stickout parameter sample is computed . in a presently contemplated embodiment , the sample is computed according to relationships : if the wire is in a short condition ( wire touching the puddle or work ): where i represents the measured current , and the parameter c1 is a scaling constant , such as 1600 , and c2 is a scaling constant , such as 2150 . in this implantation , eq . 1 generally represents wire heating , while eq . 2 represents wire heating plus arc heating . those skilled in the art will appreciate that determination of whether the electrode is in a short circuit condition may be made by reference , for example , to the voltage of the welding power ( which will decline precipitously due to the short circuit ), and / or the current . in addition to current , other parameters such as power and resistance may also be measured and used in computing stickout . with the samples computed , in a presently contemplated embodiment multiple samples are averaged as indicated by step 84 in fig4 . this averaging allows for smoothing of the samples over time and reduction of noise . in presently contemplated embodiments , for example the samples are averaged over a relatively extended period , on the order of 0 . 05 to 3 seconds . additionally , the resistance may be held constant , and the integral of i 2 may be calculated and used in computing stickout . the welding system may be configured for various welding processes , including direct current welding and pulse welding , in which sampling and / or integration is employed to calculate a stickout parameter . in pulse welding processes , the sampling rate is generally greater than the pulse frequency of the welding voltage such that the sampled data is a generally accurate representation of the welding parameter . it has been determined that the stickout length may be estimated based upon the running average of the parameter sample and the wire feed speed . for example , in a presently contemplated embodiment a look - up table is used , with interpolation , to estimate the stickout length . specifically , by way of example only , a table of the following type may be used , where a stickout length is indicated in the left - most column ( in inches ), wire feed speed is indicated in the top row , and the running average of the parameter sample is indicated in the body of the table . in a specific example , for a wirefeed speed of 150 inches per minute ( ipm ), the table may be used , by interpolating between the 100 ipm and 200 ipm columns , rendering interpolated values as follows : if , in this case , the average parameter sample value is 1100 , the stickout length may be interpolated to be between ¼ inches and ¾ inches , with a linear interpolation rendering an estimated stickout of ½ inch . a number of other methods may be devised for estimating or determinating stickout , and the present techniques are not intended to be limited to any particular stickout look - up or computation approach . the system may be calibrated during manufacture or factory testing to produce such reference look - up tables . additionally , the system may be calibrated by users at the work site to enhance customization and accuracy of the system . for example , a user may manually measure one or more stickout lengths with the corresponding parameter samples and input the data into the system . accordingly , the lookup tables may be updated on the fly as this calibration data is inputted . the abovementioned interpolation scheme may likewise be used to calculate stickout in such user calibrated systems . based upon the estimation of electrode stickout , then , multiple actions may be taken by the power supply , the wirefeeder , the system components , or information may simply be stored for later reference . fig5 illustrates several such scenarios , as indicated generally by reference numeral 88 . thus , following the stickout computation method 78 , in one contemplated embodiment , stickout is displayed for the operator as indicated by reference numeral 90 . one significant advantage of the present technique is that a unitized value for stickout may be clearly indicated , such as in inches , millimeters , or any other readily - recognized unit of measure . as described below , the stickout may be displayed on the power supply , the wirefeeder , the torch , or any other component of the system that comprises a user - viewable display . moreover , the stickout may be displayed , in certain cases , within a welding helmet in data communication with any one of these devices . still further , as indicated at reference numeral 92 , the system simply provide for monitoring and logging of stickout . as will be appreciated by those skilled in the art , such monitoring and logging may be associated with part identifications , specific parts , specific welders , specific systems , and may further reference dates and times , and so forth . such data may be analyzed or inspected to detect if a certain machine or component is particularly error prone and may require maintenance . additionally , in the event of a stickout issue , stickout data may also indicate the specific workpiece or part involved such that it can be inspected to ensure quality and weld standard . such specifications may generally be considered performance of either the welding system or the weld . accordingly , the system may be configured to may evaluate and store performance of the welding system or a weld based on stickout . this information may be stored on the wirefeeder , on the power supply , or on any other system component connected to these , including both local to the welding system and entirely remote from the welding system . as indicated at reference numeral 96 , the system may be designed to allow for retraction of the welding wire to a desired at - rest stickout length in both manual and automated operations . this would be typically be performed by reversal of the wirefeed motor in the wirefeeder ( and / or welding torch ). in certain embodiments , the welding wire may not be retracted immediately if another weld is anticipated . as such , retraction may be delayed , stopped , or lessened in order to allow for repetitive welding starts with minimal delay . finally , in certain embodiments , particularly those involving automated welding , the system may be further include a seam - tracking application 98 , in which the seam - tracking application 98 is capable of detecting the welding status such as beginning and end of the weldline . as such , the system , upon detecting a stickout issue , may initiate seam - tracking to determine the appropriate stickout . the machine may then adjust the stickout accordingly . fig6 illustrates certain functional components of the welding system described above that may be called upon for carrying out functions such as those outlined in fig5 . the stickout - responsive system 98 will typically include a current measurement component 100 . in general , this component may comprise of several components which may consist of hardware , firmware and / or software . specifically , in currently contemplated embodiments this component will include one or more current sensors , sampling circuitry ( e . g ., analog - to - digital conversion circuitry ), current measurement circuitry based upon the analog - to - digital conversion , and so forth . as described above , this component will provide current measurements to processing circuitry 102 that executes one or more routines stored on memory circuitry 104 . in a presently contemplated embodiment , the processing circuitry 102 may be the same processing circuitry used to control other aspects of the welding power supply , such as the generation of welding power by the power conversion circuitry . the memory circuitry 104 may be part of the processing circuitry , or may be functionally associated with the processing circuitry in a conventional manner . the memory circuitry will store one or more routines carried out by the processing circuitry , including a stickout calculation routine 106 . here again , the routine may follow any logic capable of estimating or determining stickout based upon measured welding parameter values , and being referred to a look - up table as discussed above . also , the stickout calculation routine may call upon various other parameters of the welding operation , particularly the wire feed speed 110 which may be the commanded wire feed speed , a fed - back wire feed speed ( e . g ., from a tachometer or encoder ) or any other desired estimation or measurement . particularly , the memory circuitry 104 may store different programs and look - up tables that correspond to different welding processes , wire types , and other attributes . for example , the memory circuitry 104 may include a different look - up table associated with each wire size , material , or shielding gas . thus , the user may indicate the specific welding process or wire type they are using , and the appropriate calculation routine 106 and look - up tables may be accessed to provide the appropriate operational instructions . the processing circuitry 102 may be adapted for interaction with other system components to carry out the stickout - based operations . for example , the operator interface 20 discussed above may include one or more display windows , one of which may be dedicated to or optionally programmable to display a stickout value . as discussed above , this display 112 is conveniently in the form of an easily recognizable unit , such as inches or millimeters . the processing circuitry 102 may also be designed to operate with alarms and / or switches as indicated by reference numeral 114 . here again , these alarms may be visual alarms , such as lights , but may also include audible alarms producing sound that can be detected by the welding operator or any other operations personnel to alert them to the fact that stickout is beyond desired limits or is beyond variability criterion . still further , the processing circuitry 102 may cooperate with communications interface circuitry 116 , such as network interface circuitry . conventional network interface circuitry may be employed , such as for transmitting data between the welding system and remote monitors or logs as indicated by reference numeral 118 . here again , this data may be associated with particular workpiece designs , individual workpieces , individual welds or workpieces , welding operators , automated welding systems , dates , times , or any other useful information for storing and evaluating the quality of welds as a function of the detected stickout . finally , the processing circuitry 102 will already be associated with a motor 46 to drive the welding wire 42 to as discussed above . for retraction of the welding wire , the processing circuitry may be capable , directly or through the intermediary of separate drive circuitry ( not shown ), of commanding the motor 46 to reverse the direction of feed of the welding wire so as to retract the welding wire back into a desired at - rest stickout length . in one presently contemplated embodiment an encoder 120 may be used , such as in the weld and torch or in the wirefeeder to detect the movement of the welding wire back to the at - rest stickout length . thus , consistent stickout may be offered at the end of each welding operation , and the wire may be maintained at a desired length outside of the contact tip but within the torch nozzle , for example . while only certain features of the invention have been illustrated and described herein , many modifications and changes will occur to those skilled in the art . it is , therefore , to be understood that the appended claims are intended to cover all such modifications and changes as fall within the true spirit of the invention . | 1 |
the light distribution system of this invention is described below with reference to a mobile communications device such as a cellular telephone , but it should be noted that the system is equally adaptable to other types of electronic devices such as personal information managers , computers , pagers , game controllers and the like . a mobile device 1 is illustrated in fig4 and it is constructed with a front cover 2 , a printed circuit board 3 , and a back cover or base 4 . these elements are assembled to form an operational unit in a conventional manner . printed circuit board 3 has a component side 5 to which all of its components are soldered and an inactive side 7 to which no components can be soldered . front cover 2 contains the user interface 6 which consists of a liquid crystal display 11 and a series of buttons forming a keyboard 12 . in order to use the user interface 6 in situations of limited ambient light , the display and buttons need to be back lit internally . an optical light guide 8 is mounted on the inactive side 7 of the circuit board 3 to receive light from an array of leds 9 connected on the component side of the circuit board 3 through openings 15 , as shown in fig2 b and 3 a . the guide 8 distributes the light emitted from the leds 9 towards , for example , the liquid crystal display 11 and keyboard 12 of the user interface 6 . in the prior art , as shown in fig1 b , an led 50 is mounted on a printed circuit board 51 with the diode chip 52 emitting light through an opening 53 in circuit board 51 . an optical light guide 54 is mounted opposite to the diode chip 52 over the opening 53 . light guide 54 is constructed with the optimizing shaped surface 55 extending substantially across the opening 53 to bend the light , depicted in fig1 b as arrows 58 , passing through the opening 53 at approximately right angles . as shown by arrows 56 and 57 , light at the side extremities of the beam will be propagated through the light guide 54 and be wasted . this can be effective , providing there is sufficient thickness in the light guide . otherwise , the inefficiencies of this configuration result in the use of higher power or a more efficient , i . e . more expensive , led than is necessary and results in undesirable power dissipation or expense . in fig1 a an edge illuminated light guide is shown where the light guide 54 is too thin to receive the full light intensity generated by the led chip 52 . the efficiency of this latter system is limited when the light guide is thin . to provide a more efficient delivery of light to the components of user interface 6 a system is provided which utilizes through the board lighting from an array of leds 9 . the light is coupled to light guide 8 by the use of input diffraction optical elements ( doe ), such as diffraction gratings 13 associated with the light guide 8 . utilizing appropriate optical relationships , an input grating pattern is designed which takes into consideration the angular spectrum and dimensions of the led , the dimensions and composition of the light guide , and the amount of light required . through these calculations the grating configuration is optimized for each application . in the preferred embodiment , an output grating pattern 14 is also designed to extract the light from the light guide in the appropriate area to illuminate user interface components , such as keyboard 12 and lcd 11 . the basic components of the light delivery system of this invention are shown in fig3 a . printed circuit board 3 supports and connects the operating components of the electronic device , i . e . mobile communications device 1 on its component side 5 . a light guide 8 is mounted to circuit board 3 at its inactive side 7 . to provide an optical path for the transmission of light to the light guide 8 , an opening 15 is constructed in the circuit board 3 . led 9 is connected to the component side 5 with its light emitting chip 10 aligned with the opening 15 . a diffraction grating 13 is constructed on the underside of the light guide 8 to receive the light emitted from diode 9 . grating 13 diffracts the light in accordance with the characteristics of the light guide 8 to cause an efficient distribution of the light within the light guide 8 . as shown in fig3 b , the diffraction surface is varied in order to accommodate the spectrum of incident angles of the typical led . as shown in fig2 b , to enhance the delivery of light to the user interface 6 , a series of output gratings 14 are constructed in the light guide 8 to extract the transmitted light out of the light guide at predetermined locations coincident with the locations of the interface components , i . e . lcd 11 and keyboard array 12 . other forms of extracting surfaces are potentially usable , for example the opening 15 having conical surface 16 , as shown in fig5 b . to accomplish the purpose of this invention , the input grating 13 is designed to diffract the light from led 9 into an angle greater than the total internal reflections γ of the light guide 8 , where , assuming a refractive index of n = 1 . 5 , γ ≈ 42 °. using this as a guide , the grating dimensions and pattern may be optimized by using known formulas ( see , diffractive optics for waveguide display , chapter 3 , pasi laakonen , jun . 16 , 2000 , doctoral thesis , university of joensuu , joensuu , finland the substance of which is incorporated into this application by reference . a pattern of gratings which is optimized for each angle of incidence is developed using the nelder mead simplex search algorithm . in addition the placement of the led relative to the grating and the length of the grating are also optimized . the grating comprises an array of minute grooves which are varied in depth , width and length to accommodate the spectrum of incident angles , as shown in fig3 b . instead of straight gratings a circular grating configuration , as shown in fig5 a , can be generated and used for either out - coupling or in - coupling . once the input and output grating configurations are established the overall pattern can be generated on a thin film by electron beam lithography or other means . this can be used as a master to impress the grating pattern on the light guide as the light guide is molded or pressed . this will allow the light guide to be manufactured with integral in - coupling and out - coupling diffractive gratings . in this manner the light guide distribution system may be made as thin as possible to accommodate overall design goals for an electronic device . light guides presently being used have a thickness in the order of from 1 . 2 to 1 . 5 mm . through the use of this invention , such light guides can be executed in thin films having a thickness in the range of 0 . 2 to 0 . 4 mm . | 8 |
the circuit shown in fig1 includes a low voltage unit 1 composed essentially of a regulated power supply 2 which is connected to power mains and which delivers a direct current at an adjustable direct voltage to a generator 3 which produces a periodic electric current at an adjustable frequency , f . regulated power supply 2 can also receive input power from a battery or any other appropriate current source . the periodic electric signal produced by generator 3 is basically a square wave signal having a constant waveform selected , in a known manner , to minimize first order harmonics , i . e ., the waveform is as close as possible to a perfect sinusoid . a filter 11 permits this periodic signal to be partially smoothed . the magnitude of the periodic current signal is variable as a function of the voltage supplied to generator 3 by regulated power supply 2 . although the waveform of the periodic signal as described above is particularly advantageous and simple to implement , any other form of periodic signal can be employed in the practice of the present invention , in particular a true sinusoidal signal . the periodic current signal produced by low voltage unit 1 is applied through a bundle of flexible conductive cables 4 to the input of a rectifier - step - up transformer unit 5 which comprises an input transformer 6 and a voltage multiplier 7 . the output of the voltage multiplier 7 is connected to a high voltage , or live , electrode 8 of an electrostatic sprayer ( not shown ) for spraying a coating product . the operator can decide to vary the voltage supplied to electrode 8 as a function of the desired spraying characteristics and / or as a function of the form of the workpieces to be coated . the voltage also varies as a function of high voltage leaks at the level of the electrode , which depend on its environment , for example on the distance to the nearest ground point . according to the invention , a calculator 10 is connected to a part of the rectifier - step - up transformer 5 and receives two signals representative of the output voltage ( u ht ) of , and the current ( i ht ) in , the rectifier . the voltage u ht is measured across a measuring resistance 15 . calculator 10 also receives input signals representative of the output voltage ( u alim ) and the current ( i alim ) from the regulated power supply 2 . the voltage u alim is measured across a measuring resistance 16 . as a function of the values for the voltage u ht and the current i ht in the rectifier - step - up transformer 5 , calculator 10 can obtain reference values for the voltage ( u htref ) and the current ( i htref ) which the rectifier - step - up transformer 5 should provide to electrode 8 . in fig1 memory 12 is shown as a component external to calculator 10 ; however , in practice , memory 12 can be a component part within calculator 10 . calculator 10 compares at least one of the measured values ( u ht , i ht ) with a corresponding reference value ( u htref , i htref ) and determines the percentage difference between the associated values . if the percentage difference is equal to or less than a selected value which is assumed to be acceptable , for example 20 %, the installation is assumed to be operating properly and its operation is maintained . if the percentage difference is greater than the selected value , calculator 10 activates a malfunction procedure which comprises operating a means 13 for shutting off operation of the low voltage unit . in the case of a regulated power supply 2 connected to power supply mains , the means 13 is a switch . simultaneously with , or in place of , operation of shut - off means 13 , calculator 10 can also trigger an alarm 14 in order to warn the operator of the occurrence of the malfunction . the threshold value for initiating a malfunction procedure is determined by the characteristics of the installation . the value of 20 % is given above solely by way of example and any value between 0 % and 1000 % can be chosen . the comparison described above takes place continually at a frequency linked to the operating speed of calculator 10 , of the order of 50 khz , given that calculator 10 is permanently connected to low voltage unit 1 and rectifier - step - up transformer 5 . taking into account the transient conditions existing during start - up of power supply 2 and the substantial variations which can occur at that time , monitoring of the measured high voltage and associated current values is not effected during a predetermined period after each start - up . in practice , this period can be fixed at several tens of milliseconds , up to one second . fig2 shows a variant of the embodiment of fig1 in which elements identical to those of fig1 have the same reference numerals increased by 100 . the high voltage , u ht , and the associated current , i ht , in rectifier - step - up transformer 105 are measured and transmitted to calculator 10 which adjusts the value of the direct voltage delivered by regulated power supply 102 and the value of the frequency , f , of the periodic current supplied by generator 103 until the high voltage achieves a desired value , u des defined by the operator via a keyboard 112 . the system thus comprises a regulation loop . on the other hand , the voltage , u t between the cables in bundle 104 , and the current i t being conducted by those cables are measured and furnished as input values to calculator 110 . starting from the desired value , u des , and theoretically or experimentally determined physical laws , calculator 110 is arranged to determine theoretical values , u tcalc , i tcalc , for the voltage u t and the current i t in the bundle of cables 104 . for example , the voltage across the secondary of transformer 106 could be expressed as where k 1 is a numerical coefficient dependent on the characteristics of transformer 106 . the voltage drop in rectifier - step - up transformer 105 has the form : ## equ1 ## where f is the frequency of the periodic signal provided by generator 103 ; c is the unitary value of the capacitance of each of the capacitors in rectifier 107 , and n is the number of voltage doubling stages in rectifier 107 ; in the illustrated embodiment , rectifier 107 contains three voltage doubling stages . where k 2 is a constant numerical coefficient characteristic of the type of cascade employed . the value for the output voltage from rectifier - step - up transformer 105 is a multiple of the voltage across the secondary of transformer 106 , the multiplying coefficient , k 3 , being the voltage gain of the cascade . the high voltage at the output of the rectifier can be expressed as a function of the other values as follows : when the value of u ht must be equal to the desired value , u des , and when i ht is known , the calculated value for u t is obtained by solving the following first order equation : the comparison between u tcalc and u t permits a determination to be made of whether the generator is functioning in an abnormal manner . one can proceed as in the embodiment of fig1 by detecting a malfunction when the difference between the calculated value , u tcalc , and the measured value , u t exceeds a given percentage and a given difference in volts , for example 5 v . in the same manner , the comparison can be made between i tcalc and i t . it is to be noted that , in this embodiment , a measurement is not performed directly on the high voltage produced in rectifier - step - up transformer 105 because the malfunction measurement is performed independently of the regulation loop . a poor contact within the measurement line , because of the lower level of u t , thus does not significantly influence the reliability of the malfunction detection . according to another embodiment of the invention , which is not shown , the frequency , f , of the periodic signal produced by generator 103 can also be used as one of the parameters defining the periodic signal . in effect , this frequency has a relation to the other measured physical quantities because it is related to the gain of the rectifier - step - up transformer . the invention can be implemented by comparing only one measured physical quantity with only one reference value , the reference value being determined as a function of one or several parameters which determine the periodic signal . in effect , for example , the output voltage depends on a combination of the supply voltage , the supply current and the frequency of the periodic signal . in the embodiments of the invention described herein , the low voltage unit 1 is physically separated from the rectifier - step - up transformer 5 and is connected thereto by a bundle of flexible cables 4 . however , the invention can also be applied to arrangements in which these subassemblies form part of an integrated or compact system . this application relates to subject matter disclosed in application number 95 08621 , filed on jul . 10 , 1995 in france , the disclosure of which is incorporated herein by reference . while the description above refers to particular embodiments of the present invention , it will be understood that many modifications may be made without departing from the spirit thereof . the accompanying claims are intended to cover such modifications as would fall within the true scope and spirit of the present invention . the presently disclosed embodiments are therefore to be considered in all respects as illustrative and not restrictive , the scope of the invention being indicated by the appended claims , rather than the foregoing description , and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein . | 1 |
referring to the drawings , and particularly to fig1 , a voter assistance terminal 300 constructed in accordance with the invention comprises a ballot marking device 302 and touchscreen or voting terminal 304 . the preferred embodiment of this voter assistance terminal 300 provides for the marking device 302 to be connected to the touchscreen 304 via a flexible cable ( not shown ) which may have conventional connectors to facilitate the closing and transport of the voter assistance terminal 300 . ( see fig2 ) voter assistance terminal 300 is used to mark a pre - printed physical ballot . in particular , an election judge , after confirming the identity and registration of the voter , issues a preprinted paper ballot 306 to the voter . the voter then has the option of either manually marking the ballot 306 in the conventional way , or of inserting the ballot into a ballot receiving slot 308 at the front of the marking device 302 of the voter assistance terminal 300 for electronic marking . the terminal 300 draws in the ballot 306 and scans a preprinted code on the ballot to determine which form or style of ballot has been inserted . it then presents a series of menu - driven voting choices on its preferably color touchscreen 304 corresponding to that particular ballot style . in the event that the voter is in need of language support , for example he or she cannot read the english language , the voting menus on the touchscreen 304 can be presented in any number of different languages and then the voter can more readily navigate through these menus . additionally , in the event that the voter has diminished motor skills , is somewhat visually impaired , or is in some other way physically handicapped and cannot vote in the conventional manner , he or she simply navigates through these touchscreen menus . furthermore , in the event that the voter cannot use the touchscreen 304 due to the severe physical impairment , blindness or any other reason , he or she can navigate through these menus via a headphone 310 and sub - panel 312 combination . more particularly , a blind voter ( for example ) would wear the headphones 310 which are connected to the marking device 302 via headphone wire 314 and jack 316 into plug 318 . although the headphones may be used in conjunction with the touchscreen display , the display may shut down ( turn black ) when the voter so elects or when the jack 316 is inserted into plug 318 in order to preserve the voter &# 39 ; s privacy as he or she navigates through these menus . as such , the sub - panel comprises , preferably four arrow - shaped key switches , up 322 , down 324 , left 326 , right 328 and a center enter key 330 . the blind voter then navigates through the menus using these keys in conjunction with pre - recorded , digitized audio prompts heard through headphones 310 . in any event , the voter assistance terminal 300 accumulates the voters choices in its internal memory during this menu driven ( visual , audio , or both ) navigation . when the voter has finished with his or her choices , he or she is prompted to mark his or her ballot . the preprinted ballot is then marked according to these choices using its internal print mechanism . the ballot is then fed back to the voter through slot 308 for confirmation and insertion into the scanner , where it is validated and tallied . referring now to fig2 , the voter assistance terminal 300 is shown in its closed or transport state . in this state , it can be easily carried via handles 332 located on both sides of its lower housing 334 . the touchscreen is safely located within recess 336 and beneath the protective cover 338 hinged to the top housing 340 via hinges 342 ( fig1 ). the ballot slot 308 is also safely located behind the lower cover 344 which forms the ramp 346 to aid in the ballot insertion when the voter assist terminal 300 is in the open position . an additional sub - panel 348 preferably comprises a message display window 350 utilizing liquid crystal or other known color display technology for displaying voter assistance terminal status and issuing prompts and instructions to the voter . it is contemplated that sub - panel 348 be interchangeable within a future sub - panel having a different message display window , or an additional sub - panel utilizing a key configuration . other features provided on the voter assist terminal 300 include a lockable module receiving receptacle 352 for receiving ballot data modules . a hinged door 354 secured by a key lock 356 may be provided to prevent tampering with the data module . an led pilot light 358 provides a steady green indication to indicate ac power , a steady yellow indication to indicate battery power and a blinking red to indicate a low - battery condition . the set - up procedure of the voter - assistance terminal of the present invention , for converting the apparatus from its closed position ( fig2 ) into its open and usable position ( fig1 ), is described in fig3 a - 3 c . referring to the closed or transport position of fig3 a , the touchscreen 304 is shown safely located within recess 336 and under top cover 338 . during the set - up procedure , ( fig3 b ) the top cover 338 is pivoted about pivot point 360 and the touchscreen 304 is pivoted about pivot point 362 . similarly the bottom cover 344 is pivoted about pivot point 364 . fig3 c illustrates the completed set - up process . in particular , top cover 338 is now fastened behind touchscreen 304 at 366 to provide support for the screen , and bottom cover 344 mates with the assembly at 368 to provide support for ramp 346 . now the voter assistance terminal is open and ready to use . when the terminal needs to be closed , the reverse process will once again transform the terminal to its closed or transport position of fig2 . while a particular embodiment of the invention has been shown and described , it will be obvious to those skilled in the art that changes and modifications may be made therein without departing from the invention in its broader aspects , and , therefore , the aim in the appended claims is to cover all such changes and modifications as fall within the true spirit and scope of the invention . | 6 |
the present invention relates to storage stable hemoglobin solutions that are partially deoxygenated and contain less than 4 moles of reducing agent per mole of hemoglobin and methods of making such storage stable hemoglobin solutions . hemoglobin can be free in solution , or in solution in a naturally occurring or artificial cell ( e . g . liposomes ) and can be derived from natural , synthetic or recombinant sources . for example , slaughter houses produce very large quantities of hemoglobin - containing blood . particular species or breeds of animals which produce a hemoglobin especially suitable for a particular use can be specifically bred in order to supply hemoglobin . transgenic animals can be produced that express non - endogenous hemoglobin ( logan , j . s . et al ., pct application pct / us92 / 05000 ). human hemoglobin can be collected from outdated human blood that must be discarded after a certain expiration date . in addition to extraction from animal sources , the genes encoding subunits of a desired naturally occurring or mutant hemoglobin can be cloned , placed in a suitable expression vector and inserted into an organism , such as a microorganism , animal or plant , or into cultured animal or plant cells or tissues . these organisms can be produced using standard recombinant dna techniques and the hemoglobin produced by these organisms can then be expressed and collected as described , for example , in hoffman , s . j . and nagai , k . in u . s . pat . no . 5 , 028 , 588 and hoffman , et al ., wo 90 / 13645 , both herein incorporated by reference . purification of hemoglobin from any source can be accomplished using purification techniques which are known in the art . for example , hemoglobin can be isolated and purified from outdated human red blood cells by hemolysis of erythrocytes followed by chromatography ( bonhard , k ., et al ., u . s . pat . no . 4 , 439 , 357 ; tayot , j . l . et al ., ep publication 0 132 178 ; hsia , j . c ., ep patent 0 231 236 b1 ), filtration ( rabiner , s . f . ( 1967 ) et al ., j . exp . med . 126 : 1127 - 1142 ; kothe , n . and eichentopf , b . u . s . pat . no . 4 , 562 , 715 ), heating ( estep , t . n ., pct publication pct / us89 / 014890 , estep , t . n ., u . s . pat . no . 4 , 861 , 867 ), precipitation ( simmonds , r . s . and owen , w . p ., u . s . pat . no . 4 , 401 , 652 ; tye , r . w ., u . s . pat . no . 4 , 473 , 494 ) or combinations of these techniques ( rausch , c . w . and feola , m ., ep 0 277 289 b1 ). recombinant hemoglobins produced in transgenic animals have been purified by chromatofocusing ( townes , t . m . and mccune , pct publication pct / us / 09624 ) while those produced in yeast and bacteria have been purified by ion exchange chromatography ( hoffman , s . j . and nagai , k . in u . s . pat . no . 5 , 028 , 588 and hoffman , et al ., wo 90 / 13645 ). the hemoglobin may be modified by genetic or chemical means for particular uses either prior to , during or after purification . for example , the oxygen affinity may be altered by chemical modification or by genetic modification of the hemoglobin through the introduction of appropriate mutations . the hemoglobin may be chemically crosslinked , or genetically linked or both chemically crosslinked and genetically linked to prevent the dissociation of the molecule into alpha / beta subunits ( dimerization ), prevent heme loss , or to increase the size of the molecule . hemoglobin solutions can be partially deoxygenated by any means known in the art . treatment of hemoglobin solutions with an inert gas such as nitrogen or argon is one such approach . this can be accomplished using gas - liquid contacting techniques wherein oxygen is transported from a solution to a non - oxygen gas phase . some options for gas - liquid contacting include : packed columns , in which the non - oxygen gas passes upward while a solution trickles downward through a bed of packing ; plate columns , similar to packed columns except that they contain a series of horizontal plates that catch the solution ; wetted - wall columns in which a solution falls as a film down a bank of vertical tubes ; gas transfer membranes , wherein oxygen is transported across a thin membrane that retains liquid on one side and a non - oxygen gas on the other side ; gas - sparged tanks , in which non - oxygen gas bubbles through a tank containing the solution ; cyclic pressurization , in which a vessel containing the solution is cyclically pressurized with a non - oxygen gas then vented to release the gas and induce bubbles to form in the solution ; and liquid atomization , in which the solution is sprayed into a chamber containing a non - oxygen gas . another approach to deoxygenation is liquid - liquid contacting techniques , in which two immiscible liquids are mixed together , one of which contains no dissolved oxygen but in which oxygen readily dissolves . after the second liquid has absorbed the oxygen , the liquids can be separated by gravity or in a centrifuge . a third approach to deoxygenation is sorption , in which solid particles with a large internal surface area that adsorb dissolved oxygen , for example molecular sieves , are added to a solution . after sorption , the solid particles can be separated from the solution with a centrifuge or filter . of these techniques , a particularly useful technique is the use of a packed column , where the solution is deoxygenated by flowing an oxygenated hemoglobin solution over the column , while flowing an inert gas countercurrent to the flow of the hemoglobin solution . the inert gas is any gas that does not bind at the heme group of a hemoglobin molecule , for example argon or nitrogen . in another embodiment , the solution is deoxygenated by repeatedly evacuating a hemoglobin solution and flushing or sweeping the hemoglobin formulation with an inert gas , such as argon or nitrogen , until the desired residual oxygen concentration is obtained to produce a partially deoxygenated hemoglobin solution . a partially deoxygenated hemoglobin solution is a hemoglobin solution that contains less than about 5 , 000 parts per million by volume ( ppm ) oxygen in the headspace . residual oxygen in the hemoglobin solution is preferably less than about 1000 ppm , more preferably less than about 500 ppm , and still more preferably less than about 150 ppm . residual oxygen in the headspace can be measured by any means known in the art including for example , sampling of the headspace and measurement of the oxygen in the headspace using a suitably equipped gas chromatograph or zirconium - based detector . for example , the residual oxygen concentration can be determined by sampling of the fill environment using a &# 34 ; mocon &# 34 ; ( mocon , minneapolis , minn .) analyzer . the fill environment is the environment in which the hemoglobin is prepared for storage as described , for example , in example 2 . fill environments include but are not limited to glove bags , glove boxes or any suitable environment in which the residual oxygen levels are controlled . the headspace above the hemoglobin formulation is considered to be in equilibrium with the fill environment . if there is no headspace in the container , then the solution is considered to be in equilibrium directly with the fill environment . if the solution is placed into a container that has been evacuated prior to filling , then the hemoglobin is considered to be in equilibrium with the last gas with which it was in contact . in addition to partially deoxygenated hemoglobin , the solutions of the instant invention also contain reducing agents . such reducing agents include but are not limited to dithionite , ferrous salts ( for example ferrous pyrophosphate ), sodium borohydride as well as other borohydrides , alpha tocopherol and ascorbate or salts therof . if the hemoglobin solution of the instant invention as a pharmaceutical , then the reducing agent is preferably a pharmaceutically acceptable reducing agent . if the hemoglobin solution of the present invention is to be used in a non - pharmaceutical application , then the reducing agent can be any reducing agent , whether or not pharmaceutically acceptable . preferably , the reducing agent is sodium ascorbate . the reducing agent can be added before or after partial deoxygenation . preferably , the reducing agent is added after the target residual oxygen level is achieved in the hemoglobin formulation . although the reducing agent can be in a liquid or solid form , the reducing agent is especially useful when it is in a thoroughly deoxygenated concentrated liquid solution . the amount of the reducing agent in the composition of the instant invention is less than 4 moles / mole of hemoglobin , more preferably less than 2 moles of reducing agent / mole of hemoglobin . the formulations can include other components in addition to the partially deoxygenated hemoglobin solution and one or more reducing agents . the hemoglobin solution of the invention can be formulated in any composition suitable for pharmaceutical or non - pharmaceutical uses . for example , a parenteral therapeutic composition can comprise a sterile isotonic saline solution containing between 0 . 001 % and 90 % ( w / v ) hemoglobin . suitable compositions can also include 0 - 200 m of one or more buffers ( for example , acetate , phosphate , citrate , bicarbonate , or good &# 39 ; s buffers ). salts such as sodium chloride , potassium chloride , sodium acetate , calcium chloride , magnesium chloride can also be included in the compositions of the invention at concentrations of 0 - 2 m . in addition , the compositions of the invention can include 0 - 2 m of one or more carbohydrates ( for example , reducing carbohydrates such as glucose , maltose , lactose or non - reducing carbohydrates such as sucrose , trehalose , raffinose , mannitol , isosucrose or stachyose ) and 0 - 2 m of one or more alcohols or poly alcohols ( such as polyethylene glycols , propylene glycols , dextrans , or polyols ). the compositions of the invention can also contain 0 . 005 - 1 % of one or more surfactants and 0 - 200 μm of one or more chelating agents ( for example , ethylenediamine tetraacetic acid ( edta ), ethylene glycol - bis ( β - aminoethyl ether ) n , n , n &# 39 ;, n &# 39 ;- tetraacetic acid ( egta ), ophenanthroline , diethylamine triamine pentaacetic acid ( dtpa also known as pentaacetic acid ) and the like ). the compositions of the invention can also be at about ph 6 . 5 - 9 . 5 . in another embodiment , the composition contains 0 - 300 mm of one or more salts , for example chloride salts , 0 - 100 mm of one or more non - reducing sugars , 0 - 100 mm of one or more buffers , 0 . 01 - 0 . 5 % of one or more surfactants , and 0 - 150 μm of one or more chelating agents . in a still further embodiment , the composition contains 0 - 150 mm nacl , 0 - 10 mm sodium phosphate , and 0 . 01 - 0 . 1 % surfactant , and 0 - 50 μm of one or more chelating agents , ph 6 . 6 - 7 . 8 . most preferably , the hemoglobin - containing composition includes 5 mm sodium phosphate , 150 mm nacl , 0 . 025 % to 0 . 08 % polysorbate 80 , and 25 μm edta , ph 6 . 8 - 7 . 6 . additional additives to the formulation can include anti - bacterial agents , oncotic pressure agents ( e . g . albumin or polyethylene glycols ) and other formulation acceptable salts , sugars and excipients known in the art . each formulation according to the present invention can additionally comprise constituents including carriers , diluents , fillers , salts , and other materials well - known in the art , the selection of which depends upon the particular purpose to be achieved and the properties of such additives which can be readily determined by one skilled in the art . the compositions of the present invention can be formulated by any method known in the art . such formulation methods include , for example , simple mixing , sequential addition , emulsification , diafiltration and the like . pharmaceutical compositions of the invention can be useful for , for example , subcutaneous , intravenous , or intramuscular injection , topical or oral administration , large volume parenteral solutions useful as blood substitutes , etc . pharmaceutical compositions of the invention can be administered by any conventional means such as by oral or aerosol administration , by transdermal or mucus membrane adsorption , or by injection . non - pharmaceutical compositions of the invention can be used as , for example , reference standards for analytical instrumentation needing such reference standards , reagent solutions , control of gas content of cell cultures , for example by in vitro delivery of oxygen to a cell culture , and removal of oxygen from solutions . in one embodiment , the compositions can be formulated for use in therapeutic applications . for example , the formulations of the present invention can be used in compositions useful as substitutes for red blood cells in any application that red blood cells are used . such compositions of the instant invention formulated as red blood cell substitutes can be used for the treatment of hemorrhage where blood volume is lost and both fluid volume and oxygen carrying capacity must be replaced . moreover , because the compositions of the instant invention can be made pharmaceutically acceptable , the formulations of the instant invention can be used not only as blood substitutes that deliver oxygen but also as simple volume expanders that provide oncotic pressure due to the presence of the large hemoglobin protein molecule . a typical dose of hemoglobin as a blood substitute is from 10 mg to 5 grams or more of extracellular hemoglobin per kilogram of patient body weight . thus , a typical dose for a human patient might be from a few grams to over 350 grams . it will be appreciated that the unit content of active ingredients contained in an individual dose of each dosage form need not in itself constitute an effective amount since the necessary effective amount could be reached by administration of a plurality of administrations as injections , etc . the selection of dosage depends upon the dosage form utilized , the condition being treated , the particular purpose to be achieved according to the determination of the ordinarily skilled artisan in the field . administration of extracellular hemoglobin can occur for a period of seconds to hours depending on the purpose of the hemoglobin usage . for example , as a blood delivery vehicle , the usual time course of administration is as rapid as possible . typical infusion rates for hemoglobin solutions as blood replacements can be from about 100 ml to 3000 ml / hour . however , when used to stimulate hematopoiesis , administration can last only seconds to five minutes and therefore administration rates can be slower because the dosage of hemoglobin is much smaller than dosages that can be required to treat hemorrhage . in a further embodiment , the formulation of the instant invention can be used to treat anemia , both by providing additional oxygen carrying capacity in a patient that is suffering from anemia , and by stimulating hematopoiesis . in addition , because the distribution of the hemoglobin in the vasculature is not limited by the size of the red blood cells , the hemoglobin of the present invention can be used to deliver oxygen to areas that red blood cells cannot penetrate . these areas can include any tissue areas that are located downstream of obstructions to red blood cell flow , such as areas downstream of thrombi , sickle cell occlusions , arterial occlusions , angioplasty balloons , surgical instrumentation and the like . the compositions of the instant invention can also be used as replacement for blood that is removed during surgical procedures where the patient &# 39 ; s blood is removed and saved for reinfusion at the end of surgery or during recovery ( acute normovolemic hemodilution or hemoaugmentation ). because the hemoglobin of the instant invention can bind nitric oxide and other non - oxygen ligands as well as oxygen , the formulations of the instant invention are also useful for the binding or delivery of nitric oxide or non - oxygen ligands . these non - oxygen ligands can be bound or delivered both in vivo or in vitro . for example , the hemoglobin of the instant invention may be used to remove excess nitric oxide from a living system . excess nitric oxide has been implicated in conditions ranging from hypotension to septic shock . likewise , nitric oxide or other non - oxygen ligands may be delivered to a system to alleviate a disease condition . for example , nitric oxide could be delivered to the vasculature to treat hypertension . other therapeutic uses of the instant invention can include drug delivery and in vivo imaging . the composition of the present invention can also be used for a number of in vitro applications . for example , the delivery of oxygen by the composition of the instant invention can be used for the enhancement of cell growth in cell culture by maintaining oxygen levels in vitro . moreover , the hemoglobin of the instant invention can be used to remove oxygen from solutions requiring the removal of oxygen , and as reference standards for analytical assays and instrumentation . the compositions of the instant invention can be stored at temperatures less than 40 ° c . for periods of 12 months or more . preferably , the hemoglobin of the present invention can be stored at 25 ° c . for periods of 12 months or more . more preferably the solution can be stored at 25 ° c . for periods of at least 6 months , most preferably the solution of the instant invention can be stored at 25 ° c . for at least three months . in another embodiment , the solutions of the instant invention can be stored at 4 ° c . for at least 6 months , more preferably 12 months . in a further embodiment , the solutions of the instant invention can be stored at temperatures less than 4 ° c . for at least three months . the hemoglobin solutions of the instant invention can be stored in oxygen impermeable containers , for example , stainless steel tanks , oxygen impermeable plastic bags , or plastic bags overwrapped with low oxygen permeably plastic bags wherein an oxygen scavenger is placed between the internal plastic bag and the overwrapped plastic bag . in another embodiment , the storage stable hemoglobin solutions can be stored in oxygen permeable or oxygen impermeable containers in an oxygen controlled environment . such oxygen controlled environments can include , for example , glove boxes , glove bags , incubators and the like . preferably the oxygen content of the oxygen controlled environment is low relative to atmospheric oxygen concentrations . stability of the hemoglobin solutions of the instant invention can be determined by any means accepted in the art . generally , stability can be determined by the measurement of degradation of the hemoglobin , such as the formation of oxidation , proteolytic or deamidation products , changes in molecular weight distribution , changes in potency , changes in functionality , increases in insoluble matter such as aggregates or modification of the product due to the presence of excipients , such as non - enzymatic glycation . in addition , stability can be determined as a loss of sterility or changes in concentration due to for example , volatilization , adsorption , chemical modification and the like . preferably , stability of hemoglobin solutions is determined by measurement of functionality , measurement of oxidation products , changes in molecular weight distribution and increases in degradation products . such degradation can be monitored by changes in the ratio of beta globin to alpha globin as described , for example , in example 1 . accordingly , storage stable hemoglobin solutions are those solutions of hemoglobin that show less than 10 % hemoglobin degradation , less than 10 % change in molecular weight distribution , or contain less than 5 % methemoglobin . storage stable solutions can also show any combination of these characteristics . the hemoglobin comprising the storage stable solution can have the functionality necessary for a specific application . for example , if the storage stable hemoglobin of the present invention is to be used as a blood substitute , then it should have a p 50 greater than about 27 mm hg , or have an n max greater than about 1 . 7 . the following examples are provided by way of describing specific embodiments of the present invention without intending to limit the scope of the invention in any way . the molecular weight distribution of the hemoglobin composition of the instant invention was determined as follows . hemoglobin solutions were diluted to approximately 4 mg / ml concentrations in 5 mm sodium phosphate , 150 mm nacl , ph 7 . 6 . aliquots ( 25 μl ) were chromatographically separated using a pharmacia &# 34 ; superose &# 34 ; 12 ( piscataway , n . j .) size exclusion column . the columns were eluted with the same buffer as the dilution buffer at a flow rate of 0 . 5 ml / min . absorbance was monitored at 280 nm . the degradation of the hemoglobin molecule can be determined by monitoring modification of the beta globin . a simple method for the quantitation of beta globin modification is by determination of changes in relative globin composition ( i . e . beta globin content versus alpha or di - alpha globin content ). either the alpha globin peak area or the di - alpha globin peak can be used in the analysis . use of the appropriate peak will depend on the composition of the hemoglobin under examination . the globin composition ( beta globin and di - alpha globin ) of the hemoglobin was determined as follows . heme was removed from hemoglobin solutions by precipitating with a cold acid acetone solution ( 0 . 6 % hcl / acetone ). hemoglobin was diluted to approximately 10 μg / μl with hplc grade water . 100 μl of this diluted hemoglobin solution was mixed with the cold acid - acetone mixture , allowed to precipitate and microcentrifuged to separate the fractions . the supernatant was aspirated and discarded ; the pellet was dried with a stream of argon and stored at - 20 ° c . until chromatographic analysis . hplc was performed using a zorbax c3 hplc analytical column ( mac - mod analytical , inc ., chadds ford , pa .). prior to analysis , the pellet was resuspended in 0 . 5 ml of 0 . 1 % trifluoroacetic acid ( tfa ) to yield a final concentration of approximately 2 mg / ml . any residual undissolved material was removed by spinning the sample for 10 minutes in a microcentrifuge prior to application on the analytical column . approximately 100 μg of protein were separated on the zorbax column using the following separation regime : 35 % solvent b for five minutes , then linear ramp to 49 % solvent b during the next 45 minutes , where solvent a was 0 . 1 % tfa in hplc - grade water and solvent b was 0 . 1 % tfa in acetonitrile . the flow rate for the separation was 1 ml / min . absorbance was monitored at 215 nm . the area of the beta polypeptide peak changed significantly under certain conditions . for example , the area of the beta peak for hemoglobin stored under high oxygen conditions in the presence of increasing ascorbate concentrations had decreased markedly during 21 days of storage . the decrease in the area of the beta peak resulted in a reduction of the ratio of the beta globin peak area to the di - alpha globin peak area . because of minor differences in the initial di - alpha content of a given hemoglobin solution , the ratio of the area of the beta peak to the di - alpha peak provided a measure of the degradation of the hemoglobin solutions that could be used for comparison of the effectiveness of different storage conditions for different hemoglobin solutions . as shown in table 1 , solutions prepared according to example 2 and analyzed for the beta / di - alpha peak ratio as described above appeared to be stable at beta / di - alpha ratios of greater than 0 . 9 if methemoglobin formation was controlled . a beta / di - alpha ratio of 0 . 9 is considered to be equivalent to approximately 10 % degradation of hemoglobin . p 50 and n max , functional properties of the hemoglobin , were determined by oxygen equilibrium binding experiments using a hemox instrument ( tcs , inc .) as described in hoffman and nagai , u . s . pat . no . 5 , 028 , 588 , herein incorporated by reference . p 50 and n max were determined at 37 ° c ., 50 mm hepes , 100 mm cl - , ph 7 . 4 . methemoglobin is hemoglobin wherein one or more of the irons of the heme prosthetic groups are in the fe + 3 ( ferric ) oxidation state . the measurement technique for methemoglobin described herein measures the oxidation state of individual heme irons . thus , the reported percentage of methemoglobin reflects the percentage of hemes that are oxidized in the hemoglobin sample . five microliters of hemoglobin solutions were added to 500 μl of 0 . 1 m tris , ph 8 . 0 . 200 μl of the diluted hemoglobin solution was then added to 2 . 8 ml of 0 . 1 m tris , ph 8 . 0 in a 4 . 5 ml cuvette for a final dilution of 1 : 1500 . the oxygenated sample ( hb ) was then analyzed by spectrophotometry in a hewlett - packard model hp 8452a spectrophotometer . absorbances at 436 , 425 , 420 , 404 , 400 nm were collected and stored in a data storage system . the cuvette was then removed from the spectrophotometer and sparged with carbon monoxide two times for 15 seconds each time . the cuvette was inverted 5 times between each sparge . the sample was then re - inserted into the spectrophotometer , and a second set of spectra were collected that corresponded to carbonmonoxy hemoglobin ( hbco ). the cuvette was then again removed from the spectrophotometer and 30 μl of 0 . 1 m kcn in 0 . 1 m tris , ph 8 . 0 was added to the sample . the sample was then inverted three times , allowed to incubate for 5 minutes , and re - inserted into the spectrophotometer for a final spectrophotometric analysis ( hbcn ). the percent methemoglobin was then calculated as follows : ## equ1 ## where a = the absorbance at the susbcripted wavelength for the superscripted hemoglobin species . hemoglobin was expressed , prepared and purified as described in co - owned pct patent application number , pct / us94 / 13034 , filed nov . 14 , 1994 , entitled &# 34 ; purification of hemoglobin &# 34 ;, incorporated herein by reference . the hemoglobin was then concentrated by diafiltration to a concentration of 100 mg / ml and polysorbate 80 was added to a final concentration of 0 . 03 % ( w / v ). the hemoglobin solution was then deoxygenated by flowing oxygen - free nitrogen gas over the hemoglobin solution for approximately 2 hours in a round bottomed flask . the solution was deoxygenated with nitrogen and then equilibrated with the oxygen mixture chosen for the study . ascorbate was prepared as a 0 . 5 m stock solution . the ascorbate solution was then deoxygenated by repeated evacuations of the stock solution and flushing with oxygen - free nitrogen gas four to five cycles . the ascorbate solutions were made up freshly for each experiment described herein . once the ascorbate solution was prepared , it was moved into a glove bag ( the &# 34 ; fill environment &# 34 ;) along with the deoxygenated hemoglobin solution and the glove bag was equilibrated to the required residual level of oxygen in the headspace of the globe bag by repeated evacuations and flushing with the appropriate oxygen / nitrogen mixture . the residual oxygen concentration in the glove bag was determined using a &# 34 ; mocon &# 34 ; apparatus as described above . after equilibration of the glove bag , the ascorbate and the hemoglobin solution were opened , and ascorbate was added to final concentrations of 0 . 5 to 5 mm . the hemoglobin solutions containing ascorbate were aliquoted into 2 ml glass vials as 0 . 5 ml aliquots . the vials were capped with gray butyl rubber stoppers and crimp sealed . the solutions were removed from the glove bag and stored in temperature controlled incubators at either 4 ° c . or 25 ° c . under ambient gas conditions . solutions were stored for up to three months . vials were withdrawn from the stored samples at appropriate time points for given stability test . these tests included , reverse phase hplc analysis for the determination of the beta and di - alpha content , molecular weight distribution by high performance size exclusion chromatography ( hp - sec ), functionality determinations using p 50 and n max values , and methemoglobin concentration . to determine the effect of ascorbate concentration on the stability of hemoglobin over time , solutions of hemoglobin were prepared as described above . these solutions contained 150 , 1000 , 5000 and 15000 ppm oxygen in the headspace and either 0 . 5 , 1 , 2 and 5 mm concentrations of ascorbate in the solution ( ratios of 0 . 3 : 1 , 0 . 6 : 1 , 1 . 3 : 1 and 3 . 2 : 1 ascorbate to hemoglobin molar ratios respectively ). solutions were stored for 3 weeks at 4 ° c . the beta to di - alpha ratio and the percentage of methemoglobin in the solutions was determined at the end of the storage period . the greatest change in the beta / di - alpha ratio was observed in samples containing high levels of both ascorbate and residual oxygen , while the greatest increase in percentage methemoglobin was observed in formulations containing oxygen and low ascorbate ( table 1 ). at low residual oxygen levels ( 1000 ppm and lower ) there was little change in the beta / di - alpha ratio whether or not there was ascorbate in the formulation . however , if there was no ascorbate in the formulation , there were high levels of methemoglobin in the formulation at the end of the storage period . at high residual oxygen levels ( 5000 and 15000 ppm ), the high ascorbate formulations ( ascorbate greater than approximately 0 . 5 mm ) showed greater changes in the beta / di - alpha ratio ( see fig2 and table 1 ) than the low ascorbate formulations . in addition , there was appreciable formation of methemoglobin in high residual oxygen formulations . it is of note that at the end of the storage period , methemoglobin was maintained at low levels except in the presence of greater than 5000 ppm oxygen and less than 1 mm ascorbate . thus even when there was no appreciable formation of methemoglobin in the hemoglobin formulation , there was modification of the polypeptide subunits . table 1______________________________________beta / di - alpha ratios and % methemoglobin in hemoglobinsolutions stored for 21 days at 4 ° c . 150 ppm o . sub . 2 15000 ppm o . sub . 2 beta / % methe - beta / % methe - di - alpha moglobin di - alpha moglobin______________________________________ 0 mm ascorbate 1 . 00 19 . 18 0 . 97 39 . 820 . 5 mm ascorbate 0 . 99 1 . 48 0 . 88 46 . 21 1 mm ascorbate 1 . 00 1 . 00 0 . 82 45 . 06 2 mm ascorbate 0 . 98 0 . 7 0 . 78 3 . 34 5 mm ascorbate 0 . 99 0 . 54 0 . 72 1 . 50______________________________________ to determine the effect of ascorbate concentration on the functionality of hemoglobin over time , solutions of hemoglobin were prepared as described above in example 4 . the functionality of the hemoglobin in the solution was determined at the end of the three week storage period by the determination of p 50 and n max as described above . there were minimal differences in the p 50 and n max values at the 150 and 1000 ppm residual oxygen levels for the different ascorbate concentrations ( table 2 ). however , at 5000 and 15000 ppm residual oxygen concentrations , higher ascorbate concentrations were accompanied by increases in p 50 values . furthermore , at 15000 ppm residual oxygen concentration , the n max decreased with increasing ascorbate concentration ( table 2 ). table 2______________________________________headspace oxygen concentrationascor - bate 150 ppm 1000 ppm 5000 ppm 15000 ppm ( mm ) p . sub . 50 n . sub . max p . sub . 50 n . sub . max p . sub . 50 n . sub . max p . sub . 50 n . sub . max______________________________________0 33 . 4 2 . 14 32 . 2 2 . 07 32 . 2 1 . 87 28 . 5 1 . 7 0 . 5 -- -- 34 . 7 2 . 16 33 . 0 1 . 79 -- -- 1 33 . 5 2 . 18 34 . 0 2 . 16 34 . 8 1 . 89 33 . 0 1 . 512 -- -- 34 . 6 2 . 16 35 . 0 1 . 92 -- -- 5 33 . 8 2 . 11 33 . 7 2 . 22 35 . 4 1 . 86 37 . 3 1 . 49______________________________________ long term , room temperature storage of partially deoxygenated / ascorbate containing hemoglobin formulations four different deoxygenated formulations , all containing 100 mg / ml hemoglobin and 2mm ascorbate and prepared as described in example 2 , were stored for 3 months at 25 ° c . the formulations all contained 150 mm nacl , 5 mm sodium phosphate , 2 mm ascorbate , 0 . 03 % polysorbate 80 ( standard formulation ) and differed in the following manners : throughout the storage period , and at the completion of the 3 month storage period , samples were analyzed for methemoglobin content , changes in molecular weight measured as % high molecular weight hemoglobin ( hmwhb ), beta / di - alpha ratio , aggregate formation by both dynamic light scattering and light obscuration techniques and functionality ( p 50 and n max ). at the conclusion of the storage period there had been no clinically relevant change in any of the parameters monitored throughout the study period ( table 3 ). table 3__________________________________________________________________________formulation # 1 formulation # 2 formulation # 3 formulation # 4initial 3 months initial 3 months initial 3 months initial 3 months__________________________________________________________________________ % methb 4 . 66 1 . 24 3 . 43 1 . 03 3 . 37 1 . 41 1 . 57 0 . 811 % hmwhb 1 . 67 2 . 16 1 . 81 2 . 42 1 . 67 2 . 4 1 . 73 2 . 53β / di - α 1 . 05 0 . 941 0 . 99 0 . 962 1 . 05 0 . 954 1 . 02 0 . 966dls ( nm ) 6 . 4 7 . 1 6 . 5 9 . 75 6 . 2 8 6 . 5 6 . 2p . sub . 50 30 . 99 33 . 62 31 . 05 34 . 41 32 . 02 34 . 93 34 . 88 35 . 08n . sub . max 2 . 23 2 . 02 2 . 19 1 . 94 2 . 17 1 . 98 2 . 35 1 . 94__________________________________________________________________________ the foregoing description of the invention is exemplary for purposes of illustration and explanation . it will be apparent to those skilled in the art that changes and modifications will be possible without departing from the spirit and the scope of the invention . it is intended that the following claims be interpreted to embrace all such changes and modifications . | 2 |
fig1 shows a schematic section taken through a rotary piston machine , perpendicular to a rotating body in the form of a shaft 7 . a piston 2 is guided in an annular conduit 1 along a divided circle extending over more than 180 °, for example a circular cylinder , and by a lever 5 embodied , for example , in the form of a circular disk , transmits the movement of the piston to the shaft 7 via a hub 6 . the piston 2 , functioning for example as a drive element , is moved by a pumping - in of an advantageously noncompressible fluid through a corresponding fluid connection 3 or 4 and a discharging of the fluid via the other fluid connection 4 or 3 . to produce the coupling between the lever 5 and the shaft 7 , the shaft 7 supports a hub 6 that can be embodied in various ways , for example to transmit the torque to the shaft 7 in one direction and to permit a freewheeling rotation in the other direction or else to transmit torque in both directions . even with only one annular conduit 1 and a corresponding embodiment of the piston 2 , it is possible to cover a relatively large angular range of between 180 ° and 320 °, for example , so that the rotary piston drive unit can be advantageously used as a unit for producing a reciprocating motion , for example for the steering of individual wheels in a vehicle , such as a forklift . in one embodiment of the rotary piston drive unit , it is possible to provide two or more annular conduits 1 or circular cylinders that are operated in parallel in the same direction or that transmit their torques in opposite directions . the respective other lever can be operated in a freely rotating fashion in relation to the shaft 7 . otherwise , the annular conduits 1 can be arranged on radially opposing sides in relation to the shaft 7 , possibly axially offset from each other in relation to the shaft 7 so that by providing a plurality of annular conduits 1 , through phase - shifted triggering , it is possible to implement a continuous 360 ° rotational movement of the shaft . also , through control without altering the design of the drive unit , with corresponding triggering of switching valves 11 , the same drive unit can be used in parallel operation of the annular conduits 1 and at other times can be used in an offset operation . hybrid forms are also possible . in addition , it is possible for the same machine to cover different torque ranges and angular ranges of motion . in another embodiment , two pistons operate in the same annular conduit chamber , with the pistons being associated with separate , axially offset levers coupled to the shaft 7 via a hub by releasable locking elements such as ratchets , as schematically depicted in fig3 . thus , the pistons can be moved relative to each other in the cylinder chamber in order to produce the driving action through suitable control . fig2 is an axial section taken through the rotary piston machine . the piston 2 in the annular conduit 1 or circular cylinder appears on the left side of the drawing . this depiction shows how the lever 5 , such as implemented in the form of a circular disk , reaches into the annular conduit 1 and , together with the annular conduit 1 , closes the cavity . the lever 5 is affixed to the piston 2 . fig3 shows a cross section taken through the rotary piston machine in the region of or near the shaft 7 and the hub 6 . in this instance , a freewheeling action is achieved by locking elements embodied in the form of ratchets 8 and nubs 9 or a set of teeth . the ratchets 8 rest against steep flanks of the nubs 9 in the drive direction whereas in the freewheeling direction , the ratchets 8 slide along past the flat flanks of the nubs 9 or the teeth . a ratchet mechanism of this kind can also comprise double ratchets that can pivot in both directions so that both a driving action and a freewheeling action are enabled in both directions , for which purpose steep and flat tooth flanks in different directions are provided on the shaft or hub , such as axially offset from one another , which cooperate with the ratchets that are then likewise axially offset . a switching magnet or hydraulic actuator , for example , can actuate the ratchets . fig4 shows a schematic depiction of the coupling of two annular conduits 1 to a rotary piston drive unit . the coupling makes it possible , with a corresponding connection to the switching valve 11 , to drive the shaft 7 with a constant torque or to pump the fluid with a constant flow by a pump 15 . thus , the fluid connections 4 a and 3 b and the fluid connections 3 a and 4 b are respectively connected via a connecting line 10 so that while the one piston , such as 2 a , is driving the shaft 7 , the other piston , such as 2 b , is being returned . the arrow in fig4 indicates the direction in which a force can be exerted on the shaft 7 . fig5 shows an embodiment of the rotary piston machine in which a pressure on the wall of the annular conduit 1 is absorbed by a claw - shaped clip 12 mounted onto the lever 5 . it is thus possible for the wall to be significantly thinner , for example , than it could be without such a clip or for the rotary piston machine to be designed for significantly higher pressure . in the gap region oriented toward the two respective adjacent lever surfaces , sealing components 13 , in particular sealing rings , can be advantageously inserted into the projections 14 on both sides in the gap region , which projections are encompassed by the clip 12 . a short lever 5 is achieved , for example , if the shaft 7 and the annular conduit 1 abut each other in the gap region and , for example , a seal is produced in the manner shown in fig5 . in another advantageous provision , the annular conduits 1 are assembled of two parts , such as in the central movement plane of the piston 2 , so that the piston 2 and the seals 13 can be used with no trouble . in this instance , it is also possible , for example , for a flange to be formed onto the outside of the annular conduits 1 for the clamping of the two shells of the circular cylinder 1 . the above - describe base unit of the rotary piston machine can be used for various purposes , for example as a centralized or decentralized steering drive unit for wheels , as a rotary drive unit for wheels , as a hydraulic servomotor , or in combination as a hydraulic pump / motor arrangement , such as for replicating a cardan shaft and the like . fig6 shows an embodiment version for the driving of a rotating body , which is situated externally in relation to the annular conduit 1 or circular cylinder . the externally situated rotating body in this instance is supported by a ball bearing on a housing section of the annular conduit 1 , in fact on an upper half of the housing , in addition to the lever that is embodied in the form of a circular disk , for example . correspondingly , the lever 5 in the form of the driving disk is routed so that it passes out through a gap at the outer circumference of the annular conduit 1 and is sealed in the gap by the sealing component 13 . the rotating body , in this instance embodied in the form of an external swivel ring 20 , is mounted onto the driving disk and in turn has an upper supporting structure 31 on which a structure to be rotated , for example a crane framework , can be mounted . it is also possible to implement a supporting structure 30 on the underside of the external swivel ring 20 , if required to meet corresponding requirements . in addition , the housing of the annular conduit 1 can be embodied in a wide variety of ways and can be connected to a base that is suitable to the respective instance . the external swivel ring 20 is supported on the housing of the annular conduit 1 by a four - point bearing component , for example . if needed , the driving disk can alternatively also be routed so that it passes out through a gap situated at the top or bottom , the north or south side , of the annular conduit 1 and can itself continue horizontally or diagonally , for example outward or inward , outside of the gap . fig7 shows an embodiment of the rotary piston machine in which the rotating body is embodied in the form of an internal swivel ring 21 to which an upper supporting structure 31 is likewise coupled . in this instance , an additional support by a ball bearing is in the lower region of a section of the annular conduit housing . here , too , it is alternatively possible to provide a lower supporting structure on the internal swivel ring 21 and a lower supporting structure 30 for accommodating the annular conduit housing . with this embodiment it is also alternatively possible , where suitable , for a gap for the lever 5 to be situated at the top or bottom of the annular conduit 1 . in any case , a reliable seal by sealing components 13 is also required . fig8 shows a detailed depiction of the sealing components 13 . these are inserted into an annular groove in the gap region on the housing component and are embodied so that they produce a reliable seal in relation to the lever 5 around the annular conduit 1 , in both the axial and radial direction . thus , the outside of the sealing component 13 oriented away from the surface of the lever 5 is by a compressive force , for example effected by a fluid , which can be the same fluid as in the annular conduit 1 that is supplied via separate conduits . the hydraulic pressure can be suitably adjusted and safeguarded , for example , by valves . also in the chamber of the annular conduit , transitions , where present , between housing components as well as between the housing and piston and / or lever 5 can be sealed by additional sealing components that are simultaneously embodied with adapted guide surfaces where necessary . the contact pressure in this instance can be provided in the manner described above . another embodiment of the rotary piston machine is shown in fig9 a , a partially cut - away detail viewed from above , and 9 b , a partially cut - away detail viewed in cross section . in this embodiment , two separate levers 5 preferably embodied as driving disks are connected to two pistons 2 that are driven in the same annular conduit 1 . a driving disk 5 is stopped by a hydraulic or electromechanical locking system equipped with locking mechanisms 16 and forms a bottom in the annular conduit against which a pressure can build up in order to drive the freely rotating driving disk 5 ′ with the other piston 2 . with this , the mobile driving disk 5 ′ can be driven to execute a rotation of approximately 315 °, for example , which causes a hydraulic or an electromechanical switching of the locking mechanism 16 . the previously driven driving disk 5 ′ with its piston 2 is stopped by the associated locking mechanism 16 and the previously stationary driving disk 5 is unlocked and released . this alternating switching of the rotary pistons 2 with their driving disks 5 , 5 ′ is able to produce any rotation angle . for the control , an oil supply line 17 and a return are formed by the housing , the driving disks 5 , 5 ′, and the pistons 2 , as shown in fig9 a and 9b . in connection with the rotating bodies described above , this design can be used in various ways in a variety of applications and structures . | 5 |
in a computing environment , there is a de facto standard way of passing work ( instructions ) from a central processing unit ( cpu ) to a direct memory access ( dma ) capable device . typically , the cpu creates data structures called descriptors and stores these descriptors in a memory ring ( e . g ., a circular buffer ). the cpu inserts at one location ( usually denominated the “ tail ”) which the device pulls descriptors off of at the other end ( i . e ., the “ head ”). after creating descriptors , the cpu modifies the tail address and notifies a device of the modified tail address . this is achieved by delivering a “ doorbell ” to the device , which amounts to writing a memory map i / o mapped doorbell configuration space register ( csr ) in the device . this can typically be a 4 - 8b write . the doorbell write typically has to obey the same memory write ordering rules as writes to ‘ normal ’ memory . as a result , as a result , the doorbell incurs a cycle cost related to maintaining store ordering . the exact cost varies with usage , but it is not insignificant for fine grain offload . in accordance with the one exemplary embodiment discussed herein , a weakly ordered ( streaming ) write is disclosed that offers various improvements over prior doorbell technology . one of the problems with existing uc ( uncacheable ) writes is that the write creates a “ shadow ” during which the microprocessor core is waiting for a go ( globally observable ) indicator , where during this period no subsequent stores can be drained . for example , as illustrated in fig1 , there is a period or interval during which the core cannot drain writes . more specifically , as illustrated in fig1 , there is a shadow , during which six operations occur between the core , caching agent ( cbo ) ( or address decoder ) and the integrated i / o ( iio ) ( or shared queue to device ). these operations include the wil 104 , writepull 108 ( or get write data ), a data transfer 112 from the core to the cbo , a data transfer 116 from the cbo to the iio , globally observable message 120 sent from the iio to the cbo , and in turn the globally observable message 124 sent from the cbo to the core . this period during which the core is waiting for the go message can be referred to as a “ shadow ,” with the time period represented by this shadow capable of being absorbed to some extent by the store buffers in the core . however , the core will eventually stall out when the store buffers are full . this manifests itself as a “ cycle cost ” for issuing the doorbell , and it is quite significant in embedded usages , such as packet processing , that are highly optimized . one exemplary aspect addresses this lengthy shadow , and provides a solution with a shorter time period before a next write , which results in a lower cycle cost for the core communicating with devices , such as direct memory access devices . an exemplary methodology for implementing this technique is utilizing a weakly ordered write that will not impede subsequent writes . it is also possible to map the doorbell as wc ( write - combining ) wc is a memory type where multiple writes to the same address are allowed to aggregate into full cache lines before being sent to the system bus . wc writes are weakly ordered , and as such , do not incur the same costs as a uc write . however , there are a number of significant issues that arise from using wc , notably : ensuring doorbell progress , as an 8b wc write may remain indefinitely in a wcb ( write - combining buffer ). fencing the write to ensure progress will incur costs similar to the original uc costs . memory fences inhibit the reordering of memory accesses in modern microprocessors . fences are useful to implement synchronization and strong shared memory semantics in multi - threaded programs . fencing in general is a serializing operation that guarantees that every load and store instruction that proceeds a fence instruction in program order becomes globally observable before any load or store instruction that follows the fence instruction . it is not possible to synchronize the ordering of doorbells across different cores . wc doorbells are used , for example , in various processor architectures , but these are all typically 64b in nature in order to solve the first issue illustrated above . this is not the most bandwidth efficient solution as an exemplary embodiment does not require a 64b doorbell . typically the embodiments described herein can utilize an 8b doorbell with sufficiency . another complication is that some microprocessor vendors do not architecturally guarantee automicity for 64b writes , which can provide further complications . the second issue identified above could be resolved by simply ensuring no reads to the doorbell area have side effects , but this constrains the device memory map , and may rule out many existing devices . again , an exemplary embodiment discussed herein can resolve one or more of the issues highlighted above . more specifically , a new instruction with the following behavior is described : in accordance with an exemplary embodiment , the instruction is an 8b write ( 4 or 16b ( or other size ) versions could also be useful ). the instruction is issued as weakly ordered regardless of the type of the underlying memory region . the instruction exits the write combining buffer automatically at the earliest possible opportunity ( unlike a normal wc mapped or non - temporal 8b write ). therefore , once the wc buffer is allocated and filled with the 8b value , it can be immediately available for eviction ( in the same manner as a full wcb would be today ). creation of one or more “ request ” descriptors destined for the i / o devices . currently these descriptors are created in wb ( write back ) open memory as part of a ring structure , where the processor architecture is adding descriptors at the “ tail ” while the i / o device is reading them at the “ head .” a memory mapped i / o ( mmio ) write acting as a “ doorbell ” is configured to alert the i / o device to the presence of new descriptors . as noted above , the code executed subsequent to this typically is not under the applicant &# 39 ; s control . if the subsequent code contains sufficient writes to fill the available store buffers during the “ uc shadow ” described above , the core will stall . one should note that even though the memory type ( optionally derived from pat / mtrr or memory type of doorbell location ) of the doorbell location is uc , the instruction executes as weakly ordered . this is necessary to allow the instruction to be used with devices having arbitrary layouts of csrs ( what most devices have today ). if the memory area containing the doorbell was mapped as wc , speculative reads might occur , which could have fatal side effects . memory type for a region of memory comes from 2 sources : mtrr — memory type range registers — these specify wide regions of memory to a specific memory type and pat — page attribute table — the pat works on a page granularity ( 4 kb , or 2 mb / 4 mb regions ). when a processor is determining a memory type for a particular request the processor looks of both the mtrr &# 39 ; s and the pat and uses the most conservative ( in general ) of the two . for example , take the scenario of sending a load to address x out to memory . the mtrr &# 39 ; s say the region is wb , but the pat says the load is going to uc memory . the pat “ wins ” since uc is more conservative than wb memory and the load is marked as uc . one should also note that even though the 8b write is weakly ordered , the 8b write will not “ stick ” in a wcb like today &# 39 ; s weakly ordered writes . furthermore , because the doorbell is weakly ordered , an sfence was added beforehand to ensure that the doorbell could not “ pass ” the descriptors and become visible before some / all descriptors . fig2 shows an exemplary hardware implementation of the above exemplary weakly ordered doorbell techniques . one assumption is that the doorbell address is mapped as uc . since uc addresses are never cached , an l1 miss is guaranteed . a wcb is allocated , and it is immediately available for eviction . however , unlike a uc store today , the doorbell is weakly ordered so subsequent writes from the logical core are allowed to progress without waiting for the doorbell store to complete . as illustrated in fig2 the architecture includes : an l1 cache 204 , write - combined buffers 208 , a device , such as a dma device 212 and an uncore 216 . the uncore is used to describe the functions of a microprocessor that are not in the core , but which are essential for core performance . the core contains the components of the processor involved in executing instructions , including the alu , fpu , l1 and l2 cache . uncore functions include , for example , the qpi controllers , l3 cache , on - die memory controller and , for example , the thunderbolt ® controller . other bus controllers ( not shown ) such as pci express and spi are typically part of the chipset . the micro architecture of the uncore 216 is typically broken down into a number of modular units . the main uncore interface to the core is referred to as a cache box ( cbox ) which interfaces with the last level cache ( llc ) and is responsible for managing cache coherency . multiple internal and external qpi links are managed by the physical layer units , referred to as pbox . connections between the pbox , cbox , ( bridges or switches ) and one or more imc &# 39 ; s ( mbox ) are managed by a system configuration controller and a router . in fig2 , in a first step , a fast doorbell is issued , which is received by the l1 cache 204 . next , and as discussed , since uc addresses are never cached , and an l1 miss is guaranteed within step 2 , the l1 allocates a write - combined buffer , which becomes immediately available for eviction . in step 3 , subsequent writes are allowed to progress to the l1 cache 204 , with the write combined buffer 208 in step 4 , evicting the fast doorbell on the in - die interconnect ( idi ) to the uncore 216 . the uncore 216 then routes , in step 5 , the doorbell to the device 212 . ( please note that technically the l1 cache does not receive the doorbell write . since it is a non - cacheable write , the l1 is not checked .) as noted above , it was not possible to synchronize the ordering of doorbells across different cores . thus , the following consequences are encountered : if only one agent is writing to the doorbell , there are no issues , an existing tail pointer update mechanism can work . this is the case for most applications . if two or more agents are writing to the doorbell , the expectation is that the agents need to synchronize their accesses to a shared descriptor area . the agents need to maintain a local shared tail pointer copy . however , existing tail pointer update mechanisms are not safe as they are an absolute value , therefore requiring a fence ( which will cost as much as the uc write ). a relative tail pointer update ( where the doorbell includes writing an incremental number of created descriptors rather than an absolute value ) could be utilized for a shared queue . this would need the device to understand a relative tail pointer update . fig3 illustrates with more specificity one problem with current techniques . as in fig1 there is a “ shadow ” period where the core is unable to drain writes . as seen in fig3 , the first time available for the core to drain writes ( shown as next wr ) occurs after the core receives the go from the llc . compare fig3 to fig4 . as shown in fig4 , an exemplary implementation of the new weakly ordered doorbell technique is illustrated . specifically , as shown in fig4 , the next write ( next wr ) can begin without substantial delay . here , the next write is shown commencing after the wil and before the writepull and fastgo are received by the core . ( wil is a write invalidate line that is essentially a memory write transaction . wil tells the uncore that a core is writing memory and to tell all other cores / agents that might have that data in their caches to invalidate the cached copies . like fastgo and extcmp , wil is an intel ® specific . an alternative manner of expressing this feature is “ memory write ” or “ write command .”) in this exemplary embodiment , the fastgo and extcmp ( external complete — see fig5 ) messages are intel ® specific constructs . the fastgo enables the core to de - allocate the internal buffers used by the doorbell ( specifically , the wcbs ). the “ next write ” doesn &# 39 ; t have to wait for the fastgo of the doorbell , but fastgo does allow resources ( like the wcb &# 39 ; s ) to be reclaimed so other writes can use them . the extcmp is the real go point for the doorbell ( analogous to the go message seen on a uc store ), when everything else in the system can see that the doorbell write has occurred . the core still should be informed when this happens for store - ordering purposes . fig5 provides a more complete picture of an exemplary embodiment of the new instruction . here , after the next write , a writepull is sent from the llc to the core . next , data is sent from the core to the llc , and in turn to the iio . the iio returns a go / extcmp to the llc which is in turn forwarded to the core . as in fig4 and 5 , the next write can occur after wil and thus not suffer the delay as experienced in current implementations . fig6 illustrates a high - level diagram of an exemplary architecture which can implement the techniques herein . in particular , fig6 includes a store buffer 604 , and l1 cache 608 , write combining buffers 612 , wcb eviction control logic 616 , and a memory system . this store buffer 604 holds all stores until they are cleared to write their data into memory . the write combining buffers 612 hold data from the stores ( that either miss the cache or the store &# 39 ; s data is uncacheable ) so the data from multiple stores can be coalesced into a single write to memory . by doing this , the wcb achieves a performance increase by reducing the number of writes out to main memory . the wcb eviction control logic 616 includes the control logic that is in charge of this functionality . the control logic attempts to prevent the wcb from doing the write until the entire buffer is full , or the wcb is forced to be evicted by external forces . examples would be all wcbs are in use , and another store wants one or the core is required to flush all store data to memory . as discussed , an exemplary technique introduced herein provides a new type of store that changes the wcb eviction control . when this new type of store writes its data into a wcb , instead of preventing the wcb from writing to memory until more stores write into the wcb , the new technique and store will cause the wcb to be evicted immediately once the store has written the wcb . stores ( writes to any location ) get output from a core into a store buffer . this is effectively a first in first out ( fifo ) of ( address to write to , data to be written ) couples . when the store is pulled from the store buffers , the address is checked against the l1 cache . if the address hits , store will be written to the l1 cache . if the store misses , the store will be allocated to the write combining buffer ( wcb ). one exemplary embodiment typically uses uncacheable ( uc ) stores to talk to other devices , such as a network interface card on a pcie bus . since uc writes are not cacheable by definition , they will always get a wcb . these uc writes will be eligible to be evicted from the wcb ( to go to the location they are destined for ) immediately . however , stores must be observable in order . this means the newer stores in the store buffers cannot be processed by the core until it is verifiable that the uc store is “ visible ” to other cores in the system . this technique is referred to as globally observable ( go ) as discussed above . once a uc store is issued to the memory sub - system , no other uc stores may be issued by the core until the first store is globally observable . once the memory sub - system notifies the core that the first uc store has reached its go point , the next uc store can be issued by the core . due to the delay imposed by waiting for the go , the interval between uc store issues is significant . in a more specific embodiment , the uc store sheet shows that the uc store first goes to the llc slice that “ owns ” the address , which then handshakes to pull the data . the uc store then pushes the data to an ordered queue in the i / o block that the address maps to ( for example , a pcie route port ). only then , can the llc slice return the go to the originating core to tell the originating core the uc write is visible to all and only then can that store start to pull more stores from the store buffers . this interval is again a significant amount of time in terms of cpu utilization , the reason for that can be seen in the cpu sheet , with these various entities all being read across the cpu die . during this interval , the cpu core continues to execute , and since it will execute stores , the store buffer fifo fills up . at this point , the cpu pipeline starts to back up and can eventually stall . as discussed , the exemplary technique herein is directed toward a new instruction that is weakly ordered . this means the instruction does not have to obey the above rule regarding that the stores must be observable in order and that newer stores in the store buffers cannot be processed by the core until the uc store is visible to other cores in the system . rather , in accordance with an exemplary embodiment , the newer stores can continue to be pulled from the store buffers without any delay . this at least translates to increased performance , and addresses the issue of the cpu stalling . another important aspect of the techniques disclosed herein is that the new instruction behaves in this matter despite the fact that the underlying address is mapped as uc . this can be important in terms of easing constraints on the address map of the device being written to , and working with older , legacy devices . fig7 illustrates an exemplary embodiment of a processor &# 39 ; s core architecture . as illustrated in fig4 , there are multiple cores with associated llcs 708 . as shown in fig7 , the componentry illustrated in fig6 can be included in one or more of the cores 704 . embodiments are not limited to computer systems . alternative embodiments of the present disclosure can be used in other devices such as handheld devices , wearable devices , embedded applications and the like . examples of handheld devices include , but are not limited to , cellular phones , internet protocol devices , digital cameras , personal digital assistants ( pdas ), and handheld pcs or computing devices . embedded applications may include , but are not limited to , a micro controller , a digital signal processor ( dsp ), system on a chip ( soc ), network computers ( netpc ), set - top boxes , network hubs , wide area network ( wan ) switches , or any other system that can perform one or more instructions in accordance with at least one embodiment . in the exemplary embodiment of fig8 , system 800 includes processor 804 which includes one or more execution units 808 to implement an algorithm ( s ) that is to perform at least one instruction . one embodiment may be described in the context of a single processor desktop or server system , but alternative embodiments may be included in a multiprocessor system . system 800 may be an example of a ‘ hub ’ system architecture . the computer system 800 includes a processor 804 to process data signals . the processor 804 , as one illustrative example , includes a complex instruction set computer ( cisc ) microprocessor , a reduced instruction set computing ( risc ) microprocessor , a very long instruction word ( vliw ) microprocessor , a processor implementing a combination of instruction sets , an out of order based processor , or any other processor device , such as a digital signal processor , for example . the processor 804 is coupled to a processor bus ( bus ) that transmits data signals between the processor 804 and other components in the system 800 , such as main memory 824 configured to store instructions , data , or any combination thereof . the other components of the system 800 may include , but are not limited to , a graphics accelerator , a memory controller hub , an i / o controller hub , a wireless transceiver , a flash bios , a network controller , an audio controller , a serial expansion port , and an i / o controller as well as other well known components . these elements perform their conventional functions that are well known to those familiar with the art and are not illustrated herein . in one embodiment , the processor 804 includes a level 1 ( l1 ) internal cache memory 820 . depending on the architecture , the processor 804 may have a single internal cache memory or multiple levels of internal cache memories ( e . g ., l1 and l2 ) as shown . other embodiments include a combination of both internal and external caches depending on the particular implementation and needs . register file 82 is capable of storing different types of data in various registers including , but not limited to , integer registers , floating point registers , vector registers , banked registers , shadow registers , checkpoint registers , status registers , configuration registers , and instructions . execution unit ( s ) 808 , include logic to perform integer and floating point operations . the execution unit ( s ) may or may not have a floating point unit . the processor 804 , in one embodiment , includes a microcode ( μcode ) rom to store microcode , which when executed , is capable of performing algorithms for certain macroinstructions or handle complex scenarios . here , microcode is potentially updateable to handle logic bugs / fixes for processor 804 . alternative embodiments of an execution unit 808 may also be used in micro controllers , embedded processors , graphics devices , dsps , and other types of logic circuits . the system 800 also includes a main memory 824 . main memory 1424 may include , but is not limited to , a dynamic random access memory ( dram ) device , a static random access memory ( sram ) device , flash memory device , or other memory device . main memory 824 is capable of storing instructions and / or data represented by data signals that are to be executed by the processor 804 . the processor 804 is coupled to the main memory 824 via a processor bus . a system logic chip , such as a memory controller hub ( mch ) may be coupled to the processor bus and main memory 824 . an mch can provide a high bandwidth memory path to memory 824 for instruction and data storage and for storage of graphics commands , data and textures . the mch can be used to direct data signals between the processor 804 , main memory 824 , and other components in the system 800 and to bridge the data signals between processor bus , main memory 824 , cache memory 820 , and system i / o , for example . the mch may be coupled to main memory 824 through a memory interface . in some embodiments , the system logic chip can provide a graphics port for coupling to a graphics controller through an accelerated graphics port ( agp ) or other graphics controller interconnect . the system 800 may also include an i / o controller hub ( ich ). the ich can provide direct connections to some i / o devices via a local i / o bus . the local i / o bus is a high - speed i / o bus for connecting peripherals to the main memory 824 , chipset , and processor 804 . some examples are the audio controller , firmware hub ( flash bios ), wireless transceiver , data storage , legacy i / o controller containing user input and keyboard interfaces , a serial expansion port such as universal serial bus ( usb ), and a network controller . the data storage device can comprise a hard disk drive , a floppy disk drive , a cd - rom device , a flash memory device , or other mass storage device . as shown in fig8 , the componentry illustrated in fig6 can be included in one or more of the cores / execution units 808 to realize the weakly ordered doorbell disclosed herein . referring now to fig9 , shown is a block diagram of an exemplary processor in accordance with an embodiment . as shown in fig9 , processor 900 may be a multicore processor including a plurality of cores 904 - 912 . in one embodiment , each such core may be configured to operate at multiple voltages and / or frequencies , and to enter turbo mode when available headroom exists ( and assuming the processor has not aged to a point at which a turbo mode is no longer available ). the various cores may be coupled via an interconnect / bus 916 to a system agent or uncore 920 that includes various components . as seen , the uncore 920 may include a shared cache 924 which may be a last level cache . in addition , the uncore may include an integrated memory controller 928 , various interfaces 932 and a power control unit 936 . as shown in fig9 , the componentry illustrated in fig6 can be included in one or more of the cores 904 , 908 , 912 to realize the weakly ordered doorbell disclosed herein . with further reference to fig1 , processor 900 may communicate with a system memory 902 , e . g ., via a memory bus . in addition , via interfaces 932 , connection can be made to various off - chip components such as peripheral devices , mass storage and so forth ( not shown ). while shown with this particular implementation in the embodiment of fig9 , the scope of the present disclosure is not limited in this regard . embodiments may be implemented in many different system types . referring now to fig1 , a multiprocessor system 1000 is shown in accordance with an implementation . as shown in fig1 , multiprocessor system 1000 is a point - to - point interconnect system , and includes a first processor 1004 and a second processor 1008 coupled via a point - to - point interconnect 1012 . as shown in fig1 , each of processors 1004 and 1008 may be multicore processors , including first and second ( or more ) processor cores , although potentially many more cores may be present in the processors . the processors each may include hybrid write mode logic in accordance with an embodiment of the present disclosure . in some embodiments , the various components illustrated herein may be implemented the multiprocessor system 1000 . for example , memory execution cluster , arr , fsfsm , etc ., may be implemented in the processor 1004 and / or the processor 1008 and associated memory / cache . while shown with two processors 1004 , 1008 , it is to be understood that the scope of the present disclosure is not so limited . in other implementations , one or more additional processors may be present . processors 1004 and 1008 are shown including integrated memory controller units 1016 and 1020 , respectively . processor 1004 also includes as part of its bus controller units point - to - point ( p - p ) interfaces 1024 and 1028 . similarly , the second processor 1008 includes p - p interfaces 1032 and 1036 . processors 1004 , 1008 may exchange information via a point - to - point ( p - p ) interface 1012 using p - p interface circuits 1028 , 1032 . as shown in fig1 , imcs 1016 and 1020 couple the processors to respective memories , namely a memory 1040 and a memory 1044 , which may be portions of main memory locally attached to the respective processors . processors 1004 , 1008 may each exchange information with a chipset 1048 via individual p - p interfaces 1052 , 1056 using point to point interface circuits 1024 , 1052 , 1036 , 1056 . chipset 1048 may also exchange information with a high - performance graphics circuit 1060 via a high - performance graphics interface 1064 . a shared cache ( not shown ) may optionally be included in either processor or outside of both processors , yet connected with the processors via , for example , the p - p interconnect , such that either or both processors &# 39 ; local cache information may be stored in the shared cache if a processor is placed into , for example , a low power mode . chipset 1048 may be coupled to a first bus 1068 via an interface 1076 . in one embodiment , first bus 1068 may be a peripheral component interconnect ( pci ) bus , or a bus such as a pci express bus or another third generation or later i / o interconnect bus , although the scope of the present disclosure is not so limited . as shown in fig1 , various i / o devices 1084 may be coupled to the first bus 1068 , along with a bus bridge 1080 which couples first bus 1068 to a second bus 1072 . in one embodiment , the second bus 1072 may be a low pin count ( lpc ) bus . various devices may be coupled to second bus 1072 including , for example , a keyboard and / or mouse or other input device 1088 , communication devices 1092 and a storage unit 1096 such as a disk drive or other mass storage device which may include instructions / code and data , in one embodiment . further , an audio i / o 1094 may be coupled to second bus 1072 as well as a network interface card 1098 . note that other architectures are possible . for example , instead of the point - to - point architecture of fig1 , a system may implement a multi - drop bus or other such architecture . as shown in fig1 , the componentry illustrated in fig6 can be included in one or more of the processors &# 39 ; cores . fig1 illustrates that the processors 1104 , 1108 may include integrated memory and i / o control logic (“ cl ”) 1112 and 1132 , respectively . for at least one embodiment , the cl 1112 , 1132 may include integrated memory controller units such as described herein . in addition . cl 1112 , 1132 may also include i / o control logic . fig1 illustrates that the memories 1140 , 1144 are coupled to the cl 1112 , 1132 , and that i / o devices 1102 are also coupled to the control logic 1112 , 1132 . legacy i / o devices 1164 are coupled to the chipset 1160 . in some embodiments , the memory execution cluster , arr , fsfsm , and other elements may be implemented in the processor 1104 and / or the processor 1108 and associated memory / cache . as shown in fig1 , the componentry illustrated in fig6 can be included in one or more of the processors &# 39 ; cores . fig1 is an exemplary system on a chip ( soc ) 1200 that may include one or more cores 1208 - 1212 . other system designs and configurations known in the art for laptops , desktops , handheld pcs , personal digital assistants , engineering workstations , servers , network devices , network hubs , switches , embedded processors , digital signal processors ( dsps ), graphics devices , video game devices , set - top boxes , micro controllers , cell phones , portable media players , hand held devices , and various other electronic devices , are also suitable . in general , a large number of systems or electronic devices capable of incorporating a processor and / or other execution logic as disclosed herein are generally suitable . referring now to fig1 , shown is a diagram of a soc 1200 in accordance with an embodiment of the present disclosure . in fig1 , an interconnect unit ( s ) 1202 is coupled to : an application processor 1204 which includes a set of one or more cores 1208 - 1212 and shared cache unit ( s ) 1216 ; a system agent unit 1240 ; a bus controller unit ( s ) 1244 ; an integrated memory controller unit ( s ) 1260 ; a set or one or more media processors 1220 which may include integrated graphics logic 1224 , an image processor 1228 for providing still and / or video camera functionality , an audio processor 1232 for providing hardware audio acceleration , and a video processor 1236 that provides video encode / decode acceleration ; a static random access memory ( sram ) unit 1256 ; a direct memory access ( dma ) unit 1252 ; and a display unit 1246 for coupling to one or more external displays . as shown in fig1 , the componentry illustrated in fig6 can be included in one or more of the cores 1208 - 12012 . fig1 illustrates an exemplary embodiment of a system on - chip ( soc ) design 1300 in accordance with embodiments of the disclosure . as an illustrative example , soc 1300 is included in user equipment ( ue ). in one embodiment , ue refers to any device to be used by an end - user to communicate , such as a hand - held phone , smartphone , tablet , ultra - thin notebook , notebook with broadband adapter , or any other similar communication device . a ue may connect to a base station or node , which can correspond in nature to a mobile station ( ms ) in a network . here , soc 1300 includes two cores — 1304 and 1308 . similar to the discussion above , cores 1304 and 1308 may conform to an instruction set architecture , such as a processor having the intel ® architecture core ™, an advanced micro devices ®, inc . ( amd ) processor , a mips - based processor , an arm - based processor design , or a customer thereof , as well as their licensees or adopters . cores 1304 and 1308 are coupled to cache control 1312 that is associated with bus interface unit 1316 and l2 cache 1320 to communicate with other parts of system 1300 . interconnect 1336 includes an on - chip interconnect , such as an iosf ( on - chip system fabric ), amba ( advanced microcontroller bus architecture ), or the like , which can implement one or more aspects of the described disclosure . interconnect 1336 provides communication channels to the other components , such as a subscriber identity module ( sim ) 1340 to interface with a sim card , a boot rom 1342 to hold boot code for execution by cores 1304 and 1308 to initialize and boot soc 1300 , an sdram controller 1346 to interface with external memory ( e . g . dram 1358 ), a flash controller 1350 to interface with non - volatile memory ( e . g ., flash 1362 ), a peripheral control 1352 ( e . g ., serial peripheral interface ) to interface with peripherals , video codecs 1328 and video interface 1332 to display and receive input ( e . g ., touch enabled input ), gpu 1324 to perform graphics related computations , etc . any of these interfaces may incorporate aspects of the embodiments described herein . in addition , the system illustrates peripherals for communication , such as a bluetooth ® module 1366 , modem 1370 , gps 1374 , and wifi 1378 . note as stated above , a ue can include a radio for communication . as a result , these peripheral communication modules may not all be included . however , in a ue some form of a radio for external communication is generally included . as shown in fig1 , the componentry illustrated in fig6 can be associated with one or more of the cores 1304 / 1308 . one or more write combine buffers ; a processor core adapted to issue a next write after a doorbell and before a globally observable message is received . any of the above aspects , further comprising an l1 cache adapted to receive the doorbell and the next write . any of the above aspects , further comprising write combine buffer eviction control logic adapted to control operation of the one or more write combine buffers . any of the above aspects , further comprising write combine buffer eviction control logic adapted to evict the doorbell . any of the above aspects , further comprising write combine buffer eviction control logic adapted to evict the doorbell on an in - die interconnect to an uncore . any of the above aspects , wherein the doorbell is routed to a device . any of the above aspects , wherein the device is a direct memory access capable device . any of the above aspects , wherein the next write is issued before one or more of a writepull , a fastgo , a data message , and an external complete message . any of the above aspects , wherein the circuit is included in each core of a multi - core architecture . any of the above aspects , wherein instructions for implementing the doorbell include : receiving , at one or more write combine buffers , a doorbell ; issuing a next write after the doorbell and before a globally observable message is received . any of the above aspects , further comprising receiving , at an l1 cache , the doorbell and the next write . any of the above aspects , further comprising controlling , through write combine buffer eviction control logic , operation of the one or more write combine buffers . any of the above aspects , further comprising evicting the doorbell on an in - die interconnect to an uncore . any of the above aspects , wherein the doorbell is routed to a device . any of the above aspects , wherein the device is a direct memory access capable device . any of the above aspects , wherein the next write is issued before one or more of a writepull , a fastgo , a data message , and an external complete message . any of the above aspects , wherein the circuit is included in each core of a multi - core architecture . any of the above aspects , wherein instructions for implementing the doorbell include : means for receiving , at one or more write combine buffers , a doorbell ; means for issuing a next write after the doorbell and before a globally observable message is received . any of the above aspects , further comprising means for receiving , at an l1 cache , the doorbell and the next write . any of the above aspects , further comprising means for controlling , through write combine buffer eviction control logic , operation of the one or more write combine buffers . any of the above aspects , further comprising means for evicting the doorbell . any of the above aspects , further comprising means for evicting the doorbell on an in - die interconnect to an uncore . any of the above aspects , wherein the doorbell is routed to a device . any of the above aspects , wherein the device is a direct memory access capable device . any of the above aspects , wherein the next write is issued before one or more of a writepull , a fastgo , a data message , and an external complete message . any of the above aspects , wherein the circuit is included in each core of a multi - core architecture . any of the above aspects , wherein instructions for implementing the doorbell include : for purposes of explanation , numerous details are set forth in order to provide a thorough understanding of the present embodiments . it should be appreciated however that the techniques herein may be practiced in a variety of ways beyond the specific details set forth herein . furthermore , while the exemplary embodiments illustrated herein show the various components of the system collocated , it is to be appreciated that the various components of the system can be located at distant portions of a system and / or on the die . the term module as used herein can refer to any known or later developed hardware , software , firmware , or combination thereof that is capable of performing the functionality associated with that element . the terms determine , calculate and compute , and variations thereof , as used herein are used interchangeably and include any type of methodology , process , mathematical operation or technique . while the above - described flowcharts have been discussed in relation to a particular sequence of events , it should be appreciated that changes to this sequence can occur without materially effecting the operation of the embodiment ( s ). additionally , the exemplary techniques illustrated herein are not limited to the specifically illustrated embodiments but can also be utilized with the other exemplary embodiments and each described feature is individually and separately claimable . additionally , the systems , methods and techniques can be implemented on one or more of a special purpose computer , a programmed microprocessor or microcontroller and peripheral integrated circuit element ( s ), an asic or other integrated circuit , a digital signal processor , a hard - wired electronic or logic circuit such as discrete element circuit , a programmable logic device such as pld , pla , fpga , pal , any comparable means , or the like . in general , any device capable of implementing a state machine that is in turn capable of implementing the methodology illustrated herein can be used to implement the various protocols and techniques according to the disclosure provided herein . examples of the processors as described herein may include , but are not limited to , at least one of qualcomm ® snapdragon ® 800 and 801 , qualcomm ® snapdragon ® 610 and 615 with 4g lte integration and 64 - bit computing , apple ® a7 processor with 64 - bit architecture , apple ® m7 motion coprocessors , samsung ® exynos ® series , the intel ® core ™ family of processors , the intel ® xeon ® family of processors , the intel ® atom ™ family of processors , the intel itanium ® family of processors , intel ® core ® i5 - 4670k and i7 - 4770k 22 nm haswell , intel ® core ® i5 - 3570k 22 nm ivy bridge , the amd ® fx ™ family of processors , amd ® fx - 4300 , fx - 6300 , and fx - 8350 32 nm vishera , amd ® kaveri processors , texas instruments ® jacinto c6000 ™ automotive infotainment processors , texas instruments ® omap ™ automotive - grade mobile processors , arm ® cortex ™- m processors , arm ® cortex - a and arm926ej - s ™ processors , broadcom ® airforce bcm4704 / bcm4703 wireless networking processors , the ar7100 wireless network processing unit , other industry - equivalent processors , and may perform computational functions using any known or future - developed standard , instruction set , libraries , and / or architecture . furthermore , the disclosed methods may be readily implemented in software using object or object - oriented software development environments that provide portable source code that can be used on a variety of computer or workstation platforms . alternatively , the disclosed system may be implemented partially or fully in hardware using standard logic circuits or vlsi design . whether software or hardware is used to implement the systems in accordance with the embodiments is dependent on the speed and / or efficiency requirements of the system , the particular function , and the particular software or hardware systems or microprocessor or microcomputer systems being utilized . moreover , the disclosed methods may be readily implemented in software and / or firmware that can be stored on a storage medium , executed on programmed general - purpose computer with the cooperation of a controller and memory , a special purpose computer , a microprocessor , or the like . in these instances , the systems and methods can be implemented as program embedded on personal computer such as an applet , java ® or cgi script , as a resource residing on a server or computer workstation , as a routine embedded in a dedicated system or system component , or the like . the system can also be implemented by physically incorporating the system and / or method into a software and / or hardware system , such as the hardware and software systems of a processor . in the description and claims , the terms “ coupled ” and / or “ connected ,” along with their derivatives , may have be used . these terms are not intended as synonyms for each other . rather , in embodiments , “ connected ” may be used to indicate that two or more elements are in direct physical and / or electrical contact with each other . “ coupled ” may mean that two or more elements are in direct physical and / or electrical contact with each other . however , “ coupled ” may also mean that two or more elements are not in direct contact with each other , but yet still co - operate or interact with each other . for example , an execution unit may be coupled with a register and / or a decode unit through one or more intervening components . in the figures arrows are used to show connections and couplings . the term “ and / or ” may have been used . as used herein , the term “ and / or ” means one or the other or both ( e . g ., a and / or b means a or b or both a and b ). in the description herein , specific details have been set forth in order to provide a thorough understanding of the embodiments . however , other embodiments may be practiced without some of these specific details . the scope of the embodiments is not to be determined by the specific examples provided above , but only by the claims below . in other instances , well - known circuits , structures , devices , and operations have been shown in block diagram form and / or without detail and / or omitted in order to avoid obscuring the understanding of the description . where considered appropriate , reference numerals , or terminal portions of reference numerals , have been repeated among the figures to indicate corresponding or analogous elements , which may optionally have similar or the same characteristics , unless specified or otherwise clearly apparent . certain operations may be performed by hardware components , or may be embodied in machine - executable or circuit - executable instructions , that may be used to cause and / or result in a machine , circuit , or hardware component ( e . g ., a processor ( s ), core ( s ), portion of a processor , circuit , etc .) programmed with the instructions performing the operations . the operations may also optionally be performed by a combination of hardware and software . a processor , machine , circuit , or hardware may include specific or particular circuitry or other logic ( e . g ., hardware potentially combined with firmware and / or software ) is operable to execute and / or process the instruction and store a result in response to the instruction . some embodiments include an article of manufacture ( e . g ., a computer program product ) that includes a machine - readable medium . the medium may include a mechanism that provides , for example stores , information in a form that is readable by the machine . the machine - readable medium may provide , or have stored thereon , an instruction or sequence of instructions , that if and / or when executed by a machine are operable to cause the machine to perform and / or result in the machine performing one or operations , methods , or techniques disclosed herein . the machine - readable medium may store or otherwise provide one or more of the embodiments of the instructions disclosed herein . in some embodiments , the machine - readable medium may include a tangible and / or non - transitory machine - readable storage medium . for example , the tangible and / or non - transitory machine - readable storage medium may include a floppy diskette , an optical storage medium , an optical disk , an optical data storage device , a cd - rom , a magnetic disk , a magneto - optical disk , a read only memory ( rom ), a programmable rom ( prom ), an erasable - and - programmable rom ( eprom ), an electrically - erasable - and - programmable rom ( eeprom ), a random access memory ( ram ), a static - ram ( sram ), a dynamic - ram ( dram ), a flash memory , a phase - change memory , a phase - change data storage material , a non - volatile memory , a non - volatile data storage device , a non - transitory memory , a non - transitory data storage device , or the like . examples of suitable machines include , but are not limited to , a general - purpose processor , a special - purpose processor , an instruction processing apparatus , a digital logic circuit , an integrated circuit , or the like . still other examples of suitable machines include a computing device or other electronic device that includes a processor , instruction processing apparatus , digital logic circuit , or integrated circuit . examples of such computing devices and electronic devices include , but are not limited to , desktop computers , laptop computers , notebook computers , tablet computers , netbooks , smartphones , cellular phones , servers , network devices ( e . g ., routers ), mobile internet devices ( mids ), media players , smart televisions , nettops , miniature pc , set - top boxes , and video game controllers . reference throughout this specification to “ one embodiment ,” “ an embodiment ,” “ one or more embodiments ,” “ some embodiments ,” for example , indicates that a particular feature may be included in the practice of the technique but is not necessarily required to be . similarly , in the description , various features are sometimes grouped together in a single embodiment , figure , or description thereof for the purpose of streamlining the disclosure and aiding in the understanding of various inventive aspects . this method of disclosure , however , is not to be interpreted as reflecting an intention that the techniques herein require more features than are expressly recited in each claim . rather , as the following claims reflect , inventive aspects lie in less than all features of a single disclosed embodiment . thus , the claims following the detailed description are hereby expressly incorporated into this detailed description , with each claim standing on its own as a separate embodiment . although embodiments described herein are describe in relation to processors , such as multicore processors including multiple cores , system agent circuitry , cache memories , and one or more other processing units , understand the scope of the present disclosure is not limited in this regard and embodiments are applicable to other semiconductor devices such as chipsets , graphics chips , memories and so forth . also , although embodiments described herein are with regard to hardware prefetching , in accordance with an embodiment the system can be used to access data in other devices as well . embodiments may be implemented in code and may be stored on a non - transitory storage medium having stored thereon instructions which can be used to program a system to perform the instructions . the storage medium may include , but is not limited to , any type of disk including floppy disks , optical disks , solid state drives ( ssds ), compact disk read - only memories ( cd - roms ), compact disk rewritables ( cd - rws ), and magneto - optical disks , semiconductor devices such as read - only memories ( roms ), random access memories ( rams ) such as dynamic random access memories ( drams ), static random access memories ( srams ), erasable programmable read - only memories ( eproms ), flash memories , electrically erasable programmable read - only memories ( eeproms ), magnetic or optical cards , or any other type of media suitable for storing electronic instructions . while the disclosed techniques may be described with respect to a limited number of embodiments , those skilled in the art will appreciate numerous modifications and variations therefrom . it is intended that the appended claims cover all such modifications and variations that fall within the spirit and scope of the present disclosure . in the detailed description , numerous specific details are set forth in order to provide a thorough understanding of the disclosed techniques . however , it will be understood by those skilled in the art that the present techniques may be practiced without these specific details . in other instances , well - known methods , procedures , components and circuits have not been described in detail so as not to obscure the present disclosure . although embodiments are not limited in this regard , discussions utilizing terms such as , for example , “ processing ,” “ computing ,” “ calculating ,” “ determining ,” “ establishing ”, “ analysing ”, “ checking ”, or the like , may refer to operation ( s ) and / or process ( es ) of a computer , a computing platform , a computing system , a communication system or subsystem , or other electronic computing device , that manipulate and / or transform data represented as physical ( e . g ., electronic ) quantities within the computer &# 39 ; s registers and / or memories into other data similarly represented as physical quantities within the computer &# 39 ; s registers and / or memories or other information storage medium that may store instructions to perform operations and / or processes . although embodiments are not limited in this regard , the terms “ plurality ” and “ a plurality ” as used herein may include , for example , “ multiple ” or “ two or more .” the terms “ plurality ” or “ a plurality ” may be used throughout the specification to describe two or more components , devices , elements , units , parameters , circuits , or the like . for example , “ a plurality of processors ” may include two or more processors . the terms “ include ” and “ comprise ,” as well as derivatives thereof , mean inclusion without limitation ; the term “ or ,” is inclusive , meaning and / or ; the phrases “ associated with ” and “ associated therewith ,” as well as derivatives thereof , may mean to include , be included within , interconnect with , interconnected with , contain , be contained within , connect to or with , couple to or with , be communicable with , cooperate with , interleave , juxtapose , be proximate to , be bound to or with , have , have a property of , or the like ; and the term “ controller ” means any device , system or part thereof that controls at least one operation , such a device may be implemented in hardware , circuitry , firmware or software , or some combination of at least two of the same . it should be noted that the functionality associated with any particular controller may be centralized or distributed , whether locally or remotely . definitions for certain words and phrases are provided throughout this document and those of ordinary skill in the art should understand that in many , if not most instances , such definitions apply to prior , as well as future uses of such defined words and phrases . it is therefore apparent that there have been provided systems and methods for a weakly order doorbell . while the embodiments have been described in conjunction with a number of embodiments , it is evident that many alternatives , modifications and variations would be or are apparent to those of ordinary skill in the applicable arts . accordingly , this disclosure is intended to embrace all such alternatives , modifications , equivalents and variations that are within the spirit and scope of this disclosure . | 6 |
according to the present invention , an input signal is divided into signal components with different frequency bands , the divided signal components with different frequency bands are delayed in time interval different withone another and then the delayed signal components are composed to produce a reverberation sound . by way of example , as shown in fig1 input signals such as audio frequency signals which are applied to an input terminal 1 are applied to a first delay unit 2a connected in series to a first path or line l 1 to delay the signals by , for example , 0 . 5 seconds . the delayed signal is then applied to an adder 3 . the input audio frequency signals are applied also to a low pass filter 4 connected in series to a second delay path or line l 2 to pass therethrough a signal component with a frequency of up to 2 . 5 khz as shown in fig2 by a curve a . the frequency signal component from the low pass filter 4 is applied to a second delay unit 2b to be delayed by , for example , 2 seconds and then applied to the adder 3 . the input audio frequency signals are further applied to a separate low pass filter 5 connected in series to a third path or line l 3 to deliver from the low pass filter 5 a frequency signal component with a frequency of up to 1khz as shown by a curve b in fig2 . the output signal from the low pass filter 5 is applied to a third delay unit 2c to be delayed by , for example , 5 seconds and then applied to the adder 3 . further , the input audio frequency signals are directly applied through a fourth path or line l 4 to a separate adder 6 . from the adder 3 there are obtained output reverberation sound signals which contain signal components delayed by 0 . 5 seconds , 2 seconds and 5 seconds , respectively , for the frequency lower than 1khz , signal components delayed by 0 . 5 seconds and 2 seconds , respectively , for the frequency between 1 to 2 . 5 khz and a signal component delayed by 0 . 5 seconds , only for the frequency higher than 2 . 5 khz . the reverberation sound signal from the adder 3 is fed to the adder 6 in which it is composed with the input audio frequency signals . thus , a sound signal added with the reverberation sound is delivered from the adder 6 to an output terminal 7 . in this case , as the delay units 2a to 2c , a well known electric charge transferring device such as a bucket brigade device or a charge coupled device is used . such a device samples an input signal with a clock pulse and delivers the sampled signals sequentially . with this device , if it is assumed that its bit number is taken as m and the frequency of the clock pulse as a control signal as f c , the delay time interval τ of theoutput signal relative to the input signal is expressed by the following equation ( 1 ). accordingly , clock pulses with the same frequency are used , the delay time interval τ can be changed by changing the bit number m . on the other hand , if the same number of the bits is used , the delay time interval τ can be varied by changing the frequency f c of the clock pulses . however , in order to avoid that the waveform fidelity of the delayed signalrelative to the original input signal is deteriorated , the frequency f c of the clock pulse must be selected higher than the maximum frequency f m of the signal to be delayed by at least 2 times . accordingly , if the maximum frequency of the input audio frequency signal is 10khz , the frequency of the clock pulse to be applied to the first delay unit 2a must be higher than 20khz . as a result , if the clock pulses of the same frequency are used and the delay time interval is varied by changing the bit number m , such a third delay unit 2c with the delay timeinterval τ of 5 seconds is required which has the bit number m of at lowest 100 , 000 and hence is very expensive . for this reason , in the illustrated embodiment , the delay time intervals ofthe first to third delay units 2a to 2c are varied by changing the frequency of the clock pulses . for example , each bit number of the first to third delay units 2a to 2c is selected to be 10 , 000 , a clock pulse s a with a frequency of 20khz is applied to the first delay unit 2a tomake its delay time interval as 0 . 5 seconds , a clock pulse s b with a frequency of 5 khz is applied to the second delay unit 2b to make its delay time interval as 2 second , and a clock pulse s c with a frequency of 2khz is applied to the third delay unit 2c to make its delay time interval as 5 seconds , respectively . if the delay time periods are varied by changing the frequencies of the clock pulses as described above , it is not necessary to use a delay unit or electric charge transferring device with a large number of bits and hence its cost becomes low . further , since the delay time period can be selected arbitrarily by changing the frequency of the clock pulse , desired reverberation characteristics can be obtained . in the above case , if signal components with different delay time intervalsare obtained for the signal components of the same frequency band and the levels of the signal components are made low as their delay time intervalsbecome long as shown in fig3 a more natural reverberation sound can be produced . fig4 to 6 show practical embodiments of the present invention , respectively , in each of which the first to third delay units 2a to 2c areformed in consideration of the above fact , and in which similar reference numerals to those used in fig1 indicate similar elements . in the embodiment of fig4 the first delay unit 2a connected into the line l 1 consists of n &# 39 ; s number of delay elements or lines da 1 toda n and ( n - 1 )&# 39 ; s number of adders ma 1 to ma n - 1 connectedbetween adjacent delay elements which are connected in series . in this case , an input audio frequency signal is applied through an amplifier ga 0 to the first delay line da 1 and also through amplifiers ga 1 to ga n - 1 to the adders ma 1 to ma n - 1 , andfurther the bit number of the delay lines become large to make the delay time interval long as the delay elements come to after - stages . in this case , the gain of the amplifiers connected to the post adders is increased . thus , from the delay unit 2a there are obtained signal components with different delay time intervals for the same audio frequency signal and their levels are different as shown in fig3 . the other delay units 2b and 2c are formed similarly and hence the corresponding elements are marked with the corresponding references with symbols b and c in place of the that a . with the embodiment of fig4 since the delay time intervals of the respective delay lines of the delay units 2b and 2c inserted into the lines l 2 and l 3 become relatively long , time intervals of n &# 39 ; s number of signal components from the delay elements become relatively long , and consequently there is a fear that a reverberation feeling is deteriorated . in order to avoid such a fear , it is sufficient that , as shown in fig4 adders 8 and 9 are connected between the input terminal 1and the delay unit 2a and between the low pass filter 4 and the delay unit 2b , respectively , and output signals from the delay units 2b and 2c are applied through amplifiers 10 and 11 to the adders 8 and 9 , respectively . thus , signal components of a short time intervals are obtained together for a frequency component with a frequency lower than 1 khz and that with a frequency lower than 2 . 5khz and the reverberation feeling is not deteriorated . in the embodiment of fig5 the first delay unit 2a inserted into the signal line l 1 is formed of n &# 39 ; s number of delay elements or lines da 1 to da n connected in cascade , an adder ma connected to the final stage of the delay line da n and amplifiers ga 1 to ga n - 1 which are supplied with output signals from the delay lines da 1 to da n - 1 and then supply their output signals to the adder ma . in this case , the bit numbers of the delay lines are selected large to make delay time intervals long as they come to the foregoing stage and the gains of the amplifiers supplied with the output signals from the foregoing stage of the delay lines are made large . the second and third delay units 2b and 2c inserted into the signal lines l 2 and l 3 are formed similarly , as shown in fig5 . in the embodiment of fig6 the first delay unit 2a inserted into the signal line l 1 is formed of an adder ma , n &# 39 ; s number of delay elementsor lines da 1 to da n connected to the adder ma and in cascade withone another and n &# 39 ; s number of amplifiers ga 1 to ga n which are supplied with output signals from the delay lines da 1 to da n andthen supply their output signals to the adder ma , respectively . in this case , the bit number or delay time interval of the respective delay lines may be selected equal , but the gains of the amplifiers supplied with output signals from the foregoing stage of the delay lines are made high . the second and third delay units 2b and 2c inserted into the signal lines l 2 and l 3 are formed similarly . in the embodiment of fig6 it may be possible that filters f 1 to f n with different pass band characteristics are inserted between feedback lines from the delay lines da 1 to da n to the adder ma shown in fig6 by dotted lines . with the present invention described as above , a reverberation sound with characteristics , which have a long delay time interval for a signal component with a low frequency but a short delay time interval for a signal component with a high frequency as in the case of the natural reverberation sound , can be easily obtained . especially , in the case wherethe delay time interval is selected by changing the frequency of the clock pulse applied to the electric charge transferring device , the bit number of the electric charge transferring device can be small and hence its construction becomes simple . further , the delay time interval can be selected at will and hence desired reverberation characteristics can be effected . it is also possible that an input audio frequency signal is sampled , the sampled value is converted into a digital signal , then delayed , and the delayed digital signal is converted to an analogue signal again . fig7 shows an embodiment of the clock pulse generator circuit which produces the clock pulses s a , s b and s c , respectively . the clock pulse generator of fig7 consists of astable multivibrators 18 , 19 and 20 . each of the astable multivibrators 18 , 19 and 20 includes a pair of transistors 21a and 21b . the collector of the transistor 21a is connected through a capacitor 22a to the base of the transistor 21b , the collector of the transistor 21b is connected through a capacitor 22b to the base of the transistor 21a , the connection points between the collectors and bases of the different transistors are connected through resistors to a voltage source terminal + b , and the bases of the transistors 21a and 21 b are supplied with base voltage through resistors 23a and 23b . the base voltages for the astable multivibrators 18 , 19 and 20 are suppliedthrough transistors 24 , 25 and 26 of an emitter - follower type , respectively , and the bases of the transistors 24 to 26 are supplied with a dc voltage through variable resistors 27 , 28 and 29 , respectively . thesevariable resistors 27 to 28 are connected in parallel with one another whose one common connection point is connected to the voltage source terminal + b and whose other common connection point is connected to the movable piece of a variable resistor 30 whose fixed part or resistor proper is connected between the voltage source terminal + b and the ground . with the pulse generator shown in fig7 the oscillation frequencies f 1 , f 2 and f 3 of the astable multivibrators 18 , 19 and 20 become high as the base voltages applied thereto through the transistors 24 , 25 and 26 become great with the assumption that the respective circuitelements are selected equal in value . accordingly , as the movable pieces ofthe variable resistors 27 to 29 are moved near the voltage source side of their fixed parts or resistors proper , the oscillation frequencies f 1 , f . sub . 2 and f 3 become high . if the variable resistors 27 to29 are adjusted independently , the condition f 1 & gt ; f 2 & gt ; f 3 or s a & gt ; s b & gt ; s c is established . thus , if the output signals fromthe astable multivibrators 18 to 20 are applied to the first to third delayunits as clock pulses , their delay time intervals τ 1 , τ 2 and τ 3 can be selected to satisfy the condition τ 1 & lt ; τ 2 & lt ; τ 3 . in this case , the variable resistor 30 acts to make high or low the oscillation frequencies of the astable multivibrators18 to 20 together , and the movable piece of the variable resistor 30 is reached along its fixed part near the voltage source side , the oscillationfrequency of each of the astable multivibrators 18 to 20 becomes high . thus , by adjusting the variable resistor 30 the astable multivibrators 18 to 20 are limited in their frequency change . it may be obvious that the present invention is not needed to be limited inscope to the illustrated examples , but many changes and variations could beeffected by those skilled in the art without departing from the spirits andscope of the novel concepts of the invention . therefore , the scope of the invention should be determined by the appended claims only . | 6 |
with reference now to the drawings , fig1 - 14 show hoop - type amusement device , generally referenced as 10 , adapted with a counter 20 in an operational position in accordance with the present invention . fig1 shows counter 20 in relation with a complex hoop - type amusement device , including an inner annular hoop member 12 and an outer octagonal hoop member 14 secured in concentric relation by connectors 16 . device 10 provides a hoop - type amusement device that rotates about the user in response to movement and gyrations produced by the user thus providing the source of amusement . in the operation of the hoop - type amusement device 10 , one point of the inner surface of the inner annular hoop member 12 remains in contact with the hips of the user , such that during one complete rotation of the device 10 , virtually every point in the entire surface of the inner annular member 12 makes contact with the hip of the user just once . as best illustrated in fig4 - 6 , counter 20 is preferably adapted to function as either a mechanical or electrical tally counter device , and is specifically configured for attachment to a portion of hoop - type amusement device 10 . counter 20 includes a housing 22 having a c - shaped connector , generally referenced as 24 . c - shaped connector 24 is preferably sized and shaped so as to allow for removable attachment of counter housing 22 to inner annular member 12 thereby allowing for removable attachment of counter 20 . as should be apparent , c - shaped connector 24 fits tightly enough around the inner annular member 12 to ensure that the counter remains rigidly secured during the operation of the hoop - type amusement device 10 . counter 20 further includes a counter actuator arm 26 pivotally connected thereto and projecting from housing 22 . when counter 20 is in operative engagement with hoop inner annular member 12 actuator arm 26 projects into the void formed radially within the inner angular member 12 . actuator arm 26 terminates in an end portion that is bent upwards so that the bottom of the actuator creates a flat surface that makes contact with the user when the actuator is triggered . as the hoop - type amusement device 10 rotates around the hips of the user , the counter actuator arm 26 is caused to move by contact with the user &# 39 ; s body once during every rotation . in turn , every actuation of counter actuator arm 26 represents one full rotation of the hoop - type amusement device 10 about the user . the number of times the counter actuator arm 26 is activated represents the total number of times the hoop - type amusement device 10 has rotated completely around the user . counter housing 22 further includes a transparent window 28 for displaying the tally to the user . as should be apparent , the tally is continuously updated in real time during the operation of the hoop - type amusement device 10 and actuation of arm 26 . counter 20 further includes a reset knob 29 to allow the user to reset the counter back to zero , or any other desired count . a counter resetting actuator 29 protrudes from the sidewall 10 of the counter housing 22 . resetting actuator 29 is used to re - set the number that is presented on the counter display to a specific number , such as zero . the number on the display can also be reset to any number depending on the preference of the user . the counter resetting actuator 29 is preferably a rotatable knob that is turned in either a clockwise or counter clockwise direction , however any suitable reset actuator structure is considered within the scope of the present invention . counter 20 can be attached to the hoop - type amusement device 10 through any suitable means . in the preferred embodiment , counter 20 is attached through a simple c - shaped connector 24 . c - shaped connector 24 consists of two c - shaped extension pieces , referenced as 24 a and 24 b , which extend from opposing lateral ends of the bottom front side of the counter housing 22 . c - shaped extension pieces 24 a and 24 b fit around the innermost member of the hoop - type amusement device 10 forming a secure connection as to limit the lateral and vertical displacement of the counter 20 during the operation of the device 10 . in a preferred attachment embodiment , counter 20 is mounted in a position so that the front of the housing 22 faces the center of the hoop - type device 10 and the display window 28 faces vertically upward . fig7 - 13 present an alternative embodiment of the present invention , wherein the counter is adapted for attachment to a component connector coupling multiple members that axe used to form a complex hoop - type device 10 . the complex device configuration can consist of multiple members of varying shapes that are each coupled together . specifically , fig8 shows a connector member 30 for use in forming an octagonal outer hoop 14 concentrically disposed around an inner circular hoop member 12 . a plurality of connectors referenced as 30 are disposed in engagement with inner member 12 , and the intersection point of two sides of the octagonal outer member 14 as best seen in fig1 . each connector 30 functions as a coupler for connecting individual side members 40 to form a complete octagonal outer member 14 , and further functions to couple octagonal outer member 14 with inner member 12 . accordingly , each connector 30 includes a first pair of tubular openings 32 that receive members forming the outer hoop member , and a second pair of tubular openings 34 that receive members forming the inner hoop member . in addition , inserts 42 may be provided to allow for the connection of members 40 to form an enlarged hoop configuration . connector 30 further includes a raised , generally cylindrical , mount 36 that functions to receive a counter 20 in press fit engagement therewith . in this embodiment , counter housing 22 is attached to a mount 36 on one of the connectors 30 . in turn , the connectors 30 receive hoop side members 40 which form each side of the octagonal shaped outer member 14 . as should be apparent , counter 20 is positioned so that the c - shaped connector 24 , which protrudes from counter housing 22 extends inwards towards the center of the hoop - type device 10 . more particularly , the c - shaped connector 24 fits around the inner circular member 12 , thereby connecting the inner member 12 to the outer member 24 . counter actuator arm 26 extends from the bottom of the counter housing 22 , and projects radially inward so as to be in position to engage a portion of the user &# 39 ; s body as the hoop rotates . as with the previous disclosed embodiment of the present invention , activation of the counter actuator arm 26 causes the number stored by counter mechanism to increase by a value of one for each actuation / revolution . since the counter actuator piece 30 can only be activated once during a full rotation of the hoop - type amusement device 10 , the value stored by the counter mechanism represents the total number of rotations performed in the operation of the device 10 . as noted above , a reset actuator 29 extends from the side of counter housing 22 into the space between the inner and outer members 12 and 14 . the reset actuator 29 can be but is not limited to a winding knob . by turning the winding knob in a specific direction , the reset actuator 29 is activated , and the number stored by the counter mechanism is set to a desired value . the instant invention has been shown and described herein in what is considered to be the most practical and preferred embodiment . it is recognized , however , that departures may be made therefrom within the scope of the invention and that obvious structural and / or functional modifications will occur to a person skilled in the art . | 0 |
as stated above it has now been found that certain salts of 11 -( 2 - pyrrolidin - 1 - yl - ethoxy )- 14 , 19 - dioxa - 5 , 7 , 26 - triaza - tetracyclo [ 19 . 3 . 1 . 1 ( 2 , 6 ). 1 ( 8 , 12 )] heptacosa 1 ( 25 ), 2 ( 26 ), 3 , 5 , 8 , 10 , 12 ( 27 ), 16 , 21 , 23 - decaene exist as single robust polymorphs . in particular the present applicants have found that the maleate salt of this compound exists as a single polymorph . whilst it is considered that the structure of maleic acid would be clear to a skilled addressee in the art in order to avoid any uncertainty the structure is shown below . initial studies into compound i involved analysis of the hydrochloride salt . it was found as summarised in table 1 below , that the initially prepared hydrochloride salt produces an inconsistent solid form with significant variability in the dsc , tga , gvs and xrpd pattern ( see fig1 to 16 ). as can be seen from the table notwithstanding the same production conditions ( batches 1 to 3 ) being used there was a wide variety of solid forms identified on analysis of the 6 hydrochloride salt batches indicating that with this salt there is a high degree of polymorphism . the xrpd for the sample of batch hcl 1 ( see table 1 ) is shown in fig1 . this diffractogram indicates this batch has relatively low levels of crystallinity and an amorphous halo indicating a mixture of phases . the thermal gravimetric analysis ( tga ) and differential scanning calorimetry ( dsc ) for the sample of batch hcl 1 is shown in fig2 . the tga shows a two stage weight loss totalling 4 . 5 % up to 100 ° c . which equates to 1 . 4 equivalents of water . this corresponds well to the two endotherms seen in the dsc with onsets of 40 ° c . and 88 ° c ., respectfully . this is most likely to be a loss of water from the sample since no process solvents were observed in the 1 h nmr . there then follows an exothermic event onset 141 ° c . which is most likely to be a phase change to a new solid form followed by a final endothermic event , probably a melt , onset 238 ° c . followed by decomposition . these physical changes can be visually seen in a hot - stage microscopy video . the gvs results for the sample of batch hcl 1 are shown in fig3 . the sample shows an initial adsorption of water in the initial adsorption cycle of + 5 . 5 % at 90 % rh . the sample then loses 5 % mass on going to dryness and then regains 2 % mass on going to 40 % rh with a total gain of 2 %. this gain of 2 % would bring the water content up to 6 . 5 % which corresponds to a dihydrate . the sample appears to be a partially dehydrated hydrate that , once it has been exposed a high enough level of humidity gains water and then permanently holds on to it during the gvs experiment . to determine if there had been a change in the solid form of the material after the gvs experiment a xrpd diffractogram was obtained and is shown in fig4 . the x - ray diffractogram post gvs is similar to that of the starting material , but with more intense peaks . also some minor peaks in the original diffractogram ( ca . 8 . 5 and 15 . 5 2theta ) have disappeared . it is likely that the material subjected to the gvs experiment contains more than one crystalline phase ( form ) and that one of the forms changes on exposure to elevated humidity . the xrpd spectrum of batch hcl 2 is shown in fig5 and as can be seen there is a low correlation with the xrpd obtained with the hcl 1 batch . the tga and dsc spectra of batch hcl 2 are shown in fig6 and have some similarities , but is not identical , to batch hcl 1 . batch hcl 2 lost 5 . 6 % water in the first phase of the tga until decomposition at 260 ° c . this water loss represents 1 . 67 equivalents of water . the dsc spectrum shows the same 3 thermal events as seen with batch hcl 1 , however the two data sets are clearly not identical . the xrpd spectrum of batch hcl 3 is shown in fig7 and did not agree well with either the hcl 1 or hcl 2 batches . the xrpd of batch hcl 3 was quite complex with many more reflections that other batches and an additional reflection at 2theta of 6 . 7 not present in other batches . the tga and dsc spectra of batch hcl 3 is shown in fig8 . the sample lost 1 . 5 % water in the first phase of the tga then another loss of 1 . 97 %, possibly solvent , at 165 ° c . until decomposition at 260 ° c . this water loss represents 0 . 5 equivalents of water , lower than the 1 . 1 equivalents ( 3 . 79 %) indicated by karl - fischer analysis . one possible reason for this is that a higher temperature is required to liberate the water trapped in the structure by means of dehydration , a small expansion of the lattice which will release water trapped or a change in the crystalline structure . the total weight lost in the tga is 3 . 4 %. the dsc spectrum shows the same 3 thermal events as seen with batches hcl 1 and 2 but with an additional endothermic event at 200 ° c ., probably a desolvation . in order to probe the behaviour observed above the hcl salt was recrystallised from refluxing acetonitrile / water to yield 79 mg of a yellow powder , batch hcl 4 . this was analysed by xrpd , tga and dsc and the data is shown in fig9 and 10 . this material was shown to be a single , isolable polymorphic form of the hcl salt ( henceforth known as ‘ group 1 ’). as an alternative to recrystallisation , direct formation of the group 1 material from the free base and aqueous acid may also be accomplished . fig9 which shows the xrpd spectrum of batch hcl 4 ( group 1 ) did not agree well with any of the previously described batches . fig1 shows the tga and dsc spectra of batch hcl 4 indicating that the sample loses 6 . 5 % of its mass between ambient and 108 ° c . two equivalents of water equates to 6 . 58 %. this correlates well with the broad endotherm observed in the dsc ( onset = 76 ° c .). the dsc then shows an exothermic phase change ( onset = 148 ° c .) then goes on to show a final endotherm onset 222 ° c . gvs analysis was carried out and the data is shown in fig1 . the sample showed very little absorption of water gaining only 1 . 6 % mass on going from 40 % rh to 90 % rh . the sample lost 2 . 8 % mass on going from 90 % rh to dryness . the sample was analysed by xrpd post gvs . the form of the sample was unchanged ( data not shown ). a second , different , isolable polymorphic form ( batch hcl 5 ) may be prepared when the hcl salt is synthesised from amorphous hcl salt via a ‘ maturation ’ process . in this process a small amount of the amorphous salt ( 10 mg ) was treated with 10 or 20 volumes of methanol or ethanol in a vial . the vials were then capped and placed in a maturation chamber that cycled from ambient to 50 ° c . with four hours spent under each condition . after approximately 18 hours the samples were filtered and analysed . this material was shown to be a single , polymorphic form of the hcl salt different from that of the group 1 material ( henceforth known as ‘ group 2 ’). fig1 shows the xrpd diffractograms for samples prepared in ethanol ( 20 vols , top ) and methanol ( 10 vols , bottom ). although there are small differences between samples it is clear that these data are quite different from other batches described herein . fig1 shows the dsc of the sample prepared in ethanol which is clearly much more complex than other batches . a third , different , isolable polymorphic form , batch hcl 6 , may be prepared when the hcl salt is synthesised from the free base in acetone or in alcoholic solvents with methanolic or aqueous hcl . fig1 shows the xrpd diffractogram , recorded on low and high resolution instruments , and , again , is different from other batches described herein . strikingly , the dsc and tga spectra shown in fig1 are very simple with very little weight loss recorded in the tga until degradation occurs at around 240 ° c . and likewise no thermal events in the dsc until melting and decomposition . this material was shown to be a single , polymorphic form of the hcl salt different from that of the group 1 and 2 materials ( henceforth known as ‘ group 3 ’). in the gvs ( fig1 ) the sample showed very little sorption of water gaining only 1 . 6 % mass on going from 40 % rh to 90 % rh . the sample lost 2 . 4 % mass on going from 90 % rh to dryness . the sample was analysed by xrpd post gvs . the form of the sample was unchanged after the experiment ( data not shown ). both the gvs experiments from batches hcl 4 and 6 ( groups 1 and 3 ) were somewhat similar to each other but different to that of batch hcl 1 , further highlighting the variable nature of the hcl salt . the group three material was stressed under conditions which might cause it to convert to group one material or , indeed , another hydrated or polymorphic form . thus samples were stored at 40 ° c ./ 75 % rh and also at 60 ° c ./ 96 % rh and analysed at regular intervals by xrpd . the results are summarised in table 2 . from the xrpd data ( not shown ) it would appear that the group three material can convert into the group one material at elevated temperature and humidity . this would have implications if the group three material was chosen as the preferred form for production as it would need to be produced in a controlled fashion and any post production manipulations , such as the formulation method , would need to be controlled to ensure that it would not convert into the group one material . in summary , the processes employed to prepare and purify 11 -( 2 - pyrrolidin - 1 - yl - ethoxy )- 14 , 19 - dioxa - 5 , 7 , 26 - triaza - tetracyclo [ 19 . 3 . 1 . 1 ( 2 , 6 ). 1 ( 8 , 12 )] heptacosa - 1 ( 25 ), 2 ( 26 ), 3 , 5 , 8 , 10 , 12 ( 27 ), 16 , 21 , 23 - decaene hcl salt are not adequately controlling the polymorphic form of the compound as there is significant batch to batch variation observed . despite careful work to identify 3 different apparently isolable solid forms ( batches hcl 4 - 6 ) it is quite clear that the larger scale batches produced ( hcl 1 - 3 ) do not closely match any of these reference standards . batches hcl 1 and 3 are both mixtures of groups 1 and 3 forms with varying quantities of amorphous content . batch hcl 2 is quite close to group 1 but unfortunately contains other unexplained peaks in the xrpd pattern . in addition even when a single polymorph is produced ( batches 4 to 6 ) these still exhibit significant water absorption ( typically up to 1 . 6 %) which makes their use in pharmaceutical formulations difficult to ensure consistent dosing . in addition the most promising of the hydrochloride salts ( batch hcl 6 — group 3 ) from the standpoint of the dsc analysis has been found to convert to other polymorphic forms under stress as discussed above indicating that this is not a stable polymorph . as a result of the unacceptable variability observed with the hydrochloride salt as discussed above an alternative robust solid form was required . further discovery endeavours identified the maleate salt as being one such robust solid form . fig1 shows the results of thermal gravimetric analysis ( top ) and differential scanning calorimetry ( bottom ) of the maleate salt . the thermal gravimetric analysis clearly demonstrates that the maleate salt shows no weight loss until the salt melts with decomposition at 200 ° c . this indicates the general temperature stability and robust nature of the maleate salt and also that it is generally not hygroscopic . in addition inspection of the differential scanning calorimetry plot indicates that no other events ( phase changes etc ) are evident for this salt up to its melt and decomposition tempature of 200 ° c . fig1 shows the high resolution x - ray diffraction pattern ( d5000 ) of the maleate salt . in the x - ray diagram shown the angle of diffraction 2theta is plotted on the horizontal ( x ) axis and the relative peak intensity on the vertical ( y ) axis . a complete listing of all peaks observed is shown in table 3 . fig1 shows the variable temperature x - ray diffraction pattern of the maleate salt . with reference to the variable temperature x - ray diffraction patterns shown it is notable that there is no change irrespective of the temperature of the experiment once again indicating the robust nature of the salt . fig2 shows the gvs data for the maleate salt . the maleate has low hygroscopicity , taking up to only less than 0 . 6 % of its weight in water between 0 and 90 % rh . fig2 shows the post - gvs xrpd data . no changes can be observed in the crystalline pattern after the gvs experiment has been carried out , again indicating the robust nature of the maleate salt . in order to determine the propensity of polymorphism for the maleate salt the material was maturated in 27 different solvents . a small amount of solid was slurried with the corresponding solvent ( see table 4 below ) and stored in the incubator and subjected to 4 h - heat / cool cycles at 50 ° c ./ r . t . for 24 h . the solvents were then removed under vacuum , and the remaining solids analysed by xrpd . in all cases only one solid form (‘ form a ’) was identified . the stability of the maleate salt form a material was tested in harsher conditions , when the samples were kept for a week in the humidity chamber at 60 ° c . and 96 % rh . fig2 shows that no changes are observed in the crystalline pattern even under these conditions . in some embodiments the maleate salt may be further characterised as showing on x - ray diffraction at least two peaks on the 2theta scale selected from the group consisting of 8 . 3 °± 0 . 5 °, 8 . 8 °± 0 . 5 °, 16 . 9 °± 0 . 5 °, 17 . 5 °± 0 . 5 °, 19 . 0 °± 0 . 5 °, 21 . 3 °± 0 . 5 °, 23 . 8 °± 0 . 5 °, 25 . 3 °± 0 . 5 °, 25 . 8 °± 0 . 5 ° and 26 . 8 °± 0 . 5 °. in some embodiments the maleate salt may be further characterised as showing on x - ray diffraction at least four peaks on the 2theta scale selected from the group consisting of 8 . 3 °± 0 . 5 °, 8 . 8 °± 0 . 5 °, 16 . 9 °± 0 . 5 °, 17 . 5 °± 0 . 5 °, 19 . 0 °± 0 . 5 °, 21 . 3 °± 0 . 5 °, 23 . 8 °± 0 . 5 °, 25 . 3 °± 0 . 5 °, 25 . 8 °± 0 . 5 ° and 26 . 8 °± 0 . 5 °. in some embodiments the maleate salt may be further characterised as showing on x - ray diffraction at least six peaks on the 2theta scale selected from the group consisting of 8 . 3 °± 0 . 5 °, 8 . 8 °± 0 . 5 °, 16 . 9 °± 0 . 5 °, 17 . 5 °± 0 . 5 °, 19 . 0 °± 0 . 5 °, 21 . 3 °± 0 . 5 °, 23 . 8 °± 0 . 5 °, 25 . 3 °± 0 . 5 °, 25 . 8 °± 0 . 5 ° and 26 . 8 °± 0 . 5 °. in some embodiments the maleate salt may be further characterised as showing on x - ray diffraction peaks on the 2theta scale at 8 . 3 °± 0 . 5 °, 8 . 8 °± 0 . 5 °, 16 . 9 °± 0 . 5 °, 17 . 5 °± 0 . 5 °, 19 . 0 °± 0 . 5 °, 21 . 3 °± 0 . 5 °, 23 . 8 °± 0 . 5 °, 25 . 3 °± 0 . 5 °, 25 . 8 °± 0 . 5 ° and 26 . 8 °± 0 . 5 °. in some embodiments the maleate salt may be further characterised as showing on x - ray diffraction peaks on the 2theta scale at 10 . 6 °± 0 . 5 °, 13 °± 0 . 5 °, 14 . 1 °± 0 . 5 °, 17 . 5 °± 0 . 5 °, 18 . 3 °± 0 . 5 °, 20 . 7 °± 0 . 5 °, 22 . 3 °± 0 . 5 °, 22 . 7 °± 0 . 5 °, 23 . 1 °± 0 . 5 °, 28 . 2 °± 0 . 5 °, 28 . 5 °± 0 . 5 °, 29 . 1 °± 0 . 5 °, 30 . 5 °± 0 . 5 °, 31 . 3 °± 0 . 5 °, 35 . 0 °± 0 . 5 ° and 36 . 8 °± 0 . 5 °. whilst the peaks discussed above are the characteristic peaks the maleate salt may also show on x - ray diffraction peaks on the 2theta scale at 7 . 0 °± 0 . 5 °, 9 . 2 °± 0 . 5 °, 11 . 4 °± 0 . 5 ° and 27 . 5 °± 0 . 5 °. as will be appreciated by a skilled worker in the field the relative intensities of the diffractions can vary depending upon a number of factors such as the method of the sample preparation and the type of instrument used . in addition in certain instances some of the peaks referred to above may not be detectable . the salts of the present invention may be produced by reaction of the free base of compound i with an appropriate form of maleic acid in an appropriate solvent and recovering from the reaction mixture the resultant salt after crystallisation , precipitation or evaporation . the reaction to form the salt may be carried out in any non - interfering solvent , or mixture of solvents , in which the free base has appropriate solubility . examples of suitable solvents of this type include toluene , tetrahydrofuran and water . the process typically involves dissolution of the free base in the appropriate solvent at elevated temperature such as greater than 20 ° c . in some embodiments , eg tetrahydrofuran , the free base is dissolved in the solvent at a temperature of about 65 ° c . in some embodiments , eg water , the free base is dissolved in the solvent at a temperature of about 95 ° c . once the free base has been dissolved in the appropriate solvent the process then involves addition of a suitable amount of the acid . the amount of acid may vary although typically the amount of acid used is a stoichiometric equivalent or a slight stoichiometric excess . following addition of the acid the process then typically involves stirring of the reaction mixture at the addition temperature for a period of 1 hour followed by cooling of the reaction mixture to a temperature below the reaction temperature to facilitate crystallisation . once the desired level of crystal formation has occurred the crystals may be isolated by filtration and dried using normal means in the art . in another embodiment the present invention provides the use of the salts of the invention in the treatment of proliferative disorders . the formulations and methodology for the use of compounds of this type and the disorders that may be treated thereby are as disclosed in pct / sg2006 / 000352 . the present invention will now be described with reference to the following non - limiting examples . hydrochloride salts were prepared as discussed above for comparative examples and analysed in an analogous manner . the free base 11 -( 2 - pyrrolidin - 1 - yl - ethoxy )- 14 , 19 - dioxa - 5 , 7 , 26 - triaza - tetracyclo [ 19 . 3 . 1 . 1 ( 2 , 6 ). 1 ( 8 , 12 )] heptacosa - 1 ( 25 ), 2 ( 26 ), 3 , 5 , 8 , 10 , 12 ( 27 ), 16 , 21 , 23 - decaene was dissolved in dichloromethane , brought to reflux and treated with activated carbon . the mixture was filtered hot through a pad of celite and washed with dichloromethane . to the filtrate was added methanolic hcl and the mixture was stirred at 10 - 15 ° c . for 2 - 3 hours . the slurry was cooled to 5 - 10 ° c ., filtered , washed with heptane and dried in a vacuum oven at 40 - 45 ° c . to afford 11 -( 2 - pyrrolidin - 1 - yl - ethoxy )- 14 , 19 - dioxa - 5 , 7 , 26 - triaza - tetracyclo [ 19 . 3 . 1 . 1 ( 2 , 6 ). 1 ( 8 , 12 )] heptacosa - 1 ( 25 ), 2 ( 26 ), 3 , 5 , 8 , 10 , 12 ( 27 ), 16 , 21 , 23 - decaene hydrochloride . compound i ( 50 mg , 0 . 106 mmol ) was suspended in either thf or toluene ( 2 ml ), and gently heated to 65 ° c . until it became a clear solution . the solution was then treated with 1 equivalent of maleic acid , heated at 65 ° c . for one hour and slowly cooled down to 5 ° c . overnight to facilitate crystallisation . the crystals thus formed were then isolated by filtration . the samples of both hydrochloride ( comparative ) and maleate salts were subjected to thermal gravimetric analysis and differential scanning calorimetry under the following conditions . dsc data were collected on a ta instruments q2000 equipped with a 50 position auto - sampler . the instrument was calibrated for energy and temperature calibration using certified indium . typically 0 . 5 - 3 mg of each sample , in a pin - holed aluminium pan , was heated at 10 ° c .· min − 1 from 25 ° c . to 270 ° c . a nitrogen purge of 50 ml · min − 1 was maintained over the sample . the instrument control software was thermal advantage v4 . 6 . 6 and the data were analysed using universal analysis v4 . 3a . alternatively , dsc data were collected on a mettler dsc 823e equipped with a 50 position auto - sampler . the instrument was calibrated for energy and temperature using certified indium . typically 0 . 5 - 3 mg of each sample , in a pin - holed aluminium pan , was heated at 10 ° c .· min − 1 from 25 ° c . to 270 ° c . a nitrogen purge at 50 ml · min − 1 was maintained over the sample . the instrument control and data analysis software was stare v9 . 01 . tga data were collected on a ta instruments q500 tga , equipped with a 16 position auto - sampler . the instrument was temperature calibrated using certified alumel . typically 5 - 30 mg of each sample was loaded onto a pre - tared platinum crucible and aluminium dsc pan , and was heated at 10 ° c .· min − 1 from ambient temperature to 300 ° c . a nitrogen purge at 60 ml · min − 1 was maintained over the sample . the instrument control software was thermal advantage v4 . 6 . 6 and the data were analysed using universal analysis v4 . 3a . alternatively , tga data were collected on a mettler tga / sdta 851e equipped with a 34 position auto - sampler . the instrument was temperature calibrated using certified indium . typically 5 - 30 mg of each sample was loaded onto a pre - weighed aluminium crucible and was heated at 10 ° c .· min − 1 from ambient temperature to 300 ° c . a nitrogen purge at 50 ml · min − 1 was maintained over the sample . the instrument control and data analysis software was stare v9 . 01 . the results of the scans are shown in the figures discussed above . the samples of both hydrochloride ( comparative ) and maleate salts were subjected to x - ray diffraction to determine the characteristic x - ray diffraction pattern . the conditions used were as follows : x - ray powder diffraction patterns were collected on a siemens d5000 diffractometer using cu kα radiation ( 40 kv , 40 ma ), θ - θ goniometer , divergence of v20 and receiving slits , a graphite secondary monochromator and a scintillation counter . the instrument is performance checked using a certified corundum standard ( nist 1976 ). samples run under ambient conditions were prepared as flat plate specimens using powder as received . approximately 35 mg of the sample was gently packed into a cavity cut into polished , zero - background ( 510 ) silicon wafer . the sample was rotated in its own plane during analysis . the details of the data collection are : alternatively , x - ray powder diffraction patterns were collected on a bruker axs c2 gadds diffractometer using cu kα radiation ( 40 kv , 40 ma ), automated xyz stage , laser video microscope for auto - sample positioning and a histar 2 - dimensional area detector . x - ray optics consists of a single göbel multilayer mirror coupled with a pinhole collimator of 0 . 3 mm . the beam divergence , i . e . the effective size of the x - ray beam on the sample , was approximately 4 mm . a θ - θ continuous scan mode was employed with a sample - detector distance of 20 cm which gives an effective 2θ range of 3 . 2 °- 29 . 7 °. typically the sample would be exposed to the x - ray beam for 120 seconds . samples run under ambient conditions were prepared as flat plate specimens using powder as received without grinding . approximately 1 - 2 mg of the sample was lightly pressed on a glass slide to obtain a flat surface . samples run under non - ambient conditions were mounted on a silicon wafer with heat - conducting compound . the sample was then heated to the appropriate temperature at ca . 10 ° c .· min − 1 and subsequently held isothermally for ca 2 minutes before data collection was initiated . the x - ray diffraction patterns for the maleate salts are shown in the figures discussed above . in order to probe the stability of the samples of the maleate salts variable temperature x - ray diffraction was carried out . thus , the salts were scanned under x - ray diffraction conditions at a series of temperatures and the characteristic peaks determined . the results of each of the scans are shown in the figures discussed above . the details of specific embodiments described in this invention are not to be construed as limitations . various equivalents and modifications may be made without departing from the essence and scope of this invention , and it is understood that such equivalent embodiments are part of this invention . | 2 |
the present invention provides a method for preparing metal oxide nanoparticles , which includes dipping a cathode and an anode formed of a metal for forming oxide , in an inorganic electrolyte solution containing halogen salt ( step 1 ); and applying voltage to the anode and the cathode to form , on the anode , metal oxide forming an anode surface . in a typical method for preparing metal oxide nanoparticles , an expensive precursor is required , a process is performed under high temperature and high pressure conditions , a surfactant is required ( where there is a possibility of contamination due to the surfactant ), the time is consumed , or a complex preparing process having a multi - stage is required . however , in the present invention , high temperature and high pressure conditions are not required , even though a surfactant is not used , individual particles are well separated from each other , and crystalline metal oxide nanoparticles may be prepared through a simple process and in a short time . hereinafter , a method for preparing metal oxide nanoparticles according to the present invention will be described in detail for each step . in the method for preparing the metal oxide nanoparticles according to the present invention , step 1 is a step of dipping a cathode and an anode formed of a metal forming oxide , in an inorganic electrolyte solution containing a halogen salt . at this time , a surfactant is not used , and a halogen salt - containing solution may be used as an electrolyte . the halogen salt - containing solution is cheaper and is easier to find than organic solvents including a surfactant . also , the surfactant is poisonous and thus is not environmentally - friendly , whereas since the halogen salt - containing solution used in the present invention uses ions ( for example , k + , na + and cl − ) that are abundant even in nature , the halogen salt - containing solution is eco - friendly . furthermore , when the surfactant is contained , nanoparticles containing a high percentage of impurities may be prepared , but since the surfactant is not used in the present invention , high purity nanoparticles may be prepared . the metal of the step 1 may be at least one selected the group consisting of indium , tin , zinc , zirconium , aluminum , titanium , nickel , iron and copper , but is not limited thereto . like this , the present invention does not use a specific metal , but may use various metals and alloys as an anode to prepare various metal oxides . the anode of the step 1 may have a wire shape or a sheet shape , but is not limited thereto , and the shape of the anode , which is able to be oxidized through electrolysis , may be appropriately selected to be used . the cathode of the step 1 may use platinum , but is not limited thereto , and a cathode capable of oxidizing the anode may be appropriately selected to be used . the halogen salt of the step 1 may use nacl , kcl or a mixture thereof , but is not limited thereto . the halogen salt is cheaper and is easier to find than the surfactant used in the typical method , and is eco - friendly . the inorganic electrolyte solution of the step 1 may have a concentration of 0 . 2 m or 3 . 5 m . the shape of a metal oxide to be prepared may be adjusted by adjusting the concentration of the inorganic electrolyte solution . when the inorganic electrolyte solution of the step 1 has a concentration of less than 0 . 2 m , metal oxide may not be rapidly formed , and when the inorganic electrolyte solution of the step 1 has a concentration of more than 3 . 5 m , an electrolyte may not be dissolved in water . in the method for preparing the metal oxide nanoparticles according to the present invention , step 2 is a step of applying voltage to the anode and the cathode to form , on the anode , metal oxide forming an anode surface . at this time , the voltage of the step 2 may be applied in a range of 5 v to 30 v . in the present invention , the metal oxide may be prepared even in the low voltage range , and the size of the metal oxide may be adjusted by adjusting the voltage level . when the voltage of the step 2 is less than 5 v , the metal oxide may not be formed , and when the voltage is applied in excess of 30 v , current excessively flows to evaporate the solution , so an unexpected result may be produced in a preparing process . the step 2 may be performed in a temperature range of 0 ° c . to 100 ° c . in the present invention , metal oxide nanoparticles may be prepared in a temperature range of 0 ° c . to 100 ° c ., or in a relatively low temperature range compared to the typical method for preparing metal oxide nanoparticles . when the step 2 is performed at a temperature of 0 ° c . or less , since the solution may be frozen not to proceed a reaction , and when the step 2 is performed at a temperature of more than 100 ° c ., the solution may be boiled . meanwhile , before performing the step 1 , the method for preparing the metal oxide nanoparticles of the present invention may further include ultrasonic - treating , washing and drying the anode . since the steps are performed , a higher purity metal oxide may be formed , and the metal oxide may be more smoothly formed . at this time , the ultrasonic - treating may be performed in at least one solvent selected from the group consisting of acetone , isopropyl , alcohol and methanol , but is not limited thereto . the washing may be performed by using deionized water , the drying may be performed by using high pressure air , but the washing and the drying are not limited thereto . also , after performing the step 2 , the method for preparing the metal oxide nanoparticles of the present invention may further include firing , washing , ultrasonic - treating , centrifuging and then firing the prepared metal oxide nanoparticles . since the steps are further performed , the prepared metal oxide nanoparticles may be separated and collected . at this time , the firing may be performed in a temperature range of 300 + c . to 600 ° c . when the firing is performed at a temperature of less than 300 ° c ., crystallinity may not well appear . also , the firing may be performed for 1 hour to 5 hours while temperature rises at a rate of 1 ° c ./ minute to 10 ° c ./ minute , but is not limited thereto . the present invention provides metal oxide nanoparticles that are manufactured through the methods and have a diameter of 1 nm to 10 nm . the metal oxide nanoparticles according to the present invention are well separated from each other . also , the metal oxide nanoparticles have crystallinity without annealing , and are prepared without using a surfactant to have a high purity . furthermore , the size of nanoparticles to be prepared may be adjusted by adjusting the voltage level . the present invention provides a lithium ion battery , a drug delivery material and a catalyst that include the metal oxide nanoparticles . since the metal oxide nanoparticles according to the present invention may be prepared through a simple process and in a short time , the metal oxide nanoparticles may be mass - produced , and be applied to all metals . therefore , the metal oxide nanoparticles may contribute to various fields such as a lithium ion battery , a supercapacitor , a catalyst , a gas sensor , a solar cell , an mri , a high heat treatment and drug delivery , and an absorption and separation . the present invention provides a method for adjusting a size of metal oxide nanoparticles , which includes dipping a cathode and an anode formed of a metal for forming oxide , in an inorganic electrolyte solution containing halogen salt ( step 1 ); and adjusting a voltage applied to the anode and the cathode ( step 2 ). in the present invention , the size of metal oxide nanoparticles may be adjusted at room temperature through a simple method for adjusting voltage in electrolyzing even though a surfactant is not used . hereinafter , a method for adjusting a size of metal oxide nanoparticles according to the present invention will be described in detail for each step . in the method for adjusting the size of the metal oxide nanoparticles , step 1 is a step of dipping a cathode and an anode formed of a metal for forming oxide , in an inorganic electrolyte solution containing a halogen salt . at this time , even though a surfactant is not used , a halogen salt - containing solution may be used as an electrolyte . the metal of the step 1 may be at least one selected the group consisting of indium , tin , zinc , zirconium , aluminum , titanium , nickel , iron and copper , but is not limited thereto . the anode of the step 1 may have a wire shape or a sheet shape , but is not limited thereto , a shape of an anode that is able to be oxidized through electrolysis , may be appropriately selected to be used . the cathode of the step 1 may use platinum , but is not limited thereto , a cathode capable of oxidizing the anode , may be appropriately selected to be used . the halogen salt of the step 1 may use nacl , kcl or a mixture thereof , but is not limited thereto . the inorganic electrolyte solution of the step 1 may have a concentration of 0 . 2 m or 3 . 5 m . when the inorganic electrolyte solution of the step 1 has a concentration of less than 0 . 2 m , metal oxide may not be rapidly formed , and when the inorganic electrolyte solution of the step 1 has a concentration of more than 3 . 5 m , an electrolyte may not be dissolved in water . in the method for adjusting the size of the metal oxide nanoparticles according to the present invention , the step 2 is a step of adjusting a voltage applied to the anode and the cathode . as voltage is increased , large - sized metal oxide nanoparticles may be prepared , and as voltage is decreased , small - sized metal oxide nanoparticles may be prepared . at this time , the voltage of the step 2 may be applied in a range of 5 v to 30 v . when the voltage of the step 2 is of less than 5 v , metal oxide may not be formed , and when the voltage is applied in excess of 30 v , current excessively flows to evaporate the solution , so an irregular result may be produced in a preparing process . the step 2 may be performed in a temperature range of 0 ° c . to 100 ° c . when the step 2 is performed at a temperature of 0 ° c . or less , since the solution may be frozen not to proceed a reaction , and when the step 2 is performed at a temperature of more than 100 ° c ., the solution may be boiled . meanwhile , before performing the step 1 , the method for preparing the metal oxide nanoparticles of the present invention may further include ultrasonic - treating , washing and drying the anode . at this time , the ultrasonic - treating step may be performed in at least solvent selected from the group consisting of acetone , isopropyl , alcohol and methanol , but is not limited thereto . the washing may be performed by using deionized water , the drying may be performed by using high pressure air , but the washing and the drying are not limited thereto . further , after performing the step 2 , the method for preparing the metal oxide nanoparticles of the present invention may further include firing , washing , ultrasonic - treating , centrifuging and then firing the prepared metal oxide nanoparticles . since the steps arte performed , the prepared metal oxide nanoparticles may be separated and collected . at this time , the firing may be performed in a temperature range of 300 ° c . to 600 ° c . when the firing is performed at a temperature of less than 300 ° c ., crystallinity may not well appear . hereinafter , the present invention will be described in more detail though examples . however , the following embodiments are strictly for the purpose of explaining the present invention , and do not limit the scope of the present invention . step 1 : an indium metal wire ( having a purity of 99 . 9 % and purchased from nilaco corporation ) was ultrasonic - treated in acetone , isopropyl , alcohol and methanol for 5 minutes , respectively , was washed by deionized water , and was dried by using high pressure air to be prepared as an anode . platinum having a size of 15 × 25 × 0 . 2 mm 3 was prepared as a cathode . a solution made by dissolving potassium chloride ( purchased from sigma aldrich ) in deionized water was prepared in a concentration of 1m as an electrolyte . step 2 : a voltage of 10 v was applied to the anode and the cathode of step 1 to prepare a metal oxide while the electrolyte was maintained at a temperature of 20 ° c . the generated various metal oxide nanoparticles were washed enough to wash out a salt by using deionized water , were ultrasonic - treated and then were collected by using a centrifugal separator . after that , the collected nanoparticles were fired by elevating the temperature at a rate of 3 ° c . per minute from a temperature of 450 ° c ., and were cooled at room temperature to prepare indium oxide nanoparticles . except that a tin metal wire was used as an anode unlike in the step 1 of example 1 , example 2 was performed in the same manner as example 1 to prepare tin oxide nanoparticles . except that a zinc metal wire was used as an anode unlike in the step 1 of example 1 , example 3 was performed in the same manner as example 1 to prepare zinc oxide nanoparticles . except that a zirconium metal wire was used as an anode unlike in the step 1 of example 1 , example 4 was performed in the same manner as example 1 to prepare zirconium oxide nanoparticles . except that an aluminum metal wire was used as an anode unlike in the step 1 of example 1 , example 5 was performed in the same manner as example 1 to prepare aluminum oxide nanoparticles . except that a titanium metal wire was used as an anode unlike in the step 1 of example 1 , example 6 was performed in the same manner as example 1 to prepare titanium oxide nanoparticles . except that a nickel metal wire was used as an anode unlike in the step 1 of example 1 , example 7 was performed in the same manner as example 1 to prepare nickel oxide nanoparticles . except that an iron metal wire was used as an anode unlike in the step 1 of example 1 , example 8 was performed in the same manner as example 1 to prepare iron oxide nanoparticles . except that a copper metal wire was used as an anode unlike in the step 1 of example 1 , example 9 was performed in the same manner as example 1 to prepare copper oxide nanoparticles . except that a nickel - iron alloy wire ( where a nickel content is 50 weight %, and an iron content is 50 weight %) was used as an anode unlike in the step 1 of example 1 , example 10 was performed in the same manner as example 1 to prepare nickel ferrite nanoparticles . except that a cobalt - iron alloy wire ( where a cobalt content is 50 weight %, and an iron content is 50 weight %) was used as an anode unlike in the step 1 of example 1 , example 11 was performed in the same manner as example 1 to prepare cobalt ferrite nanoparticles . preparing of copper - cobalt ferrite ( cu 1 co 1 fe 2 o 5 ) nanoparticles except that a copper - cobalt - iron alloy wire ( where a copper content is 33 . 3 weight %, a cobalt content is 33 . 3 weight %, and an iron content is 33 . 3 weight %) was used as an anode unlike in the step 1 of example 1 , example 12 was performed in the same manner as example 1 to prepare copper - cobalt ferrite nanoparticles . preparing of indium oxide ( 1 n 2 o 3 ) nanoparticles ( 5v ) except that a voltage of 5 v was applied unlike in the step 2 of example 1 , example 13 was performed in the same manner as example 1 to prepare indium oxide nanoparticles . preparing of indium oxide ( in 2 o 3 ) nanoparticles ( 15 v ) except that a voltage of 15 v was applied unlike in the step 2 of example 1 , example 14 was performed in the same manner as example 1 to prepare indium oxide nanoparticles . preparing of indium oxide ( in 2 o 3 ) nanoparticles ( 25 v ) except that a voltage of 25 v was applied unlike in the step 2 of example 1 , example 15 was performed in the same manner as example 1 to prepare indium oxide nanoparticles . except that nanoparticles were collected by using a centrifugal separator , and then were dried in an oven having a temperature of 60 ° c . for 12 hours unlike in the step 2 of example 3 , example 16 was performed in the same manner as example 3 to prepare zinc oxide nanoparticles . except that sodium chloride was used as an electrolyte instead of potassium chloride unlike in the step 1 of example 1 , example 17 was performed in the same manner as example 1 to prepare zinc oxide nanoparticles . in order to confirm the preparation of the metal oxide of example 16 , metal oxide nanoparticles were observed with the naked eye , and the observed result was shown in fig2 . as shown in fig2 , it may be confirmed that white zinc oxide is formed through an anodizing method to be precipitated , and it may seen that when the white zinc oxide is centrifuged and then is dried , white nanoparticles are obtained in a large amount . in order to confirm crystallinity of metal oxides prepared in examples 1 to 9 , metal oxide nanoparticles were observed with an x - ray diffraction analyzer , and the observed results were shown in fig3 to 7 . as shown in fig3 to 7 , it may be seen that each of metal oxides shows a specific peak . accordingly , it may be seen that metal oxide prepared according to the present invention shows crystallinity , and also has a high purity . the crystallinity of nanoparticles described above is caused due to an high temperature electrolyte that is raised to a temperature of 90 ° c . during anodizing . also , since a surfactant is not used , it may be seen that the nanoparticles have high purity . in order to confirm a micro structure of metal oxides prepared in examples 1 to 11 , after metal oxide nanoparticles were observed with a field - emission scanning electron microscope ( fe - sem ), the observed results were shown in fig8 to 9 , and after the metal oxide nanoparticles were observed with a transmission electron microscope ( tem ), the observed results were shown in fig1 to 11 . as shown in fig8 to 9 , it may be seen that particles of each metal oxides haves a globular shape , and exist in a well separate state from each other . also , it may be seen that each of nanoparticles is clearly observed , and lumps of nanoparticles are compressed . as shown in fig1 and 11 , it may be seen that almost all nanoparticles have a globular shape and have an average diameter of less than 10 nm . in addition , nanoparticles are uniformly distributed , and each of nanoparticles is clearly observed in a microscope image . a size distribution may be calculated from a transmission electron microscope image and an xrd pattern , the calculated size was ± 3 nm . in order to analyze a component of metal oxides prepared in example 1 to 3 , 6 to 8 , 9 and 12 , the metal oxide particles were observed with an energy dispersive x - ray analyzer ( edax ), and the results are shown fig1 and 13 . as shown in fig1 and 13 , it may be conformed that metal oxide is prepared as intended . therefore , it may be seen that various metal oxide nanoparticles are formed through an anodizing method . in order to observe a size of metal oxides prepared in examples 13 to 14 , after metal oxide nanoparticles were observed with a field - emission scanning electron microscope ( fe - sem ), the observed results were shown in fig1 , after the metal oxide nanoparticles were observed with using a scale of a photograph , the observed results were shown in fig1 to 17 , and a size according to voltage level was shown in fig1 . as shown in fig1 and 18 , in a case of example 13 in which voltage is 15 v , an average particle size was 29 nm , but as voltage was increased to 15 v and 25 v , an average particle size was increased to 32 nm and 35 nm . also , as a voltage was increased , a radius sd of particles was increased from 5 nm to 7 nm . therefore , it may seen that while voltage is adjusted in a range of 5 v to 15 v , a particle size may be adjusted in a range of 29 nm to 35 nm , and a size of particles required for a specific use may be obtained through a voltage adjustment in preparing nanoparticles . | 1 |
[ 0024 ] fig1 d illustrates a knife sheath or covering in accordance with the present invention . the sheath includes a sheath body or scabbard 200 , having a front edge 202 , back edge 203 , tip 204 , and top edge 205 . the sheath also includes a suspension or carrying strap 210 and securing member 215 . in the illustrated embodiment , the sheath body 200 is a scabbard or casing made of a robust material such as cordura nylon which is shaped to provide a particular profile when folded and stitched as shown . the suspension strap 210 , also made of cordura nylon , includes a strip of material formed into a loop , stitched together at one end , and secured to the sheath body 200 at an attachment point 220 . cordura nylon is but one of many possible materials suitable for use with the present invention . it is appreciated that several other materials may also be used without deviating from the principles of the present invention , such as plastic or polymer , metal or metal alloy , natural or synthetic fibers or fabrics , or a composite material including metals , ceramics , fabrics , fibers , polymers , or any combination thereof . as shown in fig1 d , the suspension strap 210 is angled with respect to the sheath body 200 with respect to the centerline axis of the sheath body 200 . the knife handle securing mechanism or strap 215 is shown as a strip of cordura nylon passed through an opening 225 defined by the upper end of the suspension strap 210 . although the securing strap 215 is shown as being freely slidable through the opening 225 , it can alternatively be fixedly secured thereto . hook and pile fasteners 230 and 235 , respectively , are disposed on opposing sides of the securing strap 215 so as to be engagable when the securing strap 215 is formed into a loop . [ 0026 ] fig2 through 7 illustrate additional views of the knife sheath , wherein fig2 is a view from the sheath tip 204 ; and fig3 is a view from the top edge 250 of the suspension strap 210 . fig4 is a plan view of the opposite side of the knife sheath presented in fig1 d , and fig5 is a plan view of the knife sheath side as presented in fig1 d . fig6 depicts the knife sheath from the front edge 202 , and fig7 shows the opposite back edge 203 of the knife sheath . [ 0027 ] fig2 shows the sheath from the top , illustrating the open mouth 270 of the sheath body 200 . the mouth 270 may be any form of opening or channel defined by the top edge 205 of the sheath body 200 so as to allow for the entry of a blade . fig3 shows the sheath from the bottom , wherein the tip 204 is sown or closed . it is understood however , that the particular configuration of the mouth 270 and tip 204 may vary widely depending on the particular shape of the knife and knife blade , and is by no means limited to the particular geometries displayed in the figures . [ 0028 ] fig4 illustrates the advantageous configuration of the knife sheath shown in fig1 d . as shown in fig4 body 200 has a longitudinal axis 300 . the top edge 250 of the securing strap 215 has a transverse axis 310 tangent to the top edge 250 of the suspension strap 210 . a second transverse axis 320 , parallel to transverse axis 310 is also shown . each of transverse axes 310 and 320 are orthogonal to the longitudinal axis 330 of the suspension strap 210 . an additional tangential axis 340 is shown , it being tangent to the top edge 205 of the body 200 . an angle α is therefore formed between the longitudinal axis 300 of the body 200 and the longitudinal axis 330 of the suspension strap . another angle β is formed between the tangential axis 340 and the transverse axis 320 . although the embodiment depicted in fig1 - 7 bears the particular angles and configuration shown , the angles and relative orientation of the axes discussed herein may be varied without deviating from the principles of the invention . angle α may vary from zero to forty - five degrees or more . angle β may vary from zero to forty - five degrees or more . one practical range for both angles α and β is approximately two to twenty - five degrees for each . another exemplary , yet more narrow , range for angle α would be approximately eight to fifteen degrees , while a narrower exemplary range for angle β would be approximately ten to twenty degrees . the angle α shown in fig4 is approximately 10 degrees , while the angle β is approximately twelve degrees . the sheath may be utilized such that a user inserts a belt ( not shown ) through the loop 225 formed by the suspension strap 210 . the belt may be , for example , in alignment with transverse axes 310 and 320 and may fit therebetween . if the sheath were thus to hang from the belt , the longitudinal axis 330 of the suspension strap 210 would be in substantial alignment with a gravity vector { right arrow over ( g )}. thus the angle that the body 200 would make with gravity would be angle α , while the angle that the top edge 205 of body 200 would make with the horizontal to gravity would be angle β . it is also apparent from fig4 that the tangential axis is aligned with neither the transverse axis 320 , or with a separate axis ( not shown ) transverse to the longitudinal axis 300 of the sheath body 200 . this easily confirmed by inspection of an angle γ between the axes 300 and 340 , in that angle γ is always less than a right angle . it is precisely because angles α and β are orientated with respect to a gravity vector { right arrow over ( g )} that the knife sheath has its advantageous qualities . first , because of angle α deviating from zero degrees , a user of the sheath may be able the easily insert a curved or angled knife into the sheath using a more natural motion rather than a straight up and down motion aligned with the gravity vector . second , because of angle β deviating from zero degrees , the handle portion of a curved or angled knife may be more easily buttressed against the top edge 205 of the sheath body 200 . [ 0032 ] fig5 illustrates another plan view of the sheath shown in fig4 including the body 200 , suspension strap 210 and securing strip 215 . this view of the present invention emphasizes that strap 210 may not be a loop at all , but may be a roughly “ two - dimensional ” carrying member , such as a simple rectangular strip as the securing strip 215 . the securing strip 215 may for example be affixed to the upper or proximal end portion of the carrying member 210 at a right angle , while the lower or distal end portion of the carrying member 210 may be affixed to the upper or proximal end portion of the body 200 at an angle commensurate with the alignments discussed above with regard to and illustrated in fig4 . or the securing member 215 may be omitted entirely , and the carrying member may be provided with a hole , hook , or some other mechanism for connecting to a junction or point for carrying the sheath , wherein the sheath may then freely hang such that the axis longitude 330 of the carrying member is not aligned with the axis of longitude 300 of the sheath body or scabbard 200 . [ 0033 ] fig6 is a view of the sheath from the front edge 202 . fig6 also shows a knife 400 positioned alongside the sheath yet with the blade 440 outside the body 200 for ease of viewing . the knife 400 includes a handle portion 420 , which is disposed substantially parallel to and against the suspension strap 210 , such that ends of the securing strip 215 may be wrapped around the handle 420 in the direction of the arrows d as shown . [ 0034 ] fig7 shows the sheath from the back edge 203 of the body 200 . finally , fig8 is a transverse sectional view of the sheath body 200 , taken along section 8 - 8 in fig4 . the body 200 includes an outer shell 500 , and may further include an inner shell 510 enclosing the interior space 520 of the sheath body 200 . a knife blade ( not shown ) inserted into the sheath body 200 will be thus disposed inside of the space 520 . the outer shell 500 may be made of a robust material such as cordura nylon , or some other fiber , fabric , composite , or other suitable material . the outer shell 500 may be rigid or flexible , yet substantially non - deformable . the inner shell 510 may in turn be more rigid , and may be made of a suitably rigid material such as a polymer such as polyvinylchloride ( pvc ). the sheath may also include a series of ridges 530 , which resemble linear “ bumps ” or strips that run the length of the body 200 parallel to longitudinal axis 300 , and are positioned on the inner surface of inner shell 510 as shown in fig8 . the ridges are preferably made of a softer pvc - like material , and have a sufficient adhesive property to grip a smooth metal blade through static friction . the frictional grip imposed by the ridges 530 runs along the length of a blade , and hence provides an improved means of gripping the blade and keeping the knife inside of the sheath as desired . it will be appreciated by persons skilled in the art that the present invention is not limited to what has been particularly shown and described herein above . in addition , unless mention was made above to the contrary , it should be noted that all of the accompanying drawings are not to scale . a variety of modifications and variations are possible in light of the above teachings without departing from the scope and spirit of the invention , which is limited only by the following claims . | 0 |
fig1 illustrates an example system constructed in accordance with the teachings of the invention to meter content exposure using closed caption information . the example system of fig1 meters a ) content being presented and / or consumed at the time that the content is broadcast and / or b ) content not being presented and / or consumed at the time that the content is broadcast ( e . g ., the system meters content being presented and / or consumed that was earlier recorded at the time of broadcast and is now being presented at a later time ( i . e ., time shifted viewing )). to meter content exposure , the example system of fig1 uses closed caption information and / or content identifiers . as used herein , a “ content identifier ” is any type of data and / or information associated with , embedded with , inferable from and / or injected into a piece of content , and which may be used to identify that piece of content . audience measurement codes ( e . g ., audio codes , audio watermarks , video watermarks , vertical blanking interval ( vbi ) codes , image watermarks and / or any other watermarks embedded in content by content providers such as television and / or radio broadcasters to facilitate identification of content ), public or private identifiers in bit streams , closed captioning information , metadata , signatures , or any other type ( s ) of data can serve as content identifiers . a content identifier is generally not noticeable to the audience during playback , but this is not necessarily so . for content currently being broadcast , the example system of fig1 utilizes audience measurement codes and / or signatures ( e . g ., audio , video , image and / or otherwise ) to identify the content being presented and / or consumed . in particular , the collected audience measurement codes and / or signatures may be compared with a database of audience measurement codes and / or signatures that represents known content to facilitate identification of the content being presented . likewise , for previously recorded content , the example system may also utilize audience measurement codes and / or signatures to identify the presented media content . since audience measurement codes and / or signatures determined from previously recorded content may be substantially time - shifted with respect to a reference database of audience measurement codes and / or signatures , the matching of audience measurement codes and / or signatures with the database to determine what content is being presented and / or consumed may become difficult and / or time consuming . as such , the example system of fig1 utilizes closed caption information to identify , at the time that content is presented and / or consumed , the most likely content being presented . this likely content information is then used , as described below , during matching of audience measurement codes and / or signatures determined from the previously recorded content with the database of audience measurement codes and / or signatures . in particular , the likely content information can enable comparison of extracted and / or determined audience measurement codes and / or signatures with a smaller subset of the audience measurement code database . closed caption information and / or likely presented and / or consumed content information may also be utilized for metering currently broadcasting content . to receive , play , view , record , and / or decode any type ( s ) of content , the example system of fig1 includes any type of media device 105 such as , for example , a set top box ( stb ), a digital video recorder ( dvr ), a video cassette recorder ( vcr ), a personal computer ( pc ), a game console , a television , a media player , etc . example content includes television ( tv ) programs , movies , videos , commercials , advertisements , audio , video , games , etc . in the example system of fig1 , the example media device 105 receives content via any type ( s ) of sources such as , for example : a satellite receiver and / or antenna 110 ; a radio frequency ( rf ) input signal 115 received via any type ( s ) of cable tv signal ( s ) and / or terrestrial broadcast ( s ); any type of data communication network such as the internet 120 ; any type ( s ) of data and / or media store ( s ) 125 such as , for example , a hard disk drive ( hdd ), a vcr cassette , a digital versatile disc ( dvd ), a compact disc ( cd ), a flash memory device , etc . in the example system of fig1 , the content ( regardless of its source ) may include closed caption information and / or data . alternatively or additionally , the closed caption information and / or data may be provided and / or received separately from the content itself . such separately received closed caption information and / or data may be synchronized to the content by the media device 105 and / or a content exposure meter 150 . to provide and / or broadcast content , the example system of fig1 includes any type ( s ) and / or number of content provider ( s ) 130 such as , for example , television stations , satellite broadcasters , movie studios , etc . in the illustrated example of fig1 , the content provider ( s ) 130 deliver and / or otherwise provide the content to the example media device 105 via a satellite broadcast using a satellite transmitter 135 and a satellite and / or satellite relay 140 , a terrestrial broadcast , a cable tv broadcast , the internet 120 , and / or media store ( s ) 125 . to meter exposure to and / or consumption of content , the example system of fig1 includes the content exposure meter 150 . the example content exposure meter 150 of fig1 receives audio data 155 and / or video data 160 from the example media device 105 . the example content exposure meter 150 also receives any type ( s ) of content guide information and / or data 165 . the content guide data 165 may be broadcast and / or delivered to , or downloaded and / or otherwise received by , the content exposure meter 150 via the internet 120 , the satellite input , the rf input 115 , the media device 105 and / or the media store ( s ) 125 . in some examples , content guide data 165 is an extensible markup language ( xml ) file containing , for example , tv programming information ( e . g ., a tv guide listing ) for any number of days and / or customized for the geographical location ( e . g ., zip or postal code ) of the content exposure meter 150 . the example content exposure meter 150 of fig1 may be , for example : ( a ) a pc , ( b ) may be implemented by , within and / or otherwise be associated with the example media device 105 , and / or ( c ) be an xml data collection server as described in pct patent application serial no . pct / us2004 / 000818 which is hereby incorporated by reference in its entirety . an example manner of implementing the example content exposure meter 150 is discussed below in connection with fig2 . an example process that may be carried out to implement the example content exposure meter 150 is discussed below in connection with fig6 . as described below in connection with fig2 and 6 , the example content exposure meter 150 of fig1 uses the content guide data 165 and / or data derived from the content guide data 165 , and closed caption information obtained from , for example , the video data 160 to identify , for example , one or more tv programs and / or movies that are likely being presented ( e . g ., viewed ) at and / or via the media device 105 . as described below , to enable metering of content exposure , the example content exposure meter 150 of fig1 collects and / or generates audience measurement codes and / or signatures that may be used to identify content being presented . in cases when content is presented and / or consumed out of synchronization with the time of content broadcast ( e . g ., the content being presented and / or consumed was earlier recorded at the time of broadcast and is currently being played back at and / or via the media device 105 ), the example content exposure meter 150 utilizes closed caption information and content guide information ( e . g ., electronic program guide ( epg ) information ) to identify which content , out of a set of potential content candidates , represents the content that was most probably presented to the panelist / user / household member . the example content exposure meter 150 may also use closed caption information to identify which currently broadcasting content is being presented and / or consumed . when content is stored and / or recorded , for example , at and / or via the media device 105 , any included and / or associated closed caption information and / or data is also stored . for example , if received content contains embedded closed caption information , the closed caption information is saved by virtue of the content being recorded . when performing content metering , the example content exposure meter 150 of fig1 divides the time during which content presentation occurs in to a set of presentation time intervals ( e . g ., 30 seconds ) and determines for each time interval the content most likely presented and / or consumed . the time intervals may be of any duration depending on the desired granularity of the metering to be performed . additionally , the duration of the time intervals may be fixed or may vary . for each presentation time interval , the example content exposure meter 150 of fig1 provides to a processing server 175 an ordered list of content candidates that represent the pieces of content that are and / or were most probably presented . the processing server 175 may be geographically separate from the content exposure meter 150 and / or may be co - located with the example content exposure meter 150 . in the example of fig1 , the ordered list of content candidates is provided to the processing server 175 as a list of content exposure hints 170 a . in the example of fig1 , the hints 170 a are ordered based upon the probability that the content candidate associated with each given hint is the content being presented and / or consumed during the time interval of interest and may include , for example , the three or four most probable items . the processing server 175 may receive and process content exposure hints 170 a from any number of content exposure meters 150 that may be geographically disbursed . as described below in connection with fig2 , the example content exposure meter 150 also collects any type ( s ) of audience measurement codes and / or signatures ( collectively audience measurement data ) 170 b ) from the audio data 155 . the audience measurement data 170 b is provided together with the content exposure hints 170 a to the processing server 175 . an example table used by the content exposure meter 150 to provide the hints 170 a and audience measurement data 170 b to the processing server 175 is discussed below in connection with fig4 . additionally or alternatively , the hints 170 a and audience measurement data 170 b may be formatted as an xml file . the audio measurement data 170 b may include and / or represent video codes , video signatures , image codes , image signatures , etc . for simplicity of discussion , the following disclosure references the use of any type of codes and / or signatures as audience measurement data 170 b . to facilitate the creation of hints 170 a to identify content that is presented and / or consumed out of synchronization with the time of content broadcast ( e . g ., previously recorded content ), the example content exposure meter 150 stores and / or otherwise retains content guide data 165 ( e . g ., epg data ) and / or data derived from the content guide data 165 collected during previous time periods ( e . g ., in the last 14 days ). in this way , as described below , the content exposure meter 150 can use currently collected and / or previously collected content guide data 165 and / or data derived from the currently collected and / or previously collected content guide data 165 to identify content presented ( e . g ., displayed , viewed and / or listened to ) at and / or via the media device 105 . in the illustrated example , the time period over which the content guide data 165 and / or data derived from the content guide data 165 is retained by the example content exposure meter 150 is the time period for which the example processing server 175 is programmed to compute and / or tabulate statistics regarding content exposure . in the illustrated example of fig1 , the hints 170 a and audience measurement data ( e . g ., codes and / or signatures ) 170 b are provided from the content exposure meter 150 to the processing server 175 on an occasional , periodic , or real time basis . any type ( s ) of technique ( s ) for downloading and / or transferring data from the example content exposure meter 150 to the example processing server 175 can be used . for example , the hints 170 a and audience measurement data 170 b can be transferred via the internet 120 , a public - switched telephone network ( pstn ) 180 , and / or a dedicated network . additionally or alternatively , the example content exposure meter 150 may periodically or aperiodically store the hints 170 a and audience measurement data 170 b on any type ( s ) of non - volatile storage medium ( e . g ., recordable compact disc ( cd - r )) that can be transported ( e . g ., picked up , mailed , etc .) to a processing service and then loaded onto the example processing server 175 . the example processing server 175 of fig1 utilizes the hints 170 a and audience measurement data 170 b received from the example content exposure meter 150 to determine which content was presented and / or consumed at and / or via the example media device 105 to form content exposure data for the media device 105 and / or for a collection of one or more media devices 105 . for example , the processing server 175 utilizes the hints 170 a to more efficiently compare the audience measurement data ( e . g ., codes and / or signatures ) 170 b collected by the content exposure meter 150 with the database of audience measurement data ( e . g ., codes and / or signatures ) stored and / or otherwise available at the processing server 175 . as discussed previously , the database of audience measurement data at the example processing server 175 ideally represents a large portion of the universe of content , thereby , increasing the likelihood of the accurate identification of any content presented and / or consumed at the example media device 105 . however , the larger the size of the database , the greater the processing power required to perform a search of all the audience measurement data stored in the database to identify a match . the example processing server 175 of fig1 may , for example , receive audience measurement data from the content provider ( s ) 130 and / or determine the audience measurement data for content 185 received at and / or by the processing server 175 . additionally , the content represented by the audience measurement data stored in the database may include content that has been broadcast and / or that will be broadcast , and / or content that has not yet been broadcast but that is otherwise available to the user via dvd , vcr , or other storage medium . using the hints 170 a , the example processing server 175 can limit the amount of audience measurement data that must be compared and , thus , process content exposure metering information 170 b from a substantially larger number of content exposure meters 150 . an example processing server 175 is discussed below in connection with fig5 . an example process that may be carried out to implement the example processing server 175 is discussed below in connection with fig7 . the example processing server 175 of fig1 combines the determined content exposure data for a plurality of metered media devices 105 associated with a plurality of respondents to develop meaningful content exposure statistics . for instance , the processing server 175 of the illustrated example uses the combined content exposure data to determine the overall effectiveness , reach and / or audience demographics of viewed content by processing the collected data using any type ( s ) of statistical method ( s ). fig2 illustrates an example manner of implementing the example content exposure meter 150 of fig1 . to process the content guide data 165 , the example content exposure meter 150 of fig2 includes any type of indexing engine 205 . an example indexing engine 205 implements any method ( s ), algorithm ( s ) and / or technique ( s ) to process an xml file containing a plurality of records . processing the xml file causes the creation of an index that identifies keyword ( s ) that distinguish the plurality of records represented by the xml file . consider an example xml file that contains a tv guide listing in which each record in the xml file represents a separate tv program . each record in the xml file contains data about the tv program such as , for example , the channel number on which the tv program is broadcast , the name associated with the channel on which the tv program is broadcast , the program name of the tv program , a description of the content of the tv program , and the time at which the tv program is to be broadcast . the example indexing engine 205 indexes the xml data to remove as much redundant information as possible while retaining keywords useful for distinguishing the listed tv programs . for example , consider a 6 - 6 : 01 pm time slot having multiple tv programs with names and / or description that include “ news .” because the term “ news ” is “ locally common ” ( e . g ., appears in a second program in the relevant time period ), the example indexing engine 205 of fig2 does not include “ news ” in the indexed list of keywords . however , if one of those same tv programs includes in its program information a less locally commonly used term ( e . g ., the name of a special guest and / or a description of a special segment ), the example indexing engine 205 would include the less locally commonl term ( e . g ., the name of the special guest and / or one or more words from the description ) in the indexed list of keywords . to store the indexed keywords that may be developed by the indexing engine 205 or any other keyword server , the example content exposure meter 150 of fig2 includes a keyword database 210 . the keywords stored in the keyword database 210 are indexed to an associated channel number , channel name , program name , program information ( e . g ., description ) and / or broadcast time information . the example keyword database 210 may use any type ( s ) and / or number of data structure ( s ) ( e . g ., matrices , array ( s ), variable ( s ), register ( s ), data table ( s ), etc .) to store the indexed keywords . in the illustrated example , the keyword database 210 is stored in , for example , any type ( s ) of memory (- ies ) and / or machine accessible file ( s ) 215 . the example keywords database 210 of fig2 includes indexed keywords for a current time period ( e . g ., the current week ) as well as any number of previous time periods . the number and duration of time periods included in the keywords database 210 depends upon how far back in time the processing server 175 computes and / or tabulates statistics regarding content exposure . for example , the processing server 175 may be configured only to consider content from the previous fourteen ( 14 ) days . the example indexing engine 205 of fig2 periodically or aperiodically deletes and / or otherwise removes old keywords . to extract and / or decode closed caption data and / or information from the video data 160 , the example content exposure meter 150 of fig2 includes any type of closed caption decoding engine 220 . using any type ( s ) of method ( s ), algorithm ( s ), circuit ( s ), device ( s ) and / or technique ( s ), the example closed caption decoding engine 220 of fig2 decodes , for example , line 21 of national television system committee ( ntsc ) television signals or line 22 of phase alternation line ( pal ) television signals to extract closed caption text 222 . in the example system of fig1 and 2 , the example closed caption decoding engine 220 decodes the closed caption text 222 in real time with the review , display , viewing and / or playback of content at and / or via the media device 105 . additionally or alternatively , the video data 160 could be stored at the content exposure meter 150 and processed by the closed caption decoding engine 220 in non - real time . the example closed caption decoding engine 220 of fig2 also extracts and / or decodes the time information that is associated with the closed caption data and / or information ( i . e ., closed caption timestamps ) and that is embedded together with the closed caption data and / or information in the video data 160 . to determine the content most likely being presented and / or consumed at and / or via a media device , the example content exposure meter 150 of fig2 includes a closed caption matcher 225 . using any type ( s ) of method ( s ), algorithm ( s ), circuit ( s ), device ( s ) and / or technique ( s ), the example closed caption matcher 225 of fig2 compares the stream of closed caption text 222 with the indexed keywords in the keywords database 210 . when a match is determined , the content corresponding to the match is recorded . over a pre - determined time interval ( e . g ., 5 minutes ), the example closed caption matcher 225 counts the total number of matches identified and the number of matches made for each specific content ( e . g ., tv program ). in the example of fig2 , at the end of each time interval , the probability that a given content candidate is actually being presented and / or consumed is the number of matches for each content candidate divided by the total number of matches . the content candidate ( e . g ., tv program ) having the highest probability is the most likely content currently being presented and / or consumed . in the example of fig1 and 2 , the four pieces of content having the highest probability ( i . e ., most probably content being presented and / or consumed ) are provided to the processing server 175 as hints 170 a for the current time interval . however , any number of hints 170 a could be provided to the processing server 175 . fig3 illustrates an example histogram that represents the probability 305 ( i . e ., likelihood ) that each of a plurality of tv programs 310 was presented and / or consumed ( e . g ., viewed ) during each time interval 315 having a time duration of t minutes . as illustrated , each of the tv programs 310 is illustrated with a bar having a height that represents the likelihood that the tv program was being viewed during the interval 315 . in the example of fig3 , the most likely watched channel during the interval 315 was the evening news on the “ fox ” tv channel during the 6 : 00 - 6 : 01 pm time period on mar . 3 , 2006 , as indicated with bar 320 . in the illustrated examples of fig1 - 3 , the time period is determined based on the closed caption timestamp and , thus , has a granularity that is finer than the program start time , end time and / or program duration . the granularity depends upon the granularity of the closed caption time stamps and the length of the interval 315 . at the end of the interval 315 , the “ fox ”, “ nbc ”, “ abc ” and “ cbs ” are provided as hints to the processing server 175 . as the media device 105 continues to provide video data 160 , the closed caption matcher 225 of fig2 continues identifying and counting matches and , then at the end of each interval 325 , determines the probabilities for that interval 325 , and identifies to the processing server 175 the most likely four content candidates as hints 170 a associated with the time interval 325 currently being processed . additionally or alternatively , if a sufficient set of keywords is not available , the example closed caption matcher 225 of fig2 may not be able to identify the content being presented and / or consumed with certainty . for example , the example closed caption matcher 225 may only be able to identify that the tv station being watched is abc but not distinguish which tv program is being presented and / or consumed . likewise , the closed caption matcher 225 may be able to identify that the evening news is being presented and / or consumed , but not which tv channel . alternatively , no hints 170 a may be available for a given time interval . to collect audio codes for the audio data 155 , the example content exposure meter 150 of fig2 includes any type of audio code engine 230 . using any type ( s ) of method ( s ), algorithm ( s ), circuit ( s ), device ( s ) and / or technique ( s ), the example audio code engine 230 searches , locates , extracts and / or decodes audio codes inserted into the audio data 155 by content providers , such as television and / or radio broadcasters , to facilitate identification of content . such audio codes are commonly used in the industry for the purposes of detecting the exposure to content . however , persons of ordinary skill in the art will readily appreciate that not all content has inserted audio codes and / or signatures . to collect and / or generate audio signatures for the audio data 155 , the example content exposure meter 150 of fig2 includes any type of audio signature engine 235 . using any type ( s ) of method ( s ), algorithm ( s ), circuit ( s ), device ( s ) and / or technique ( s ), the example audio signature engine 235 of fig2 processes the audio data 155 to determine binary fingerprints and / or signatures that substantially and / or uniquely identify corresponding portions of the audio data 155 . an example audio signature is computed by applying data compression to the audio data 155 . in the illustrated examples of fig1 and 2 , the example closed caption matcher 225 provides the audience measurement data ( e . g ., audio codes and / or signatures and / or signatures ) 170 b together with the hints information 170 a to the processing server 175 . while an example content exposure meter 150 has been illustrated in fig2 , the elements , modules , logic , memory and / or devices illustrated in fig2 may be combined , re - arranged , eliminated and / or implemented in any way . for example , the example closed caption matcher 225 , the example indexing engine 205 , and / or the example keyword database 210 could be implemented separately from the example content exposure meter 150 ( e . g ., by and / or within the example processing server 175 ). in such examples , the content exposure meter 150 provides the closed caption information 222 and the audience measurement data 170 b to the processing server 175 , which generates the hints information 170 a at the processing server 175 . as described more fully below in connection with fig5 , the processing server 175 uses the generated hints information 170 a and the audience measurement data 170 b to identify content presented and / or consumed at and / or via a media device 105 being metered by the content exposure meter 150 . further , the example indexing engine 205 , the example keywords database 210 , the example memory and / or file 215 , the example closed caption matcher 225 , the example closed caption decoding engine 220 , the example audio code engine 230 , the example audio signature engine 235 and / or , more generally , the example content exposure meter 150 may be implemented by hardware , software , firmware and / or any combination of hardware , software and / or firmware . for example , the example indexing engine 205 , the example keywords database 210 , the example memory and / or file 215 , the example closed caption matcher 225 , the example closed caption decoding engine 220 , the example audio code engine 230 and / or the example audio signature engine 235 may be implemented via machine accessible instructions executed by any type of processor 150 such as , for example , a processor from the intel ®, sun ®, amd ® families of processors and / or microcontrollers . moreover , a content exposure meter may include additional elements , modules , logic , memory and / or devices and / or may include more than one of any of the illustrated elements , modules and / or devices such as , for example , a video code engine or a video signature engine . fig4 is an example hints and tuning information table having a plurality of entries 405 that each correspond to one of the hints 170 a provided by the content exposure meter 150 . in the example of fig4 , each of the plurality of entries 405 contains a time period interval identifier 410 , a content timestamp 412 that indicates when the content was presented and / or consumed , and hints information that includes one or more of : ( a ) a listing of the highest probability content sources ( e . g ., tv channels ) 415 , ( b ) a listing of the highest probability pieces of content ( e . g ., tv programs ) 420 , ( c ) a listing of the highest probability broadcast times 425 . according to the example of fig4 , each of the plurality of entries 405 also contains any audience measurement data 430 ( e . g ., audio codes and / or audio signatures ) located , extracted , decoded , identified and / or computed during the time period . the extent to which a particular timestamp entry 412 and a particular broadcast time 425 match is indicative of whether the corresponding content was presented and / or consumed live and / or was previously recorded and / or captured . while an example hints and tuning information table is illustrated in fig4 , persons of ordinary skill in the art will readily appreciate that any type ( s ) of file ( s ), data structure ( s ), table ( s ), etc may be used by the content exposure meter 150 to format the data prior to sending the data to the processing server 175 . also , more or fewer types of information may be included in the table . fig5 illustrates an example manner of implementing at least a portion of the example processing server 175 of fig1 . to determine audio codes and / or signatures for audio data 185 provided by and / or obtained from the content provider ( s ) 130 , the example processing server 175 of fig5 includes any type of audio code engine 505 . using any type ( s ) of method ( s ), algorithm ( s ), circuit ( s ), device ( s ) and / or technique ( s ), the example audio code engine 505 searches , locates , extracts and / or decodes and / or signatures audio codes and / or signatures inserted into the audio data 185 by content providers , such as television and / or radio broadcasters , to facilitate identification of content . such audio codes are commonly used in the industry for the purposes of detecting the exposure to content . however , persons of ordinary skill in the art will readily appreciate that not all content contains audio codes . additionally or alternatively , the content provider ( s ) 130 may only provide audio codes for content for which exposure and / or consumption statistics are desired . to determine audio signatures for the audio data 185 , the example processing server 175 of fig5 includes any type of audio signature engine 510 . using any type ( s ) of method ( s ), algorithm ( s ), circuit ( s ), device ( s ) and / or technique ( s ), the example audio signature engine 510 of fig5 processes the audio data 185 to determine binary fingerprints and / or signatures that substantially and / or uniquely identify corresponding portions of the audio data 185 . an example audio signature is computed by applying data compression to the audio data 185 . in the example of fig5 , audience measurement data 515 ( e . g ., audio codes and / or audio signatures ) located , decoded , extracted , identified and / or computed by the example audio code engine 505 and / or the example audio signature engine 510 and / or received from the content provider ( s ) 130 are stored using any type ( s ) and / or number of database ( s ) and / or data structure ( s ) ( e . g ., matrices , array ( s ), variable ( s ), register ( s ), data table ( s ), etc .) and are stored in , for example , any type ( s ) of memory (- ies ) and / or machine accessible file ( s ) 520 . the example audience measurement database 515 of fig5 is indexed by associated channel number , channel name , program name , program information ( e . g ., description ) and / or broadcast time information . the example audience measurement database 515 includes audio codes and / or signatures corresponding to content that is currently being broadcast , to content that was broadcast , and / or content that will be broadcast in the future . the amount of data in the database 515 may be selected based on the desired time period over which the example processing server 175 is programmed to compute and / or tabulate statistics regarding content exposure and / or consumption . for example , the example processing server 175 of fig5 may be configured to only consider content that is and / or was broadcast and / or was otherwise available during the previous fourteen ( 14 ) days . however , if mounting of stored media is desired ( e . g ., dvds ), then the database 515 should not be limited based on time . to identify content presented and / or consumed at and / or via a media device 105 , the example processing server 175 of fig5 includes a content matcher 525 . the example content matcher 525 of fig5 utilizes the hints 170 a and audience measurement data 170 b received from a content exposure meter 150 to determine which content was presented and / or consumed at and / or via the example media device 105 to form content exposure data 530 for the media device 105 . in particular , the example content matcher 525 utilizes the provided hints 170 a to identify a subset of the codes and / or signatures stored in the audience measurement database 515 of the processing server 175 to compare with the audience measurement data 170 b collected from the example media device 105 . a match between the audience measurement data 170 b and a particular audio code and / or signature 515 indicates that the content corresponding to the particular audio code / signature stored in the processing server 175 is the content that was presented and / or consumed at and / or via the media device 105 . using the hints 170 a , the content matcher 525 can substantially reduce the number of audience measurement data from the database 515 that must be compared with the audience measurement data 170 b collected by the content exposure meter 150 . as a result , the content measurement data 170 b can be processed for a substantially larger number of content exposure meters 150 . an example process that may be carried out to implement the example content matcher 525 of fig5 is discussed below in connection with fig7 . in the example of fig5 , content exposure data 530 is stored using any type ( s ) and / or number of data structure ( s ) ( e . g ., matrices , array ( s ), variable ( s ), register ( s ), data table ( s ), etc .) and is stored in , for example , any type ( s ) of memory (- ies ) and / or machine accessible file ( s ) 535 . the content exposure data 530 may include content exposure data for a plurality of other metered media devices 105 associated with a plurality of respondents to develop meaningful content exposure statistics . the combined content exposure data 530 may be statistically processed to determine , for example , the overall effectiveness , reach and / or audience demographics of presented and / or consumed content . while an example processing server 175 has been illustrated in fig5 , the elements , modules , logic , memory and / or devices illustrated in fig5 may be combined , re - arranged , eliminated and / or implemented in any way . for example , the example closed caption matcher 225 , the example indexing engine 205 , and / or the example keyword database 210 of fig2 could be implemented by and / or within the processing server 175 . in such examples , the content exposure meter 150 provides the closed caption information 222 and the audience measurement data 170 b to the processing server 175 . based on the received closed caption information 222 , the processing server 175 generates the hints information 170 a at the processing server 175 . in some examples , the processing server 175 receives closed caption information 222 from some content exposure meters 150 and receives hints information 170 a from other content exposure meters 150 . further , the example audio code engine 505 , the example audio signature engine 510 , the memory 520 , the example content matcher 525 , the example memory 535 and / or , more generally , the example processing server 175 may be implemented by hardware , software , firmware and / or any combination of hardware , software and / or firmware . for example , the example audio code engine 505 , the example audio signature engine 510 , the memory 520 , the example content matcher 525 , the example memory 535 may be implemented via machine accessible instructions executed by any type of processor 175 such as , for example , a processor from the intel ®, sun ®, or amd ® families of processors and / or microcontrollers . moreover , a content exposure meter may include additional elements , modules , logic , memory and / or devices and / or may include more than one of any of the illustrated elements , modules and / or devices such as , for example , a video code engine or a video signature engine . fig6 and 7 are flowcharts representative of example processes that may be executed to implement the example content exposure meter 150 and the example processing server 175 of fig1 , respectively and / or , more generally , to meter content exposure using closed caption information . the example processes of fig6 and / or 7 may be executed by a processor , a controller and / or any other suitable processing device . for example , part or all of the flow diagrams of fig6 and / or 7 may be embodied in coded instructions stored on a tangible medium such as a flash memory , or ram associated with a processor ( e . g ., the example central processing unit 805 discussed below in connection with fig8 ). alternatively , some or all of the example processes of fig6 and / or 7 may be implemented using an application specific integrated circuit ( asic ), a programmable logic device ( pld ), a field programmable logic device ( fpld ), discrete logic , hardware , firmware , etc . also , some or all of the example processes of fig6 and / or 7 may be implemented manually or as combinations of any of the foregoing techniques , for example , a combination of firmware and / or software and hardware . further , although the example processes of fig6 and 7 are described with reference to the flowcharts of fig6 and 7 , persons of ordinary skill in the art will readily appreciate that many other methods of implementing the example content exposure meter 150 and / or the example processing server 175 of fig1 , respectively , and / or , more generally , to meter content exposure using closed caption information and program guide data may be employed . for example , the order of execution of the blocks may be changed , and / or some of the blocks described may be changed , eliminated , sub - divided , or combined . additionally , persons of ordinary skill in the art will appreciate that the example processes of fig6 and / or 7 may be carried out sequentially and / or carried out in parallel by , for example , separate processing threads , processors , devices , circuits , etc . the example process of fig6 begins with a closed caption matcher ( e . g ., the example closed caption matcher 225 of fig2 ) obtaining and / or receiving the portion of closed caption text ( i . e ., word and / or words ) collected during the next time interval from a closed caption decoding engine 220 ( block 605 ). the closed caption matcher 225 then compares the closed caption text against indexed keywords in a keyword database ( e . g ., the keyword database 210 of fig2 ) ( block 610 ). if a match of at least one closed caption word with at least one indexed keyword is identified ( block 615 ), the content corresponding to the matching keyword is identified ( e . g ., the example content 320 of fig3 ) and the histogram information for the identified content is updated ( block 620 ). if a match is not identified ( block 615 ), the updating of the histogram is skipped . the closed caption matcher 225 then determines if the end of the time interval currently being processed ( e . g ., the example interval 315 of fig3 ) has arrived ( i . e ., if a boundary of the time interval 315 ( i . e ., an interval boundary ) has occurred ) ( block 630 ). if an interval boundary has not occurred ( block 630 ), control returns to block 605 to get the next closed caption text ( block 605 ). if an interval boundary has occurred ( block 630 ), the closed caption matcher 225 obtains and / or receives any audio codes and / or signatures collected from the content presented and / or consumed during the just ended time interval ( block 635 ) and obtains and / or receives the audio signatures computed for the content presented and / or consumed during the just ended time interval ( block 640 ). the closed caption matcher 225 then creates and / or adds a hints and audience measurement data entry ( e . g ., an entry 405 of fig4 ) into the table and / or sends the hints and audience measurement data to a processing server 175 . the example process of fig7 begins with a content matcher ( e . g ., the example content matcher 525 of fig5 ) reading the hints 170 a and audience measurement data 170 b for a time interval 315 ( e . g ., the example entry 405 of fig4 ) ( block 705 ). the content matcher 525 identifies the most probable content , content stream and / or broadcast time ( block 710 ) and determines if audio codes for the most probable content , content stream and / or broadcast time are available ( block 715 ). additionally or alternatively , the content matcher 525 may at block 710 utilize a content timestamp ( e . g ., the example timestamp 412 of fig4 ) when selecting the most probable content , content stream and / or broadcast time . for example , the content matcher 525 may first select a content candidate that is associated with the presentation of live content ( e . g ., being presented while the content is being broadcast ). if applicable audio codes are included in the audience measurement data 170 b ( block 715 ), the content matcher 525 compares the audio codes and / or signatures with the audio codes and / or signatures 515 corresponding to the content candidate ( block 720 ). if there is a match ( block 725 ), the content matcher 525 credits , tallies and / or tabulates a presentation of the content candidate ( i . e ., identifies the content candidate as the content that was presented and / or consumed ) together with the timestamp ( e . g ., the example timestamp 412 of fig4 ) in the content exposure data 530 ( block 730 ). the timestamp indicates the time of content exposure . if at block 715 applicable audio codes and / or signatures are not available , or if at block 725 the audio codes and / or signatures do not match , the content matcher 525 determines if audio signatures for the most probable content candidate are available ( block 735 ). if audio signatures are not available ( block 735 ), the content matcher 525 assumes the most probable candidate content , source and / or broadcast time was presented and / or consumed and records the exposure of the candidate content together with the timestamp ( e . g ., the example timestamp 412 of fig4 ) in the content exposure data 530 ( block 730 ). the timestamp indicates the time of content exposure . if the audio signatures are available ( block 735 ), the content matcher 525 compares the audio signatures with the audio signatures 515 corresponding to the content candidate ( block 740 ). if the audio signatures match ( block 745 ), the content matcher 525 records the match ( i . e ., identifies the content candidate as the content that was presented and / or consumed ) together with the timestamp ( e . g ., the example timestamp 412 of fig4 ) in the content exposure data 530 ( block 730 ). the timestamp indicates the time of content expousre . if the audio signatures do not match ( block 745 ), the content matcher 525 determines if there are more hints ( block 750 ). if there are no more hints ( block 750 ), control proceeds to block 755 to determine if there are additional time intervals of hints to be processed . additionally or alternatively , the content matcher 525 compares the audience measurement data collected from the media device 105 with all of the audience measurement data 515 stored in the database to determine if a match is identified . if there are more hints ( block 750 ), the content matcher 525 identifies the next most probable content candidate ( block 760 ). control then returns to block 715 . at block 755 , if more hints 170 a and audience measurement data 170 b for more intervals is available ( block 755 ), control returns to block 705 to process the next time interval . if not more hints 170 a and audience measurement data 170 b is available ( block 755 ), control exits from the example machine accessible instructions of fig7 . fig8 is a schematic diagram of an example processor platform 800 that may be used and / or programmed to , for example , carry out the example processes of fig6 and / or 7 to implement the example content exposure meter 150 and the example processing server 175 of fig1 , respectively and / or , more generally , to meter content exposure using closed caption information and program guide data . for example , the processor platform 800 can be implemented by one or more general purpose microprocessors , microcontrollers , etc . the processor platform 800 of the example of fig8 includes a general purpose programmable and / or specialized processor 805 . the processor 805 executes coded instructions 810 and / or 812 present in main memory of the processor 805 ( e . g ., within a random access memory ( ram ) 815 and / or a read - only memory ( rom ) 820 ). the processor 805 may be any type of processing unit , such as a processor and / or microcontroller from any of the intel ®, sun ®, and / or amd ® families of processors and / or microcontrollers . the processor 805 may carry out , among other things , the example processes illustrated in fig6 and / or 7 . the processor 805 is in communication with the main memory ( including the ram 815 and a rom 820 ) via a bus 825 . the ram 815 may be implemented by dram , sdram , and / or any other type of ram device . the rom 820 may be implemented by flash memory and / or any other desired type of memory device . access to the memories 815 and 820 is typically controlled by a memory controller ( not shown ) in a conventional manner . the ram 815 may be used , for example , to store the example keywords database 210 of fig2 , and / or the example audience measurement database 515 and / or the example content exposure data 530 of fig5 . the processor platform 800 also includes a conventional interface circuit 835 . the interface circuit 835 may be implemented by any type of well - known interface standard , such as an external memory interface , serial port , general purpose input / output , etc . one or more input devices 835 and one or more output devices 840 are connected to the interface circuit 835 . the input devices 835 may be used , for example , to receive audio data 155 , video data 160 , content guide data 165 , audio data 185 , etc . the output devices 840 may be used , for example , to send the audience measurement data 170 b and / or the hints 170 a from the content exposure meter 150 to the processing server 175 . although certain example methods , apparatus and articles of manufacture have been described herein , the scope of coverage of this patent is not limited thereto . on the contrary , this patent covers all methods , apparatus and articles of manufacture fairly falling within the scope of the appended claims either literally or under the doctrine of equivalents . | 7 |
referring to the drawing and more particularly to fig1 there is shown an hid lamp embodying the invention in the form of a high pressure mercury vapor lamp 1 . it comprises a glass outer envelope or jacket 2 of ellipsoidal shape having a neck 3 to the end of which is attached a screw base 4 . the neck 3 is closed by a re - entrant stem 5 having a press portion through which extend relatively stiff inlead wires 6 , 7 . the inlead wires are connected exteriorly to the contact surfaces of the base , namely the insulated center contact or eyelet 8 and the base shell 9 . inner arc tube 10 is made of fused silica , commonly referred to as quartz , and encloses a charge of mercury and an inert starting gas , suitably argon at a pressure of about 20 torr . in a metal halide lamp , the filling would include additionally small quantities of one or more metallic halides , for instance sodium and scandium iodides . the arc tube is provided at opposite ends with a pair of main discharge supporting electrodes 11 , 12 to which connections are made by inleads which include thin foil portions 13 sealed through the flattened or pressed ends 14 of the tube . a fine tungsten wire 15 sealed into the arc tube at its lower end serves as an auxiliary starting electrode and is connected through a current limiting resistor 16 to inlead 7 by way of side rod 17 . the side rod is welded to inlead 7 at the base end and extends to anchoring dimple 18 at the dome end of the envelope which it engages by a looped clip 19 . the arc tube is attached to the mount frame by clamping its flat ends 14 between strap clips 20 which are welded to side rod 17 , the lower clip being additionally welded to reverted portion 21 of the side rod . the arc discharge through mercury vapor at a pressure exceeding 1 atmosphere generates both visible and ultraviolet radiation which pass readily through the fused silica wall of the arc tube 10 . however the glass wall of the outer envelope 2 is opaque to the ultraviolet radiation which is harmlessly absorbed . in deluxe mercury lamps , the outer envelope is coated internally with a phosphor layer ( not shown ) which converts some of the shorter wavelength radiation produced by the discharge into visible light including red whereby the color rendition from the lamp is greatly improved . there is no oxygen in the space within outer envelope 2 ; it may be either evacuated or filled with an inactive gas such as argon . it is possible for the jacket to be punctured , for instance by a projectile from an air rifle , and the arc tube to remain intact . or again when a lamp as illustrated is operated base up , the jacket could shatter and fall off upon being struck by a ball or other projectile and the arc tube and connections thereto remain intact . the lamp may continue to operate in this fashion for a considerable time during which ultraviolet radiation from the arc tube may escape and create a safety hazard . in accordance with my invention , the foregoing hazardous possibilities are eliminated by providing an oxidizable link incorporating a thin oxidizable metallic film in one of the connections within the outer envelope which go from the inleads 6 or 7 to the main electrodes 11 or 12 . the alkaline earth metals beryllium , magnesium , calcium , strontium and barium form such films . radium of the same group ii a should be avoided because it is radioactive . also beryllium is generally considered hazardous because of its easy absorption by the human body . the preferred film material is barium on account of its low cost and ready availability . as best seen in fig2 the oxidizable link comprises a ceramic wafer 22 having metal leads 23 , 24 embedded in it from opposite edges . lead 23 is spot - welded to electrode inlead 12 &# 39 ; and lead 24 to inlead 6 . spaced and parallel extending metal contact strips 25 , 26 are fixed to the surface of the wafer and connected to leads 23 , 24 , respectively . a barium getter ring 27 consisting of a channeled or slightly dished metal ring containing vaporizable barium powder is supported by means of a wire 28 attached to lead 23 . it is arranged so that the channeled side in which the powder is laid faces the contact strips 25 , 26 . as part of the lamp manufacturing process , the arc tube and mount frame assembly comprising arc tube 10 supported on glass stem 5 is inserted into the outer envelope 2 and the stem sealed to the neck of the envelope . at this stage , the outer envelope is exhausted of air and the barium getter ring 27 is flashed in vacuum . flashing may be accomplished by inductively coupling high frequency current into the ring to bring it up to a temperature sufficient to vaporize the barium . the barium deposits as a very thin silvery film 29 indicated in fig2 which conductively bridges the contact strips 25 , 26 . the outer jacket may then be tipped off under vacuum or , in the case of some hid lamps , after having first been back - filled with an inert gas such as argon . other inert gases , for instance krypton , could be used but since argon is by far the cheapest , no other is used . nitrogen must not be used because it reacts with barium to form non - conductive barium nitride . in operation of the lamp , so long as the outer jacket remains intact the fuse link remains passive and the barium film serves as a low resistance conductive bridge between the contact strips 25 , 26 . the desirability of a low resistance provides a measure of the minimum thickness which the film should have . in the event of puncture or fracture of the outer jacket , air upon entering will start to react with the barium film causing it to oxidize and its resistance to increase . the film heats up more and the oxidation process intensifies until the film becomes fully oxidized and non - conducting , whereupon the arc tube is permanently extinguished . in order to form the conductive barium film 29 , the getter ring 27 must be flashed in a vacuum . with some exhaust machines used in lamp manufacture , when the finished lamp must have a filling of argon in the outer envelope , it may not be practical to first exhaust the jacket in order to flash the barium and thereafter back - fill with argon . in such case , the alternative of an oxidizable link enclosed in a separate smaller envelope may be used , which in turn is enclosed within the outer envelope of the lamp . as illustrated in fig3 the ceramic wafer 22 supporting the contact strips 25 , 26 is sealed in a small glass envelope or bottle 31 along with the getterring 27 . the leads 23 , 24 project through the wall of the bottle . the bottle is evacuated , flashed and tested , and then welded into the mount frame in lieu of the wafer of fig2 . the lamp is then placed on the exhaust machine and finished in the conventional manner , that is going directly to an argon fill . after the lamp has been thus completed , the internal glass bottle 31 is opened by any suitable means . for instance , a laser beam may be focused on the glass wall of the bottle to puncture a hole through it . alternatively , radio frequency radiation may be applied to heat and melt a low temperature metal seal such as an indium plug 32 sealing the neck of the bottle 31 . the gas pressure in the outer envelope will assist in opening the inner bottle by driving the indium ball in . the barium film fuse is then ready to operate and extinguish the arc tube should the outer envelope be punctured and air admitted into the jacket . while the invention has been illustrated and described in detail by reference to a large mercury vapor lamp ( 400 watts ) generally used outdoors , it is equally applicable to metal halide lamps . also the fuse link of the invention is readily varied in current rating and adapted to various sizes of lamps including the miniature metal halide lamps disclosed in u . s . pat . no . 4 , 161 , 672 -- cap et al . | 7 |
in the present invention , a ceramic diaphragm structure is produced by using a green substrate and a green sheet , both having shrinkage rates and mid - sintering temperatures satisfying the following formulae 1 ), 2 ), and 3 ): ( symbols in the formulae mean as described above .) further , in the substrate a difference in average sintering temperature shown by the formula 4 ) should be larger than 0 , or a difference in average shrinkage rate shown by the formula 5 ) should be larger than 0 . ## equ5 ## in the formula 4 ), n denotes a number of layers constituting a green substrate . t 70 ( substrate ), denotes mid - sintering temperature (° c .) of a layer positioned in number n place from the bottom of the laminate in the ceramic green substrate having the ceramic green sheet thereon as shown in fig3 . t n and t n + 1 denote distances from a lower and an upper surfaces , respectively , of the layer positioned in numbers n place to a neutral line 5 of the substrate , with putting - for a surface under the neutral line and + for a surface over the neutral line . the neutral line 5 is a line formed by connecting middle points to one another between the lower surface of the lowest layer 4 and the upper surface of the layer 6 positioned in number n place after firing the unitary laminate . in the formula 5 ), s ( substrate ) n denote a shrinkage rate (%) of a layer positioned in number n place from the lowest layer of the substrate having a green sheet thereon . incidentally , s ( substrate ) in the formula 1 ) can be calculated by the following formula 8 ): ## equ6 ## ( n and s ( substrate ), mean as described above . c n denotes a thickness of the layer positioned in number n from the bottom of the unitary laminate after firing the unitary laminate . c denotes a thickness of a substrate after firing the unitary laminate .) t 70 ( substrate ) can be calculated by the following formula 9 ): ## equ7 ## ( n , t 70 ( substrate ) n , c n , and c mean as described above .) when a green sheet is constituted of a plurality of layers , s ( sheet ) and t 70 ( sheet ) can be calculated in the same manner . therefore , according to the method of the present invention , influence of a mid - sintering temperature and a shrinkage rate of a green substrate to a green sheet with a change by a distance from the green sheet is adjusted . that is , a green substrate is constituted of a plurality of layers each having an independent mid - sintering temperature and an independent shrinkage rate , and the values are adjusted . accordingly , a diaphragm portion can have a protrudent shape toward the side opposite to the window portion formed in a substrate , and a waviness of a diaphragm structure and / or a warpage of a ceramic plate including diaphragm structures can be advantageously minimized . specifically , in a substrate 7 after firing the unitary laminate shown in fig4 differences in average sintering temperature and in average shrinkage rate are calculated by formulae 4 ) and 5 ) as follows : ## equ8 ## incidentally , t 1 - t 6 and s 1 - s 6 denote a mid - sintering temperature and a shrinkage rate , respectively , of the layer positioned in number n place . the fifth layer has a thickness of 200 μm after firing . the other layer has a thickness of 100 μm after firing . when layers constituting a green substrate are connected to one another , a connecting layer is formed in each of the gaps between the layers . in such a case , the connecting layer is treated as a substrate in the aforementioned calculation . in the present invention , a mid - sintering temperature (° c .) of a green substrate in a portion below a neutral line of the substrate after firing the unitary laminate is preferably higher than that of a green sheet in view of enhancing a forming stability of a protrudent shape . the mid - sintering temperature (° c .) of a green substrate below the neutral line after firing is expressed by the following formula 6 ): ## equ9 ## ( m denotes the number of layers positioned below a neutral line among the layers constituting a substrate after firing a unitary laminate . a n denotes a thickness of the layer positioned in number n place from the lowest layer among the layers constituting a substrate after firing the unitary laminate . however , regarding the layer positioned in number m from the lowest layer , a n denotes a thickness from the lower surface of the layer to the neutral line . t 70 ( substrate ) n means as described above . a denotes a distance from the lower surface of the lowest layer of a substrate to the neutral line after firing the unitary laminate .) a mid - sintering temperature (° c .) of a green sheet is expressed by the following formula 7 ): ## equ10 ## ( l denotes the number of layers constituting a green sheet . t 70 ( sheet ) n denotes a mid - sintering temperature (° c .) of a layer positioned in number n place from the lowest layer among the layers constituting a green sheet when the unitary laminate is positioned so that the green sheet is disposed upside of the substrate . b n denote a thickness of the layer positioned in number n place from the lowest layer among the layers constituting a diaphragm plate . b denote a thickness of a diaphragm plate . in the present invention , a ceramic diaphragm structure is produced by using a green substrate and a green sheet satisfying the above condition . specifically , it is produced as follows : in the beginning , a green substrate and a green sheet are molded . as a material of a green substrate and a green sheet , there may be used mullite , beryllia , spinel , titania , aluminum nitride , silicon nitride , stabilized zirconia , a partially stabilized zirconia , alumina , or a mixture thereof . alternatively , there may be used a raw material which becomes one of the aforementioned material after firing . particularly , a material for a green sheet is preferably a partially stabilized zirconia , stabilized zirconia , alumina , a mixture thereof , or a raw material which becomes one of these materials after firing . more preferably , as the present inventor disclosed in japanese patent laid open 5 - 270912 , there is used a material having as a main component a partially stabilized zirconia consisting mainly of tetragonal crystals or a mixed crystals consisting of at least two kinds selected from tetragonal crystals , cubic crystals , monoclinic crystals . a material for the green substrate is preferably the same as that of the green sheet in view of ensuring reliability and unitary forming of the green substrate and the green sheet . alternatively , there may be used a ceramic material such as a glass - ceramic or cordierite . incidentally , the green sheet is desirably formed with using a partially stabilized zirconia , stabilized zirconia , alumina , a material containing a mixture thereof as a main component , or a raw material which becomes one of these materials after firing , the material having a form of powder having an average particle diameter of 0 . 05 - 1 . 0 μm in view of mechanical strength of a diaphragm portion . a diaphragm plate of a ceramic diaphragm structure is preferably 30 μm or less , more preferably 3 - 20 μm . the diaphragm plate has a relative density ( bulk density / theoretical density ) of preferably 90 % or more , more preferably 95 % or more , furthermore preferably 98 % or more in view of strength , young &# 39 ; s modulus , or the like . a thickness of a substrate is not particularly limited , and it is suitably determined depending on its use of a diaphragm structure . however , a total thickness of a substrate is preferably 50 μm or more in order to increase an effect of the present invention . a green substrate and a green sheet can be obtained by preparing a slurry or a paste obtained by adding a binder , a plasticizer , a dispersant , a sintering aid , an organic solvent , etc ., to the aforementioned material ; molding constituent members by a conventionally known method such as a doctor blading , a calendering method , a printing method , and a reverse roll coater method ; subjecting the constituent members to cutting , trimming , punching , or the like as necessary ; and piling up the constituent members so as to give a predetermined shape and a predetermined thickness . then , a green sheet is superposed on a green substrate so as to prepare a unitary laminate . the green sheet is superposed on the green substrate so as to cover a window portion formed in the green sheet . the unitary laminate can be obtained by heat - pressing or the like . finally , the unitary laminate is subjected to firing so as to obtain a ceramic diaphragm structure which diaphragm portion has a protrudent shape toward the side opposite to the window portion formed in a substrate . incidentally , a firing temperature is preferably 1200 - 1700 ° c ., more preferably 1300 - 1600 ° c . the present invention is described in more detail on the basis of examples . however , the present invention is by no means limited to the examples . by a method of the present invention , there is produced a ceramic diaphragm structure having a substrate having two layers so as to satisfy the aforementioned formulae 1 ), 2 ), 3 ), and 4 ). to 100 parts by weight of a partially stabilized zirconia powder ( containing 0 . 1 - 0 . 5 % of alumina ) having an average particle diameter of 0 . 4 - 1 . 0 μm were added 7 . 6 parts by weight of poly ( vinyl butyral ) as a binder , 3 . 8 parts by weight of dioctyl phthalate as a plasticizer , 80 parts by weight of mixture of toluene and 2 - propanol in the ratio of 1 : 1 ( by volume ) as a solvent , and 0 - 2 . 0 parts by weight of sorbitan fatty acid ester as a dispersant as necessary . they were mixed together by a ball mill for 5 - 50 hours so as to obtain a slurry . the slurry was deaired and a viscosity was adjusted so that the slurry for the green sheet has a viscosity of 2000 cps and that the slurry for the green substrate has a viscosity of 20000 cps . the aforementioned slurry was molded so as to have a predetermined shape by a doctor blading to obtain each layer constituting a green substrate and by a reverse roll coater method to obtain a green sheet . incidentally , a shrinkage rate becomes smaller when a time for mixing a material by a ball mill is longer , or when an amount of a dispersant is larger . a mid - sintering temperature becomes lower when a time for mixing in a ball mill is longer or when an amount of alumina is larger . by controlling these factors , a shrinkage rate of a green substrate is adjusted to be 20 . 76 %, and a shrinkage rate of a green sheet is adjusted to be 21 . 50 %. a mid - sintering temperature of the first layer ( when a ceramic diaphragm structure is disposed so that a diaphragm plate is placed in the upper side , a layer positioned in number n from the bottom is referred to as nth layer . hereinbelow , the same manner .) of a green substrate was adjusted to be 1310 ° c ., a mid - sintering temperature of the second layer was adjusted to be 1330 ° c ., and a mid - sintering temperature of a green sheet was adjusted to be 1272 ° c . by laminating the aforementioned layers , a green substrate consisting of two layers was produced . further , a green sheet is superposed on the green substrate , and they are heated and pressed at 100 ° c . with a pressure of 200 kg / cm 2 so as to obtain a unitary laminate . the unitary laminate is fired at 1500 ° c . for 3 hours so as to produce a ceramic plate including four diaphragm structures 3 each having three window portions 8 shown in fig5 . a window portion , i . e ., a diaphragm portion 1 had a rectangular shape having dimensions of 0 . 5 × 0 . 7 mm after firing . a distance between two adjacent windows along the side having 0 . 5 mm was 0 . 3 mm . additionally , the first layer 9 of the substrate 2 was provided with a throughhole 10 having a diameter of 0 . 2 mm after firing and connecting with a window portion 8 . in the substrate 2 , the first layer 9 and the second layer 11 each had a thickness of 100 μm after firing . a diaphragm plate 12 had a thickness of 10 μm after firing . the aforementioned diaphragm structures were measured for a presence of protrudent shape in a diaphragm . each of the diaphragm structures were measured for amount of a waviness , and a ceramic plate including the diaphragm structures were measured for amounts of a warpage . the results are shown in table 1 . additionally , table 1 expresses differences in average sintering temperatures and in average shrinkage rate of a green substrate , and a mid sintering temperature ( t 7 ( substrate )), a shrinkage rate ( s ( substrate ) of a whole green substrate , and a mid - sintering temperature in the portion of a green substrate under the neutral line which were calculated on the basis of formulae 4 ), 5 ), 8 ), 9 ) and 6 ). incidentally , when these are calculated , samples of 10 × 10 mm taken from a sheet constituting these layers were measured for a mid - sintering temperature ( t 70 ( substrate ) n ) and a shrinkage rate ( s ( substrate ) n ) of each layer of the green substrate . the results are also shown in table 1 . in each of examples 2 - 8 , a ceramic plate having four ceramic diaphragm structures which satisfies the aforementioned formulae 1 ), 2 ), 3 ), and at least one of the formulae 4 ) and 5 ) and which consists of two layers was produced in the same manner as in example 1 except that a mid - sintering temperature and a shrinkage rate of each of the layers constituting a green substrate were changed . in each of examples 4 and 8 , a mid - sintering temperature and a shrinkage rate of a green sheet were 1262 ° c . and 21 . 38 %, respectively . the aforementioned diaphragm structures were measured for a protrudent shape of a diaphragm portion , a waviness of the diaphragm structures and / or a warpage of a ceramic plate including the diaphragm structures . the results are shown in table 1 . in table 1 are also shown values such as a difference in average sintering temperature of a green substrate , the values being calculated on the basis of a mid - sintering temperature and a shrinkage rate of each of layers constituting the green substrate and the aforementioned formulae . table 1__________________________________________________________________________ mid - sinter - difference difference ing in in temperature presenceex - thick - t . sub . 70 t . sub . 70 average average below warpage of pro - am - ness ( substrate ). sub . n ( substrate ) s ( substrate ). sub . n s ( substrate ) sintering shrinkage neutral and / or trudentple n layer ( μm ) (° c .) (° c .) (%) (%) temperature rate line (° c .) waviness shape__________________________________________________________________________1 first layer 100 1310 1320 20 . 76 20 . 76 & gt ; 0 0 1310 small present second layer 100 1330 20 . 762 first layer 100 1272 1291 20 . 00 20 . 36 & gt ; 0 & gt ; 0 1272 small present second layer 100 1310 20 . 723 first layer 100 1340 1355 20 . 47 20 . 47 & gt ; 0 0 1340 small present second layer 100 1370 20 . 474 first layer 100 1330 1365 20 . 45 20 . 45 & gt ; 0 0 1330 small present second layer 100 1400 20 . 455 first layer 100 1322 1322 20 . 70 20 . 84 0 & gt ; 0 1322 small present second layer 100 1322 20 . 976 first layer 100 1322 1322 20 . 00 20 . 54 0 & gt ; 0 1322 small present second layer 100 1322 21 . 077 first layer 100 1310 1310 22 . 48 22 . 78 0 & gt ; 0 1310 small present second layer 100 1310 23 . 078 first layer 100 1360 1360 18 . 00 20 . 19 0 & gt ; 0 1360 small present second layer 100 1360 22 . 38__________________________________________________________________________ a ceramic plate having diaphragm structures which satisfies the aforementioned formulae 1 ), 2 ), and 3 ) or the formulae 2 ) and 3 ) and which satisfies none of the formulae 4 ) and 5 ) or the formulae 1 ), 4 ) and 5 ) was produced in the same manner as in example 1 except that a mid - sintering temperature and a shrinkage rate of each of the layers constituting a green substrate are different from those of example 1 . incidentally , a mid - sintering temperature and a shrinkage rate of a green sheet are 1272 ° c . and 21 . 50 %, respectively , which are the same as those of example 1 . the aforementioned diaphragm structures were measured for a protrudent shape of a diaphragm portion , a waviness of the diaphragm structures and / or a warpage of a ceramic plate including the diaphragm structures . the results are shown in table 2 . in table 2 are also shown values such as a difference in average sintering temperature of a green substrate , the values being calculated on the basis of a mid - sintering temperature and a shrinkage rate of each of layers constituting the green substrate and the aforementioned formulae . table 2__________________________________________________________________________com - mid - sinter - para - difference difference ingtive in in temperature presenceex - thick - t . sub . 70 t . sub . 70 average average below warpage of pro - am - ness ( substrate ). sub . n ( substrate ) s ( substrate ). sub . n s ( substrate ) sintering shrinkage neutral and / or trudentple n layer ( μm ) (° c .) (° c .) (%) (%) temperature rate line (° c .) waviness shape__________________________________________________________________________1 first layer 100 1272 1272 20 . 00 20 . 00 0 0 1272 small absent second layer 100 1272 20 . 002 first layer 100 1310 1310 20 . 72 20 . 72 0 0 1310 medium present second layer 100 1310 20 . 723 first layer 100 1330 1330 20 . 79 20 . 79 0 0 t330 large present second layer 100 1330 20 . 794 first layer 100 1330 1320 20 . 76 20 . 76 & lt ; 0 0 1330 large present second layer 100 1310 20 . 765 first layer 100 1322 1322 20 . 97 20 . 97 0 0 1322 large present second layer 100 1322 20 . 976 first layer 100 1322 1322 20 . 97 20 . 84 0 & lt ; 0 1322 verv present second layer 100 1322 21 . 70__________________________________________________________________________ a ceramic plate having diaphragm structures which substrate consists of five layers was produced so as to satisfy the formulae 1 ), 2 ), 3 ), 4 ), and 5 ). with 100 weight parts of an alumina powder having an average diameter ranging from 0 . 2 to 0 . 8 μm were mixed 11 weight parts of poly ( vinyl butyral ) resin as a binder , 5 . 5 weight parts of dioctyl phthalate as a plasticizer , 11 weight parts of a mixture of toluene and 2 - propanol in the ratio of 1 : 1 by volume as a solvent , and 0 - 3 . 0 weight parts of sorbitan fatty acid ester as a dispersant as necessary by a ball mill for 5 - 50 hours so as to prepare a slurry . the slurry was deaired , and viscosity of the slurry was adjusted to be 2000 cps for a green sheet and 20000 cps for a green substrate . each of the layers constituting a green substrate and a green sheet was formed in the same manner as in example 1 . by controlling the same factor as example 1 , a shrinkage rate and a mid - sintering temperature of the green sheet were adjusted to be 21 . 40 % and 1270 ° c ., respectively . on the other hand , shrinkage rates of the green substrate were adjusted to be 20 . 50 %, 20 . 63 %, 20 . 59 %, 20 . 38 %, and 20 . 79 % from the first layer , and mid - sintering temperatures of the green substrate were adjusted to be 1310 ° c ., 1340 ° c ., 1330 ° c ., 1360 ° c ., and 1330 c . the aforementioned layers were piled up so as to obtain the green substrate consisting of five layers . then , the green sheet was superposed on the green substrate so as to obtain a unitary laminate , which was subjected to a heat pressing treatment at 100 ° c . under 200 kg / cm 2 for one minute . the unitary laminate was fired at 1550 ° c . for 3 hours so as to obtain a ceramic plate 15 having four diaphragm structures 3 having three windows 8 as shown in fig6 . a shape of each of the window portion 8 , i . e ., diaphragm portion 1 has a rectangular shape having dimensions of 0 . 8 × 1 . 2 mm after firing . distance between two adjacent windows 8 was 0 . 5 mm along a side of 0 . 8 mm after firing . the fourth and the second layers of the substrate 2 had the similar shape as the fifth layer . the first and the third layers were provided with throughholes 10 each having a diameter of 0 . 2 mm after firing and being connected with each of the window portions 8 . the first , second , third , fourth , and fifth layers of the substrate 2 had a thickness of 200 μm , 250 μm , 100 μm , 50 μm , and 100 μm , respectively . a thickness of a diaphragm plate 12 had a thickness of 20 μm . the aforementioned diaphragm structures were measured for a protrudent shape of a diaphragm portion , a waviness of the diaphragm structures and / or a warpage of a ceramic plate including the diaphragm structures . the results are shown in table 3 . in table 3 are also shown values such as differences in average sintering temperature and average shrinkage rate of a green substrate and a mid - sintering temperature and a shrinkage rate of the whole green substrate and a mid - sintering temperature of a portion below a neutral line of a green substrate , the values being calculated on the basis of the aforementioned formulae . a ceramic plate having diaphragm structures which substrate consists of five layers was produced so as to satisfy the formulae 1 ), 2 ), 3 ), and 4 ) in the same manner as in example 9 except that each of the layers constituting a green substrate had a different mid - sintering temperature and a different shrinkage rate from those of example 9 . incidentally , the green sheet had a mid - sintering temperature of 1260 ° c . and a shrinkage rate of 21 . 30 %. the aforementioned diaphragm structures were measured for a protrudent shape of a diaphragm portion , a waviness of the diaphragm structures and / or a warpage of a ceramic substrate including the diaphragm structures . the results are shown in table 3 . in table 3 are also shown values such as a difference in average sintering temperature of a green substrate , the values being calculated on the basis of a mid - sintering temperature and a shrinkage rate of each of layers constituting the green substrate and the aforementioned formulae . a ceramic plate having diaphragm structures which satisfies the formulae 1 ), 2 ), and 3 ), and which does not satisfy 4 ) was produced in the same manner as in example 9 except that a mid - sintering temperature and a shrinkage rate of each of layers constituting a green substrate were different from those of example 9 . incidentally , a mid - sintering temperature and a shrinkage rate of a green sheet used for a diaphragm plate were 1270 ° c . and 21 . 40 %, respectively , as in example 9 . the aforementioned diaphragm structures were measured for a protrudent shape of a diaphragm portion , a waviness of the diaphragm structures and / or a warpage of a ceramic plate including the diaphragm structures . the results are shown in table 3 . in table 3 are also shown values such as a difference in average sintering temperature of a green substrate , the values being calculated on the basis of a mid - sintering temperature and a shrinkage rate of each of layers constituting the green substrate and the aforementioned formulae . table 3__________________________________________________________________________ mid - sinter - difference difference ing in in temperature presence thick - t . sub . 70 t . sub . 70 average average below warpage of pro - ness ( substrate ). sub . n ( substrate ) s ( substrate ). sub . n s ( substrate ) sintering shrinkage neutral and / or trudentn layer ( μm ) (° c .) (° c .) (%) (%) temperature rate line (° c .) waviness shape__________________________________________________________________________example 9first layer 200 1310 1330 20 . 50 20 . 59 & gt ; 0 & gt ; 0 1323 small presentsecond layer 250 1340 20 . 63third layer 100 1330 20 . 59fourth layer 50 1360 20 . 38fifth layer 100 1330 20 . 79example 10first layer 200 1330 1336 20 . 72 20 . 78 & gt ; 0 & lt ; 0 1326 small presentsecond layer 250 1320 20 . 91third layer 100 1345 20 . 78fourth layer 50 1370 20 . 38fifth layer 100 1360 20 . 79comparativeexample 7first layer 200 1360 1325 20 . 72 20 . 53 & lt ; 0 & lt ; 0 1339 large presentsecond layer 250 1310 20 . 30third layer 100 1300 20 . 53fourth layer 50 1315 20 . 38fifth layer 100 1320 20 . 79__________________________________________________________________________ in each example , all the diaphragm portions had a protrudent shape , and there was only a small degree of waviness caused in the diaphragm structures and / or a warpage of a ceramic plate including the diaphragm structures . on the other hand , in each comparative example , some of the diaphragm portions did not have a protrudent shape . concerning the diaphragm portions which had a protrudent shape in comparative examples , the diaphragm structures or a ceramic plate including the diaphragm structures had a large degree of warpage or waviness . in a method of the present invention , mid - sintering temperatures and shrinkage rates of a green substrate and a green sheet are controlled so as to satisfy predetermined formulae . accordingly , it makes possible an adjustment in consideration of a change of influence of a mid - sintering temperature and a shrinkage rate of a green substrate on a green sheet , the adjustment including a change of influence depending on a distance from the green sheet . as a result , a diaphragm portion has a protrudent shape toward the side opposite to the window portion of the substrate , and a waviness of a diaphragm structure and / or a warpage of a ceramic plate including diaphragm structures after firing can be advantageously minimized . accordingly , when a diaphragm structure is used as a sensor , a variance of detection preciseness can be prevented . when a diaphragm structure is used as a piezoelectric / electrostrictive actuator , a deterioration or variance of displacement can be avoided . | 2 |
reference is made to fig1 , which illustrates a lubricating - fluid infusion apparatus 1 for implementing a lubricating - fluid infusion method involving the present invention . the lubricating - fluid infusion apparatus 1 is made up of a vacuum chamber 2 , an dispenser 3 , a lubricating fluid tank 4 , and , for pumping down the interior of these components , a vacuum pumping device and a gas - introduction mechanism r , as well as their connecting supply lines . in this implementation , a general rotary pump p is employed as the vacuum pumping device . the gas - introduction mechanism r , comprising a flow control valve w , and a filter f for preventing dust from invading the mechanism , introduces ambient air into the supply lines . to further ensure that invasion of dust is prevented , the flow control valve w adjusted to make it so that the air inflow speed does not grow excessively large . reference marks g 1 and g 2 indicate penning gauges , which enable the internal pressure of the vacuum chamber 2 and fluid tank 4 to be monitored . the dispenser 3 is made up of a valve mechanism 30 ( shown in fig3 ) and a cylindrical capillary tube 32 mounted in the tip of the valve mechanism . the dispenser 3 is connected to the bottom portion of the fluid tank 4 through a feed duct 42 . a dynamic - pressure bearing device 5 is set inside the vacuum chamber 2 , and is infused with lubricating fluid supplied through the tip of the capillary tube 32 . the vacuum chamber 2 is of glass manufacture in a lidded cylindrical form that is open - ended along the underside ; thus the status within the chamber may be observed from without . as depicted in fig1 , the open - ended portion of the chamber along its underside is closed off by a pedestal 21 . this occlusion is maintained airtight by means of a not - illustrated o - ring made of rubber . the vacuum chamber 2 is connected to the rotary pump p and the gas - introduction mechanism r via ventilation valves v and w . fig2 illustrates the fluid tank 4 and the dispenser 3 . as depicted in fig2 a , an empty space 45 is left in the upper portion of the reservoir 4 , and by pumping down this space , the concentration of gas dissolved in the lubricating fluid can be lowered . relevant to that operation is a conduit 42 b connected to this region of the reservoir 4 , through which the pressure of the empty space 45 is reduced / elevated . during pump - down , a stirring mechanism is operated to promote the reducing of the concentration of gas dissolved into the lubricating fluid . the stirring mechanism is made up of a rod 44 furnished with a magnet , and a stirrer 43 likewise furnished with a magnet , wherein rotating the rod 44 rotates the stirrer 43 in the interior of the fluid tank 4 . the fluid tank 4 interior is joined to the dispenser 3 via the feed duct 42 , and in turn is joined to the exterior through the capillary tube 32 mounted in the tip of the dispenser 3 . in order to dispense lubricating fluid into the dynamic - pressure bearing device , a sufficiently large , stabilized ejection pressure must be attendant on the lubricating fluid sent into the dispenser 3 . otherwise , the fluid - dispensing volume will vary with each dispensing operation , which is prohibitive of assuring uniform product quality , especially in cases in which bearing devices are mass - produced . for that purpose , in the fig2 a instance , ejection pressure is imparted to the lubricating fluid by introducing air at atmospheric pressure into the empty space 45 . meanwhile , represented in fig2 b is a different method , in which ejection pressure is imparted to lubricating fluid stored within a cylinder 46 by placing a plummet 48 onto a plunger 47 fitted into the cylinder 46 . an advantage to the fig2 b method is that pressure may be imparted to the lubricating fluid without exposing it to air . however , because the lubricating fluid once having been fed into the fluid tank 4 can no longer be degassed , the fluid must be adjusted ahead of time to adequately reduce the concentration of gas dissolved in the fluid . which of these two methods to choose is best decided by the technician taking other factors into consideration . as will be detailed later , in the lubricating - fluid infusion apparatus 1 , with the interior of the fluid tank 4 in a reduced - pressure state in order to degas the lubricating fluid , the capillary tube 32 tip is in a situation in which it is exposed to atmospheric pressure . under those circumstances , external air tries to enter in , heading toward the fluid tank 4 . conversely , when the infusion apparatus 1 dispenses lubricating fluid , on the one hand the tip of the capillary tube 32 is under reduced pressure ; on the other , the empty space 45 is put at atmospheric pressure , imparting dispensing pressure to the lubricating - fluid . under these circumstances , the lubricating fluid tries to flow out , heading toward the exterior . in either case , the flow has to be stopped with the valve mechanism . consequently , what is sought in a valve mechanism for the dispenser 3 is that the valve will not give rise to leaking not only when the internal pressure is in a higher state , but also when the external pressure is . a valve mechanism 30 of the structure illustrated in fig3 can be employed as such a valve . the description now turns to fig3 , a sectional view illustrating key features of the dispenser 3 . from the end portion of the cylindrical capillary tube 32 , mounted in the tip of the dispenser 3 , fluid is dispensed into the dynamic - pressure bearing device . joined to the fluid tank 4 via the feed duct 42 is an inlet 34 through which lubricating fluid imparted with delivery pressure is supplied . in a supply hole 35 formed in a valve base part 31 , an occluding rod 33 is accommodated for being pressed back and forth by a drive mechanism 38 . when the occluding rod 33 is pressed downward in the figure by the drive mechanism 38 , it closes off an occlusion hole 37 , forming a shutoff ( fig3 a ). conversely , when the rod is drawn upward in the figure , the occlusion hole 37 is cleared , permitting the passage of lubricating fluid ( fig3 b ). the drive mechanism 38 can be a device having the lone capability of simply shifting the occluding rod 33 back and forth , and can be constituted from , for example , a spring and an electromagnet . the occluding rod 33 can thus be driven at high speed merely by electrical on / off switching . in a valve mechanism 30 configured in this way , the occlusion established by the occluding rod 33 and the occlusion hole 37 is located extremely close to the basal end of the capillary tube 32 ( nozzle ); moreover , forward of the shutoff , there is no surplus cavity in which air bubbles and the like would get stuck . the lubricating - fluid flowpath in the dispenser 30 running forward of the occlusion is constituted almost exclusively by the cavity in the interior of the cylindrical capillary tube 32 . initially the vacuum chamber 2 is lifted up into its opened state as indicated in fig4 a , and the dynamic - pressure bearing device 5 is set in a predetermined position atop the pedestal 21 . to heighten the accuracy with which the bearing device is located into place , a special jig or a precision - movable stage may be employed . in this state , the inside of the vacuum chamber 2 is at atmospheric pressure whereas the empty space 45 in the fluid tank 4 is continuously evacuated , wherein the space is pumped down to a pressure of 10 pa ( first pressure ). at the same time , by the magnet - equipped rod 44 rotating , the stirrer 43 plunged into the fluid tank 4 interior rotates , thus stirring the lubricating fluid . gastightness between the fluid tank 4 and the vacuum chamber 2 is maintained by the dispenser 3 . with the lubricating fluid being exposed to an atmosphere of 10 pa in pressure , the evacuation and stirring are continued . under such conditions , the concentration of gas present dissolved within the lubricating fluid may be deemed to be at a concentration about in equilibrium with that of the atmosphere of 10 pa in pressure . next the vacuum chamber 2 is lowered to close off its open - ended side against the pedestal 21 , and the interior is pumped down . the dispenser 3 and the fluid tank 4 are lowered together with the vacuum chamber 2 , shifting to a low position . as a result , the tip of the capillary tube 32 is positioned into the seal section 53 ( fig5 ) formed in the open portion of the bearing gap of the dynamic - pressure bearing device 5 . at the same time , as a result of the fluid tank 4 having shifted downward , the change in relative position of the rod 44 brings its magnetic force out of action , and thus the stirrer 43 stops rotating , halting the stirring action . then the evacuation level for the vacuum chamber 2 is adjusted ( pressure - adjusting step ) so that the internal pressure of the vacuum chamber 2 will go to a pressure ( second pressure ) somewhat higher than the first pressure . after that , in order to impart delivery pressure to the lubricating fluid , ambient air is introduced into the empty space 45 , raising it to atmospheric pressure . ambient air is advantageous as the most readily available source for supplying constant pressure . nevertheless , the space 45 does not necessarily have to be brought to atmospheric pressure , but according to requirements may equally well be brought beneath atmospheric or above atmospheric pressure , freely selected using a suitable device . next , the valve mechanism 30 is opened for a predetermined duration to deliver the proper quantity of lubricating fluid that the dynamic - pressure bearing device 5 is meant to retain . at that time , although the lubricating fluid in the fluid tank 4 interior will have been exposed to air at atmospheric pressure , because the stirring will have been stopped , in particular the lubricating fluid being drawn out from the lower portion of the fluid tank 4 will have been in a state of approximate equilibrium with the first pressure . the lubricating fluid being ejected flows out from the tip of the capillary tube 32 . at that point , lubricating fluid flowing out from the tip of the capillary tube 32 will not froth , because the internal pressure of the vacuum chamber 2 will have gone to 30 pa ( second pressure ), which is greater than the first pressure . therefore , the process of wiping up lubricating fluid having splattered due to frothing and become stuck to the dynamic - pressure bearing device can be omitted . what is more , the elimination of loss due to frothing reduces dispensing volume variation , making the dispensing volume more accurate . it should be noted that in advance of the pressure - adjusting step , the interior of the vacuum chamber 2 may if necessary be momentarily pumped down to a pressure ( fifth pressure ) lower than the second pressure . for example , the chamber interior may be pumped down to the same 10 - pa level as the first pressure . doing so makes evacuation of the bearing even more thorough . prior to fluid dispensing , however , the chamber must be pressurized to a pressure ( second pressure ) higher than the first pressure to prevent the fluid from frothing . fig5 represents an enlarged view of the vicinity of the seal section 53 of the dynamic - pressure bearing device 5 right after having been infused with fluid . the seal 53 is formed in the open end of the bearing gap — marked with reference numeral 54 in the figure — in between the shaft 51 and the sleeve 52 . the tip of the cylindrical capillary tube 32 is drawn near the seal 53 , to just short of touching its wall surfaces , in which state the lubricating fluid is dispensed . the shaft 51 constitutes a bearing - device rotary component , and the sleeve 52 constitutes a bearing - device stationary component . with the seal section 53 being formed in the open portion of the bearing gap , it surrounds the rotary component . lubricating fluid having been dispensed spreads around the entire the seal section due to its affinity for the seal - section wall surfaces , but does not reach the depths of the bearing gap 54 . at this stage the lubricating fluid — marked with reference numeral 6 in fig5 — need not fill the seal section in its entirety , but must occupy the entire circuit of seal area of the gap . moreover , by the bearing - device environs having been pumped down to 30 pa beforehand , the bearing gap will have been pumped down to a pressure near that , and thus the lubricating fluid will be in a state in which due to its affinity for the wall surfaces it will readily enter into the depths of the bearing gap . the right - hand side of fig5 schematically represents the immediate post - dispensing state of the fluid . immediately post - dispensing the lubricating fluid 6 pools in the open portion of the bearing device , but by its affinity for the wall surfaces the fluid transitions at once into the state sketched on the left - hand side of the figure . in the figure left - hand side , the lubricating fluid has in part crept into the depths of the bearing gap 54 , lowering the liquid surface of the lubricating fluid in the seal section 53 by that extent . depending on the configuration of the seal section 53 , and on the quantity of lubricating fluid that the bearing is meant to hold , in some cases the requisite amount of lubricating fluid cannot be dispensed in a one - time operation . in such cases , the fluid dispensing job may be divided into two or more cycles . the second and subsequent fluid - dispensing operations then can be carried out by estimating the time , following the first - cycle fluid - dispensing job , for the lubricating fluid to spread around the entire seal section 53 and its liquid surface to drop sufficiently . after the fluid dispensing operation is finished , the vacuum chamber 2 interior is repressurized ( third pressure ). the repressurization develops a pressure differential between the lubricating fluid 6 interior / exterior , forcing the lubricating fluid 6 into the depths of the bearing gap 54 and completing the lubricating - fluid dispensing job . although it is easiest to repressurize back to atmospheric pressure , repressurization to a pressure lower than atmospheric will not impede the dispensing process , as long as the pressure is sufficient to force the lubricating fluid all the way into the bearing gap . in addition , the vacuum chamber 2 may again be evacuated and the fluid dispensing process carried out again , once lubricating fluid has been forced into the gap and sufficient space in the seal section 53 has been secured . reference is now made to fig6 , which , like fig5 , is an enlarged view of a bearing - device seal section , in this case in a dynamic - pressure bearing device 5 ′ in which the upper - end face of the sleeve has a slope 60 . a fluid - repellent film is formed on the slope and shaft surfaces . in implementations in which the dynamic - pressure bearing device is structured in this way , the dispensed lubricating fluid fills over the slope ( right half of the figure ), and by capillary action subsequently permeates its way into the bearing gap ( left half of the figure ). benefits of having the slope 60 are not only that a large volume of lubricating fluid may be dispensed at once , but also that lubricating fluid does not get left behind on the upper - end face of the sleeve . the dynamic - pressure bearing device 5 on which the dispensing procedure has been finished is then run through a procedure to check for the presence of air encroachment . although the reliability of the bearing - device infusion method of present invention is extraordinarily high , foul dispensings can arise nevertheless . thus , inspection for excluding such rejects is carried out . fig7 is a diagram for explaining this procedure . the dispensing - processed bearing device 5 is put under atmospheric pressure . as far as the pressure environment for this procedure is concerned , as long as the pressure is higher than a later - described fourth pressure , inspection is in principle possible , but atmospheric pressure , being quite readily realized , is advantageous . the dynamic - pressure bearing device 5 is set inside a vacuum case 91 furnished with an evacuation mechanism , and anchored using a suitable jig . in that situation , the level of the lubricating fluid in a state in which atmospheric pressure has been applied is measured . the measurement is made using a laser displacement sensor 93 , whose beam passes through a glass lid 92 on the vacuum case 91 . next a vacuum pump p and a venting valve are operated to lower the internal pressure of the vacuum case 91 to 1000 pa , which is the fourth pressure . in this state , the fluid level is once again measured , and is compared with the level before the pressure was reduced . if upon this second measurement the amount by which the level has risen exceeds a predetermined value , the device is excluded as a reject ; if not , the device is rendered an acceptable item . when the dynamic - pressure bearing device is shipped by airfreight , the aircraft will fly in the lower regions of the stratosphere , which at maximum elevation is in the neighborhood of 14 km into the sky . at that elevation the atmospheric pressure is on the order of 140 hpa , which is considerably larger than 1000 pa ( 10 hpa ). consequently , if a dynamic - pressure bearing device has passed the reduced - pressure test at 1000 pa , then even if the device is transported in a cargo bay that is not pressurized in the least , the likelihood of fluid leakage occurring may be deemed to be extremely small . the lubricating fluid that is fed into the lubricating - fluid infusion apparatus 1 is subjected to a special degassing process in advance , which shortens the time required for the degassing process within the fluid tank 4 . in an infusion method of the present invention , lubricating fluid that is insufficiently degassed because the interior of the fluid tank 4 is repeatedly exposed to the air may be deaerated with greater assurance in a separate vacuum chamber initially . fig8 illustrates the configuration of a degassing device utilized for such objectives . a vacuum case 9 is placed atop a magnetic - stirrer drive mechanism 8 , and within a lubricating - fluid reservoir 7 inside the case 9 lubricating fluid 6 is contained . the vacuum case 9 interior is pumped down by a vacuum pump p to a pressure lower than the first pressure . a good target is pumping down to 10 pa or less to keep on evacuating the case further . long - term stirring in that state is continued , reducing dissolved gas until the level at which it is in equilibrium with this pressure ambient . in addition to the advance degassing process , means may be devised so as to produce a deaerating effect when the lubricating fluid is fed into the fluid tank 4 . fig9 represents a method of trickle feeding lubricating fluid into the fluid tank 4 . specifically , the lubricating fluid is fed into a funnel 100 , and via a microflow valve 101 is trickled in drops into the fluid tank 4 . the fluid tank 4 interior is pumped down to 10 pa or so . with the surface area per unit volume of the drops being large , degassing proceeds rapidly . and degassing is promoted further by the drops undergoing shock when they strike the inner surface of the fluid tank and the liquid surface . not - illustrated heaters are attached to the vacuum case 9 and the fluid tank 4 utilized for the preprocess degassing . the lubricating fluid is deaerated having been heated up by the heaters to 60 degrees . degassing proceeds swiftly because in general the solubility of gasses in a liquid drops as the temperature of the liquid rises . the best mode , explained in the foregoing , for embodying the present invention is not limited by the content set forth herein . for example , as the dynamic - pressure bearing device into which lubricating fluid is dispensed , a shaft - rotating type has been depicted , but the effects of the present invention when applied to a shaft - stationary type of dynamic - pressure bearing device do not alter . as a lubricating - fluid stirring mechanism , an example that employs a magnetic stirrer has been illustrated , but rotating the stirrer by utilizing a terminal or other device that introduces rotation into the vacuum chamber yields similar effects . | 5 |
as shown in fig3 system 100 according to an embodiment of the invention includes a power source 110 which supplies power through power converter 120 to drive a load 800 . demand sensor 180 senses the power consumed by the load . value converter 130 receives the observed power consumption value and projects the power output that power source 110 must produce in order to meet the load demand . this power supply requirement value is outputted to lookup tables 140 and 170 . lookup table 140 maps the power supply requirement value to a power demand value . a value based at least on part on this power demand value is inputted to fuel supply controller 160 , which controls the supply of fuel to power source 110 accordingly . lookup table 170 maps the power supply requirement value to a rate target value . after an observed rate value as indicated by supply rate sensor 190 is subtracted from the rate target value , the resulting rate error value is inputted to stabilizer 150 , which produces an inertia compensation value . the power demand value is modified by this inertia compensation value , and the modified power demand value is inputted to fuel supply controller 160 . power source 110 receives fuel via fuel supply controller 160 and produces power . this power , which is inputted to power converter 120 , may be produced as mechanical energy , as thermal energy or as some other form of energy . power source 110 may be an engine 210 , as shown in fig4 such as a diesel engine . in an exemplary implementation , as shown in fig5 power source 110 is a gas turbine 212 which consumes a fossil fuel ( e . g ., diesel fuel ) received via fuel supply controller 160 and which produces mechanical power by turning a drive shaft . in a particular implementation , the operation of gas turbine 212 is characterized by a speed of a compressor and a speed of a turbine output shaft , which need not be linked except by thermodynamic pressure . turbine 212 may have several compressors and / or output shafts , and turbine 212 may also be of another type such as a vapor or steam turbine . power converter 120 converts the power received from power source 110 into a form as required by load 400 . for example , this conversion may be from thermal to electrical power , or from electrical to mechanical power , or from thermal to mechanical power . in one implementation of the invention , power converter 120 comprises a generator that receives mechanical power outputted by power source 110 ( e . g ., by turning a drive shaft ) and converts it into electrical power . in an exemplary implementation , power converter 120 comprises two or more generators and a gearbox that receives the mechanical power and distributes it among the generators in predetermined proportion . power converter 120 may also include rectifiers , inverters , and / or filters to produce an output in the form required by load 800 . in the exemplary implementations of fig4 and 5 , electrical load 810 may comprise one or more motors which propel a fuel - powered locomotive that incorporates a system as described herein . demand sensor 180 outputs an observed power consumption value that relates to the power demand of load 800 . this demand value may be expressed , for example , as watts or joules . in the exemplary implementations of fig4 and 5 , demand sensor 180 outputs a signal that relates to a level of electrical power demanded by electrical load 810 . for example , demand sensor 180 may include one or more voltage sensors and one or more current sensors , wherein a power demand value corresponding to a particular component of electrical load 810 is obtained by multiplying together corresponding voltage and current values . values may be sensed or outputted by demand sensor 180 according to a given digital sampling rate , for example , 50 hz . in a case where load 800 consumes thermal power ( i . e ., for heating and / or for cooling ), demand sensor 180 may produce a value relating to a difference between a temperature of a component of load 800 and an ambient or a desired temperature . as above , the sensing and / or the output of values by the demand sensor 180 may be either analog or digital . value converter 130 receives the observed power consumption value from demand sensor 180 and produces a power supply requirement value in response . the power supply requirement value represents a projection of the power that power source 110 must supply in order to meet the load demand . in one implementation , value converter 130 produces the power supply requirement value by applying an efficiency reciprocal function to the observed power consumption value , wherein the efficiency reciprocal function represents the inverse of the efficiency of conversion of power converter 120 . in this way , an estimate of the level of power output by power source 110 that will produce the load power demand at the output of energy converter 120 may be obtained . in a case where the efficiency reciprocal function may be expressed as a constant factor ( i . e ., the relationship between power inputted to and power outputted by power converter 120 is linear ), value converter 130 may be constructed as a constant multiplier . in another case ( e . g ., for a more complex relationship ), value converter 130 may comprise one or more lookup tables whereby a particular demand level may be interpolated to a corresponding power supply requirement . in the exemplary implementations of fig4 and 5 , value converter 130 may compensate for the efficiency of one or more generators , gear boxes , rectifiers , inverters , and / or other components that may appear in the power path between the output of power source 110 and the input of electrical load 810 . lookup table 170 receives the power supply requirement value produced by value converter 130 and outputs a corresponding rate target value . the map between the input power value and the output rate value that characterizes lookup table 170 may be optimized according to a particular criterion such as fuel consumption , emissions production , operating temperature , etc . in an exemplary implementation , for example , lookup table 170 applies a map that is optimized for minimum fuel consumption . the relationship mapped by lookup table 170 may be a function of one or more other values as well . for example , a performance of a turbine 212 may also depend on a temperature of the air at the compressor intake , as the density of air may change dramatically with large changes in temperature . similarly , large changes in altitude may also result in air changes in the ambient air pressure that will affect air density as well . therefore , lookup table 170 may be implemented as a matrix of tables . each such table may indicate a different mapping of power to rate , and the choice between the tables may be determined by sensed operating parameters such as air pressure and temperature , fuel characteristics , etc . supply rate sensor 190 outputs an observed rate value that relates to the rate of energy supply by power source 110 . in the exemplary implementations of fig4 and 5 , supply rate sensor 190 is implemented as a speed sensor 290 and outputs a value obtained by sampling ( at a rate of 50 hz ) the rotational position or speed of a drive shaft driven by power source 110 . in this case , the value outputted by speed sensor 290 relates to a speed of the drive shaft in revolutions per minute ( rpm ). in adder 80 , the observed rate value produced by supply rate sensor 190 is subtracted from the rate target value outputted by lookup table 170 to obtain a rate error value . stabilizer 150 receives the rate error value and outputs an inertia compensation value according to one or more predetermined stabilization profiles . in an exemplary implementation , stabilizer 150 is a governor 250 that is implemented as a proportional - integral controller . the operation of such a controller is characterized by a proportional gain kp and an integral gain ki . proportional - integral controllers tend to decrease rise time and steady state error while increasing overshoot . other forms of controllers ( such as proportional , derivative , or proportional - integral derivative ) may also be used for stabilizer 150 if different performance characteristics are desired . although incorporating a derivative gain allows a system to reach the steady state sooner , such controllers also tend to add noise to the system . in exemplary implementations of fig4 and 5 , the extra response provided by incorporating a derivative gain has not been necessary in practice . lookup table 140 receives the power supply requirement value produced by value converter 130 and produces the power demand value . in the exemplary implementation of fig4 and 5 , the power demand value relates to a speed of a compressor of a turbine 212 , which speed is strongly correlated with turbine output power . as with lookup table 170 , the relationship between power and speed , for example , that is mapped by lookup table 140 may depend on other operating parameters such as pressure and temperature as well . therefore , lookup table 140 may be similarly implemented as a matrix of ( e . g ., 64 ) tables , wherein sensed values of such other operating parameters are used to select the desired mapping . fuel supply controller 160 receives the modified power demand value outputted by adder 70 and adjusts the supply of fuel to power source 110 , accordingly . in the exemplary implementations of fig4 and 5 , fuel supply controller 160 monitors the speed of a compressor of turbine 212 , and adjusts the fuel supply such that the compressor speed complies with the modified power demand value . in another implementation , fuel supply controller 160 may control the fuel supply based upon other monitored values in order to maintain a desired correspondence between the modified power demand value and the operation of power source 110 . because of the quick feedback path provided through lookup table 140 , system 100 may adapt quickly to meet changes in the load demand level , thereby reducing both response time and fuel consumption . in the exemplary implementation of fig4 and 5 , because the power demand value is modified by the inertia compensation value before it is inputted to fuel supply controller 160 , the inertia encountered by the generated power in transfer from power source 110 to load 800 may be counteracted by increasing or decreasing the power demand value as appropriate . in these exemplary implementations , inertia is encountered in attempting to change the speed of the turbine output shaft , the components of the gear box , and the components of the generator , for example . when adder 80 returns a positive value ( i . e ., the speed of the output shaft of turbine 212 is insufficient to support the power demand of electrical load 810 ), an augmented power demand value is inputted to fuel supply controller 160 in order to accelerate the inertial components more quickly to the desired speed . when the value outputted by adder 80 is negative ( i . e ., the turbine output speed is higher than the power demanded by electrical load 810 requires ), then a reduced power demand value is inputted to fuel supply controller 160 such that the load may pull part of the required power out of the inertial components and thereby decelerate them to the appropriate speed more quickly . fig6 is a block diagram of a system according to an alternative embodiment of the invention . in this embodiment , override 320 inputs a minimum rate requirement b to maximum function block 310 . maximum function block 310 outputs the maximum between the override rate b and the rate target value outputted by lookup table 170 . such an embodiment may be used in a case where a minimum rate is desired or required , regardless of the power demand of load 800 . in the exemplary implementations of fig4 and 5 , for example , it may be necessary to operate a generator at a minimum speed , regardless of the power drawn by electrical load 810 . it is possible that the additional mode of operation described in fig6 may only be initiated in the case of a malfunction of one or more components of load 800 . because the relationship between power and rate which is mapped in lookup table 140 may be nonlinear , it may not be desirable to use fixed values for k p and k i in stabilizer 150 . k p and k i values which are appropriate at low values of low power demand , for example , may not be appropriate at high levels of demand , due in part to this nonlinearity . in the alternative implementation shown in fig7 such a difficulty may be avoided by moving the conversion from power to rate performed in lookup table 140 to a point subsequent to the summation in adder 70 . in this case , stabilizer 450 converts the rate error value into an inertia compensation value that relates to power rather than rate . as a consequence , fixed values of k p and k i may be used in stabilizer 450 . lookup table 440 may be adjusted as necessary to perform the new mapping or mappings . alternatively , as shown in the embodiment of fig8 the rate values may be squared in squaring function blocks 460 and 470 before differentiation in adder 80 . in this case , stabilizer 452 performs a similar conversion with possibly different fixed values of kp and ki . because of the squaring of the rate values , the value outputted by stabilizer 452 bears . a closer resemblance to power ; and , therefore , it is possible in the implementation to use the same mappings in lookup table 140 . as shown in fig9 and 10 , the modification described in fig6 may be combined with the modifications shown in fig7 and 8 . fig1 shows an apparatus 105 according to an embodiment of the invention . this apparatus may be constructed and supplied separately from power source 110 and power converter 120 for use with possibly different power generation systems . similarly , the apparatus shown in fig1 may be used to perform a function similar to that of the system shown in fig8 . the foregoing presentation of the described embodiments is provided to enable any person skilled in the art to make or use the present invention . various modifications to these embodiments are possible , and the generic principles presented herein may be applied to other embodiments as well . for example , the invention may be implemented in part or in whole ( as appropriate to the particular embodiment ) as a hard - wired circuit or as a circuit configuration fabricated into an application - specific integrated circuit or field programmable gate array . likewise , the invention may be implemented in part or in whole as a firmware program loaded or fabricated into non - volatile storage ( such as read - only memory or flash memory ) as machine - readable code , such code being instructions executable by an array of logic elements such as a microprocessor or other digital signal processing unit . further , the invention may be implemented in part or in whole as a software program loaded as machine - readable code from or into a data storage medium such as a magnetic , optical , magnetooptical , or phase - change disk or disk drive ; a semiconductor memory ; or a printed bar code . thus , the present invention is not intended to be limited to the embodiments shown above but rather is to be accorded the widest scope consistent with the principles and novel features disclosed in any fashion herein . | 7 |
hereinafter , exemplary embodiments of the present invention are described in detail with reference to the accompanying drawings . the same reference numbers are used throughout the drawings to refer to the same or similar parts . detailed descriptions of well - known functions and structures incorporated herein may be omitted to avoid obscuring the subject matter of the present invention . fig1 is a perspective view depicting a detachable rotational filter supporter according to the present invention . fig2 is a disassembled view depicting a detachable rotational filter supporter according to the present invention . fig3 is a front view depicting a detachable rotational filter supporter according to the present invention . fig4 is a partially enlarged view of fig3 . fig5 is a cross - sectional view , taken along line a - a , in fig4 . as shown in fig1 to fig5 , the detachable rotational filter supporter includes a housing 10 , an inflow part 20 , an outflow part 30 , a base 40 , hinges 50 , a locking part 60 , a compression spring 70 , a protrusion 75 , and a check valve 80 . the housing 10 forms a receiving hole 11 therein , in which a neck portion of a filter 90 is placed . more specifically , the housing 10 is configured to include an outer body 12 and an inner body 13 , so that the check valve 80 can be installed therein . the inner body 13 forms the receiving hole 11 therein , in which a neck portion of a filter 90 is place . the housing 10 is pivotally installed with respect to the hinge 50 . the inflow part 20 is configured in such a way that : its one end ( or an inlet ) is formed at one side of the outer body 12 to communicate with the outside and to receive unfiltered water ; and its opposite end ( or an outlet ) is formed to communicate with the receiving hole 11 . the inflow part 20 includes a narrow portion 21 of a flow channel at one side thereof , so that the inlet has a larger diameter than the outlet . the inlet 20 serves to guide unfiltered water to the filter 90 . the narrow portion 21 of a flow channel can be formed as a sloping surface , as shown in fig6 . also , the narrow portion 21 can be formed as a round shape , as shown in fig7 . the outflow part 30 is configured in such a way that : its outlet for discharging water , purified through the filter 90 , is formed at another side of the outer body 12 of the housing 10 ; and its inlet for receiving purified water from the filter is formed in the inner body 13 of the housing 10 so as to communicate with the receiving hole 11 . the outflow part 30 serves to discharge water purified through the filter 90 . as shown in fig3 , the filter 90 is configured to include : an outer tube - type boy 92 , shape as a cylindrical form , with a neck 91 ; an inner tube - type body 93 installed in the cylindrical outer body 92 , forming a first flow channel communicated with the inflow part 20 , in which the inner tube - type body 93 forms a second flow channel communicated with the outflow part 30 therein ; a filter member 94 installed in the flow channel of the inner tube - type body 93 for purifying unfiltered water that flows in through the inflow part 20 ; and a filter cap 95 whose outer portion is communicated with the inflow part 20 and whose inner portion is communicated with the outflow part 30 , in which the filter cap 95 is installed to the upper end of the inner tube - type body 93 , dividing the neck 91 of the outer tube - type body 92 into an outer portion and inner portion . it is preferable that the neck 91 of the outer tube - type body 92 forms a locking groove at the outer periphery thereof , to which a locking part 60 is fitted . the filter member 94 is made of any one of a carbon block filter , a bamboo block filter , a π - ceramic filter , and an ultra filtration filter , or made of the combination of two or more of the filters listed above . since the filter 90 is configured to include well - known elements , its detailed description will be omitted in the following . the base 40 is installed to the housing 10 in such a way as to form a receiving space 14 in the bottom of the housing 10 , i . e ., in the lower portion of the housing 10 . the base 40 forms a through - hole 41 , whose axis is the same as the receiving hole 11 , for allowing the neck 91 of the outer tube - type body 92 to pass through . the receiving space 14 allows for the installation of the locking part 60 so that the locking part 60 can slidably move in the receiving space 14 . therefore , the receiving space 14 is communicated with the receiving hole 11 . here , the locking part 60 holds the neck 91 of the filter 90 received in the receiving hole 11 . the hinges 50 form a pair and are installed to both the inflow part 20 and outflow part 30 , respectively . the respective hinges 50 form a flow - hole 51 therein . the hinges 50 are inserted into the inlet of the inflow part 20 and into the outlet of the outflow part 30 , respectively , so that the inflow part 20 can be communicated with the outflow part 30 through their flow holes 51 . the pair of hinges 50 is rotatable with respect to the axis established by the inflow part 20 and the outflow part 30 . also , one side of the respective hinges 50 is fixed to the inner wall of the water purifier . also , opposite sides of the hinges 50 , which are located opposite the inflow part 20 and outflow part 30 , are each connected to u - shaped flow pipes installed into the water purifier . it is preferable that a first o - ring 52 is inserted between the hinge 50 and the housing 10 to prevent water leakage . more preferably , the number of the first o - ring 52 should be at least one or more . the locking parts 60 form a pair , and are slidably installed to the receiving space 14 horizontally . as shown in fig8 , each locking part 60 forms : an arc portion 61 for holding the neck 91 of the outer tube - type body 92 of the filter 90 on one side ( i . e ., a facing side ) thereof ; and a thin plate 62 at the opposite side thereof , which is protrudent to the opposite outside . the arc portion 61 is formed to receive the locking groove 96 formed at a portion of the neck 91 of the outer tube - type body 92 of the filter 90 . as shown in fig9 , it is preferable that the locking part 60 includes a chamfered portion 63 formed as the upper edge of the arc portion 61 is chamfered , so that the art portion 61 can be received smoothly by the locking groove of the filter 90 . also , it is preferable that the thin plate 62 contacting the protrusion 75 is formed to be semicircular at its free end . it is preferable that the outer tube - type body 12 of the housing 10 includes a through - hole 15 at its both sides , through which the thin plate 62 passes . when the thin plate 62 of the locking part 60 is located within the housing 10 , the arc portion 61 holds the filter 90 . on the contrary , when the locking part 60 is slid by the compression spring 70 and thus the thin plate 62 is exposed to the outside from the housing 10 , the arc portion 61 releases the filter 90 . at least two or more compression springs 70 are installed between the pair of locking parts 60 so as to elastically push the locking parts 60 to the outside . the protrusion 75 is protrudently formed from the hinge 50 . when the protrusion 75 contacts the thin plate 62 of the locking part 60 , the arc portion 61 contacts the neck 91 of the filter 90 , so that it can be received in the locking groove 96 formed at the portion of neck 91 to hold the filter 90 . when the housing 10 is rotated , the protrusion 75 is released from the thin plate 62 . the check valve 80 is installed to one side of the inflow part 20 . the check valve 80 opens or closes the flow channel of the inflow part 20 when the filter 90 is installed to or separated from the water purifier . as shown in fig6 and fig7 , the check valve 80 is configured in such a way that : a first shaft 81 is located at one side of the narrow portion 21 of a flow channel ; a first head 82 is formed at one end of the first shaft 81 , and installed to the narrow portion 21 of a flow channel , so that the opposite end of the first head 82 is located at the receiving hole 11 , contacting the upper surface of the neck 91 of the outer tube - type body 92 , received in the receiving hole 11 , and the opposite end of the first head 82 is placed within the inflow part 20 ; a block plate 83 is formed between the first head 82 and the first shaft 81 , and closely contacts the narrow portion 21 of a flow channel to close the flow channel of the inflow part 20 when the opposite end of the first head 82 is located at the receiving hole 11 ; and a first spring 84 whose one end closely contacts the block plate 83 and whose opposite end closely contacts the flow channel , so as to elastically and constantly push the block plate 83 . when a portion of the neck 91 of the filter 90 is located at the receiving hole 11 of the housing 10 , its upper surface contacts the first head 82 , so that the opposite end of the first head 82 is located within the inflow part 20 and the block plate 83 is separated from the narrow portion 21 of a flow channel , thereby opening the inflow part 20 . when the filter 90 is separated from the water purifier , the first spring 84 closely joins the block plate 83 and the narrow portion 21 of a flow channel , thereby closing the inflow part 20 . it is preferable that a second o - ring 85 is inserted between the first head 82 and the block plate 83 so as to enhance water tightness when the check valve 80 closes the flow channel of the inflow part 20 . the second o - ring 85 is placed in a groove 86 formed between the first head 82 and the block plate 83 . the inflow part 20 is formed as an l - shape so that the check valve 80 can be easily installed to the inflow part 20 . it is preferable to further include : a receiving portion 87 formed at a bent part that is positioned in the same direction as a vertical part , in which the receiving portion 87 is communicated with the surface of the inner body 13 ; and a plate 88 , installed to the surface of the inner body 13 , for closing one side of the receiving portion . it is preferable to further include a protrusion part 89 a protrudent from one side of the plate 88 . the protrusion part 89 a is placed in the receiving portion 87 . the protrusion part 89 a forms a receiving region therein to receive the first spring 84 and the first shaft 81 installed in the receiving portion 87 . the outflow part 30 can be configured to include a flow channel enlarging part 31 at its one end , so that the inlet can be smaller in diameter than the outlet . it is preferable that the flow channel enlarging part 31 is formed to have a step , so that a backward flow check valve 100 , which will be described later , can be easily installed . fig1 is a perspective view depicting another embodiment of a detachable rotational filter supporter with a backward flow check valve , according to the present invention . as shown in fig1 , it is preferable that the detachable rotational filter supporter according to the present invention further includes a backward flow check valve 100 at one side of the outflow part 30 . more preferably , the inflow channel enlarging part 31 is formed in the step . the backward flow check valve 100 minimizes leakage of purified water that remains in the outflow part 30 when the filter 90 is separated from the water purifier . fig1 is a large view depicting a primary part of the detachable rotational filter supporter with a check valve of fig1 . fig1 is a view that explains an operating state of the check valve . as shown in fig1 and fig1 , the backward flow check valve 100 is configured to include : a body 110 that is installed to the flow channel enlarging part 31 , includes an o - ring 111 at the periphery thereof , forms a hollow cavity 112 therein , forms a tri - ped 113 at one side thereof , and includes a connecting frame 115 that generates a hole 114 simultaneously when the free ends of the tri - ped 113 are connected thereto ; a second shaft 120 slidably installed and extended through the hole 114 , wherein the second shaft 120 including , a second head 121 that closely joins its one end with the hollow cavity 112 and closes the hollow cavity 112 ; and a second spring 130 installed between the second head 121 and the connecting frame 115 for elastically and continuously pushing the second head 121 . that is , as shown in fig1 , when purified water is output from the filter 90 , the second head 121 is retreated from the hollow cavity 112 , overcoming the elastic force of the second spring 130 , and is separated from the edge of the periphery forming the hollow cavity 112 by the purified water pressure , thereby opening the outflow part 30 . on the contrary , when purified water is blocked , by the elastic force of the second spring 130 , the second head 121 is moved to the hollow cavity 112 and contacts the edge of the periphery forming the hollow cavity 112 , thereby closing the outflow part 30 . in the following description , the operation of the detachable rotational filter supporter will be explained with reference to figures . fig1 is a perspective view depicting a state where a filter is separated from a housing of the detachable rotational filter supporter according to the present invention . fig1 is a cross - sectional view , taken along line b - b , in fig1 . fig1 is a cross - sectional view , taken along line c - c , in fig1 . fig1 is a view depicting an operating state of the detachable rotational filter supporter according to the present invention . the filter 90 to be replaced is separated from a water purifier as follows : the hosing 10 is rotated with respect to filter 90 or vice versa , as shown in fig1 . that is , the housing 10 is rotated with respect to the hinges 50 fixed to the inner wall of the water purifier , because parts of the flow - holes 51 of the hinges 50 are rotatably installed to the inflow part 20 and outflow part 30 , respectively , which are located at both sides of the housing 10 . while the housing 10 is rotated , the protrusions 75 formed at the hinges 50 are separated from the thin plates 62 of the locking parts 60 . the locking parts 60 are moved to the outside from the housing 10 by the compression springs 70 installed between the locking parts 60 , and then exposed through the through - holes 15 to the outside , as shown in fig1 . the arc portions 61 of the locking parts 60 are separated from the locking grove 96 of the neck 91 of the filter 90 , thereby releasing the filter 90 . as a result , the filter 90 is separated from the housing 10 . when the filter 90 is separated from the housing 10 , the opposite end of the first head 82 of the check valve 80 contacts to the upper surface of the neck 91 of the filter 90 and becomes located in the receiving hole 11 . that is , the second spring 84 pushes the block plate 83 , so that the block plate 83 closely contacts the narrow portion 21 of a flow channel and closes the inflow part 20 . also , the second o - ring 85 , placed in a groove 86 formed between the first head 82 and the block plate 83 , contacts the narrow portion 21 of a flow channel to enhance water tightness . when the inflow part 20 is blocked , the second head 121 closes the hollow cavity 112 by the operation of the second spring 130 of the backward flow check valve 100 and thus closes the outflow part 30 . now , a new filter 90 is installed to the water purifier as follows . the neck 91 of the new filter 90 is inserted into the receiving hole 11 . the upper surface of the neck 91 contacts the opposite end of the first head 82 and thus the first head 82 is moved into the inflow part 20 . while the filter 90 is inserted , the block plate 83 having contacted the narrow portion 21 of a flow channel of the inflow part 20 is separated from the narrow portion 21 so that the flow channel of the inflow part 20 is opened . when the inflow part 20 is opened , unfiltered water passes through the new filter 90 to generate purified water . when the purified water flows into the outflow part 30 , the second head 121 of the backward flow check valve 100 is separated from the hollow cavity 112 by the purified water pressure and thus the outflow part 30 is opened . after that , the housing 10 is rotated to the original position . the protrusions 75 of the hinges 50 contact the thin plates 62 of the locking parts 60 so that the locking parts 60 are slid into the housing 10 . the arc portions 61 of the locking parts 60 are placed into the locking groove 96 of the neck 91 of the new filter 90 , so that the new filter 90 can be locked thereto . as described in the foregoing , the detachable rotational filter supporter according to the present invention allows the filters to be easily separated therefrom in such a way that : the protrusion formed at the hinge is released from the locking part when the housing is rotated ; the filter is unlocked when the locking part is moved to the outside by the spring ; the check valve blocks the flow channel when the filter begins to be separated from the housing , and allows the filters to be easily installed thereto in such a way that : while the separating order is inversely performed , the flow channel is opened ; and the filter can be easily installed thereto when the housing is rotated to the original position . in addition , the detachable rotational filter supporter according to the present invention allows general users to conveniently replace the filters themselves , since the filters can be easily installed to and separated from the water purifier . although exemplary embodiments of the present invention have been described in detail herein above , it should be understood that many variations and modifications of the basic inventive concept herein described , which may appear to those skilled in the art , will still fall within the spirit and scope of the exemplary embodiments of the present invention as defined in the appended claims . | 1 |
referring now to the drawings in detail wherein like reference numerals have been used throughout the various figures to designate like elements , there is shown in fig1 a catheter constructed in accordance with the principles of the present invention and designated generally as 10 . in a first embodiment of the present invention , as seen in fig1 the catheter 10 essentially includes an elongated flexible member 12 which may be made of polyurethane . however , the flexible member 12 may be made from a variety of materials such as silicone rubber or plasticized pvc . the flexible member 12 is preferably approximately 110 centimeters long with an outside diameter of approximately 2 . 5 millimeters . as should be readily apparent to those skilled in the art , only the working portion of the catheter 10 is shown in the drawings . the working portion of the flexible member 12 has a proximal end 14 and a distal end 16 . carried on the working portion of the flexible member 12 of the catheter 10 are first , second , and third spaced apart electrode arrays , the details of which will be described hereinafter . electrical wires ( not shown ) from the electrode arrays pass through the interior of the flexible member 12 to a manifold secured to the remote end of the flexible member 12 for connecting the catheter 10 to appropriate electronic equipment . located adjacent the proximal end 14 is the first electrode array . the array includes approximately ten electrodes 18 a - 18 j where each electrode has an approximate length of five millimeters and each electrode is spaced approximately five millimeters away from each adjacent electrode . the second electrode array , located distal to the first array , consists of approximately twelve electrodes 20 a - 20 l . the length of each of these electrodes is also approximately five millimeters and each electrode is spaced approximately five millimeters away from each adjacent electrode . the third electrode array , located adjacent the distal end 16 consists of approximately seven electrodes 22 a - 22 g . the length of each of these electrode is approximately five millimeters and each is spaced approximately ten millimeters away from each adjacent electrode . located within the second array of electrodes 20 a - 20 l is an atrial pacing / sensing electrode 24 . also , located at the distal end 16 of the flexible member 12 are bi - polar pacing / sensing stimulation electrodes 26 a and 26 b . a steering arrangement known in the art may be associated with the catheter 10 in order to direct the placement of the electrode arrays . in order to perform a defibrillation procedure , the flexible member 12 is introduced into the vascular system from the jugular area in a manner known in the art . the flexible member 12 is then guided into the patient &# 39 ; s heart 28 until it is placed in the desired position . the flexible member 12 is positioned so that the first electrode array 18 a - 18 j is positioned within the superior vena cava 30 , the second electrode array 20 a - 20 l is positioned within the right atrium 32 , and the distal end 16 with the third electrode array 22 a - 22 g is positioned within the coronary sinus 34 . with the flexible member 12 properly in place , electric shocks are applied through the catheter in order to defibrillate the patient &# 39 ; s heart 28 . this is accomplished by connecting the contact pin ( not shown ) at the proximal end of the proximal lead ( not shown ) attached to the first and second electrode arrays and the contact pin ( not shown ) of the distal lead of the third electrode array to an appropriate power source . thereafter , low energy electrical current is supplied through the electrical leads to the corresponding electrode arrays in order to achieve a normal sinus rhythm in the patient . more specifically , the atrial pacing / sensing electrode 24 and the bi - polar pacing / sensing stimulation electrodes 26 a and 26 b , sense the occurrence , if any , of fibrillation . if fibrillation is sensed , the heart 28 is defibrillated or cardioverted by the application of at least one electrical shock between the first and second arrays of electrodes 18 a - 18 j and 20 a - 20 l , respectively , which are connected to the proximal electrical lead and the third array of electrodes 22 a - 22 g which is connected to the distal electrical lead . the two proximal common arrays 18 a - 18 j and 20 a - 20 l on the catheter are coupled together as an anode and the single array 22 a - 22 g on the distal end 16 of the catheter is a cathode . the polarity of the arrays can be reversed to attempt lower defibrillation thresholds in certain patients . approximately 1 - 50 joules of energy are discharged through the sinoatrial node and the atrioventricular node to terminate atrial fibrillation . in a second embodiment of the present invention , as seen in fig2 the catheter 110 , similar to the catheter of the first embodiment , includes an elongated flexible member 112 which may be made of the same types of materials and have the same dimensions as discussed above . again , only the working portion of the catheter 110 is shown . the working portion of the flexible member 112 has a proximal end 114 and a distal end 116 . carried on the working portion of the flexible member 112 of the catheter 110 are first , second ; and third spaced apart electrode arrays , the details of which will be described hereinafter . electrical wires ( not shown ) from the electrode arrays pass through the interior of the flexible member 112 to a manifold secured to the remote end of the flexible member 112 for connecting the catheter 110 to appropriate electronic equipment . located adjacent the proximal end 114 is the first electrode array . the array includes approximately ten electrodes 118 a - 118 j where each electrode has an approximate length of five millimeters and each electrode is spaced approximately five millimeters away from each adjacent electrode . the second electrode array , located distal to the first array , consists of approximately twelve electrodes 120 a - 120 l . the length of each of these electrodes is also approximately five millimeters and each electrode is spaced approximately five millimeters away from each adjacent electrode . the third electrode , located adjacent the distal end 116 consists of approximately seven electrodes 122 a - 122 g . the length of each of these electrode is approximately five millimeters and each is spaced approximately ten millimeters away from each adjacent electrode . located within the second array of electrodes 120 a - 120 l is an atrial pacing / sensing electrode 124 . also , located at the distal end 116 of the flexible member 112 are bi - polar pacing / sensing stimulation electrodes 126 a and 126 b . a steering arrangement known in the art may be associated known with the catheter 110 in order to direct the placement of the electrode arrays . in order to perform a defibrillation procedure , the flexible member 112 is introduced into the vascular system from the jugular area in a manner known in the art . the flexible member 112 is then guided into the patient &# 39 ; s heart 128 until it is placed in the desired position . the flexible member 112 is positioned so that the first electrode array 118 a - 118 j is positioned within the superior vena cava 130 , the second electrode array 120 a - 120 l is positioned within the right atrium 132 , and the distal end 116 with the third electrode array 122 a - 122 g is positioned within the right ventricle 134 instead of the coronary sinus , as in the first embodiment , in an attempt to obtain lower defibrillation thresholds . with the flexible member 112 properly in place , electric shocks are applied through the catheter in order to defibrillate the patient &# 39 ; s heart . this is accomplished by connecting the contact pin ( not shown ) at the proximal end of the proximal lead ( not shown ) attached to the first and second electrode arrays 118 a - 118 j and 120 a - 120 l , respectively , and the contact pin ( not shown ) of the distal lead of the third electrode array 122 a - 122 g to an appropriate power source . thereafter , low energy electrical current is supplied through the electrical leads to the corresponding electrode arrays in order to achieve a normal sinus rhythm in the patient . more specifically , the atrial pacing / sensing electrode 124 and the bi - polar pacing / sensing stimulation electrodes 126 a and 126 b , sense the occurrence , if any , of fibrillation . if fibrillation is sensed , the heart 128 is defibrillated or cardioverted by the application of at least one electrical shock between the first and second arrays of electrodes 118 a - 118 j and 120 a - 120 l , respectively , which are connected to the proximal electrical lead and the third array of electrodes 122 a - 122 g which is connected to the distal electrical lead . the two proximal common arrays 118 a - 118 j and 120 a - 120 l on the catheter are coupled together as an anode and the single array 122 a - 122 g on the distal end 116 of the flexible member 112 is a cathode . the polarity of the arrays can be reversed to attempt lower defibrillation thresholds in certain patients . as in the first embodiment , approximately 1 - 50 joules of energy are discharged through the sinoatrial node and the atrioventricular node to terminate atrial fibrillation . it should be noted that in both of the embodiments , a continuous flexible electrode may be substituted for any or all of the electrode arrays . this ensures that the electrode is sufficiently flexible so that the same can be easily bent and straightened , as desired , without causing damage to the same . such an electrode is preferably formed by a process of ion - beam assisted deposition ( ibad ). this technology is described in detail in each of u . s . pat . nos . 5 , 468 , 562 ; 5 , 474 , 797 ; and 5 , 492 , 763 , the disclosures of which are incorporated herein by reference . the use of this technique for forming an electrode catheter is also described in co - pending application ser . no . 08 / 751 , 436 , filed on nov . 20 , 1996 , entitled “ temporary atrial defibrillation catheter with improved electrode configuration and method of fabrication .” the subject matter of this co - pending application , commonly owned , is also incorporated herein by reference . the electrodes may also be applied by sputtering , vacuum deposition , printing , or spraying . an advantage of the present system is that it is easy to use because only one catheter is needed . that is , the three electrode arrays are combined onto one single catheter . it is far easier and faster for physicians to place one catheter , as opposed to two separate devices , in a patient . also , it is less traumatic and safer for the patient to have one catheter placed within his or her body as opposed to two or more devices . another advantage of the present system is that it is easier to use than pulmonary artery defibrillation catheters because electrophysiologists are more familiar with superior vena cava , right atrium , and coronary sinus catheter placement which is routinely used in their practice as opposed to pulmonary artery placement which is used more in pressure monitoring in critical care . the present invention may be embodied in other forms without departing from the spirit or essential attributes thereof and accordingly , reference should be made to the claims rather than to the foregoing specification as indicating the scope thereof . | 0 |
the embodiments of the present invention are described more fully hereinafter with reference to the accompanying drawings , which form a part hereof , and which show , by way of illustration , specific exemplary embodiments by which the invention may be practiced . this invention may , however , be embodied in many different forms and should not be construed as limited to the embodiments set forth herein . rather , these embodiments are provided so that this disclosure will be thorough and complete , and will fully convey the scope of the invention to those skilled in the art . as used herein , the term “ or ” is an inclusive “ or ” operator , and is equivalent to the term “ and / or ,” unless the context clearly dictates otherwise . in addition , throughout the specification , the meaning of “ a ”, “ an ” and “ the ” include plural references . the term “ coupled ” implies that the elements may be directly connected together or may be coupled through one or more intervening elements . main components of an embodiment of a device for fixing an apparatus for reinforcing a weakened or fractured bone are shown in fig1 a and fig1 b . the device 100 includes a cap 110 which is at one end of the device . the device 100 further includes a tube 120 with an elongated shape . the cap 110 is at one end of the tube 120 . in an embodiment , the cap 110 and the tube 120 are formed from the same rod or bulk in order to possess a better rigidity or stiffness , and the cap 110 may have a through hole 115 at the center . the cap 110 may be composed of two annuli 1101 and 1102 as shown in fig1 a . the annulus 1101 with a larger diameter is disposed farther away from a tapered , tube end 121 of the tube 120 compared to the annulus 1102 . the tube 120 is preferably made with a material such as metal or its alloy . in some embodiments , titanium or its alloy may be selected . in other embodiments , the tube 120 can be either constructed from a single metal , such as stainless steel , and gold or from composite materials such as fiber reinforced metal . preferably , the tube 120 is rigid or substantially rigid in order to resist or minimize deformation under any applied external force . moreover , the tube 120 further includes a lumen . the lumen may extend through the cap 110 to form a tunnel which opens at both ends of the device 100 . in an embodiment , the tapered , tube end 121 distal to the cap 110 is preferably designed as a tapered shape as shown in fig1 a . the tapered angle can be between 0 to 45 degrees . preferably , it can be between 0 to 30 degrees . in some embodiments according to the present disclosure , the angle is designed to be between 2 to 15 degrees . one of the purposes of introducing a tapered end design is to facilitate the tube 120 sliding into a press - fitting outer barrel 200 which may have an inner diameter designed to be interlocked with the outer diameter of the tube 120 . the tube 120 can further include at least one aperture 122 which is disposed proximally to the cap 110 . the aperture 122 can be formed of various shapes such as a circle , slot , and triangle , and the aperture 122 allows materials to pass into and out of the tube 120 . in an embodiment , the inner wall of the tube 120 proximal to the tapered , tube end 121 can be threaded . with a threaded inner wall 125 , the device 100 can be easily fastened with a gear ( not shown ) which is designed to accurately dispose or implant the device 100 at a desired fracture or weakened bone position . those skilled in the art should recognize that the term “ bone ” used herein can be referred to vertebrae , tibia , fibula , humerus , ulna , radius and other bones and still be within the scope and spirit of the disclosed embodiments . the present disclosure further discloses an apparatus 10 for reinforcing a weakened or fractured bone as shown in fig2 . the apparatus 10 includes a device 100 and a barrel 200 . the device 100 can be the same as the aforementioned device 100 or can be slightly modified to fit in the apparatus 10 . the elongated barrel 200 includes a securing part 201 at one end . the barrel 200 further includes an adjustable part 202 adjacent to the securing part 201 . in an embodiment , the securing part 201 is connected with the adjustable part 202 , and the term “ connected ” used herein may refer to any connecting ways and should not be limited to such as jointed , welded , mounted , integrated , or as an integral unit . in an embodiment , the securing part 201 and the adjustable part 202 are formed / machined from the same piece of rod or bulk in order to possess a better rigidity or stiffness . the materials selected for the barrel 200 can be metal or its alloy . in an embodiment , the material selected for the barrel is the same as that of the device 100 . in some embodiments , titanium or its alloy may be selected . in other embodiments , the tube 120 can be constructed of a single metal , such as stainless steel , and gold , or be constructed of a composite material such as fiber reinforced metal . the barrel 200 may have a lumen inside . in other words , both the securing part 201 and the adjustable part 202 are hollow in order to be assembled with the device 100 . the inner diameter ( if the hollowed - out pattern is circular ) of the securing part 201 can be designed to be press fitted with the adjustable part 202 . the outer rim of the securing part 201 can be trimmed to different shapes such as circular or polygonal . in an embodiment , the securing part 201 is hexagonal - shaped or a shape of the combination of rectangle and circle . in an embodiment , the securing part 201 is a bolt head with a through hole as shown in fig2 . fig2 depicts a tubular adjustable part 202 . those skilled in the art should recognize that the adjustable part is not limited to a tube or a cannula . in an embodiment , a part of the adjustable part 202 is carved out to form at least one slotted or patterned hole in the wall of the adjustable part 202 . in another embodiment , a part of the adjustable part 202 is carved out to form a meshed pattern . the slotted or patterned hole ( s ) of the adjustable part 202 allows the tubular adjustable part 202 to deform easily when an external force is applied on the barrel 200 along the axial direction of the tubular barrel 200 . the hollowed patterns also allow reinforcing materials to flow into and out of the barrel 200 . in an embodiment , the adjustable part 202 can expand from a first geometry to a larger volume second geometry , for example , from a tubular shape to a cage , crown , or lantern - like object . the outer surface of the adjustable part 202 may be other than straight , and it can be machined to have a curved or bowed outer surface for the purpose of stress distribution . therefore , the adjustable part 202 may have a straight , convex , or concave outer surface or the combination thereof . in an embodiment , the thickness of the adjustable part 202 is designed to be non - uniform . the thickness variation may help the adjustable part 202 expand to a desired geometry . the barrel 200 of an embodiment as illustrated in fig3 includes an adjustable part 202 with a thickest portion at the intermediate part 2021 which is between two thinner portions 2022 and 2023 . the location of the thickest portion may affect the stress distribution when the barrel 200 is under an external force . therefore , the stress distribution can be modified by changing the expansion geometry of the adjustable part 202 . fig4 a illustrates an embodiment with an adjustable part 202 with a thickest portion at the center of the intermediate part 2021 , allowing the adjustable part 202 to expand to a desired geometry , such as a symmetric or asymmetric cage , as shown in fig4 b . in another embodiment , the adjustable part 202 has a thickest portion at the intermediate part 2021 but closer to the securing part 201 , allowing the adjustable part 202 to expand to a crown - shaped object . those skilled in the art should realize that the arrangement of the thickest portion on the adjustable part 202 is not limited to the aforementioned embodiments . any non - uniform thickness design for the adjustable part is within the scope of the present disclosure , and although the aforementioned embodiments use a slotted pattern for illustration , a meshed design is also included . in another embodiment , the barrel 200 with a mesh - patterned hole adjustable part 202 may expand like a balloon or a lantern . referring to fig5 , an example of integration of the apparatus 10 is further described . in the apparatus 10 , the barrel 200 is designed to encase , enclose or envelope the device 100 . in an embodiment , the inner diameter of the securing part 201 is defined to be the same as or substantially the same as the outer diameter of the tube 120 . the outer diameter of the annulus 1101 is greater than the inner diameter of the adjustable part 202 . the device 100 is inserted or slid into the portion 2022 distal to the securing part 201 with the tapered , tube end 121 inserted first . the device 100 can be placed inside the barrel 200 until the portion 2022 hits the annulus 1101 . the tapered , tube end 121 with an outer diameter smaller than the inner diameter of the securing part 201 can move into the securing part 201 with less resistance . since the inner wall proximal to the tapered , tube end 121 is threaded , a handling gear ( not shown here ) with a threaded end can be screwed into the apparatus 10 from the securing part 201 of the barrel 200 . with the gear engaged , the apparatus 10 can be disposed to any desired location of a fractured or weakened bone during treatment . those skilled in the art should recognize that the handling gear can be any device or apparatus which is designed for the operator to screw into the apparatus 10 , and any variation or modification is within the scope and spirit of the disclosed embodiments . fig6 - 13 illustrate an embodiment of an expanding apparatus 30 according to the present invention and also refer to fig1 - 4 for the following description . the expanding apparatus 30 includes an outer tube 400 , which has a through hole 402 with a connection portion 403 . the connection portion 403 is corresponding to the securing part 201 , i . e . the securing part 201 can be inserted and fit into the connection portion 403 . at the other end , a base 405 is attached to the outer tube 400 with a hole in connection with the through hole 402 . the base 405 further includes a first pressing surface 406 . as described above , the apparatus of the present invention , as an implant , can be expanded with the expanding apparatus 30 , comprising an outer tube 400 , an inner coupling member or a packing 900 , a hollow body 500 , and a handle 600 . the outer tube 400 has the through hole 402 axially set within the outer tube 400 . the connection portion 403 is set at one end of the outer tube 400 and corresponding to the securing part 201 with a polygonal shape and chamfered at the edge thereof , and the securing part 201 can be inserted and fit into the connection portion 403 . the base 405 is attached to the other side of the outer tube 400 and includes the first pressing surface 406 . one end of the packing 900 forms a second pressing surface 901 against the first pressing surface 406 , and a recess 902 is set at the other end of the packing 900 . a third pressing surface 903 is formed at the both sides of the recess 902 . further , a first fitting hole 904 ( in an axial direction ), an outer rim 905 ( at the peripheral ) and a fitting portion 906 are set on the packing 900 . a second fitting hole 501 and a third fitting hole 502 are sequentially set at one end within the hollow body 500 , and a second inner thread 503 is set at the other end . an inner tube 510 is set at the third fitting hole 502 , a tunnel 511 is axially set within the inner tube 510 , a lock 512 is set at one side of the inner tube 510 , and a first external threaded portion 513 is set at the other side of the inner tube 510 . the first external threaded portion 513 is linked to the first threaded inner wall 125 of the apparatus ( implant ) 10 , and the inner tube 510 is sequentially fit into the first fitting hole 904 and the through hole 402 to fit the fitting portion 906 into the third fitting hole 502 , to fit the outer rim 905 into the second fitting hole 501 , and to embed the lock 512 into the recess 902 , to restrict the shift of the packing 900 only in the axial direction and not over the outer rim 905 on the hollow body 500 . a second external thread 601 is set outside the handle 600 . a steering portion 610 , a bearing or a component with similar mechanism , is connected to one side of the handle 600 , and a twisting portion 602 is set at the other side of the handle 600 in a wing shape , which is easy for twisting to the user . the second external thread 601 is connected to the second inner thread 503 , and the steering portion 610 forms a fourth pressing surface 611 . the method to use the expanding apparatus 30 can be summarized in the following steps : a ) connecting the connection portion 403 of the outer tube 400 to the securing part 201 , b ) rotating the hollow body 500 to thread the first external threaded portion 513 into the threaded inner wall 125 ; c ) adding an outer tube 710 as shown in fig1 and implanting the apparatus 10 into a part of damaged bone ( such as spine ) 700 ; d ) rotating the twisting portion 602 of the handle 600 while holding the hollow body 500 , making the fourth pressing surface 611 of the steering portion 610 press the third pressing surface 903 of the packing 900 , and also enabling the second pressing surface 901 of the packing 900 to push the first pressing surface 406 of the outer tube 400 ; and e ) continuingly twisting the twisting portion 602 of the handle 600 and pushing the apparatus 10 by the outer tube 400 , deforming the adjustable part 202 by the torque from the twisting portion 602 and making a press fit between the hole of the securing part 2011 and the tapered , tube end 121 . in the above description , the adjustable part 202 can form a curve with different gradients in the axial direction after expansion . in the above description , the handle 600 of the expanding apparatus 30 can be replaced by a container 800 for bone cement and an injecting handle 1000 to form an injector apparatus 60 . the container 800 includes a piston 810 and a shell 820 , and the piston 810 is movable in the axial direction and set within the shell 820 . an exit 821 is formed at one side of the shell 820 , and a room 822 is set within the shell 820 and connected to the exit 821 . the room 822 is useful for accommodating a material 830 , which is a mixture for reinforcing bone ( e . g ., bone cement ). a second external thread 1001 is formed outside the injecting handle 1000 , a chamber 1002 is set within one side of the injecting handle 1000 , and a twisting part 1003 is formed at the other side in a wing shape for twisting . the second external thread 1001 is linked to the second inner thread 503 . the container 800 is set at the chamber 1002 when the piston 810 is against the bottom of the chamber 1002 , and the exit 821 is connected to the tunnel 511 . the method to inject the material by using the aforesaid injector apparatus can be done by the following steps : a ) holding the hollow body 500 and twisting the twisting part 1003 or the injecting handle 1000 , making the bottom of the chamber 1002 to push the piston 810 and enable the material 830 in the room 822 sequentially delivered out the exit 821 , the tunnel 511 , the device 100 , the aperture 122 , the barrel 200 and the window of the barrel , and into the damaged bone 700 to - be - treated ; and b ) relieving the injecting handle 1000 , holding the base 405 of the outer tube 400 , simultaneously twisting in a reverse direction of the hollow body 500 , and ejecting the injection module . while the invention has been described above with references to specific embodiments thereof , it can be seen that many changes , modifications and variations in the materials , arrangements of parts and steps can be made without departing from the inventive concept disclosed herein . accordingly , the spirit and broad scope of the appended claims are intended to embrace all such changes , modifications and variations that may occur to one having skill in the art upon a reading of the disclosure . | 0 |
the present invention provides novel polymorphs of 5 - amino or a substituted amino 1 , 2 , 3 - triazole or their substituted amino 1 , 2 , 3 - triazoles ( cai ) prepared by a novel process and include a class of compounds of the formula i . the novel polymorphs of cai include , but are not limited to form 1 or form 2 as characterized by techniques such as nmr , dsc , ft - ir and xrdp . wherein p is 0 to 2 ; m is 0 to 4 ; and n is 0 to 5 ; x is o , s , so , so 2 , co , chcn , ch 2 or c ═ nr 6 where r 6 is hydrogen , lower alkyl , hydroxy , lower alkoxy , amino , lower alkylamino , dilower alkyl amino or cyano ; and , r 4 and r 5 are independently halogen ( f , cl , br ), cyano , trifluoromethyl , lower alkanoyl , nitro , lower alkyl , lower alkoxy , carboxy , lower carbalkoxy , trifluoromethoxy , acetamido , lower alkylthio , lower alkylsulfinyl , lower alkylsulfonyl , trichlorovinyl , trifluoromethylthio , trifluoromethylsulfinyl , or trifluoromethylsulfonyl ; r 2 is amino , mono or dilower alkyl amino , acetamido , acetimido , ureido , formamido , formimido or guanidino ; and r 3 is carbamoyl , cyano , carbazoyl , amidino or n - hydroxycarbamoyl ; wherein the lower alkyl , lower alkyl containing , lower alkoxy and lower alkanoyl groups contain from 1 to 3 carbon atoms . the 5 - amino or a substituted amino 1 , 2 , 3 - triazole compound is reacted with orotic acid , to form orotate compounds of 5 - amino or a substituted amino 1 , 2 , 3 - triazole compound in the ratio in the range of 1 : 1 to 1 : 4 ( base : acid ) by the improved and safer process of the invention to form ctos for use according to the methods of the present invention . the novel polymorphs of cai are further reacted with orotic acid to form orotate compounds of a class of compounds of the formula ii : wherein p is 0 to 2 ; m is 0 to 4 ; and n is 0 to 5 ; x is o , s , so , so 2 , co , chcn , ch 2 or c ═ nr 6 where r 6 is hydrogen , lower alkyl , hydroxy , lower alkoxy , amino , lower alkylamino , dilower alkyl amino or cyano ; and , r 4 and r 5 are independently halogen ( f , cl , br ), cyano , trifluoromethyl , lower alkanoyl , nitro , lower alkyl , lower alkoxy , carboxy , lower carbalkoxy , trifluoromethoxy , acetamido , lower alkylthio , lower alkylsulfinyl , lower alkylsulfonyl , trichlorovinyl , trifluoromethylthio , trifluoromethylsulfinyl , or trifluoromethylsulfonyl ; r 2 is amino , mono or dilower alkyl amino , acetamido , acetimido , ureido , formamido , formimido or guanidino ; and r 3 is carbamoyl , cyano , carbazoyl , amidino or n - hydroxycarbamoyl ; wherein the lower alkyl , lower alkyl containing , lower alkoxy and lower alkanoyl groups contain from 1 to 3 carbon atoms . the preferred embodiments of “ cto ” as defined herein , has the empirical formula of c 22 h 16 cl 3 n 7 o 6 , molecular weight of 580 . 76 . two transition melting points at 201 ° c . and 236 ° c . cto includes new polymorphs of cai ionically bonded orotic acid . cai has many polymorphs , including , but not limited to form 1 ( pattern 1 ) or form 2 ( pattern 2 ). the two embodiments of cto have different transition melting points , for example , cto ( form 1 , pattern 1 ) has melting points at about 136 ° c ., 194 ° c . and 235 ° c . ; and cto ( form 2 , pattern 2 ) has melting points at about 137 ° c . and 234 ° c . the two embodiments of cto have a 1 h nmr spectrum consistent with the structure cai : orotic acid ( fig1 and fig2 , respectively ) and ft - ir patterns consistent with form 1 and form 2 ( fig3 and fig4 , respectively ). cto is crystalline as shown by x - ray powder diffraction patterns for form 1 and form 2 ( fig5 and fig6 respectively ). an additional embodiment includes the formulation of different polymorphs of cai and orotic acid ( cao ). the new polymorphs of 5 - amino or a substituted amino 1 , 2 , 3 - triazole ( cai ) or 5 - amino or substituted amino 1 , 2 , 3 - triazoles are mixed with ortic acid in the range of 1 : 1 to 1 : 4 ( base : acid ) to provide formulations of cao use according to the methods of the present invention . the novel process of the invention wherein compounds of the invention can be prepared is shown in reaction scheme ii below in five ( 5 ) steps . more specifically , the novel process uses diphenylphosphoryl azide to react with intermediate 858 . b in step 3 instead of with sodium azide . it eliminates step 3 in prior art to form intermediate 858 . c . see scheme i above ( six steps ). the detailed processes are described in the examples . 858 . a through 858 . f represents intermediate products and cto as summarized below : 858 . a represents t - butyldimethylsilyl - 3 , 5 - dichlorobenzyl ether . 858 . b represents 3 , 5 - dichloro - 4 -( 4 - chlorobenzoyl ) benzyl alcohol . 858 . c represents 3 , 5 - dichloro - 4 -( 4 ′- chlorobenzoyl ) benzyl chloride . 858 . d represents 3 , 5 - dichloro - 4 -( 4 ′- chlorobenzoyl ) benzyl azide . 858 . e represents 5 - amino - 1 -( 4 -( 4 - chlorobenzoyl )- 3 , 5 - dichlorobenzyl )- 1 , 2 , 3 - triazole - 4 - carboxamide . 858 . f represents 5 - amino - 1 -( 4 -( 4 - chlorobenzoyl )- 3 , 5 - dichlorobenzyl )- 1 , 2 , 3 - triazole - 4 - carboxamide , compound with orotic acid , ( cai : orotic acid ) ( cai : orotate ) ( cto ). importantly , it has been observed that different polymorphs of cai , cto and cao manufactured by the above process exhibit less gastric lesions and toxicity in rodents when compared with cai which was synthesized by procedures described in prior art . this may be related to the absence of use of toxic ingredients such as sodium azide or potassium azide . the new process has also resulted in the production of new polymorphs of cai , cto and cao . thus , compounds of the invention include molecules that crystallize into more that one different crystal structure and exhibit different chemical properties of different polymorphs of cai as characterized by techniques such as nmr , dsc , ft - ir and xrdp ( fig1 to 6 ). 5 - amino or substituted amino 1 , 2 , 3 - triazoles as well as substitute derivatives thereof been manufactured into different polymorphs having chemical and biological properties that have overcome the disadvantages of cai produced by procedures described in prior art . in addition , 5 - amino or substituted amino 1 , 2 , 3 - triazole as well as substitute derivatives have been chemically reacted with orotic acid to form orotates ( cto ) in the ratio 1 : 1 to 1 : 4 ( base : acid , having unique bioavailability , pharmacokinetic properties , safety and effectiveness . an alternate embodiment includes polymorphs of 5 - amino or substituted amino 1 , 2 , 3 - triazoles as well as substitute derivatives thereof , mixed with orotic acid , in the ratio 1 : 1 to 1 : 4 ( base : acid ) to form formulations of cai and orotic acid ( cao ). the above pharmaceutical compositions and formulations may be formulated into pharmaceutical preparations for administration to mammals for prevention and treatment of primary and metastatic neoplasms , chronic myeloid leukemia , macular degeneration , retinopathies and other cell proliferative diseases . many of the triazole orotate compounds may be provided as organic acid salts directly or with pharmaceutically compatible counterions , a form in which they are merely water - soluble . salts tend to be more soluble in aqueous or other protonic solvents than are the corresponding free base forms . the therapeutic compounds or pharmaceutical compositions may be administered intravenously , intraperitoneally , subcutaneously , intramuscularly , intrathecally , orally , rectally , topically , or by aerosol . formulations suitable for oral administration include solid powder formulations , liquid solutions of the active compound dissolved in diluents such as saline , water or peg 400 ; capsules or tablets , each containing a predetermined amount of the active agent as solid , powder , granules or gelatin ; suspensions in an approximate medium ; and emulsions . formulations suitable for parenteral administration include aqueous and non - aqueous isotonic sterile solutions , which contain buffers , antioxidants and preservatives . the formulations may be in unit dose or multi - dose sealed containers . patient dosages for oral administration of cto range from 0 . 25 - 500 mg / day , commonly 25 - 100 mg / day , and typically from 50 - 400 mg / day . stated in terms of patient body weight , usual dosage range from 0 . 005 to 10 mg / kg / day , commonly from 0 . 5 - 2 . 0 mg / kg / day , typically from 1 . 0 to 8 . 0 mg / kg / day . stated in terms of patient body surface areas , usual dosage range from 0 . 1 - 300 mg / m 2 / day , commonly from 20 - 250 mg / m 2 / day , typically from 25 - 50 mg / m 2 / day . dosage amount and interval may be adjusted individually to provide plasma levels of the active moiety which are sufficient to maintain the anti - proliferative , anti - metastatic effects , antiangiogenic effects or other therapeutic effects in diseases which rely on aberrant signal transduction and proliferation . doses may be adjusted depending on the route of administration , for example for intravenous , for inhalation / aerosol , for direct intraperitoneal or subcutaneous , for topical or for intrathecal administrations . a variety of delivery systems for the pharmacological compounds may be employed , including , but not limited to , liposomes , nanoparticles , suspensions and emulsions . the pharmaceutical compositions also may comprise suitable solid or gel phase carriers or excipients . examples of such carriers or excipients include , but are not limited to , calcium carbonate , calcium phosphate , various sugars , starches , cellulose derivatives , gelatin , and polymers such as polyethylene glycols . furthermore , one may administer the drug in a targeted drug delivery system , for example , in a liposome coated with tumor - specific antibody , as nanoparticles and other forms . the liposomes or nanoparticles may be targeted to and taken up selectively by the tumor or other disease target . one of the most difficult properties to build into a newly discovered lead molecule is the desired pharmacokinetic profile , particularly in the case of orally dosed compounds . “ most experienced medicinal chemists would prefer to start in a structural series that has inherently good pharmacokinetic properties , albeit with poor potency on the target receptor , and then set about improving the potency on the target , rather than working in the other direction ”, “ organic chemistry in drug discovery , drug discovery ”, science 303 : 1810 - 1813 ( 2004 ). the present invention relates generally to the method of increasing the oral bioavailability , delivery and clearance of cto , a unique orotate of l651582 in the ratio 1 : 1 : to 1 : 4 ( base : acid ). the present invention provides processes to prepare orotate salts of water - insoluble drugs having an ionizable center , to improve the drugs &# 39 ; oral bioavailability , toxicology profile and efficacy . preferably the cto is in the ratio 1 : 1 and more preferably it is in the ratio 1 : 2 and most preferably it is in the ratio 0 . 7 : 1 . 3 . the absorption of drugs via the oral route is a subject of intense investigation in the pharmaceutical industry since good bioavailability implies that the drug is able to reach the systemic circulation by mouth . oral absorption is affected by both the drug properties and the physiology of the gastrointestinal tract , including drug dissolution from the dosage form , the manner in which the drug interacts with the aqueous environment and membrane , permeation across the membrane and irreversible removal by first - pass organs such as the intestine , liver and lung . some pharmaceutical agents that exhibit low - solubility show poor bioavailability or irregular absorption , the degree of irregularity being affected by factors such as dose level , fed state of the patient , and physicochemical properties of the drug . the majority of drug absorption occurs at the small intestine because of the large surface area since the presence of the villi and microvilli increases the absorptive area manifold . the circulation of the intestine is unique in that the intestine is the anterior or portal tissue that regulates the flow of substrates to the liver . the intestinal venous blood constitutes about 75 % of the blood supply to the liver . therefore , for drugs that are highly cleared by the intestine , the contribution of the liver , kidney or lung to drug metabolism will become reduced . conversely , for drugs that are poorly extracted by the intestine , the substrate is able to reach the next organs , the liver and the lung for removal . therefore , the concentration of drug entering the intestine and the intestinal flow rate alter the rate of drug delivery and affect the rates of intestinal and clearance through hepatic first - pass metabolism . “ drug bioavailability ” is defined here as the amount of drug systemically available over time . the present invention increases drug bioavailability of pharmaceutical agents by converting them into orotate salts . this may be achieved by altering the hydrophilic and lipophilic properties of the drug so that the drug permeates the membrane wall and blood perfusion rate becomes the overall rate - limiting step for absorption , or by inhibiting drug biotransformation in the gut and / or by inhibiting active back transport systems in the gut that decrease the net transport of drugs across the gut membrane into the blood stream . in either case , the composition responsible for increased drug bioavailability is the orotate salt of the pharmaceutical agent . for reasons that are not immediately apparent , it has been discovered that conversion of a water - insoluble l651582 into cto ( base : acid , 0 . 5 : 1 to 1 : 2 ) provides a method for increasing the bioavailability of an orally administered pharmaceutical agent to a mammal in need of treatment . changes in the integrated systemic concentrations overtime are indicated by area under the curve ( auc ) or c max , both parameters well known in the art . the present invention provides methods wherein a composition provides an increase in bioavailability of the orotate salt of the pharmaceutical agent as measured by auc of at least 25 % to 100 % relative to dosing of the pharmaceutical agent . the invention provides a composition that increases the bioavailability of the orotate salt of the pharmaceutical agent as measured by cmax of at least 50 % to 100 % “ side effects ” or “ toxicity ” or “ adverse drug reactions ” of chemotherapeutic agents are observed in the acute phase of chemotherapy administration and in patients cured of the cancer with subclinical tissue damage . there is a higher recognition of drug - related tissue side effects which may be quite severe , disabling and irreversible . the clinician must be aware of the potential tissue / organ complications of chemotherapeutic agents and where appropriate perform a baseline tissue examination before initiating the therapy . “ clearance ” of drug occurs by perfusion of blood to the organs of extraction . “ extraction ” refers to the proportion of drug presented to the organ which is removed irreversibly ( excreted ) or altered to a different chemical form ( metabolism ). the present invention provides a method to increase clearance of the orotate derivatives of cto from noncancerous or normal tissues as measured by pharmacological studies at least 25 % to 100 % relative to dosing of the pharmaceutical agent . “ bioavailability ” of a drug following oral dosing is the extent to which or rate at which the active moiety of the drug or metabolite enters systemic circulation , thereby gaining access to the site of action . the physiochemical properties of a drug govern its absorptive potential , and binding to serum proteins . the efficacy of the drug depends on its interaction with the molecular target . therefore , the properties of the dosage form which partly depend on its chemical characteristics and on processes for manufacture of the drug in bulk quantities . differences in bioavailability , efficacy , transport and clearance among chemical formulations of a given drug can have clinical significance . “ absorption ” rate is important because even when a drug is absorbed completely , it may be absorbed too slowly to produce a therapeutic blood level quickly enough or so rapidly that toxicity results from high drug concentrations given to achieve the therapeutic level after each dose . absorption occurs by one of three methods , either passive diffusion , active transport or facilitated active transport . passive diffusion is simply the passage of molecules across the mucosal barrier until the concentration of molecules reaches osmotic balance on both sides of the membrane . in active transport the molecule is actively pumped across the mucosa . in facilitated transport , a carrier generally a protein , is required to convey the molecule across the membrane for absorption . the present invention provides cto compounds in chemical configurations that permit the drug to be delivered successfully to different tissues and organs and even cross the blood brain barrier , to reach the brain . orotic acid , a free pyrimidine is important in the synthesis of uridylate ( upp ) a major pyrimidine nucleotide . pyrimidines play a central role in cellular regulation and metabolism . they are substrates for dna / rna biosynthesis , regulators of the biosynthesis of some amino acids , and cofactors in the biosynthesis of phospholipids , glycolipids , sugars and polysaccharides . the classical de novo pyrimidine biosynthetic pathway ends with the synthesis of ump . biochemistry , ed . lubert stryer , ed , w . h . freeman & amp ; co ny , 4 th ed , 739 - 762 ( 1995 ). the present invention provides a class of ctos that undergo dissolution to release the drug as a charged molecule and free orotic acid , which may prevent binding of the drug to proteins and facilitate transport to the target and rapid clearance . the invention provides embodiments showing increase in effectiveness of the cto as measured by improvement in 1 ) efficacy of cto compared with formulation of equivalent dose of cai + orotic acid , 2 ) bioavailability and clearance of cto when given as encapsulated solid cto compared to cto in peg - 400 , 3 ) transport of orally administered cto to the brain through the blood brain barrier , 4 ) transport of orally administered cto to different eye tissues , including the choroid - retina complex and vitreous humor in dogs . importantly , the preclinical toxicity of cto was determined in dogs by the po route at 175 , 350 , 1025 mg / kg / day and no deaths occurred after 28 days . 3 , 5 - dichlorobenzyl alcohol ( 1 mole ) is treated with tert - butyldimethylsilyl chloride ( 1 . 05 mole ), imidazole , 99 % ( 2 . 44 mole ), 4 - dimethylaminopyridine in n , n - dimethylformamide at cold temperature to produce t - butyldimethylsilyl - 3 , 5 - dichlorobenzyl ether ( 858 . a1 ) at the extraction work - up . react t - butyldimethylsilyl - 3 , 5 - dichlorobenzyl ether ( 858 . a1 ) ( 1 mole ) with n - butyllithium 1 . 6m solution in hexane followed by 4 - chlorobenzoyl chloride , ( 1 . 01 mole ), in tetrahydrofuran , while cold and treat the intermediate with aqueous hydrochloric acid to give 3 , 5 - dichloro - 4 -( 4 - chlorobenzoyl ) benzyl alcohol ( 858 . b ). 3 , 5 - dichloro - 4 -( 4 - chlorobenzoyl ) benzyl alcohol ( 858 . b ) ( 1 mole ) is reacted with diphenylphosphoryl azide ( diphenylphosphonic azide ) ( dppa ) ( 1 . 2 mole , and 1 , 8 - diazabicyclo [ 5 . 4 . 0 ] undec - 7 - ene , ( synonym : dbu ) ( 1 . 2 mole )) in toluene at cold temperature , followed by aqueous work - up and alcohol titration , to give 3 , 5 - dichloro - 4 -( 4 ′- chlorobenzoyl ) benzyl azide ( 858 . d ). dppa is an organic compound that is used in the synthesis of other organic compounds . aust . j . chem 26 : 1591 - 1593 ( 1973 ). the stability of dppa towards heating is shown by its distillation at 157 ° c . and by the fact that vigorous evolution of nitrogen is not observed until a temperature of 175 ° c . is reached . 3 , 5 - dichloro - 4 -( 4 ′- chlorobenzoyl ) benzyl azide ( 858 . d ) ( 1 mole ) is reacted with cyanoacetamide ( 1 . 69 mole ) in hot acetonitrile , and potassium carbonate , ( 6 . 2 mole ) to give 5 - amino - 1 -( 4 -( 4 - chlorobenzoyl )- 3 , 5 - dichlorobenzyl )- 1 , 2 , 3 - triazole - 4 - carboxamide ( 858 . e ). 5 - amino - 1 -( 4 -( 4 - chlorobenzoyl )- 3 , 5 - dichlorobenzyl )- 1 , 2 , 3 - triazole - 4 - carboxamide ( 858 . e ) ( 1 mole ) is reacted with orotic acid ( 1 . 03 mole ) and methanol / water mixture to give 5 - amino - 1 -( 4 -( 4 - chlorobenzoyl )- 3 , 5 - dichlorobenzyl )- 1 , 2 , 3 - triazole - 4 - carboxamide , solid compound with orotic acid , ( cai : orotic acid ; 1 : 1 ) ( cto ) ( 858 . f ), mw 580 . 76 g , having transitional melting points of about 151 ° c ., 238 ° c . and 332 ° c ., measured by differential scanning calorimetry . the xrpd pattern indicates that the cto is composed of crystalline and amorphous ( polymorphic ) material . the effect of cto m . w . of 580 . 8 and cai m . w . of 424 . 6 + orotic acid m . w . of 156 . 1 , was studied in s . c .- implanted ht29 human colon tumor xenografts in male , athymic ncr - nu / nu mice . 6 week old mice were implanted with ht29 fragments and 13 days later were sorted in 3 groups of ten . for the next 14 days ( 13 - 26 days ), group 1 control ( c ) received the vehicle ; group 2 = 343 mg / kg / dose ; group 3 = 240 mg / kg / day cai + 103 mg / kg / day orotic acid . at 41 days , the mean tumor volume ( mm 3 ) was measured as shown below : group 1 ( control )= 1436 mm 3 group 2 ( cto 343 mg / kg / day )= 864 mm 3 ( p = 0 . 0050 , gr2 vs gr 1 ) group 3 ( cai 250 mg / kg / day + orotic acid 103 mg / kg / day )= 1268 mm 3 ( p = 0 . 2706 , gr 3 vs gr 1 ). these results suggest that cto is more effective in inhibiting tumor growth than an equivalent amount of cai and orotic acid that are not chemically reacted . however , cai + orotic acid formulation did show some tumor inhibition . comparison of cto given orally as solid in capsule or as liquid in peg - 400 the bioavailability of cto ( base : acid , 0 . 7 : 1 . 3 ) was determined by administering a single dose 685 mg / kg by capsule ( group 1 ) or by oral gavage in peg400 ( group 2 ). two dogs ( 1f / 1m ) were used in each group . blood samples were collected at 0 , 1 , 2 , 4 , 8 , 12 , 24 , 48 , 72 , and 92 hours . cai was measured by hplc / ms . group 1 receiving capsule : plasma concentrations after 1 hr were 155 and 174 ng / ml for male and female dogs . c max was 5800 ng / ml at 12 hrs for male and 7950 ng / ml at 24 hrs for female . half life was 18 hr and 22 . 7 hr and auc values were 326 and 277 ug / ml , for male and female respectively . group 2 receiving gavage in peg400 : plasma concentrations after 1 hr were 511 and 570 ng / ml for male and female dogs . c max was 6634 ng / ml at 24 hrs for male and 5350 ng / ml at 24 hr for female . bioavailability was 81 . 8 % of that in group 1 ( 100 %). these results show that cto given as solid in capsule had a better absorption pattern and bioavailability than cto in peg400 . based on these and additional results , cto will be administered as solid in capsules to patients . cto was given orally ( in peg400 ) to six week old mice sorted in two groups of 6 . two doses were administered — group 1 = 513 mg / kg ; group 2 = 342 mg / kg . eight hours after treatment with cto , the mice were euthanized for measurement of cto concentration ( as cai ) in brain tissue . results obtained were : group 1 - cai levels were 15167 ± 2372 ng / g tissue ; group 2 levels of cai were 10950 ± 1704 ng / g tissue , both in the therapeutic range ( 6000 ng / ml ). since the cto was administered orally , these results indicate that cto crosses the blood brain barrier and reaches the target organ , brain . the present invention is not to be limited in scope by the embodiment disclosed in the example which is intended as an illustration of one aspect of the invention and any methods which are functionally equivalent are within the scope of the invention . indeed , various modifications of the invention in addition to those shown and described herein will become apparent to those skilled in the art from the foregoing description . such modifications are intended to fall within the scope of the appended claims . those skilled in the art will recognize , or be able to ascertain using no more than routine experimentation , any equivalents to the specific embodiments of the invention described herein . such equivalents are intended to be encompassed by the claims . | 2 |
aside from the preferred embodiment or embodiments disclosed below , this invention is capable of other embodiments and of being practiced or being carried out in various ways . thus , it is to be understood that the invention is not limited in its application to the details of construction and the arrangements of components set forth in the following description or illustrated in the drawings . if only one embodiment is described herein , the claims hereof are not to be limited to that embodiment . moreover , the claims hereof are not to be read restrictively unless there is clear and convincing evidence manifesting a certain exclusion , restriction , or disclaimer . there is shown in fig1 one process flow diagram 10 according to this invention , which begins with the air flow in 12 to a particle counter 14 which may include a filter 16 that filters out large particles above some size , for example 10 microns . the air is then submitted to the particle counter 18 . if the particle count is below a certain level , no further action is taken ; if it is above a certain level then a collection apparatus 20 is actuated . the collection apparatus may include a linear virtual impactor which receives the air on a substrate and collects particles ; it also pre - concentrates particles in the correct size range . this results in a major and minor air flow . the major portion of the air flow , after passing through the linear virtual impactor or other collection apparatus , exits as indicated at the air flow out 22 . there may be a particle counter ambient threshold detector 24 . this is used to keep track of the ambient particle count as it varies during the day and from day to day and week to week so that the particle count at 18 can be more accurate . for example , if there were construction going on during the day in an airport where this device was installed the particulate matter in the air during the day might be very high and so the high particle count would exceed its threshold every time , which would not be an accurate representation . in that case the particle counter ambient threshold detector 24 would note a raised ambient level which can then be used to adjust the threshold high particle count . practically , the threshold is set at some percentage of the ambient particle level . a typical count in a typical ambient condition , would be , for example , 100 particles per liter of air in the 1 - 10 micron size range ( respirable size range ). once the collection apparatus 20 has been actuated a portion of the flow , the minor flow , is directed as indicated at 26 so that the substrate containing the sample of particles 28 is submitted now to a uv detector 30 . uv detector 30 may seek to detect the fluorescence back - scatter of the particles in a particular wavelength range , for example , 300 - 500 nm , but it not limited to this range , with a uv excitation wavelength of , for example , 365 nm , but is not fixed at this value . if the uv fluorescence threshold for the sensitivity of the sample is not met 32 no further action may be taken as indicated at 34 and the substrates will be referred back for cleaning . the uv threshold sensitivity may be , for example some number of photons above the background response of the substrate . if the threshold is met then in this embodiment the ir spectral absorption of the particles on the sample is measured either in reflection or transmission 36 . the particular ir wavelength range shown in fig1 is 5 . 5 - 11 um , but the detector may operate anywhere between 2 . 5 and 100 um , but is not limited to this range and can be any appropriate range in the infrared spectrum . the ir threshold response for the sample particles , may be for example , based on a degree of “ matching ” or correlations between the sample absorption spectrum and target threat absorption spectrum , both of which are normalized / corrected so as to take amplitude or offset out of the equation . typically , a reliable decision or correlation requires a sample of approximately 1 , 000 particles . if the ir threshold is not met 38 , then the system may at this time take no further action as at 40 and the substrates will be referred back for cleaning . if it is met then a threat may be detected 42 and if it is a threat , an alarm is triggered 44 . if no threat was detected the substrates are cleaned of all sample particles 46 and the collection apparatus returns to its quiescent state . in fig1 the particle count is the first screening . if the particle count threshold is not reached then no uv detection is effected . the uv detection actually functions as a second screen for if the uv detection does not find the particle sample sensitivity to be above a certain threshold the ir spectroscopy will not occur . in another embodiment , however , as shown in fig2 , process flow diagram 10 a is essentially the same except for the portion following the collection of the particles 28 . in flow process diagram 10 a after the collection of the particles on the substrate 28 both the uv detection 30 and ir detection 36 are instituted simultaneously , then the output on each is checked to see whether the uv threshold 50 has been met in one case and the ir threshold 52 has been met in the other . if both thresholds have been met then and gate 54 will pass the information to the threat detection operation 42 which will trigger a threat alarm 44 . if both thresholds are not met , and gate 54 does not provide the affirmative signal , so a threat is not detected 42 , no further action is taken and the substrates will be referred for cleaning 46 . a pumping system provides both the major air flow through the particle counter and the linear virtual impactor collector and the minor flow through the collection apparatus . the pumping system may include a pump for each . a flow chart 100 depicting the method of the invention is shown in the fig3 . this description begins with the particle count 102 . if the particle count does not meet or exceed the threshold 104 the system returns to the particle count operation 102 . if it does exceed the threshold a pump is actuated 106 to begin the flow to the linear virtual impactor to accumulate the sample particles on the substrate . the particle counter that does the particle counting 102 typically has its own internal pump , which is operating continuously . once the pump is activated the collection apparatus is also actuated 108 and the particles are collected on a substrate 110 . the collection apparatus then moves the substrate to a first station for uv analysis 112 . if no threat is detected there 114 the substrate is cleaned 116 and referred back to the particle count operation 102 . if a threat is detected then an inquiry is made as to whether the particle count is sufficient for an ir analysis 118 ; if not additional particles are collected 120 and then an ir analysis is done 122 . if the ir analysis indicates a sensitivity of the sample particles above a certain threshold 124 then a threat alarm is triggered 126 ; if not the system refers on line 128 to clean the substrate 116 and return to the particle count operation 102 . a schematic block diagram of the system according to this invention is shown in fig4 including a particle counter 150 which has its own pump 152 , a system pump 154 and a uv detector unit 156 including a uv source 158 and uv detector 160 . typically , this is a reflective detector . also shown is the ir detector unit 162 including an ir source 164 , an ir detector 166 and ir analyzer 168 . the analyzer may be a spectrometer which measures sample absorbance at the desired frequencies to identify whatever contaminates or constituents the system is set to detect in aerosols . the collection apparatus 170 includes a linear actuator or other device which can move a substrate from a collection point , where , for example , the linear virtual impactor can load the sample particles onto a substrate and then the linear actuator moves the substrate to the uv detector unit 156 and the ir detector unit 162 . the entire system 148 is operated by controller 171 which may be a pc , for example . controller 171 monitors particle counter 150 . if the particle count goes above a particular threshold it turns on the pump and operates collection apparatus 170 to bring a substrate in front of the impaction nozzle being supplied by pump 154 , where upon a number of sample particles are collected on to the substrate from the air for a predetermined duration dependent on the inlet concentration . controller 171 now moves collection apparatus to bring the substrate to the uv detector unit 156 and the ir detector unit 162 . it monitors the output of both the uv 156 and ir 162 detector units . if both units find a response in the sample particles above some threshold level the controller determines that a threat alarm is necessary as indicated previously with respect to fig1 , for example . the uv detection unit having met its threshold may be a precondition to the operation of ir detection unit 162 or they may both be operated simultaneously and a threshold - met indication from both may be required to produce a threat alarm . in one particular embodiment the system 148 a , fig5 is implemented using aerosol particle counter 150 mounted on a housing base 180 along with the other components . particle counter 150 has an inlet 202 for inducting air and a collection apparatus 170 including linear actuator 182 which moves the substrate 184 in a removable holder from the particle deposition nozzle 186 to the uv detector unit 156 and the ir detector unit 162 . an auxiliary pump 188 is provided for the minor flow while the pump 152 , fig4 , provides the flow for the particle counter . the optical particle counter 150 flow and major flow have to be independent : the counter 150 flow is always on , while the major flow for the linear virtual impact collector is supplied by pump 154 . the uv detector unit 156 includes both the source 158 and detector 160 . the ir detector unit 162 includes an infrared spectrometer 190 and an infrared transmission microscope 192 . the infrared source appears at 194 . although specific features of the invention are shown in some drawings and not in others , this is for convenience only as each feature may be combined with any or all of the other features in accordance with the invention . the words “ including ”, “ comprising ”, “ having ”, and “ with ” as used herein are to be interpreted broadly and comprehensively and are not limited to any physical interconnection . moreover , any embodiments disclosed in the subject application are not to be taken as the only possible embodiments . in addition , any amendment presented during the prosecution of the patent application for this patent is not a disclaimer of any claim element presented in the application as filed : those skilled in the art cannot reasonably be expected to draft a claim that would literally encompass all possible equivalents , many equivalents will be unforeseeable at the time of the amendment and are beyond a fair interpretation of what is to be surrendered ( if anything ), the rationale underlying the amendment may bear no more than a tangential relation to many equivalents , and / or there are many other reasons the applicant can not be expected to describe certain insubstantial substitutes for any claim element amended . other embodiments will occur to those skilled in the art and are within the following claims . | 6 |
“ 500 mg or 1000 mg ” as used herein , means the strength of tablet composition containing 500 mg clarithromycin , or the dose administered as 2 × 500 mg of clarithromycin , respectively . “ c max ” as used herein , means maximum plasma concentration of the erythromycin derivative , produced by the ingestion of the composition of the invention or the ir comparator . “ c min ” as used herein , means minimum plasma concentration of the erythromycin derivative , produced by the ingestion of the composition of the invention or the ir comparator . “ c avg ” as used herein , means the average concentration within the 24 - hour interval . “ t max ” as used herein , means time to the maximum observed plasma concentration . “ auc ” as used herein , means area under the plasma concentration - time curve , as calculated by the trapezoidal rule over the complete 24 - hour interval for all the formulations . “ degree of fluctuation ( dfl )” as used herein , is expressed as : dfl =( c max − c min )/ c avg . “ erythromycin derivative ” as used herein , means erythromycin having no substituent groups , or having conventional substituent groups , in organic synthesis , in place of a hydrogen atom of the hydroxy groups and / or a methyl group of the 3 ′- dimethylamino group , which is prepared according to the conventional manner . “ pharmaceutically acceptable ” as used herein , means those compounds which are , within the scope of sound medical judgment , suitable for use in contact with the tissues of humans and lower animals without undue toxicity , irritation , allergic response , and the like , in keeping with a reasonable benefit / risk ratio , and effective for their intended use in the chemotherapy and prophylaxis of antimicrobial infections . “ adverse effects ” as used herein , means those physiological effects to various systems in the body such as cardiovascular systems , nervous system , digestive system , and body as a whole , which cause pain and discomfort to the individual subject . “ taste perversion ” as used herein , means the perception of a bitter metallic taste normally associated with the erythromycin derivatives , particularly , with clarithromycin . the pharmaceutical composition of the invention comprise a pharmaceutically active compound and a pharmaceutically acceptable polymer . the pharmaceutically active compound is an erythromycin derivative . preferably , the erythromycin derivative is 6 - o - methoxy erythromycin a , known as clarithromycin . the amount of the erythromycin derivative varies from about 45 % to about 60 % by weight of the composition . preferably , the composition comprises about 50 % by weight of the erythromycin derivative . the pharmaceutically acceptable polymer is a water - soluble hydrophilic polymer selected from the group consisting of polyvinylpyrrolidine , hydroxypropyl cellulose , hydroxypropylmethyl cellulose , methyl cellulose , vinyl acetate / crotonic acid copolymers , methacrylic acid copolymers , maleic anhydride / methyl vinyl ether copolymers and derivatives and mixtures thereof . preferably , the polymer is selected from hydroxypropyl cellulose , hydroxypropylmethyl cellulose , and methyl cellulose . more preferably , the polymer is hydroxypropylmethyl cellulose . most preferably , the polymer is a low viscosity hydroxypropyl - methyl cellulose with viscosity ranging from about 50 cps to about 200 cps . the most preferred low viscosity polymer is a hydroxypropylmethyl cellulose with a viscosity of about 100 cps , commercially available under the tradename methocel ™ k 100 lv from the dow chemical company . the amount of the polymer in the composition generally varies from about 5 % to about 50 % by weight of the composition . preferably , the amount of polymers varies from about 10 % to about 35 % by weight of the composition . most preferably , the amount of polymer varies from about 10 % to about 30 % by weight of the polymer . the composition of the invention further comprise pharmaceutically acceptable excipients and / or fillers and extenders , such as lactose , starches , glucose , sucrose , mannitol , and silicic acid , lubricants such as talc , calcium stearate , magnesium stearate , solid polyethylene glycols , sodium lauryl sulfate , and mixtures thereof . the amount of the lubricants generally varies from about 0 . 5 % to about 10 % by weight of the composition . preferably , the lubricants used are magnesium stearate and talc in the total amounts ranging from about 1 . 0 % to about 4 . 0 % by weight of the composition . the amount of fillers and extenders varies from about 10 % to about 40 % by weight of the composition . a particularly preferred composition for the extended release of the active compound therefrom comprises : the formulations are generally prepared by dry blending the polymer , filler , erythromycin derivative , and other excipients followed by granulating the mixture using water until proper granulation is obtained . the granulation is done by methods known in the art . the wet granules are dried in a fluid bed dryer , sifted and ground to appropriate size . lubricating agents are mixed with the dried granulation to obtain the final formulation . the compositions of the invention can be administered orally in the form of tablets , pills , or suspensions . the tablets can be prepared by techniques known in the art and contain a therapeutically useful amount of erythromycin derivative and such excipients as are necessary to form the tablet by such techniques . tablets and pills can additionally be prepared with enteric coatings and other release - controlling coatings for the purpose of light protection , and swallowability . the coating may be colored with a pharmaceutically accepted dye . the amount of dye and other excipients in the coating liquid may vary and will not impact the performance of the extended release tablets . the coating liquid generally comprises film - forming polymers such as hydroxy - propyl cellulose , hydroxypropylmethyl cellulose , cellulose ester or ether , an acrylic polymer or a mixture of polymers . the coating solution is generally an aqueous solution further comprising propylene glycol , sorbitan monoleate , sorbic acid , fillers such as titanium dioxide , a pharmaceutically acceptable dye . liquid dosage forms for oral administration may include pharmaceutically acceptable emulsions , microemulsions , solutions , suspensions , syrups and elixirs containing inert diluents commonly used in the art such as water . such compositions may also comprise adjuvants , such as wetting agents ; emulsifying and suspending agents ; and sweetening , flavoring and perfuming agents . the daily dose of the composition of this invention administered to a host in single dose can be in the amounts from 500 mg to 1000 mg once a day for five to fourteen days . the bioavailability study for the formulations of the invention can be done by administering the er formulation in a tablet form to healthy subjects and measuring the levels of erythromycin derivative in the plasma at different time intervals over a period of twenty four hours . plasma samples are assayed for erythromycin derivative at bas analytics ( west lafayette , ind .) using a validated high - performance liquid chromatographic procedure similar to that described in the literature . see for example , chu sy , et al ., “ simultaneous determination of clarithromycin and 14 ( r )- hydroxyclarithromycin in plasma and urine using high - performance liquid chromatography with electrochemical detection ”, j . chromatog ., 571 , pp 199 - 208 ( 1991 ). adverse effects including those related to the digestive system , nervous system , respiratory system and special senses , including taste perversion , are measured by dosing subjects with multiple doses of 1000 mg of er and ir tablets per day , respectively . the adverse effects are monitored , reported spontaneously by subjects and recorded on case report forms for the study database . the invention will be understood more clearly from the following examples , which are given solely by way of illustration and serve to provide a clear understanding of the invention and to illustrate its different embodiments as well as its various advantages . methocel ™ ( k 100 lv ) available from the dow chemical company was loaded into a mixer , and dry blended with clarithromycin . the mixture was granulated using water until proper granulation was obtained . the granulation was then dried , sifted and ground to appropriate size . talc and magnesium stearate were screened and blended with dry granulation . the granulation was then loaded into hopper and compressed into tablets . the tablets were then coated with an aqueous coating . three different formulations a , b , and c were prepared according to the general method described above . the compositions of three different tablet formulations are given below in table 1 . the bioavailability study to determine the concentration - time plasma profile was done on healthy subjects . the study was conducted as a phase i , single - dose , open , randomized , four - period , balanced crossover study described below . twenty - four ( 24 ) healthy adult subjects were enrolled and 23 completed all phases of the study . for the 23 subjects who completed all phases of the study ( 12 males , 11 females ), the mean age was 29 years ( range : 19 to 49 years ), the mean weight was 69 . 0 kg ( range : 51 . 5 to 85 kg ) and the mean height was 172 cm ( range : 157 to 192 cm ). clarithromycin 500 mg extended release tablets corresponding to the formulations a , b , and c of example 1 and the 500 mg ir clarithromycin tablet ( reference formulation ), currently sold by abbott laboratories under the tradename biaxin ™, were administered to the 23 healthy subjects . the study was conducted according to a single - dose , open - label , randomized four - period crossover design in which each subject received a single 500 mg dose of clarithromycin during each 30 minutes period after starting breakfast . wash - out periods of one week separated the doses . seven ( 7 ) ml blood samples were collected prior to dosing ( 0 hour ) and at 0 . 5 , 1 . 0 , 2 . 0 , 3 . 0 , 4 . 0 , 6 . 0 , 8 . 0 , 12 . 0 , 16 . 0 , 24 . 0 , 36 . 0 and 48 . 0 hour after each dose . plasma samples were assayed for clarithromycin at bas analytics ( west lafayette , ind .) using a validated high performance liquid chromatographic procedure . values for clarithromycin pharmacokinetic parameters , including observed c max , t max , and auc 0 -∞ , were calculated using standard noncompartmental methods . the mean plasma concentration - time profiles for the single - dose study are illustrated in fig1 . [ 0056 ] fig1 illustrates that all the three formulations of the invention are substantially equivalent in extended release of clarithromycin over a period of 24 hours . table ii summarizes the pharmacokinetic results obtained after single - dosing in the above study . table ii auc 0 - ∞ formulation cmax ( μg / ml ) t max ( h ) ( μg · h / ml a 1 . 19 ± 0 . 60 * 5 . 0 ± 1 . 7 * 15 . 0 ± 6 . 5 * b 1 . 33 ± 0 . 70 *# 5 . 5 ± 2 . 4 * 15 . 1 ± 6 . 5 * c 1 . 01 ± 0 . 48 * 5 . 5 ± 2 . 2 * 14 . 8 ± 7 . 5 * reference tablet 2 . 57 ± 0 . 70 2 . 2 ± 0 . 5 17 . 7 ± 5 . 6 for c max , auc 0 -∞ , t max , and the logarithms of c max , and auc 0 -∞ , an analysis of variance ( anova ) was performed with sequence , subject nested within sequence , period and formulation as the sources of variation . effects for subjects were random and all other effects were fixed . within the framework of anova , the formulations were compared pairwise , with each test at a significance level of 0 . 05 . also within the framework of the anova for the logarithm of auc 0 -∞ , bioequivalence of the er formulations to the ir reference formulation was assessed using the two one - sided tests procedure via 90 % confidence intervals . the confidence intervals were obtained by exponetiating the endpoints of the confidence intervals for the difference of logarithm means . point estimates of relative bioavailability and 90 % confidence intervals for the two one - sided tests procedure from analysis of log - transformed auc 0 -∞ are set forth in table iii below . table iii relative bioavailability formulation comparison point estimate 90 % confidence interval a vs reference 0 . 815 0 . 737 - 0 . 902 b vs reference 0 . 835 0 . 755 - 0 . 925 c vs reference 0 . 787 0 . 711 - 0 . 871 the auc 0 -∞ central values were lower for the three er formulations than for the reference ir tablet . the lower c max values and the later t max values suggest that all the er formulations with varying weight percent of polymer , provide extended - release of clarithromycin in vivo . the lower auc 0 -∞ values for the er formulations may suggest that for a single 500 mg dose administered under nonfasting conditions , the extent of absorption of clarithromycin was reduced relative to that of the reference ir tablet . twenty - four ( 24 ) healthy adult subjects were enrolled and 23 completed all phases of the study . of the 23 who completed the study ( 19 males , 4 females ), the mean age was 30 years ( range : 20 to 47 years ), the mean weight was 72 kg ( range : 51 to 87 kg ) and the mean height was 176 cm ( range : 159 to 189 . 5 cm ). the clarithromycin dosage forms included 500 mg er tablets of example 1 containing 10 % or 20 % by weight of k 100 lv , respectively , and a reference 500 mg ir tablet ( biaxin ). the study was conducted according to a single - and multiple - dose , open - label , randomized three - period crossover design . a single 1000 mg dose of er formulation a tablets ( two 500 mg tablets ) was administered in the morning on day 1 . beginning on day 3 , a multiple dose regimen of 1000 mg clarithromycin ( two 500 mg tablets ) was administered each morning for three days ( days 3 - 5 ). a single 1000 mg dose of er formulation b tablets ( two 500 mg tablets ) was administered in the morning on day 1 . beginning on day 3 , a multiple dose regimen of 1000 mg clarithromycin ( two 500 mg tablets ) was administered each morning for three days ( days 3 - 5 ). a single 500 mg dose of ir tablet ( biaxin ) was administered in the morning on day 1 . beginning on day 3 , a multiple dose regimen of 500 mg reference tablet biaxin was administered every twelve hours for three days . each morning dose was administered thirty minutes after breakfast . every evening dose was administered thirty minutes after starting the evening snack . wash - out periods of at least one week separated the last dose in a period and the first dose in the following period . seven ( 7 ) ml blood samples were collected before dosing on day 1 ( 0 hr ) and at 0 . 5 , 1 . 0 , 2 . 0 , 3 . 0 , 4 . 0 , 6 . 0 , 8 . 0 , 12 . 0 , 16 . 0 , 24 . 0 , 36 . 0 , and 48 . 0 hour after dosing . for regimen c , the 12 hour sample was collected within 5 minutes before the evening dose on day 5 . plasma harvested from each blood sample was divided into two parts : approximately 5 ml for bioassay and the remainder of the sample for high performance liquid chromatographic ( hplc ) assay . plasma samples were assayed for clarithromycin at bas analytics ( west lafayette , ind .) using a validated high performance liquid chromatographic procedure . pharmacokinetic parameter estimates were calculated using noncompartmental methods . for the day 1 data , the parameters estimated included c max , t max , auc 0 -∞ or auc 0 - 48 , and t 1 / 2 . for the day 5 data , the parameters estimated included c max , t max , c min , auc 0 - 24 , and dfl . no statistical analyses were performed on the bioassay data . analyses of variance ( anova ) were performed for day 1 and day 5 pharmacokinetic variables with effects for regimen , period , sequence , and subject nested within sequence . the c max and auc 0 - values for regimen c were normalized to a 1000 mg dose . for the day 1 and day 5 auc and c max values and for the day 5 dfl values for both analytes , logarithmic transformation was employed . each of the regimens a and b were compared to the reference regimen c at a significance level of 0 . 05 . within the framework of the anovas for the day 5 auc values , equivalence of the er formulations of the invention to the ir reference tablet was assessed using the two one - sided tests procedure via 90 % confidence intervals . the mean plasma concentration - time profiles for the multiple - dose study are illustrated in fig2 . table iv summarizes ( mean ± sd ) of the day 5 pharmacokinetic , parameter estimates for the clarithromycin in the er and ir formulations . table iv c max c min t max auc 0 - 24 fluctuation formulation ( μg / ml ) ( μg / ml ) ( h ) ( μg · h / ml0 index a 2 . 45 ± 0 . 69 * 0 . 70 ± 0 . 37 8 . 6 ± 4 . 4 * 39 . 6 ± 12 . 8 1 . 11 ± 0 . 31 *† b 2 . 66 ± 0 . 87 * 0 . 67 ± 0 . 39 6 . 9 ± 3 . 3 * 40 . 2 ± 13 . 8 1 . 24 ± 0 . 37 * ir 3 . 21 ± 0 . 78 0 . 78 ± 0 . 29 1 . 9 ± 0 . 6 40 . 8 ± 11 . 8 1 . 47 ± 0 . 26 reference point estimates of the relative bioavailability and 90 % confidence intervals for the two one - sided tests procedures of day 5 auc 0 - 24 are set forth in table v below . the results presented are for logarithmic - transformed clarithromycin auc 0 - 24 values . table v relative bioavailability formulation comparison point estimate 90 % confidence interval a vs reference 0 . 964 0 . 893 - 1 . 039 b vs reference 0 . 970 0 . 899 - 1 . 046 for this multiple dose study under nonfasting conditions , both the 10 % and 20 % polymer er formulations were bioequivalent to the reference ir tablet with respect to the auc 0 - 24 . the significantly lower c max central values and later t max values suggest that both the formulations provide extended release of clarithromycin in vivo . the significantly lower dfls indicate that plasma concentrations fluctuate less for the er tablet regimens than for the ir tablet regimen . additionally , the significantly lower dfl for regimen a compared to regimen b indicates that plasma concentrations from the 20 % polymer fluctuate less than those from the 10 % polymer tablet . the adverse effects , including taste perversion ( taste profile ), were studied for the multiple - dose regimes described above . the formulations a and b of example 1 ( 500 mg tablets ) and the ir biaxin ( reference ) 500 mg tablet were administered to healthy subjects in a multiple - dose regimen as described above . a single dose ( 2 × 500 mg ) of the formulations a and b of example 1 , was administered to the subjects , followed by a 48 hour wash - out period . multiple dosing in the morning with the 2 × 500 mg regimen , once - a - day , followed the washout for the next three days . a single dose of 500 mg ir biaxin tablet was administered to the subjects , followed by a 48 hour wash - out period . multiple dosing with the 500 mg tablet , twice - a - day followed the washout for three days . the adverse effects to the body as a whole , cardiovascular system , digestive system , nervous system , respiratory system , skin and appendages , and special senses were measured by monitoring the subjects at regular time intervals . subjects who reported the same costart term more than once were counted only once for that costart term . the results of the adverse effects are set forth in table vi below . table vi dosing regimen a b reference body system ( n m 24 ) ( n m 23 ) ( n m 23 ) costart term percent of total subjects overall 9 ( 37 . 5 %) 10 ( 43 . 5 %) 11 ( 47 . 8 %) body as a whole 6 ( 25 . 0 %) 3 ( 13 . 0 %) 1 ( 4 . 3 %) asthenia 2 ( 8 . 3 %) 1 ( 4 . 3 %) 0 ( 0 . 0 %) chills 0 ( 0 . 0 %) 1 ( 4 . 3 %) 0 ( 0 . 0 %) headache 2 ( 8 . 3 %) 2 ( 8 . 7 %) 0 ( 0 . 0 %) neck rigidity 1 ( 4 . 2 %) 0 ( 0 . 0 %) 0 ( 0 . 0 %) pain 2 ( 8 . 3 %) 0 ( 0 . 0 %) 1 ( 4 . 3 %) cardiovascular system 1 ( 4 . 2 %) 0 ( 0 . 0 %) 0 ( 0 . 0 %) hypertension 1 ( 4 . 2 %) 0 ( 0 . 0 %) 0 ( 0 . 0 %) digestive system 4 ( 16 . 7 %) 4 ( 17 . 4 %) 4 ( 17 . 4 %) abdominal pain 1 ( 4 . 2 %) 0 ( 0 . 0 %) 0 ( 0 . 0 %) constipation 0 ( 0 . 0 %) 0 ( 0 . 0 %) 2 ( 8 . 7 %) diarrhea 2 ( 8 . 3 %) 3 ( 13 . 0 %) 1 ( 4 . 3 %) dyspepsia 2 ( 8 . 3 %) 2 ( 8 . 7 %) 1 ( 4 . 3 %) flatulence 0 ( 0 . 0 %) 1 ( 4 . 3 %) 0 ( 0 . 0 %) nausea 0 ( 0 . 0 %) 0 ( 0 . 0 %) 1 ( 4 . 3 %) nervous system 0 ( 0 . 0 %) 1 ( 4 . 3 %) 2 ( 8 . 7 %) depersonalization 0 ( 0 . 0 %) 1 ( 4 . 3 %) 0 ( 0 . 0 %) hypesthesia 0 ( 0 . 0 %) 1 ( 4 . 3 %) 1 ( 4 . 3 %) insomnia 0 ( 0 . 0 %) 1 ( 4 . 3 %) 0 ( 0 . 0 %) somnolence 0 ( 0 . 0 %) 0 ( 0 . 0 %) 1 ( 4 . 3 %) respiratory system 1 ( 4 . 2 %) 1 ( 4 . 3 %) 3 ( 13 . 0 %) cough increased 1 ( 4 . 2 %) 0 ( 0 . 0 %) 0 ( 0 . 0 %) hiccup 0 ( 0 . 0 %) 0 ( 0 . 0 %) 1 ( 4 . 3 %) pharyngitis 0 ( 0 . 0 %) 1 ( 4 . 3 %) 2 ( 8 . 7 %) rhinitis 1 ( 4 . 2 %) 1 ( 4 . 3 %) 0 ( 0 . 0 %) skin and appendages 0 ( 0 . 0 %) 2 ( 8 . 7 %) 2 ( 8 . 7 %) rash 0 ( 0 . 0 %) 1 ( 4 . 3 %) 1 ( 4 . 3 %) skin disorder 0 ( 0 . 0 %) 1 ( 4 . 3 %) 2 ( 8 . 7 %) special senses 3 ( 12 . 5 %) 3 ( 13 . 0 %) 6 ( 26 . 1 %) eye disorder 0 ( 0 . 0 %) 1 ( 4 . 3 %) 0 ( 0 . 0 %) taste perversion 3 ( 12 . 5 %) 2 ( 8 . 7 %) 6 ( 26 . 1 %) it is evident from the above table vi that the adverse effects to the digestive , nervous and respiratory systems normally associated with biaxin are reduced with the er tablets . the taste perversion with the formulations of the invention is significantly reduced . it is reasonably believed that the reduced adverse effects , particularly taste perversion , would lead to better compliance and a higher incidence of completion of the prescribed treatment regimen . the results of a comparative pharmacokinetic study of the controlled release formulation a of the co - owned , pending u . s . patent application ser . no . 08 / 574 , 877 , filed dec . 19 , 1995 , as compared with the ir ( biaxin ) are set forth in table vii below . table vii clarithromycin clarithromycin 1000 mg 500 mg bid once - daily reference 90 % pk - parameter ( formulation a ) ( biaxin ) point confidence unit mean a s . d . b mean a s . d . b estimator c interval auc 0 - 24 ( μg * h / ml ) 27 . 298 10 . 086 28 . 256 10 . 770 97 . 4 86 . 9 - 109 . 2 c max ( μg / ml ) 2 . 432 0 . 905 2 . 701 0 . 785 89 . 0 78 . 2 - 101 . 3 t max ( h ) 5 . 217 1 . 858 2 . 043 0 . 706 c min ( μg / ml ) 0 . 469 0 . 292 0 . 597 0 . 241 71 . 7 60 . 0 - 85 . 7 dfl 1 . 800 0 . 572 1 . 900 0 . 616 the mean dfl for the composition of the invention is statistically lower than the ir in vivo profile . the lower dfl indicates that the er formulations of the invention provide less variable clarithromycin concentrations throughout the day than the ir and the sustained release compositions . the mean dfl values for the controlled release formulation and for the ir are substantially equal in value as can be seen in the above table . c . f . 1 . 800 ± 0 . 572 ( for controlled release ) with 1 . 900 ± 0 . 616 ( ir ). two well - controlled , double - blind clinical trials were conducted to compare the safety and efficacy of extended - release clarithromycin ( er ) and immediate - release clarithromycin ( ir ) in patients with acute maxillary sinusitis ( ams ) and patients with acute bacterial exacerbation of chronic bronchitis ( aecb ). a total of 910 patients were enrolled for the studies . of the 910 patients , 459 patients were treated with er formulation of the invention and 444 patients were treated with the ir ( reference ) formulation . two hundred eighty three ( 283 ) patients , enrolled in the ams study , and 627 patients , enrolled in the aecb study , were randomly assigned in a 1 : 1 ratio to receive either the er formulation of the invention or the ir formulation . of the 283 patients enrolled in this study , 142 patients received a single dose of clarithromycin er tablets 500 mg × 2 qd ( 1000 mg daily ) for 14 days , and 141 patients received clarithromycin ir tablets , 500 mg bid ( 1000 mg daily ) for 14 days . of the 627 patients enrolled in this study , 317 patients received a single dose of clarithromycin er tablets 500 mg × 2 qd ( 1000 mg daily ) for 7 days , and 303 patients received clarithromycin ir tablets , 500 mg bid ( 1000 mg daily ) for 7 days . the results of the study are summarized below in table viii . table viii clarithromycin er reference 1000 mg . once - daily biaxin number of patients 0 . 6 % 3 . 0 %* discontinued due to drug - ( 3 / 459 ) ( 13 / 444 ) related gi adverse events number of patients with severe 0 . 2 % 0 . 2 %* drug - related gi adverse events 1 / 459 ( 8 / 444 ) from the above results , it can be seen that patients taking the extended - release formulation of clarithromycin were significantly less likely to stop taking clarithromycin due to gastrointestinal adverse events and these patients suffered significantly fewer severe gastrointestinal adverse effects . | 0 |
δ 4 - dh ( ec . 1 . 3 . 99 . 6 ) useful in the practice of this invention is a dehydrogenase possessing a specificity to 3 - oxo - 5β - steroid and is widely found in microorganisms such as those belonging to the genus pseudomonas [ j . chem . soc . ; chem . comm . 3 , 115 ( 1974 ); j . biol . chem . 218 , 675 ( 1956 ), ibid . 234 , 2014 ( 1959 ); biochem . biophy . acta 56 , 584 ( 1962 )], the genus of arthrobactor [ eur . j . biochem . 47 , 555 ( 1974 )]; the genus of nocardia [ chemical and pharmaceutical bulletin 21 , 2794 ( 1973 ), ibid . 23 , 2164 ( 1975 ); dissertation abstracts 35 , 3839 ( 1975 )]; the genus of corynebacterium ( u . s . pat . no . 3 , 639 , 212 ), etc . there is no limitation to the source of the enzyme . the amount of δ 4 - dh to be used may be , in terms of the reaction concentration , 50 - 10 , 000 units / λ , preferably 300 - 3 , 000 units / λ . any reducing chromophoric agents may be used for the purpose of this invention so long as their intramolecular potential may change by accepting electrons thereby producing a chromophore which is capable of absorbing radiation of only a ray with a specific wavelength . specifically , they may be tetrazolium compounds , including but not limited to , nitroblue tetrazolium ( hereinafter abbreviated as &# 34 ; ntb &# 34 ;), 3 -( p - indophenyl )- 2 -( p - nitrophenyl )- 5 - phenyl - 2h - tetrazolium chloride ( hereinafter abbreviated as &# 34 ; int &# 34 ;), 3 -( 4 , 5 - dimethyl - 2 - thiazolyl )- 2 , 5 - diphenyl - 2h - tetrazolium bromide ( hereinafter abbreviated as &# 34 ; mtt &# 34 ;) and 1 , 1 &# 39 ;-( 3 , 3 &# 39 ;- dimethoxy - 4 , 4 &# 39 ;- biphenylene )- bis { 5 -( 4 - nitropheny )- 3 -[ 4 -( 2 - hydroxy - 3 -( 2 - hydroxyethyldiethylamino )- propxoy ) phenyl ]}- 2h - tetrazolium chloride ( hereinafter abbreviated as &# 34 ; w . s . ntb &# 34 ;). the concentration of the tetrazolium compound may be in the range of 50 - 2 , 000 μmole / λ , preferably , 100 - 1 , 000 μmole / λ . as 3 - oxo - 5β - steroid to which the quantitative analysis of this invention is applicable may be , beside dehydrochoric acid , 5β - androstan - 3 , 17 - dione , δ 1 - 5β - androstene - 3 , 17 - dione , 5β - pregnane - 3 , 20 - dione , 21 - hydroxy - 5β - pregnane - 3 , 20 - dione , etc . samples usable for the analysis may , therefore , be serum , plasma , urine and the like . in practicing the quantitative analysis of this invention , the sample , reducing chromophoric agent and δ 4 dh may be added in an arbitrary order to a buffer , and after reaction the optical density of the reaction solution is measured . any conventional buffers may be used for the quantitative analysis of this invention , including , for example , phosphate buffers , tris buffers and good &# 39 ; s buffers with a ph range of from 6 to 10 . there is no special limitation on the temperature at which the reaction is conducted to the extent that δ 4 dh may not be deactivated . usually , a temperature of 20 - 40 ° c ., preferably of close to 37 ° c ., may be used . the quantitation of 3 - oxo - 5β - steroid may be made , upon termination of the reaction by the addition of a terminating solution to the reaction mixture , by measuring the optical density of the colored substance in the mixture , or alternatively , by measuring the increase in the optical density of the colored substance in a prescribed period of time . inorganic acids such as hydrochloric acid , sulfuric acid and phosphoric acid or organic acids such as citric acid and acetic acid may be used for a terminating solution . the reagent for the quantitative analysis of this invention may be that consisting of a buffer solution added with 60 - 2 , 400 μmole / λ of the reducing chromophoric agent and 60 - 12 , 000 units / λ of δ 4 dh . it is possible to prepare a buffer solution added with either one of the reducing chromophoric agent or δ 4 dh in advance and to add the other when the reagent is used . this invention makes use of the enzymes which are capable of specifically recognizing the structure of 3 - oxo - 5β - steroid and the colorimetry of the colored substance . the invention thus eliminates the need for the procedures on the samples such as a heat treatment , deproteinization and extraction , thus requiring only a small quantity of the samples , as much as 50 - 200 μλ in one quantitation , and yet giving an excellent sensitivity . the quantitative analysis of this invention can be applied to a loading test , in which a metabolism of dehydrochoric acid administered in a body is measured , thus providing a very simple and precise liver function test . other features of the invention will become apparent in the course of the following description of the exemplary embodiments which are given for illustration of the invention and are not intended to be limiting thereof . 0 . 5 mλ of 50 mmole / λ phosphate buffer solution ( ph8 ) containing 500 μmole / λ ntb and 1 , 500 units / λ δ 4 dh ( hereinafter referred to as &# 34 ; reagent &# 34 ;) was added with 100 μλ of samples , and reacted precisely for 10 minutes at 37 ° c ., upon which 0 . 5 mλ of the terminating solution ( 0 . 1n - hcλ ) was added . after the resultant liquid was allowed to stand for 5 minutes , its optical density at a wave length of 540 nm was measured . the same samples were added to the reagent not containing δ 4 dh and the above procedures were exactly repeated as a blank test . the samples used were serum added with dehydrochoric acid and diluted to various concentrations with the same serum but not containing dehydrochoric acid . δ 4 dh used was that separated from pseudomonas testosteroni cultured in accordance with the method proposed by levy et al [ j . biol . chem . 234 , 2014 ( 1959 )], and purified . the result obtained are shown in table 1 below . table 1______________________________________dehydrochoric acidconcentration optical density ( mole / l ) at 540 nm______________________________________20 0 . 02240 0 . 04660 0 . 07780 0 . 101100 0 . 122140 0 . 172180 0 . 226______________________________________ the same procedures were repeated on samples of serum added with in various concentrations the reagent of example 1 , but containing 5μ - androstan - 3 , 17 - dione ( a methanol solution ) instead of dehydrochloric acid . the result is shown in table 2 . table 2______________________________________5β - androstan - 3 , 17 - dioneconcentration optical density ( mole / l ) at 540 nm______________________________________20 0 . 06540 0 . 13260 0 . 20180 0 . 270100 0 . 332120 0 . 403______________________________________ a liver cirrhosis patient and a healthy subject were each intravenously given 1g of dehydrochoric acid . the changes of the dehydrochoric acid level in serum after the administration were determined according to the same procedure as in example 1 and using the reagent of example 1 . the results are shown in the appended fig1 . the elimination constant ( keλ ), the half - life period ( t 1 / 2 ) and the area under concentration curve of the compound in blood ( auc ) are given in table 3 . table 3______________________________________ liver cirrhosisparameter healthy subject patient______________________________________t1 / 2 ( min ) 9 . 76 4 . 41kel ( min . sup .- 1 ) 0 . 071 0 . 157auc ( μg · min / ml ) 2727 1398______________________________________ obviously , numerous modifications and variations of the present invention are possible in light of the above teachings . it is therefore to be understood that the scope of the appended claims , the invention may be practiced otherwise than as specifically described herein . | 2 |
fig1 shows an example user interface 100 for a database application that includes a database message builder interface 102 in a text editing mode . in general , the database message builder interface 102 provides a user with tools for combining unstructured data ( e . g ., free - form text ) with structured data retrieved from a database records , and submitting the combined unstructured data and structured data to an application such as email , text or instant messaging ( e . g ., sms ), or a network resource such as a social networking website . the examples that follow use text and text strings as examples of unstructured and structured data . however , any unstructured and structured data can be used with the database message builder . the database application user interface 100 can include a main window 104 . the main window 104 can provide a collection of user interface elements that give a user the tools needed to input , organize , query , browse , and / or view the content of a database . for example , the main window can include a list control 106 that shows a collection of items representative of databases that can be accessed through the database application user interface 100 . in the illustrated example , the user has selected an item 108 that represents a car collection database . a form interface region 110 can provide user interface elements that the user can manipulate to interact with the content of a database . in the illustrated example , the form interface region 110 is laid out to present interface elements associated with the fields of a car collection database . in some examples , the car collection database can include multiple records , each record representing a car , and each record including various fields for storing information related to the car such as the year , make , model an data and location of purchase . the form interface region can include a year input box 112 , a make input box 114 , a model input box 116 , a “ purchased from ” input box 118 , and a purchase date input box 120 . these input boxes can have correspondingly record fields in the car collection database . the database application user interface 100 can include a database message builder button 122 . when the database message builder button 122 is activated by the user , the database message builder interface 102 is displayed . in some implementations , the database message builder interface 102 can be a pop - up or balloon dialog , as illustrated in fig1 . in other implementations , the database message builder interface 102 can be a sub - region of the database application user interface 100 . for example , the database message builder interface 102 can occupy an area of the database application user interface 100 that is visible all or most of the time . in another example , the database message builder interface 102 can occupy an area that is visible only when needed , such as a drawer control that opens or extends inward or outward from an edge of the database application user interface 100 when activated and can then close or shut when the user is finished . in some implementations , database message building functionality can be included in an application using an application programming interface ( api ) in place of the user interface 102 . the api can allow a programmer to access database message builder methods and classes according to call conventions defined by a database message builder api specification . the database message builder interface 102 can include an input box 124 . the input box 124 can be a user interface control that can be used by the user to input , edit , and view text - based information . the user can combine free form , unstructured text with structured text retrieved from fields of the database by interacting with the input box 124 . for example , the unstructured text elements , “ alyx bought a ,” “ from ,” “ on ,” as well as spaces and punctuation marks , can be combined with the structured text elements “ 1979 ,” “ cadillac ,” “ phaeton ,” “ tom &# 39 ; s junk yard ,” and “ dec . 6 , 2007 ” retrieved from the database . other examples of such uses will be discussed further in the descriptions of fig2 and 3 . a selector control 126 can be provided so the user can select a target application or network resource to receive the message of combined structured and unstructured text displayed in the input box 124 . for example , the selector control 126 can provide the user with selections for popular social networking services such as twitter ™, facebook ™, linkedin ™, or myspace ™. the selector control 126 can also provide the user with selections for applications , such as email , instant messaging , text messaging ( e . g ., sms ), word processing , a clipboard , or other application that can accept text input . an activation button 128 can be included to initiate a transmission of the combined text to the selected service or application . in the illustrated example , the user can press the activation button 128 , and the combined text “ alyx bought a 1979 cadillac phaeton from tom &# 39 ; s junk yard on dec . 6 , 2007 ,” will be sent ( e . g ., “ tweeted ”) to the twitter social network service . in another example , if an email application is selected using the selector control 126 , the activation button 128 can initiate the creation of a new email message that can be pre - populated with the combined text . a counter indicator 130 displays a count of the total characters in the combined text string , the maximum number of characters allowed by the selected target service or application , or both . for example , the twitter service can allow users to submit strings of 140 characters maximum , the facebook service can allow a 1000 character limit , and sms messages can be 160 characters long , whereas an email application may present no practical limit on the number of characters that may be used . in some implementations , the counter indicator 130 can provide the user with feedback that may be useful while the user is editing the combined structured and unstructured text . for example , the counter indicator 130 can help the user avoid sending combined text that exceeds the target service &# 39 ; s or application &# 39 ; s maximum allowable character limit , which may result in the service or application rejecting the string , returning an error , truncating the string at the allowable limit , or some other possibly undesirable result . in some implementations , a toggle button 132 can be selected to toggle the database message builder interface 102 into a token editing mode , as is illustrated by and discussed in the description of fig2 . fig2 shows another view of the example database application user interface 100 where the database message builder interface 102 is in a token editing mode . while in the token editing mode , the database message builder interface 102 can present the structured text as a collection of tokens 212 - 220 ( e . g ., visual placeholders for information retrieved from the database ). in some implementations , the tokens 212 - 220 can be visually differentiated from unstructured text . for example , the tokens 212 - 220 can be displayed using a different font , color , background , or with some other modification that can make them visually distinguishable from the unstructured text . in some implementations , the tokens 212 - 220 can be indicative of the database fields they represent . for example , the token 212 is labeled with the word “ year ,” and represents the content of the “ year ” field of the database , the token 214 labeled “ make ” represents the content of the “ make ” field , and so on . in some implementations , the user can place the tokens in the input box 124 by dragging and dropping the input boxes 112 - 120 into the desired position within the items displayed in the input box 124 . in some implementations , the user can place the tokens in the input box 124 by indicating a position ( e . g ., pointing , clicking ), and then selecting a field name from a list ( e . g ., a pop - up menu ). in some implementations , designated characters can be used to delimit tokens . for example , curly braces can be used to delimit the field names associated with tokens , and the user could enter the string , “ i wish i owned a { year } { make } { model }.” in such an example , the user can edit both the unstructured text and the tokens entirely from a keyboard . when the user selects the toggle button 132 again , the database message builder interface 102 toggles out of token editing mode , and returns the database message builder interface 102 to the text editing mode as illustrated in fig1 . when in the text editing mode , the tokens 212 - 220 are replaced by the string content stored in the fields they represent for a given record of the database . in the example of fig1 , the user is looking at a record containing information about a 1979 cadillac phaeton , and the token 216 is replaced by the structured text string “ phaeton ”, which is held in the “ model ” field of the currently displayed record . similarly , the token 220 is replaced by the structured text string “ dec . 6 , 2007 ” which is held by the “ purchase date ” field of the currently displayed record . in some implementations , the user can browse through multiple database records , and the database message builder interface 102 can update some or all of the tokens 212 - 220 with the structured text from the currently selected record , thereby providing a combined collection of structured and unstructured text that is based upon the fields of a given database record , and this combined collection may in turn be submitted to the selected application or network resource . in some implementations , the user can select a database record other than the one currently shown , or a record not shown at all , from which structured text can be retrieved . for example , the user may be provided with a record number selector that the user can manipulate to identify the desired record without requiring that the selected record be displayed . in some implementations , the database message builder interface 102 can present the user with a preset string in the input box 124 . for example , one or more preconfigured combinations of the tokens 212 - 220 and the unstructured text may be associated with the database user interface 100 or the selected database , and one of these combinations can be presented to the user when the database message builder button 122 is selected . in some implementations , the user can edit the combination of the tokens 212 - 220 and the unstructured text , and save the combination as a preset string associated with a selected database . for example , the combination of the tokens 212 - 220 and the unstructured text may only make sense in the context of the selected car collection database , therefore the combination may be saved in association with that database . in another example , the user may also have a database of aircraft , and a preset string such as “ alyx flew through the sky in a [ make ] [ model ] in [ year ].” such a preset string would make sense in the context of the aircraft database ( e . g ., “ alyx flew through the sky in a boeing 747 in 2009 .”) but not in the context of the car collection database ( e . g ., “ alyx flew through the sky in a cadillac phaeton in 1972 .”). in such an example , it can be advantageous to save the preset string in association with the aircraft database but not in association with the car collection database . fig3 is a flow diagram of an example method 300 for building and sending a database message . the method 300 can start when a user interface is displayed 302 . in some implementations , the user interface can be the database application user interface 100 of fig1 and 2 . a message building window is then presented 304 to the user . for example , the database message builder interface 102 can be displayed in response to a user input such as a press of the database message builder button 122 . alternatively , database message builder functionality can be accessed through an api . structured data can be retrieved 306 from one or more fields of a database . examples of such databases have been discussed in relation to fig1 and 2 , and additional examples of such databases will be discussed in the description of fig4 . unstructured data can be received 308 by the message building window , for example , by the user entering character strings into a text input control such as the input box 124 . the structured data can be displayed 310 as tokens within the unstructured data . in some implementations , the tokens may appear as visual placeholders within the unstructured data . for example , a token that represents a database field intended to hold a person &# 39 ; s first name can be placed within a string of unstructured text , such as , “ this database record refers to { first name }.” a current character count can be displayed 312 . the current character count is a count of the characters received as unstructured data plus a count of the characters retrieved as structured data from a field of the database ( e . g ., the field displayed as tokens ). for example , the previously described string of structured and unstructured data , “ this database record refers to { first name },” includes 32 characters , spaces , and punctuation marks , and this number can be added to a count of the characters included in a database entry for the “ first name ” field ( e . g ., a field that stores the string “ bob ” would add three additional characters to the count ). a current character limit can also be displayed 314 . in some implementations , the current character limit can be a number that indicates the maximum number of characters that may be used in the database message . in some implementations , the current character limit can reflect limits imposed by applications or network resources . for example , the twitter service allows users to submit “ tweets ” of 140 characters or less . in another example , sms messaging standards allow for messages of 160 characters or less . these limits or other values can then be displayed as the current character limit . a target application or network resource can be determined 316 . for example , the determination can be made when the user uses the selector control 126 to choose a target application ( e . g ., email , instant messaging , word processing ) or network resource ( e . g ., social network , blog ). in some implementations , an updated current character limit can be displayed when a target is determined . for example , when the user targets a different application or network resource , the newly selected target may be associated with a different character limit than was the previous target , and the different character limit can be displayed to reflect the character limit associated with the newly selected target . the method 300 can then wait 318 for user input . for example , some or all of the steps 302 - 316 may be performed or repeated until the user presses the toggle button 132 , thereby switching the database message builder interface 102 from the token editing mode to the text editing mode . when the user input is received , the displayed tokens are replaced 320 with structured data retrieved from the database . in the example of the previously described string of structured and unstructured data , “ this database record refers to { first name },” the token “{ first name }” can be replaced by the content included in a field of a record of the database , such as “ bob .” in this example , the resulting string would be displayed as , “ this database record refers to bob .” in some implementations , when the tokens are replaced with structured data retrieved from the database , the current character count can be updated and displayed . for example , the string , “ this database record refers to bob ,” includes 32 characters of unstructured data and 3 characters of structured data , for a total of 35 characters , and in this example the number “ 35 ” can be displayed 314 as the current character count in the counter indicator 130 . the resulting message ( in this example a text string ) of structured and unstructured data is then sent 322 to the target application or network resource . in some implementations , the message can be sent in response to a user input , such as the user pressing the activation button 128 . for example , by pressing the activation button 128 , combined structured and unstructured data ( e . g ., “ this database record refers to bob ,” “ alyx bought a 1979 cadillac phaeton from tom &# 39 ; s junk yard on dec . 6 , 2007 ”) can be posted directly to a social networking site , an email , a blog , or to other types of applications and network resources . once the data is sent , a response can be received from the target application or network resource , which can then be handled by the database message builder application . for example , a response can be a confirmation that the database message was successfully received , an error , the data and time that the database message was accepted , etc . in some implementations , the database message builder can automatically cycle through and send out database messages for each database record . for example , a user can click a button that says “ twitter all records .” the database message builder can then automatically send the constructed message ( s ) for each database record . fig4 is a block diagram of an example database 400 . in some implementations , the database 400 can be an integrated collection of logically related records or files consolidated into a common pool that provides data for one or more users . for example , the database 400 can be structured as a relational database , hierarchical database , a network database , an xml file , a text file , a delimited file ( e . g ., tab - delimited , csv ), or other type of collection of data . in general , the database 400 can be structured as a collection of tables , wherein each table includes a collection of records that represent a collection of related data , and the records within a table can share a common collection of fields for storing datum . for example , in a table structured to represent a collection of personal contacts , each record can represent a single person . the fields can represent attributes like first name , last name , street address , phone number , or other information about the person . the database 400 can include a structured data table 410 , a string configuration table 450 , and a target configuration table 470 . the structured data table 410 can include a collection of one or more records , such as a record 412 . the record 412 includes a collection of fields 414 - 418 . in some implementations , fields 414 - 418 can be implemented and arranged by the user to store a collection of related data . for example , the structured data table 410 can be designed to store information about a car collection ( e . g ., as was illustrated in the example of fig1 ), wherein each record represents a car in the collection . the fields 414 - 418 can store information such as the make , model , year , or other information that may be associated with a car in a collection . the string configuration table 450 can include one or more records such as a record 452 . in some implementations , the record 452 can store a preset string of structured and unstructured data . for example , the record 452 includes a table field 454 , an unstructured text field 456 , and a field token field 458 . the table field 454 can include information that associates the record and the preset string with a particular table of structured data , such as the table 410 . in some implementations , by associating the record 452 with the table 410 , the preset string described by the content of the record 452 can be made available for use in the database message builder interface 102 of fig1 and 2 only in the context of the table 410 . the unstructured text field 456 can include the unstructured text portion of the preset string , and the field tokens field 458 can include information about the fields and / or placement of structured data within the unstructured text portion of the preset string . in some example , the field tokens field 458 can be implemented as one or more sub - tables of the string configuration table 450 , wherein each record of the sub - table can represent a single token and token placement location within a preset string . in other implementations , the tokens that represent structured data can be combined with the unstructured text in a single field . for example , tokens representing the car collection database fields “ year ,” “ make ,” and “ model ” can be represented as character delimited substrings within a preset string of unstructured text such as , “ alyx owns a & lt ; year & gt ; & lt ; make & gt ; & lt ; model & gt ;.” the target configuration table 470 can store information about target applications and network resources . the target configuration table 470 can include one or more records , such as a record 472 that represents a single application or network resource . the record 472 can include a resource or application identifier field 474 to store the name of a target network resource or application . for example , the resource or application identifier field 474 can store values such as “ twitter ” or “ apple mail .” a location field 475 can store an address or file location for the network resource or application . for example , the location field 475 can store values such as “ http :// www . twitter . com ” or “/ mac hd / applications / applemail ”. a character limit field 476 can be included to store a number that can describe the maximum number of characters that the network resource or application can permit . for example , the character limit field 476 can store the number “ 140 ” in association with the “ twitter ” service , or may store no value or a reserved value ( e . g ., zero , − 1 ) for targets that do not define a maximum character count such as email applications . a user information field 477 is included to store user name , password , or other information . in some implementations , the data stored in the user information field 477 can be used to log into a network resource or application , and post combined strings of structured and unstructured text under the user &# 39 ; s identity . fig5 is a schematic diagram of an example of a generic computer system 500 . the system 500 can be used for the operations described in association with the method 300 according to one implementation . for example , the system 500 may be included in either or all of a computer executing the database application user interface 100 , the process 300 , or the database 400 . the system 500 can be included in a personal computer , mobile phone , email device , media player , electronic tablet , website server ( in the cloud ) or any other computing device . in some implementations , the system 500 can include a processor 510 , a memory 520 , a storage device 530 , and an input / output device 540 . each of the components 510 , 520 , 530 , and 540 are interconnected using a system bus 550 . the processor 510 is capable of processing instructions for execution within the system 500 . in one implementation , the processor 510 is a single - threaded processor . in another implementation , the processor 510 is a multi - threaded processor . the processor 510 is capable of processing instructions stored in the memory 520 or on the storage device 530 to display graphical information for a user interface on the input / output device 540 . in some implementations , the system 500 can include multiple processors or processing cores . the memory 520 can store information within the system 500 . in one implementation , the memory 520 can be a computer - readable medium . in one implementation , the memory 520 can be a volatile memory unit . in another implementation , the memory 520 can be a non - volatile memory unit . the storage device 530 can be capable of providing mass storage for the system 500 . in one implementation , the storage device 530 can be a computer - readable medium . in various different implementations , the storage device 530 can be a cd rom , dvd , a hard disk device , an optical disk device , or a tape device . the input / output device 540 provides input / output operations for the system 500 . in one implementation , the input / output device 540 can include a keyboard and / or pointing device . in another implementation , the input / output device 540 can include a display unit for displaying graphical user interfaces . the features described can be implemented in digital electronic circuitry , or in computer hardware , firmware , software , or in combinations of them . the apparatus can be implemented in a computer program product tangibly embodied in an information carrier , e . g ., in a machine - readable storage device or in a propagated signal , for execution by a programmable processor ; and method steps can be performed by a programmable processor executing a program of instructions to perform functions of the described implementations by operating on input data and generating output . the described features can be implemented advantageously in one or more computer programs that are executable on a programmable system including at least one programmable processor coupled to receive data and instructions from , and to transmit data and instructions to , a data storage system , at least one input device , and at least one output device . a computer program is a set of instructions that can be used , directly or indirectly , in a computer to perform a certain activity or bring about a certain result . a computer program can be written in any form of programming language , including compiled or interpreted languages , and it can be deployed in any form , including as a stand - alone program or as a module , component , subroutine , or other unit suitable for use in a computing environment . suitable processors for the execution of a program of instructions include , by way of example , both general and special purpose microprocessors , and the sole processor or one of multiple processors of any kind of computer . generally , a processor will receive instructions and data from a read - only memory or a random access memory or both . the essential elements of a computer are a processor for executing instructions and one or more memories for storing instructions and data . generally , a computer will also include , or be operatively coupled to communicate with , one or more mass storage devices for storing data files ; such devices include magnetic disks , such as internal hard disks and removable disks ; magneto - optical disks ; and optical disks . storage devices suitable for tangibly embodying computer program instructions and data include all forms of non - volatile memory , including by way of example semiconductor memory devices , such as eprom , eeprom , and flash memory devices ; magnetic disks such as internal hard disks and removable disks ; magneto - optical disks ; and cd - rom and dvd - rom disks . the processor and the memory can be supplemented by , or incorporated in , asics ( application - specific integrated circuits ). to provide for interaction with a user , the features can be implemented on a computer having a display device such as a crt ( cathode ray tube ) or lcd ( liquid crystal display ) monitor for displaying information to the user and a keyboard and a pointing device such as a mouse or a trackball by which the user can provide input to the computer . the features can be implemented in a computer system that includes a back - end component , such as a data server , or that includes a middleware component , such as an application server or an internet server , or that includes a front - end component , such as a client computer having a graphical user interface or an internet browser , or any combination of them . the components of the system can be connected by any form or medium of digital data communication such as a communication network . examples of communication networks include , e . g ., a lan , a wan , and the computers and networks forming the internet . the computer system can include clients and servers . a client and server are generally remote from each other and typically interact through a network , such as the described one . the relationship of client and server arises by virtue of computer programs running on the respective computers and having a client - server relationship to each other . although a few implementations have been described in detail above , other modifications are possible . in addition , the logic flows depicted in the figures do not require the particular order shown , or sequential order , to achieve desirable results . in addition , other steps may be provided , or steps may be eliminated , from the described flows , and other components may be added to , or removed from , the described systems . accordingly , other implementations are within the scope of the following claims . a number of implementations have been described . nevertheless , it will be understood that various modifications may be made without departing from the spirit and scope . for example , advantageous results may be achieved if the steps of the disclosed techniques were performed in a different sequence , if components in the disclosed systems were combined in a different manner , or if the components were replaced or supplemented by other components . the functions and processes ( including algorithms ) may be performed in hardware , software , or a combination thereof , and some implementations may be performed on modules or hardware not identical to those described . accordingly , other implementations are within the scope of the following claims . | 6 |
fig3 is a partial view of a wafer 52 with a plurality of masks 53 for sliders according to a first embodiment of the invention . the substrate 43 is a material which is amenable to drie , for example , silicon . the masks 53 outline the shape of the sliders and the sacrificial extension 32 and optionally the guide rails . the mask 53 is made of a material that is resistant to drie , for example , photoresist or alumina . when the wafer 52 is subjected to drie with the ions being directed substantially perpendicular to the surface of the wafer , the individual sliders with the sacrificial extension are cut out in the shape of the mask . although non - rie - able material in the head structure ( not shown ) may also be used to define the shape of the sacrificial extension , this has the disadvantage of potentially allowing some of the head material to be sputtered off and redeposited in the kerf and thereby interfering with the clean separation of the sliders . the details of the cross - sectional shape of the sacrificial extension 32 and optional guide rails 34 are determined by the shape of the mask 53 . the shape and dimension of these features will vary according to various embodiments of the invention . the shape of the sacrificial extension need not include a planar surface and , therefore , can include curved and irregular shapes . the mask 53 in combination with drie allows the removal or more material between the sliders than is feasible using prior art sawing techniques . by lessening the amount of material to be removed by lapping , the technique of the invention allows the lapping process to proceed more quickly than under the prior art . fig4 shows an isometric view of a slider having a sacrificial extension 32 according to the first embodiment of the invention as shown in fig3 after the drie process has cut the slider from the wafer . the view of slider 20 in fig4 is of the trailing edge of the slider surface , i . e ., the surface that is the last to pass over the moving magnetic media when in use . the guide rails 34 and the sacrificial extension 32 extend the entire length of the slider , from the trailing edge to the leading edge . the head elements 31 are illustrated as a shaded area that extends into the sacrificial extension 32 . the sacrificial extension 32 may also include the anchor base ( not shown ) which is used in the prior art to support the fragile pole tips during wafer fabrication . the anchor base may , in fact , be part of the mask since it is typically made from a material such as nife which is not readily etchable in a drie process . the internal structure of the head elements 31 are according to the prior art and the details of these structures are independent of the invention . thus , the invention can be used with any head structure which includes lapping as part of the fabrication process . the head elements 31 include an upper layer of material that is not subject to reactive ion etching ( non - rie - able ), for example , cofe or a nife alloy , and , therefore , can be used as part of the mask as well . the body of the slider 43 is a material that is removable by drie . silicon is preferred as a material for the body of the slider , but other rie - able materials can be used . the embodiment shown includes optional symmetric guide rails 34 that are disposed on the outer edges of the slider bottom surface which will be lapped . the guide rails 34 aid in the lapping process by keeping the lapped surface from canting to one side . the sliders must be held during lapping with the sacrificial extension 32 confronting the lapping plate and may be moved in relation to the lapping plate or the lapping plate may be moved . the guide rails 34 would ideally both be the same height and width , but need not be the same height or width as the sacrificial extension 32 . at some point during the lapping process the surfaces of guide rails 34 and sacrificial extension 32 will become coplanar as protruding material is worn away . the guide rails 34 are distinct from the aerodynamic rails which are used to control the flying characteristics of the slider . the guide rails 34 may be completely removed during lapping as will be noted in more detail hereinafter . fig5 is a magnified view of the sacrificial extension 32 from fig4 . this figure illustrates the optional planes at which the lapping process may be terminated . the aa - plane is the bottom of the sacrificial extension 32 prior to lapping . in other embodiments the bottom of the sacrificial extension 32 may be shorter than the guide rails 34 . the bb - plane is one plane at which the lapping may be terminated leaving a portion of the sacrificial extension 32 and the guide rails ( not shown ) extending below the surrounding slider surface which is shown as plane cc . the lapping may also be continued until the dd - plane is reached at which point the sacrificial extension and the guide rails will have been completely removed , as well as , some material from the slider surface . the plane at which lapping is terminated is typically referred to as the abs although additional material for overcoats , aerodynamic structures , etc . may be added after lapping which will result in the true , final abs being slightly lower than the actual lapping plane . fig6 shows an isometric view of a slider having a sacrificial extension 32 t according to the second embodiment of the invention . in this embodiment the sacrificial extension 32 t is structurally weak in the transverse direction because it is formed with a narrow neck ( like an inverted “ t ”) which facilitates breaking to allow a significant amount of material to be removed as lapping begins and therefore tends to further reduce the lapping time . the planes shown in fig7 for optional points to stop lapping and thus define the abs are the same as illustrated in fig6 and fig4 . fig8 is a midline cross - sectional view of a slider and mask according to the invention taken perpendicular to the trailing end 800 of the slider 20 and the surface to be lapped , plane 802 . in this view , the details of the rails are not shown . fig8 shows that the sacrificial extension 32 extends the entire length of slider 20 . the mask 53 covers the entire surface of the slider which is overcoat 61 which has been deposited over the head elements according to the prior art . plane 802 is indicated for reference as the bottom of the sacrificial extension 32 or an as - lapped abs surface . the guide rails ( not shown ) also extend the full length of the slider parallel to the sacrificial extension 32 . fig9 is a partial view of a wafer 52 with a plurality of masks 53 c for sliders according to a third embodiment of the invention having a channel 55 in the top surface ( the surface parallel to the abs ). fig1 is an isometric view of a slider 20 according to the third embodiment of the invention . a channel 55 is sized to allow the sacrificial extension 32 t or 32 ( not shown ) to extend into what would otherwise be an adjacent slider . this allows the sliders to be position more densely and , therefore , more efficiently on the wafer . for this efficiency to be achieved the guide rails 34 must not extend as far as the sacrificial extension 32 t or 32 . however , multiple channels 55 may exist in adjacent sliders to accommodate other sacrificial extensions such as guide rails 34 . the sacrificial extensions are not necessarily placed along the central plane of the slider . the option exists for placing the magnetic transducer elements off - axis with the sacrificial extension below the sensor . fig1 illustrates the trailing edge of a slider prior to lapping according to an embodiment of the invention having the sacrificial extension and magnetic transducer elements offset from the midline of the slider . other sacrificial extensions such as guide rails 34 may be formed at other locations on the abs side of the slider to improve lapping uniformity and / or flatness . as shown in fig1 , for example , the sacrificial extension 32 and guide rails 34 are symmetric about the central plane of the slider . ideally , this will prevent the skew of the slider . in alternative embodiment illustrated in fig1 the offset sacrificial extension 32 t may be formed with a narrow neck which facilitates breaking as described above . as an example , an inverted “ t ” structure can be placed off the central axis of the slider with or without other sacrificial extensions to improve the rate of the lapping of the slider . one issue for any lapping process is determining when enough material has been removed to achieve the correct stripe height of the sensor and also the throat height of the inductive write head . electronic lapping guides ( elg &# 39 ; s ) have been used in the prior art for this purpose . an elg can be used with the sacrificial extension structure by including it in the guide rails , the sacrificial extension itself or any other portion of the slider which will remain after lapping . in an alternative embodiment of the invention , the sensor structure could be used to determine the stripe height of the sensor and the throat height . using the sensor has the advantage of allowing a simpler head structure , but adds the complexity of having to electrically connect the sensor structure during lapping without causing any electrical or mechanical damage to the sensor . using the sensor as a lapping end - point detector is not exclusive to sliders with sacrificial extensions described herein , but can be used an alternative head design and lapping method to achieve a reproducible abs plane for the slider . except where express materials , thickness values , etc ., have been given above , the layers , structures and materials in a slider embodying the invention are according to the prior art and are fabricated according to the prior art . the compositions given herein have been described without regard to small amounts of impurities that are inevitably present in practical embodiments as is well known to those skilled in the art . although the embodiments of the invention have been described in a particular embodiment , the invention as described herein is not limited to this application and various changes and modifications will be apparent to those skilled in the art which will be within the scope of the invention . | 6 |
a grommet protection member according to the present invention may be provided with a drain opening for draining water entering between the grommet protection member and a grommet . according to this configuration , water entering between the grommet protection member and the grommet can be quickly drained without retaining it . the grommet protection member may be provided with a pair of segments that is divided in radial direction in at least one location so as to be capable of being opened , and link portions are provided at open ends of the two segments so that the segments are capable of being linked to each other such that the segments can be held in an annular shape that can surround the outer circumferential surface of the grommet . according to this configuration , as the grommet protection member is formed by the segments that can be opened and closed , the operation of surrounding the outer circumferential surface of the grommet can be performed easily and smoothly . in addition , preferably , the grommet protection member comprises two separate segments that are divided in radial direction at two locations together with the flange , and the link portions linking the two segments are formed at the two divided locations , and upon attachment to the grommet , the two segments are joined together so that the flange continues in circumferential direction . according to this configuration , as the grommet protection member is divided , it can be easily attached to the grommet , and as the flange is circumferentially continuous , it can provide sealing in the circumferential direction without a break . according to this configuration , as no orientation is set for joining the segments , workability is improved . furthermore , outwardly extending link portions may be formed on both end portions of both segments such that the segments can be linked together by fastening screws . according to this configuration , the segments can be securely tightened against the elasticity of the grommet by fastening the link portions with the screws . furthermore , in an electric wire connection device according to another invention , sealing lips may be formed circumferentially on an inner circumferential surface side of the grommet that opposes the attachment member , the sealing lips being capable of coming into direct contact with an outer circumferential surface of the attachment member , and upon attachment of a grommet protection member to the grommet , the sealing lips may be positioned in a portion immediately below a flange . according to this configuration , as the flange of the grommet protection member compresses the portion above the sealing lips , the sealing function can be effectively enhanced . moreover , in the electric wire connection device , auxiliary lips may be provided circumferentially on the inner circumferential surface side of the grommet outside of a region tightened by the flange , the auxiliary lips being provided in locations between which the sealing lips are interposed in a front - rear direction . according to this configuration , even if the seal lips may deteriorate over time by receiving the tightening force of the flange , the sealing function can be preserved for a long period of time as the auxiliary lips are provided outside of the region tightened by the flange . hereinafter , embodiments 1 and 2 , which embody an electric wire connection device of the present invention , will be described with reference to the drawings . it should be noted that in the description below , the terms “ front and rear ” are defined so that a direction of moving away from a casing is “ rear ” and a direction of approaching the casing is “ front ”. fig1 - 9 show embodiment 1 of the present invention . more specifically , the battery power of a hybrid vehicle is supplied to a motor via an inverter . a bundle of a plurality of electric wires ( wire harness ) is used as the power feeder therebetween . fig1 shows an electric wire connection device of embodiment 1 , illustrating a connection on an inverter side . as shown in fig1 and fig2 , a through hole 2 is opened at a connecting portion of the casing 1 ( made of metal ) on the inverter side , and a casing - side connector 3 is attached to the inside of the through hole 2 , projecting outward . a hood portion 4 of the casing - side connector 3 is formed in an oval shape that is elongate in the width direction , and three male terminal fittings 5 are accommodated in the hood portion 4 and are arranged in a row in the width direction . moreover , a boss portion 6 projects rearward from the portion above the through hole 2 on the front wall of the casing 1 , and a bolt hole 7 ( screw hole ) is provided at the central portion of the boss portion 6 . in this embodiment , the wire harness w includes three electric wires . as shown in fig2 , the electric wires w 1 included in the wire harness w are collectively covered from the outside with a braided wire 8 and an outer cover 9 that is located outside the braided wire 8 . moreover , a female terminal fitting 10 is connected to the end of each electric wire w 1 . the female terminal fittings 10 are respectively accommodated in corresponding cavities in a harness - side connector 11 . the harness - side connector 11 is formed to be capable of being fitted to the hood portion 4 of the casing - side connector 3 , and the male and female terminal fittings 5 and 10 are electrically connected to each other in a proper fitting state . moreover , a first sealing ring 12 is fitted to a portion on the front end portion side of the outer circumferential surface of the harness - side connector 11 , and thus being capable of coming into direct contact with the inner circumferential surface of the hood portion 4 and providing sealing between both portions . a step 13 is formed at an intermediate portion in the longitudinal direction on the outer circumferential surface of the harness - side connector 11 , and a second sealing ring 14 is fitted to a portion near the border of the step 13 . the second sealing ring 14 comes into direct contact with the inner circumferential surface of a step portion 16 of a shielding shell 15 ( attachment member ), which will be described immediately below , in a water - tight state . the wire harness w is inserted through the shielding shell 15 as shown in fig2 , and the harness - side connector 11 is accommodated in the shielding shell 15 in a state where the harness - side connector 11 projects forward from the shielding shell 15 . a metal plate is formed into a tubular shape as the shielding shell 15 , and as shown in fig3 and fig4 , the front end portion thereof is provided with a cap portion 17 ( attached portion ) for attachment to the casing 1 . as shown in fig1 and fig3 , the cap portion 17 is open toward the casing 1 side , and has a substantially mountain - like shape in which the center on the upper end side in the drawing is a peak . an insertion hole 20 is formed in the peak portion of the cap portion 17 , and a fixing bolt 18 is inserted into the insertion hole 20 , penetrating from the rear surface side . additionally , the shielding shell 15 is fixed to the casing 1 by screwing the fixing bolt 18 into the bolt hole 7 on the casing 1 side . it should be noted that as shown in fig7 , the head of the bolt 18 is removably covered with a bolt cap 21 after the bolt 18 is screwed in . in this embodiment , the bolt cap 21 is connected , via a string - shaped hinge piece 26 , to an attachment tool ( not shown ) that is fixed together with the bolt 18 . as shown in fig4 , the step portion 16 extends rearward from the cap portion 17 , and a connecting portion 19 extends further rearward from the step portion 16 . both the connecting portion 19 and the step portion 16 are formed to have an oval cross section that is elongate in the width direction ( horizontal direction ). an opening 22 is formed on the rear end surface of the connecting portion 19 , and the wire harness w can be inserted through the opening 22 ( see fig2 ). as shown in fig2 , the outer circumferential surface of the rear end portion of the connecting portion 19 is covered with the braided wire 8 . an annular fastening tool 23 is tightened with a screw or the like , and thus the braided wire 8 is fastened and fixed to the connecting portion 19 . the step portion 16 is disposed coaxially with respect to the connecting portion 19 . the step portion 16 is formed to be slightly larger than the connecting portion 19 , having an oval cross section , and is shorter in the front - rear direction than the connecting portion 19 . the step portion 16 is continuous with the height position on the lower end portion side of the cap portion 17 , and the above - described bolt 18 is disposed at the height position spaced apart from the upper surface of the step portion 16 . as shown in fig6 and fig7 , two reinforcing ribs on both sides interposing the bolt 18 in the width direction as seen in a plan view , that is , four reinforcing ribs 25 in total , are formed by striking so as to project rearward from the rear surface of the cap portion 17 at the border portion with the upper surface of the step portion 16 . as shown in fig2 , the second sealing ring 14 of the harness - side connector 11 is caused to abut against the step between the step portion 16 and the connecting portion 19 , and thereby the harness - side connector 11 is positioned in the front - rear direction . a grommet 27 is made of a single piece of an elastic soft material ( rubber material ) in a hollow shape . as shown in fig5 , the grommet 27 is configured to include a main portion 28 , a skirt portion 29 , and a pressure attachment portion 30 interposed therebetween . the main portion 28 has an extending tubular portion 31 that extends rearward . the extending tubular portion 31 is formed in a cylindrical shape through which the wire harness w can be inserted , and is formed coaxially with the axis of the entire grommet 27 . as shown in fig2 , sealing edges 32 are formed along the entire circumferences at the opening edge and the position entering forward from the opening edge on the inner circumferential surface of the extending tubular portion 31 . the main portion 28 is formed to have an oval cross section that can be matched with the outer circumferential surface of the connecting portion 19 of a shielding case , and the main portion 28 is formed so as to be capable of surrounding the entire outer circumferential surface of the front half portion of the connecting portion 19 in a state where the grommet 27 covers the shielding shell 15 . it should be noted that as shown in fig5 and fig7 , an expanded portion 33 is formed at the position on the pressure attachment portion 30 side on the outer side surface of the main portion 28 , expanding outward in the width direction . the inside of the expanded portion 33 is a space for accommodating a fastening portion ( portion fastened by a screw or the like ) of the fastening tool 23 that fastens the above - described braided wire 8 to the connecting portion 19 of the shielding shell 15 . the pressure attachment portion 30 is formed in a recess groove shape and connects the skirt portion 29 and the main portion 28 . accordingly , its cross section has an oval shape that is slightly smaller than the main portion 28 . the outer circumferential surface of the pressure attachment portion 30 is fastened by a grommet protection member 42 , which will be explained below . in the pressure attachment portion 30 , both border walls on the connecting portion 19 side and the skirt portion 29 side have a substantially vertically rising shape . as shown in fig2 , a pair of sealing lips 36 that are spaced apart from each other in the front - rear direction projects from the central portion of the entire inner circumferential surface of the pressure attachment portion 30 . as described below , both sealing lips 36 are positioned substantially immediately below a flange 50 of the grommet protection member 42 when the grommet protection member 42 is attached . upon attachment of the grommet protection member 42 , both sealing lips 36 are moderately squeezed and come into direct contact along the outer circumferential surface of the front half portion of the connecting portion 19 of the shielding shell 15 . as shown in fig5 , a pair of auxiliary lips 37 is formed at positions close to both front and rear end portions of the inner circumferential surface of the pressure attachment portion 30 , projecting from the entire inner circumferential surface . as shown in the drawing , the projecting height of the auxiliary lip 37 is set to substantially the same height as that of the sealing lip 36 . as the auxiliary lip 37 is sufficiently spaced apart in the front - rear direction from the position immediately below the flange 50 of the grommet protection member 42 , in a state where the grommet protection member 42 fastens the auxiliary lip 37 as described below , the squeezed amount of the auxiliary lip 37 is smaller than that of the sealing lip 36 . however , the auxiliary lip 37 correspondingly has an excellent durability compared with the sealing lip 36 , and it can be expected to maintain the sealing performance for a long period of time . the grommet 27 of this embodiment has a shape in which the skirt portion 29 extends further forward from the pressure attachment portion 30 . the skirt portion 29 is open forward , and is formed to have an oval cross section that can be fitted to the outer circumferential surface of the step portion 16 of the shielding shell 15 . the skirt portion 29 is formed to come into direct contact along the outer circumferential surface of the step portion 16 together with the rising wall rising from the pressure attachment portion 30 in a state where the grommet 27 is attached to the shielding shell 15 . moreover , the skirt portion 29 excluding a part of its upper surface is formed to have substantially the same front - rear width as the front - rear width of the step portion 16 . as shown in fig5 and fig6 , a cut - out portion 38 is formed at the front edge portion of the region near the central portion of the upper surface of the skirt portion 29 , that is , the region in which the above - described reinforcing ribs 25 of the shielding shell 15 are formed , in order to prevent interference with the reinforcing ribs 25 . the central portion in the width direction of the front edge of the cut - out portion 38 is provided with a recess 39 by cutting out a range of a predetermined width . the recess 39 is for preventing interference with the bolt cap 21 , and a thin portion 39 a that is thinner than its surroundings ( by thinning the outer surface side ) is formed in a region on the front side of the portion in which the recess 39 is formed . two turn - up preventing ribs 40 are formed on both sides interposing the recess 39 of the cut - out portion 38 in the width direction . the turn - up preventing ribs 40 are each formed in the front - rear direction in a range extending from the front edge to the rear edge of the cut - out portion 38 . next , the grommet protection member 42 will be described . by surrounding the entire outer circumferential surfaces of the skirt portion 29 of the grommet 27 and the pressure attachment portion 30 , the grommet protection member 42 , can protect the outer circumferential surfaces of the skirt portion 29 and the pressure attachment portion 30 from high - pressure washing water and prevent the opening edge of the skirt portion 29 of the grommet 27 from turning up . moreover , in addition to the above - described function , the grommet protection member 42 has the function of fastening the skirt portion 29 of the grommet 27 . as shown in fig1 , the grommet protection member 42 of embodiment 1 is configured to include a pair of segments 42 a that are both formed into an identical shape . both segments 42 a are formed of a resin plate that is harder than the material of the grommet 27 . both segments 42 a are formed to have a protection portion 43 , a pair of link portions 44 extending outward in the width direction from both ends of the protection portion 43 , and a flange 50 that is formed to project from the inner circumferential surfaces of both segment 42 a . as shown in fig2 and 6 , the protection portions 43 of both segments 42 a have a front - rear width that is approximately equal to or slightly shorter than the length from the front edge of the skirt 29 of the grommet 27 to the rear edge of the pressure attachment portion 30 , and the segments 42 a are formed into a shape that conforms to the shape of the outer circumferential surface of the grommet 27 . as shown in fig2 , in a state where the grommet protection member 42 is attached to the grommet 27 , the inner surfaces of the protection portions 43 of both segments 42 a are in approximately direct contact along the outer circumferential surface of the skirt portion 29 , and the front edges thereof are positioned slightly forward of the front edge of the skirt portion 29 and adapted to approximately abut against the rear surface of the cap portion 17 of the shielding shell 15 . as shown in fig8 and 9 , when joined together , both segments 42 a surround the skirt portion 29 and the pressure attachment portion 30 of the grommet 27 , coming into direct contact along the entire circumferential surfaces of the portions . the front edge portion of the protection portion 43 of the segment 42 a is cut out to form a drain opening 45 . the drain opening 45 drains water entering between the grommet protection member 42 and the grommet 27 and prevents the inside of the grommet protection member 42 from being filled with water . the dimension in the width direction of the drain opening 45 is set to be approximately the same as the width dimension of the cut - out portion 38 of the grommet 27 , and its dimension in the depth direction ( front - rear direction ) is set to be approximately the same as the length dimension from the front edge of the skirt portion 29 of the grommet 27 to the rear edge of each turn - up preventing rib 40 . as shown in fig6 , in a state where the grommet protection member 42 is attached to the grommet 27 , the drain opening 45 is matched with the region in which the turn - up preventing ribs 40 of the grommet 27 are formed to expose the entire region . on the other hand , the link portions 44 are formed to protrude from the approximately central portions of both edges of the protection portion 43 . a through hole 47 penetrates the central portion of each link portion 44 to pass a bolt 46 therethrough . in a state where both segments 42 a are joined together from the upward and downward directions , both protection portions 43 form a loop having an oval shape , surrounding the entire outer circumferential surfaces of the skirt portion 29 and the pressure attachment portion 30 of the grommet 27 . moreover , in a state where both segments 42 a are joined , the through holes 47 of the corresponding link portions 44 are aligned with each other , and both segments 42 a are held in a joined state with bolts 46 and nuts 49 . furthermore , as shown in fig1 , fig9 , etc ., the flange 50 is integrally formed on the inner surfaces of the protection portions 43 of both segments 42 a . the flange 50 is formed circumferentially along the entire length of the segments 42 a , protruding from a position on the rear edge of the segments 42 a rear of the link portions 44 . both end surfaces of the flange 50 are formed into flat surfaces that are flush with both end surfaces of the protection portion 43 . accordingly , in a state where both segments 42 a are joined together , the end surfaces of both segments 42 a are brought into abutment with each other , while the corresponding end surfaces of the flange 50 are brought into alignment and abutment with each other . as a result , in the joined state , the flange 50 continuously surrounds the entire outer circumferential surface of the attachment pressure portion 30 of the grommet 27 in the same plane . as previously described , when the grommet protection member 42 is attached to the grommet 27 , the flange 50 is positioned on the outer circumferential surface of the pressure attachment portion 30 of the grommet 27 so that the sealing lips 36 are approximately immediately below the flange 50 . in particular , the flange 50 is adapted to pressure the area between both sealing lips 36 . moreover , the protruding height of the flange 50 is set to be able to come into contact with and press against the outer circumferential surface of the pressure attachment portion 30 of the grommet 27 so as to properly compress the sealing lips 36 once the grommet protection member 42 is attached to the grommet 27 . the flange 50 is formed to have a curved shape with a protruding rounded edge . next , the effects of this embodiment 1 configured as described above will be described . an example of operations for connecting the end portion of the wire harness w to the casing 1 is described . first , the harness - side connector 11 , the shielding shell 15 , and the grommet 27 are attached to the end portion of the wire harness w ( as shown in fig1 ). to attach the grommet 27 , the skirt portion 29 is fitted to come into direct contact with the outer circumferential surface of the step portion 16 of the shielding shell 15 so that the recess 39 of the grommet 27 is positioned below the insertion hole 20 of the shielding shell 15 . subsequently , one of the segments 42 a of the grommet protection member 42 is matched with the skirt portion 29 and the pressure attachment portion 30 of the grommet 27 from below , and the other segment 42 a is fitted from the above . then , the corresponding link portions 44 of both segments 42 a are aligned with each other . next , the bolts 46 and the nuts 49 are tightened via the through holes 47 to hold both segments 42 a in a joined state . at this point , the front edge of the grommet protection member 42 is aligned with or slightly forward of the front edge of the skirt portion 29 of the grommet 27 , thereby ensuring that the front edge portion of the grommet 27 is covered with the grommet protection member 42 . in this way , as the grommet protection member 42 is split into two pieces in a radial direction ( vertical direction ) in this embodiment 1 , the grommet protection member 42 can be easily attached to the grommet 27 . moreover , upon joining of both segments 42 a , the flange 50 of the grommet protection member 42 assumes a circumferentially continuous form to come into contact with and press against the entire outer circumferential surface of the pressure attachment portion 30 of the grommet 27 . at this point , as the shielding lips 36 are positioned approximately directly below the flange 50 , the shielding lips 36 are properly compressed around their entire circumferences so as to be in direct contact with the outer circumferential surface of the connecting portion 19 of the grommet 27 in a water - tight manner . the harness - side connector 11 and the casing - side connector 3 are then fitted to each other . in that process , the cap portion 17 of the shielding shell 15 is caused to hit against the wall surface of the casing 1 , concealing the projecting portion of the casing - side connector 3 and the boss portion 6 . when the bolt 18 is screwed into the bolt hole 7 of the boss portion 6 in this state , the shielding shell 15 is fixed , and the operations for connecting the end portion of the wire harness w to the casing 1 side are completed . incidentally , as previously described , high - pressure washing water is sometimes blown to the portion in which the end portion of the wire harness w is connected to the casing 1 . in this embodiment 1 , as a measure taken against that , first , the flange 50 is integrally formed on the grommet protection member 42 so as to be able to reliably cut off water between the grommet 27 and the shielding shell 15 . if a dedicated fastening component , such as a bundling band , is employed to seal the grommet 27 to the shielding shell 15 , the number of components is increased , and the number of operations is also increased due to the addition of the tightening operation . in that regard , in this embodiment , as the flange 50 is integrally formed on the grommet protection member 42 , the number of components does not increase . moreover , as the sealing between the shielding shell 15 and the grommet 27 is completed simultaneously with the operation of attaching the grommet protection member 42 to the grommet 27 , the work efficiency is increased without increasing the number of operations . furthermore , as the sealing lips 36 are positioned approximately directly below the flange 50 , the flange 50 can be reliably caused to compress the sealing lips 36 . moreover , the end portion of the grommet 27 is surrounded by and covered with the grommet protection member 42 . more specifically , the grommet protection member 42 conceals the entire circumference of the front - rear range of the grommet 27 that extends from the front edge of the skirt portion 29 nearly to the rear edge of the pressure attachment portion 30 . accordingly , as the skirt portion 29 and the pressure attachment portion 30 of the grommet 27 are not directly exposed to high - pressure washing water , such that the front edge of the skirt portion 29 of the grommet 27 can be prevented from turning up . moreover , during washing , high - pressure washing water enters the inside of the grommet protection member 42 through the gap between the pressure attachment portion 30 and the grommet protection member 42 . however , as the water is smoothly drained through the drain openings 45 , the situation in which the sealing is reduced due to the pressure of water filled in the inside of the grommet protection member 42 can be avoided . furthermore , in the grommet 27 of embodiment 1 , the skirt portion 29 further extends from the pressure attachment portion 30 and is brought into direct contact with the step portion 16 of the shielding shell 15 . that is , although the pressure attachment portion 30 is usually formed as the end portion of the grommet 27 , in this embodiment , a channel through which water infiltrates inside the grommet 27 is elongated by extending the skirt portion 29 , which also enhances water resistance . furthermore , there is a concern that the sealing lips 36 are likely to be deteriorated by receiving the fastening force by the flange 50 . as a measure taken against such a problem , in this embodiment , the auxiliary lips 37 are formed outside the region to be fastened , such that a constant sealing force is also obtained at that region . accordingly , it is possible to maintain a constant sealing function for a long period of time . fig1 shows embodiment 2 of the present invention . fig1 shows the inner surface of a segment 60 a of a grommet protection member according to embodiment 2 . in embodiment 1 , the flange 50 was shown to have a form continuous for the entire length of both segments 60 a . in embodiment 2 , however , the flange 61 is divided into a plurality of segments longitudinally ( circumferentially ) at certain intervals in a staggered arrangement of two adjacent rows , one in the front and one in the rear , such that the segments of the flange 61 overlap each other in the front - rear direction . although each row of the flange 61 is arranged to have breaks in the circumferential direction , the overlapping positional relationship between the front and rear rows creates a condition in which they press against the sealing lips of the grommet along the entire circumference thereof without a break . the configuration is otherwise identical with embodiment 1 , such that identical effects to those of embodiment can be exerted . the present invention is not limited to the embodiment explained by the above description and the drawings . other embodiments , which will be explained below , for example , are also included in the technical scope of the present invention . although , in the above - described embodiment , a configuration was shown in which the flange 50 was provided with a uniform height along their entire circumference , the height may not have to be uniform . for example , if the grommet protection member 42 is elongated in the width direction ( vertical direction as seen in fig8 ), there is a concern that the pressing force against the grommet is reduced in the central portion compared with that in the end portions . in such a case , the flange 50 may be formed to have a height gradually increasing from both ends in the width direction to the central portion in order to provide a uniform sealing pressure . although , in the above - described embodiment , the grommet protection member 42 was made of a synthetic resin , it may be made of metal . although , in the above - described embodiment , a configuration in which the skirt portion 29 extended from the grommet 27 was shown , the skirt portion 29 may not have to be provided . rather , the pressure attachment portion 30 may form the longitudinal end portion . although , in the above - described embodiment , the grommet protection member 42 was divided into the two independent segments 42 a , the segments 42 a may be connected with a hinge at one end so that they can be opened and closed and may be provided with link portions only on the other end . in that case , the means for fastening the link portions is not limited to a bolt and a nut . a clip provided on one link portion and a hole provided in the other will be sufficient , and various other forms of such elastic locking means can also be contemplated . although , in the above - described embodiment , the auxiliary lips 37 were provided on the grommet 27 , they may be omitted . localized pressure is applied to the shielding shell 15 on the grommet 27 immediately below the flange 50 . accordingly , if a sufficient sealing function is exerted in this region , the sealing lips 36 may be omitted . | 7 |
fig1 shows rigid frame 100 that provides structural support for a bag in the baggage system of the present invention . rigid frame 100 is preferably formed using 0 . 25 - inch solid aluminum rods , with top rounded corners 101 - 104 . rigid frame 100 is sewn between the outer material of the bag and the waterproof inside lining of the bag . fig2 ( a )- 2 ( c ) show side , front and back panels of primary bag 200 , in accordance with one embodiment of the present invention . in this embodiment , for example , primary bag 200 has dimensions 17 inches by 13 inches by 9 inches . other suitable sizes are possible . as shown in fig2 ( c ), primary bag 200 includes handle 201 , anchor - straps 202 a and 202 b , and wrap - around straps 203 a - 203 e . anchor - straps 202 a and 202 b , which are provided for wrapping around the metal bars of a baggage rack of a motorcycle , prevent the bag from lifting up off the luggage rack . wrap - around straps 203 a - 203 e ( preferably formed of webbing material ) are designed for wrapping around a passenger &# 39 ; s back rest of a motorcycle to prevent the bag from moving in the direction of travel . self - repairing zipper 204 , which is provided across the front panel and the side panels of primary bag 200 , allows access to the inside of primary bag 200 and secures its contents while in motion . in one embodiment , the outer material of primary bag 200 is preferably lamb skin leather . inside the bag , a waterproof lining is preferably provided . a suitable material for the waterproof lining may be , for example , plastic . as discussed above , a rigid frame ( e . g ., rigid frame 100 of fig1 ) provides structural support for primary bag 100 . both side panels of primary bag 200 may be made substantially the same . as shown in fig2 ( a ), each side panel of primary bag 200 is provided side - strap 205 for securing one or more side pouches to a side panel of primary bag 200 . as shown in fig2 ( b ), on the front panel , front - straps 206 a and 206 b are provided to secure front pouches . side strap 205 and 15 front - straps 206 a and 206 b are preferably made from webbing material . as shown in fig2 ( c ), a ring ( 215 a , 215 b , 215 c , 215 d ) is attached to each corner of the back panel of the primary bag 200 to allow a secondary bag to be attached by means of clips ( preferably , metal clips ). fig3 ( a )- 3 ( c ) show side , front and back panels of secondary bag 300 , in accordance with one embodiment of the present invention . as in primary bag 200 , a rigid frame ( e . g ., rigid frame 100 ) is sewn between the outer material ( e . g ., lamb skin leather ) and the waterproof ( e . g ., plastic ) inside lining of secondary bag 300 . in this embodiment , both side panels of secondary bag 300 are substantially the same . as shown in fig3 ( c ), secondary bag 300 includes handle 301 and material 302 , which is attached along the top and bottom edges of the back panel of secondary bag 300 to create a cavity between material 302 and the back panel of the secondary bag 300 . material 302 is preferably lamb skin leather . wrap - around straps 203 a - 203 e of the primary bag 200 pass through the cavity behind material 302 , so that secondary bag 300 may be secured on the passenger &# 39 ; s back rest along with the primary bag , and thereby prevents secondary bag 300 from sliding in the direction of travel . self - repairing zipper 304 , which is provided across the front panel and the side panels of secondary bag 300 , allows access to the inside of secondary bag 300 and secures its contents while in motion . in this embodiment , both side panels of secondary bag 300 are substantially the same . as shown in fig3 ( a ), each side panel of secondary bag 300 is provided side - strap 305 for securing one or more side pouches to the side panel . as shown in fig3 ( b ), on the front 35 panel , front - straps 306 a and 306 b are provided to secure front pouches . side strap 305 and front - straps 306 a and 306 b are preferably made from webbing material . as shown in fig3 ( c ), a clip ( 316 a , 316 b , 316 c , 316 d ) is provided at each corner of the back panel of the secondary bag 300 to help secure secondary bag 300 to a primary bag ( e . g ., primary bag 200 of fig2 ( a )- 2 ( c )) and to prevent secondary bag 300 from rotating around the passenger &# 39 ; s back rest . the clips are preferably made of metal . the front and side panels of the primary and the secondary bags are equipped to support additional pouches that may be attached . fig4 ( a )- 4 ( b ) show front and side views of single front pouch 400 , according to one embodiment of the present invention . as shown in fig4 ( a ) and 4 ( b ), single front pouch 400 has dimensions 13 inches by 14 inches by 2 . 5 inches . other suitable sizes are also possible . single front pouch 400 may be attached to either a primary bag or a secondary bag . as shown in fig4 ( b ), back panel 401 of single front pouch 400 is provided by a stiff backing material ( e . g ., a stiff cowhide ) on which solid pieces of material 402 a and 402 b ( e . g ., lamb skin leather ) are attached . each solid piece of material is attached to back panel 401 along its top and bottom edges to create a cavity between the material and back panel 401 through which one of front - straps of the primary or secondary bag ( e . g ., 206 a or 206 b of primary bag 200 , or 306 a or 306 b of secondary bag 300 ) may pass through to secure front pouch 400 to the primary or secondary bag . flap 403 is provided to cover single compartment 404 and to provide access to the inside of front pouch 400 , which is preferably lined by a waterproof plastic material . fig5 ( a ) and 5 ( b ) show front and side views of dual - compartment front pouch 500 , according to one embodiment of the present invention . as shown in fig5 ( a ) and 5 ( b ), dual - compartment front pouch 500 includes compartments 504 a and 504 b . front pouch 500 may be attached to either a primary bag or a secondary bag . as shown in fig5 ( b ), back panel 501 of front pouch 500 is provided by a stiff backing material ( e . g ., a stiff cowhide ) on which solid pieces of material 502 a and 502 b ( e . g ., lamb skin leather ) are attached . each solid piece of material is attached to back panel 501 along its top and bottom edges to create a cavity between the material and back panel 501 through which one of front - straps of the primary or secondary bag ( e . g ., 206 a or 206 b of primary bag 200 , or 306 a or 306 b of secondary bag 300 ) may pass through to secure front pouch 500 to the primary or secondary bag . flaps 503 a and 503 b are provided to cover and to provide access to the inside each of compartments 504 a and 504 b of front pouch 500 , which is preferably lined by a waterproof plastic material . fig6 ( a )- 6 ( c ) show front , side and top views of single - compartment side pouch 600 , according to one embodiment of the present invention . side pouch 600 had dimensions 6 inches by 14 inches by 2 . 5 inches and may be attached to the side of either a primary bag or a secondary bag ( e . g ., primary bag 200 of fig2 or secondary bag 300 of fig3 ) . back panel 601 may be formed out of the same stiff backing material ( e . g ., cowhide ) as the back panel 501 of fig5 ( b ). solid piece of material 602 ( e . g ., lamb skin leather ) is attached along the left and right edges of back panel 601 to create a cavity between material 602 and back panel 601 , allowing a side - strap ( e . g ., side - strap 205 of fig2 or side - strap 305 of fig3 ) to pass through , so as to secure side pouch 600 to the side panel of a primary bag or a secondary bag . flap 603 covers the top of the single compartment of side pouch 600 in order to safely secure the contents inside . fig7 ( a )- 7 ( c ) show front , side and top views of dual - compartment side pouch 700 , according to one embodiment of the present invention . side pouch 700 may be attached to the side of either a primary bag or a secondary bag ( e . g ., primary bag 200 of fig2 or secondary bag 300 of fig3 ) . back panel 701 may be formed out of the same stiff backing material ( e . g ., cowhide ) as the back panel 501 of fig5 ( b ). solid piece of material 702 ( e . g ., lamb skin leather ) is attached along the left and right edges of back panel 701 to create a cavity between material 702 and back panel 701 , allowing a side - strap ( e . g ., side - strap 205 of fig2 or side - strap 305 of fig3 ) to pass through , so as to secure dual - compartment side pouch 700 to the side panel of a primary bag or a secondary bag . flaps 703 a and 703 b cover the top and bottom compartments of side pouch 700 in order to safely secure the contents inside . fig8 ( a )- 8 ( c ) show front , side and top views of cold - drink pouch 800 , according to one embodiment of the present invention . cold - drink pouch 800 may be attached to the side of either a primary bag or a secondary bag ( e . g ., primary bag 200 of fig2 or secondary bag 300 of fig3 ) . back pane 801 may be formed out of the same stiff backing material ( e . g ., cowhide ) as the back panel 501 of fig5 ( b ). solid piece of material 802 ( e . g ., lamb skin leather ) is attached along the left and right edges of back panel 801 to create a cavity between material 802 and back panel 801 , allowing a side - strap ( e . g ., side - strap 205 of fig2 or side - strap 305 of fig3 ) to pass through , so as to attach cold - drink pouch 800 to the side panel of a primary bag or a secondary bag . self - repairing zipper 805 is provided at near the top of cold - drink pouch 800 along the top surface and the side surfaces to provide access to contents of cold - drink pouch 800 . the inside of cold - drink pouch 800 may be lined by a waterproof plastic and thermally insulated from the outside . the above detailed description is provided to illustrate specific embodiments of the present invention and is not intended to be limiting . numerous variations and modifications of the present invention are possible . the present invention is set forth in the accompanying claims . | 1 |
while the present teachings are described in conjunction with various embodiments and examples , it is not intended that the present teachings be limited to such embodiments . on the contrary , the present teachings encompass various alternatives , modifications and equivalents , as will be appreciated by those of skill in the art . referring to fig2 a , an optical device 200 a of the invention includes a wavelength division multiplexor 202 a coupled to an optical grating demultiplexor 210 . the wavelength division multiplexor 202 a has an input port 204 and first and second output ports 206 and 208 , respectively . the function of the wavelength division multiplexor 202 a is to separate wavelength channels λ 1 to λ 8 received at the input port 204 into first and second groups of wavelength channels λ 1 to λ 4 and λ 5 to λ 8 , respectively , and direct them to the first and the second output ports 206 and 208 , respectively . the first and the second output ports 206 and 208 are coupled to first and second input ports 212 and 214 , respectively , of the optical grating demultiplexor 210 . the function of the optical grating demultiplexor 210 is to demultiplex the first and the second groups of wavelength channels λ 1 to λ 8 and to direct the demultiplexed channels towards a plurality of output ports 216 to 219 of the optical grating demultiplexor 210 . the first and the second input ports 212 and 214 of the optical grating demultiplexor 210 are offset from each other so as to couple a wavelength channel of the first group λ 1 to λ 4 from the first input port 212 , together with a wavelength channel of the second group λ 5 to λ 8 from the second input port 214 , into a same output port 216 , 217 , 218 , or 219 , of the optical grating demultiplexor 210 . thus , the output port 216 has the wavelength channels λ 1 and λ 5 ; the output port 217 has the wavelength channels λ 2 and λ 6 ; the output port 218 has the wavelength channels λ 3 and λ 7 ; and the output port 219 has the wavelength channels λ 4 and λ 8 . advantageously , the presence of two offset input ports 212 and 214 allows the wavelengths λ 1 and λ 5 to be individually selectable by adjusting the magnitude of the offset between the input ports 212 and 214 . the wavelength adjustability will be illustrated further below . turning now to fig2 b , an optical device 200 b is an alternative embodiment of the optical device 200 a . one difference between the optical devices 200 a and 200 b is that the optical device 200 b includes an optical interleaver 202 b instead of the wdm filter 202 a . the function of the optical interleaver 202 b is to separate wavelength channels λ 1 to λ 8 received at the input port 204 into first and second groups of wavelength channels λ 1 , λ 3 , λ 5 , λ 7 and λ 2 , λ 4 , λ 6 , λ 8 , respectively , and direct them to the first and the second output ports 206 and 208 , respectively . the optical interleaver preferably has an input channel spacing twice as small as a channel spacing of the optical grating demultiplexor 310 . advantageously , the optical grating demultiplexor 210 can have a larger channel spacing than the channel spacing of an optical network wherein the optical device 200 b is used . for example , the optical grating demultiplexor 210 can have a 100 ghz channel spacing , while the optical network it is used in can have a 50 ghz channel spacing . as noted above , one important advantage of the invention is the adjustability of wavelengths of the channels that are coupled together in the same output port 216 , 217 , 218 , or 219 of the optical grating demultiplexor . turning to fig2 c , an optical device 200 c is shown . the optical device 200 c is a variant of the optical device 200 b . one difference between the optical devices 200 b and 200 c is that an optical grating demultiplexor 211 of the optical device 200 c has an input 220 that is offset by an additional amount of as compared to a position of the corresponding input 214 of the optical grating demultiplexor 210 of the optical device 200 b of fig2 b . the additional offset is illustrated at 225 in fig2 c . the additional offset determines which ones of the wavelength channels λ 2 , λ 4 , λ 6 , λ 8 are coupled to which ones of the output ports 216 to 219 of the optical grating demultiplexor 211 . referring now to fig3 , a spectrum 311 shows the wavelength channels λ 1 to λ 8 at the input port 204 of the optical devices 200 b and 200 c of fig2 b and 2c . in fig3 , a spectrum 312 shows the wavelength channels λ 1 , λ 3 , λ 5 , λ 7 at the upper input port 212 of the optical grating demultiplexors 210 and 211 . a spectrum 313 shows even wavelength channels λ 2 , λ 4 , λ 6 , λ 8 at the lower input port 214 of the optical grating demultiplexor 210 of fig2 b . in fig3 , the spectrum 313 is shifted so that the even wavelength channels λ 2 , λ 4 , λ 6 , λ 8 line up with the odd wavelength channels λ 1 , λ 3 , λ 5 , λ 7 , due to the offset between the input ports 212 and 214 of the optical grating demultiplexor 210 of fig2 b . as a result of the offset , the pairs of wavelength channels λ 1 and λ 2 ; λ 3 and λ 4 ; λ 5 and λ 6 ; λ 7 and λ 8 are coupled into the output ports 216 to 219 , respectively . the output ports 216 to 219 are shown in fig3 lined up with the corresponding wavelength channel pairs λ 1 and λ 2 ; λ 3 and λ 4 ; λ 5 and λ 6 ; λ 7 and λ 8 . a spectrum 314 shows the even wavelength channels λ 2 , λ 4 , λ 6 , λ 8 at the lower input port 220 of the optical grating demultiplexor 211 of fig2 c . in fig3 , the spectrum 314 is shifted as shown at 325 so that the wavelength channels λ 4 , λ 6 , λ 8 line up with the wavelength channels λ 1 , λ 3 , λ 5 due to the additional offset shown at 225 . as a result of the additional offset , the pairs of wavelength channels λ 1 and λ 4 ; λ 3 and λ 6 ; λ 5 and λ 8 are coupled into the output ports 216 to 218 , respectively . the output ports 216 to 218 are shown in fig3 lined up with the corresponding wavelength channel pairs λ 1 and λ 4 ; λ 3 and λ 6 ; λ 5 and λ 8 . the remaining wavelength channels λ 2 and λ 7 are coupled into an additional output port 315 and the output port 219 , respectively . the additional output port 315 is not shown in fig2 c . by properly selecting the additional offset , one can increase the wavelength separation of the wavelength channels coupled together into a same output port of the optical grating demultiplexor 211 . in fig3 , for example , wavelength channel pairs λ 1 and λ 4 at the output port 216 are separated three times more than the input channels λ 1 and λ 2 . advantageously , selecting wavelength channels that are separated by at least three times more than the input channel spacing to be directed to a same output port , simplifies subsequent demultiplexing of these channels , because of the increased wavelength separation of these wavelength channels . at the same time , the advantage brought in by the interleaver 202 b , specifically a wider channel spacing of the optical grating demultiplexor 211 , is kept . in other words , the optical grating demultiplexor 211 can have a channel spacing that is twice bigger than the channel spacing at the input of the optical device 200 c . referring now to fig4 , a more general form of an optical device of the invention is presented . an optical device 400 of the invention has a 1 : m wavelength selective coupler 402 having one input port 404 and m output ports 406 - 1 . . . 406 - m , wherein m ≧ 3 . the 1 : m wavelength selective coupler 402 is coupled to an m : n optical grating demultiplexor 410 having m input ports 412 - 1 . . . 412 - m and n output ports 416 - 1 . . . 416 - n , wherein n ≧ 3 . the m output ports 406 - 1 . . . 406 - m of the 1 : m wavelength selective coupler 402 are coupled to the m input ports 412 - 1 . . . 412 - m of the m : n optical grating demultiplexor 410 , respectively . the function of the 1 : m wavelength selective coupler 402 is to separate wavelength channels λ 1 1 . . . λ n 1 , λ 1 2 . . . λ n 2 , . . . , and λ 1 m . . . λ n m into m groups of wavelength channels λ 1 1 . . . λ n 1 ; λ 1 2 . . . λ n 2 ; . . . ; and λ 1 m . . . λ n m , each group being directed to a corresponding output port 406 - 1 ; 406 - 2 ; . . . ; 406 - m . the function of the optical grating demultiplexor 410 is to demultiplex wavelength channels of each of the m groups received at m input ports 412 - 1 . . . 412 - m and to direct the demultiplexed channels λ 1 1 . . . λ 1 m ; λ 2 1 . . . λ 2 m ; . . . ; and λ n 1 . . . λ n m towards the output ports 416 - 1 . . . 416 - n , respectively . by properly selecting the positions of the input ports 412 - 1 . . . 412 - m of the m : n optical grating demultiplexor 410 , one can select which wavelength channels are directed to which one of the output ports 416 - 1 . . . 416 - n . the positions of the input ports are selected based on a grating equation of an optical grating used in the m : n optical grating demultiplexor 410 . the grating equations of some commonly used optical gratings are given further below . the wdm coupler 202 a or 402 can use any type of a wavelength selective filter such a dichroic ( thin film ) optical filter , for example . the wdm couplers 202 a and 402 and the interleaver 202 b can be replaced with any other type of a wavelength selective coupler for separating wavelength channels received at the input port 204 into at least two groups of ( not necessarily adjacent ) wavelength channels . the optical interleaver 202 b preferably includes at least one mach - zehnder ( mz ) interferometer . two serially coupled mz interferometers forming a lattice filter are further preferable . the optical grating demultiplexors 210 , 211 , and 410 can include an arrayed waveguide grating ( awg ), a bulk echelle grating , a slab echelle grating , or a bulk diffraction grating . referring to fig5 , an optical device 500 of the invention includes serially coupled a 1 × 2 wavelength selective coupler 502 and an awg demultiplexor 510 having an input slab section 521 , a waveguide section 522 coupled to the input slab section 521 , an output slab section 523 coupled to the waveguide section 522 , two input waveguides 512 and 514 coupled to the input slab section 521 , and a plurality of output waveguides 516 to 519 coupled to the output slab sections 523 . the awg demultiplexor 510 is preferably based on an athermal awg using any athermal awg types known to a person skilled in the art . the wavelength selective coupler 502 is preferably waveguide based , so it can be integrated on the same waveguide substrate as the awg demultiplexor 510 . the principle of adjustability of which wavelength channel is directed to which output port ( depending on the input port position ) will now be explained . the relative position of the input ports 212 and 214 of the optical grating demultiplexor 210 ; the relative position of the input ports 212 and 220 of the optical grating demultiplexor 211 ; the relative position of the input ports 412 - 1 . . . 412 - m of the m : n optical grating demultiplexor 410 ; and the relative position of the input ports 512 and 514 of the arrayed waveguide grating demultiplexor 510 is defined by a grating equation of a particular optical grating used in these devices . the grating equations of various optical gratings are known to one of ordinary skill in the art . the grating equation of an arrayed waveguide grating , for example , is n s ( λ ) p sin ( θ in )+ n s ( λ ) p sin ( θout )+ n w ( λ ) δ l = mλ ( 1 ), wherein n s ( λ ) is a refractive index of the slab sections 521 and 523 , n w ( λ ) is a refractive index of the waveguide section 522 , θ in is an input beam angle of an optical beam emitted by the input waveguide 512 or the input waveguide 514 , θ out is an output beam angle of an optical beam coupled into the output waveguides 516 to 519 , δl is an optical path difference between neighboring waveguides of the waveguide section 522 , p is a waveguide spacing of the waveguide section 522 , and m is an order of diffraction . according to the grating equation ( 1 ), by selecting proper angles θ in , which depends on a position of an input waveguide , different wavelength channels can be coupled into a same output waveguide in a different orders of diffraction m or even in a same order of diffraction m . the grating equation of a free - space diffraction grating is similar to equation ( 1 ) above : wherein n is refractive index of a medium the diffraction grating is in , and d is a groove spacing of the diffraction grating . by properly selecting the input beam angles θ in , one can couple different wavelength channels into a same output port . the input beam angles θ in and the output beam angles θ out depend on position of the input and output ports of the free - space diffraction grating and on a focal length of a lens or lenses used to collimate the input and the output beams . these free space lenses correspond to the input and the output slabs 521 and 523 of the arrayed waveguide grating demultiplexor 510 of fig5 . in the optical grating demultiplexors 210 , 211 , and 410 , the input ports 212 , 214 , 220 , and 412 - 1 to 412 - m can be disposed so that different wavelength channels can be directed to a same output port by diffracting into different orders of diffraction . this provides for a freedom to space the input ports apart by enough of a distance to prevent crosstalk , for example . furthermore , according to the present invention and the equations ( 1 ) and ( 2 ) above , the input ports 212 , 214 , 220 , and 412 - 1 to 412 - m can also be disposed so that different wavelength channels are directed to a same output port by diffracting into a same order of diffraction m . this provides an important design benefit because the optical grating demultiplexors 210 , 211 , and 410 do not need to be optimized for operation in different orders of diffraction , which allows one to achieve a better optical performance in a single order of diffraction m . turning now to fig6 , an optical network 600 of the invention includes nodes 602 and 604 coupled by a length of an optical fiber 606 . each of the nodes includes the optical device 200 a of the invention , a plurality of duplex filters 612 coupled to the output ports 216 to 219 of the optical grating demultiplexors 210 , for separating wavelength channels present at the output ports 216 to 219 , a plurality of receivers 620 each coupled to a particular one of the duplex filters 612 , and a plurality of transmitters 630 each coupled to a particular one of the duplex filters 612 . as seen in fig6 , the wavelength channels λ 5 to λ 8 are transmission wavelength channels for the node 602 and are accordingly reception wavelength channels for the node 604 . the wavelength channels λ 1 to λ 4 are reception wavelength channels for the node 602 and are transmission wavelength channels for the node 604 . of course , the wavelength selective coupler 502 , the interleaver 202 b , or the 1 × m wavelength selective splitter 402 can be used in place of the wavelength division multiplexor 202 a , and the awg demultiplexor 510 , the optical grating demultiplexor 211 , or the m × n optical grating demultiplexor 410 can be used in place of the optical grating demultiplexor 210 . the transmitters 630 are preferably laser diodes , although light emitting diodes ( leds ) can also be used . the receivers 620 are preferably pin or avalanche photodiodes . | 6 |
fig1 through 3b show a solid - state light emitting display and a fabrication method thereof according to a first embodiment of the present invention . referring to fig1 , solid - state light emitting display of this embodiment at least comprises a metallic board 1 and a plurality of luminous microcrystals 3 . the metallic board 1 is preferably a flexible sheet , its thickness is , e . g ., under 500 . mu . m , but it is not limited to this , e . g . it can also be an inflexible sheet . the metallic board 1 can be selected from stainless steel , such as number 304 , 316 , 430 aluminum alloy , such as series 2 to series 6 , and plate that is made from other suitable metal , and the metallic board 1 has formed conductive circuitry 11 thereon . in this exemplary embodiment , the conductive circuitry 11 can be fabricated by the conventional ic ( integrated circuit ) fabricating process or other suitable fabricating process , so as to make the conductive circuitry 11 include a plurality of electrical connecting pads 111 and ic ( integrated circuit ) components 113 . to illustrate the drawing in a clear and concise manner , the drawing in the present application is directed to merely part of the metallic board 1 and conductive circuitry 11 . the electrical connecting pads 111 can be , e . g ., bond pad made from gold , the ic component 113 can be , e . g ., active component , passive component , tft ( thin - film transistor ) component or other suitable component , but they are not limited to all these . concurrently , the metallic board 1 can perform contact or non - contact or the like polishing and smoothing fabricating process , so as to keep the surface flat . furthermore , a silicon oxide insulating layer 13 is further set between the metallic board 1 and the conductive circuitry 11 , thereby avoiding short circuit of the metallic board 1 for contacting with the conductive circuitry 11 , the thickness of the insulating layer 13 is e . g ., less than 10 . mu . m . the luminous microcrystals 3 is disposed on the surface of the metallic board 1 and set a conductive connecting device 14 to electrically connect with the conductive circuitry 11 ; before setting the luminous microcrystals 3 on the metallic board 1 , firstly removing the insulating layer 13 at the position where setting the luminous microcrystals 3 on the metallic board 1 , so that the luminous microcrystals 3 can contact and then conduct with the metallic board 1 . in the exemplary embodiment , such luminous microcrystals 3 are fabricated by the light emitting diode wafer through the microcrystalline fabricating process , and the light emitting diode wafer is fabricated by the epitaxy fabricating process . microcrystalline fabricating process is shown in fig2 a , epitaxial layer 101 including a plurality of light emitting diodes as luminous microcrystals is formed on the substrate for epitaxy 10 by light emitting diode wafer through dry etching technology , and the light emitting diode wafer is fabricated by the conventional epitaxy fabricating process , when removing the substrate for epitaxy 10 and detaching the epitaxial layer 101 , structures of many tiny bare crystals , i . e . luminous microcrystals 3 shown in fig2 b is formed . at this time , by virtue of the self - assembly technology , such as pick - and - place assembly of single component , parallel assembly , or the other suitable assembly technology , the luminous microcrystals 3 are assembled on the metallic board 1 formed conductive circuitry thereon , and the electrical connecting is completed . in other words , the method for fabricating solid - state light emitting display of this embodiment at least comprises : providing a metallic board 1 formed conductive circuitry 11 thereon ; and setting a plurality of luminous microcrystals 3 on the surface of the metallic board 1 and electrically connecting the luminous microcrystals 3 with the conductive circuitry 11 . the step of providing a metallic board formed with a conductive circuitry includes , polishing and planishing a metallic board , setting an insulating layer on the metallic board , setting a conductive circuit layer on the insulating layer , and removing the insulating layer at the position where assembling the luminous microcrystals on the metallic board . during the steps of setting a plurality of luminous microcrystals on the surface of the metallic board and electrically connecting the luminous microcrystals with the conductive circuitry , which comprises , setting a conductive connecting device for electrical connection on the conductive circuitry and luminous microcrystals , wherein , further comprising , setting a protection layer on the conductive circuitry , the luminous microcrystals and the conductive connecting device , or setting a protection layer on the conductive circuitry , the luminous microcrystals and the conductive connecting device , and setting a condensing layer on the protection layer . the above - described ic ( integrated circuit ) fabricating process , smoothness fabricating process , self - assembly fabricating process , epitaxy fabricating process , microcrystalline fabricating process and the like are known in the art , thus , herein will not be described again , the fabricating process of the present invention is not limited to this embodiment , and is capable of other change . in the exemplary embodiment , such luminous microcrystals 3 can be combined by light emitting diodes with different and same colors , e . g ., combined by light emitting diodes with r ( red ), g ( green ), b ( blue ) and the like , and the solid - state light emitting display of the present invention further comprises a protection layer . referring to fig3 a , a protection layer 15 is set for covering such luminous microcrystals 3 and the conductive circuitry 11 , the protection layer 15 assumes rectangular microstructure ; certainly , due to good stability of such luminous microcrystals 3 in the atmosphere , it is ok as long as the protection layer 15 can protect the surface without achieving the extend of pressurizing or vacuuming as the conventional technology , i . e . protect the luminous microcrystals 3 and make the ray pass through . preferably , in another exemplary embodiment , referring to fig3 b , the protection layer 15 assumes wavy or other capable of focusing light microstructure , and the protection layer 15 can be made from the material permeable to light , so as to provide the effect of , e . g ., protecting the luminous microcrystals 3 and the conductive circuitry 11 surface , and the light focusing effect , but it is not used to limit the present invention . of course , in one another exemplary embodiment , the solid - state light emitting display according to the present invention further comprises , setting a protection layer 15 for covering such luminous microcrystals 3 and the conductive circuitry 11 , and a condensing layer ( not illustrated ) disposed on the protection layer 15 , wherein the protection layer 15 and condensing layer assume wavy microstructures , and the protection layer 15 and condensing layer can be made from the material permeable to light , so as to respectively provide the effect of , e . g ., protecting the luminous microcrystals 3 and the conductive circuitry 11 surface , and the light focusing effect . this exemplary embodiment differs from the conventional technology in that it uses metallic board 1 as substrate , except that the metallic board 1 has conductivity , can act as the common electrode of the active type substrate and avoid the static problem during display using and fabricating process , the thermostability of the metal can be compatible in the high temperature ic fabricating process so as to simplify such as thin film fabricating process of the active component in the conductive circuitry , and the metal surface has favorable light reflectivity , so that the ray produced by the luminous microcrystals 3 acting as light emitting component can be reflected to the direction of the user , thereby upgrading lightness , and the heat produced in operating can be dissipated by the relatively high heat conduction coefficient of the metal , thereby solving the most involved heat emission problem of the light emitting component . concurrently , this exemplary embodiment employs such as luminous microcrystals 3 of the light emitting diode with bare crystal structure as solid - state light emitting component , the luminous microcrystals 3 fabricated by , e . g ., the conventional epitaxy fabricating process and microcrystalline fabricating process can provide image pitch of 100 to 200 . mu . m and high efficiency of solid - state light source , thereby providing excellent luminous efficiency and reaction time , and due to the quite small volume , even if bending the metallic board 1 , the horizontal position of the luminous microcrystals 3 on the surface of the metallic board can not be changed either , or the luminous microcrystals 3 can not be fallen off , the stability of the solid - state light emitting diode in the atmosphere can simplify the encapsulation fabricating process of the solid - state light emitting display according to the present invention , and concurrently upgrade the reliability and longevity of the display . thus , compared with the conventional technology , the solid - state light emitting display and fabrication method thereof according to the present invention can employs solid - state light emitting diode to provide spontaneous light source with energy saving and high photoelectric transducing efficiency , so as to provide display quality with high color saturation of wide color gamut . furthermore , except for the characteristics of short reaction time and wide visual angle , the stability of the solid - state light emitting diode in the atmosphere can simplify the encapsulation fabricating process of the display and concurrently upgrade the reliability and longevity of the display . synchronously , the design of the present invention adopts metallic board as substrate , such quite thin metallic board can fabricate thin - film diode with high efficiency and eliminate static , as well as provide optimal approach for heat emission of luminous microcrystals of the light emitting diode , so as to significantly upgrade the luminous efficiency and display quality of the display , thereby solving various drawbacks of the conventional technology that can not meet various requirement characteristics of the display . accordingly , the application of the present invention can provide a solid - state light emitting display and fabrication method thereof with high quality , environmental protection and energy saving , lightness and thickness , and flexibility , except for excellent photoelectric effects , e . g ., luminous efficiency and reaction time , it can also simplify the encapsulation fabricating process , thereby concurrently upgrading the reliability and longevity of the display , and make the light emitting component of the display have preferable approach for heat emission , as well as can eliminate static problem , thereby the present invention can even be applied in the product requiring flexure and can upgrade the property value . fig4 shows a solid - state light emitting display and a fabrication method thereof according to a second embodiment of the present invention . the components identical or similar to the first exemplary embodiment is expressed as the same or similar component reference numbers , of which the detailed description is left out , in order to illustrate the present invention in a more clear and concise manner . with reference to fig4 , the solid - state light emitting display comprises a metallic board 1 formed with a conductive circuitry , a plurality of luminous microcrystals 3 disposed on the surface of the metallic board 1 which is grounded and electrically connecting with the conductive circuitry 11 , and a fluorescent powder layers 17 at least respectively covering such luminous microcrystals 3 . in the exemplary embodiment , such luminous microcrystals 3 can be , e . g ., ultraviolet light emitting diode , or other suitable component , and the fluorescent powder layers 17 are formed by putting the fluorescent powders with different and same color on the luminous microcrystals 3 and part of the conductive circuitry 11 . attention should be paid to , the fluorescent powder layers 17 can be respectively assembled by a plurality of combinations with same and different colors , such as r ( red ), g ( green ) and b ( blue ), the luminous microcrystals 3 vitalizes the fluorescent powder layers 17 to produce tricolor , thereby forming the true color effect , but it is not limited to this . accordingly , except that employing spontaneous light which can directly produce tricolor , the present invention can also employ , e . g . ultraviolet light of the ultraviolet light emitting diode to vitalize the fluorescent powder layers 17 for producing tricolor , furthermore , both of these can provide display quality with high color saturation of wide color gamut . in conclusion , the solid - state light emitting display and fabrication method thereof according to the present invention employs the display technology with high quality , environmental protection and energy saving , lightness and thickness , and flexibility , and also uses the solid - state luminous microcrystals with high efficiency as photounit of the display with single pixel , which can provide excellent luminous efficiency and the characteristics of spontaneous light emitting display , such as short reaction time and wide visual angle , and the stability of the solid - state light emitting diode in the atmosphere can simplify the encapsulation fabricating process of the display , and concurrently upgrade the reliability and longevity of the display , application of metallic board can provide high efficiency of the solid - state luminous microcrystals and the optimal approach for heat emission , so as to significantly upgrade the luminous efficiency and display quality of the display . accordingly , the present invention can solve various drawbacks of the conventional technology , and the present invention has design elasticity , so as to efficiently improve the property value . the invention has been described using exemplary preferred embodiments . however , it is to be understood that the scope of the invention is not limited to the disclosed embodiments . on the contrary , it is intended to cover various modifications and similar arrangements . the scope of the claims , therefore , should be accorded the broadest interpretation so as to encompass all such modifications and similar arrangements . | 6 |
fig1 - 4 show various views of an embodiment of a ligament - tensioning device 1 in various states ( described below ), with fig1 showing the device co - operating with a positioning tool . the ligament - tensioning device 1 comprises a distal bearing plate 5 , which is approximately kidney - shaped in plan view , and , arranged in parallel therewith and opposite thereto , two proximal bearing plates 7 and 9 each of which overlaps approximately half of the distal bearing plate , the proximal bearing plates each comprising a lower part 7 a , 9 a and an upper part 7 b , 9 b . for positioning the ligament - tensioning device 1 with the aid of the positioning tool 3 there are provided on the front side edges of the distal and proximal bearing plates respective cylindrical recesses 11 as engagement portions ( fig1 shows the recesses in the proximal bearing plates , more specifically in the upper parts 7 b , 9 b thereof , while fig2 shows the central recess 11 in the distal bearing plate 5 ). the proximal bearing plates 7 and 9 ( or , more specifically , the lower parts 7 a , 9 a thereof ) are joined to the illustrated device 1 by means of a scissor - type guide means 13 and are tensioned against the device by a steel compression spring 15 as spring element . as can be seen most clearly in fig2 and 3 , the helical spring 15 is seated in a matching circular recess 17 on the upper side of the distal bearing plate 5 , and a similar mounting ( not shown ) is provided on the underside of the respective associated proximal bearing plate . the scissor - type guide means 13 comprises medial and lateral scissor joints 19 , 21 which each comprise two limbs 19 a , 19 b and 21 a , 21 b pivotally connected by means of a hinge pin 23 , 25 , respectively . the limbs 19 a , 21 a are joined to one another at one end by means of an integrally formed bridge or connecting bar 27 , while a slide peg or pin 29 a , 31 a is inserted in their other end for connection to the lower part 9 a ( omitted in fig2 and 3 ) of the second bearing plate . in a similar way , one end of each of the limbs 19 b , 21 b can be joined by means of a connecting rod 33 inserted perpendicular to the plane of extension , which rod projects beyond the medial or lateral outer side of the respective limb and forms further slide pegs ( not shown separately ) thereon . the opposite ends of the limbs 19 b , 21 b are in turn each provided with a separate slide pin 29 b , 31 b , respectively . those slide pegs 29 b , 31 b engage ( as can be seen most clearly in fig3 ) in correspondingly dimensioned grooves 35 , 37 in the distal bearing plate 5 which , in the in - use position of the ligament - tensioning device , run dorsally - ventrally and fix the scissor - type guide means so as to be slidable therewith in the distal bearing plate 5 . ( as can be seen to some extent in the portion of fig3 showing the lower part 7 a of the first proximal bearing plate 7 ( see detail “ a ”), a corresponding groove structure , which does not have a separate reference numeral herein , is provided in the proximal bearing plates ). as can be seen most clearly in fig2 , on the ventral side edge ( front edge ) of the distal bearing plate 5 , on both sides of an extension containing the cylindrical recess 11 there are mounted two pivotable hook elements 41 , 43 , each of which comprises a hex key engagement portion 41 a , 43 a and an integrally formed hook portion 41 b , 43 b , respectively . as can be seen in fig2 in the region of the first proximal bearing plate , the hook portions engage in a recess on the upper side of the respective bearing plate lower part , which recess is shaped to correspond to the shape of the hook , with only the recess 45 in the lower part 7 a of the first proximal bearing plate being shown in fig2 . by means of such engagement , the proximal bearing plates are held at a minimum distance from the distal bearing plate . by rotation of the respective hook element 41 , 43 with a suitable tool , that locking is released and the proximal bearing plate in question can be moved away from the distal bearing plate under the bias of the associated compression spring 15 until its movement comes to a standstill in force equilibrium with the capsule / ligament tension acting at the site of use . whereas in fig1 - 4 a cylindrical helical spring 15 is shown as the spring element , fig5 shows , as a modification , a double - cone helical spring 15 ′ which , by virtue of its lesser overall height in the tensioned state , can be used preferably in the ligament - tensioning device 1 according to fig1 - 4 , it being possible ( in a configuration not shown ) for the pitch of the winding in the lower and upper regions of greater diameter to be smaller than in the central region , in order that a trouble - free spring action is realized over the entire travel . the above - described ligament - tensioning device 1 is constructed for use in a knee joint and is shown in that in - use state in various views in fig6 a to 6d . the figures clearly show the matching of the dimensions , especially the length / width ratio , and the configuration of the two proximal bearing plates 7 , 9 to the anatomical conditions of the knee joint and the overall dimensions and relative sizes of the tibia t and the ( resected ) femur f . as shown , the device can have a length : width ratio of approximately 3 : 2 in accordance with that of a proximal tibia . fig7 a to 7d show a diagrammatic view , comparable to fig6 a - 6d , of a modified configuration of a ligament - tensioning device 1 ′ with a coupled - on sizer 47 . a sizer serves for the intra - operative coupling of tibia and femur in flexion so that axis transmission of the tibial axis , taking account of the ligament tension , to the femur can be effected . it is accordingly possible to define the optimum size and position of a knee implant in the ventral - dorsal direction and in rotation . attention should be drawn to the provision of connecting means between the ligament - tensioning device 1 ′ and the sizer 47 , namely two clip - like extensions or connecting bars 49 a , 49 b on the distal bearing plate 5 , which engage over the proximal bearing plates ( not shown ) at one side edge thereof and make a connection to a base plate 51 of the sizer 47 . the implementation of the invention is not confined to the embodiments described herein and the last - mentioned modification of the spring element , but is also possible in a multiplicity of embodiments which lie within the scope of the invention . for example , in some embodiments , a scissor - type guide means may be turned through 90 ° with respect to the embodiment shown , and in which some of the slide pegs or pins can be constructed simultaneously as bearing pins for the fixed positioning of a limb end in the associated bearing plate . in such embodiments , it is also possible for such a bearing pin to be used simultaneously as hinge pin of the pivotable locking hooks . furthermore , in the case of the proximal bearing plates it is also possible for the upper parts to be omitted , and numerous degrees of freedom exist in respect of the exact shape and relative dimensions of the bearing plates . 7 a , 9 a lower parts of the proximal bearing plates 7 b , 9 b upper parts of the proximal bearing plates | 0 |
in fig1 there is disclosed a flame detection circuit means 10 which is adapted to be connected to an ultraviolet responsive tube 11 that is positioned to detect a flame . the system disclosed typically would be used in a burner control system for safe operation of a burner . the present system could also be used where a system has been developed for the use of an ultraviolet responsive tube for uncontrolled fires , such as fire alarm and control systems . the ultraviolet responsive tube 11 is connected to an input circuit means generally disclosed at 12 having a pair of terminals 13 and 14 which are adapted to be connected to the ultraviolet tube 11 with the input circuit means 12 powered by an alternating current potential source means 15 . this source means typically would be a 60 hertz source of proper voltage to function with the particular tube 11 . the input circuit means 12 further includes a parallel combination of a resistor 16 and a capacitor 17 that are in turn connected by conductor 20 to a parallel combination of a diode 21 and a second capacitor 22 . the parallel combination of the diode 21 and capacitor 22 are connected to the potential source means 15 and to a conductor 23 that forms a common or ground for the overall system . the tube 11 is in series with a resistor 24 . the capacitors 22 and 17 along with the resistances 16 , 24 , and the diode 21 form a series circuit which provides for a cyclic charging and discharging of the capacitor means . the charging and discharging of the capacitor means varies dependent on the state of conduction of the tube 11 and will be discussed subsequently . a diode 25 is connected to a resistor 26 that is paralleled by a capacitor 27 with the diode 25 connected to the input circuit means 12 . the parallel combination of the resistor 26 and the capacitor 27 act as an integrating means . the integrating means made up of the resistor 26 and the capacitor 27 has a conductor 30 at which point a signal voltage is developed dependent on the state of conduction of the tube 11 . the signal voltage on conductor 30 is fed through a resistor 31 to a further conductor 32 . the conductor 32 is connected to a resistor 33 and a flame current meter jack 29 along with a capacitor 34 , which are in parallel , to the common conductor 23 . the parallel combination of the resistor 33 ( including jack 29 ) and the capacitor 34 is connected through a further resistor 35 to a diode 36 that forms an input to a three stage transistor amplifier generally disclosed at 40 . the output of the transistor amplifier or flame amplifier means 40 is a transistor 41 that is connected in series with a switch means 42 . the switch means 42 has been specifically disclosed as a relay that is connected between a supply conductor 43 and the transistor 41 which in turn is connected to the ground conductor 23 . the conduction of the transistor 41 in response to a signal across the diode 36 controls the pull in and drop out of the switch means or relay 42 provided the conductor 43 is energized from a source , such as a direct current potential 44 that has been shown as a conventional battery . in reality the source 44 would be a potential developed through rectification and voltage regulation from an alternating current source that can be common to source means 15 . to this point , the circuit described is the type of circuit mentioned in the background of the invention as an ultraviolet responsive tube flame detection circuit means that is not protected from the inadvertent presence of a resistance across the terminals 13 and 14 . the circuitry added to the flame detection circuit means described to this point constitutes the recognition of the problem involved and a means of providing a flame detection circuit means that is immune from resistance shorts across the terminals 13 and 14 . a pulse responsive circuit means is disclosed at 50 that provides for the novel function . the pulse responsive circuit means 50 includes a transistor 51 that is connected from the conductor 43 through a diode 52 to a junction point 53 of a resistor 54 and a capacitor 55 . the junction point 53 is connected to a gate 56 of a field effect transistor generally disclosed at 60 and which contains a source and a drain connected so that the field effect transistor 60 short circuits the resistor 33 . this short circuit eliminates the signal voltage present on the conductor 32 unless the field effect transistor 60 can be driven out of conduction by a voltage at 53 on its gate 56 . this requires the presence of a charge on the capacitor 55 which is provided when the transistor 51 properly conducts through the diode 52 . the transistor 51 has its base connected by a resistor 61 to the source voltage on conductor 43 and the resistor 61 is paralleled by a diode 62 . the diode 62 is connected through a capacitor 63 via a conductor 64 to a junction 65 . the voltage at junction 65 is the voltage that is generated across the resistor 24 and is indicative of the state of conduction of the tube 11 . this will be brought out in the description below in connection with fig2 and 3 . the circuit is completed by connecting a resistor 66 to amplifier means 40 through conductor 67 along with conductor 68 to a further direct current potential 70 . this provides a negative bias on amplifier means 40 that must be overcome by the flame signal current to switch the relay 42 . if it is first assumed that there is no flame present , the application of voltage to the present system does not allow for the relay 42 to become conductive . with no flame present , the tube 11 is a substantially open circuit and therefore the input circuit means 12 does not provide a source of potential across the resistor 24 . there is a voltage developed across the capacitor 63 which is developed by the direct current potential source 44 charging the capacitor 63 through the resistor 61 and back through the resistor 24 . with the tube 11 in a nonconductive state , there is no signal on the conductor 30 , but even if there were , the field effect transistor 60 , being in a conductive state , would short that signal out . in the event that a flame is positioned to cause the tube 11 to conduct , the conduction of that tube would generate a current in the resistor 24 as is shown in fig2 . a current does not occur during the positive half of the applied wave form generated by the source 15 , nor does it occur until the tube 11 is supplied with a sufficiently negative potential across the terminals 13 and 14 for the tube to breakdown and suddenly conduct . this is shown by the sharp change in current at time 70 . the current then continues to conduct at 71 until the current reaches the zero line at which time the tube 11 is caused to become nonconductive by the normal configuration of its connection in the input circuit means 12 . the sudden conduction of current in resistor 24 at time 70 changes the voltage that has been built up across the capacitor 63 and this sudden change in voltage at the capacitor 63 causes the transistor 51 to be suddenly driven into conduction . the sudden conduction of a transistor 51 provides a pulse of current as disclosed at 72 ( of fig3 ) to the junction 53 of the capacitor 55 and the gate 56 of the field effect transistor 60 . the circuit is designed so that a small number of pulses are required to raise the voltage across capacitor 55 at the gate 56 of the field effect transistor 60 to turn the transistor 60 &# 34 ; off &# 34 ;. at this same period of time the pulses of &# 34 ; on &# 34 ; and &# 34 ; off &# 34 ; being generated are being supplied at the output diode 25 as an input or signal voltage on conductor 30 to charge the capacitor 27 which forms the control signal for the transistor amplifier means 40 . it is obvious that when a voltage is provided on the conductor 30 and the field effect transistor 60 is driven out of conduction , that the voltage on conductor 30 then becomes a driving signal for the transistor amplifier means 40 which in turn turns &# 34 ; on &# 34 ; the transistor 41 to pull in the switch means 42 indicating the presence of a flame at the tube 11 as soon as the negative bias set through resistor 66 has been overcome . it will be understood that the wave forms disclosed in fig2 and 3 must occur for a repetitive number of cycles in order to charge the capacitors 27 and 55 to provide an appropriate signal to the transistor amplifier means 40 to energize the output switch means 42 . this eliminates the possibility of a transient or stray type of signal accidentally energizing the control switch means 42 . if the circuit is considered with a resistance across the terminals 13 and 14 , it will found that the signal that appears across the resistor 24 is that disclosed in fig2 at 73 . in this case the sharp leading edge is not present , and the necessary pulse of current 72 ( disclosed in fig3 ) is not allowed to pass by the transistor 51 . the presence of a resistance across the terminals 13 and 14 of the present circuit therefore is properly detected and rejected as an unsafe condition without pulling in the control switch means 42 as had occurred in the circuit prior to the addition of the present invention . the present disclosure teaches a simple expedient for protecting a circuit against a false indication of flame by the simple addition of a pulse responsive circuit means . the particular type of pulse responsive circuit means is not critical , and it is quite obvious that when this teaching becomes known , that other circuit modifications would become obvious to one skilled in the art . for that reason , the applicant wishes to become limited in the scope of his invention solely by the scope of the appended claims . | 5 |
as summarized above , aspects of the invention include multi - mode communication ingestible event marker devices . ingestible event marker devices of the invention include an ingestible component comprising a conductive communication module and at least one additional non - conductive communication module . the non - conductive communication module may be integrated with the ingestible component or at least a portion or all of the non - conductive communication module may be associated with a packaging component of the ingestible event marker device . systems of the invention that include the ingestible event marker devices and a receiver may be configured to provide medication information and control measures across the entire life cycle of the ingestible event marker . the life cycle includes , for example , medication manufacture , supply chain management , pharmacy management , and patient use management . ingestible event marker devices of some embodiments may include an ingestible component that includes an integrated circuit component comprising a conductive communication module ( for example present as an integrated identifier ) and at least a second non - conductive communication module , where the number of additional non - conductive communication modules may vary , for example one or more , two or more , three or more , etc . accordingly , the ingestible event marker devices of the invention may be viewed as multi - mode communication ingestible event marker devices , since they include at least two distinct communication modules , one of which is a conductive communication module . as indicated above , the at least second non - conductive communication module may be associated with the ingestible component or partially or wholly associated with a packaging component of the device , if present . as such , ingestible event marker devices of the invention may or may not include packaging associated with the ingestible component , where packaging may be configured in a variety of different formats , such as blister packs , multi - dose containers , and the like . in some instances , the communications modules are dynamically combined with medication components ( when present ) to achieve highly effective and accurate information and control solutions in a viable , cost - effective manner . for example , in one embodiment , the communications modules are implemented as an integral part of a pill and / or medication packaging . further , the systems can communicate with various other devices , including transmitters / receivers associated with inventory control , pharmacy control , and inter - and intra - body devices . as summarized above , the devices and systems of the invention include at least one non - conductive communication module . by non - conductive communication module is meant a communication module that communicates using a communications protocol other than a conductive communication protocol which uses body fluid as a conduction medium ( for example , as further described in pct published application publication nos . wo 2006 / 116718 ; wo 2008 / 008281 ; wo 2008 / 095183 and wo 2008 / 063626 ; the disclosures of which are herein incorporated by reference ). non - conductive communication protocols , i . e ., modes , of interest include , but are not limited to : wireless radio - frequency modes ; magnetic induction modes ; optical modes , such as infra - red frequency optical modes ; acoustic modes ; as well as wired modes , i . e ., direct modes . accordingly , in some instances the non - conductive communication module may be at least one module selected from the group consisting of a wireless radio - frequency module , a magnetic induction module ; an optical module , an acoustic module , and a wired module . in some embodiments of interest , the non - conductive communication module is a wireless radio - frequency module . while the wireless radio - frequency communication module may vary , in some instances this module is a radio - frequency identification ( rfid ) module . for ease of description purposes only , embodiments of the invention will now be further described in terms of embodiments where the non - conductive communication module is an rfid communication module . however , as noted above the non - conductive communication module may vary widely . in some instances , the rfid module incorporates , for example , an integrated circuit and an rf antenna . the rfid module may be communicatively associated with a conductive module incorporating , for example , an integrated circuit and a conductive antenna . either of the rfid module or the conductive module , or both , may function in conjunction with medication and / or medication packaging to receive , process , store , and / or transmit information related to or associated with the medication . as indicated above , the devices and systems can be used across multiple and varied applications to provide secure , controlled , and accurate communications in viable , cost - effective implementations . broadly , the devices and systems facilitate information communication and control measures up to the entire life cycle of an ingestible event marker . the systems are capable of application in a variety of communications environments , particularly in environments where wireless communications are preferred . for example , the communications environments include inventory control environments as well as inter - body and intra - body communications . inter - body and intra - body communications include , for example , active , passive , and semi - passive systems associated with data transmission and reception from implantable , ingestible , insertable , and attachable medical devices and medications associated with the human body or other living organisms . the medical devices are capable of communication and / or integration with systems of the invention . as reviewed above , the ingestible event marker devices of the invention include an ingestible component that comprises at least an integrated circuit and a conductive communications module . this structure is collectively referred to herein as an ingestible event marker , and ingestible event markers may or may not include additional components , such as a physiologically acceptable vehicle and / or an pharmaceutically active agent . accordingly , the ingestible event markers described herein , sometimes referred to herein as “ iems ”, at least include an ingestible component that includes an integrated circuit that comprises a conductive communication module , where the conductive communication module includes a conductive transmitter . the integrated circuit and conductive communication module may be collectively referred to as an identifier . identifiers of interest are structures that generate ( for example emit ) a detectable signal upon contact of the ingestible event marker identifier with a target physiological location ( or locations ). the ingestible event marker identifiers may vary depending on the particular embodiment and intended application of the composition , as long as they are activated ( turned on ) upon contact with a target physiological location , such as the stomach or small intestine . as such , an ingestible event marker identifier may be a structure that emits a signal when activated at a target site , for example when it contacts a target body site . the ingestible event marker identifier may be any component or device that is capable of providing a detectable signal following activation . ingestible event marker identifiers according to embodiments of the invention include a signal generation component . the ingestible event marker identifier may be configured to emit a signal once the composition comes into contact with a physiological target site . depending on the embodiment , the target physiological site or location may vary , where representative target physiological sites of interest include , but are not limited to : a location in the gastrointestinal tract , such as the mouth , esophagus , stomach , small intestine , large intestine , etc . ingestible event marker identifiers may be configured to be activated upon contact with fluid at the target site , e . g ., stomach fluid , regardless of the particular composition of the target site . where desired , the ingestible event marker identifier may be configured to be activated by interrogation , following contact of the composition with a target physiological site . the ingestible event marker identifier may be configured to be activated at a target site , where the target site is reached after a specified period of time . depending on the needs of a particular application , the signal obtained from the ingestible event marker identifier may be a generic signal , such that the signal is a signal that merely identifies that the composition has contacted the target site . alternatively , the signal may be a unique signal , such as a signal which in some way uniquely identifies that a particular ingestible event marker from a group or plurality of different ingestible event markers , for example a batch of ingestible event markers , has contacted a target physiological site . as such , the ingestible event marker identifier may be one that emits a signal that cannot be distinguished from the signal emitted by the ingestible event marker identifier of any other ingestible event marker member of a batch from which the ingestible event markers are obtained . alternatively , each ingestible event marker member of a batch of ingestible event markers may have an ingestible event marker identifier that emits a unique signal , at least with respect to all of the other ingestible event marker identifiers of the ingestible event marker members of the batch . the ingestible event marker identifier may emit a unique signal that is a universally unique signal ( where such a signal may be analogous to a human fingerprint which is distinct from any other fingerprint of any other individual and therefore uniquely identifies an individual on a universal level ). the signal may either directly convey information about a given event , or provide an identifying code , which may be used to retrieve information about the event from a database , such as a database linking identifying codes with compositions . where desired , the signal may be encrypted in a manner that provides control over access to the signal and informational content thereof . the ingestible event marker identifier at least generates a conductive ( near field ) signals , which signal is one that is communicated via a conductive communication protocol that uses body fluid as a conduction medium ( for example , as further described in pct published application publication nos . wo 2006 / 116718 ; wo 2008 / 008281 ; wo 2008 / 095183 and wo 2008 / 063626 ; the disclosures of which are herein incorporated by reference ). depending on the given embodiment , the ingestible event marker identifier may transmit a given signal once . alternatively , the ingestible event marker identifier may be configured transmit a signal with the same information ( identical signals ), two or more times , where the collection of discrete identical signals may be collectively referred to as a redundant signal . the ingestible event marker identifiers may vary depending on the particular embodiment and intended application of the composition so long as they are activated upon contact with a target physiological location , such as the stomach . ingestible event marker identifiers may include an activation component , such as a battery that is completed by stomach acid , and a transmission element . in these embodiments , the identifier may be viewed as including a “ wet battery ” power source , which power source at least provides power to the conductive communication module , and may or may not provide power to the non - conductive communication module , as further developed below . examples of different types of ingestible event marker identifiers of interest include , but are not limited to , those ingestible event marker identifiers described in pct application serial no . pct / us2006 / 016370 published as wo / 2006 / 116718 ; pct application serial no . pct / us2007 / 082563 published as wo / 2008 / 052136 ; pct application serial no . pct / us2007 / 024225 published as wo / 2008 / 063626 ; pct application serial no . pct / us2007 / 022257 published as wo / 2008 / 066617 ; pct application serial no . pct / us2008 / 052845 published as wo / 2008 / 095183 ; pct application serial no . pct / us2008 / 053999 published as wo / 2008 / 101107 ; pct application serial no . pct / us2008 / 056296 published as wo / 2008 / 112577 ; pct application serial no . pct / us2008 / 056299 published as wo / 2008 / 112578 ; and pct application serial no . pct / us2008 / 077753 ; the disclosures of which are herein incorporated by reference . an example of an ingestible event marker of interest is depicted in fig1 a and 1b . the ingestible event marker 10 shown in fig1 a and 1b includes an integrated circuit component 20 ( also referred to herein as the identifier ) as well as upper and lower electrodes 22 and 24 , where the upper and lower electrodes are fabricated from dissimilar materials and are configured such that upon contact with stomach fluid current runs through the integrated circuit to cause one or more functional blocks in the circuit to emit a detectable signal . the marker shown in fig1 a and 1b includes a virtual dipole signal amplification element 30 ( sometimes referred to herein as a “ skirt ”), as reviewed in greater detail in pct application serial no . pct / us20008 / 077753 , the disclosure of which is herein incorporated by reference . in one example , the iem includes a conductive antenna , a conductive modulator , and a wet battery . the digestive system liquids , for example , activate the battery , which acts as a power source for various ingestible event marker components . detection events occur via liquid contact . data is transmitted via the conductive antenna to a receiving device . the ingestible event marker devices may be used in conjunction with receivers configured to receive the conductive signal emitted by the conductive communication module of the ingestible event maker . one example of an attachable medical device is a transmitter / receiver ( which may be referred to herein as a raisin receiver ), permanently associated with a body ( such as implanted in a body ) or removably attachable to an external portion of a body . receivers of interest include , but are not limited to , those receivers configured to detect a conductively transmitted signal described in pct published application publication nos . wo 2006 / 116718 ; wo 2008 / 008281 ; wo 2008 / 095183 and wo 2008 / 063626 ; the disclosures of which are herein incorporated by reference . as such , the iem can be communicably associated with a transmitting and / or receiving device such as the raisin , supra . the transmitting / receiving device includes in - body devices , external devices removably or permanently attachable to the body , and remote devices , i . e ., devices not physically associated with the body , but capable of communication with the ingestible event marker . various embodiments of the devices and systems , including communication - enabled pills and packaging , enable identification of the iem and any medication thereof ( if present ). “ pill ” as used below is representative of any communication - enabled medication . iem packaging includes , for example , a “ blister ” pack capable of housing an individual iem ( such as a pill or a limited number of pills or capsules ). the iem packaging further includes containers , boxes , wrappings , iv bags , and so forth associated with the medication . in various embodiments , the communication components can be sovereign to the pill . in other embodiments , the communication components can be distributed , e . g ., the rf module or portions thereof are physically associated with the packaging and the conductive communications module is physically associated with the ingestible component , such as a pill or capsule . for example , rfid communications can be terminated when the pill is removed from the packaging due to the physical severance of rfid module components from the remainder of the device . in one embodiment , the rfid antenna is located on the medication packaging and is separated from the remainder of the device via a “ snap - off ” mechanism , thus preventing rf communications with the ingestible component once it has been removed from its packaging . in another embodiment , the rfid antenna is removed at the time the pharmacy delivers iem to the patient . in the above examples , other rfid module components , such as a data storage component , can be associated with the rf antenna in such a way that they are separated from the remainder of the system along with the antenna . alternatively , the rf antenna could remain attached to the pill while another part of the rfid module is separated from the pill . as such , in some instances at least a portion of the non - conductive communication module is configured to be separable from the ingestible component in a manner that does not compromise the function of the conductive communication module . one advantage of separating part or all of the rfid module from the conductive communications module in this manner is the patient privacy protection afforded by termination of rfid communications . in some embodiments , some or all of the data readable on or written to the rfid system will be removable via severance of the rfid module from the conductive module to protect patient privacy . however , in other embodiments , retention of such data after separation could be desirable for long term tracking and / or identification purposes . the rfid components can be used to encode the pill or the medication packaging with various data such as medication identification information , dosage information , lot and batch numbers , and expiration dates . these data can be manipulated in any manner to optimize functionality . for example , quality control processes can read each iem &# 39 ; s information and aggregate the information consistent with optimal inventory , shipping tracking , and financial processes . automated sorters can communicate with each iem to efficiently process , sort , and package medications . similarly , shipping operations can be tracked and controlled to ensure positive medication identification , medication location , and so forth . in one example , once medication distribution has commenced , the device and system can be used to check for counterfeit medications , such as might be received from international points or from other locations lacking good regulatory practices . pharmacy operations can be optimized with use of the devices and systems . for example , upon receipt of medications into the pharmacy , the staff can scan the medication packaging and the medications to ensure receipt of the expected products and authenticity of the medication . prior to dispensing the medication to a patient , the pharmacy can encode the medication packaging , containers , and individual medications with patient - pertinent information . for example , such information includes patient identification , medication identification and patient - specific dosage and expiration information . further information includes contraindicated medications , warnings , and so forth . in this manner , the history , traceability , efficacy and safety of the medication are addressed . in addition , various embodiments of the devices can interoperate with dispensing devices in systems of interest . for example , once medication information is read into the system , the dispensing device aggregates various medications into a container or even a single iem or formulation for a particular patient . in various embodiments , the device can be a very small , low range unit . a very strong rf detector , such as an rfid wand or a gate that individual pills pass through , e . g ., a funnel as depicted in certain of the figures , can be used to communicate with the device outside the body , for example , within a range of 100 μm to ten meters , such as 3 μm to 3 centimeters , e . g . approximately 1 centimeter . once ingested , however , the low range of the rfid communication module does not facilitate communication with random devices , i . e ., those not intended or authorized to communicate with the iem . in this manner , privacy concerns regarding unauthorized or unintentional communication of information associated with the iem are minimized . higher range rfid devices i . e ., functioning with in a range of one meter to 20 meters , such as one meter to three meters , e . g . 2 meters , may be employed for some tracking applications . in this application , privacy protection can be provided by separation of rfid and conductive communications modules as described above . alternatively , privacy may be provided in this and any particular communication by employing suitable encryption techniques , such that any signal of interest where privacy considerations are of concern is encrypted . any convenient encryption protocol may be employed . the frequency range in which the rfid module operates can also be selected to achieve various design goals . low frequency rf , i . e . radio waves in the hz / khz range , for example , between 5 khz and 500 khz , such as 125 khz , may be preferable for communications while the device is in use by the patient . however mhz / ghz range rf , e . g . in the range of 1 mhz to 1 ghz , such as 13 . 56 mhz , can facilitate tracking of the system prior to patient use . multiple rfid modules can be combined within one system to facilitate these different needs . once the iem reaches the patient environment , information associated with the iem can be used for a variety of purposes . for example , the iem may interoperate with the iem container and with a receiver such as the raisin , supra , to ensure that the person attempting to open the iem container is actually the person for whom it is prescribed . further communication activities include an information control system , in which medication information associated with the iem device is compared against patient data received from one or multiple sources to determine , for example , if a medication is contraindicated , subject to appropriate dosage amounts and times , or other events and / or conditions . after patient ingestion , information stored by the iem may be recovered from one or more of the communications modules . for example , communication capabilities can be performed after ingestion via the conductive communication components , for example , using the ingestible event marker and a raisin receiver . in some embodiments , a device with a limited rf range maintains patient privacy respecting to information stored by the system . other embodiments of the system provide for separation of rfid module components to prevent rf access to the device . data can be stored in the device and reprogrammed with secure digital signature at each transaction . when patient expulsion of a iem has taken place , various embodiments permit communication with a device such as a sensor to determine , for example , data related to the patient or the medication , or transit time through the body . alternatively , in various embodiments , the data is erased ( or various components / subcomponents associated with the data are destroyed or separated from the system ) to protect privacy concerns after expulsion . in fig2 , there is shown a communications environment 100 including an ingestible event marker device 102 , according to one embodiment , which includes both a conductive communication module and an rfid module . the rfid module of the device 102 interacts via a communication link 104 with a receiver configured to receive a signal from at least one of the conductive communication module or rfid communication module of the device . for example , receiver 106 may be an rfid wand 106 . in communication environment 100 , the device 102 interacts with , e . g ., brings in power from , the rfid wand 106 . the rfid wand 106 , for example , operates on a radio frequency and transmits data to and / or receives data from the device 102 . in this manner , communication can be achieved without reliance on liquid contact to activate a power source . in addition , in certain embodiments , the device 102 is powered by the radio signal of the associated communication device , e . g ., rfid wand 106 . in this manner , the device 102 provides a relatively small size overall to facilitate ease of ingestion , implantation , maintenance , and traversal activities related to the body . more particularly , fig3 shows the ingestible event marker device 102 of fig1 , according to one embodiment . the device 102 includes a pill 202 and a communications module 204 . the communications module includes an integrated circuit (“ chip ”) 206 , an rf antenna 208 , lead ( s ) 210 , and an antenna skirt 212 . the pill 202 may have various pharmaceutical configurations , such capsules , caplets , gel caps , solid pills , tablets , and other types of pill medications . the pill 202 may include a physiologically acceptable vehicle , and may or may not further include a pharmaceutically active agent . the chip 206 is permanently or removably affixed to , or integrated with , at least a portion of the pill 202 . the chip 206 includes various combinations of components / subcomponents ( not shown ). for example , the chip 206 can include or be otherwise associated with a memory , a processor , a storage unit , a transmitter and / or receiver , or other components associated with data processing , storage , transmission , and receipt . the rf antenna 208 permanently or removably attaches to , or is otherwise in communication with , the chip 206 via leads 210 . in various embodiments , the antenna 210 is integrated , or otherwise associated with , the antenna skirt 212 ( also referred to above as a virtual - dipole signal amplifier ). in various embodiments , the antenna skirt 212 can be flexible , inflexible , foldable , unfoldable , rollable , unrollable , expandable or otherwise manipulated . in this manner , the folded antenna skirt 212 facilitates ingestion / implantation , yet expands in the body to promote communication transmittal and reception . the antenna skirt can be implemented in various materials or combinations of materials , so long as the functionality described herein is carried out . fig4 shows a cross - sectional view of an ingestible event marker device 300 , according to another embodiment . the ingestible event marker 300 includes packaging 302 , such as a “ blister ” pack . chip 206 of device 300 includes an rfid communication module electrically coupled to the rf antenna 208 via the leads 210 . the rf antenna 208 can be integrated into or formed in any manner associated with the packaging 302 . the chip 206 can be located or associated with either the blister pack , e . g ., where separate communicably associated chips can be attached to the blister pack and the pill . alternatively , chip 206 may be part of an ingestible component ( not shown ) such as a pill , such as where chip 206 further includes a conductive communication module . communication associated with the blister pack can be achieved without having all of the rfid components onboard an ingestible component , thus providing an alternative to ingestion of the entire rfid communication . therefore , the rfid off - board components , i . e ., components not physically associated with the ingestible component , need not consist of edible materials . as illustrated below , an rfid communication module 204 may be associated to varying degrees with conductive components of an iem . for example , fig5 shows a schematic of a first pill communication system 400 , sometimes referred to as a “ sender ”, including the rf antenna 208 powered by an induction power source 402 . the induction power source 402 includes , for example , the rfid wand 106 ( shown in fig2 ). the rf antenna 208 is communicably associated with a first modulator 404 , which modulates a signal associated with data 406 , which can be stored , for example , in a memory ( not shown ) or other media . the pill communication system 400 further includes a conductive antenna 408 powered by a wet battery 410 . the wet battery 410 is activated , for example , by digestive liquids . the conductive antenna 408 is communicably associated with a second modulator 412 , which modulates a signal associated with the conductive antenna 408 . the second modulator 412 is communicably associated with data 406 , which can be associated , for example , in a memory ( not shown ) or other media . in this manner , common data , e . g . data 406 can be transmitted via two different links , depending on the desired functionality . for example , data can be modulated and transmitted via the rf antenna 208 during manufacturing , shipping , pharmacy , and home operations . the same ( or different ) data can be transmitted via the conductive antenna 408 after ingestion of the pill . in various embodiments , after expulsion from the body , a time of expulsion can be determined and used , for example , to calculate a total transmittal time through the body . in some embodiments , some or all of the data stored on the system can be erased , destroyed , etc . for example , the pill includes fusible links ( not shown ) and use a portion of the power to completely erase data from memory or physically destroy memory . for example , when the conductive communication module power source , e . g . wet battery , is activated , the power provided triggers data deletion . in this manner , if the pill is recovered there is no data to be retrieved by unauthorized sources and the patient &# 39 ; s privacy interests are preserved . separating the data into separate modules ( not shown ) further allows a portion of stored data to be deleted , e . g . patient or dosage information , while allowing a portion of the data to remain , e . g . medication identifying information . a further advantage offered by separation between portions of the rfid communications module and the conductive communications module is a failsafe mechanism for obtaining data stored on the pill . that is , if one communications module fails , the other module remains available to facilitate communications . for example , if one or more components of the conductive communications module cease to function , an rfid wand 106 ( shown in fig2 ) could be used to power the pill communication system 400 inductively to obtain information from data 406 . moreover , separating the conductive communication module from the rfid communication module components facilitates physical disabling of a part of the system via a “ snap - off ” mechanism as described supra . fig6 shows a schematic of a second pill communication system 500 , according to one embodiment . the second pill communication system includes a spiral conductive rf antenna 502 , an rf modulator 404 , a conductive modulator 412 and data 406 . the antenna is communicably associated with an rf modulator 404 powered by an induction power source . the rf modulator 404 modulates a signal associated with the antenna . the rf modulator 404 is communicably associated with data 406 , which can be associated , for example , in a memory ( not shown ) or other media . the antenna 502 is further communicably associated with a conductive modulator 412 powered by , e . g ., a wet battery . the conductive modulator modulates a signal associated with the antenna . the conductive modulator is communicably associated with data 406 , which can be associated , for example , in a memory ( not shown ) or other media . in this manner , the second pill communication system accommodates both conductive and rf modulation of signals associated with a single antenna . an iem device featuring a single antenna which facilitates both conductive and rf communications would potentially reduce the component , design , and test costs associated with the complete system . moreover , the modes of failure are reduced as components are removed from the system . the potential for antenna failure is reduced when the system includes one antenna rather than two . fig7 shows a schematic of a third pill communication system 600 , according to one embodiment . the third pill communication system 600 includes an antenna 502 , a modulator 602 , and data 406 . the modulator 602 modulates a signal from the antenna 502 and can be powered by one or more sources , e . g ., a wet battery and / or an inductive power source . in one embodiment , for example , the modulator 504 is a 125 kilohertz ( khz ) modulator . in other examples , the modulator is a 13 megahertz ( mhz ) modulator or other frequency bands . in this manner , the second pill communication system 500 accommodates both inductive and conductive power sources in a single modulator / antenna design , permitting multiple types of communication in multiple communication environments . the advantages of component integration as illustrated in fig5 , supra , are further realized with further reduction of the number of components in the system . fig8 a and 8b show a first rfid module 602 and a second rfid module 604 , according to one embodiment . the first rfid module 602 is configured in association with a small chip 606 ( integrated circuit or flexible electrode ). the small chip 606 is , for example , between 10 micrometers and 10 millimeters on a side , such as 100 micrometers to 5 millimeters , e . g . one millimeter on a side , having a cathode on a first side ( not shown ) and an anode on a second side ( not shown ). the chip 606 is embedded in a skirt 608 by which conductive transmission is generated by modulating current . an antenna 504 runs along , i . e ., is associated with , the perimeter of the chip 606 . the antenna 504 includes , for example , a multi - turn / multi - layer antenna that acts as the antenna for an rifd link . in one embodiment , the antenna is relatively small . in various embodiments , an insulating layer ( not shown ) is introduces over the antenna 504 to extend range . for example , the insulting layer includes several hundred microns of plastic over the antenna 504 . in this manner , the pharmaceutical rfid unit 602 is compact , and therefore easily ingestible / implantable while still operable in an acceptable communication range . in various other embodiments , the antenna 504 matches a refractive index of the body . in this manner , the rfid antenna facilitates interbody , intrabody , and extrabody communications . the second rfid module 604 is configured in association with a small chip 606 having a cathode layer ( not shown ) on top of the chip 606 . the layer of metal is patterned with the antenna 504 , e . g ., densely patterned with the antenna 504 having a multi - turned , spiral - patterned design . the metal layer has slits cut therein , such as single spiral slit cut . when the cathode material is deposited , the antenna 504 serves as a conductor which provides the substrate for attaching the cathode and also the current collector for extracting electrical energy from it . in this manner , the antenna 504 becomes shorted when wet , thus permitting the rfid module to function in a dry environment ( manufacturing , pharmacy , etc .) but not in liquid environment , e . g ., inside the body . this promotes privacy by disabling rfid communications with the lifecycle pharma informatics system while it is in the body . in various embodiments , the antenna 504 is configured according to any pattern and / or location respective to the lifecycle pharma informatics system . patterns include , for example , spirals , squiggles , curves , multi - turned , straight , curved , single layer , multi - layer , and other designs and combinations of designs . fig9 shows an ingestible event marker identifier that includes an rfid communication module , according to an embodiment . in fig9 , iem identifier 900 includes integrated circuit component 910 and skirt 920 . integrated circuit component 910 includes both a conductive communication module and an rfid communication module . identifier 910 also includes rfid antenna 930 . iem identifiers that include both conductive communication modules and non - conductive communication modules , such as rfid communications modules , find use in a variety of different applications which may span the product lifetime of an ingestible event marker . abilities and functionalities provided by such identifiers include , but are not limited to : reading of iem identifier information and storing pedigree information at of one or more of the iem manufacturing stage , supply chain stage , pharmacy management stage , and patient use stage . complete pedigrees for a given iem , from manufacture to use and / or disposal may readily be obtained . audit capability may be provided at every point in the supply chain . automated sorting gates and cryptographic signatures may be employed to verify product authenticity , as desired . iem devices including both conductive communication and non - conductive communication modules may be fabricated using any convenient manufacturing protocol . in some instances , the manufacturing protocol that is employed is a high - throughput manufacturing protocol . such high - throughput manufacturing protocols include , but are not limited to , those described in u . s . provisional application ser . no . 61 / 142 , 849 , the disclosure of which is herein incorporated by reference . one high - throughput manufacturing protocol in which the iem includes an identifier having both conductive and rfid communication modules and a tablet physiologically acceptable carrier that includes an active pharmaceutical agent is schematically illustrated in fig1 . the process 1000 illustrated in fig1 begins with an iem identifier 1010 that includes and conductive and rfid communication module ( such as the identifier illustrated in fig9 ) being combined with an active pharmaceutical agent ( api ) and a physiologically acceptable vehicle 1020 into a tablet iem at stage 1030 . following tablet compression , the resultant tablet may be coated at stage 1040 and any printing or labeling applied at stage 1050 to product the final iem . next , the iem is sent to bulk packaging stage 1060 , where the resultant bulk package of iems is shipped at stage 1070 to pharmacy 1080 for ultimate sale to a customer . box 1090 illustrates examples of points in the process where the rfid communication module may be employed to transmit information to the iem and or receive information from the iem . for example , programming information may be transmitted to the iem via the rfid communication module at any of points 1092 , 1094 , 1096 and 1098 . alternatively and / or in addition to transmitting programming information to the iem via the rfid communication module at any of points 1092 , 1094 , 1096 and 1098 , identifying information may be retrieved from the iem at any of these points , e . g ., to facilitate packaging , sorting , handling , etc . fig1 provides a view of a sorter device that includes an rfid receiver / transmitter , where the sorter device may be used in a manufacturing , and supply chain and / or pharmacy system ( for example at any of points 1092 , 1094 , 1096 and 1098 . in fig1 , hopper 1100 includes a larger number of iems 1110 , where the iems include both conductive and rfid communication modules , such as the iem shown in fig9 . funnel 1120 dispenses iems into dispenser counter 1130 . dispenser counter 1130 includes 1 , 2 or 3 coils 1135 for rfid communication ( where three are shown in the figure ). dispenser counter includes tube 1137 which ensures dispensing of a single iem at a time into container 1140 . container 1140 is filled with identified and sorted iems . an example of an embodiment of container 1140 is shown in fig1 . container 1140 of fig1 includes multiple iems 1110 that have been identified by system 1100 . container also includes an rfid tag , 1150 and a bar code 1160 . also shown is cap 1170 . the system 1100 and container 1140 may be employed with an informatics system to readily know the exact contents of the container , including the pedigree information for each iem present in the container . fig1 provides a flow diagram of an iem product lifetime and provides examples of the types of information that be generated by iem devices that include both conductive and non - conductive communication modules . in fig1 , raw materials from raw material suppliers 1300 are sent to manufactures 1310 for manufacture of iems . distributor 1315 and 1320 transfer iems from the manufacture to a pharmacy , such as a hospital pharmacy 1330 or retail pharmacy 1335 , and ultimately to a patient 1340 . non - conductively communication information may be employed prior to patient ingestion to , among other activities , provide for product authentication the manufacturer 1310 and the first distributor 1315 , provide for verified product repackaging between the first distributor 1315 and the second distributor 1320 , accurately implement prescription filling at pharmacy 1330 or 1335 with fewer filling errors . conductively obtained information can be employed to obtain dosing information from the patient 1340 which is employed by health care practitioners 1350 as well as pharmacies ( to manage prescriptions ) and manufacturers 1310 ( for market intelligence , such as sales projections , etc .). uses of conductively obtained iem information are further described in pct published application publication nos . wo 2006 / 116718 ; wo 2008 / 008281 ; wo 2008 / 095183 and wo 2008 / 063626 ; the disclosures of which are herein incorporated by reference . it is to be understood that this invention is not limited to particular embodiments described , as such may vary . it is also to be understood that the terminology used herein is for the purpose of describing particular embodiments only , and is not intended to be limiting , since the scope of the present invention will be limited only by the appended claims . where a range of values is provided , it is understood that each intervening value , to the tenth of the unit of the lower limit unless the context clearly dictates otherwise , between the upper and lower limit of that range and any other stated or intervening value in that stated range , is encompassed within the invention . the upper and lower limits of these smaller ranges may independently be included in the smaller ranges and are also encompassed within the invention , subject to any specifically excluded limit in the stated range . where the stated range includes one or both of the limits , ranges excluding either or both of those included limits are also included in the invention . unless defined otherwise , all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs . although any methods and materials similar or equivalent to those described herein can also be used in the practice or testing of the present invention , representative illustrative methods and materials are now described . all publications and patents cited in this specification are herein incorporated by reference as if each individual publication or patent were specifically and individually indicated to be incorporated by reference and are incorporated herein by reference to disclose and describe the methods and / or materials in connection with which the publications are cited . the citation of any publication is for its disclosure prior to the filing date and should not be construed as an admission that the present invention is not entitled to antedate such publication by virtue of prior invention . further , the dates of publication provided may be different from the actual publication dates which may need to be independently confirmed . it is noted that , as used herein and in the appended claims , the singular forms “ a ”, “ an ”, and “ the ” include plural referents unless the context clearly dictates otherwise . it is further noted that the claims may be drafted to exclude any optional element . as such , this statement is intended to serve as antecedent basis for use of such exclusive terminology as “ solely ,” “ only ” and the like in connection with the recitation of claim elements , or use of a “ negative ” limitation . certain ranges have been presented herein with numerical values being preceded by the term “ about .” the term “ about ” is used herein to provide literal support for the exact number that it precedes , as well as a number that is near to or approximately the number that the term precedes . in determining whether a number is near to or approximately a specifically recited number , the near or approximating unrecited number may be a number which , in the context in which it is presented , provides the substantial equivalent of the specifically recited number . as will be apparent to those of skill in the art upon reading this disclosure , each of the individual embodiments described and illustrated herein has discrete components and features which may be readily separated from or combined with the features of any of the other several embodiments without departing from the scope or spirit of the present invention . any recited method can be carried out in the order of events recited or in any other order which is logically possible . although the foregoing invention has been described in some detail by way of illustration and example for purposes of clarity of understanding , it is readily apparent to those of ordinary skill in the art in light of the teachings of this invention that certain changes and modifications may be made thereto without departing from the spirit or scope of the appended claims . accordingly , the preceding merely illustrates the principles of the invention . it will be appreciated that those skilled in the art will be able to devise various arrangements which , although not explicitly described or shown herein , embody the principles of the invention and are included within its spirit and scope . furthermore , all examples and conditional language recited herein are principally intended to aid the reader in understanding the principles of the invention and the concepts contributed by the inventors to furthering the art , and are to be construed as being without limitation to such specifically recited examples and conditions . moreover , all statements herein reciting principles , aspects , and embodiments of the invention as well as specific examples thereof , are intended to encompass both structural and functional equivalents thereof . additionally , it is intended that such equivalents include both currently known equivalents and equivalents developed in the future , i . e ., any elements developed that perform the same function , regardless of structure . the scope of the present invention , therefore , is not intended to be limited to the exemplary embodiments shown and described herein . rather , the scope and spirit of present invention is embodied by the appended claims . | 7 |
carbonic acid ( 20 mmol ), thionylchloride ( 40 mmol ) and a catalytical amount of dmf are mixed with toluene ( 20 ml ) and heated to reflux for 3 - 6 h . the mixture is cooled to r . t . and concentrated in vacuo . the crude product is dried at 0 . 1 mbar , when appropriate . the acyl chlorides are added without further purification to thiosemicarbazide ( 4 mmol ) in dry pyridine ( 4 ml ) at 0 ° c . the mixture is stirred for further 12 h at r . t . excess pyridine is removed in vacuo . the crude mixture was crystallised from ethanol to remove pyridinium - hydrochloride . the acylated thiosemicarbazide ( 0 . 5 mmol ) was dissolved in 3 ml of ethanol . bromoacetophenone ( 0 . 5 mmol ) was added , and the mixture was refluxed for 30 min . the product precipitated on cooling to r . t . the salt was suspended in dichloromethane and neutralized by nahco 3 - sol . ( 3 × 25 ml ) and washed with brine ( 1 × 25 ml ). the dichloromethane extract was dried over mgso 4 and concentrated in vacuo . the crude product was recrystallised ( ethylacetate , ethanol ) or purified by chromatography ( silica gel , ethylacetate / hexane ) to provide the final compound in & gt ; 95 % purity . 1 h - nmr ( 300 mhz , dmso - d 6 ): δ = 11 . 10 ( s , 1h , 5 - nh ); 9 . 78 ( s , 1h , 6 - nh ); 9 . 10 ( s , 1 arom . h , 1 - ch ); 8 . 80 ( d , 1 arom . h , 2 - ch , j = 3 . 7 hz ); 8 . 27 ( d , 1 arom . h , 4 - ch , j = 8 . 0 hz ); 7 . 84 ( d , 2 arom . h , 8 - ch , j = 7 . 4 hz ); 7 . 60 ( dd , 1 arom . h , 3 - ch , j = 4 . 9 . 7 . 8 hz ); 7 . 40 ( t , 2 arom . h , 9 - ch , j = 7 . 5 hz ); 7 . 32 - 7 . 27 ( m , 2h , arom . h , 10 - ch , thiazol ) ppm . 1 h - nmr ( 300 mhz , dmso - d 6 ): δ = 11 . 16 ( s , 1h , 6 - nh ); 9 . 85 ( s , 1h , 7 - nh ); 9 . 08 ( s , 1 arom . h , 1 - ch ); 8 . 80 ( d , 1 arom . h , 2 - ch , j = 3 . 6 hz ); 8 . 57 ( s , 1 arom . h , 12 - ch ); 8 . 27 ( d , 1 arom . h , 4 - ch , j = 7 . 9 hz ); 7 . 88 ( d , 1 arom . h , 3 - ch , j = 7 . 2 hz ); 7 . 73 ( s , 1h , 9 - ch , thiazol ); 7 . 65 - 7 . 59 ( m , 2 arom . h , 13 - ch , 15 - ch ); 7 . 46 - 7 . 39 ( m , 2 arom . h , 14 - ch , 16 - ch ) ppm . 1 h - nmr ( 300 mhz , dmso - d 6 ): δ = 11 . 05 ( s , 1h , 6 - nh ); 9 . 78 ( s , 1h , 7 - nh ); 8 . 55 ( s , 1 arom . h , 3 - ch ); 8 . 10 - 7 . 96 ( m , 4 arom . h , 1 - ch , 4 - ch , 5 - ch ); 7 . 80 ( d , 2 arom . h , 10 - ch , j = 8 . 5 hz ); 7 . 67 - 7 . 63 ( m , 2 arom . h , 2 - ch ); 7 . 59 ( d , 2 arom . h , 9 - ch , j = 8 . 5 hz ); 7 . 36 ( s , 1h , 8 - ch thiazol - h ) ppm . 1 h - nmr ( 300 mhz , dmso - d 6 ): δ = 11 . 12 ( s , 1h , 11 - nh ); 9 . 84 ( s , 1h , 10 - nh ); 8 . 59 ( s , 1 arom . h , 17 - ch ); 8 . 57 ( s , 1 arom . h , 7 - ch ); 8 . 10 - 8 . 00 ( m , 4 arom . h , 9 - ch , 10 - ch , 2 - ch ); 7 . 87 ( d , 1 arom . h , 19 - ch , j = 7 . 1 hz ); 7 . 74 ( s , 1 arom . h , 15 - ch , thiazol ); 7 . 66 - 7 . 60 ( m , 3 arom . h , 3 - ch , 4 - ch , 21 - ch ); 7 . 44 ( d , 1 arom . h , 22 - ch , j = 8 . 2 hz ); 7 . 38 ( t , 1 arom . h , 20 - ch , j = 7 . 3 hz ) ppm . 13 c - nmr ( 75 mhz , dmso - d 6 ): δ = 172 . 9 ( 13 - c , thiazol ); 167 . 4 ( conr ); 159 . 4 ( coor ); 153 . 0 ( 14 - c , thiazol ); 144 . 8 ( 23 - c ); 139 . 1 ( 17 - ch ); 135 . 2 ( 6 - ch ); 132 . 7 ( 8 - c ); 132 . 3 ( 5 - ch ); 130 . 3 ( 1 - c ); 129 . 7 ( 7 - ch ); 129 . 5 ( 3 - ch ); 129 . 0 ( 10 - ch ); 128 . 8 ( 2 - ch ); 128 . 4 ( 4 - ch ); 127 . 7 ( 19 - c ); 125 . 4 ( 20 - c ); 124 . 5 ( 9 - ch ); 121 . 1 ( 16 - c ); 119 . 9 ( 18 - c ); 116 . 5 ( 22 - ch ); 110 . 7 ( 15 - ch , thiazol ) ppm . 1 h - nmr ( 300 mhz , dmso - d 6 ): δ = 10 . 99 ( s , 1h , 5 - nh ); 9 . 78 ( s , 1h , 6 - nh ); 8 . 96 ( s , 1 arom . h , 11 - ch ); 8 . 03 - 7 . 98 ( m , 2 arom . h , 3 - ch ); 7 . 87 ( d , 1 arom . h , 13 - ch , j = 7 . 5 hz ); 7 . 70 ( s , 1 arom . h , 9 - ch , thiazol - h ); 7 . 60 ( dd , 1 arom . h , 15 - ch , j = 7 . 8 , 15 . 2 hz ); 7 . 45 - 7 . 36 ( m , 4 arom . h , 2 - ch , 14 - ch , 16 - ch ) ppm . 13 c - nmr ( 75 mhz , dmso - d 6 ): δ = 172 . 1 ( 7 - c , thiazol ); 165 . 8 ( c — f ); 158 . 7 ( conr ); 152 . 2 ( coor ); 149 . 5 ( 17 - c ); 146 . 2 ( 11 - ch ); 144 . 0 ( 8 - c , thiazol ); 135 . 8 ( 4 - c ); 131 . 1 ( 10 - c ); 130 . 1 ( 3 - ch ); 128 . 9 ( 15 - ch ); 127 . 7 ( 13 - ch ); 125 . 5 ( 14 - ch ); 124 . 6 ( 16 - ch ); 120 . 4 ( 12 - c ); 115 . 6 ( 2 - ch ); 110 . 0 ( 9 - ch , thiazol ) ppm . 1 h - nmr ( 300 mhz , dmso - d 6 ): δ = 9 . 58 ( s , 1h , 5 - nh ); 9 . 03 ( s , 1h , 4 - nh ); 8 . 78 ( s , 1h , 6 - nh ); 8 . 27 ( d , 2 arom . h , 9 - ch , j = 8 . 7 hz ); 8 . 1 ( d , 2 arom . h , 8 - ch , j = 8 . 7 hz ); 7 . 67 ( s , 1h , 7 - ch , thiazol - h ); 7 . 53 ( d , 2 arom . h , 3 - ch , j = 7 . 9 hz ); 7 . 25 ( t , 2 arom . h , 2 - ch , j = 7 . 8 hz ); 6 . 96 ( t , 1 arom . h , 1 - ch , j = 7 . 3 hz ) ppm . the crude product obtained from the generic procedure was recrystallized from ethyl acetate to provide 88 mg ( 31 %) of n ′-( 4 -( 4 -( nitrophenyl ) thiazol - 2 - yl )- 1h - benz [ d ] imidazol - 5 - carbhydrazid as pale yellow green solid . 1 h - nmr ( 300 mhz , dmso - d 6 ): δ = 12 . 74 ( s , 1h , 2 - nh ), 10 . 89 ( s , 1h , 6 - nh ), 9 . 79 ( s , 1h , 7 - nh ), 8 . 38 - 8 . 11 ( m , 6h , 1 - h , 3 - h , 4 - h , 5 - h , 10 - h ), 7 . 80 - 7 . 64 ( m , 3h , 8 - h , 9 - h ) ppm . the crude product obtained from the generic procedure was recrystallized from ethyl acetate to provide 33 % of compound 44 . thioflavine s ( ths ) assay for aggregation of tau : 10 μm of the tau construct k19 were incubated with compounds in a concentration range from 1 nm up to 200 μm in the presence of 2 . 5 μm heparin in 50 mm nh 4 ac buffer over night at 37 ° c . after addition of 20 μm ths the signal was measured at 521 nm ( emission ) at an excitation wavelength of 440 nm . the results of this assay are presented in the ic50 column and dc50 column of table 1 below . selection of an n2a , tet - on , g418 - resistant cell line : n2a cells were cotransfected with both the puhd172 - 1 plasmid ( encoding the rtta , obtained from h . bujard , heidelberg ) and peu - 1 plasmid ( encoding g418 resistance , a derivative of prc / cmv , invitrogen ) ( ratio 20 : 1 ; 1 μg / well of 6 - well plates ) using the dotap transfection reagent ( roche , basel , ch ). the cells were cultured in eagle &# 39 ; s minimum essential medium ( mem ) supplemented with 10 % defined fetal bovine serum and subjected to g418 ( 600 μg / ml ) and selection . the cells were fed with fresh media every 4 days for 3 - 4 weeks when single colonies appeared . clones were tested for the induction level by transient transfection of puhg 16 - 3 plasmid and the induction of β - galactosidase was measured . the pbi - 5 plasmid was also transiently transfected into these cells , the luciferase assay showed 230 - fold induction . generation of inducible tet - on cell lines : the dna fragments encoding the appropriate tau constructs ( k18wt , k18δk280 , k18 / δk280 / pp ) were inserted into the bidirectional vector pbi - 5 between clai and sali restriction sites ( pbi - 5 is an unpublished derivative of pbi - 2 , baron et al ., 1995 ). the pbi - 5 / k18 - derived plasmids with px343 ( plasmid encoding the hygromycin resistance ) were used for cotransfection of n2a / tet - on , g418 - resistant cells with the aid of dotap ( 20 : 1 plasmid ratio ; 1 μg / well of 6 - well plates ). the cells were seeded at 4 × 10 5 cells per well . on the following day cells were transferred to 100 - mm dishes and selected with 100 μg / ml of hygromycin and 600 μg / ml of g418 . clonal cell lines were screened for the inducible expression of k18 derivatives by measuring luciferase activity with the luciferase assay and immunofluorescence for tau protein with the polyclonal pan - tau antibody k9ja . induction of k18 - derivatives in tet - on n2a cells : the inducible n2a / k18 - derivatives cells were cultured in mem medium supplemented with 10 % fetal calf serum , 2 mm glutamine and 0 . 1 % nonessential amino acids . the expression of k18 constructs was induced by adding 1 μg doxycyclin ( dox ) per 1 ml medium . the induction was continued for 7 - 11 days , the medium was changed 3 times ( always complemented with doxycyclin ). for tau solubility assays the cells were collected by pelleting during centrifugation at 1000 × g for 5 min . the levels and solubility of tau k18 / δk280 were determined following greenberg and davies ( 1990 ). the cells were homogenized ( diax900 , heidolph , schwabach , germany ) in 10 vol ( w / v ) of buffer consisting of 10 mm tris - hcl ( ph 7 . 4 ), 0 . 8 m nacl , 1 mm egta , and 10 % sucrose . the homogenate was spun for 20 min at 20000 × g , and the supernatant was retained . the pellet was re - homogenized in 5 vol of homogenization buffer and re - centrifuged . both supernatants were combined , brought to 1 % n - laurylsarkosinate ( w / v ) and incubated for 1 hr at room temperature while shaking , followed by centrifugation at 100 000 × g for 1 hr . the sarkosyl - insoluble pellets were resuspended in 50 mm tris - hcl ( ph 7 . 4 ), 0 . 5 ml per 1 g of starting material . the supernatant and sarkosyl - insoluble pellet samples were analyzed by western blotting . the amount of material loaded for supernatant and sarkosyl - insoluble pellet represented about 0 . 5 % and 15 % of the total material present in the supernatant and pellet respectively ( the ratio between supernatant and sarkosyl insoluble pellet was always 1 : 30 ). for quantification of tau levels in each fraction , the western blots were probed with pan - tau antibody k9ja and analyzed by densitometry ( las 3000 and aida software , raytest , straubenhardt , germany ). quantitation of tau aggregation in cells by thioflavin s ( ths ) staining : tet - on inducible undifferentiated n2a cells were treated with 1 μg / ml doxycyclin for 5 , 7 or 9 days in a culture dish . after that the cells were trypsinized and transferred to coverslips and incubated overnight . the cells on the coverslips were fixed with 4 % paraformaldehyde in pbs for 15 min , then permeabilized with 80 % meoh for 6 min at − 20 ° c ., and incubated with 0 . 1 % thioflavin s for 5 min and washed three times in ethanol ( 50 %). the samples were incubated with antibody k9ja in 5 % goat serum ( pbs ). the secondary anti rabbit antibody labeled with cy5 was also diluted with 5 % goat serum in pbs and incubated for 45 min . the cells were washed twice with pbs , once with water and mounted . cells containing distinct ths signals indicating the presence of insoluble aggregated material with β - pleated sheets were scored in many independent fields containing a total of 500 cells . neurotoxicity assay : neurotoxicity was assessed using an ldh ( lactate dehydrogenase ) assay kit ( roche , mannheim , germany ) according to the manufacturer &# 39 ; s specifications . in the viability assay the aggregation inhibitor compound was added at a final concentration of 10 μm to uninduced n2a cells . the activity of ldh was measured spectrophotometrically at 492 nm . cell death was calculated as percent of ldh released into medium , compared to total ldh obtained after total cell lysis . the results of this assay are presented in the ldh column of table 1 below . tau aggregation and inhibition assay in cells : the n2a / k18δk280 cells were grown in nunc flasks in mem medium supplemented with g418 ( 300 μg / ml ) and hygromycin ( 100 μg / ml ). the protein expression in the control sample was induced by addition of 1 μg / ml doxycyclin ( final concentration ) and cells were incubated for 5 days . in the inhibition assay the aggregation inhibitor compound was added together with doxycyclin at a final concentration of 10 μm . after 5 days of protein expression the cells were transferred to glass coverslips coated with polylysine , fixed with 3 . 7 % paraformaldehyde in pbs , and briefly permeabilized with 80 % meoh . next the cells were incubated with 0 . 01 % thioflavin - s , followed by incubation with rabbit antibody k9ja and secondary anti rabbit antibody labeled with cy5 . for assaying the dissolution of preformed tau aggregates the inducible n2a cells were incubated with 1 μg / ml doxycyclin for 5 days . after that the medium was exchanged for a new one containing 1 μg / ml doxycyclin and 10 μm of the inhibitor compound and the incubation was continued for two more days . transfer of cells onto cover slips and staining with ths and tau antibody was performed as above . finally the cells showing ths staining were scored in independent fields containing at least 500 cells . the results of this assay are presented in the inhibition in cells column of table 1 below . std - nmr : all std nmr experiments were made in 3 mm match ® tubes in a 700 mhz spectrometer with cryogenic probe head at 295 k . the quantity of protein was kept small by the small diameter of the sample tubes . the spectra were measured with a spectral width of 11 . 0208 ppm and 32k data points with application of the watergate water suppression ( w5 - sequence ). the suppression of the protein resonances was reached by a spin lock pulse with a length of 15 ms and a attenuation of 11 db . we used a pulse program in which the presaturation was accomplished alternating after each scan for the on and off resonance experiment at the selected frequencies . thus artefacts are prevented during the difference formation due to in homogeneities . as point of irradiation for the on resonance experiments we selected 540 hz ( 0 . 77 ppm ). as point of irradiating for the off resonance experiments 40 , 000 hz ( 57 . 1 ppm ) was selected . the saturation duration in all experiments was 4 seconds , the attenuation of the saturation power 45 db . 2044 scans were collected per experiment . after phase correction the fid was multiplied by an exponential function to improve the signal to noise ratio , which caused a line broadening of 1 hz . for the determination of the binding epitope a sample with 33 . 33 μm bsc3094 , μm soluble k18 and 80 μm dtt - d 6 in 200 μl pbs / d 2 o was used . subsequently , std spectrum and reference spectrum were compared with one another and the magnitude of the std effects and the binding epitope were determined . fig1 demonstrates the binding epitope of compound bsc3094 with tau construct k18 derived from std nmr . effects larger than 50 % form the binding epitope . for the determination of the dissociation constant a sample with 10 μm soluble k18 and 80 μm dtt - d 6 in 200 μl pbs / d 2 o was prepared . then the concentration of bsc3094 was varied to 16 . 7 , 33 . 3 , 50 . 0 , 67 . 7 , 83 . 3 , 100 . 0 and 200 . 0 μm . this corresponds to a change of the excess of bsc3094 to the tau construct of 1 . 67 - fold to 20 - fold . evaluation of the data until 83 . 3 μm resulted in the dissociation constants . fig2 demonstrates the determination of dissociation constant of k18 - bsc3094 complex by std - nmr using the titration data for proton i . regression analysis of the data yields a k d = 62 ± 12 μm . surface plasmon resonance : surface plasmon resonance experiments were accomplished at a biacore t100 instrument at a temperature of 298 k using cm5 - chips . as buffer system sterile pbs buffer with 1 % dmso was used . 325 fmol of soluble tau construct k18 was immobilized . we selected for the regeneration a 20 second injection with 50 mm of hydrochloric acid followed by 60 seconds as a stabilization period . a flow rate of 30 μl / min was selected . as time of contact the maximally possible time of 700 seconds and as dissociation and a stabilization time in each case 300 seconds were selected . the evaluation of the kinetic data was accomplished by use of the biacore t100 evaluation software . further modifications and alternative embodiments of various aspects of the invention will be apparent to those skilled in the art in view of this description . accordingly , this description is to be construed as illustrative only and is for the purpose of teaching those skilled in the art the general manner of carrying out the invention . it is to be understood that the forms of the invention shown and described herein are to be taken as examples of embodiments . elements and materials may be substituted for those illustrated and described herein , parts and processes may be reversed , and certain features of the invention may be utilized independently , all as would be apparent to one skilled in the art after having the benefit of this description of the invention . changes may be made in the elements described herein without departing from the spirit and scope of the invention as described in the following claims . | 2 |
compounds of the invention , including n - oxides thereof and salts of the compounds or n - oxides , can be prepared using known organic synthesis techniques and can be synthesized according to any of numerous possible synthetic routes . the reactions for preparing compounds of the invention can be carried out in suitable solvents , which can be readily selected by one of skill in the art of organic synthesis . suitable solvents can be substantially non - reactive with the starting materials ( reactants ), the intermediates , or products at the temperatures at which the reactions are carried out , e . g ., temperatures that can range from the solvent &# 39 ; s freezing temperature to the solvent &# 39 ; s boiling temperature . a given reaction can be carried out in one solvent or a mixture of more than one solvent . depending on the particular reaction step , suitable solvents for a particular reaction step can be selected by the skilled artisan . preparation of compounds of the invention can involve the protection and deprotection of various chemical groups . the need for protection and deprotection , and the selection of appropriate protecting groups , can be readily determined by one skilled in the art . the chemistry of protecting groups can be found , for example , in t . w . greene and p . g . m . wuts , protective groups in organic synthesis , 3 rd ed ., wiley & amp ; sons , inc ., new york ( 1999 ), which is incorporated herein by reference in its entirety . reactions can be monitored according to any suitable method known in the art . for example , product formation can be monitored by spectroscopic means , such as nuclear magnetic resonance spectroscopy ( e . g ., 1 h or 13 c ), infrared spectroscopy , spectrophotometry ( e . g ., uv - visible ), mass spectrometry , or by chromatographic methods such as high - performance liquid chromatography ( hplc ) or thin layer chromatography ( tlc ). compounds of formula i and intermediates thereof may be prepared according to the following reaction schemes and accompanying discussion . unless otherwise indicated , r 1 , r 2 , r 3 , r 4 , t 1 , t 2 , t 3 , x 1 , x 2 , x 3 , x 4 and structural formula i in the reaction schemes and discussion that follow are as defined above . in general , the compounds of this invention may be made by processes which include processes analogous to those known in the chemical arts , particularly in light of the description contained herein . certain processes for the manufacture of the compounds of this invention and intermediates thereof are provided as further features of the invention and are illustrated by the following reaction schemes . other processes are described in the experimental section . the schemes and examples provided herein ( including the corresponding description ) are for illustration only , and not intended to limit the scope of the present invention . scheme 1 refers to preparation of compounds of formula i . referring to scheme 1 , compounds of formula 1 - 1 , 1 - 2 , 1 - 3 and 1 - 5 [ where z 1 is a halogen ( e . g . cl , br or i ), z 2 is a boronic ester ( e . g . 4 , 4 , 5 , 5 - tetramethyl - 1 , 3 , 2 - dioxaborolan - 2 - yl ) or boronic acid and y is a simple alkyl ( e . g . methyl , ethyl )] are either commercially available or can be obtained by the methods described herein . a compound of formula 1 - 4 can be made by coupling a compound of formula 1 - 1 and 1 - 3 under suitable conditions such as a suzuki reaction [ a . suzuki , j . organomet . chem . 1999 , 576 , 147 - 168 ; n . miyaura and a . suzuki , chem . rev . 1995 , 95 , 2457 - 2483 ; a . f . littke et al ., j . am . chem . soc . 2000 , 122 , 4020 - 4028 ]. the coupling can be accomplished , for example , by heating a mixture of a compound of formula 1 - 1 and 1 - 3 in the presence of a base ( such as k 2 co 3 ), a metal catalyst [ such as a palladium catalyst , e . g pd ( dppf ) cl 2 ], in an appropriate solvent ( such as 1 , 4 - dioxane ). alternatively , a compound of formula 1 - 1 can be converted to a compound of formula 1 - 2 ( wherein z 2 is defined as above ). for example , this reaction can be accomplished by reacting a compound of formula 1 - 1 ( wherein z 1 is halogen such as br ) with 4 , 4 , 4 ′, 4 ′, 5 , 5 , 5 ′, 5 ′- octamethyl - 2 , 2 ′- bi - 1 , 3 , 2 - dioxaborolane , a suitable base ( such as potassium acetate ), and a palladium catalyst { such as [ 1 , 1 ′- bis ( diphenylphosphino ) ferrocene ] dichloropalladium ( ii )} in a suitable solvent such as toluene . a compound of formula 1 - 2 can then be coupled with a compound of formula 1 - 5 following similar conditions described above to give a compound of formula 1 - 4 . the alkyl ester moiety of compound 1 - 4 can subsequently be hydrolyzed to a compound of formula 1 - 6 in the presence of a suitable base ( e . g . naoh ). alternatively , a compound of formula 1 - 6 can be prepared by the directly coupling of a compound of formula 1 - 2 and a compound of formula 1 - 5 in the presence of an aqueous base ( e . g . naoh ) and a metal catalyst [ such as a palladium catalyst , e . g . pd ( pph 3 ) 4 ] in an appropriate solvent ( e . g . acetonitrile ) at elevated temperature . subsequently a compound of formula i can be prepared by coupling of a compound of formula of 1 - 6 with an amine ( r 1 — nh 2 ) by amidation methods well known to those skilled in the art . for example , the reaction can be accomplished in the presence of a base ( e . g . et 3 n ) and a peptide coupling agent ( e . g . hatu ) in an appropriate solvent ( e . g . dichloromethane ) at an appropriate temperature ( e . g . ambient temperature ). alternatively , a compound of formula i can be prepared directly from an ester of formula 1 - 4 by reacting it with an amine ( r 1 — nh 2 ) in the presence of a base ( e . g . 1 , 3 , 4 , 6 , 7 , 8 - hexahydro - 2h - pyrimido [ 1 , 2 - a ] pyrimidine ) in an appropriate solvent ( e . g . n , n - dimethylformamide ) at an appropriate temperature ( e . g . at an elevated temperature ). scheme 2 refers to preparation of intermediates of formula 1 - 4 . referring to scheme 2 , a compound of formula 2 - 2 can be obtained by coupling of a compound of formula 1 - 2 with a compound of formula 2 - 1 [ wherein z 1 can be , for example , a halogen ( e . g . cl , br or i ) and z 3 can be , for example , 6 - methyl - 1 , 3 , 6 , 2 - dioxazaborocane - 4 , 8 - dione ] under suitable conditions such as a suzuki reaction [ a . suzuki , j . organomet . chem . 1999 , 576 , 147 - 168 ; n . miyaura and a . suzuki , chem . rev . 1995 , 95 , 2457 - 2483 ; a . f . littke et al ., j . am . chem . soc . 2000 , 122 , 4020 - 4028 ]. the coupling can be accomplished , for example , by heating a mixture of a compound of formula 1 - 2 and 2 - 1 in the presence of a base ( such as kf ), a metal catalyst [ such as a palladium catalyst , e . g pd ( pph 3 ) 4 ], in an appropriate solvent ( such as acetonitrile ). a compound of formula 2 - 2 can then be coupled to a compound of formula r 4 — z 1 under suzuki reaction conditions such as those already described to furnish an intermediate of formula 1 - 4 , which can be used in scheme 1 to give compounds of formula i . scheme 3 refers to a 3 - step preparation of a compound of formula 3 - 3 ( which is a specific compound of formula i wherein one of r 2 and r 3 is h and the other is f ) from a compound of formula 3 - 1 ( which is a specific compound of formula i wherein both r 2 and r 3 are h ). benzylic bromination of a compound of formula 3 - 1 by a brominating agent such as n - bromosuccinimide ( nbs ) in the presense of a radical initator such as azobisisobutyronitrile ( aibn ) followed by hydrolysis under aqueous conditions will furnish an intermediate benzylic hydroxyl compound of formula 3 - 2 . conversion of the hydroxyl group of the compound of formula 3 - 2 into a leaving group followed by treatment with a fluorinating agent ( e . g . a hf - amine complex such as hf - pyridine or triethylamine trihydrofluoride ) will give a compound of formula 3 - 3 . this conversion can be accomplished , for example , by treating the compound of formula 3 - 2 with with an activating agent such as 1 , 1 , 2 , 2 , 3 , 3 , 4 , 4 , 4 - nonafluorobutane - 1 - sulfonyl fluoride in the presence of triethylamine trihydrofluoride . additional starting materials and intermediates useful for making the compounds of the present invention can be obtained from chemical vendors such as sigma - aldrich or can be made according to methods described in the chemical art . those skilled in the art can recognize that in all of the schemes described herein , if there are functional ( reactive ) groups present on a part of the compound structure such as a substituent group , for example r 1 , r 2 , r 3 , r 4 , t 1 , t 2 , t 3 , x 1 , x 2 , x 3 , x 4 , etc ., further modification can be made if appropriate and / or desired , using methods well known to those skilled in the art . for example , a — cn group can be hydrolyzed to afford an amide group ; a carboxylic acid can be converted to an amide ; a carboxylic acid can be converted to an ester , which in turn can be reduced to an alcohol , which in turn can be further modified . for another example , an oh group can be converted into a better leaving group such as a methanesulfonate , which in turn is suitable for nucleophilic substitution , such as by a cyanide ion ( cn − ). for another example , an — s — can be oxidized to — s (═ o )— and / or — s (═ o ) 2 —. for yet another example , an unsaturated bond such as c ═ c or ceo can be reduced to a saturated bond by hydrogenation . in some embodiments , a primary amine or a secondary amine moiety ( present on a substituent group such as r 3 , r 4 , r 9 , r 10 , etc .) can be converted to an amide , sulfonamide , urea , or thiourea moiety by reacting it with an appropriate reagent such as an acid chloride , a sulfonyl chloride , an isocyanate , or a thioisocyanate compound . one skilled in the art will recognize further such modifications . thus , a compound of formula i having a substituent that contains a functional group can be converted to another compound of formula i having a different substituent group . similarly , those skilled in the art can also recognize that in all of the schemes described herein , if there are functional ( reactive ) groups present on a substituent group such as r 3 , r 4 , r 9 , r 10 , etc ., these functional groups can be protected / deprotected in the course of the synthetic scheme described here , if appropriate and / or desired . for example , an oh group can be protected by a benzyl , methyl , or acetyl group , which can be deprotected and converted back to the oh group in a later stage of the synthetic process . for another example , an nh 2 group can be protected by a benzyloxycarbonyl ( cbz ) or boc group ; conversion back to the nh 2 group can be carried out at a later stage of the synthetic process via deprotection . as used herein , the term “ reacting ” ( or “ reaction ” or “ reacted ”) refers to the bringing together of designated chemical reactants such that a chemical transformation takes place generating a compound different from any initially introduced into the system . reactions can take place in the presence or absence of solvent . compounds of formula i may exist as stereoisomers , such as atropisomers , racemates , enantiomers , or diastereomers . conventional techniques for the preparation / isolation of individual enantiomers include chiral synthesis from a suitable optically pure precursor or resolution of the racemate using , for example , chiral high - performance liquid chromatography ( hplc ). alternatively , the racemate ( or a racemic precursor ) may be reacted with a suitable optically active compound , for example , an alcohol , or , in the case where the compound contains an acidic or basic moiety , an acid or base such as tartaric acid or 1 - phenylethylamine . the resulting diastereomeric mixture may be separated by chromatography and / or fractional crystallization and one or both of the diastereoisomers converted to the corresponding pure enantiomer ( s ) by means well known to one skilled in the art . chiral compounds of formula i ( and chiral precursors thereof ) may be obtained in enantiomerically enriched form using chromatography , typically hplc , on an asymmetric resin with a mobile phase consisting of a hydrocarbon , typically heptane or hexane , containing from 0 % to 50 % 2 - propanol , typically from 2 % to 20 %, and from 0 % to 5 % of an alkylamine , typically 0 . 1 % diethylamine . concentration of the eluate affords the enriched mixture . stereoisomeric conglomerates may be separated by conventional techniques known to those skilled in the art . see , e . g ., stereochemistry of organic compounds by e . l . eliel and s . h . wilen ( wiley , new york , 1994 ), the disclosure of which is incorporated herein by reference in its entirety . suitable stereoselective techniques are well known to those of ordinary skill in the art . where a compound of formula i contains an alkenyl or alkenylene ( alkylidene ) group , geometric cis / trans ( or z / e ) isomers are possible . cis / trans isomers may be separated by conventional techniques well known to those skilled in the art , for example , chromatography and fractional crystallization . salts of the present invention can be prepared according to methods known to those of skill in the art . the compounds of formula i that are basic in nature are capable of forming a wide variety of salts with various inorganic and organic acids . although such salts must be pharmaceutically acceptable for administration to animals , it is often desirable in practice to initially isolate the compound of the present invention from the reaction mixture as a pharmaceutically unacceptable salt and then simply convert the latter back to the free base compound by treatment with an alkaline reagent and subsequently convert the latter free base to a pharmaceutically acceptable acid addition salt . the acid addition salts of the basic compounds of this invention can be prepared by treating the basic compound with a substantially equivalent amount of the selected mineral or organic acid in an aqueous solvent medium or in a suitable organic solvent , such as methanol or ethanol . upon evaporation of the solvent , the desired solid salt is obtained . the desired acid salt can also be precipitated from a solution of the free base in an organic solvent by adding an appropriate mineral or organic acid to the solution . if the inventive compound is a base , the desired pharmaceutically acceptable salt may be prepared by any suitable method available in the art , for example , treatment of the free base with an inorganic acid , such as hydrochloric acid , hydrobromic acid , sulfuric acid , nitric acid , phosphoric acid and the like , or with an organic acid , such as acetic acid , maleic acid , succinic acid , mandelic acid , fumaric acid , malonic acid , pyruvic acid , oxalic acid , glycolic acid , salicylic acid , isonicotinic acid , lactic acid , pantothenic acid , bitartric acid , ascorbic acid , 2 , 5 - dihydroxybenzoic acid , gluconic acid , saccharic acid , formic acid , methanesulfonic acid , ethanesulfonic acid , benzenesulfonic acid , p - toluenesulfonic acid , and pamoic [ i . e ., 4 , 4 ′- methanediylbis ( 3 - hydroxynaphthalene - 2 - carboxylic acid )] acid , a pyranosidyl acid , such as glucuronic acid or galacturonic acid , an alpha - hydroxy acid , such as citric acid or tartaric acid , an amino acid , such as aspartic acid or glutamic acid , an aromatic acid , such as benzoic acid or cinnamic acid , a sulfonic acid , such as ethanesulfonic acid , or the like . those compounds of formula i that are acidic in nature are capable of forming base salts with various pharmacologically acceptable cations . examples of such salts include the alkali metal or alkaline earth metal salts , and particularly the sodium and potassium salts . these salts are all prepared by conventional techniques . the chemical bases which are used as reagents to prepare the pharmaceutically acceptable base salts of this invention are those which form non - toxic base salts with the acidic compounds of formula i . these salts may be prepared by any suitable method , for example , treatment of the free acid with an inorganic or organic base , such as an amine ( primary , secondary or tertiary ), an alkali metal hydroxide or alkaline earth metal hydroxide , or the like . these salts can also be prepared by treating the corresponding acidic compounds with an aqueous solution containing the desired pharmacologically acceptable cations , and then evaporating the resulting solution to dryness , for example under reduced pressure . alternatively , they may also be prepared by mixing lower alkanolic solutions of the acidic compounds and the desired alkali metal alkoxide together , and then evaporating the resulting solution to dryness in the same manner as before . in either case , stoichiometric quantities of reagents are , for example , employed in order to ensure completeness of reaction and maximum yields of the desired final product . pharmaceutically acceptable salts of compounds of formula i ( including compounds of formula ia or ib ) may be prepared by one or more of three methods : ( i ) by reacting the compound of formula i with the desired acid or base ; ( ii ) by removing an acid - or base - labile protecting group from a suitable precursor of the compound of formula i or by ring - opening a suitable cyclic precursor , for example , a lactone or lactam , using the desired acid or base ; or ( iii ) by converting one salt of the compound of formula i to another by reaction with an appropriate acid or base or by means of a suitable ion exchange column . all three reactions are typically carried out in solution . the resulting salt may precipitate out and be collected by filtration or may be recovered by evaporation of the solvent . the degree of ionization in the resulting salt may vary from completely ionized to almost non - ionized . polymorphs can be prepared according to techniques well - known to those skilled in the art , for example , by crystallization . when any racemate crystallizes , crystals of two different types are possible . the first type is the racemic compound ( true racemate ) referred to above wherein one homogeneous form of crystal is produced containing both enantiomers in equimolar amounts . the second type is the racemic mixture or conglomerate wherein two forms of crystal are produced in equimolar amounts each comprising a single enantiomer . while both of the crystal forms present in a racemic mixture may have almost identical physical properties , they may have different physical properties compared to the true racemate . racemic mixtures may be separated by conventional techniques known to those skilled in the art — see , for example , stereochemistry of organic compounds by e . l . eliel and s . h . wilen ( wiley , new york , 1994 ). the invention also includes isotopically labeled compounds of formula i wherein one or more atoms is replaced by an atom having the same atomic number , but an atomic mass or mass number different from the atomic mass or mass number usually found in nature . isotopically labeled compounds of formula i ( or pharmaceutically acceptable salts thereof or n - oxides thereof ) can generally be prepared by conventional techniques known to those skilled in the art or by processes analogous to those described herein , using an appropriate isotopically labeled reagent in place of the non - labeled reagent otherwise employed . prodrugs in accordance with the invention can , for example , be produced by replacing appropriate functionalities present in the compounds of formula i with certain moieties known to those skilled in the art as ‘ pro - moieties ’ as described , for example , in design of prodrugs by h . bundgaard ( elsevier , 1985 ). the compounds of formula i should be assessed for their biopharmaceutical properties , such as solubility and solution stability ( across ph ), permeability , etc ., in order to select the most appropriate dosage form and route of administration for treatment of the proposed indication . compounds of the invention intended for pharmaceutical use may be administered as crystalline or amorphous products . they may be obtained , for example , as solid plugs , powders , or films by methods such as precipitation , crystallization , freeze drying , spray drying , or evaporative drying . microwave or radio frequency drying may be used for this purpose . they may be administered alone or in combination with one or more other compounds of the invention or in combination with one or more other drugs ( or as any combination thereof ). generally , they will be administered as a formulation in association with one or more pharmaceutically acceptable excipients . the term “ excipient ” is used herein to describe any ingredient other than the compound ( s ) of the invention . the choice of excipient will to a large extent depend on factors such as the particular mode of administration , the effect of the excipient on solubility and stability , and the nature of the dosage form . pharmaceutical compositions suitable for the delivery of compounds of the present invention ( or pharmaceutically acceptable salts thereof ) and methods for their preparation will be readily apparent to those skilled in the art . such compositions and methods for their preparation may be found , for example , in remington &# 39 ; s pharmaceutical sciences , 19th edition ( mack publishing company , 1995 ). the compounds of the invention ( including n - oxides thereof and pharmaceutically acceptable salts of the foregoing ) may be administered orally . oral administration may involve swallowing , so that the compound enters the gastrointestinal tract , and / or buccal , lingual , or sublingual administration by which the compound enters the blood stream directly from the mouth . formulations suitable for oral administration include solid , semi - solid and liquid systems such as tablets ; soft or hard capsules containing multi - or nano - particulates , liquids , or powders ; lozenges ( including liquid - filled ); chews ; gels ; fast dispersing dosage forms ; films ; ovules ; sprays ; and buccal / mucoadhesive patches . liquid formulations include suspensions , solutions , syrups and elixirs . such formulations may be employed as fillers in soft or hard capsules ( made , for example , from gelatin or hydroxypropyl methyl cellulose ) and typically comprise a carrier , for example , water , ethanol , polyethylene glycol , propylene glycol , methyl cellulose , or a suitable oil , and one or more emulsifying agents and / or suspending agents . liquid formulations may also be prepared by the reconstitution of a solid , for example , from a sachet . the compounds of the invention may also be used in fast - dissolving , fast - disintegrating dosage forms such as those described by liang and chen , expert opinion in therapeutic patents 2001 , 11 , 981 - 986 . for tablet dosage forms , depending on dose , the drug may make up from 1 weight % to 80 weight % of the dosage form , more typically from 5 weight % to 60 weight % of the dosage form . in addition to the drug , tablets generally contain a disintegrant . examples of disintegrants include sodium starch glycolate , sodium carboxymethyl cellulose , calcium carboxymethyl cellulose , croscarmellose sodium , crospovidone , polyvinylpyrrolidone , methyl cellulose , microcrystalline cellulose , lower alkyl - substituted hydroxypropyl cellulose , starch , pregelatinized starch and sodium alginate . generally , the disintegrant will comprise from 1 weight % to 25 weight %, for example , from 5 weight % to 20 weight % of the dosage form . binders are generally used to impart cohesive qualities to a tablet formulation . suitable binders include microcrystalline cellulose , gelatin , sugars , polyethylene glycol , natural and synthetic gums , polyvinylpyrrolidone , pregelatinized starch , hydroxypropyl cellulose and hydroxypropyl methylcellulose . tablets may also contain diluents , such as lactose ( monohydrate , spray - dried monohydrate , anhydrous and the like ), mannitol , xylitol , dextrose , sucrose , sorbitol , microcrystalline cellulose , starch and dibasic calcium phosphate dihydrate . tablets may also optionally comprise surface active agents , such as sodium lauryl sulfate and polysorbate 80 , and glidants such as silicon dioxide and talc . when present , surface active agents may comprise from 0 . 2 weight % to 5 weight % of the tablet , and glidants may comprise from 0 . 2 weight % to 1 weight % of the tablet . tablets also generally contain lubricants such as magnesium stearate , calcium stearate , zinc stearate , sodium stearyl fumarate , and mixtures of magnesium stearate with sodium lauryl sulfate . lubricants generally comprise from 0 . 25 weight % to 10 weight %, for example , from 0 . 5 weight % to 3 weight % of the tablet . other possible ingredients include anti - oxidants , colorants , flavoring agents , preservatives and taste - masking agents . exemplary tablets contain up to about 80 % drug , from about 10 weight % to about 90 weight % binder , from about 0 weight % to about 85 weight % diluent , from about 2 weight % to about 10 weight % disintegrant , and from about 0 . 25 weight % to about 10 weight % lubricant . tablet blends may be compressed directly or by roller to form tablets . tablet blends or portions of blends may alternatively be wet -, dry -, or melt - granulated , melt - congealed , or extruded before tabletting . the final formulation may comprise one or more layers and may be coated or uncoated ; it may even be encapsulated . the formulation of tablets is discussed in pharmaceutical dosage forms : tablets , vol . 1 , by h . lieberman and l . lachman ( marcel dekker , new york , 1980 ). consumable oral films for human or veterinary use are typically pliable water - soluble or water - swellable thin film dosage forms which may be rapidly dissolving or mucoadhesive and typically comprise a compound of formula i , a film - forming polymer , a binder , a solvent , a humectant , a plasticizer , a stabilizer or emulsifier , a viscosity - modifying agent and a solvent . some components of the formulation may perform more than one function . the compound of formula i ( or pharmaceutically acceptable salts thereof or n - oxides thereof ) may be water - soluble or insoluble . a water - soluble compound typically comprises from 1 weight % to 80 weight %, more typically from 20 weight % to 50 weight %, of the solutes . less soluble compounds may comprise a smaller proportion of the composition , typically up to 30 weight % of the solutes . alternatively , the compound of formula i may be in the form of multiparticulate beads . the film - forming polymer may be selected from natural polysaccharides , proteins , or synthetic hydrocolloids and is typically present in the range 0 . 01 to 99 weight %, more typically in the range 30 to 80 weight %. other possible ingredients include anti - oxidants , colorants , flavorings and flavor enhancers , preservatives , salivary stimulating agents , cooling agents , co - solvents ( including oils ), emollients , bulking agents , anti - foaming agents , surfactants and taste - masking agents . films in accordance with the invention are typically prepared by evaporative drying of thin aqueous films coated onto a peelable backing support or paper . this may be done in a drying oven or tunnel , typically a combined coater dryer , or by freeze - drying or vacuuming . solid formulations for oral administration may be formulated to be immediate and / or modified release . modified release formulations include delayed -, sustained -, pulsed -, controlled -, targeted and programmed release . suitable modified release formulations for the purposes of the invention are described in u . s . pat . no . 6 , 106 , 864 . details of other suitable release technologies such as high energy dispersions and osmotic and coated particles are to be found in verma et al ., pharmaceutical technology on - line , 25 ( 2 ), 1 - 14 ( 2001 ). the use of chewing gum to achieve controlled release is described in wo 00 / 35298 . the compounds of the invention ( including n - oxides thereof and pharmaceutically acceptable salts of the foregoing ) may also be administered directly into the blood stream , into muscle , or into an internal organ . suitable means for parenteral administration include intravenous , intraarterial , intraperitoneal , intrathecal , intraventricular , intraurethral , intrasternal , intracranial , intramuscular , intrasynovial and subcutaneous . suitable devices for parenteral administration include needle ( including microneedle ) injectors , needle - free injectors and infusion techniques . parenteral formulations are typically aqueous solutions which may contain excipients such as salts , carbohydrates and buffering agents ( for example to a ph of from 3 to 9 ), but , for some applications , they may be more suitably formulated as a sterile non - aqueous solution or as a dried form to be used in conjunction with a suitable vehicle such as sterile , pyrogen - free water . the preparation of parenteral formulations under sterile conditions , for example , by lyophilization , may readily be accomplished using standard pharmaceutical techniques well known to those skilled in the art . the solubility of compounds of formula i ( including n - oxides thereof and pharmaceutically acceptable salts of the foregoing ) used in the preparation of parenteral solutions may be increased by the use of appropriate formulation techniques , such as the incorporation of solubility - enhancing agents . formulations for parenteral administration may be formulated to be immediate and / or modified release . modified release formulations include delayed -, sustained -, pulsed -, controlled -, targeted and programmed release . thus compounds of the invention may be formulated as a suspension or as a solid , semi - solid , or thixotropic liquid for administration as an implanted depot providing modified release of the active compound . examples of such formulations include drug - coated stents and semi - solids and suspensions comprising drug - loaded poly ( dl - lactic - coglycolic acid ) ( plga ) microspheres . the compounds of the invention ( including n - oxides thereof and pharmaceutically acceptable salts of the foregoing ) may also be administered topically , ( intra ) dermally , or transdermally to the skin or mucosa . typical formulations for this purpose include gels , hydrogels , lotions , solutions , creams , ointments , dusting powders , dressings , foams , films , skin patches , wafers , implants , sponges , fibers , bandages and microemulsions . liposomes may also be used . typical carriers include alcohol , water , mineral oil , liquid petrolatum , white petrolatum , glycerin , polyethylene glycol and propylene glycol . penetration enhancers may be incorporated . see e . g ., finnin and morgan , j . pharm . sci . 1999 , 88 , 955 - 958 . other means of topical administration include delivery by electroporation , iontophoresis , phonophoresis , sonophoresis and microneedle or needle - free ( e . g ., powderject ™, bioject ™, etc .) injection . formulations for topical administration may be formulated to be immediate and / or modified release . modified release formulations include delayed -, sustained -, pulsed -, controlled -, targeted and programmed release . the compounds of the invention ( including n - oxides thereof and pharmaceutically acceptable salts of the foregoing ) can also be administered intranasally or by inhalation , typically in the form of a dry powder ( either alone ; as a mixture , for example , in a dry blend with lactose ; or as a mixed component particle , for example , mixed with phospholipids , such as phosphatidylcholine ) from a dry powder inhaler , as an aerosol spray from a pressurized container , pump , spray , atomizer ( for example an atomizer using electrohydrodynamics to produce a fine mist ), or nebulizer , with or without the use of a suitable propellant , such as 1 , 1 , 1 , 2 - tetrafluoroethane or 1 , 1 , 1 , 2 , 3 , 3 , 3 - heptafluoropropane , or as nasal drops . for intranasal use , the powder may comprise a bioadhesive agent , for example , chitosan or cyclodextrin . the pressurized container , pump , spray , atomizer , or nebulizer contains a solution or suspension of the compound ( s ) of the invention comprising , for example , ethanol , aqueous ethanol , or a suitable alternative agent for dispersing , solubilizing , or extending release of the active , a propellant ( s ) as solvent and an optional surfactant , such as sorbitan trioleate , oleic acid , or an oligolactic acid . prior to use in a dry powder or suspension formulation , the drug product is micronized to a size suitable for delivery by inhalation ( typically less than 5 microns ). this may be achieved by any appropriate comminuting method , such as spiral jet milling , fluid bed jet milling , supercritical fluid processing to form nanoparticles , high pressure homogenization , or spray drying . capsules ( made , for example , from gelatin or hydroxypropyl methyl cellulose ), blisters and cartridges for use in an inhaler or insufflator may be formulated to contain a powder mix of the compound of the invention , a suitable powder base such as lactose or starch and a performance modifier such as l - leucine , mannitol , or magnesium stearate . the lactose may be anhydrous or in the form of the monohydrate . other suitable excipients include dextran , glucose , maltose , sorbitol , xylitol , fructose , sucrose and trehalose . a suitable solution formulation for use in an atomizer using electrohydrodynamics to produce a fine mist may contain from 1 μg to 20 mg of the compound of the invention per actuation and the actuation volume may vary from 1 μl to 100 μl . a typical formulation may comprise a compound of formula i or a pharmaceutically acceptable salt thereof , propylene glycol , sterile water , ethanol and sodium chloride . alternative solvents which may be used instead of propylene glycol include glycerol and polyethylene glycol . suitable flavors , such as menthol and levomenthol , or sweeteners , such as saccharin or saccharin sodium , may be added to those formulations of the invention intended for inhaled / intranasal administration . formulations for inhaled / intranasal administration may be formulated to be immediate and / or modified release using , for example , pgla . modified release formulations include delayed -, sustained -, pulsed -, controlled -, targeted and programmed release . in the case of dry powder inhalers and aerosols , the dosage unit is determined by means of a valve which delivers a metered amount . units in accordance with the invention are typically arranged to administer a metered dose or “ puff ” containing from 0 . 01 to 100 mg of the compound of formula i . the overall daily dose will typically be in the range 1 μg to 200 mg , which may be administered in a single dose or , more usually , as divided doses throughout the day . the compounds of the invention ( including n - oxides thereof and pharmaceutically acceptable salts of the foregoing ) may be administered rectally or vaginally , for example , in the form of a suppository , pessary , or enema . cocoa butter is a traditional suppository base , but various alternatives may be used as appropriate . formulations for rectal / vaginal administration may be formulated to be immediate and / or modified release . modified release formulations include delayed -, sustained -, pulsed -, controlled -, targeted and programmed release . the compounds of the invention ( including n - oxides thereof and pharmaceutically acceptable salts of the foregoing ) may also be administered directly to the eye or ear , typically in the form of drops of a micronized suspension or solution in isotonic , ph - adjusted , sterile saline . other formulations suitable for ocular and aural administration include ointments , gels , biodegradable ( e . g ., absorbable gel sponges , collagen ) and non - biodegradable ( e . g ., silicone ) implants , wafers , lenses and particulate or vesicular systems , such as niosomes or liposomes . a polymer such as crossed - linked polyacrylic acid , polyvinylalcohol , hyaluronic acid , a cellulosic polymer , for example , hydroxypropyl methyl cellulose , hydroxyethyl cellulose , or methyl cellulose , or a heteropolysaccharide polymer , for example , gelan gum , may be incorporated together with a preservative , such as benzalkonium chloride . such formulations may also be delivered by iontophoresis . formulations for ocular / aural administration may be formulated to be immediate and / or modified release . modified release formulations include delayed -, sustained -, pulsed -, controlled -, targeted , or programmed release . the compounds of the invention ( including n - oxides thereof and pharmaceutically acceptable salts of the foregoing ) may be combined with soluble macromolecular entities , such as cyclodextrin and suitable derivatives thereof or polyethylene glycol - containing polymers , in order to improve their solubility , dissolution rate , taste - masking , bioavailability and / or stability for use in any of the aforementioned modes of administration . drug - cyclodextrin complexes , for example , are found to be generally useful for most dosage forms and administration routes . both inclusion and non - inclusion complexes may be used . as an alternative to direct complexation with the drug , the cyclodextrin may be used as an auxiliary additive , i . e ., as a carrier , diluent , or solubilizer . most commonly used for these purposes are alpha -, beta - and gamma - cyclodextrins , examples of which may be found in international patent applications nos . wo 91 / 11172 , wo 94 / 02518 and wo 98 / 55148 . since the present invention has an aspect that relates to the treatment of the disease / conditions described herein with a combination of active ingredients which may be administered separately , the invention also relates to combining separate pharmaceutical compositions in kit form . the kit comprises two separate pharmaceutical compositions : a compound of formula i a prodrug thereof or a salt of such compound or prodrug and a second compound as described above . the kit comprises means for containing the separate compositions such as a container , a divided bottle or a divided foil packet . typically the kit comprises directions for the administration of the separate components . the kit form is particularly advantageous when the separate components are for example administered in different dosage forms ( e . g ., oral and parenteral ), are administered at different dosage intervals , or when titration of the individual components of the combination is desired by the prescribing physician . an example of such a kit is a so - called blister pack . blister packs are well known in the packaging industry and are being widely used for the packaging of pharmaceutical unit dosage forms ( tablets , capsules , and the like ). blister packs generally consist of a sheet of relatively stiff material covered with a foil of a transparent plastic material . during the packaging process recesses are formed in the plastic foil . the recesses have the size and shape of the tablets or capsules to be packed . next , the tablets or capsules are placed in the recesses and the sheet of relatively stiff material is sealed against the plastic foil at the face of the foil which is opposite from the direction in which the recesses were formed . as a result , the tablets or capsules are sealed in the recesses between the plastic foil and the sheet . in some embodiments , the strength of the sheet is such that the tablets or capsules can be removed from the blister pack by manually applying pressure on the recesses whereby an opening is formed in the sheet at the place of the recess . the tablet or capsule can then be removed via said opening . it may be desirable to provide a memory aid on the kit , e . g ., in the form of numbers next to the tablets or capsules whereby the numbers correspond with the days of the regimen which the tablets or capsules so specified should be ingested . another example of such a memory aid is a calendar printed on the card , e . g ., as follows “ first week , monday , tuesday , etc . . . . second week , monday , tuesday , . . . ” etc . other variations of memory aids will be readily apparent . a “ daily dose ” can be a single tablet or capsule or several pills or capsules to be taken on a given day . also , a daily dose of formula i compound can consist of one tablet or capsule while a daily dose of the second compound can consist of several tablets or capsules and vice versa . the memory aid should reflect this . in another specific embodiment of the invention , a dispenser designed to dispense the daily doses one at a time in the order of their intended use is provided . for example , the dispenser is equipped with a memory aid , so as to further facilitate compliance with the regimen . an example of such a memory aid is a mechanical counter which indicates the number of daily doses that has been dispensed . another example of such a memory aid is a battery - powered micro - chip memory coupled with a liquid crystal readout , or audible reminder signal which , for example , reads out the date that the last daily dose has been taken and / or reminds one when the next dose is to be taken . the invention will be described in greater detail by way of specific examples . the following examples are offered for illustrative purposes , and are not intended to limit the invention in any manner . those of skill in the art will readily recognize a variety of non - critical parameters that can be changed or modified to yield essentially the same results . additional compounds within the scope of this invention may be prepared using the methods illustrated in these examples , either alone or in combination with techniques generally known in the art . in the following examples and preparations , “ dmso ” means dimethyl sulfoxide , “ n ” where referring to concentration means normal , “ m ” means molar , “ ml ” means milliliter , “ mmol ” means millimoles , “ μmol ” means micromoles , “ eq .” means equivalent , “° c .” means degrees celsius , “ mhz ” means megahertz , “ hplc ” means high - performance liquid chromatography . the following illustrate the synthesis of various compounds of the present invention . additional compounds within the scope of this invention may be prepared using the methods illustrated in these examples , either alone or in combination with techniques generally known in the art . experiments were generally carried out under inert atmosphere ( nitrogen or argon ), particularly in cases where oxygen - or moisture - sensitive reagents or intermediates were employed . commercial solvents and reagents were generally used without further purification . anhydrous solvents were employed where appropriate , generally acroseal ® products from acros organics or drisolv ® products from emd chemicals . in other cases , commercial solvents were passed through columns packed with 4 å molecular sieves , until the following qc standards for water were attained : a ) & lt ; 100 ppm for dichloromethane , toluene , n , n - dimethylformamide and tetrahydrofuran ; b ) & lt ; 180 ppm for methanol , ethanol , 1 , 4 - dioxane and diisopropylamine . for very sensitive reactions , solvents were further treated with metallic sodium , calcium hydride or molecular sieves , and distilled just prior to use . products were generally dried under vacuum before being carried on to further reactions or submitted for biological testing . mass spectrometry data is reported from either liquid chromatography - mass spectrometry ( lcms ), atmospheric pressure chemical ionization ( apci ) or gas chromatography - mass spectrometry ( gcms ) instrumentation . chemical shifts for nuclear magnetic resonance ( nmr ) data are expressed in parts per million ( ppm , 6 ) referenced to residual peaks from the deuterated solvents employed . in some examples , chiral separations were carried out to separate enantiomers of certain compounds of the invention ( in some examples , the separated enantiomers are designated as ent - 1 and ent - 2 , according to their order of elution ). in some examples , the optical rotation of an enantiomer was measured using a polarimeter . according to its observed rotation data ( or its specific rotation data ), an enantiomer with a clockwise rotation was designated as the (+)- enantiomer and an enantiomer with a counter - clockwise rotation was designated as the (−)- enantiomer . racemic compounds can optionally be indicated by the presence of (+/−) adjacent to the structure ; in these cases , indicated stereochemistry represents the relative ( rather than absolute ) configuration of the compound &# 39 ; s substituents . reactions proceeding through detectable intermediates were generally followed by lcms , and allowed to proceed to full conversion prior to addition of subsequent reagents . for syntheses referencing procedures in other examples or methods , reaction conditions ( reaction time and temperature ) may vary . in general , reactions were followed by thin - layer chromatography or mass spectrometry , and subjected to work - up when appropriate . purifications may vary between experiments : in general , solvents and the solvent ratios used for eluents / gradients were chosen to provide appropriate r f s or retention times . preparations below describe preparations of p1 - p3 that can be used as starting materials / intermediates for preparation of certain examples of compounds of the invention . trans - 4 - aminotetrahydro - 2h - pyran - 3 - ol ( 30 . 0 g , 256 mmol ) and n - acetyl - d - phenylalanine ( 99 %, 53 . 6 g , 256 mmol ) were suspended in ethanol ( 3 l ), equally divided between two flasks . the mixtures were heated at reflux until they became homogeneous ; at this point the volume in each flask had been reduced to approximately 1 . 3 l . after the solutions had cooled to room temperature , the precipitates were isolated via filtration and washed with ethanol to provide a white solid ( 38 g ). this material was suspended in ethanol ( 900 ml ) and heated at reflux for 30 minutes , during which time the volume was reduced to approximately 800 ml . the mixture was cooled first to room temperature , and then in an ice bath for 30 minutes , whereupon the solid was collected via filtration to provide the product as a white solid . yield : 36 . 0 g , 111 mmol , 43 %. 1 h nmr ( 400 mhz , dmso - d 6 ) δ 7 . 62 ( d , j = 7 . 8 hz , 1h ), 7 . 11 - 7 . 26 ( m , 5h ), 4 . 15 - 4 . 24 ( m , 1h ), 3 . 71 - 3 . 82 ( m , 2h ), 3 . 20 - 3 . 35 ( m , 2h ), 3 . 04 ( dd , j = 13 . 6 , 4 . 8 hz , 1h ), 2 . 93 ( dd , j = 10 . 5 , 10 . 3 hz , 1h ), 2 . 71 - 2 . 86 ( m , 2h ), 1 . 79 - 1 . 87 ( m , 1h ), 1 . 75 ( s , 3h ), 1 . 39 - 1 . 52 ( s , 1h ). another sample of p1 , synthesized in the same manner , was found to have a negative (−) rotation ; upon reaction with benzyl carbonochloridate and sodium bicarbonate , the resulting benzyl [( 3r , 4s )- 3 - hydroxytetrahydro - 2h - pyran - 4 - yl ] carbamate was found to exhibit & gt ; 99 . 5 % purity upon chiral supercritical fluid chromatography analysis ( column : phenomenex lux amylose - 2 , 5 μm ; gradient : 5 % to 60 % methanol in carbon dioxide ). the indicated absolute stereochemistry for p1 was assigned in accordance with that determined by single crystal x - ray analysis of example 9 , as p1 was used in the synthesis of 9 in route 2 of example 9 . the indicated absolute stereochemistry of p1 was assigned also based on an x - ray crystal structure determination ( see below ) carried out on a sample of p1 prepared in the same manner described herein above and recrystallized from acetone / water . data collection was performed on a bruker apex diffractometer at − 150 ° c . data collection consisted of omega and phi scans . the structure was solved by direct methods using shelx software suite in the space group p2 1 . the structure was subsequently refined by the full - matrix least squares method . all non - hydrogen atoms were found and refined using anisotropic displacement parameters . during refinement , residual electron density was noted along an infinite channel along the b axis of the structure . these residuals were modeled as half occupied water molecules . the hydrogen atoms located on nitrogen and oxygen were found from the fourier difference map and refined freely . the remaining hydrogen atoms were placed in calculated positions and were allowed to ride on their carrier atoms . the final refinement included isotropic displacement parameters for all hydrogen atoms . the absolute stereochemistry of the 4 - aminotetrahydro - 2h - pyran - 3 - ol was determined in relation to the known stereocenter of n - acetyl - d - phenylalanine the final r - index was 4 . 9 %. a final difference fourier revealed no missing or misplaced electron density . pertinent crystal , data collection and refinement are summarized in table p1 - 1 . atomic coordinates , bond lengths , bond angles , and displacement parameters are listed in tables p1 - 2 to p1 - 5 . platon , a . l . spek , j . appl . cryst . 2003 , 36 , 7 - 13 . mercury , c . f . macrae , p . r . edington , p . mccabe , e . pidcock , g . p . shields , r . taylor , m . towler , and j . van de streek , j . appl . cryst . 2006 , 39 , 453 - 457 . olex2 , o . v . dolomanov , l . j . bourhis , r . j . gildea , j . a . k . howard , and h . puschmann , j . appl . cryst . 2009 , 42 , 339 - 341 . parameters ( å 2 × 10 3 ) for p1 . u ( eq ) is defined as one third anisotropic displacement parameters ( å 2 × 10 3 ) for p1 . form : − 2π 2 [ h 2 a * 2 u 11 + . . . + 2 h k a * b * u 12 ]. compound p1 ( 3 . 00 g , 9 . 25 mmol ) was suspended in a mixture of dichloromethane and methanol ( 1 : 1 , 80 ml ), and treated with amberlyst ® a26 ( oh ) resin ( 15 g ). the resulting mixture was stirred at room temperature overnight , whereupon it was filtered , and the collected resin was thoroughly washed with dichloromethane . the filtrate was concentrated in vacuo , affording the product as a light yellow solid . the product exhibited a positive (+) rotation . yield : 1 . 00 g , 8 . 54 mmol , 92 %. 1 h nmr ( 400 mhz , cd 3 od ) δ 3 . 82 - 3 . 90 ( m , 2h ), 3 . 38 ( ddd , j = 12 . 0 , 11 . 9 , 2 . 2 hz , 1h ), 3 . 23 ( ddd , j = 10 . 0 , 9 . 1 , 4 . 8 hz , 1h ), 3 . 03 ( dd , j = 11 . 0 , 10 . 1 hz , 1h ), 2 . 61 ( ddd , j = 11 . 4 , 9 . 0 , 4 . 6 hz , 1h ), 1 . 80 - 1 . 87 ( m , 1h ), 1 . 46 ( dddd , j = 13 . 4 , 12 . 2 , 11 . 5 , 4 . 7 hz , 1h ). a mixture of ( 1s , 2s )- 2 - aminocyclohexanol ( 500 mg , 4 . 34 mmol ), p - toluenesulfonic acid monohydrate ( 82 . 6 mg , 0 . 434 mmol ), magnesium sulfate ( 1 . 4 g , 12 mmol ), and benzophenone ( 775 mg , 4 . 25 mmol ) in toluene ( 20 ml ) was stirred at 110 ° c . for 42 hours . the reaction mixture was concentrated in vacuo ; silica gel chromatography ( gradient : 0 % to 90 % ethyl acetate in petroleum ether ) afforded the product as a colorless oil . yield : 344 mg , 1 . 23 mmol , 29 %. iodomethane ( 175 mg , 1 . 23 mmol ) was added to a 0 ° c . solution of c46 ( 344 mg , 1 . 23 mmol ) and sodium hydride ( 60 % in oil , 59 . 1 mg , 1 . 48 mmol ) in tetrahydrofuran ( 20 ml ), and the reaction mixture was stirred at room temperature overnight . the reaction was quenched by addition of water ( 10 ml ), and the resulting mixture was concentrated in vacuo . silica gel chromatography ( gradient : 0 % to 7 % ethyl acetate in petroleum ether ) provided the product as a colorless oil . yield : 184 mg , 0 . 627 mmol , 51 %. 1 h nmr ( 400 mhz , cdcl 3 ) δ 7 . 61 ( br d , j = 7 hz , 2h ), 7 . 29 - 7 . 48 ( m , 6h ), 7 . 19 - 7 . 25 ( m , 2h ), 3 . 38 ( s , 3h ), 3 . 33 - 3 . 42 ( m , 1h ), 3 . 23 - 3 . 32 ( m , 1h ), 2 . 03 - 2 . 12 ( m , 1h ), 1 . 52 - 1 . 76 ( m , 4h ), 1 . 25 - 1 . 39 ( m , 1h ), 1 . 03 - 1 . 17 ( m , 2h ). a mixture of c47 ( 200 mg , 0 . 682 mmol ), 1 m hydrochloric acid ( 20 ml ), and tetrahydrofuran ( 20 ml ) was stirred at room temperature overnight . solvent was removed in vacuo , the residue was partitioned between ethyl acetate ( 15 ml ) and water ( 15 ml ), and the aqueous layer was washed with ethyl acetate ( 2 × 20 ml ). the aqueous layer was then concentrated under reduced pressure to afford the product as a white solid . yield : 130 mg , quantitative . 1 h nmr ( 400 mhz , cd 3 od ) δ 3 . 40 ( s , 3h ), 3 . 12 ( ddd , j = 10 . 4 , 10 . 3 , 4 . 4 hz , 1h ), 2 . 87 - 2 . 98 ( m , 1h ), 2 . 27 - 2 . 36 ( m , 1h ), 2 . 01 - 2 . 09 ( m , 1h ), 1 . 75 - 1 . 87 ( m , 2h ), 1 . 24 - 1 . 48 ( m , 3h ), 1 . 07 - 1 . 19 ( m , 1h ). n - bromosuccinimide ( 468 mg , 2 . 63 mmol ) was added portion - wise to a 50 ° c . solution of methyl 5 - aminopyridine - 2 - carboxylate ( 400 mg , 2 . 6 mmol ) in acetonitrile ( 15 ml ), and the reaction mixture was heated at 50 ° c . overnight . crude reaction mixtures from six additional small - scale reactions of this transformation were added ( total starting material quantity : 760 mg , 5 . 0 mmol ), and the resulting mixture was concentrated in vacuo , then purified via silica gel chromatography ( gradient : 2 % to 66 % ethyl acetate in petroleum ether ), providing the product as a red solid . yield : 150 mg , 0 . 65 mmol , 13 %. 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 23 ( s , 1h ), 8 . 16 ( s , 1h ), 4 . 61 ( br s , 2h ), 3 . 97 ( s , 3h ). a mixture of c1 ( 135 mg , 0 . 584 mmol ), 4 , 4 , 4 ′, 4 ′, 5 , 5 , 5 ′, 5 ′- octamethyl - 2 , 2 ′- bi - 1 , 3 , 2 - dioxaborolane ( 223 mg , 0 . 878 mmol ), [ 1 , 1 ′- bis ( diphenylphosphino ) ferrocene ] dichloropalladium ( ii ) ( 64 . 1 mg , 87 . 6 μmol ), and potassium acetate ( 206 mg , 2 . 10 mmol ) in toluene ( 10 ml ) was stirred at 100 ° c . for 20 hours . the reaction mixture was allowed to cool , and used in the next step without purification . to the crude toluene solution of c2 from the previous step were added 1 -[ 4 -( bromomethyl ) phenyl ]- 1h - pyrazole ( 155 mg , 0 . 654 mmol ), [ 1 , 1 ′- bis ( diphenylphosphino ) ferrocene ] dichloropalladium ( ii ) ( 44 . 9 mg , 61 . 4 μmol ), potassium carbonate ( 113 mg , 0 . 818 mmol ), 1 , 4 - dioxane ( 10 ml ), and water ( 0 . 5 ml ). the reaction mixture was stirred at 80 ° c . for 18 hours , whereupon it was filtered through a pad of diatomaceous earth . the filtrate was concentrated in vacuo ; silica gel chromatography ( gradient : 20 % to 100 % ethyl acetate in petroleum ether ) afforded the product as a yellow solid . yield : 120 mg , 0 . 39 mmol , 67 % over two steps . 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 12 ( s , 1h ), 7 . 89 - 7 . 93 ( m , 2h ), 7 . 73 ( d , j = 1 . 4 hz , 1h ), 7 . 66 ( br d , j = 8 . 5 hz , 2h ), 7 . 24 - 7 . 28 ( m , 2h , assumed ; partially obscured by solvent peak ), 6 . 48 ( dd , j = 2 . 4 , 1 . 9 hz , 1h ), 4 . 02 ( br s , 2h ), 3 . 95 - 3 . 98 ( m , 5h ). to a solution of c3 ( 160 mg , 0 . 519 mmol ) and copper ( ii ) chloride dihydrate ( 133 mg , 0 . 780 mmol ) in acetonitrile ( 5 ml ) was added tert - butyl nitrite ( 107 mg , 1 . 04 mmol ). after the reaction mixture had been stirred at room temperature for 15 minutes , it was heated at 50 ° c . for 4 hours . the reaction mixture was filtered , and the filtrate was concentrated in vacuo ; the residue was partitioned between aqueous ammonium hydroxide ( 50 ml ) and ethyl acetate ( 50 ml ), and the aqueous layer was extracted with ethyl acetate ( 2 × 50 ml ). the combined organic layers were dried over sodium sulfate , filtered , and concentrated under reduced pressure . purification via preparative thin layer chromatography on silica gel ( eluent : 1 : 1 petroleum ether / ethyl acetate ) provided the product as a yellow solid . yield : 50 mg , 0 . 15 mmol , 29 %. lcms m / z 327 . 8 [ m + h ] + . 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 69 ( s , 1h ), 7 . 89 - 7 . 98 ( m , 2h ), 7 . 73 ( s , 1h ), 7 . 67 ( br d , j = 8 . 5 hz , 2h ), 7 . 29 ( br d , j = 8 . 5 hz , 2h ), 6 . 46 - 6 . 50 ( m , 1h ), 4 . 18 ( s , 2h ), 3 . 99 ( s , 3h ). a solution of c4 ( 25 mg , 76 μmol ) in 1 , 4 - dioxane ( 2 ml ) was added to a solution of sodium hydroxide ( 6 . 1 mg , 0 . 15 mmol ) in water ( 2 ml ), and the reaction mixture was stirred at room temperature for 30 minutes . it was then adjusted to a ph of 4 - 5 via addition of a mixture of concentrated hydrochloric acid ( 2 ml ) and water ( 2 ml ). removal of solvent under reduced pressure afforded the product as a yellow gum , which was employed in the next step without additional purification . lcms m / z 313 . 8 [ m + h ] + . a solution of c5 ( from the previous step , 20 mg , 64 μmol ), ( 3r , 4s )- 4 - aminotetrahydro - 2h - pyran - 3 - ol , n - acetyl - d - phenylalanine salt ( p1 ) ( 41 . 4 mg , 0 . 128 mmol ), triethylamine ( 32 . 3 mg , 0 . 319 mmol ), and o -( 7 - azabenzotriazol - 1 - yl )- n , n , n ′, n ′- tetramethyluronium hexafluorophosphate ( hatu , 72 . 7 mg , 0 . 191 mmol ) in acetonitrile ( 3 ml ) was stirred at 25 ° c . for 4 hours . the reaction mixture was concentrated in vacuo , and the residue was purified by reversed phase hplc ( column : phenomenex gemini c18 , 8 μm ; mobile phase a : aqueous ammonia , ph 10 ; mobile phase b : acetonitrile ; gradient : 36 % to 56 % b ) to afford the product as a white solid . yield : 4 . 0 mg , 9 . 7 μmol , 13 % over two steps . lcms m / z 434 . 9 [ m + n + ]. 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 50 ( s , 1h ), 8 . 05 ( s , 1h ), 7 . 97 - 8 . 03 ( m , 1h ), 7 . 91 ( d , j = 2 . 4 hz , 1h ), 7 . 72 ( br d , j = 1 hz , 1h ), 7 . 65 ( br d , j = 8 . 5 hz , 2h ), 7 . 29 ( br d , j = 8 . 5 hz , 2h ), 6 . 45 - 6 . 49 ( m 1h ), 4 . 19 ( s , 2h ), 3 . 89 - 4 . 12 ( m , 4h ), 3 . 58 - 3 . 67 ( m , 1h ), 3 . 42 - 3 . 52 ( m , 1h ), 3 . 22 ( dd , j = 11 . 3 , 10 . 0 hz , 1h ), 2 . 00 - 2 . 07 ( m , 1h ), 1 . 72 - 1 . 85 ( m , 1h ). 4 - bromo - 1 - methyl - 1h - pyrazole ( 11 . 5 g , 71 . 4 mmol ), [ 1 , 1 ′- bis ( diphenylphosphino ) ferrocene ] dichloropalladium ( ii ) ( 1 . 96 g , 2 . 68 mmol ), and cesium carbonate ( 31 . 3 g , 96 . 1 mmol ) were added to a solution of [ 3 - fluoro - 4 -( methoxycarbonyl ) phenyl ] boronic acid ( 9 . 5 g , 48 mmol ) in 1 , 4 - dioxane ( 200 ml ) and water ( 20 ml ). the reaction mixture was stirred for 3 hours at reflux , whereupon it was filtered . the filtrate was concentrated in vacuo ; silica gel chromatography ( gradient : 0 % to 45 % ethyl acetate in petroleum ether ) afforded the product as an off - white solid . yield : 6 . 7 g , 29 mmol , 60 %. 1 h nmr ( 400 mhz , cdcl 3 ) δ 7 . 93 ( dd , j = 8 . 0 , 7 . 9 hz , 1h ), 7 . 80 ( s , 1h ), 7 . 69 ( s , 1h ), 7 . 29 ( dd , j = 8 . 2 , 1 . 6 hz , 1h ), 7 . 21 ( dd , j = 12 . 1 , 1 . 6 hz , 1h ), 3 . 97 ( s , 3h ), 3 . 93 ( s , 3h ). lithium aluminum hydride ( 2 . 72 g , 71 . 7 mmol ) was added portion - wise to a − 78 ° c . solution of c6 ( 6 . 7 g , 29 mmol ) in tetrahydrofuran ( 400 ml ). the reaction mixture was allowed to stir for 1 hour at − 78 ° c ., then for 3 hours in an ice - ethanol cooling bath . while still under ice - ethanol cooling , the reaction was quenched via drop - wise addition of water ( 3 ml ) and aqueous sodium hydroxide solution ( 15 %, 3 ml ). the resulting mixture was filtered , the filtrate was concentrated in vacuo , and the residue was purified by silica gel chromatography ( gradient : 0 % to 100 % ethyl acetate in petroleum ether ) to provide the product as a white solid . yield : 4 . 0 g , 19 mmol , 66 %. 1 h nmr ( 400 mhz , cd 3 od ) δ 7 . 97 ( s , 1h ), 7 . 82 ( s , 1h ), 7 . 42 ( dd , j = 7 . 9 , 7 . 8 hz , 1h ), 7 . 35 ( dd , j = 7 . 8 , 1 . 2 hz , 1h ), 7 . 26 ( dd , j = 11 . 5 , 1 . 2 hz , 1h ), 4 . 64 ( s , 2h ), 3 . 91 ( s , 3h ). a solution of thionyl chloride ( 1 . 58 g , 13 . 3 mmol ) in toluene ( 25 ml ) was added drop - wise to a water bath - cooled solution of c7 ( 2 . 5 g , 12 mmol ) in chloroform ( 53 ml ) and toluene ( 50 ml ). the reaction mixture , still in the water bath , was stirred overnight , then concentrated in vacuo , affording the product as a white solid . yield : 2 . 9 g , 11 mmol , 92 %. 1 h nmr ( 400 mhz , cd 3 od ) δ 8 . 40 ( br s , 1h ), 8 . 34 ( br s , 1h ), 7 . 40 - 7 . 53 ( m , 3h ), 4 . 69 ( s , 2h ), 4 . 08 ( s , 3h ). a mixture of 2 , 4 - dichloro - 5 - methylpyridine ( 33 g , 0 . 20 mol ), [ 1 , 1 ′- bis ( diphenylphosphino ) ferrocene ] dichloropalladium ( ii ) ( 7 . 45 g , 10 . 2 mmol ), and triethylamine ( 61 . 8 g , 611 mmol ) in ethanol ( 500 ml ) was stirred under carbon monoxide ( 30 psi ) at 60 ° c . for 4 hours . the reaction mixture was filtered , the filtrate was concentrated under reduced pressure , and the residue was purified by silica gel chromatography ( gradient : 10 % to 50 % ethyl acetate in petroleum ether ), providing the product as a yellow oil . yield : 25 . 0 g , 0 . 125 mol , 62 %. 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 56 ( s , 1h ), 8 . 11 ( s , 1h ), 4 . 48 ( q , j = 7 . 1 hz , 2h ), 2 . 44 ( s , 3h ), 1 . 44 ( t , j = 7 . 1 hz , 3h ). a mixture of c9 ( 16 g , 80 mmol ), 4 , 4 , 4 ′, 4 ′, 5 , 5 , 5 ′, 5 ′- octamethyl - 2 , 2 ′- bi - 1 , 3 , 2 - dioxaborolane ( 30 . 5 g , 120 mmol ), [ 1 , 1 ′- bis ( diphenylphosphino ) ferrocene ] dichloropalladium ( ii ) ( 5 . 86 g , 8 . 01 mmol ), and potassium acetate ( 28 . 3 g , 288 mmol ) in toluene ( 1 . 2 l ) was stirred at 130 ° c . for 20 hours . after filtration of the reaction mixture , the filtrate was concentrated under reduced pressure . the residue was purified by chromatography on silica gel ( gradient : 10 % to 50 % ethyl acetate in petroleum ether ) to provide a yellow solid ( 20 g ), which was diluted with petroleum ether ( 50 ml ) and stirred at room temperature for 20 minutes . the solid was collected via filtration to afford the product ( 8 . 8 g ) as a white solid . the corresponding filtrate was concentrated in vacuo and the residue was purified by silica gel chromatography ( gradient : 0 % to 30 % ethyl acetate in petroleum ether ); the isolated material ( 4 . 5 g ) was washed with petroleum ether ( 5 ml ) to yield additional product ( 3 . 5 g ) as a white solid . combined yield : 12 . 3 g , 42 . 2 mmol , 53 %. 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 57 ( s , 1h ), 8 . 39 ( s , 1h ), 4 . 48 ( q , j = 7 . 2 hz , 2h ), 2 . 57 ( s , 3h ), 1 . 45 ( t , j = 7 . 2 hz , 3h ), 1 . 37 ( s , 12h ). to a mixture of c10 ( 50 mg , 0 . 17 mmol ), c8 ( 49 . 3 mg , 0 . 189 mmol ), and sodium hydroxide ( 34 . 3 mg , 0 . 858 mmol ) in a mixture of acetonitrile ( 5 ml ) and water ( 0 . 2 ml ) was added tetrakis ( triphenylphosphine ) palladium ( 0 ) ( 19 . 8 mg , 17 . 1 μmol ), and the reaction mixture was stirred at 80 ° c . for 4 hours . it was then concentrated in vacuo and diluted with water ( 10 ml ). the resulting mixture was acidified to ph 1 with hydrochloric acid and filtered ; the filtrate was concentrated under reduced pressure to afford the product as a yellow solid ( 40 mg ), which was used in the following step without additional purification . o -( 7 - azabenzotriazol - 1 - yl )- n , n , n ′, n ′- tetramethyluronium hexafluorophosphate ( 46 . 7 mg , 0 . 123 mmol ) was added to a mixture of c11 ( 40 mg , ≦ 0 . 12 mmol ), p1 ( 87 . 7 mg , 0 . 270 mmol ), and triethylamine ( 74 . 6 mg , 0 . 737 mmol ) in dichloromethane ( 4 ml ). the reaction mixture was stirred at 25 ° c . for 20 hours , whereupon it was treated with additional p1 ( 40 mg , 0 . 12 mmol ), and stirring was continued for 20 hours . the reaction mixture was concentrated in vacuo ; preparative thin layer chromatography on silica gel ( eluent : 10 : 1 dichloromethane / methanol ) provided the product as a white solid . yield : 17 mg , 40 μmol , 24 % over two steps . lcms m / z 425 . 0 [ m + h ] + . 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 33 ( s , 1h ), 8 . 11 ( br d , j = 6 hz , 1h ), 7 . 94 ( s , 1h ), 7 . 73 ( s , 1h ), 7 . 60 ( s , 1h ), 7 . 14 - 7 . 19 ( m , 2h ), 6 . 99 ( dd , j = 8 , 8 hz , 1h ), 4 . 40 ( d , j = 3 . 3 hz , 1h ), 4 . 09 ( dd , j = 11 . 4 , 5 . 1 hz , 1h ), 4 . 02 ( s , 2h ), 3 . 95 ( s , 3h ), 3 . 88 - 4 . 0 ( m , 2h ), 3 . 59 - 3 . 67 ( m , 1h ), 3 . 47 ( ddd , j = 12 , 12 , 2 hz , 1h ), 3 . 22 ( dd , j = 11 . 3 , 10 . 0 hz , 1h ), 2 . 37 ( s , 3h ), 1 . 99 - 2 . 07 ( m , 1h ), 1 . 74 - 1 . 86 ( m , 1h ). phosphorus tribromide ( 11 . 3 g , 41 . 7 mmol ) was added drop - wise to a 0 ° c . solution of 2 -[ 4 -( hydroxymethyl ) phenyl ]- 6 - methyl - 1 , 3 , 6 , 2 - dioxazaborocane - 4 , 8 - dione ( 10 g , 38 mmol ) in dichloromethane ( 150 ml ) and acetonitrile ( 150 ml ). the reaction mixture was stirred overnight at room temperature , whereupon it was quenched via addition of saturated aqueous sodium bicarbonate solution . the aqueous layer was extracted with dichloromethane ( 3 × 200 ml ), and the combined organic layers were dried , filtered , and concentrated in vacuo . the residue was washed with tert - butyl methyl ether ( 2 × 200 ml ) to afford the product as a white solid . yield : 10 . 7 g , 32 . 8 mmol , 86 %. lcms m / z 327 . 8 [ m + h ] + . 1 h nmr ( 400 mhz , cd 3 od ) δ 7 . 47 ( ab quartet , j ab = 8 . 2 hz , □ ab = 24 . 1 hz , 4h ), 4 . 57 ( s , 2h ), 4 . 26 ( d , j = 17 . 1 hz , 2h ), 4 . 06 ( d , j = 17 . 1 hz , 2h ), 2 . 57 ( s , 3h ). to a solution of c10 ( 2 . 0 g , 6 . 9 mmol ) and c12 ( 2 . 69 g , 8 . 25 mmol ) in acetonitrile ( 100 ml ) were added tetrakis ( triphenylphosphine ) palladium ( 0 ) ( 397 mg , 0 . 344 mmol ) and potassium fluoride ( 2 . 0 g , 34 mmol ). the reaction mixture was stirred for 4 hours at 80 ° c ., whereupon it was diluted with water ( 400 ml ) and extracted with ethyl acetate ( 3 × 200 ml ). the combined organic layers were concentrated in vacuo and the residue was purified by chromatography on silica gel ( gradient : 0 % to 5 % methanol in dichloromethane ) to provide the product as a yellow solid . yield : 1 . 2 g , 2 . 9 mmol , 42 %. lcms m / z 410 . 9 [ m + h ] + . 1 h nmr ( 400 mhz , cd 3 od ) δ 8 . 43 ( s , 1h ), 7 . 86 ( s , 1h ), 7 . 48 ( d , j = 7 . 8 hz , 2h ), 7 . 20 ( d , j = 7 . 8 hz , 2h ), 4 . 39 ( q , j = 7 . 1 hz , 2h ), 4 . 25 ( d , j = 17 . 1 hz , 2h ), 4 . 13 ( s , 2h ), 4 . 05 ( d , j = 17 . 1 hz , 2h ), 2 . 56 ( s , 3h ), 2 . 36 ( s , 3h ), 1 . 38 ( t , j = 7 . 2 hz , 3h ). 2 - bromo - 1 , 3 - thiazole ( 90 mg , 0 . 55 mmol ), tetrakis ( triphenylphosphine ) palladium ( 0 ) ( 423 mg , 0 . 366 mmol ), and cesium carbonate ( 238 mg , 0 . 730 mmol ) were added to a solution of c13 ( 150 mg , 0 . 37 mmol ) in 1 , 4 - dioxane ( 3 ml ) and water ( 0 . 3 ml ). the reaction mixture was stirred overnight at 80 ° c ., and then filtered . the filtrate was concentrated under reduced pressure ; silica gel chromatography ( gradient : 0 % to 3 % methanol in dichloromethane ) afforded the product as a yellow gum . yield : 50 mg , 0 . 15 mmol , 40 %. 1 , 3 , 4 , 6 , 7 , 8 - hexahydro - 2h - pyrimido [ 1 , 2 - a ] pyrimidine ( 95 %, 350 mg , 2 . 39 mmol ) was added to a solution of c14 ( 476 mg , 1 . 41 mmol ) and p1 ( 456 mg , 1 . 41 mmol ) in n , n - dimethylformamide ( 2 . 8 ml ), and the reaction mixture was heated at 60 ° c . overnight . it was then cooled and partitioned between water and ethyl acetate . the aqueous layer was extracted with ethyl acetate , and the combined organic layers were washed with saturated aqueous sodium chloride solution , dried over magnesium sulfate , filtered , and concentrated in vacuo . silica gel chromatography ( gradient : 50 % to 100 % ethyl acetate in heptane ) afforded a yellow solid ( 497 mg ). this was combined with the product ( 148 mg ) of a similar reaction carried out on c14 ( 278 mg , 0 . 821 mmol ), and the combined material was heated in a slurry with ethyl acetate . a small amount of heptane was added , and the suspension was allowed to stir and cool to room temperature over 3 hours . the resulting solid was collected via filtration to provide the product as a white powder . yield : 300 mg , 0 . 73 mmol , 33 %. lcms m / z 410 . 1 [ m + h ] + . 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 33 ( s , 1h ), 8 . 13 ( br d , j = 6 hz , 1h ), 8 . 02 ( s , 1h ), 7 . 90 ( br d , j = 8 . 1 hz , 2h ), 7 . 86 ( d , j = 3 . 3 hz , 1h ), 7 . 33 ( d , j = 3 . 2 hz , 1h ), 7 . 19 ( br d , j = 8 . 0 hz , 2h ), 4 . 35 ( br s , 1h ), 4 . 06 - 4 . 13 ( m , 3h ), 3 . 91 - 4 . 04 ( m , 2h ), 3 . 65 ( ddd , j = 9 . 5 , 9 . 5 , 5 hz , 1h ), 3 . 48 ( ddd , j = 12 , 12 , 2 hz , 1h ), 3 . 23 ( dd , j = 11 , 10 hz , 1h ), 2 . 32 ( s , 3h ), 2 . 01 - 2 . 08 ( m , 1h ), 1 . 75 - 1 . 87 ( m , 1h ). to a solution of c13 ( 120 mg , 0 . 29 mmol ) in 1 , 4 - dioxane ( 3 ml ) and water ( 0 . 3 ml ) were added 5 - bromo - 1 , 3 - thiazole ( 72 mg , 0 . 44 mmol ), [ 1 , 1 ′- bis ( diphenylphosphino ) ferrocene ] dichloropalladium ( ii ) ( 214 mg , 0 . 292 mmol ), and potassium carbonate ( 80 . 9 mg , 0 . 585 mmol ). the reaction mixture was stirred overnight at 110 ° c ., whereupon it was filtered . the filtrate was concentrated under reduced pressure , and the residue was purified by silica gel chromatography ( gradient : 0 % to 3 % methanol in dichloromethane ) to afford the product as a yellow gum . yield : 50 mg , 0 . 15 mmol , 52 %. to a solution of c15 ( 50 mg , 0 . 15 mmol ) in methanol ( 2 ml ) and water ( 2 ml ) was added sodium hydroxide ( 29 . 5 mg , 0 . 738 mmol ), and the reaction mixture was stirred for 4 hours at reflux . it was then acidified via addition of 1 m hydrochloric acid and concentrated in vacuo to provide the product , which was used in the next step without additional purification to a solution of c16 ( from the previous step , 46 mg , 0 . 15 mmol ) in dichloromethane ( 5 ml ) were added o -( 7 - azabenzotriazol - 1 - yl )- n , n , n ′, n ′- tetramethyluronium hexafluorophosphate ( 56 . 4 mg , 0 . 148 mmol ), trans - 4 - aminotetrahydro - 2h - pyran - 3 - ol ( 34 . 7 mg , 0 . 296 mmol ), and triethylamine ( 45 . 0 mg , 0 . 445 mmol ), and the reaction mixture was stirred overnight at room temperature . the reaction mixture was concentrated in vacuo and the residue was purified by preparative thin layer chromatography on silica gel ( gradient : 20 : 1 dichloromethane / methanol ) to provide the racemate of the products as a yellow gum . yield : 35 mg , 85 μmol , 57 % over two steps . this material was separated into its component enantiomers via reversed phase hplc ( column : chiral technologies chiralpak ad , 10 μm ; mobile phase : 55 % ethanol in aqueous ammonia ) to provide 4 and 5 , both as white solids ( examples 4 and 5 are designated according to their respective retention time shown below ). 4 : yield : 10 . 4 mg , 25 . 4 μmol , 30 % for the chiral separation . lcms m / z 409 . 9 [ m + h ] + . 1 h nmr ( 400 mhz , cd 3 od ) δ 8 . 95 ( s , 1h ), 8 . 42 ( s , 1h ), 8 . 15 ( s , 1h ), 7 . 85 ( s , 1h ), 7 . 62 ( d , j = 8 . 2 hz , 2h ), 7 . 26 ( d , j = 8 . 2 hz , 2h ), 4 . 14 ( s , 2h ), 3 . 87 - 4 . 00 ( m , 3h ), 3 . 59 - 3 . 69 ( m , 1h ), 3 . 47 ( ddd , j = 12 . 0 , 11 . 8 , 2 . 2 hz , 1h ), 3 . 19 ( dd , j = 10 . 9 , 10 . 0 hz , 1h ), 2 . 36 ( s , 3h ), 1 . 97 - 2 . 05 ( m , 1h ), 1 . 64 - 1 . 76 ( m , 1h ). retention time : 1 . 23 minutes ( column : chiral technologies chiralpak ad - 3 , 4 . 6 × 50 mm , 3 μm ; mobile phase : 3 : 2 [ ethanol , containing 0 . 05 % diethylamine ]/ carbon dioxide ; flow rate : 3 ml / minute ). 5 : yield : 6 . 8 mg , 17 μmol , 20 % for the chiral separation . lcms m / z 409 . 9 [ m + h ] + . 1 h nmr ( 400 mhz , cd 3 od ) δ 8 . 94 ( s , 1h ), 8 . 41 ( br s , 1h ), 8 . 15 ( s , 1h ), 7 . 85 ( br s , 1h ), 7 . 61 ( d , j = 8 . 0 hz , 2h ), 7 . 25 ( d , j = 8 . 0 hz , 2h ), 4 . 13 ( s , 2h ), 3 . 86 - 4 . 00 ( m , 3h ), 3 . 59 - 3 . 69 ( m , 1h ), 3 . 43 - 3 . 51 ( m , 1h ), 3 . 19 ( dd , j = 10 . 5 , 10 . 5 hz , 1h ), 2 . 35 ( s , 3h ), 1 . 96 - 2 . 05 ( m , 1h ), 1 . 63 - 1 . 77 ( m , 1h ). retention time : 2 . 21 minutes ( column : chiral technologies chiralpak ad - 3 , 4 . 6 × 50 mm , 3 μm ; mobile phase : 3 : 2 [ ethanol , containing 0 . 05 % diethylamine ]/ carbon dioxide ; flow rate : 3 ml / minute ). [ 1 , 1 ′- bis ( diphenylphosphino ) ferrocene ] dichloropalladium ( ii ) ( 10 . 7 mg , 14 . 6 μmol ) was added to a mixture of c13 ( 60 mg , 0 . 15 mmol ), 3 - bromo - 1 - methyl - 1h - pyrazole ( 28 . 3 mg , 0 . 176 mmol ), and potassium carbonate ( 60 . 6 mg , 0 . 438 mmol ) in toluene ( 5 ml ) and water ( 0 . 2 ml ), and the reaction mixture was stirred at 100 ° c . overnight . after removal of solvents in vacuo , the residue was purified by preparative thin layer chromatography on silica gel ( eluent : 20 : 1 dichloromethane / methanol ) to give the crude product as a brown solid ( 50 mg ); this was used in the next step without additional purification . compound c17 ( from the previous step , 50 mg , 0 . 15 mmol ) and sodium hydroxide ( 23 . 9 mg , 0 . 598 mmol ) were combined in a mixture of methanol ( 2 ml ) and water ( 2 ml ), and stirred overnight at 80 ° c . the reaction mixture was then concentrated in vacuo to remove methanol , and acidified to a ph of 1 with hydrochloric acid . after removal of solvent under reduced pressure , the residue ( 60 mg ) was used directly in the following step . to a solution of c18 ( from the previous step , 60 mg , 0 . 15 mmol ), p1 ( 83 . 6 mg , 0 . 258 mmol ) and triethylamine ( 59 . 3 mg , 0 . 586 mmol ) in dichloromethane ( 5 ml ) was added o -( 7 - azabenzotriazol - 1 - yl )- n , n , n ′, n ′- tetramethyluronium hexafluorophosphate ( 44 . 5 mg , 0 . 117 mmol ). the reaction mixture was stirred at 25 ° c . overnight , then at 40 ° c . for 3 hours , whereupon it was concentrated in vacuo . preparative thin layer chromatography on silica gel ( eluent : 10 : 1 dichloromethane / methanol ) provided the product as a white solid . yield : 5 . 1 mg , 13 μmol , 9 % over three steps . lcms m / z 406 . 9 [ m + h ] + . 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 31 ( s , 1h ), 8 . 08 - 8 . 15 ( m , 1h ), 8 . 02 ( s , 1h ), 7 . 71 ( d , j = 7 . 9 hz , 2h ), 7 . 37 ( d , j = 2 . 0 hz , 1h ), 7 . 13 ( d , j = 8 . 0 hz , 2h ), 6 . 50 ( d , j = 2 . 1 hz , 1h ), 4 . 41 ( br s , 1h ), 4 . 05 ( s , 2h ), 3 . 95 ( s , 3h ), 3 . 90 - 4 . 13 ( m , 3h ), 3 . 60 - 3 . 69 ( m , 1h ), 3 . 43 - 3 . 52 ( m , 1h ), 3 . 19 - 3 . 27 ( m , 1h ), 2 . 30 ( s , 3h ), 2 . 00 - 2 . 08 ( m , 1h ), 1 . 74 - 1 . 86 ( m , 1h ). aqueous potassium carbonate solution ( 3 . 0 m , 17 ml , 51 mmol ) was added to a solution of [ 4 -( hydroxymethyl ) phenyl ] boronic acid ( 96 %, 4 . 0 g , 25 mmol ) and 4 - bromo - 1 , 3 - thiazole ( 96 %, 6 . 48 g , 37 . 9 mmol ) in 1 , 4 - dioxane ( 75 ml ). tetrakis ( triphenylphosphine ) palladium ( 0 ) ( 885 mg , 0 . 766 mmol ) was added , and the reaction mixture was heated at 100 ° c . overnight . after cooling to room temperature , the reaction mixture was diluted with water and extracted several times with ethyl acetate . the combined organic layers were washed with saturated aqueous sodium chloride solution , dried over magnesium sulfate , filtered , and concentrated in vacuo ; silica gel chromatography ( gradient : 25 % to 50 % ethyl acetate in heptane ) provided the product as a cream - colored solid . yield : 3 . 60 g , 18 . 8 mmol , 75 %. lcms m / z 192 . 0 [ m + h ] + . 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 92 ( d , j = 2 . 0 hz , 1h ), 7 . 95 ( br d , j = 8 . 2 hz , 2h ), 7 . 56 ( d , j = 2 . 0 hz , 1h ), 7 . 46 ( br d , j = 8 . 3 hz , 2h ), 4 . 76 ( s , 2h ). compound c19 ( 600 mg , 3 . 14 mmol ) was dissolved in a mixture of dichloromethane ( 5 ml ) and acetonitrile ( 5 ml ), then treated in a drop - wise manner with phosphorus tribromide ( 99 %, 0 . 298 ml , 3 . 14 mmol ). the reaction mixture was allowed to stir at room temperature overnight , whereupon it was quenched with saturated aqueous sodium bicarbonate solution and extracted several times with ethyl acetate . the combined organic layers were washed with saturated aqueous sodium chloride solution , dried over magnesium sulfate , filtered , and concentrated in vacuo . silica gel chromatography ( gradient : 10 % to 25 % ethyl acetate in heptane ) afforded the product as a white solid . yield : 525 mg , 2 . 07 mmol , 66 %. lcms m / z 254 . 0 , 256 . 0 [ m + h ] + . 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 91 ( d , j = 2 . 0 hz , 1h ), 7 . 93 ( br d , j = 8 . 4 hz , 2h ), 7 . 58 ( d , j = 2 . 0 hz , 1h ), 7 . 48 ( br d , j = 8 . 5 hz , 2h ), 4 . 55 ( s , 2h ). aqueous cesium carbonate solution ( 3 m , 5 . 0 ml , 15 mmol ) was added to a solution of c20 ( 1 . 27 g , 5 . 00 mmol ) and c10 ( 1 . 5 g , 5 . 2 mmol ) in tetrahydrofuran ( 28 ml ), and the resulting solution was sparged with nitrogen gas for 50 minutes . after addition of bis ( tri - tert - butylphosphine ) palladium ( 0 ) ( 99 %, 516 mg , 0 . 999 mmol ), the reaction mixture was heated at 40 ° c . overnight . it was then allowed to cool to room temperature , and was partitioned between water and ethyl acetate . the aqueous layer was extracted with 30 ml portions of ethyl acetate , and the combined organic layers were washed with saturated aqueous sodium chloride solution , dried over magnesium sulfate , filtered , and concentrated in vacuo . silica gel chromatography ( gradient : 20 % to 80 % ethyl acetate in heptane ) provided the product as a white solid . yield : 872 mg , 2 . 58 mmol , 52 %. lcms m / z 339 . 0 [ m + h ] + . 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 86 ( d , j = 2 . 0 hz , 1h ), 8 . 50 - 8 . 52 ( m , 1h ), 7 . 92 ( s , 1h ), 7 . 86 ( br d , j = 7 . 8 hz , 2h ), 7 . 50 ( d , j = 2 . 0 hz , 1h ), 7 . 17 ( br d , j = 7 . 8 hz , 2h ), 4 . 45 ( q , j = 7 . 1 hz , 2h ), 4 . 06 ( s , 2h ), 2 . 31 ( s , 3h ), 1 . 42 ( t , j = 7 . 1 hz , 3h ). compound c21 ( 872 mg , 2 . 58 mmol ) was reacted with p1 according to the method described for synthesis of 3 in example 3 . in this case , the crude product obtained after ethyl acetate extraction was taken up as a slurry in hot ethyl acetate ( 15 ml ), which was then allowed to stir and cool for 2 hours . collection of the precipitate via filtration afforded the product as a white solid . yield : 525 mg , 1 . 28 mmol , 50 %. lcms m / z 410 . 2 [ m + h ] + . 1 h nmr ( 400 mhz , dmso - d 6 ) δ 9 . 18 ( br d , j = 1 hz , 1h ), 8 . 51 ( d , j = 8 . 4 hz , 1h ), 8 . 43 ( s , 1h ), 8 . 12 ( br d , j = 1 hz , 1h ), 7 . 94 ( d , j = 8 . 0 hz , 2h ), 7 . 78 ( s , 1h ), 7 . 26 ( d , j = 8 . 0 hz , 2h ), 4 . 93 ( d , j = 5 . 7 hz , 1h ), 4 . 12 ( s , 2h ), 3 . 71 - 3 . 83 ( m , 3h ), 3 . 51 - 3 . 61 ( m , 1h ), 3 . 27 - 3 . 36 ( m , 1h , assumed , partially obscured by solvent peak ), 3 . 01 ( dd , j = 10 . 5 , 10 . 5 hz , 1h ), 2 . 33 ( s , 3h ), 1 . 77 - 1 . 85 ( m , 1h ), 1 . 55 - 1 . 68 ( m , 1h ). a mixture of c9 ( 680 mg , 3 . 41 mmol ), 4 , 4 , 4 ′, 4 ′, 5 , 5 , 5 ′, 5 ′- octamethyl - 2 , 2 ′- bi - 1 , 3 , 2 - dioxaborolane ( 1 . 04 g , 4 . 10 mmol ), tricyclohexylphosphine ( 48 mg , 0 . 17 mmol ), tris ( dibenzylideneacetone ) dipalladium ( 0 ) ( 93 mg , 0 . 10 mmol ), and potassium acetate ( 1 . 00 g , 10 . 2 mmol ) in 1 , 4 - dioxane ( 25 ml ) was stirred in a sealed vial at 150 ° c . for 5 . 5 hours . the reaction mixture was filtered , and the filtrate ( a 1 , 4 - dioxane solution of c22 ) was used directly in the following step . a mixture of c22 ( from the previous step , as a crude solution in 1 , 4 - dioxane , 3 . 41 mmol ), 1 -[ 4 -( bromomethyl ) phenyl ]- 1h - pyrazole ( 1 . 25 g , 5 . 27 mmol ), [ 1 , 1 ′- bis ( diphenylphosphino ) ferrocene ] dichloropalladium ( ii ) ( 175 mg , 0 . 239 mmol ), and potassium carbonate ( 1 . 32 g , 9 . 55 mmol ) in 1 , 4 - dioxane ( 60 ml ) and water ( 1 ml ) was stirred at 80 ° c . for 20 hours . the reaction mixture was filtered through diatomaceous earth , and the filtrate was concentrated in vacuo . silica gel chromatography ( gradient : 10 % to 50 % ethyl acetate in petroleum ether ) afforded the product as an off - white gum . yield : 800 mg , 2 . 5 mmol , 73 % over two steps . 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 53 ( s , 1h ), 7 . 89 - 7 . 93 ( m , 2h ), 7 . 71 - 7 . 73 ( m , 1h ), 7 . 64 ( br d , j = 8 . 5 hz , 2h ), 7 . 20 ( br d , j = 8 . 4 hz , 2h ), 6 . 47 ( dd , j = 2 . 3 , 1 . 9 hz , 1h ), 4 . 47 ( q , j = 7 . 2 hz , 2h ), 4 . 07 ( s , 2h ), 2 . 32 ( s , 3h ), 1 . 44 ( t , j = 7 . 1 hz , 3h ). a mixture of c23 ( 800 mg , 2 . 5 mmol ) and sodium hydroxide ( 398 mg , 9 . 95 mmol ) in methanol ( 15 ml ) and water ( 15 ml ) was stirred at 80 ° c . for 2 hours . the reaction mixture was then diluted with water ( 50 ml ), concentrated under reduced pressure to remove methanol , and acidified to a ph of 3 - 4 with concentrated hydrochloric acid . after extraction with a mixture of dichloromethane and methanol ( 20 : 1 ; 3 × 50 ml ), the combined organic layers were dried over sodium sulfate , filtered , and concentrated in vacuo to provide the product as a yellow solid . yield : 620 mg , 2 . 1 mmol , 84 %. a solution of c24 ( 800 mg , 2 . 73 mmol ), trans - 4 - aminotetrahydro - 2h - pyran - 3 - ol ( 383 mg , 3 . 27 mmol ), o -( 7 - azabenzotriazol - 1 - yl )- n , n , n ′, n ′- tetramethyluronium hexafluorophosphate ( 1 . 24 g , 3 . 26 mmol ), and triethylamine ( 828 mg , 8 . 18 mmol ) in dichloromethane ( 30 ml ) was stirred at room temperature for 2 hours . the reaction mixture was concentrated in vacuo , and the residue was purified via chromatography on silica gel ( gradient : 0 % to 4 % methanol in dichloromethane ). the resulting yellow solid ( 950 mg , 2 . 4 mmol , 88 %) was separated into its component enantiomers using reversed phase hplc ( column : chiral technologies chiralpak ad , 10 μm ; mobile phase : 55 % ethanol in aqueous ammonia ) to provide 8 and 9 , both as white solids . compound 8 was found to have a negative (−) rotation , and 9 exhibited a positive (+) rotation . the indicated absolute stereochemistry was assigned based on an x - ray crystal structure determination carried out on 9 ( see below ). 8 : yield : 360 mg , 0 . 92 mmol , 34 %. lcms m / z 392 . 9 [ m + h ] + . 1 h nmr ( 400 mhz , cd 3 od ) δ 8 . 42 ( s , 1h ), 8 . 18 ( d , j = 2 . 5 hz , 1h ), 7 . 86 ( s , 1h ), 7 . 69 - 7 . 71 ( m , 1h ), 7 . 69 ( br d , j = 8 . 7 hz , 2h ), 7 . 30 ( br d , j = 8 . 7 hz , 2h ), 6 . 51 ( dd , j = 2 , 2 hz , 1h ), 4 . 15 ( s , 2h ), 3 . 87 - 3 . 99 ( m , 3h ), 3 . 63 ( ddd , j = 9 . 5 , 9 . 5 , 5 hz , 1h ), 3 . 43 - 3 . 51 ( m , 1h ), 3 . 19 ( dd , j = 11 , 10 hz , 1h ), 2 . 37 ( s , 3h ), 1 . 98 - 2 . 05 ( m , 1h ), 1 . 64 - 1 . 76 ( m , 1h ). retention time : 0 . 91 minutes ( column : chiral technologies chiralpak ad - 3 , 4 . 6 × 50 mm , 3 μm ; mobile phase : 2 : 3 [ ethanol , containing 0 . 05 % diethylamine ]/ carbon dioxide ; flow rate : 4 ml / minute ). 9 : yield : 340 mg , 0 . 87 mmol , 32 %. lcms m / z 393 . 0 [ m + h ] + . 1 h nmr ( 400 mhz , cd 3 od ) δ 8 . 42 ( s , 1h ), 8 . 18 ( dd , j = 2 . 5 , 0 . 4 hz , 1h ), 7 . 86 ( s , 1h ), 7 . 70 - 7 . 71 ( m , 1h ), 7 . 69 ( br d , j = 8 . 7 hz , 2h ), 7 . 30 ( br d , j = 8 . 5 hz , 2h ), 6 . 51 ( dd , j = 2 . 5 , 1 . 9 hz , 1h ), 4 . 15 ( s , 2h ), 3 . 87 - 3 . 99 ( m , 3h ), 3 . 64 ( ddd , j = 10 , 9 , 5 hz , 1h ), 3 . 47 ( ddd , j = 11 . 8 , 11 . 7 , 2 . 3 hz , 1h ), 3 . 19 ( dd , j = 11 . 0 , 10 . 0 hz , 1h ), 2 . 37 ( s , 3h ), 1 . 98 - 2 . 06 ( m , 1h ), 1 . 64 - 1 . 76 ( m , 1h ). retention time : 1 . 61 minutes ( column : chiral technologies chiralpak ad - 3 , 4 . 6 × 50 mm , 3 μm ; mobile phase : 2 : 3 [ ethanol , containing 0 . 05 % diethylamine ]/ carbon dioxide ; flow rate : 4 ml / minute ). a sample of 9 was crystallized from a very concentrated solution of ethyl acetate and diethyl ether ; the resulting solid was slurried with 1 : 1 ethyl acetate / heptane and filtered . this material was subjected to x - ray structural analysis to determine its absolute configuration : data collection was performed on a bruker apex diffractometer at room temperature . data collection consisted of omega and phi scans . the structure was solved by direct methods using shelx software suite in the space group p2 1 2 1 2 1 . the structure was subsequently refined by the full - matrix least squares method . all non - hydrogen atoms were found and refined using anisotropic displacement parameters . the hydrogen atoms located on nitrogen and oxygen were found from the fourier difference map and refined with distances and displacement parameters restrained . the remaining hydrogen atoms were placed in calculated positions and were allowed to ride on their carrier atoms . the final refinement included isotropic displacement parameters for all hydrogen atoms . assignment of the c20 vs n4 position on the pyrazole was done by examination of bond lengths and competitive refinement . analysis of the absolute structure using likelihood methods ( hooft , 2008 ) was performed using platon ( spek , 2003 ). the results indicate that the absolute structure has been correctly assigned . the method calculates that the probability that the structure is correct is 100 . 0 . the hooft parameter is reported as 0 . 08 with an esd of 0 . 04 . the final r - index was 2 . 9 %. a final difference fourier revealed no missing or misplaced electron density . pertinent crystal , data collection and refinement information is summarized in table 1 . atomic coordinates , bond lengths , bond angles , torsion angles and displacement parameters are listed in tables 2 - 5 . platon , a . l . spek , j . appl . cryst . 2003 , 36 , 7 - 13 . mercury , c . f . macrae , p . r . edington , p . mccabe , e . pidcock , g . p . shields , r . taylor , m . towler , and j . van de streek , j . appl . cryst . 2006 , 39 , 453 - 457 . olex2 , o . v . dolomanov , l . j . bourhis , r . j . gildea , j . a . k . howard , and h . puschmann , j . appl . cryst . 2009 , 42 , 339 - 341 . r . w . w . hooft , l . h . strayer , and a . l . spek , j . appl . cryst . 2008 , 41 , 96 - 103 . h . d . flack , acta cryst . 1983 , a39 , 867 - 881 . a hot solution of p1 ( 2 . 54 g , 7 . 83 mmol ) in methanol ( 200 ml ) was treated with silicycle siliabond ® carbonate resin ( 0 . 59 mmol / g , 100 g , 59 mmol ), and the resulting mixture was stirred at room temperature overnight . the resin was removed via filtration , and the filter cake was thoroughly washed with methanol . the combined filtrates were concentrated in vacuo ; the residue was combined with n , n - dimethylformamide ( 70 ml ), c24 ( 2 . 00 g , 6 . 82 mmol ), and triethylamine ( 1 . 4 ml , 10 mmol ), then treated with o -( 7 - azabenzotriazol - 1 - yl )- n , n , n ′, n ′- tetramethyluronium hexafluorophosphate ( 99 %, 3 . 93 g , 10 . 2 mmol ). after the reaction mixture had stirred at room temperature overnight , it was diluted with half - saturated aqueous sodium bicarbonate solution , and extracted several times with ethyl acetate . the combined organic layers were washed twice with half - saturated aqueous sodium bicarbonate solution , twice with water , and once with saturated aqueous sodium chloride solution , dried over magnesium sulfate , filtered , and concentrated under reduced pressure . silica gel chromatography ( gradient : 5 % to 10 % methanol in dichloromethane ), followed by crystallization from a very concentrated solution of ethyl acetate and heptane , provided the product as a white solid . this material exhibited a positive (+) rotation , and was found to be crystalline via powder x - ray diffraction . yield : 2 . 00 g , 5 . 10 mmol , 75 %. lcms m / z 393 . 1 [ m + h ] + . 1 h nmr ( 400 mhz , cd 3 od ) δ 8 . 42 ( s , 1h ), 8 . 19 ( dd , j = 2 . 5 , 0 . 5 hz , 1h ), 7 . 86 ( s , 1h ), 7 . 70 - 7 . 71 ( m , 1h ), 7 . 69 ( br d , j = 8 . 7 hz , 2h ), 7 . 30 ( br d , j = 8 . 7 hz , 2h ), 6 . 51 ( dd , j = 2 . 4 , 1 . 9 hz , 1h ), 4 . 15 ( s , 2h ), 3 . 87 - 3 . 99 ( m , 3h ), 3 . 64 ( ddd , j = 9 . 7 , 9 . 6 , 4 . 9 hz , 1h ), 3 . 47 ( ddd , j = 11 . 9 , 11 . 9 , 2 . 2 hz , 1h ), 3 . 19 ( dd , j = 11 . 1 , 9 . 8 hz , 1h ), 2 . 37 ( s , 3h ), 1 . 98 - 2 . 05 ( m , 1h ), 1 . 64 - 1 . 76 ( m , 1h ). a mixture of 4 -( bromoacetyl ) benzonitrile ( 9 . 5 g , 42 mmol ) and acetamide ( 6 . 26 g , 106 mmol ) in toluene ( 200 ml ) was heated at reflux for 48 hours , whereupon it was filtered . after the filtrate had been concentrated in vacuo , silica gel chromatography ( gradient : 0 % to 20 % ethyl acetate in petroleum ether ) afforded the product as a white solid . yield : 7 . 5 g , 41 mmol , 98 %. 1 h nmr ( 400 mhz , cdcl 3 ) δ 7 . 92 ( s , 1h ), 7 . 81 ( br d , j = 8 . 5 hz , 2h ), 7 . 68 ( br d , j = 8 . 7 hz , 2h ), 2 . 54 ( s , 3h ). compound c25 ( 6 . 0 g , 33 mmol ) and concentrated sulfuric acid ( 50 ml ) were combined in methanol ( 100 ml ) and heated at reflux for 24 hours . the reaction mixture was slowly poured into ice water ( 300 ml ), and the resulting mixture was adjusted to a ph of 7 - 8 with solid sodium hydroxide . upon removal of methanol under reduced pressure , copious yellow solid precipitated ; this was collected via filtration to provide the product as a yellow solid . yield : 6 . 5 g , 30 mmol , 91 %. 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 06 ( d , j = 8 . 4 hz , 2h ), 7 . 90 ( s , 1h ), 7 . 77 ( d , j = 8 . 4 hz , 2h ), 3 . 92 ( s , 3h ), 2 . 53 ( s , 3h ). lithium aluminum hydride ( 4 . 19 g , 110 mmol ) was added to a − 78 ° c . solution of c26 ( 6 . 00 g , 27 . 6 mmol ) in tetrahydrofuran ( 200 ml ), and the reaction mixture was allowed to stir at − 30 ° c . for 1 hour . water ( 4 . 5 ml ) and aqueous sodium hydroxide solution ( 15 %, 4 . 5 ml ) were slowly added to the reaction mixture . it was then diluted with ethyl acetate ( 200 ml ) and filtered ; the filtrate was dried over sodium sulfate , filtered , and concentrated in vacuo to afford the product as a white solid . yield : 4 . 0 g , 21 mmol , 76 %. 1 h nmr ( 400 mhz , cdcl 3 ) δ 7 . 81 ( s , 1h ), 7 . 69 ( d , j = 8 . 2 hz , 2h ), 7 . 39 ( d , j = 8 . 0 hz , 2h ), 4 . 71 ( s , 2h ), 2 . 52 ( s , 3h ), 2 . 00 - 2 . 14 ( br s , 1h ). thionyl chloride ( 7 . 55 g , 63 . 5 mmol ) was slowly added to a solution of c27 ( 4 . 0 g , 21 mmol ) in dichloromethane ( 150 ml ), and the reaction mixture was stirred at room temperature for 2 hours . removal of solvent in vacuo provided the product as a yellow solid . yield : 4 . 2 g , 17 . 2 mmol , 82 %. 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 04 ( s , 1h ), 7 . 90 ( d , j = 8 . 2 hz , 2h ), 7 . 51 ( d , j = 8 . 2 hz , 2h ), 4 . 61 ( s , 2h ), 2 . 96 ( s , 3h ). to a mixture of c28 ( 122 mg , 0 . 500 mmol ), c10 ( 175 mg , 0 . 601 mmol ), and sodium hydroxide ( 100 mg , 2 . 5 mmol ) in acetonitrile ( 5 ml ) and water ( 0 . 2 ml ) was added tetrakis ( triphenylphosphine ) palladium ( 0 ) ( 58 mg , 50 μmol ). the reaction mixture was stirred at 80 ° c . for 6 hours , whereupon it was diluted with water ( 10 ml ) and washed with ethyl acetate ( 10 ml ). the aqueous layer was acidified to a ph of 3 with hydrochloric acid , and the mixture was concentrated under reduced pressure to provide the product ( 160 mg ), a portion of which was used in the next step without further purification to a mixture of c29 ( 120 mg , 0 . 38 mmol ), trans - 4 - aminotetrahydro - 2h - pyran - 3 - ol ( 68 . 4 mg , 0 . 584 mmol ) and triethylamine ( 118 mg , 1 . 17 mmol ) in dichloromethane ( 10 ml ) was added o -( 7 - azabenzotriazol - 1 - yl )- n , n , n ′, n ′- tetramethyluronium hexafluorophosphate ( 148 mg , 0 . 389 mmol ), and the reaction mixture was stirred at room temperature overnight , then at 30 ° c . overnight . after the reaction mixture had been concentrated in vacuo , the residue was purified twice by preparative thin layer chromatography on silica gel ( eluent : 10 : 1 dichloromethane / methanol ). the resulting compound was separated into its component enantiomers via reversed phase hplc ( column : chiral technologies chiralpak ad , 10 μm ; mobile phase : 55 % ethanol in aqueous ammonia ) to provide 10 and 11 , both as white solids . compound 10 was found to have a negative (−) rotation , and 11 exhibited a positive (+) rotation . compounds 10 and 11 are designated according to their rotation signs . 10 : yield : 16 . 1 mg , 39 . 5 μmol , 10 % over two steps . lcms m / z 429 . 9 [ m + n + ]. 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 30 ( s , 1h ), 8 . 12 ( br d , j = 6 hz , 1h ), 7 . 99 ( s , 1h ), 7 . 78 ( s , 1h ), 7 . 62 ( d , j = 8 . 0 hz , 2h ), 7 . 13 ( d , j = 7 . 8 hz , 2h ), 4 . 46 ( br s , 1h ), 4 . 04 ( s , 2h ), 3 . 89 - 4 . 14 ( m , 3h ), 3 . 59 - 3 . 68 ( m , 1h ), 3 . 42 - 3 . 52 ( m , 1h ), 3 . 23 ( dd , j = 10 . 8 , 10 . 5 hz , 1h ), 2 . 51 ( s , 3h ), 2 . 30 ( s , 3h ), 1 . 99 - 2 . 09 ( m , 1h ), 1 . 73 - 1 . 87 ( m , 1h ). retention time : 0 . 63 minutes ( column : chiral technologies chiralpak ad - 3 , 4 . 6 × 50 mm , 3 μm ; mobile phase : 3 : 2 [ methanol , containing 0 . 05 % diethylamine ]/ carbon dioxide ; flow rate : 3 ml / minute ). 11 : yield : 7 . 8 mg , 19 μmol , 5 % over two steps . lcms m / z 430 . 0 [ m + na + ]. 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 31 ( s , 1h ), 8 . 12 ( br d , j = 6 hz , 1h ), 8 . 00 ( s , 1h ), 7 . 78 ( s , 1h ), 7 . 63 ( d , j = 8 . 2 hz , 2h ), 7 . 13 ( d , j = 8 . 2 hz , 2h ), 4 . 45 ( br s , 1h ), 4 . 09 ( dd , j = 11 . 4 , 4 . 8 hz , 1h ), 4 . 04 ( s , 2h ), 3 . 90 - 4 . 03 ( m , 2h ), 3 . 64 ( br ddd , j = 9 . 5 , 9 . 5 , 5 hz , 1h ), 3 . 47 ( ddd , j = 12 . 0 , 11 . 9 , 2 . 1 hz , 1h ), 3 . 23 ( dd , j = 11 . 2 , 10 . 1 hz , 1h ), 2 . 51 ( s , 3h ), 2 . 30 ( s , 3h ), 2 . 00 - 2 . 08 ( m , 1h ), 1 . 74 - 1 . 86 ( m , 1h ). retention time : 1 . 02 minutes ( column : chiral technologies chiralpak ad - 3 , 4 . 6 × 50 mm , 3 μm ; mobile phase : 3 : 2 [ methanol , containing 0 . 05 % diethylamine ]/ carbon dioxide ; flow rate : 3 ml / minute ). a mixture of c24 ( 50 mg , 0 . 17 mmol ), cis - 2 - aminocyclohexanol ( 29 . 4 mg , 0 . 255 mmol ), o -( 7 - azabenzotriazol - 1 - yl )- n , n , n ′, n ′- tetramethyluronium hexafluorophosphate ( 194 mg , 0 . 510 mmol ), and triethylamine ( 86 . 2 mg , 0 . 852 mmol ) in dichloromethane ( 5 ml ) was stirred overnight at 40 ° c . the reaction mixture was concentrated in vacuo and the residue was purified by reversed phase hplc ( column : dikma diamonsil ® c18 ( 2 ), 5 μm ; mobile phase a : 0 . 225 % formic acid in water ; mobile phase b : acetonitrile ; gradient : 40 % to 60 % b ) to afford a racemic mixture of 12 and 13 as a white solid . yield : 35 mg , 90 μmol , 53 %. this material was separated into its component enantiomers via chiral hplc ( column : chiral technologies chiralpak ad , 10 μm ; mobile phase : 55 % methanol in aqueous ammonia ) to provide 12 and 13 , both as white solids . compound 12 was found to have a negative (−) rotation , and 13 exhibited a positive (+) rotation [ compounds 12 and 13 are designated according to their rotation signs ]. 12 : yield : 11 . 5 mg , 29 . 4 μmol , 33 % from the chiral separation . lcms m / z 390 . 9 [ m + h ] + . 1 h nmr ( 400 mhz , cd 3 od ) δ 8 . 40 ( s , 1h ), 8 . 17 - 8 . 22 ( m , 1h ), 7 . 85 ( s , 1h ), 7 . 65 - 7 . 74 ( m , 3h ), 7 . 30 ( br d , j = 8 . 3 hz , 2h ), 6 . 49 - 6 . 54 ( m , 1h ), 4 . 15 ( s , 2h ), 3 . 91 - 3 . 99 ( m , 2h ), 2 . 36 ( s , 3h ), 1 . 56 - 1 . 88 ( m , 6h ), 1 . 36 - 1 . 50 ( m , 2h ). retention time : 0 . 84 minutes ( column : chiral technologies chiralpak ad - 3 , 4 . 6 × 50 mm , 3 μm ; mobile phase : 3 : 2 [ methanol , containing 0 . 05 % diethylamine ]/ carbon dioxide ; flow rate : 3 ml / minute ). 13 : yield : 12 . 5 mg , 32 . 0 μmol , 36 % from the chiral separation . lcms m / z 391 . 0 [ m + h ] + . 1 h nmr ( 400 mhz , cd 3 od ) δ 8 . 40 ( s , 1h ), 8 . 19 ( d , j = 2 . 4 hz , 1h ), 7 . 85 ( s , 1h ), 7 . 69 - 7 . 73 ( m , 1h ), 7 . 68 ( d , j = 8 . 5 hz , 2h ), 7 . 30 ( d , j = 8 . 4 hz , 2h ), 6 . 51 ( dd , j = 2 , 2 hz , 1h ), 4 . 14 ( s , 2h ), 3 . 91 - 3 . 99 ( m , 2h ), 2 . 36 ( s , 3h ), 1 . 56 - 1 . 88 ( m , 6h ), 1 . 35 - 1 . 50 ( m , 2h ). retention time : 1 . 91 minutes ( column : chiral technologies chiralpak ad - 3 , 4 . 6 × 50 mm , 3 μm ; mobile phase : 3 : 2 [ methanol , containing 0 . 05 % diethylamine ]/ carbon dioxide ; flow rate : 3 ml / minute ). a solution of 6 - methyl - 5 - nitropyridine - 2 - carboxylic acid ( 4 . 0 g , 22 mmol ) in methanol ( 50 ml ) was treated with thionyl chloride ( 8 . 22 ml , 113 mmol ) and heated at reflux for 17 hours . after removal of solvent in vacuo , the residue was partitioned between ethyl acetate and saturated aqueous sodium bicarbonate solution . the organic layer was dried over sodium sulfate , filtered , and concentrated under reduced pressure to afford the product . yield : 3 . 7 g , 19 mmol , 86 %. lcms m / z 197 . 0 [ m + h ] + . 1 h nmr ( 400 mhz , dmso - d 6 ) δ 8 . 57 ( d , j = 8 . 4 hz , 1h ), 8 . 12 ( d , j = 8 . 4 hz , 1h ), 3 . 92 ( s , 3h ), 2 . 77 ( s , 3h ). an argon - purged solution of c30 ( 3 . 7 g , 19 mmol ) in ethyl acetate ( 50 ml ) was treated with 10 % palladium on carbon ( 500 mg ) and hydrogenated in a parr shaker ( 40 psi hydrogen ) for 4 hours . the reaction mixture was then filtered through diatomaceous earth ; concentration of the filtrate in vacuo provided the product ( 3 . 1 g ), which was used directly in the following step . lcms m / z 166 . 9 [ m + h ] + . 1 h nmr ( 400 mhz , dmso - d 6 ) δ 7 . 66 ( d , j = 8 . 3 hz , 1h ), 6 . 91 ( d , j = 8 . 3 hz , 1h ), 5 . 91 ( s , 2h ), 3 . 77 ( s , 3h ), 2 . 29 ( s , 3h ). a solution of c31 ( from the previous step , 3 . 1 g , 19 mmol ) in acetonitrile ( 15 ml ) was treated with n - bromosuccinimide ( 3 . 3 g , 19 mmol ) and stirred at room temperature for 2 hours . removal of solvent in vacuo provided a residue , which was partitioned between ethyl acetate and water . the organic layer was dried over sodium sulfate , filtered , and concentrated under reduced pressure ; silica gel chromatography afforded the product as an off - white solid . yield : 3 . 3 g , 13 mmol , 68 % over 2 steps . lcms m / z 245 . 0 , 246 . 8 [ m + h ] + . 1 h nmr ( 400 mhz , dmso - d 6 ) δ 7 . 90 ( s , 1h ), 6 . 12 ( br s , 2h ), 3 . 78 ( s , 3h ), 2 . 40 ( s , 3h ). a mixture of copper ( ii ) chloride ( 1 . 7 g , 13 mmol ) and tert - butyl nitrite ( 2 . 0 ml , 17 mmol ) in acetonitrile ( 75 ml ) was stirred at room temperature for 5 minutes , then heated to 60 ° c . compound c32 ( 2 . 8 g , 11 mmol ) was added , and stirring was continued at 60 ° c . for 4 hours . the reaction mixture was concentrated in vacuo and partitioned between ethyl acetate and water ; the organic layer was dried over sodium sulfate , filtered , concentrated under reduced pressure , and subjected to silica gel chromatography . further purification via reversed phase hplc ( column : waters xterra shield rp18 obd prep , 10 μm ; mobile phase a : 5 mm ammonium acetate in water ; mobile phase b : acetonitrile ; gradient : 10 % to 40 % b ) afforded c33 and c34 , both as white solids . c33 : yield : 260 mg , 1 . 2 mmol , 11 %. lcms m / z 220 . 3 , 222 . 1 [ m + h ] + . 1 h nmr ( 400 mhz , dmso - d 6 ) δ 8 . 11 ( s , 1h ), 3 . 89 ( s , 3h ), 2 . 67 ( s , 3h ). c34 : yield : 520 mg , 2 . 0 mmol , 18 %. lcms m / z 263 . 7 , 265 . 7 , 268 . 0 [ m + h ] + . 1 h nmr ( 400 mhz , dmso - d 6 ) δ 8 . 20 ( s , 1h ), 3 . 89 ( s , 3h ), 2 . 68 ( s , 3h ). a mixture of 1 -[ 4 -( bromomethyl ) phenyl ]- 1h - pyrazole ( 1 . 42 g , 5 . 99 mmol ), 4 , 4 , 4 ′, 4 ′, 5 , 5 , 5 ′, 5 ′- octamethyl - 2 , 2 ′- bi - 1 , 3 , 2 - dioxaborolane ( 1 . 98 g , 7 . 80 mmol ), [ 1 , 1 ′- bis ( diphenylphosphino ) ferrocene ] dichloropalladium ( ii ), dichloromethane complex ( 245 mg , 0 . 300 mmol ), and potassium acetate ( 1 . 77 g , 18 . 0 mmol ) in 1 , 4 - dioxane ( 80 ml ) was stirred at 100 ° c . for 6 hours . the reaction mixture was filtered through diatomaceous earth ; the filtrate was concentrated in vacuo and subjected to silica gel chromatography ( gradient : 0 % to 15 % ethyl acetate in petroleum ether ) to afford the product as an off - white solid . yield : 1 . 4 g , 4 . 9 mmol , 82 %. 1 h nmr ( 400 mhz , cdcl 3 ) δ 7 . 88 ( d , j = 2 . 4 hz , 1h ), 7 . 69 - 7 . 72 ( m , 1h ), 7 . 56 ( br d , j = 8 . 4 hz , 2h ), 7 . 27 ( br d , j = 8 . 2 hz , 2h ), 6 . 43 - 6 . 46 ( m , 1h ), 2 . 33 ( s , 2h ), 1 . 24 ( s , 12h ). a mixture of c33 ( 160 mg , 0 . 727 mmol ), c35 ( 310 mg , 1 . 09 mmol ), [ 1 , 1 ′- bis ( diphenylphosphino ) ferrocene ] dichloropalladium ( ii ) ( 53 mg , 72 μmol ) and potassium carbonate ( 201 mg , 1 . 45 mmol ) in tetrahydrofuran ( 20 ml ) and water ( 1 ml ) was stirred at 90 ° c . for 40 hours . after addition of water ( 15 ml ) to the reaction mixture , it was extracted with ethyl acetate ( 2 × 15 ml ), and the combined organic layers were dried over sodium sulfate , filtered , and concentrated in vacuo . silica gel chromatography ( gradient : 0 % to 40 % ethyl acetate in petroleum ether ) provided the product as a white solid . yield : 130 mg , 0 . 380 mmol , 52 %. a mixture of c36 ( 130 mg , 0 . 380 mmol ) and sodium hydroxide ( 76 . 1 mg , 1 . 90 mmol ) in methanol ( 10 ml ) and water ( 5 ml ) was stirred at 80 ° c . for 2 hours . after removal of methanol under reduced pressure , water ( 10 ml ) was added and the mixture was acidified with hydrochloric acid to a ph of 3 . filtration afforded the product as a white solid . yield : 105 mg , 0 . 320 mmol , 84 %. lcms m / z 327 . 8 [ m + h ] + . 1 h nmr ( 400 mhz , cd 3 od ) δ 8 . 20 ( s , 1h ), 7 . 87 ( s , 1h ), 7 . 66 - 7 . 76 ( m , 3h ), 7 . 37 ( br d , j = 8 hz , 2h ), 6 . 49 - 6 . 55 ( m , 1h ), 4 . 26 ( s , 2h ), 2 . 70 ( s , 3h ). o -( 7 - azabenzotriazol - 1 - yl )- n , n , n ′, n ′- tetramethyluronium hexafluorophosphate ( 184 mg , 0 . 479 mmol ) was added to a solution of c37 ( 105 mg , 0 . 320 mmol ), p2 ( 41 . 2 mg , 0 . 352 mmol ), and triethylamine ( 67 . 6 μl , 0 . 485 mmol ) in n , n - dimethylformamide ( 4 ml ). after the reaction mixture had been stirred at room temperature overnight , it was diluted with half - saturated aqueous sodium bicarbonate solution and extracted three times with ethyl acetate . the combined organic layers were washed twice with half - saturated aqueous sodium bicarbonate solution , twice with water , and once with saturated aqueous sodium chloride solution , then dried over magnesium sulfate , filtered , and concentrated in vacuo . purification via chromatography on silica gel ( gradient : 0 % to 50 % [ 80 : 20 : 1 dichloromethane / methanol / concentrated ammonium hydroxide ] in dichloromethane ) was followed by crystallization from a very concentrated solution of warm 1 : 1 ethyl acetate / heptane , affording the product as a white solid . compound 14 was found to have a positive (+) rotation . yield : 112 mg , 0 . 262 mmol , 82 %. lcms m / z 427 . 1 , 429 . 1 [ m + h ] + . 1 h nmr ( 400 mhz , cd 3 od ) δ 8 . 64 ( br d , j = 8 hz , 1h ), 8 . 19 ( dd , j = 2 . 5 , 0 . 6 hz , 1h ), 7 . 83 ( br s , 1h ), 7 . 70 - 7 . 71 ( m , 1h ), 7 . 69 ( br d , j = 8 . 7 hz , 2h ), 7 . 36 ( br d , j = 8 . 8 hz , 2h ), 6 . 51 ( dd , j = 2 . 5 , 1 . 9 hz , 1h ), 4 . 25 ( s , 2h ), 3 . 87 - 3 . 99 ( m , 3h ), 3 . 65 ( ddd , j = 10 , 10 , 5 hz , 1h ), 3 . 47 ( ddd , j = 12 , 12 , 2 hz , 1h ), 3 . 18 ( dd , j = 11 . 1 , 10 hz , 1h ), 2 . 70 ( d , j = 0 . 3 hz , 3h ), 1 . 96 - 2 . 03 ( m , 1h ), 1 . 66 - 1 . 78 ( m , 1h ). 1 - chloro - 3 -( chloromethyl ) benzene ( 25 . 7 ml , 202 mmol ) was added drop - wise over a period of 10 minutes to a solution of 5 - hydroxy - 2 -( hydroxymethyl )- 4h - pyran - 4 - one ( 25 . 0 g , 176 mmol ) and sodium hydroxide ( 7 . 74 g , 194 mmol ) in aqueous methanol ( 1 : 10 , 300 ml ). the reaction mixture was heated to 80 ° c . for 5 hours , whereupon it was poured into ice - cold water . the resulting solid was isolated via filtration , then sequentially washed with water , diethyl ether ( 500 ml ), and hexanes to afford the product as a white solid . yield : 45 g , 170 mmol , 97 %. a suspension of c38 ( 10 g , 37 mmol ) in acetone ( 200 ml ) was cooled to 20 ° c . and slowly treated with jones reagent ( chromic acid content : 6 . 91 g , 69 . 1 mmol ) over a period of 20 minutes . the reaction mixture was concentrated to half of its initial volume , whereupon it was diluted with ethyl acetate ( 200 ml ) and extracted with saturated aqueous sodium bicarbonate solution ( 2 × 200 ml ). the aqueous layer was acidified with 3 m hydrochloric acid and extracted with ethyl acetate ( 300 ml ). this organic layer was washed with saturated aqueous sodium chloride solution , dried over sodium sulfate , filtered , and concentrated in vacuo to provide the product as a solid . yield : 5 . 0 g , 18 mmol , 49 %. lcms m / z 281 . 2 , 283 . 3 [ m + h ] + . 1 h nmr ( 300 mhz , dmso - d 6 ) δ 8 . 39 ( s , 1h ), 7 . 4 - 7 . 5 ( m , 4h ), 6 . 95 ( s , 1h ), 5 . 01 ( s , 2h ). a mixture of ammonia ( 25 % aqueous solution , 14 . 6 ml , 195 mmol ) and c39 ( 6 . 0 g , 21 mmol ) was placed in a sealed tube and heated at 90 ° c . for 3 hours . the reaction mixture was then cooled to 5 ° c ., diluted with diethyl ether ( 25 ml ), and filtered , affording the product as a solid . yield : 5 . 5 g , 20 mmol , 95 %. lcms m / z 280 . 2 , 282 . 3 [ m + h ] + . 1 h nmr ( 300 mhz , dmso - d 6 ) δ 7 . 50 ( s , 1h ), 7 . 3 - 7 . 4 ( m , 3h ), 7 . 25 ( s , 1h ), 6 . 58 ( s , 1h ), 5 . 02 ( s , 2h ). a suspension of c40 ( 5 . 0 g , 18 mmol ) in phosphorus oxychloride ( 27 ml , 290 mmol ) was heated at 95 ° c . for 30 minutes . the reaction mixture was concentrated in vacuo and quenched with water ( 50 ml ); the resulting solid was collected via filtration . silica gel chromatography ( eluent : 5 % methanol in chloroform ) provided the product as a white solid . yield : 1 g , 3 mmol , 17 %. lcms m / z 298 . 3 , 300 . 3 , 302 . 3 [ m + h ] + . 1 h nmr ( 300 mhz , dmso - d 6 ) δ 13 . 2 ( br s , 1h ), 8 . 7 ( s , 1h ), 8 . 1 ( s , 1h ), 7 . 6 ( s , 1h ), 7 . 4 - 7 . 6 ( m , 3h ), 5 . 50 ( s , 2h ). to a 0 ° c . mixture of c41 ( 1 . 5 g , 5 . 0 mmol ) in dichloromethane ( 20 ml ) was added oxalyl chloride ( 1 . 28 g , 10 . 1 mmol ) and n , n - dimethylformamide ( 184 mg , 2 . 52 mmol ). after the reaction mixture had been stirred at room temperature for 2 hours , it was cooled to 0 ° c . and treated in a drop - wise manner with methanol ( 1 ml ). the reaction mixture was then stirred at room temperature for 30 minutes , whereupon it was concentrated to dryness . the residue was washed with water ( 10 ml ) and filtered ; the filter cake was dried under vacuum . the resulting material was washed with petroleum ether ( 10 ml ) and filtered to afford the product as a white solid . yield : 1 . 5 g , 4 . 8 mmol , 96 %. 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 55 ( br s , 1h ), 8 . 29 ( s , 1h ), 7 . 48 ( s , 1h ), 7 . 37 ( br s , 3h ), 5 . 36 ( br s , 2h ), 4 . 05 ( s , 3h ). [ 1 , 1 ′- bis ( diphenylphosphino ) ferrocene ] dichloropalladium ( ii ) ( 305 mg , 0 . 417 mmol ) was added to a mixture of c42 ( 1 . 3 g , 4 . 2 mmol ), 4 , 4 , 4 ′, 4 ′, 5 , 5 , 5 ′, 5 ′- octamethyl - 2 , 2 ′- bi - 1 , 3 , 2 - dioxaborolane ( 2 . 54 g , 10 . 0 mmol ), and potassium acetate ( 1 . 23 g , 12 . 5 mmol ) in toluene ( 100 ml ). the reaction mixture was heated to 120 ° c . for 16 hours . lcms indicated that the desired { 5 -[( 3 - chlorobenzyl ) oxy ]- 2 -( methoxycarbonyl ) pyridin - 4 - yl } boronic acid had been generated : lcms m / z 321 . 7 [ m + h ] + . a solution of 1 -[ 4 -( bromomethyl ) phenyl ]- 1h - pyrazole ( 2 . 47 g , 10 . 4 mmol ) in 1 , 4 - dioxane ( 100 ml ) and water ( 10 ml ) was added to the reaction mixture , followed by potassium carbonate ( 1 . 72 g , 12 . 4 mmol ) and [ 1 , 1 ′- bis ( diphenylphosphino ) ferrocene ] dichloropalladium ( ii ) ( 304 mg , 0 . 415 mmol ). after the reaction mixture had been stirred at 80 ° c . for 16 hours , it was filtered and the filtrate was concentrated to dryness . the residue was dissolved in ethyl acetate ( 100 ml ), washed with water ( 60 ml ), dried over sodium sulfate , filtered , and concentrated in vacuo . silica gel chromatography ( gradient : 0 % to 60 % ethyl acetate in petroleum ether ) afforded the product as an off - white solid . yield : 850 mg , 1 . 96 mmol , 47 %. lcms m / z 434 . 0 [ m + h ] + . 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 34 ( s , 1h ), 7 . 98 ( s , 1h ), 7 . 89 - 7 . 93 ( m , 1h ), 7 . 70 - 7 . 74 ( m , 1h ), 7 . 60 - 7 . 66 ( m , 2h ), 7 . 23 - 7 . 34 ( m , 5h , assumed ; partially obscured by solvent peak ), 7 . 16 - 7 . 22 ( m , 1h ), 6 . 45 - 6 . 48 ( m , 1h ), 5 . 21 ( s , 2h ), 4 . 07 ( s , 2h ), 3 . 97 ( s , 3h ). a mixture of c43 ( 850 mg , 1 . 96 mmol ) and palladium on carbon ( 42 mg ) in methanol ( 60 ml ) was stirred for 4 hours at 30 ° c . under a hydrogen atmosphere ( 40 psi ). the reaction mixture was filtered and the filtrate was concentrated in vacuo ; the residue was washed with tert - butyl methyl ether ( 20 ml ) to provide the product as a brown solid . yield : 600 mg , 1 . 9 mmol , 97 %. 1 h nmr ( 400 mhz , cdcl 3 ), characteristic peaks : δ 7 . 91 - 8 . 02 ( m , 1h ), 7 . 91 ( s , 1h ), 7 . 75 ( s , 1h ), 7 . 57 - 7 . 69 ( m , 2h ), 7 . 30 - 7 . 43 ( m , 2h ), 6 . 49 ( s , 1h ), 4 . 13 ( br s , 2h ), 3 . 97 ( br s , 3h ). to a suspension of c44 ( 70 . 0 mg , 0 . 226 mmol ) in acetonitrile ( 2 ml ) was added potassium carbonate ( 46 . 9 mg , 0 . 339 mmol ) and iodomethane ( 33 . 7 mg , 0 . 237 mmol ) at 20 ° c . after the mixture had been stirred for 2 hours , n , n - dimethylformamide ( 2 ml ) and additional iodomethane ( 10 mg , 70 μmol ) were added . stirring was continued for 18 hours at 20 ° c ., whereupon the reaction mixture was partitioned between dichloromethane ( 2 ml ) and water ( 2 ml ). the aqueous layer was extracted with dichloromethane ( 3 × 2 ml ), and the combined organic layers were dried over sodium sulfate , filtered , and concentrated in vacuo . preparative thin layer chromatography on silica gel ( eluent : 1 : 1 petroleum ether / ethyl acetate ) afforded the product as a white solid . yield : 20 mg , 62 μmol , 27 %. lcms m / z 323 . 8 [ m + h ] + . to a solution of c45 ( 15 mg , 46 μmol ) in n , n - dimethylformamide ( 0 . 6 ml ) was added p2 ( 7 . 61 mg , 65 . 0 μmol ) and 1 , 3 , 4 , 6 , 7 , 8 - hexahydro - 2h - pyrimido [ 1 , 2 - a ] pyrimidine ( 6 . 46 mg , 46 . 4 μmol ), and the reaction mixture was stirred for 20 hours at 50 ° c . compound p2 ( 7 . 61 mg , 65 . 0 μmol ) and 1 , 3 , 4 , 6 , 7 , 8 - hexahydro - 2h - pyrimido [ 1 , 2 - a ] pyrimidine ( 6 . 46 mg , 46 . 4 μmol ) were added again , and stirring was continued for 20 hours at 50 ° c . after concentration of the reaction mixture in vacuo , preparative thin layer chromatography on silica gel ( eluent : ethyl acetate ) provided the product as a white solid . yield : 6 . 0 mg , 15 μmol , 33 %. lcms m / z 408 . 9 [ m + h ] + . 1 h nmr ( 400 mhz , cd 3 od ) δ 8 . 32 ( s , 1h ), 8 . 16 - 8 . 19 ( m , 1h ), 7 . 88 ( s , 1h ), 7 . 69 - 7 . 71 ( m , 1h ), 7 . 66 ( br d , j = 8 . 7 hz , 2h ), 7 . 36 ( br d , j = 8 . 5 hz , 2h ), 6 . 49 - 6 . 53 ( m , 1h ), 4 . 08 ( s , 2h ), 4 . 04 ( s , 3h ), 3 . 86 - 3 . 99 ( m , 3h ), 3 . 58 - 3 . 67 ( m , 1h ), 3 . 42 - 3 . 51 ( m , 1h ), 3 . 15 - 3 . 22 ( m , 1h ), 1 . 96 - 2 . 05 ( m , 1h ), 1 . 62 - 1 . 75 ( m , 1h ). a mixture of 1 -[( 25 )- tetrahydrofuran - 2 - yl ] methanamine ( 0 . 38 m solution in n , n - dimethylformamide , 300 μl , 110 μmol ), c24 ( 0 . 25 m solution in n , n - dimethylformamide , 300 μl , 75 μmol ), and triethylamine ( 32 μl , 230 μmol ) was treated with o -( 7 - azabenzotriazol - 1 - yl )- n , n , n ′, n ′- tetramethyluronium hexafluorophosphate ( 0 . 50 m solution in n , n - dimethylformamide , 150 μl , 75 μmol ). the reaction vessel was sealed and shaken at 30 ° c . for 16 hours , whereupon solvent was removed using a speedvac ® concentrator . the residue was subjected to purification via reversed phase hplc ( column : phenomenex gemini c18 , 8 μm ; mobile phase a : 0 . 225 % formic acid in water ; mobile phase b : acetonitrile ; gradient : 40 % to 80 % b ) to afford the product . yield : 9 . 1 mg , 24 μmol , 32 %. lcms m / z 377 [ m + h ] + . retention time : 2 . 97 minutes ( column : waters xbridge c18 , 2 . 1 × 50 mm , 5 μm ; mobile phase a : 0 . 0375 % trifluoroacetic acid in water ; mobile phase b : 0 . 01875 % trifluoroacetic acid in acetonitrile ; gradient : 10 % to 100 % b over 4 . 0 minutes ; flow rate : 0 . 8 ml / minute ). a mixture of c36 ( 25 mg , 73 μmol ) and sodium hydroxide ( 12 mg , 0 . 30 mmol ) in methanol ( 3 ml ) and water ( 1 ml ) was stirred at 70 ° c . for 3 hours , whereupon the ph was adjusted to approximately 7 via addition of 1 m hydrochloric acid . the resulting mixture was concentrated to dryness to provide the crude carboxylic acid as an off - white solid ( 25 mg ). this material was combined with ( 1s , 2s )- 2 - aminocyclohexanol , hydrochloride salt ( 23 mg , 0 . 15 mmol ), o -( 7 - azabenzotriazol - 1 - yl )- n , n , n ′, n ′- tetramethyluronium hexafluorophosphate ( 43 . 3 mg , 0 . 114 mmol ) and triethylamine ( 15 mg , 0 . 15 mmol ) in n , n - dimethylformamide ( 12 ml ), and the reaction mixture was stirred at room temperature for 20 hours . it was then concentrated to dryness , diluted with water ( 20 ml ), and extracted with ethyl acetate ( 4 × 30 ml ). the combined organic layers were dried , filtered , and concentrated under reduced pressure . preparative thin layer chromatography ( eluent : 1 : 2 petroleum ether / ethyl acetate ) afforded the product as an off - white solid . yield : 7 . 0 mg , 16 μmol , 22 %. lcms m / z 447 . 0 [ m + na + ]. 1 h nmr ( 400 mhz , cdcl 3 ) δ 7 . 99 ( br d , j = 6 hz , 1h ), 7 . 92 ( s , 1h ), 7 . 87 - 7 . 92 ( m , 1h ), 7 . 71 ( s , 1h ), 7 . 63 ( d , j = 8 . 3 hz , 2h ), 7 . 25 - 7 . 32 ( m , 2h , assumed ; partially obscured by solvent peak ), 6 . 44 - 6 . 48 ( m , 1h ), 4 . 17 ( s , 2h ), 3 . 74 - 3 . 86 ( m , 1h ), 3 . 45 - 3 . 55 ( m , 1h ), 3 . 31 - 3 . 39 ( m , 1h ), 2 . 67 ( s , 3h ), 2 . 00 - 2 . 17 ( m , 2h ), 1 . 72 - 1 . 84 ( m , 2h ), 1 . 22 - 1 . 48 ( m , 4h ). a mixture of c24 ( 120 mg , 0 . 41 mmol ), ( 1s , 2s )- 2 - aminocyclohexanol ( 56 . 5 mg , 0 . 490 mmol ), o -( 7 - azabenzotriazol - 1 - yl )- n , n , n ′, n ′- tetramethyluronium hexafluorophosphate ( 187 mg , 0 . 492 mmol ), and triethylamine ( 124 mg , 1 . 23 mmol ) in dichloromethane ( 10 ml ) was stirred overnight at room temperature . the reaction mixture was concentrated in vacuo and the residue was purified by silica gel chromatography ( gradient : 0 % to 4 % methanol in dichloromethane ) to yield the product as a white solid . yield : 145 mg , 0 . 371 mmol , 90 %. lcms m / z 391 . 1 [ m + h ] + . 1 h nmr ( 400 mhz , cd 3 od ) δ 8 . 41 ( s , 1h ), 8 . 19 ( d , j = 2 . 5 hz , 1h ), 7 . 86 ( s , 1h ), 7 . 70 ( d , j = 1 . 6 hz , 1h ), 7 . 68 ( d , j = 8 . 5 hz , 2h ), 7 . 30 ( d , j = 8 . 3 hz , 2h ), 6 . 51 ( dd , j = 2 . 4 , 1 . 9 hz , 1h ), 4 . 15 ( s , 2h ), 3 . 69 - 3 . 79 ( m , 1h ), 3 . 47 - 3 . 57 ( m , 1h ), 2 . 36 ( s , 3h ), 1 . 98 - 2 . 08 ( m , 2h ), 1 . 68 - 1 . 81 ( m , 2h ), 1 . 31 - 1 . 45 ( m , 4h ). method a describes a specific method for preparations of certain exemplar compounds of the invention . a mixture of amine r 1 — nh 2 ( 75 μmol ), the requisite 4 - benzylpyridine - 2 - carboxylic acid or 4 -( heteroarylmethyl ) pyridine - 2 - carboxylic acid ( 0 . 15 m solution in n , n - dimethylformamide , 500 μl , 75 μmol ), and n , n - diisopropylethylamine ( 40 μl , 230 μmol ) was treated with o -( 7 - azabenzotriazol - 1 - yl )- n , n , n ′, n ′- tetramethyluronium hexafluorophosphate ( 0 . 375 m solution in n , n - dimethylformamide , 200 μl , 75 μmol ). the reaction vessel was sealed and shaken at 50 ° c . for 16 hours , whereupon solvent was removed using a speedvac ® concentrator . the residue was subjected to purification via reversed phase hplc ( column : phenomenex gemini c18 , 8 μm ; mobile phase a : 0 . 225 % formic acid in water ; mobile phase b : acetonitrile ; gradient 30 % to 70 % b ) to afford the product . table 6 below lists some additional examples of compounds of invention ( examples 19 - 54 ) that were made using methods , starting materials or intermediates , and preparations described herein . 2 . examples 20 and 21 were synthesized as the racemic mixture . separation was carried out via reversed phase hplc ( column : chiral technologies chiralpak ad , 10 μm ; mobile phase : 55 % ethanol in aqueous ammonia ). the indicated absolute configurations were assigned on the basis of the relative biological activity of these two compounds ( see table 7 ), with reference to the known configurations and relative biological activity of examples 8 and 9 . compound 20 exhibited a retention time of 0 . 73 minutes ( and designated as trans , ent - 1 ), while 21 eluted at 1 . 37 minutes ( and designated as trans , ent - 2 ), in the following supercritical fluid chromatographic system : column : chiral technologies chiralpak ad - 3 , 4 . 6 × 50 mm , 3 μm ; mobile phase : 3 : 2 [ methanol , containing 0 . 05 % diethylamine ]/ carbon dioxide ; flow rate : 3 ml / minute . 3 . compound c24 was converted to its methyl ester via treatment with hydrogen chloride in methanol at 60 ° c . 5 - methylpyrimidin - 2 - amine and trimethylaluminum were combined in toluene and tetrahydrofuran , and heated at 30 ° c . for 16 hours . the methyl ester was then added , and the reaction mixture was heated at 80 ° c . to provide the product . 4 . conditions for analytical hplc . column : waters xbridge c18 , 2 . 1 × 50 mm , 5 μm ; mobile phase a : 0 . 0375 % trifluoroacetic acid in water ; mobile phase b : 0 . 01875 % trifluoroacetic acid in acetonitrile ; gradient : 1 % to 5 % b over 0 . 6 minutes ; 5 % to 100 % b over 3 . 4 minutes ; flow rate : 0 . 8 ml / minute . 5 . conditions for analytical hplc . column : waters xbridge c18 , 2 . 1 × 50 mm , 5 μm ; mobile phase a : 0 . 0375 % trifluoroacetic acid in water ; mobile phase b : 0 . 01875 % trifluoroacetic acid in acetonitrile ; gradient : 10 % to 100 % b over 4 . 0 minutes ; flow rate : 0 . 8 ml / minute . 6 . in this case , the column used for purification was a dikma diamonsil ( 2 ) c18 , 5 μm . 7 . racemic 2 , 2 - difluorocyclohexanamine was utilized ; separation of enantiomers 46 and 47 was carried out via supercritical fluid chromatography ( column : phenomenex amylose - 2 , 5 μm ; mobile phase : 4 : 1 carbon dioxide / methanol ). example 46 was the first - eluting enantiomer , followed by example 47 . examples 46 and 47 are designated according to their respective retention time . 8 . conditions for analytical supercritical fluid hplc . column : chiral technologies chiralcel oj - h , 4 . 6 × 100 mm , 5 μm ; mobile phase : 4 : 1 carbon dioxide / methanol ; flow rate : 1 . 5 ml / minute . 9 . compound c9 was reacted at elevated temperature with chloro ( 4 - methoxybenzyl ) zinc in the presence of bis ( tri - tert - butylphosphine ) palladium ( 0 ) to provide the requisite ethyl 4 -( 4 - methoxybenzyl )- 5 - methylpyridine - 2 - carboxylate . 10 . the compound of example 9 was oxidized with 3 - chloroperoxybenzoic acid to provide example 53 . 11 . this nmr data was obtained on material isolated after chromatography on silica gel , but before the final hplc purification . 12 . the requisite ethyl 5 -( difluoromethyl )- 4 -( 4 , 4 , 5 , 5 - tetramethyl - 1 , 3 , 2 - dioxaborolan - 2 - yl ) pyridine - 2 - carboxylate was prepared in the following manner : ethyl 4 - chloro - 5 - methylpyridine - 2 - carboxylate was converted to ethyl 4 - chloro - 5 -( hydroxymethyl ) pyridine - 2 - carboxylate using the method described by l . f . tietze et al ., chem . eur . j . 2008 , 14 , 2527 - 2535 . dess - martin oxidation to the corresponding aldehyde was followed by reaction with ( diethylamino ) sulfur trifluoride to afford ethyl 4 - chloro - 5 -( difluoromethyl ) pyridine - 2 - carboxylate . further reaction using the conditions described for conversion of c9 to c22 in examples 8 and 9 provided the appropriate intermediate . to a solution of c23 ( 2 . 00 g , 6 . 22 mmol ) in tetrachloromethane ( 62 ml ) was added n - bromosuccinimide ( 96 %, 1 . 15 g , 6 . 20 mmol ), followed by 2 , 2 ′- azobisisobutyronitrile ( aibn ; 102 mg , 0 . 621 mmol ). the reaction mixture was heated to 75 ° c . while being irradiated with a 75 watt fluorescent light bulb . after 1 hour , the reaction mixture was cooled to 0 ° c . and filtered ; the filtrate was concentrated in vacuo and purified via chromatography on silica gel ( eluent : 35 % ethyl acetate in heptane ) to afford the product as a light yellow solid . yield : 1 . 85 g , 4 . 62 mmol , 74 %. 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 52 ( s , 1h ), 8 . 37 ( s , 1h ), 7 . 92 ( d , j = 2 . 5 hz , 1h ), 7 . 71 ( d , j = 1 . 7 hz , 1h ), 7 . 68 ( br d , j = 8 . 7 hz , 2h ), 7 . 44 ( br d , j = 8 . 5 hz , 2h ), 6 . 46 ( dd , j = 2 . 4 , 1 . 9 hz , 1h ), 6 . 35 ( s , 1h ), 4 . 47 ( q , j = 7 . 1 hz , 2h ), 2 . 35 ( s , 3h ), 1 . 43 ( t , j = 7 . 1 hz , 3h ). water ( 7 ml ) was added to a solution of c48 ( 1 . 15 g , 2 . 87 mmol ) in acetone ( 7 ml ); the resulting white suspension was allowed to stir at room temperature for three hours . the reaction mixture was partitioned between water and ethyl acetate , and the organic layer was dried over magnesium sulfate , filtered , and concentrated in vacuo . silica gel chromatography ( gradient : 50 % to 100 % ethyl acetate in heptane ) afforded the product as a white solid . yield : 706 mg , 2 . 09 mmol , 73 %. lcms m / z 338 . 1 [ m + h ] + . 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 44 ( s , 1h ), 8 . 34 - 8 . 40 ( m , 1h ), 7 . 83 - 7 . 87 ( m , 1h ), 7 . 67 - 7 . 71 ( m , 1h ), 7 . 52 - 7 . 59 ( m , 2h ), 7 . 25 - 7 . 32 ( m , 2h ), 6 . 42 - 6 . 46 ( m , 1h ), 5 . 92 ( s , 1h ), 4 . 46 ( q , j = 7 hz , 2h ), 2 . 16 ( s , 3h ), 1 . 43 ( t , j = 7 hz , 3h ). 1 , 1 , 2 , 2 , 3 , 3 , 4 , 4 , 4 - nonafluorobutane - 1 - sulfonyl fluoride ( 1 . 36 ml , 7 . 57 mmol ) and triethylamine trihydrofluoride ( 1 . 24 ml , 7 . 61 mmol ) were added to a solution of c49 ( 1 . 28 g , 3 . 79 mmol ) in acetonitrile ( 7 . 6 ml ). n , n - diisopropylethylamine ( 4 . 0 ml , 23 mmol ) was then introduced , and the reaction mixture was stirred at room temperature for 1 hour . after the reaction had been quenched , via addition of saturated aqueous sodium bicarbonate solution , the mixture was extracted with ethyl acetate ; the organic layer was dried over magnesium sulfate , filtered , and concentrated under reduced pressure . silica gel chromatography ( gradient : 0 % to 100 % ethyl acetate in heptane ) provided the product as a yellow oil . yield : 832 mg , 2 . 45 mmol , 65 %. lcms m / z 340 . 4 [ m + h ] + . 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 54 ( s , 1h ), 8 . 32 ( s , 1h ), 7 . 91 - 7 . 95 ( m , 1h ), 7 . 68 - 7 . 76 ( m , 3h ), 7 . 33 - 7 . 40 ( m , 2h ), 6 . 57 ( d , j hf = 47 hz , 1h ), 6 . 45 - 6 . 49 ( m , 1h ), 4 . 49 ( q , j = 7 hz , 2h ), 2 . 21 ( s , 3h ), 1 . 45 ( t , j = 7 hz , 3h ). 1 , 3 , 4 , 6 , 7 , 8 - hexahydro - 2h - pyrimido [ 1 , 2 - a ] pyrimidine ( 95 %, 289 mg , 1 . 97 mmol ) was added to a solution of c50 ( 394 mg , 1 . 16 mmol ) and p1 ( 377 mg , 1 . 16 mmol ) in n , n - dimethylformamide ( 2 . 3 ml ). the reaction mixture was heated to 75 ° c . overnight , whereupon it was cooled and partitioned between water and ethyl acetate . the aqueous layer was extracted with ethyl acetate , and the combined organic layers were washed with saturated aqueous sodium chloride solution , dried over magnesium sulfate , filtered , and concentrated in vacuo . the component diastereomers were separated using supercritical fluid chromatography [ column : chiral technologies chiralpak ic , 5 μm ; mobile phase : 3 : 2 carbon dioxide /( 25 % methanol in ethyl acetate )]. the first - eluting enantiomer was 55 , obtained as an off - white solid , which exhibited a positive (+) rotation . yield : 140 mg , 0 . 341 mmol , 29 %. lcms m / z 411 . 5 [ m + h ] + . 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 41 ( s , 1h ), 8 . 36 ( s , 1h ), 8 . 14 ( br d , j = 6 . 4 hz , 1h ), 7 . 94 ( d , j = 2 . 4 hz , 1h ), 7 . 71 - 7 . 76 ( m , 3h ), 7 . 37 - 7 . 41 ( m , 2h ), 6 . 58 ( d , j hf = 47 . 1 hz , 1h ), 6 . 49 ( dd , j = 2 . 4 , 1 . 8 hz , 1h ), 4 . 11 ( dd , j = 11 . 5 , 5 . 0 hz , 1h ), 3 . 95 - 4 . 05 ( m , 2h ), 3 . 66 ( ddd , j = 9 . 6 , 9 . 5 , 5 . 0 hz , 1h ), 3 . 50 ( ddd , j = 11 . 9 , 11 . 9 , 2 . 2 hz , 1h ), 3 . 25 ( dd , j = 11 . 3 , 10 . 0 hz , 1h ), 2 . 24 ( s , 3h ), 2 . 03 - 2 . 10 ( m , 1h ), 1 . 76 - 1 . 88 ( m , 1h ). this material was taken up in hot ethyl acetate and allowed to cool slowly until crystals were observed ; one of these crystals of 55 was analyzed via x - ray crystallography ( see below ); this provided the relative configurations of the stereocenters in 55 . because the absolute configurations of the stereocenters in the ( 3r , 4s )- 4 - aminotetrahydro - 2h - pyran - 3 - ol moiety are known ( see the single crystal x - ray determination of p1 above ), the absolute configuration at the benzylic fluorine of 55 is thus established as shown . the later - eluting diastereomer from the separation was therefore assigned as 56 ; this product was obtained as a light yellow oil . yield : 143 mg , 0 . 348 mmol , 30 %. lcms m / z 411 . 5 [ m + h ] + . 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 40 ( s , 1h ), 8 . 36 ( s , 1h ), 8 . 13 ( br d , j = 6 hz , 1h ), 7 . 94 ( d , j = 2 . 5 hz , 1h ), 7 . 70 - 7 . 75 ( m , 3h ), 7 . 36 - 7 . 41 ( m , 2h ), 6 . 58 ( d , j hf = 47 . 1 hz , 1h ), 6 . 49 ( dd , j = 2 . 4 , 1 . 8 hz , 1h ), 4 . 11 ( dd , j = 11 . 4 , 4 . 8 hz , 1h ), 3 . 95 - 4 . 05 ( m , 2h ), 3 . 66 ( ddd , j = 9 . 6 , 9 . 4 , 5 . 0 hz , 1h ), 3 . 50 ( ddd , j = 11 . 9 , 11 . 9 , 2 . 2 hz , 1h ), 3 . 25 ( dd , j = 11 . 4 , 9 . 8 hz , 1h ), 2 . 24 ( s , 3h ), 2 . 03 - 2 . 10 ( m , 1h ), 1 . 82 ( dddd , j = 13 , 12 , 12 , 4 . 7 hz , 1h ). this material was dissolved in dichloromethane and slowly concentrated , providing an off - white solid that exhibited a negative (−) rotation . data collection was performed on a bruker apex diffractometer at room temperature . data collection consisted of omega and phi scans . the structure was solved by direct methods using shelx software suite in the space group p2 1 2 1 2 1 . the structure was subsequently refined by the full - matrix least squares method . all non - hydrogen atoms were found and refined using anisotropic displacement parameters . the hydrogen atom located on nitrogen was found from the fourier difference map and refined with distance restrained . the remaining hydrogen atoms were placed in calculated positions and were allowed to ride on their carrier atoms . the final refinement included isotropic displacement parameters for all hydrogen atoms . the absolute configuration of the benzylic fluorine atom was determined in relation to the known stereocenters of the ( 3r , 4s )- 4 - aminotetrahydro - 2h - pyran - 3 - ol moiety ( see the x - ray structure of p1 above ). the final r - index was 3 %. a final difference fourier revealed no missing or misplaced electron density . pertinent crystal , data collection and refinement information is summarized in table e55 - 1 . atomic coordinates , bond lengths , bond angles , and displacement parameters are listed in tables e55 - 2 to e55 - 5 . platon , a . l . spek , j . appl . cryst . 2003 , 36 , 7 - 13 . mercury , c . f . macrae , p . r . edington , p . mccabe , e . pidcock , g . p . shields , r . taylor , m . towler , and j . van de streek , j . appl . cryst . 2006 , 39 , 453 - 457 . olex2 , o . v . dolomanov , l . j . bourhis , r . j . gildea , j . a . k . howard , and h . puschmann , j . appl . cryst . 2009 , 42 , 339 - 341 . parameters ( å 2 × 10 3 ) for 55 . u ( eq ) is defined as one third anisotropic displacement parameters ( å 2 × 10 3 ) for 55 . form : − 2π 2 [ h 2 a * 2 u 11 + . . . + 2 h k a * b * u 12 ]. triethylamine ( 27 . 1 g , 268 mmol ) and tert - butyl ( dimethyl ) silyl trifluoromethanesulfonate ( 53 g , 200 mmol ) were added to a solution of ( 4 - bromophenyl ) methanol ( 25 . 0 g , 133 mmol ) in dichloromethane ( 500 ml ), and the reaction mixture was stirred at 15 ° c . for 18 hours . after the addition of saturated aqueous ammonium chloride solution ( 500 ml ), the mixture was extracted with dichloromethane ( 2 × 300 ml ), and the combined organic layers were dried over sodium sulfate , filtered , and concentrated in vacuo . chromatography on silica gel ( eluent : petroleum ether ) provided the product as a colorless oil . yield : 34 . 6 g , 115 mmol , 86 %. 1 h nmr ( 400 mhz , cdcl 3 ) δ 7 . 46 ( d , j = 8 . 4 hz , 2h ), 7 . 21 ( d , j = 8 . 4 hz , 2h ), 4 . 70 ( s , 2h ), 0 . 95 ( s , 9h ), 0 . 11 ( s , 6h ). to a − 78 ° c . solution of c51 ( 10 . 0 g , 33 . 2 mmol ) in tetrahydrofuran ( 120 ml ) was added n - butyllithium ( 2 . 5 m in hexanes , 15 . 9 ml , 39 . 8 mmol ). after the reaction mixture had stirred at − 78 ° c . for one hour , a solution of 2 - chloro - n - methoxy - n - methylacetamide ( 5 . 48 g , 39 . 8 mmol ) in tetrahydrofuran ( 100 ml ) was added in a drop - wise manner , while the reaction mixture was maintained at − 78 ° c . stirred was continued at − 40 ° c . to − 50 ° c . for 1 hour , whereupon the reaction was quenched by addition of saturated aqueous ammonium chloride solution ( 200 ml ) at − 40 ° c . to − 20 ° c . the aqueous phase was extracted with ethyl acetate ( 3 × 200 ml ), and the combined organic layers were dried over sodium sulfate , filtered , and concentrated under reduced pressure . the residue was purified by silica gel chromatography ( gradient : 1 % to 15 % ethyl acetate in petroleum ether ) to provide the product as a colorless gum , which became a white solid upon standing . yield : 8 . 50 g , 28 . 4 mmol , 86 %. 1 h nmr ( 400 mhz , cdcl 3 ) δ 7 . 94 ( d , j = 8 . 3 hz , 2h ), 7 . 46 ( d , j = 8 . 0 hz , 2h ), 4 . 81 ( s , 2h ), 4 . 72 ( s , 2h ), 0 . 96 ( s , 9h ), 0 . 12 ( s , 6h ). step 3 . synthesis of [ 4 -( 1 , 3 - oxazol - 4 - yl ) phenyl ] methanol ( c53 ), 4 -[ 4 -({[ tert - butyl ( dimethyl ) silyl ] oxy } methyl ) phenyl ]- 1 , 3 - oxazole ( c54 ), and 4 -( 1 , 3 - oxazol - 4 - yl ) benzyl formate ( c55 ) a solution of c52 ( 3 . 50 g , 11 . 7 mmol ) in formamide ( 20 ml ) was heated at 100 ° c . for 18 hours . after the reaction mixture had cooled , saturated aqueous sodium bicarbonate solution ( 50 ml ) was added , and the mixture was extracted with ethyl acetate ( 3 × 50 ml ). the combined organic layers were concentrated in vacuo and purified via silica gel chromatography ( gradient : 0 % to 50 % ethyl acetate in petroleum ether ) to provide the three products . compound c53 was obtained as a yellow solid . yield : 300 mg , 1 . 7 mmol , 14 %. 1 h nmr ( 400 mhz , cdcl 3 ) δ 7 . 94 ( s , 1h ), 7 . 92 ( s , 1h ), 7 . 71 ( d , j = 8 . 2 hz , 2h ), 7 . 39 ( d , j = 8 . 2 hz , 2h ), 4 . 70 ( s , 2h ). compound c54 was isolated as a red gum . yield : 200 mg , 0 . 69 mmol , 6 %. 1 h nmr ( 400 mhz , cdcl 3 ) δ 7 . 94 ( s , 2h ), 7 . 73 ( br d , j = 8 . 3 hz , 2h ), 7 . 38 ( br d , j = 8 hz , 2h ), 4 . 78 ( s , 2h ), 0 . 96 ( s , 9h ), 0 . 12 ( s , 6h ). compound c55 was obtained as a red solid . yield : 600 mg , 3 . 0 mmol , 26 %. 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 17 ( t , j = 0 . 8 hz , 1h ), 7 . 98 ( d , j = 0 . 9 hz , 1h ), 7 . 96 ( d , j = 0 . 8 hz , 1h ), 7 . 78 ( br d , j = 8 . 4 hz , 2h ), 7 . 44 ( br d , j = 8 hz , 2h ), 5 . 24 ( s , 2h ). tetraethylammonium fluoride hydrate ( 347 mg , 2 . 07 mmol ) was added to a solution of c54 ( 400 mg , 1 . 4 mmol ) in tetrahydrofuran ( 6 ml ), and the reaction mixture was stirred at 50 ° c . for 3 hours . after the solvent had been removed under reduced pressure , the residue was subjected to silica gel chromatography ( gradient : 0 % to 50 % ethyl acetate in petroleum ether ) to provide the product as a yellow solid . yield : 180 mg , 1 . 0 mmol , 71 %. lcms m / z 175 . 8 [ m + h ] + . to a solution of c55 ( 1 . 1 g , 5 . 4 mmol ) in a mixture of tetrahydrofuran and water ( 1 : 1 , 10 ml ) was added sodium hydroxide ( 433 mg , 10 . 8 mmol ). the reaction mixture was stirred at 18 ° c . for 1 hour , whereupon it was extracted with ethyl acetate ( 3 × 5 ml ). the combined organic layers were washed with saturated aqueous sodium chloride solution , concentrated in vacuo , and purified using chromatography on silica gel ( gradient : 0 % to 50 % ethyl acetate in petroleum ether ) to afford the product as a yellow solid . yield : 820 mg , 4 . 7 mmol , 87 %. lcms m / z 175 . 8 [ m + h ] + . 1 h nmr ( 400 mhz , cdcl 3 ) δ 7 . 97 ( s , 1h ), 7 . 96 ( s , 1h ), 7 . 76 ( d , j = 8 . 2 hz , 2h ), 7 . 44 ( d , j = 7 . 9 hz , 2h ), 4 . 74 ( s , 2h ). thionyl chloride ( 2850 mg , 24 . 0 mmol ) was added drop - wise to a solution of c53 ( 1 . 40 g , 7 . 99 mmol ) in chloroform ( 10 ml ) maintained in a water bath . the reaction mixture was stirred for 1 hour at 25 ° c ., whereupon it was concentrated in vacuo to afford the product as a yellow solid . yield : 1 . 50 g , 6 . 52 mmol , 82 %. lcms m / z 193 . 8 [ m + h ] + . 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 03 ( s , 1h ), 7 . 99 ( s , 1h ), 7 . 77 ( d , j = 8 . 2 hz , 2h ), 7 . 46 ( d , j = 7 . 9 hz , 2h ), 4 . 63 ( s , 2h ). compound c10 ( 90 . 2 mg , 0 . 310 mmol ), [ 1 , 1 ′- bis ( diphenylphosphino ) ferrocene ] dichloropalladium ( ii ) ( 18 . 9 mg , 25 . 8 μmol ), and potassium carbonate ( 71 . 4 mg , 0 . 517 mmol ) were added to a solution of c56 ( 50 mg , 0 . 22 mmol ) in a mixture of 1 , 4 - dioxane ( 2 ml ) and water ( 0 . 2 ml ). the mixture was degassed with nitrogen for 5 minutes , whereupon it was heated to 100 ° c . for 18 hours . the reaction solution was taken directly into the following step . lcms m / z 344 . 9 [ m + na + ]. to a solution of c57 ( from the previous step , plus a second small - scale reaction , ≦ 0 . 26 mmol ) in 1 , 4 - dioxane ( 2 . 5 ml ) were added water ( 2 . 5 ml ) and sodium hydroxide ( 49 . 6 mg , 1 . 24 mmol ); the reaction mixture was stirred for 20 hours at 25 ° c ., then extracted with petroleum ether ( 3 ml ). the aqueous layer was filtered , and the filtrate was acidified to ph 3 - 5 via addition of 2 m aqueous hydrochloric acid . it was then extracted with dichloromethane ( 3 × 10 ml ), and the combined dichloromethane layers were dried over sodium sulfate , filtered , and concentrated in vacuo to afford the product as an off - white solid . yield : 62 mg , 0 . 21 mmol , 81 % over 2 steps . lcms m / z 294 . 9 [ m + h ] + . 1 -[ 3 -( dimethylamino ) propyl ]- 3 - ethylcarbodiimide hydrochloride ( edci ; 56 . 5 mg , 0 . 295 mmol ), 1h - benzotriazol - 1 - ol ( 42 . 7 mg , 0 . 316 mmol ), and triethylamine ( 64 . 0 mg , 0 . 632 mmol ) were added to a solution of c58 ( 62 mg , 0 . 21 mmol ) in a mixture of dichloromethane ( 5 ml ) and n , n - dimethylformamide ( 3 ml ). the mixture was stirred for 4 hours at 25 ° c ., whereupon p2 ( 29 . 6 mg , 0 . 253 mmol ) was added and stirring was continued for 18 hours at 25 ° c . additional 1 -[ 3 -( dimethylamino ) propyl ]- 3 - ethylcarbodiimide hydrochloride ( 56 . 5 mg , 0 . 295 mmol ), 1h - benzotriazol - 1 - ol ( 42 . 7 mg , 0 . 316 mmol ), and triethylamine ( 64 . 0 mg , 0 . 632 mmol ) were introduced , and the reaction mixture was stirred for another 30 minutes ; additional p2 ( 29 . 6 mg , 0 . 253 mmol ) was then added , and stirring was carried out for another 18 hours at 25 ° c . the reaction mixture was diluted with dichloromethane ( 20 ml ), washed sequentially with saturated aqueous citric acid solution ( 20 ml ) and aqueous sodium hydroxide solution ( 1 m , 20 ml ), and concentrated in vacuo . the residue was subjected to preparative thin layer chromatography on silica gel ( eluent : 1 : 2 petroleum ether / ethyl acetate ), followed by reversed phase hplc purification ( column : phenomenex gemini c18 , 5 μm ; mobile phase a : water containing 0 . 225 % formic acid ; mobile phase b : acetonitrile containing 0 . 225 % formic acid ; gradient : 23 % to 43 % b ). the product was obtained as a white solid . yield : 20 mg , 51 μmol , 24 %. lcms m / z 394 . 1 [ m + h ] + . 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 32 ( s , 1h ), 8 . 12 ( br d , j = 6 hz , 1h ), 8 . 00 ( s , 1h ), 7 . 92 - 7 . 96 ( m , 2h ), 7 . 68 ( d , j = 8 . 2 hz , 2h ), 7 . 17 ( d , j = 8 . 2 hz , 2h ), 4 . 33 - 4 . 46 ( br m , 1h ), 4 . 09 ( dd , j = 12 , 5 hz , 1h ), 4 . 06 ( s , 2h ), 3 . 90 - 4 . 04 ( m , 2h ), 3 . 59 - 3 . 68 ( m , 1h ), 3 . 43 - 3 . 52 ( m , 1h ), 3 . 23 ( dd , j = 10 . 9 , 10 . 2 hz , 1h ), 2 . 32 ( s , 3h ), 2 . 00 - 2 . 08 ( m , 1h ), 1 . 74 - 1 . 87 ( m , 1h ). a mixture of 5 - methoxy - 4 - oxo - 1 , 4 - dihydropyridine - 2 - carboxylic acid ( 30 . 0 g , 177 mmol ) and thionyl chloride ( 250 ml ) was stirred at 100 ° c . for 18 hours , whereupon the reaction mixture was concentrated in vacuo . the residue was dissolved in anhydrous ethanol ( 200 ml ); the resulting solution was heated at reflux for 20 minutes and then cooled to 20 ° c . after the mixture had been neutralized by addition of anhydrous sodium carbonate , it was filtered . the filtrate was cooled in an ice - ethanol bath , and stirred for 30 minutes ; the precipitate was collected via filtration to afford the product as an off - white solid . the resulting filtrate was concentrated to a smaller volume under reduced pressure and cooled in an ice - ethanol bath . the precipitate was collected via filtration , providing additional product . combined yield : 14 . 2 g , 65 . 8 mmol , 37 %. lcms m / z 215 . 8 [ m + h ] + . 1 h nmr ( 400 mhz , dmso - d 6 ) δ 8 . 58 ( s , 1h ), 8 . 09 ( s , 1h ), 4 . 32 ( q , j = 7 . 1 hz , 2h ), 4 . 08 ( s , 3h ), 1 . 32 ( t , j = 7 . 1 hz , 3h ). a mixture of c59 ( 100 mg , 0 . 46 mmol ), 4 , 4 , 4 ′, 4 ′, 5 , 5 , 5 ′, 5 ′- octamethyl - 2 , 2 ′- bi - 1 , 3 , 2 - dioxaborolane ( 177 mg , 0 . 697 mmol ), potassium acetate ( 114 mg , 1 . 16 mmol ), and [ 1 , 1 ′- bis ( diphenylphosphino ) ferrocene ] dichloropalladium ( 11 ) ( 33 . 9 mg , 46 . 3 μmol ) in toluene ( 10 ml ) was stirred at 130 ° c . for 18 hours . the reaction mixture was used directly in the following step . lcms m / z 225 . 9 [ m + h ] + . 1 , 4 - dioxane ( 10 ml ) and water ( 2 ml ) were added to c60 ( as a toluene solution from the previous step , ≦ 0 . 46 mmol ). compound c28 ( 169 mg , 0 . 692 mmol ), [ 1 , 1 ′- bis ( diphenylphosphino ) ferrocene ] dichloropalladium ( 11 ) ( 33 . 8 mg , 46 . 2 μmol ), and potassium carbonate ( 160 mg , 1 . 16 mmol ) were then introduced , and the reaction mixture was stirred at 80 ° c . for 4 hours . after removal of solvents in vacuo , the residue was purified by preparative thin layer chromatography on silica gel ( eluent : 1 : 1 petroleum ether / ethyl acetate ), affording the product as a light yellow gum . yield : 150 mg , 0 . 426 mmol , 93 % over two steps . lcms m / z 353 . 0 [ m + h ] + . 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 33 ( s , 1h ), 7 . 91 ( s , 1h ), 7 . 78 ( s , 1h ), 7 . 64 ( d , j = 8 . 3 hz , 2h ), 7 . 23 ( d , j = 8 . 0 hz , 2h ), 4 . 43 ( q , j = 7 . 1 hz , 2h ), 4 . 01 ( s , 2h ), 4 . 00 ( s , 3h ), 2 . 52 ( s , 3h ), 1 . 42 ( t , j = 7 . 1 hz , 3h ). sodium hydroxide ( 32 mg , 0 . 80 mmol ) and c61 ( 150 mg , 0 . 426 mmol ) were combined in a mixture of methanol ( 3 ml ) and water ( 3 ml ) and stirred at 30 ° c . for 2 hours . the reaction mixture was then acidified to ph 2 via addition of 1 m aqueous hydrochloric acid . removal of solvent in vacuo afforded the product as a light yellow gum . yield : 130 mg , 0 . 40 mmol , 95 %. lcms m / z 324 . 9 [ m + h ] + . to a solution of c62 ( 65 mg , 0 . 20 mmol ) in dichloromethane ( 3 ml ) were added triethylamine ( 77 μl , 0 . 55 mmol ), 1 -[ 3 -( dimethylamino ) propyl ]- 3 - ethylcarbodiimide hydrochloride ( 53 . 0 mg , 0 . 277 mmol ), and 1h - benzotriazol - 1 - ol ( 37 . 4 mg , 0 . 277 mmol ). after the reaction mixture had been stirred at 10 ° c . for 1 hour , p2 ( 30 . 2 mg , 0 . 258 mmol ) was added , and stirring was continued at 10 ° c . for 16 hours . it was then warmed to 30 ° c . for another 5 hours , whereupon it was treated with o -( 7 - azabenzotriazol - 1 - yl )- n , n , n ′, n ′- tetramethyluronium hexafluorophosphate ( 40 mg , 0 . 11 mmol ). after 1 hour , the reaction mixture was filtered through amberlyst ® a - 26 ( hydroxide form ) ion exchange resin ; the filtrate was concentrated in vacuo and purified via reversed phase hplc ( column : agela durashell c18 , 5 μm ; mobile phase a : water containing 0 . 225 % formic acid ; mobile phase b : acetonitrile ; gradient : 28 % to 48 %). the product was isolated as a white solid . yield : 7 . 0 mg , 8 %. lcms m / z 445 . 9 [ m + n + ]. 1 h nmr ( 400 mhz , cd 3 od ) δ 8 . 31 ( s , 1h ), 8 . 10 ( s , 1h ), 7 . 85 ( s , 1h ), 7 . 64 ( br d , j = 8 . 2 hz , 2h ), 7 . 27 ( br d , j = 8 . 2 hz , 2h ), 4 . 04 ( s , 2h ), 4 . 03 ( s , 3h ), 3 . 86 - 3 . 99 ( m , 3h ), 3 . 58 - 3 . 66 ( m , 1h ), 3 . 42 - 3 . 51 ( m , 1h ), 3 . 18 ( dd , j = 10 . 7 , 10 . 2 hz , 1h ), 2 . 49 ( s , 3h ), 1 . 96 - 2 . 04 ( m , 1h ), 1 . 62 - 1 . 75 ( m , 1h ). [ 4 -( hydroxymethyl ) phenyl ] boronic acid ( 96 %, 4 . 0 g , 25 mmol ) and 4 - bromo - 1 , 3 - thiazole ( 96 %, 6 . 48 g , 37 . 9 mmol ) were dissolved in 1 , 4 - dioxane ( 75 ml ). aqueous potassium carbonate solution ( 3 m , 17 ml , 51 mmol ) was added , followed by tetrakis ( triphenylphosphine ) palladium ( 0 ) ( 880 mg , 0 . 76 mmol ), and the reaction mixture was heated overnight at 100 ° c . it was then cooled to room temperature , diluted with water , and extracted several times with ethyl acetate . the combined organic layers were washed with saturated aqueous sodium chloride solution , dried over magnesium sulfate , filtered , and concentrated under reduced pressure . purification via chromatography on silica gel ( gradient : 25 % to 50 % ethyl acetate in heptane ) afforded the product as a cream - colored solid . yield : 3 . 60 g , 18 . 8 mmol , 75 %. lcms m / z 192 . 0 [ m + h ] + . 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 92 ( d , j = 2 . 0 hz , 1h ), 7 . 95 ( br d , j = 8 . 2 hz , 2h ), 7 . 56 ( d , j = 2 . 0 hz , 1h ), 7 . 46 ( br d , j = 8 . 3 hz , 2h ), 4 . 76 ( s , 2h ). to a solution of c63 ( 2 . 00 g , 10 . 5 mmol ) in acetonitrile ( 40 ml ) were added 1 , 1 , 2 , 2 , 3 , 3 , 4 , 4 , 4 - nonafluorobutane - 1 - sulfonyl fluoride ( 2 . 1 ml , 11 . 7 mmol ) and triethylamine trihydrofluoride ( 1 . 88 ml , 11 . 5 mmol ), followed by n , n - diisopropylethylamine ( 3 . 64 ml , 20 . 9 mmol ). the reaction mixture was stirred for six hours , whereupon the reaction was quenched via addition of saturated aqueous sodium bicarbonate solution . the mixture was extracted several times with ethyl acetate , and the combined organic layers were dried over magnesium sulfate , filtered , and concentrated in vacuo . chromatography on silica gel ( eluent : 10 % ethyl acetate in heptane , followed by 25 % ethyl acetate in heptane ) provided the product as a white solid . yield : 800 mg , 4 . 1 mmol , 39 %. 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 93 ( s , 1h ), 7 . 98 ( d , j = 8 . 1 hz , 2h ), 7 . 58 - 7 . 61 ( m , 1h ), 7 . 47 ( d , j = 7 . 5 hz , 2h ), 5 . 43 ( d , j hf = 47 . 7 hz , 2h ). n - bromosuccinimide ( 96 %, 1 . 16 g , 6 . 26 mmol ) was added to a solution of c64 ( 1 . 10 g , 5 . 69 mmol ) in tetrachloromethane ( 40 ml ). 2 , 2 ′- azobisisobutyronitrile ( 96 %, 97 mg , 0 . 57 mmol ) was added , and the reaction mixture was heated at reflux for two hours . after it had been cooled to room temperature , the reaction mixture was quenched with water , and extracted several times with dichloromethane . the combined organic layers were washed with saturated aqueous sodium chloride solution , dried over magnesium sulfate , filtered , and concentrated in vacuo . silica gel chromatography ( eluent : 10 % ethyl acetate in heptane ) afforded the product as a light pink solid ( 1 . 25 g ). by 1 h nmr analysis , this material was contaminated with a small amount of unreacted c64 . yield , corrected for c64 remaining in the isolated product : 1 . 08 g , 3 . 97 mmol , 70 %. 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 92 ( d , j = 2 . 0 hz , 1h ), 7 . 98 - 8 . 03 ( m , 2h ), 7 . 63 ( d , j = 2 . 0 hz , 1h ), 7 . 57 - 7 . 61 ( m , 2h ), 7 . 46 ( d , j hf = 49 . 4 hz , 1h ). 1 , 4 - dioxane ( 10 ml ) was added to a mixture of c10 ( 400 mg , 1 . 37 mmol ), c65 ( 449 mg , 1 . 65 mmol ), and tetrakis ( triphenylphosphine ) palladium ( 0 ) ( 159 mg , 0 . 138 mmol ) in a sealable reaction vessel . aqueous cesium carbonate solution ( 3 m , 1 . 4 ml , 4 . 2 mmol ) was introduced , the reaction vessel was sealed , and the reaction mixture was heated at 50 ° c . for two hours . after the reaction mixture had cooled to room temperature , it was diluted with ethyl acetate , washed sequentially with water and with saturated aqueous sodium chloride solution , dried over magnesium sulfate , filtered , and concentrated in vacuo . purification via silica gel chromatography ( eluent : 25 % ethyl acetate in heptane , followed by 50 % and then 75 % ethyl acetate in heptane ) provided the product as a yellow oil . yield : 350 mg , 0 . 98 mmol , 72 %. lcms m / z 357 . 4 [ m + h ] + . 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 89 ( d , j = 2 . 0 hz , 1h ), 8 . 55 - 8 . 56 ( m , 1h ), 8 . 35 ( s , 1h ), 7 . 94 - 7 . 98 ( m , 2h ), 7 . 59 ( d , j = 2 . 0 hz , 1h ), 7 . 34 - 7 . 39 ( m , 2h ), 6 . 59 ( d , j hf = 47 . 1 hz , 1h ), 4 . 51 ( qd , j = 7 . 1 , 0 . 6 hz , 2h ), 2 . 23 ( s , 3h ), 1 . 47 ( t , j = 7 . 1 hz , 3h ). step 5 . synthesis of (+)- 4 -{ fluoro [ 4 -( 1 , 3 - thiazol - 4 - yl ) phenyl ] methyl }- n -[( 3r , 4s )- 3 - hydroxytetrahydro - 2h - pyran - 4 - yl ]- 5 - methylpyridine - 2 - carboxamide ( diastereomer 1 ) ( 59 ) and ( )-{ fluoro [ 4 -( 1 , 3 - thiazol - 4 - yl ) phenyl ] methyl }- n -[( 3r , 4s )- 3 - hydroxytetrahydro - 2h - pyran - 4 - yl ]- 5 - methylpyridine - 2 - carboxamide ( diastereomer 2 ) ( 60 ) a mixture of c66 ( 350 mg , 0 . 98 mmol ), p1 ( 414 mg , 1 . 28 mmol ), and 1 , 3 , 4 , 6 , 7 , 8 - hexahydro - 2h - pyrimido [ 1 , 2 - a ] pyrimidine ( 98 %, 237 mg , 1 . 67 mmol ) in n , n - dimethylformamide ( 5 ml ) was stirred at 60 ° c . overnight . the reaction mixture was diluted with water and extracted several times with ethyl acetate . the combined organic extracts were washed sequentially with saturated aqueous sodium bicarbonate solution and saturated aqueous sodium chloride solution , dried over magnesium sulfate , filtered , and concentrated under reduced pressure . the residue was subjected to chromatography on silica gel ( gradient : 75 % to 100 % ethyl acetate in heptane ) to afford the racemic product as a colorless oil , which slowly solidified upon standing . yield : 350 mg , 0 . 82 mmol , 84 %. this material was separated into its component diastereomers using supercritical fluid chromatography ( column : chiral technologies chiralcel od - h , 5 μm ; mobile phase : 65 : 35 carbon dioxide / methanol ). the first - eluting diastereomer was 59 ( diastereomer 1 ), isolated as a solid ; this material exhibited a positive (+) rotation . yield : 120 mg , 0 . 281 mmol , 34 % for the purification . lcms m / z 428 . 5 [ m + h ] + . 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 89 ( d , j = 2 . 0 hz , 1h ), 8 . 43 ( s , 1h ), 8 . 35 - 8 . 36 ( m , 1h ), 8 . 16 ( br d , j = 6 hz , 1h ), 7 . 94 - 7 . 98 ( m , 2h ), 7 . 59 ( d , j = 2 . 0 hz , 1h ), 7 . 35 - 7 . 40 ( m , 2h ), 6 . 59 ( d , j hf = 47 . 1 hz , 1h ), 4 . 11 ( br dd , j = 11 . 4 , 5 . 0 hz , 1h ), 3 . 95 - 4 . 05 ( m , 2h ), 3 . 67 ( ddd , j = 9 . 7 , 9 . 4 , 5 . 0 hz , 1h ), 3 . 50 ( ddd , j = 11 . 9 , 11 . 9 , 2 . 2 hz , 1h ), 3 . 25 ( dd , j = 11 . 4 , 9 . 9 hz , 1h ), 2 . 25 ( s , 3h ), 2 . 04 - 2 . 11 ( m , 1h ), 1 . 82 ( dddd , j = 13 , 12 , 12 , 5 hz , 1h ). the second - eluting product was 60 ( diastereomer 2 ), obtained as a colorless oil that slowly solidified . this material exhibited a negative (−) rotation . yield : 120 mg , 0 . 281 mmol , 34 % for the purification . lcms m / z 428 . 5 [ m + h ] + . 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 89 ( d , j = 2 . 0 hz , 1h ), 8 . 41 ( s , 1h ), 8 . 35 ( s , 1h ), 8 . 17 ( br d , j = 6 hz , 1h ), 7 . 95 ( br d , j = 8 hz , 2h ), 7 . 58 ( d , j = 2 . 0 hz , 1h ), 7 . 34 - 7 . 39 ( m , 2h ), 6 . 58 ( d , j hf = 47 . 1 hz , 1h ), 4 . 11 ( br dd , j = 11 . 4 , 5 . 1 hz , 1h ), 3 . 95 - 4 . 05 ( m , 2h ), 3 . 67 ( ddd , j = 9 . 6 , 9 . 5 , 5 . 0 hz , 1h ), 3 . 49 ( ddd , j = 11 . 9 , 11 . 9 , 2 . 2 hz , 1h ), 3 . 25 ( dd , j = 11 . 4 , 9 . 9 hz , 1h ), 2 . 24 ( s , 3h ), 2 . 03 - 2 . 10 ( m , 1h ), 1 . 75 - 1 . 87 ( m , 1h ). a mixture of 4 - bromo - 1 , 3 - dimethyl - 1h - pyrazole ( 200 mg , 1 . 14 mmol ), [ 4 -( hydroxymethyl ) phenyl ] boronic acid ( 260 mg , 1 . 71 mmol ), potassium carbonate ( 474 mg , 3 . 43 mmol ) and tetrakis ( triphenylphosphine ) palladium ( 0 ) ( 132 mg , 0 . 114 mmol ) in 1 , 4 - dioxane ( 12 ml ) and water ( 3 ml ) was heated at 100 ° c . for 16 hours . the reaction mixture was concentrated in vacuo ; purification using silica gel chromatography ( gradient : 0 % to 100 % ethyl acetate in petroleum ether ) provided the product ( 190 mg ) as a yellow solid . by 1 h nmr and mass spectroscopic analysis , this material was contaminated with triphenylphosphine oxide . yield , corrected for triphenylphospine oxide content : 120 mg , 0 . 59 mmol , 52 %. lcms m / z 202 . 9 [ m + h ] + . 1 h nmr ( 400 mhz , cdcl 3 ), product peaks only : δ 7 . 43 ( s , 1h ), 7 . 39 ( br s , 4h ), 4 . 72 ( s , 2h ), 3 . 89 ( s , 3h ), 2 . 40 ( s , 3h ). thionyl chloride ( 1 . 0 ml , 14 mmol ) was added to a solution of c67 ( 280 mg ; when corrected for triphenylphospine oxide contamination : 180 mg , 0 . 9 mmol ) in chloroform ( 20 ml ), and the reaction mixture was stirred at 16 ° c . for 3 hours . removal of solvent in vacuo provided the crude product as a yellow solid ( 380 mg ). a portion of this material was used in the following step . potassium carbonate ( 161 mg , 1 . 16 mmol ) and [ 1 , 1 ′- bis ( diphenylphosphino ) ferrocene ] dichloropalladium ( ii ) ( 28 . 4 mg , 38 . 8 μmol ) were added to a solution of c68 ( from the previous step , 100 mg , 0 . 24 mmol ) and c10 ( 136 mg , 0 . 467 mmol ) in 1 , 4 - dioxane ( 18 ml ) and water ( 2 ml ). the reaction mixture was stirred at 80 ° c . for 8 hours , whereupon it was cooled to room temperature and filtered . the filtrate was concentrated to dryness under reduced pressure and purified via chromatography on silica gel ( gradient : 85 % to 100 % ethyl acetate in petroleum ether ), affording the product as a light yellow oil . yield : 60 mg , 0 . 17 mmol , 70 % over 2 steps . lcms m / z 349 . 9 [ m + h ] + . sodium hydroxide ( 27 . 5 mg , 0 . 688 mmol ) was added to a solution of c69 ( 60 mg , 0 . 17 mmol ) in a mixture of tetrahydrofuran ( 5 ml ) and water ( 5 ml ). the reaction mixture was stirred at 50 ° c . for 16 hours , then concentrated to dryness under reduced pressure to provide the product ( 74 mg ) as a light yellow oil ; this material was used in the following step without further purification . lcms m / z 321 . 9 [ m + h ] + . 1 -[ 3 -( dimethylamino ) propyl ]- 3 - ethylcarbodiimide hydrochloride ( 66 . 2 mg , 0 . 345 mmol ) and 1h - benzotriazol - 1 - ol ( 46 . 7 mg , 0 . 346 mmol ) were added to a solution of c70 ( from the previous step , 74 mg , ≦ 0 . 17 mmol ) in dichloromethane ( 3 ml ), and the reaction mixture was stirred at 18 ° c . for 1 hour . compound p2 ( 27 . 0 mg , 0 . 230 mmol ) was then introduced , and stirring was continued at 18 ° c . for 18 hours . o -( 7 - azabenzotriazol - 1 - yl )- n , n , n ′, n ′- tetramethyluronium hexafluorophosphate ( 131 mg , 0 . 344 mmol ) was then added , and stirring was continued at 18 ° c . for 20 hours . the reaction mixture was filtered and subjected to preparative thin layer chromatography on silica gel ( eluent : ethyl acetate ), then purified by reversed phase hplc purification ( column : agela durashell c18 , 5 μm ; mobile phase a : water containing 0 . 225 % formic acid ; mobile phase b : acetonitrile containing 0 . 225 % formic acid ; gradient : 25 % to 45 % b ). the product was obtained as a white solid . yield : 22 4 mg , 53 . 2 μmol , 31 % over 2 steps . lcms m / z 421 . 0 [ m + h ] + . 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 32 ( s , 1h ), 8 . 08 - 8 . 18 ( br m , 1h ), 8 . 00 ( s , 1h ), 7 . 40 ( s , 1h ), 7 . 30 ( br d , j = 7 . 8 hz , 2h ), 7 . 12 ( br d , j = 8 . 0 hz , 2h ), 4 . 04 ( s , 2h ), 3 . 90 - 4 . 13 ( m , 3h ), 3 . 88 ( s , 3h ), 3 . 58 - 3 . 69 ( m , 1h ), 3 . 42 - 3 . 53 ( m , 1h ), 3 . 23 ( dd , j = 10 . 5 , 10 . 4 hz , 1h ), 2 . 38 ( s , 3h ), 2 . 34 ( s , 3h ), 1 . 99 - 2 . 08 ( m , 1h ), 1 . 73 - 1 . 87 ( m , 1h ). table 6 - 1 below lists some additional examples of compounds of the invention ( examples 62 - 72 ) that were made using methods , starting materials or intermediates , and preparations described herein . examples 62 - 72 ( including method of preparation , non - commercial starting materials , structures and 1 h nmr ( 400 mhz , cd 3 od ) δ 8 . 48 ( s , 1h ), 8 . 20 ( d , j = 2 . 4 hz , 1h ), 8 . 00 ( s , 1h ), 7 . 67 - 7 . 72 ( m , 3h ), 7 . 38 ( br d , j = 8 . 7 hz , 2h ), 7 . 08 ( t , j hf = 72 . 7 hz , 1h ), 6 . 52 ( dd , j = 2 , 2 hz , 1h ), 4 . 17 ( s , 2h ), 3 . 87 - 3 . 99 ( m , 3h ), 3 . 60 - 3 . 67 ( m , 1h ), 3 . 42 - 3 . 51 ( m , 1h ), 3 . 18 ( dd , j = 11 , 10 hz , 1h ), 1 . 95 - 2 . 02 ( m , 1h ), 1 . 64 - 1 . 77 ( m , 1h ); 444 . 9 1 h nmr ( 600 mhz , dmso - d 6 ) δ 8 . 49 ( d , j = 2 . 4 hz , 1h ), 8 . 48 ( s , 1h ), 8 . 35 ( br d , j = 7 . 9 hz , 1h ), 8 . 14 ( s , 1h ), 7 . 90 ( d , j = 8 . 5 hz , 2h ), 7 . 74 - 7 . 76 ( m , 1h ), 7 . 47 ( br d , j = 8 hz , 2h ), 6 . 97 ( d , j hf = 46 . 2 hz , 1h ), 6 . 54 - 6 . 56 ( m , 1h ), 4 . 64 ( br d , j = 5 hz , 1h ), 3 . 56 - 3 . 64 ( m , 1h ), 3 . 42 - 3 . 50 ( m , 1h ), 2 . 21 ( s , 3h ), 1 . 86 - 1 . 96 ( m , 2h ), 1 . 58 - 1 . 69 ( m , 2h ), 1 . 19 - 1 . 36 ( m , 4h ); 409 . 4 1 h nmr ( 600 mhz , dmso - d 6 ) δ 8 . 50 ( d , j = 2 . 5 hz , 1h ), 8 . 48 ( s , 1h ), 8 . 36 ( br d , j = 8 . 0 hz , 1h ), 8 . 13 ( s , 1h ), 7 . 90 ( br d , j = 8 . 4 hz , 2h ), 7 . 74 - 7 . 76 ( m , 1h ), 7 . 48 ( br d , j = 8 . 3 hz , 2h ), 6 . 97 ( d , j hf = 46 . 3 hz , 1h ), 6 . 55 ( dd , j = 2 . 0 , 1 . 8 hz , 1h ), 4 . 66 ( d , j = 5 . 4 hz , 1h ), 3 . 56 - 3 . 63 ( m , 1h ), 3 . 43 - 3 . 50 ( m , 1h ), 2 . 21 ( s , 3h ), 1 . 87 - 1 . 97 ( m , 2h ), 1 . 59 - 1 . 68 ( m , 2h ), 1 . 21 - 1 . 33 ( m , 4h ); 409 . 3 8 . 38 ( br s , 1h ), 8 . 33 ( s , 1h ), 8 . 11 ( br d , j = 6 hz , 1h ), 7 . 99 ( s , 1h ), 7 . 92 ( s , 1h ), 7 . 90 ( s , 1h ), 7 . 34 - 7 . 41 ( m , 2h ), 4 . 28 - 4 . 37 ( br m , 1h ), 4 . 09 ( dd , j = 11 . 5 , 4 . 8 hz , 1h ), 4 . 02 ( s , 2h ), 3 . 96 ( s , 3h ), 3 . 90 - 4 . 01 ( m , 1h ), 3 . 59 - 3 . 68 ( m , 1h ), 3 . 44 - 3 . 52 ( m , 1h ), 3 . 23 ( dd , j = 11 . 2 , 10 . 2 hz , 1h ), 2 . 34 ( s , 3h ), 2 . 01 - 2 . 08 ( m , 1h ), 1 . 74 - 1 . 86 ( m , 1h ); 408 . 0 8 . 32 ( s , 1h ), 8 . 14 ( br d , j = 6 hz , 1h ), 8 . 00 ( d , 1h ), 7 . 82 - 7 . 90 ( br s , 2h ), 7 . 44 ( br d , j = 8 . 2 hz , 2h ), 7 . 13 ( br d , j = 8 . 2 hz , 2h ), 4 . 09 ( dd , j = 11 , 5 hz , 1h ), 4 . 05 ( s , 2h ), 3 . 91 - 4 . 04 ( m , 3h ), 3 . 64 ( ddd , j = 9 . 6 , 9 . 5 , 5 . 0 hz , 1h ), 3 . 48 ( ddd , j = 11 . 9 , 11 . 9 , 2 . 2 hz , 1h ), 3 . 23 ( dd , j = 11 . 4 , 9 . 9 hz , 1h ), 2 . 34 ( s , 3h ), 1 . 99 - 2 . 08 ( m , 1h ), 1 . 80 ( dddd , j = 13 , 12 , 12 , 5 hz , 1h ); 393 . 5 8 . 32 ( s , 1h ), 8 . 16 ( br d , j = 6 hz , 1h ), 8 . 01 ( s , 1h ), 7 . 73 ( d , j = 0 . 7 hz , 1h ), 7 . 58 - 7 . 59 ( m , 1h ), 7 . 39 ( br d , j = 8 . 3 hz , 2h ), 7 . 10 ( br d , j = 8 . 3 hz , 2h ), 4 . 32 - 4 . 45 ( br s , 1h ), 4 . 09 ( br dd , j = 11 . 4 , 5 . 0 hz , 1h ), 4 . 04 ( s , 2h ), 3 . 98 - 4 . 04 ( m , 1h ), 3 . 95 ( s , 3h ), 3 . 90 - 3 . 98 ( m , 1h ), 3 . 65 ( ddd , j = 9 . 6 , 9 . 6 , 5 . 0 hz , 1h ), 3 . 48 ( ddd , j = 11 . 9 , 11 . 9 , 2 . 2 hz , 1h ), 3 . 23 ( dd , j = 11 . 4 , 9 . 9 hz , 1h ), 2 . 33 ( s , 3h ), 2 . 01 - 2 . 08 ( m , 1h ), 1 . 80 ( dddd , j = 13 . 0 , 11 . 9 , 11 . 9 , 4 . 8 hz , 1h ); 407 . 5 8 . 84 - 8 . 90 ( m , 1h ), 8 . 13 ( s , 1h ), 8 . 00 ( s , 1h ), 7 . 96 ( br d , j = 6 hz , 1h ), 7 . 85 ( d , j = 8 . 2 hz , 2h ), 7 . 49 - 7 . 52 ( m , 1h ), 7 . 25 - 7 . 31 ( m , 2h , assumed ; partially obscured by solvent peak ), 4 . 43 - 4 . 54 ( br m , 1h ), 4 . 08 ( dd , j = 11 . 5 , 4 . 9 hz , 1h ), 4 . 03 ( s , 2h ), 4 . 00 ( s , 3h ), 3 . 96 - 4 . 0 ( m , 1h ), 3 . 87 - 3 . 96 ( m , 1h ), 3 . 57 - 3 . 66 ( m , 1h ), 3 . 42 - 3 . 51 ( m , 1h ), 3 . 22 ( dd , j = 10 . 9 , 10 . 3 hz , 1h ), 1 . 98 - 2 . 06 ( m , 1h ), 1 . 72 - 1 . 84 ( m , 1h ); 448 . 0 [ m + na + ] 8 . 31 ( s , 1h ), 8 . 12 ( br d , j = 6 hz , 1h ), 8 . 01 ( s , 1h ), 7 . 80 ( d , j = 8 . 2 hz , 2h ), 7 . 28 ( s , 1h ), 7 . 15 ( d , j = 8 . 2 hz , 2h ), 4 . 39 - 4 . 47 ( br m , 1h ), 4 . 10 ( dd , j = 12 , 5 hz , 1h ), 4 . 06 ( s , 2h ), 3 . 90 - 4 . 04 ( m , 2h ), 3 . 60 - 3 . 68 ( m , 1h ), 3 . 43 - 3 . 52 ( m , 1h ), 3 . 23 ( dd , j = 11 . 2 , 9 . 8 hz , 1h ), 2 . 77 ( s , 3h ), 2 . 30 ( s , 3h ), 2 . 00 - 2 . 08 ( m , 1h ), 1 . 75 - 1 . 87 ( m , 1h ); 423 . 9 1 h nmr ( 400 mhz , cd 3 od ) δ 8 . 30 ( s , 1h ), 8 . 17 ( s , 1h ), 7 . 87 ( s , 1h ), 7 . 60 - 7 . 74 ( m , 3h ), 7 . 35 ( br d , j = 8 hz , 2h ), 6 . 47 - 6 . 54 ( m , 1h ), 4 . 06 ( s , 2h ), 4 . 03 ( s , 3h ), 3 . 65 - 3 . 77 ( br m , 1h ), 3 . 45 - 3 . 56 ( br m , 1h ), 1 . 95 - 2 . 09 ( br m , 2h ), 1 . 65 - 1 . 82 ( br m , 2h ), 1 . 25 - 1 . 45 ( br m , 4h ); 407 . 0 characteristic peaks : 8 . 13 ( s , 1h ), 8 . 00 ( s , 1h ), 7 . 91 - 7 . 94 ( m , 2h ), 7 . 87 ( br d , j = 7 hz , 1h ), 7 . 67 ( br d , j = 8 . 3 hz , 2h ), 7 . 23 - 7 . 29 ( m , 2h , assumed ; partially obscured by solvent peak ), 4 . 02 ( s , 2h ), 3 . 99 ( s , 3h ), 2 . 01 - 2 . 16 ( m , 2h ), 1 . 72 - 1 . 81 ( m , 2h ), 1 . 22 - 1 . 47 ( m , 4h ); 407 . 9 1 h nmr ( 400 mhz , cd 3 od ) δ 8 . 30 ( s , 1h ), 8 . 10 ( s , 1h ), 7 . 84 ( s , 1h ), 7 . 64 ( br s , 2h ), 7 . 27 ( br s , 2h ), 4 . 04 ( s , 2h ), 4 . 03 ( s , 3h ), 3 . 66 - 3 . 76 ( m , 1h ), 3 . 46 - 3 . 55 ( m , 1h ), 2 . 49 ( s , 3h ), 1 . 97 - 2 . 07 ( m , 2h ), 1 . 68 - 1 . 80 ( m , 2h ), 1 . 27 - 1 . 43 ( m , 4h ); 422 . 0 1 . the requisite 5 -( difluoromethoxy )- 4 -[ 4 -( 1h - pyrazol - 1 - yl ) benzyl ] pyridine - 2 - carboxylic acid was prepared via reaction of c44 with sodium chloro ( difluoro ) acetate and potassium carbonate at elevated temperature . 3 . the diastereomeric examples 63 and 64 were separated using supercritical fluid chromatography ( column : chiral technologies chiralcel od - h , 5 μm ; mobile phase : 3 : 1 carbon dioxide / methanol ). example 63 was the first - eluting diastereomer , and example 64 was the second - eluting diastereomer . 4 . suzuki reaction of ( 6 - chloropyridin - 3 - yl ) methanol with 1 - methyl - 4 -( 4 , 4 , 5 , 5 - tetramethyl - 1 , 3 , 2 - dioxaborolan - 2 - yl )- 1h - pyrazole afforded [ 6 -( 1 - methyl - 1h - pyrazol - 4 - yl ) pyridin - 3 - yl ] methanol . subsequent bromination with phosphorus tribromide provided the requisite 5 -( bromomethyl )- 2 -( 1 - methyl - 1h - pyrazol - 4 - yl ) pyridine . 5 . suzuki reaction of c13 with 4 - bromo - 1 - trityl - 1h - pyrazole provided ethyl 5 - methyl - 4 -[ 4 -( 1 - trityl - 1h - pyrazol - 4 - yl ) benzyl ] pyridine - 2 - carboxylate ; removal of the trityl group with 1 m hydrochloric acid in methanol afforded the requisite ethyl 5 - methyl - 4 -[ 4 -( 1h - pyrazol - 4 - yl ) benzyl ] pyridine - 2 - carboxylate . 6 . the requisite 4 -[ 4 -( chloromethyl ) phenyl ]- 2 - methyl - 1 , 3 - thiazole , hydrochloride salt , was prepared via chlorination of [ 4 -( 2 - methyl - 1 , 3 - thiazol - 4 - yl ) phenyl ] methanol with thionyl chloride . this assay was designed to select and characterize compounds that affect the activity of human m1 muscarinic acetylcholine receptors ( similar m1 pam flipr assays can be found , for example , at u . s . pat . no . 8 , 664 , 234 ). human m1 receptors were stably expressed in chinese hamster ovary ( cho ) cells ( hd bioscience ). the effect of test compounds on intracellular calcium was measured on an flipr tetra ( molecular devices ) using the fluo - 8 , am calcium dye ( molecular probes ) with a red dye quenching agent ( sigma ). cho cells expressing hm1 cells had been previously cultured and frozen in assay ready vials . cell vials were thawed , then plated at a density of 10 , 000 cells per well in a 384 well black wall , clear bottom plate ( greiner # 781090 ) and incubated overnight at 37 degrees c . with 5 % co 2 . cells were grown and plated in f12 nutrient media ( gibco brl # 21700 - 075 ) supplemented with 10 % fbs ( hyclone # ch30160 . 03 ) and pen / strep ( gibco # 15070 - 063 ). after overnight incubation , cell plates were removed from the incubator and the growth media was discarded and replaced with loading solution containing the following : 2 μm fluo - 8 - am ( molecular probes # f14242 ), 2 mm probenecid ( sigma # p8761 ), lx acid red 1 ( sigma # 210633 ), in hbss buffer containing ( grams / l ): 0 . 1 cacl 2 , 0 . 1 mgcl 2 * 6h 2 o , 0 . 049 mgso 4 , 0 . 4 kcl , 0 . 06 kh 2 po 4 , 8 . 06 nacl , 0 . 12 na 2 hpo 4 * 12h 2 o , 1 . 1 d - glucose * h 2 o , 0 . 35 nahco 3 , 4 . 766 hepes , ph 7 . 4 . the plate was incubated in the loading solution at 37 degrees c . in the dark for 1 hour . test compounds were initially prepared as 100 % dmso stock solutions , then transferred and serially diluted in 384 - well compound plates ( greiner # 784201 ). each compound was tested at 10 concentrations in duplicate per experiment . positive and negative controls for positive allosteric modulator evaluation were 30 μm acetylcholine ( ach ) and an ec 10 - ec 30 concentration of acetylcholine , approximately 2 nm but could be adjusted for each experiment to maintain the ec 10 - ec 30 range . after the 1 - hour dye loading incubation , test compounds were added to the cell plate containing fluo - 8 . approximately 10 minutes after compound addition , an ec 10 - ec 30 concentration of acetylcholine was added to each well and the fluorescence measured to determine the pam potentiation of the compound . data was exported from the flipr tetra as maximum fluorescence / minimum fluorescence for each well . the percent effect for each compound well was determined using the mean values for the positive and negative controls on each plate for each read . percent effect was 100 *( compound negative control )/( positive control negative control ). dose response curves were fitted to the compound percent effect data using a 4 - parameter logistic fit model to determine pam ( positive allosteric modulator ) inflection point values . compounds with inverted u dose response curves had the concentrations greater than the concentration giving the peak response excluded from the fit . data was reported as inflection point . the compounds of examples 1 - 72 had activity according to this assay , generally with an inflection point ( ip ) of 10 μm or less ( using inflection point as a measure of activity ). such a result is indicative of the intrinsic activity of the compounds of the invention as m1 allosteric modulators . various modifications of the invention , in addition to those described herein , will be apparent to those skilled in the art from the foregoing description . such modifications are also intended to fall within the scope of the appendant claims . each reference ( including all patents , patent applications , journal articles , books , and any other publications ) cited in the present application is hereby incorporated by reference in its entirety . | 2 |
fig1 is a diagram showing a basic system to which a control device for a fuel cell system according to the present invention is applied . with reference to fig1 , a description will first be given of the basic system to which the control device for the fuel cell system according to the present invention is applied . in a fuel cell stack 10 , while an electrolyte membrane is being kept in an appropriate humid state , reactive gases ( oxygen o 2 and hydrogen h 2 ) are supplied to generate electricity . to achieve this , a cathode line 20 , an anode line 30 and a cooling water circulation line 40 are connected to the fuel cell stack 10 . a current generated by the fuel cell stack 10 is detected by a current sensor 101 . a voltage generated by the fuel cell stack 10 is detected by a voltage sensor 102 . air containing the oxygen o 2 supplied to the fuel cell stack 10 flows as a cathode gas along the cathode line 20 . in the cathode line 20 , a compressor 21 , a wrd ( water recovery device ) 22 and a cathode pressure adjustment valve 23 are provided . a bleed line 200 is also provided in parallel to the cathode line 20 . the bleed line 200 is branched from the cathode line 20 that is downstream with respect to the compressor 21 but is upstream with respect to the wrd 22 , and is combined with the cathode line 20 that is downstream with respect to the cathode pressure adjustment valve 23 . with this configuration , part of the air blown by the compressor 21 flows into the bleed line 200 , and bypasses the fuel cell stack 10 . in the bleed line 200 , a bleed valve 210 is provided . the bleed line 200 corresponds to a bypass passage in the scope of claims . the bleed valve 210 corresponds to a bypass valve in the scope of claims . in the present embodiment , the compressor 21 is , for example , a centrifugal turbo compressor . the compressor 21 is arranged in the cathode line 20 that is upstream with respect to the fuel cell stack 10 and the wrd 22 . the compressor 21 is driven by a motor m . the compressor 21 adjusts the quantity of flow of the cathode gas flowing along the cathode line 20 . the quantity of flow of the cathode gas is adjusted by the rotation speed of the compressor 21 . the wrd 22 humidifies the air introduced into the fuel cell stack 10 . the wrd 22 includes a humidified portion through which a gas that is a humidification target flows and a humidifying portion through which a water - containing gas that is a humidifying source flows . the air introduced by the compressor 21 flows through the humidified portion . the water - containing gas flows through the humidifying portion via the fuel cell stack 10 . the cathode pressure adjustment valve 23 is provided in the cathode line 20 that is downstream with respect to the fuel cell stack 10 . the cathode pressure adjustment valve 23 adjusts the pressure of the cathode gas flowing along the cathode line 20 . the pressure of the cathode gas is adjusted by the degree of opening of the cathode pressure adjustment valve 23 . a pressure p1 of the cathode gas flowing along the cathode line 20 that is upstream with respect to the compressor 21 is detected by a cathode pressure sensor 201 . the cathode pressure sensor 201 is provided upstream with respect to the compressor 21 . the quantity of flow q of the cathode gas flowing along the cathode line 20 is detected by a cathode quantity - of - flow sensor 202 . the cathode quantity - of - flow sensor 202 is provided downstream with respect to the compressor 21 but upstream with reference to the wrd 22 . the pressure of the cathode gas flowing along the cathode line 20 is detected by a cathode pressure sensor 203 . the cathode pressure sensor 203 is provided downstream with respect to the compressor 21 but upstream with respect to the wrd 22 . furthermore , in fig1 , the cathode pressure sensor 203 is located downstream with respect to the cathode quantity - of - flow sensor 202 . the bleed valve 210 is provided in the bleed line 200 . the bleed valve 210 adjusts the quantity of flow of the cathode gas flowing along the bleed line 200 . the quantity of flow of the cathode gas is adjusted by the degree of opening of the bleed valve 210 . the hydrogen h 2 supplied to the fuel cell stack 10 flows as an anode gas along the anode line 30 . in the anode line 30 , a cylinder 31 , an anode pressure adjustment valve 32 and a purge valve 33 . in the cylinder 31 , the hydrogen h 2 is stored so as to be in a high pressure state . the cylinder 31 is provided most upstream of the anode line 30 . the anode pressure adjustment valve 32 is provided downstream with respect to the cylinder 31 . the anode pressure adjustment valve 32 adjusts the pressure of the anode gas newly supplied from the cylinder 31 to the anode line 30 . the pressure of the anode gas is adjusted by the degree of opening of the anode pressure adjustment valve 32 . a purge valve 34 is provided downstream with respect to the fuel cell stack 10 . when the purge valve 34 is opened , the anode gas is purged . the pressure of the anode gas flowing along the anode line 30 is detected by an anode pressure sensor 301 . the anode pressure sensor 301 is provided downstream with respect to the adjustment valve 32 but upstream with respect to the fuel cell stack 10 . cooling water supplied to the fuel cell stack 10 flows along the cooling water circulation line 40 . in the cooling water circulation line 40 , a radiator 41 , a three - way valve 42 and a water pump 43 are provided . a bypass line 400 is provided in parallel to the cooling water circulation line 40 . the bypass line 400 is branched from the cooling water circulation line 40 that is upstream with respect to the radiator 41 , and is combined with the cooling water circulation line 40 that is downstream with respect to the radiator 41 . hence , the cooling water flowing along the bypass line 400 bypasses the radiator 41 . the radiator 41 cools the cooling water . in the radiator 41 , a cooling fan 410 is provided . the three - way valve 42 is located in a combination portion between the bypass line 400 and the cooling water circulation line 40 . the three - way valve 42 adjusts , according to the degree of opening , the quantity of flow of the cooling water flowing along the line on the radiator side and the quantity of flow of the cooling water flowing along the bypass line . thus , the temperature of the cooling water is adjusted . the water pump 43 is located downstream with respect to the three - way valve 42 . the water pump 43 feeds the cooling water flowing through the three - way valve 42 to the fuel cell stack 10 . the temperature of the cooling water flowing along the cooling water circulation line 40 is detected by a water temperature sensor 401 . the water temperature sensor 401 is provided upstream with respect to the portion where the bypass line 400 is branched . a controller inputs the signals of the current sensor 101 , the voltage sensor 102 , the cathode pressure sensor 201 , the cathode quantity - of - flow sensor 202 , the cathode pressure sensor 203 , the anode pressure sensor 301 and the water temperature sensor 401 . then , the controller outputs the signals to control the operations of the compressor 21 , the cathode pressure adjustment valve 23 , the bleed valve 210 , the anode pressure adjustment valve 32 , the purge valve 34 , the three - way valve 42 and the water pump 43 . with this configuration , the fuel cell stack 10 is kept at an appropriate temperature , and while the electrolyte membrane is being kept in an appropriate humid state , the reactive gases ( the oxygen o 2 and the hydrogen h 2 ) for generating electricity are supplied sufficiently , with the result that it is possible to perform stable electric generation . power generated by the fuel cell stack 10 is supplied through a dc / dc converter 11 to a travel motor 12 , a battery 13 and a load 14 . fig2 is a correlation diagram between the charging rate soc of the battery and the generated power of the fuel cell stack . the inventors are in the process of developing a system that uses the generated power of the fuel cell stack 10 and / or the power of the battery 13 to drive the travel motor 12 and the load 14 . in order not to reduce the life of the battery 13 , it is preferable to manage the battery charging rate soc to a predetermined value . however , since power is consumed significantly in a transient operating state , the battery charging rate soc is more likely to be varied . even in a steady operating state , the battery charging rate soc is more likely to be varied by a variation in the generated power of the fuel cell stack or a variation in an auxiliary load . although in the first place , the battery charging rate soc is calculated by totaling current sensor values , resetting is performed as necessary to remove an error . in this way , an error is removed , and at the same time the battery charging rate soc is likely to be varied . it is important to reduce the variation in the battery charging rate soc described above and to manage the battery charging rate soc to the predetermined value . hence , as shown in fig2 , when the battery charging rate soc is higher than a management value , the generated power of the fuel cell stack 10 is reduced . in this way , the battery 13 is discharged . consequently , the battery charging rate soc approaches the management value . when the battery charging rate soc is lower than the management value , the generated power of the fuel cell stack 10 is increased . in this way , the battery 13 is charged . consequently , the battery charging rate soc approaches the management value . fig3 is a diagram illustrating a problem to be solved in the present embodiment . as described above , depending on whether the battery charging rate soc is higher or lower than the predetermined value ( management value ), the generated power of the fuel cell stack 10 is adjusted , and thus the battery charging rate soc is managed to the predetermined value ( management value ). however , when the generated power of the fuel cell stack 10 is adjusted , conventionally , as shown in fig3 , the quantity of flow supplied from the compressor is controlled to vary the quantity of flow of the air flowing along the cathode line 20 . here , the rotation speed of the compressor 21 is varied . for example , when a vehicle is at rest , the sound of the compressor 21 is varied , and thus a passenger feels such sound harsh to have an uncomfortable feeling . hence , in the present embodiment , without the rotation speed of the compressor 21 being varied , the generated power of the fuel cell stack 10 is adjusted . fig4 is a control flowchart that is performed by a controller of the control device for the fuel cell system according to the present invention . the controller repeatedly performs this flowchart every minute time ( for example , 10 milliseconds ). in step s 1 , the controller computes the amount of air supplied to the fuel cell stack 10 . specific details will be described later . in step s 2 , the controller determines an operation mode . specific details will be described later . in step s 3 , the controller determines whether or not the operation mode is a sound vibration mode . if the operation mode is not the sound vibration mode , the controller transfers the processing to step s 4 whereas if the operation mode is the sound vibration mode , the controller transfers the processing to step s 5 . in step s 4 , the controller performs a normal mode . specific details will be described later . in step s 5 , the controller performs the sound vibration mode . specific details will be described later . fig5 is a block diagram showing the function of computing the amount of air supplied to the fuel cell stack . the following individual blocks shown in the block diagram indicate the individual functions of the controller as imaginary units , and the blocks do not mean physical entities . the block b 101 computes travel power based on a shift range , an accelerator pedal operation amount and a vehicle speed . specifically , among a plurality of maps prepared previously , a map corresponding to the present shift range is selected . then , the accelerator pedal operation amount and the vehicle speed are applied to the map , and the travel power (= power necessary for the motor to satisfy the requirement of a driver ) for which the motor produces a torque necessary for travel is computed . the block b 102 computes the generated power for managing the battery charging rate soc to the management value . the block b 103 adds the consumption power of the auxiliary load , the travel power computed by the block b 101 and the generated power computed by the block b 102 to determine target generated power to be generated by the fuel cell . in the generated power of the battery , when the battery is charged , a positive value is set whereas when the battery is discharged , a negative value is set . when the battery needs charging , in order to perform the charging by the generated power of the fuel cell , it is necessary for the fuel cell to increase the generated power with consideration given to the charging for the battery . on the other hand , when the battery needs discharging , in order for the battery to compensate for part of the power to the motor , it is necessary to reduce the generated power of the fuel cell . the block b 104 computes the amount of air supplied to the fuel cell stack 10 based on the target generated power computed by the block b 103 . as described above , the processing of step s 1 in the flowchart has been performed . fig6 is a diagram showing a subroutine that determines the operation mode . in step s 21 , the controller determines whether or not the sound pressure level of the compressor 21 is higher than that of background noise . the sound pressure level is preferably detected by attaching , for example , a microphone . preferably , the determination in the present step is performed , for example , when the vehicle is at rest or when the fuel cell is in an idle state ( the state where the power to the motor is 0 , and only the power supply to the auxiliary device and the battery is performed ). if the determination result is negative , the controller transfers the processing to step s 22 whereas if the determination result is positive , the controller transfers the processing to step s 23 . in step s 23 , the controller determines the sound vibration mode . fig7 is a diagram showing a subroutine in a normal mode operation . in step s 41 , the controller computes the amount of air corresponding to the generated power required for the fuel cell . on the other hand , the amount of air is compared with the minimum quantity of flow that the compressor 21 achieves . as this quantity of flow , there is a quantity of flow for avoiding the surge of the compressor 21 ( for example , when the quantity of flow in the compressor is low , if the pressure of the stack is high , a surge is produced , and hence , the minimum quantity of flow for preventing a surge is set ). then , the quantity of flow of air corresponding to the generated power is compared with the minimum quantity of flow that the compressor needs to achieve , and if the quantity of flow of air corresponding to the generated power is higher , the compressor 21 supplies the quantity of flow of air corresponding to the generated power . on the other hand , if the minimum quantity of flow that the compressor 21 needs to achieve is higher , the compressor 21 supplies this quantity of flow . in step s 42 , the controller computes the amount of air flowing along the bleed line 200 . when the compressor 21 supplies the quantity of flow corresponding to the generated power of the fuel cell , the quantity of flow that is bled is 0 . however , when the compressor 21 supplies the minimum quantity of flow that the compressor 21 needs to achieve , the quantity of flow higher than that needed by the fuel cell is supplied to the fuel cell . since an unnecessary quantity of flow is supplied to the fuel cell stack , for example , the humid state of the fuel cell is disadvantageously dried . since the electric generation is determined by the load of an external load , the unnecessary air does not affect the power balance . hence , in order to prevent the unnecessary air from being supplied to the fuel cell , the bleed valve is opened such that only the amount of air necessary for the electric generation is supplied to the fuel cell stack . in the present step , the quantity of flow to the bleed valve is computed . specific details will be described later . in step s 43 , the controller adjusts the degree of opening of the bleed valve 210 such that the amount of air computed in step s 42 flows along the bleed line 200 . fig8 is a block diagram showing the function of computing the amount of air bled in the normal mode operation . the block b 421 subtracts the amount of air supplied to the fuel cell stack 10 from the lower limit quantity of flow in the compressor 21 . when the quantity of flow supplied is excessively low , the compressor 21 may be subjected to a surge . the lower limit quantity of flow in the compressor 21 refers to the minimum quantity of flow for preventing such a problem . when the amount of air supplied to the fuel cell stack 10 is higher than the lower limit quantity of flow in the compressor 21 , the block b 421 outputs a negative value . when the amount of air supplied to the fuel cell stack 10 is lower than the lower limit quantity of flow in the compressor 21 , the block b 421 outputs a positive value . when the output result of the block b 421 is a positive value , the block b 422 outputs such a positive value as it is whereas when the output result is a negative value , the block b 422 outputs zero . the case of a negative value is that under conditions in which the compressor 21 supplies the air necessary for the electric generation of the fuel cell stack , the bleed valve 210 is preferably all closed . specifically , it is necessary to compute a value at which the bleed valve does not pass the air , and since such a value is 0 , in the case of a negative value , the value is set at zero . on the other hand , the case of a positive value is the conditions under which the compressor 21 passes a higher quantity of flow than the quantity of flow that the fuel cell stack needs . here , the bleed valve 210 passes the quantity of flow that is the positive value , as it is , to the bleed line 200 , and thus only the quantity of flow necessary for the electric generation is supplied to the fuel cell stack . a description will now be given again of the blocks b 423 , b 424 and b 425 . in the above discussion , the computation of the quantity of flow bled in a case where the minimum quantity of flow for avoiding the surge of the compressor 21 itself is set as the quantity of flow in the compressor 21 has been described . here , a description will be given of the computation of the quantity of flow bled in a case where the quantity of flow for the dilution of the purge gas of the fuel cell is set in the compressor 21 . nitrogen on the cathode side is permeated , through an ion exchange membrane , which is an electric generation area , to the anode side of the fuel cell stack . since in order to stably generate electricity on the anode side , it is necessary to maintain highly concentrated hydrogen , the nitrogen is purged together with hydrogen gas either periodically or by detecting the concentration of the nitrogen . in this way , it is necessary to keep the concentration of the hydrogen within the anode high . on the other hand , when the purge is performed , the hydrogen is discharged out of the fuel cell stack together with the nitrogen , and in the present embodiment , in order for the concentration of the hydrogen to be reduced to a predetermined concentration or less , the off - gas of the hydrogen is mixed with the off - gas of the oxygen to perform the dilution . in general , when the generated power is high , since the quantity of flow of air necessary for the electric generation of the fuel cell stack is supplied , and thus the quantity of flow necessary for the dilution is supplied , the compressor 21 supplies the amount of air corresponding to the generated power . however , when the generated power is lower , with respect to the hydrogen to be purged from the fuel cell stack , the desired concentration of the hydrogen or less may not be achieved only by the quantity of flow necessary for the electric generation . hence , the quantity of flow necessary for the dilution is supplied by the compressor 21 . when the quantity of flow necessary for the dilution is passed , with respect to the quantity of flow necessary for the electric generation of the fuel cell stack , the bleed valve 210 is used to pass the unnecessary quantity of flow to the bleed line 200 , and this point is the same as what has been described above . the block b 423 first subtracts the quantity of flow consumed by the electric generation from the amount of air supplied to the fuel cell stack 10 . thus , the amount of air that is discharged without being consumed in the fuel cell stack 10 is output . the block b 424 subtracts the amount of air that is discharged without being consumed in the fuel cell stack 10 from a dilution requirement air amount . when the purge valve 34 is opened , the anode gas h 2 is discharged . the amount of air necessary to dilute the anode gas h 2 is the dilution requirement air amount . when the amount of air that is discharged without being consumed by the electric generation in the fuel cell stack 10 is higher than the dilution requirement air amount , the block b 424 outputs a negative value . when the amount of air that is discharged without being consumed by the electric generation in the fuel cell stack 10 is lower than the dilution requirement air amount , the block b 424 outputs a positive value . when the output result of the block b 424 is the positive value , the block b 425 outputs it as it is whereas the output result of the block b 424 is the negative value , the block b 425 outputs zero . the block b 426 compares the output of the block b 422 and the output of the block b 425 , and outputs the higher one as a bleed air amount . in the present embodiment , the supply amount by the compressor 21 is varied according to the electric generation of the fuel cell . in particular , while the fuel cell is performing an idle operation , when the generated power required by the fuel cell is varied by soc control , the rotation speed of the compressor 21 is varied according to such variation , with the result that there is a concern that under conditions in which background noise is low , an uncomfortable feeling is given to the driver . even when the compressor 21 itself passes the minimum quantity of flow or the quantity of flow for the dilution , if the quantity of flow of air based on the electric generation requirement of the fuel cell is increased by the requirement of the soc , there is a concern that the rotation speed of the compressor 21 is likewise varied . hence , a description will be given below of a control logic for preventing the rotation speed of the compressor 21 from being varied according to the requirement of the soc when background noise is low . fig9 is a diagram showing a subroutine of a sound vibration mode operation . in step s 51 , the controller supplies a sound vibration mode air amount ( constant value ) from the compressor 21 . this value is preferably a value that is , in the sound vibration mode , higher than the maximum amount of air set based on the electric generation requirement . this is because such a value is set and thus it is possible to prevent the rotation speed of the compressor 21 from being varied completely based on the soc requirement . even in the sound vibration mode , since the compressor 21 supplies the quantity of flow higher than the quantity of flow based on the electric generation requirement of the fuel cell stack , the amount of air unnecessary for the electric generation of the fuel cell stack is passed to the bleed line 200 by the bleed valve 210 . in step s 52 , the controller first computes the amount of air passed to the bleed line 200 . specific details will be described later . in step s 53 , the controller adjusts the degree of opening of the bleed valve 210 such that the amount of air computed in step s 52 is passed to the bleed line 200 . fig1 is a block diagram showing the function of computing the amount of air bled in the sound vibration mode operation . a block b 521 subtracts the amount of air supplied to the fuel cell stack 10 from the lower limit quantity of flow in the compressor 21 . the block b 521 is basically the same as the block b 421 . when the output result of the block b 521 is a positive value , the block b 522 outputs such a positive value as it is whereas when the output result is a negative value , the block b 522 outputs zero . the block b 522 is basically the same as the block b 422 . a block b 523 subtracts the quantity of flow consumed by the electric generation from the amount of air supplied to the fuel cell stack 10 . the block b 523 is basically the same as the block b 423 . a block b 524 subtracts the amount of air that is discharged without being consumed by the electric generation in the fuel cell stack 10 from the dilution requirement air amount . the block b 524 is basically the same as the block b 424 . when the output result of the block b 524 is a positive value , the block b 525 outputs such a positive value as it is whereas when the output result is a negative value , the block b 525 outputs zero . the block b 525 is basically the same as the block b 425 . a block b 526 subtracts the amount of air corresponding to the generated power required by the fuel cell stack 10 from the sound vibration mode air amount . under conditions in which the compressor 21 supplies the amount of air in the sound vibration mode , it is desired to supply only the air necessary for the electric generation to the fuel cell stack . the amount of air supplied to the bleed line 200 to achieve this is computed as described above . in the sound vibration mode operation , since the sound vibration mode air amount is higher than the amount of air supplied to the fuel cell stack 10 , the block b 526 outputs a positive value . since the output result of the block b 526 is a positive value , a block b 527 generally outputs the positive value as it is . however , since it is assumed that a certain abnormality occurs in computation by a computer and thus the quantity of flow based on the electric generation requirement may become higher than the sound vibration mode air amount , the block b 526 deals with this case . if a negative value is output from the block b 526 , the block b 527 deals with this case by outputting zero . a block b 528 compares the output of the block b 522 , the output of the block b 525 and the output of the block b 527 , and outputs the highest one as the amount of air bled . fig1 is a diagram illustrating an operation in the normal mode operation in a first embodiment . in the normal mode operation , the amount of air corresponding to the electric generation requirement to the fuel cell is supplied from the compressor . however , if the quantity of flow supplied is excessively low , a surge is likely to occur . hence , even when the quantity of flow supplied is low such as when the electric generation is low in fig1 , the air corresponding to the lower limit quantity of flow in the compressor 21 is supplied , and an extra amount of air exceeding the quantity of flow ( fc stack supply air amount ) necessary for generating the target generated power of the fuel cell stack is passed to the bleed line . when the electric generation is increased , the amount of air higher than when the electric generation is low is supplied from the compressor . as described above , in the normal mode operation , the quantity of flow in the compressor 21 is varied according to the state of the operation . fig1 is a diagram illustrating an operation in the sound vibration mode operation in the first embodiment . in the sound vibration mode operation , the sound vibration mode air amount is supplied from the compressor 21 . this sound vibration mode air amount is a constant value regardless of when the electric generation is decreased or when the electric generation is increased . the extra amount of air exceeding the quantity of flow ( fc stack supply air amount ) necessary for generating the target generated power of the fuel cell stack is passed to the bleed line . in other words , the amount of air supplied to the fuel cell stack is adjusted according to the amount of air bled . fig1 is a time chart illustrating the operation in the sound vibration mode operation in the first embodiment . as described above , the fuel cell system adjusts the generated power of the fuel cell stack 10 according to whether the battery charging rate soc is higher or lower than the predetermined value ( management value ), and thereby manages the battery charging rate soc to the predetermined value ( management value ). in the present embodiment , a constant sound vibration mode air amount is supplied from the compressor 21 . in other words , the rotation speed of the compressor 21 is kept constant . then , by adjusting the amount of air bled , the amount of air supplied to the fuel cell stack is adjusted . when the generated power of the fuel cell stack 10 is adjusted , the rotation speed of the compressor 21 is varied , and thus the passenger feels harsh sound to have an uncomfortable feeling . by contrast , in the present embodiment , since the rotation speed of the compressor 21 is kept constant , the operating sound of the compressor 21 is not varied , and thus the passenger does not have an uncomfortable feeling . in the present embodiment , only when the sound pressure level of the compressor 21 is higher than that of background noise , the sound vibration mode operation is performed to keep the rotation speed of the compressor 21 at a high constant speed . when the sound pressure level of the compressor 21 is lower than that of background noise , even if the sound of the compressor 21 is varied , it is not recognized . however , when the sound pressure level of the compressor 21 is higher than that of background noise , the variation in the sound of the compressor 21 is recognized . the rotation speed of the compressor 21 is kept at a high constant speed , and power is wastefully consumed accordingly . hence , in the present embodiment , the operation scene in the sound vibration mode is limited , and thus it is possible to avoid waste power consumption as much as possible . fig1 is a diagram showing an operation mode determination subroutine in a second embodiment of the fuel cell system according to the present invention . in the following description , parts having the same functions as described above are identified with the same symbols , and their description will be omitted as necessary . in the first embodiment , for example , whether or not the sound pressure level of the compressor 21 is higher than that of background noise is determined directly by a sound pressure level detected by the microphone . however , in such a method , the microphone is needed , and thus the cost is increased . in the present embodiment , whether or not the sound pressure level of the compressor 21 is higher than that of background noise is estimated ( determined indirectly ) based on the state of the operation . specific details will be described later . in step s 211 , the controller determines whether or not the vehicle is at rest . if the determination result is negative , the controller transfers the processing to step s 212 whereas if the determination result is positive , the controller transfers the processing to step s 23 . in step s 212 , the controller determines whether or not the shift range is a parking range (“ p range ”) or a neutral range (“ n range ”). if the determination result is negative , the controller transfers the processing to step s 213 whereas if the determination result is positive , the controller transfers the processing to step s 23 . in step s 213 , the controller determines whether or not the vehicle is travelling at a low speed . the low - speed travel refers to travel at a speed lower than a speed when the sound pressure level of background noise is lower than that of the compressor 21 . a threshold value for determining whether or not the vehicle is travelling at a low speed is set by previously performing an experiment or the like . if the determination result is negative , the controller transfers the processing to step s 214 whereas if the determination result is positive , the controller transfers the processing to step s 23 . in step s 214 , the controller determines whether or not the mode is a quiet mode . the quiet mode is set by the operation of a switch by the driver and the like . if the determination result is negative , the controller transfers the processing to step s 215 whereas if the determination result is positive , the controller transfers the processing to step s 23 . in step s 215 , the controller determines whether or not the fuel cell stack 10 is in a low electric generation state . the low electric generation state refers to a state where the amount of electricity is lower than an amount of electricity when the sound pressure level of background noise is lower than that of the compressor 21 . a threshold value for determining whether or not the fuel cell stack 10 is in the low electric generation state is set by previously performing an experiment or the like . if the determination result is negative , the controller transfers the processing to step s 22 whereas if the determination result is positive , the controller transfers the processing to step s 23 . in step s 23 , the controller determines the sound vibration mode . in the present embodiment , in the operation scene where the sound pressure level of background noise is lower than that of the compressor 21 , it is estimated that the sound pressure level of background noise is lower than that of the compressor 21 . in this way , without use of a microphone , it is possible to estimate ( indirectly determine ) whether or not the sound pressure level of the compressor 21 is higher than that of background noise . thus , it is possible to reduce the cost to be inexpensive . fig1 is a diagram showing a sound vibration mode operation subroutine in a third embodiment of the fuel cell system according to the present invention . since steps s 51 to s 53 are the same as in the first embodiment , their description will be omitted . in step s 54 , the controller determines whether or not a surge occurs in the compressor 21 . this is determined based on the amount of air supplied by the compressor 21 and a pressure ratio in the compressor 21 ( a ratio ( p2 / p1 ) of an exit pressure p2 to an entrance pressure p1 of the compressor 21 ). if the determination result is negative , the controller transfers the processing to step s 55 whereas if the determination result is positive , the controller transfers the processing to step s 56 . in step s 55 , the controller determines whether or not a differential pressure between the front and back surfaces of the electrolyte membrane of the fuel cell does not exceed a membrane resistance differential pressure . the pressure on the cathode side is computed by subtracting a loss caused by the passing of the cathode gas through the wrd 22 or the like from the detection value of the cathode pressure sensor 203 . the pressure on the anode side is detected by the anode pressure sensor 301 . as the case where the differential pressure between the front and back surfaces of the electrolyte membrane of the fuel cell exceeds the membrane resistance differential pressure , a case where the pressure on the cathode side is high and a case where the pressure on the anode side is high can be generally considered . however , in the present embodiment , since the mode is the sound vibration mode ( the mode in which as compared with the normal mode , the amount of air supplied from the compressor 21 is increased ), the case where the pressure on the cathode side is high applies . if the determination result is negative , the controller temporarily stops the processing whereas if the determination result is positive , the controller transfers the processing to step s 56 . in step s 56 , the controller increases the degree of opening of the cathode pressure adjustment valve 23 . fig1 is a diagram illustrating an operation method of the compressor 21 in the normal mode operation . in fig1 , the horizontal axis is the quantity of flow of air , and the vertical axis is the pressure ratio ( the ratio ( p2 / p1 ) of the exit pressure p2 to the entrance pressure p1 of the compressor 21 ). in the present embodiment , although when the sound pressure level of background noise is low such as in the idle operation , the sound vibration mode operation is performed , even if the idle operation is performed , a case where the normal mode operation is performed will be considered . in the idle operation , an operation point of the compressor 21 required from the generated power of the fuel cell stack 10 is a . in other words , the quantity of flow in the compressor 21 is preferably q a . however , since the operation point a is in a surge region above a surge line , a surge may occur in the compressor 21 . hence , the quantity of flow is set at q b , and the compressor 21 is operated at operation point b . however , in this state , an extra amount of air is inevitably supplied to the fuel cell stack 10 . hence , ( q b - q a ) is bled . when the electric generation is increased , an operation point of the compressor 21 required from the generated power of the fuel cell stack 10 is c . in other words , the quantity of flow in the compressor 21 is preferably q c . however , since the operation point c is in the surge region above the surge line , a surge may occur in the compressor 21 . hence , the quantity of flow is set at q d , and the compressor 21 is operated at operation point d . however , in this state , an extra amount of air is inevitably supplied to the fuel cell stack 10 . hence , ( q d - q c ) is bled . as described above , in the normal mode , the quantity of flow in the compressor 21 is adjusted from q b to q d , and the quantity of flow exceeding the quantity of flow necessary for the electric generation is bled . fig1 is a diagram illustrating a problem when in the sound vibration mode operation , the cathode pressure adjustment valve is not controlled . then , a case where the sound pressure level of background noise is low and the sound vibration mode operation is performed will be considered . although in the present embodiment , when a surge is likely to occur in the compressor 21 ( yes in step s 54 ), the quantity of flow in the compressor 21 is increased ( step s 56 ), and the degree of opening of the cathode pressure adjustment valve 23 is increased ( step s 57 ), a case where the degree of opening of the cathode pressure adjustment valve 23 is not adjusted will be temporarily considered . in the sound vibration mode , a sound vibration mode air amount q e is supplied from the compressor 21 . however , in the idle operation , the quantity of flow required from the generated power of the fuel cell stack 10 may be q a . hence , in the idle operation , the sound vibration mode air amount q e is supplied from the compressor 21 , and ( q e - q a ) is bled . then , a case where the amount of electricity is increased and the quantity of flow q c is supplied to the fuel cell stack 10 will be considered , and q c = q a + δq . here , the amount of air supplied from the compressor 21 remains the sound vibration mode air amount q e , and ( q e - q c ) is bled . here , if the degree of opening of the cathode pressure adjustment valve 23 is not adjusted , the amount of air supplied to the fuel cell stack 10 is increased by δq , and the exit pressure p2 of the compressor 21 is increased accordingly , with the result that there is a possibility that it is impossible to avoid a surge . as the exit pressure p2 of the compressor 21 is increased , the pressure on the cathode side of the electrolyte membrane of the fuel cell is increased . consequently , the differential pressure of the front and back surfaces of the electrolyte membrane is likely to exceed the membrane resistance differential pressure . fig1 is a diagram illustrating the effect of action in a third embodiment in the sound vibration mode operation . as described above , when the amount of electricity is increased and the quantity of flow q c is supplied to the fuel cell stack 10 , if no measure is taken , the amount of air supplied to the fuel cell stack 10 is increased by δq , and the exit pressure p2 of the compressor 21 is increased accordingly , with the result that there is a possibility that it is impossible to avoid a surge . hence , in the present embodiment , the degree of opening of the cathode pressure adjustment valve 23 is increased , and thus the exit pressure p2 of the compressor 21 is prevented from being increased , with the result that the compressor 21 is operated at operation point e0 . then , the extra amount of air ( q e - q c ) is bled . in this way , it is possible to prevent a surge from occurring in the compressor 21 . when the degree of opening of the cathode pressure adjustment valve 23 is excessively increased , as indicated by c1 , it is likely that the exit pressure p2 of the compressor 21 is excessively lowered . in this case , the pressure on the cathode side of the electrolyte membrane of the fuel cell is low . consequently , the differential pressure of the front and back surfaces of the electrolyte membrane is likely to exceed the membrane resistance differential pressure . in order to avoid this problem , the degree of opening of the cathode pressure adjustment valve 23 is adjusted . in this way , it is possible to protect the electrolyte membrane . fig1 is a diagram showing an operation mode determination subroutine in a fourth embodiment of the fuel cell system according to the present invention . in step s 221 , the controller determines whether or not the bleed valve 210 is currently open . if the determination result is negative , the controller transfers the processing to step s 22 whereas if the determination result is positive , the controller transfers the processing to step s 23 . in step s 23 , the controller determines the sound vibration mode . when the bleed valve 210 is open , at present , the compressor 21 supplies the amount of air exceeding the amount of air necessary for the electric generation of the fuel cell stack 10 , and bleeds the extra amount of air . in this case , an amount of air exceeding the sound vibration mode air amount is likely to be supplied . thus , it is possible to supply the sound vibration mode air amount without wastefully operating the compressor 21 . even if the sound vibration mode air amount is not exceeded , since the amount of air bled is present , as compared with the case where the bleed valve 210 is closed , it is possible to supply the sound vibration mode air amount with a small amount . hence , in the present embodiment , it is possible to prevent the compressor 21 from being wastefully operated to waste power . fig2 is a diagram showing an operation mode determination subroutine in a fifth embodiment of the fuel cell system according to the present invention . in step s 231 , the controller determines whether or not a dilution air amount excessing the amount of air necessary for the electric generation of the fuel cell stack 10 is needed . if the determination result is negative , the controller transfers the processing to step s 232 whereas if the determination result is positive , the controller transfers the processing to step s 23 . in step s 232 , the controller determines whether or not an operation in which the amount bled is increased for a transient operation is being performed . in the transient operation , since it is likely that the electric generation of the fuel cell stack 10 is rapidly increased , it is likely that the compressor 21 is previously rotated beyond necessity and the amount bled is increased . the controller determines whether or not the state of the operation described above is present . if the determination result is negative , the controller transfers the processing to step s 233 whereas if the determination result is positive , the controller transfers the processing to step s 23 . in step s 233 , the controller determines whether or not a surge avoiding operation is being performed . the surge avoiding operation is an operation in which in order to avoid a surge , the compressor 21 is rotated beyond necessity and the amount bled is increased . if the determination result is negative , the controller transfers the processing to step s 233 whereas if the determination result is positive , the controller transfers the processing to step s 23 . in step s 234 , the controller determines whether or not the fuel cell stack 10 has just been started up . immediately after the fuel cell stack 10 has been started up , the anode pressure is increased and purge is continuously performed . hence , at that time , in order to dilute purged hydrogen , the amount bled is increased . in order to increase the amount bled , the compressor 21 supplies an amount of air exceeding the amount of air necessary for the electric generation of the fuel cell stack 10 . the controller determines whether or not the state of the operation described above is present . if the determination result is negative , the controller transfers the processing to step s 22 whereas if the determination result is positive , the controller transfers the processing to step s 23 . in step s 23 , the controller determines the sound vibration mode . in the present embodiment , in the scene where the compressor 21 currently supplies an amount of air exceeding the amount of air necessary for the electric generation of the fuel cell stack 10 and an extra amount of air is bled , the sound vibration mode operation is performed . in such a scene , it is likely that an amount of air exceeding the sound vibration mode air amount is supplied . thus , it is possible to supply the sound vibration mode air amount without wastefully operating the compressor 21 . even if the sound vibration mode air amount is not exceeded , since the amount of air bled is present , it is possible to supply the sound vibration mode air amount by a small increase in amount . hence , in the present embodiment , it is possible to prevent the compressor 21 from being wastefully operated to waste power . fig2 is a diagram showing a sound vibration mode subroutine in a sixth embodiment of the fuel cell system according to the present invention . since steps s 51 and s 52 are the same as in the first embodiment , their description will be omitted . in step s 521 , the controller computes surplus generated power . the surplus generated power is power that is generated in the fuel cell stack 10 when the entire amount of air supplied from the compressor 21 is supplied to the fuel cell stack 10 without being bled . a specific computation method will be described later . in step s 522 , the controller determines whether or not the surplus generated power is lower than the target generated power . the target generated power is computed , for example , as shown in fig5 . if the determination result is negative , the controller transfers the processing to step s 53 whereas if the determination result is positive , the controller transfers the processing to step s 523 . in step s 523 , the controller increases the quantity of flow in the compressor 21 such that the surplus generated power exceeds the target generated power . a specific computation method will be described later . fig2 is a block diagram showing the function of computing the surplus generated power . a block b 5211 adds together the amount of air actually supplied to the fuel cell stack and the amount of air bled . a block b 5212 applies the amount of air to a preset map to determine the surplus generated power . fig2 is a block diagram showing the function of computing an increased amount of air supplied by the compressor . a block b 5231 computes , based on the target generated power , the amount of air supplied to the fuel cell stack 10 . a block b 5232 computes an increased amount of air by subtracting the amount of air actually supplied from the compressor 21 from the amount of air computed in the block b 5231 . fig2 is a diagram illustrating the effect of action in the sixth embodiment . in the present embodiment , when the target generated power is increased , the amount of air supplied from the compressor is increased . in this way , for example , even if the target generated power is increased by a decrease in the battery charging rate soc and the like , the fuel cell stack 10 can appropriately generate electricity . although the embodiments of the present invention have been described above , the embodiments described above simply indicate part of examples to which the present invention is applied , and it is not intended that the technical range of the present invention is limited to the specific configurations of the embodiments described above . for example , in the sound vibration mode , a constant amount of air ( sound vibration mode air amount ) is supplied so that the operating sound of the compressor is not varied . however , if the constant amount of air ( sound vibration mode air amount ) is excessive , the passenger may feel harsh sound to have an uncomfortable feeling without the operating sound of the compressor being varied . hence , the compressor is preferably operated in such a range that the passenger does not have such an uncomfortable feeling . even when as in the sixth embodiment , the amount of air supplied from the compressor is increased halfway , an upper limit may be provided so that the passenger does not have an uncomfortable feeling . this application claims priority based on japanese patent application no . 2011 - 219298 filed on oct . 3 , 2011 with japan patent office , the entire disclosure of which is incorporated herein by reference . | 8 |
referring to fig1 apparatus 10 is provided for expressing milk from one breast , or from two breasts simultaneously . the apparatus 10 includes a first collector or expresser 12 and a second expresser 14 . it is likely that both expressers would generally be used , but only one expresser could be used , if desired , preferably by disconnecting the vacuum line from the unused expresser and covering the unused vacuum port of the pump with a cap ( not shown ). a pump 16 is connected to both expressers 12 , 14 through vacuum lines 18 , 20 , and air pressure lines 22 , 24 . the vacuum and pulsation lines can be configured in any suitable way . in fig1 vacuum hoses 18 a , 20 a and pressure hoses 22 a , 24 a are connected to the pump 16 and a connector 17 . vacuum hoses 18 b , 20 b and pressure hoses 22 b , 24 b are connected to the other end of the connector 17 and the expressers 12 , 14 with adapters 23 ( fig2 ), if needed . the connector 17 has openings for the lines 18 , 20 , 22 and 24 , and a throat 19 which connects the vacuum lines 18 , 20 to each other , creating a common vacuum at the expressers 12 , 14 , as seen in fig1 . a threaded needle valve 21 in the throat 19 permits easy adjustment of the vacuum by venting atmospheric air into the system as desired . the connector 17 can be secured to a housing , if desired , to provide easy vacuum and pressure transmission through the housing . the pump 16 creates a vacuum which engages the breasts , and contributes to drawing the milk from the breasts . the pump also creates reciprocating compression and release pressure pulsation around the areola and some or all of the nipple , as will be seen . the pump 16 can be powered by line voltage , a battery , manually or the like . the expressers 12 , 14 are shown in greater detail in fig2 and 5 . each expresser includes a manifold 26 , a cup assembly 28 which fits over a breast , a cap 30 , a filter 31 ( fig5 ), a sealing device 33 a such as a wipe washer , o - ring or the like , and a collection vessel 34 . gaskets 33 b and 33 c are also included , to better seal the vacuum system . a valve 36 can be included , though it is not necessary . the collection vessel can be a bottle made of plastic - like material or the like or a bag , and can be oriented at an obtuse angle with respect to the cup assembly , as shown . the manifold 26 includes an opening 38 which is preferably threaded , so that a collection vessel such as a plastic milk bottle can be threadedly secured to the manifold 26 , with the valve 36 . the valve 36 is preferably a one - way check valve such as a duck bill valve or the like . when using the valve 36 , the gasket 33 c is not needed because the valve 36 seals the opening 38 . a vent 37 in the manifold 26 is helpful because it keeps the collection vessel 34 at atmospheric pressure when the valve 36 is used . however , it is also possible to eliminate the valve 36 , in which case there is also no need for the vent 37 . a vacuum is applied to the expresser through a port 42 in the cap 30 , and is drawn through a vacuum path in the manifold 26 through an outlet opening 44 in the top of the manifold . the vacuum is drawn through an internal orifice 46 to the opening 38 in the midsection of the vacuum path , which is beneath the port 42 and the cup assembly 28 . the vacuum tends to close the valve 36 , which in conjunction with the vent 37 , prevents a substantial buildup of vacuum in the collection vessel 34 . the vacuum is drawn from the opening 38 to a manifold vacuum inlet 40 through a channel 50 . the vacuum inlet 40 forms a cup assembly opening that is in communication with a milk outlet port 48 in the cup assembly 28 . when milk is drawn from the breast , the milk passes through the channel 50 under the force created by the vacuum , but most of the milk drops into the valve 36 through the force of gravity , and does not enter the orifice 46 . cleaning is easier because milk is not drawn into the vacuum path beyond the collection vessel 34 . when sufficient milk collects in the valve 36 , the weight of the milk forces the valve open , which releases the milk into the collection vessel 34 . because the milk falls down , the vacuum lines are not contaminated . in this manner , the milk is collected without contaminating the vacuum lines 18 , 20 ( fig1 ). the cup assembly 28 has a milk inlet port 52 in addition to the outlet port 48 . the components of the cup assembly 28 include a bell housing 54 , a donut shaped pad 56 , and a flexible liner 58 , shown disassembled in fig4 . the cup assembly 28 also has an air pressure pulsation port 60 which forms part of a pressure path and allows pressurized air to enter a space 62 between the case bell housing 54 and the liner 58 . the cup assembly 28 is assembled by placing the donut shaped pad 56 in the housing 54 as shown , and does not need further securement . the pad 56 is preferably made of a suitable foam material which is sized to fit snugly in the housing 54 . however , the pad 56 can be easily removed by placing a finger through the opening in the ring and pulling the ring out . the liner 58 is installed in the cup assembly 28 by securing an end 63 to the liner 58 in a groove 64 formed in the housing 54 ( fig2 and 4 ). the end 63 and groove 64 are shaped to provide locking press fit type of securement . the liner could also be affixed to the housing 54 by heat or chemical bonding . the liner 58 extends from the groove 64 over and around the pad 56 and inside of the housing 54 to a bottom end 66 of the housing 54 . an end 68 of the liner 58 is inserted into a groove 70 near the end 68 for securement in a press fit fashion . the liner 58 can be any suitable shape , including the shape shown in fig2 which includes a relatively narrow section 72 near the inlet opening 52 , and a wider section 74 between the section 72 and the outlet end 48 of the cup assembly 28 . this shape places more pressure around the areola region of the breast , while placing less pressure on the nipple itself . by sealing the liner to the case at both ends , the assembly can be washed without taking the liner off , if a cleaning cap 75 is placed over the pressure inlet 60 ( fig4 ). the cup assembly 28 can be press fit into a circular groove 76 in the manifold 26 , seen in fig5 . the groove 76 is formed by an outside wall 78 and an inside boss 80 . the boss 80 can extend outwardly as far as desired , and can be any suitable shape , such as circular , triangular , square , rectangular , elliptical , hexagonal , etc . since the boss 80 is hollow and prevents the liner 58 from collapsing under outside air pressure , the boss 80 protects any part of the nipple which is inside the boss from a pinching action caused by pressure when the liner is collapsed , as seen in fig6 . abrasion is avoided because there is more room for breast extension during milk expression . the boss 80 also keeps the throat of the cup assembly open , so that the flow of milk is not inhibited . the cap 30 ( fig2 and 5 ) includes an air pressure / pulsation channel 82 which extends from a pressure inlet 84 to the port 60 , as well as the port 42 for the vacuum path . the cap 30 can be press fit over the manifold opening 44 and the cup assembly air pressure / pulsation port 60 , and can be easily removed . when installed , the cap 30 farther secures the cup assembly in the manifold , but both the cap and the manifold can be removed without tools for cleaning purposes . the filter 31 , if used , further prevents liquids , fats and solid components in the milk from entering the vacuum lines and the pump . the filter 31 is preferably permeable to air flow when dry and also when wet , which can happen if milk contacts the filter . thus , if the filter becomes wet due to milk and / or water , air can still pass through the filter because the filter remains permeable to air . an example of such a filter is versapor r1200 ( part no . 66393 ) by pall corp . referring again to fig1 the pump 16 has two halves 104 , 106 secured together by screws or the like 108 to form a chamber 110 . the screws 108 also secure a movable diaphragm 112 in place . the diaphragm 112 divides the chamber 110 into two halves 110 a , 110 b . the diaphragm 112 is oscillated in a back and forth manner by a motor 114 . about 41 - 65 pulsations per minute at the breast ( one pulsation being the result of both a back and forth motion of the diaphragm ) are believed to produce suitable results , with about 52 pulsations per minute producing good results . the motor can be secured to the housing by bolts 116 or the like . the motor 114 can be a stepper motor , which is one form of a linear actuator , which has a shaft 118 . the shaft 118 moves in and out of the motor 114 in the axial direction without rotation . the shaft 118 is threaded , and is moved by a rotating threaded ring 120 , which is similar to a nut . rotation of the ring 120 moves the shaft 118 linearly . in this manner , the shaft 118 can move the diaphragm 112 back and forth essentially directly , without large , complex linkages . the distal end of the shaft 118 can be guided by an opening 122 in an end cap 124 . the end cap 124 is secured by bolts 126 . the pump 16 also has vacuum outlets 128 , 130 in the chamber 110 , on opposite sides of the diaphragm 112 . the vacuum lines 18 , 20 are connected to the vacuum outlets 128 , 130 . check valves such as duck bill valves 136 , 138 control the vacuum and pumping operation , and exhaust valves 140 , 142 release the pressure created in the chamber halves 110 a , 110 b by the movement of the diaphragm 112 . however , some of the pressure generated by the diaphragm is transmitted through the pressure lines 22 , 24 to the collectors 12 , 14 . the pressure forces the liners 58 against the breasts ( see fig6 ), which further stimulates release of milk . while the vacuum is fairly continuous , though , the pressure pulsates , in part because the pressure is quickly bled through vents 143 in the pressure lines 22 , 24 . in fact , when the diaphragm moves away from a pressure line 22 , or 24 , air is drawn out and a partial vacuum can be created . fig7 shows the effect of adequately vented pulsation pressure on the vacuum supplied to the liner . the pump 16 generates a vacuum v sys . without pulsation pressure , the vacuum is fairly steady at v sys . when pressure pulses are applied to the outside of the liner , though , the vacuum periodically increases to v peak . those periodic increases stimulate milk production with less discomfort and a lower v sys than is needed if pressure pulses are not applied . preferably , a minimum v sys of 0 . 5 ″ mercury is maintained during use , and the maximum vacuum v peak does not exceed 5 ″ mercury . the maximum vacuum v peak is preferably 3 . 0 ″- 4 . 1 ″ mercury . however , the maximum differential between v sys and v peak is preferably between 1 ″ and 4 . 5 ″ mercury . the vents 143 are sized to obtain a desired v peak , and avoid stalling due to overload . if the vents are too small , v peak will be too high and stalling could occur . if the vents are too large , v peak will be too low . the device is light weight , portable and compact because large motor linkages are eliminated . wear is also reduced by simplifying the power train in this manner . the motor 114 can be any suitable device which creates a fairly self - contained drive system which is relatively small in size and fairly quiet . in fact , the motor can be an ordinary motor 144 with a threaded rotating shaft 146 , as seen in fig8 . in that embodiment , a fixed ring 148 is attached to the diaphragm . the ring 148 is also threaded , so when the shaft 146 rotates clockwise and counter - clockwise , the diaphragm 112 moves back and forth . the motor can be controlled in any suitable manner , such as the control system 150 shown in fig9 . an application specific integrated circuit or the like has an mpu ( micro processing unit ) 152 and a rom ( read only memory ) 154 , programmed to cause a motor driver 156 to set the desired rate of rotation and the direction of rotation of the motor . the rotation rate , as well as the timing of the back and forth motion of the diaphragm , can be controlled in this manner . the diaphragm 112 can be any suitable configuration , such as that shown in fig1 which features a flat stiff middle section flanked by soft corrugations . another design is shown in fig1 and 11 , where a diaphragm 158 has a plurality of rings 160 joined by corrugations 162 . in use , power is applied to the pump 16 , and the expressers 12 , 14 are placed over the breasts . the vacuum v sys created by the pump 16 secures the expressers 12 , 14 on the breasts and helps draw milk from the breasts . the pressure pulsations massage and compress the breasts to stimulate milk production , and reduce the amount of vacuum needed to collect the milk . the air pressure lines are vented to obtain strong pulses without overloading the system . this reduces discomfort to the breasts . the device can be easily disassembled without tools , cleaned and reassembled . the many advantages of this invention are now apparent . the pulsation pulses stimulate milk production , without overloading the system due to excessive pressure build - up in the pressure lines . cleaning is more convenient because milk does not enter the vacuum lines . moreover , the entire collector can be easily disassembled for cleaning and reassembled without tools . the bosses in the expressers protect the end of the nipple from irritation , which is comfortable . moreover , the entire pump is small , lightweight and relatively quiet . while the principles of the invention have been described above in connection with a specific apparatus and applications , it is to be understood that this description is made only by way of example and not as a limitation on the scope of the invention . for example , various aspects of the invention could be used to milk animals , as well as humans . | 0 |
as shown in the figures , compression screw assembly 10 consists of lag screw 20 , compression plate 30 , clip 40 , wrench 50 , stabilizing rod 60 , clip holder 70 , clip pusher 80 and compression screw 90 . referring to fig1 and 20 , lag screw 20 includes a screw head 21 formed at one end of an elongated shaft 22 adapted to be installed into the shaft of the fractured bone , through the fracture , and anchored in the head of the fractured bone . shaft 22 has a substantially circular cross section with flat portions 23 formed on either side of its outer edge . the second end of lag screw 20 includes drive portion 24 . the cross section of drive portion 24 is smaller than that of the remainder of lag screw 20 , and is preferably of a modified hexagonal configuration having six sides , one pair of opposing sides being of a different length than the other four sides . drive portion 24 is adapted to fit within bore 54 of wrench 50 when compression screw assembly 10 is assembled . lag screw 20 has a bore extending therethrough so that lag screw 20 can be inserted over a guide wire . the bore of lag screw 20 contains a threaded portion 25 so that compression screw 90 can be threaded therein . in addition , the threaded portion formed at the lower end of stabilizing rod 60 is inserted within threaded portion 25 when compression screw assembly 10 is assembled . as shown in fig1 , 3 , 19 and 20 compression plate 30 includes barrel member 31 having a bore 32 extending therethrough of a size that permits bore 32 to accept the second end of lag screw 20 through end 33 of compression plate 30 . the surface of bore 32 of barrel member 31 includes two flat portions 34 corresponding to flat portions 23 formed on the outer surface of lag screw 20 to permit inserton of clip 40 between flat portions 34 of barrel member 31 and flat portions 23 formed on the outer surface of lag screw 20 . each flat portion 34 includes an indentation 35 adapted to receive a tang 44 of clip 40 . end 36 of bore 32 is adapted to receive compression screw 90 therein . compression plate 30 also includes a member 37 for enabling compression plate 30 to be anchored to the shaft of the bone . member 37 contains a plurality of holes 38 for the insertion of bone screws therethrough in order to anchor compression plate 30 to the shaft of the bone . clip 40 , illustrated in fig1 through 7 , and 17 through 19 , includes ring 41 having two flat portions 42 . the inner surface of ring 41 is of a size that permits ring 41 to accept the second end of lag screw 20 and wrench 50 ; the outer edge of ring 41 is of a size adapted to permit insertion of clip 40 into bore 32 of barrel member 31 and bore 72 of clip holder 70 that clip 40 can be inserted within bore 32 of barrel member 31 between the outer edge of lag screw 20 and the inner edge of barrel member 31 . two elongated members 43 extend perpendicularly from flat portions 42 of ring 41 . members 43 include tangs 44 which are adapted to be received by indentations 35 formed in the inner surface of barrel 31 of compression plate 30 and grooves 75 of clip holder 70 . referring to fig1 through 20 , wrench 50 includes bore 51 adapted to receive stabilizing rod 60 . as shown in fig1 , the shaft of wrench 50 includes a first portion or lower shaft 52 and a second portion or upper shaft 57 . lower shaft 52 has a smaller circumference than upper shaft 57 . the lower shaft 52 of wrench 50 has an outer surface cross - section adapted to match that of lag screw 20 and includes flat portions 53 which correspond to flat portions 23 of lag screw 20 . the end of lower shaft 52 contains drive portions 54 , the inner surface of which has a shape corresponding to drive portion 24 of lag screw 20 and is adapted to accept drive portion 24 . depth markings 55 , formed in the non - flat portions of wrench 50 , are used as assembly 10 is installed in a bone shaft . lower shaft 52 includes stops 56 formed on its outer surface at its upper end . stops 56 are protruding portions of lower shaft 52 which are used to prevent premature separation of clip 40 and clip holder 70 . the outer edge of upper shaft 57 of wrench 50 is of a larger circumference than that of lower shaft 52 and does not include any flat portions . upper shaft 57 ends in a t - shaped handle 58 . the plane passing through both arms of handle 58 is perpendicular to the plane passing through flat portions 53 . as illustrated in fig1 through 20 , stabilizing rod 60 is inserted through bore 51 of wrench 50 . stabilizing rod 60 is cannulated so that compression screw system 10 can be threaded over a guide wire to aid in directing the insertion of lag screw 20 into the bone . stabilizing rod 60 includes a threaded portion at its lower end which can be threaded within portion 25 of lag screw 20 . stabilizing rod 60 also includes knurled end 62 . clip holder 70 , shown in fig8 through 12 and 17 through 20 , includes an upper barrel portion 71 having a bore 72 extending therethrough and two elongated members 73 extending therefrom . the inner surface of clip holder 70 includes flat portions 74 . the inner surface of clip holder 70 is adapted to receive clip 40 and includes grooves 75 that receive tangs 44 of clip 40 . referring to fig1 through 20 , clip pusher 80 includes barrel portion 81 having a bore 82 extending therethrough , and knurled end 83 . barrel portion 81 includes slots 84 formed in either side . as clip pusher 80 is slid along wrench 50 , the lower end of each slot 84 engages a stop 56 to prevent further movement of clip pusher 80 along wrench 50 . ring 85 is disposed within knurled end 83 to frictionally engage upper shaft 57 of wrench 50 as clip pusher 80 is slid along wrench 50 . the outer surface of clip pusher 80 includes flat portions 86 at its lower end corresponding to flat portions 74 of clip holder 70 . compression screw 90 , shown in fig1 includes threaded shaft 91 which can be threaded into portion 25 of lag screw 20 , and includes slot drive 92 . other well known drives , such as the hex drive , may be used . in order to assemble compression screw assembly 10 , clip pusher 80 is mounted , knurled end 83 first , over the lower shaft 52 of wrench 50 so that flat portions 53 of wrench 50 are aligned with slots 84 of clip pusher 80 . clip pusher 80 is slid along shaft 52 of wrench 50 until slots 84 engage stops 56 of wrench 50 and ring 85 engages upper shaft 57 of wrench 50 . clip 40 then is inserted within bore 72 of clip holder 70 so that flat portions 42 of clip 40 are aligned with flat portions 74 of clip holder 70 and tangs 44 of clip 40 are disposed within grooves 75 of clip holder 70 . elongated members 43 of clips 40 are disposed under elongated members 73 of clip holder 70 . clip holder 70 , now containing clip 40 , is mounted , barrel portion 71 first , over lower shaft 52 of wrench 50 until clip holder 70 engages clip pusher 80 . once clip 40 , clip pusher 80 and clip holder 70 are in place , compression plate 30 is slid end 36 first , over lower shaft 52 of wrench 50 . wrench stabilizing rod 60 is inserted within bore 51 of wrench 50 . the threaded portion of stabilizing rod 60 is threaded within portion 25 of lag screw 20 and drive portion 24 of lag screw 20 is inserted within corresponding drive portion 54 of wrench 50 . to use the compression screw system of the present invention , the surgeon must first insert a guide wire in to the fractured bone , and then use a reamer to ream out the root diameter corresponding to the size of lag screw 20 and the opening for the outside diameter of the barrel member 31 of compression plate 30 . because stabilizing rod 60 is cannulated , compression screw assembly 10 can be inserted over the guide wire . lag screw 20 is then threaded partway into the bone by turning handle 58 of wrench 50 . compression plate 30 is slid forward over insertion wrench 50 and over shaft 22 of lag screw 20 until compression plate 20 is flush against the bone . lag screw 20 is then threaded fully into the bone to the proper depth as indicated by depth markings 55 on wrench 50 . if lag screw 20 and compression plate 30 are to be inserted so that lag screw 20 is non - rotatably secured to compression plate 30 , clip pusher 80 with clip holder 70 and clip 40 attached is pushed forward until clip holder 70 touches and centers on compression plate 30 , then pushed again , more firmly , to slide clip 40 from within clip holder 70 and into barrel member 31 of compression plate 30 so that tangs 44 of clip 40 become disposed within indentations 35 of barrel member 31 . once clip 40 is in place , clip pusher 80 and clip holder 70 are slipped back down insertion wrench 50 . stabilizing rod 60 is unthreaded from lag screw 20 and wrench 50 and stabilizer rod 60 are removed . regardless of whether clip 40 is inserted , compression screw 90 may be inserted through barrel 31 of compression plate 30 and threaded into threaded portion 25 of lag screw 20 to obtain a tight compression between lag screw 20 and compression plate 30 . once the desired amount of compression has been achieved , compression screw 90 may be removed or left in place at the option of the surgeon . finally , compression plate 30 is anchored to the bone by inserting bone screws through apertures 38 of member 37 and into the bone . | 0 |
the window unit 10 which can be seen from fig1 has a window 11 and a frame 12 . the window 11 is designed as a laminated - glass window which is made up of an outer window part 11 . 1 and of an inner window part 11 . 2 , these being permanently connected to one another by means of an intermediate layer 11 . 3 . the frame 12 is connected to the window 11 along the border region of the latter . the window unit 10 is connected to a vehicle - body part 14 by means of a bead of adhesive 13 . in that exemplary embodiment of the window unit 10 which can be seen from fig2 , the frame 11 is of two - part design and is made up of a basic frame 15 and of an additional frame 16 . on its side which is directed toward the window 11 , the basic frame 15 has an abutment surface 17 by means of which it butts against the inside 18 of the window 11 , in the border region thereof , and is permanently connected to said window by means of an application of adhesive 19 . on its outside , which is located on the right in fig2 , the basic frame 15 has a connection surface 21 . this serves for connection to the additional frame 16 . the connection surface 21 is aligned at least more or less normal to the surface of the window 11 . the additional frame 16 forms a transition from the window 11 to the vehicle - body part 14 ( fig1 ). it thus has a profile section 22 with two abutment lips 23 and 24 . the abutment lip 23 butts against the peripheral surface of the window 11 . the abutment lip 24 butts against an opposite surface section of the vehicle - body part 14 ( fig1 ). the profile section 22 is configured such that , with the window unit 10 in the installed position , the two abutment lips butt against the respectively adjacent part with a certain amount of prestressing . if the window 11 is designed as a laminated - glass window , as is illustrated in fig2 , it is expedient for the abutment lip 23 to butt against the outer window part 11 . 1 of the laminated - glass window . in the case of the additional frame 16 , the profile section 22 is adjoined by a second profile section 25 , which extends at least more or less as far as the plane of the underside of the basic frame 15 . on the side which is directed toward the basic frame 15 , said profile section 25 has a connection surface 26 which is coordinated with the connection surface 21 of the basic frame 15 . the basic frame 15 is arranged on the window 11 such that its connection surface 21 is at least more or less flush with the border of the window 11 , in particular with the border of the outer window part 11 . 1 . depending on the given features of the window 11 and / or of the vehicle - body part 14 , it may also be expedient , however , for the basic frame to be aligned with an equidistant line in relation to the border of the window 11 . the additional frame 16 is permanently connected to the basic frame 15 by means of an application of adhesive 27 , which has been provided either on the connection surface 21 or on the connection surface 26 or else on both connection surfaces . the additional frame 16 is arranged on the basic frame 15 such that its abutment lip 23 is located at least more or less level with the border of the outer window part 11 . 1 . in this way , it is easily possible to compensate , on the one hand , for window - size tolerances and , on the other hand , for tolerances relating to the course taken by the border of the window . however , it is also possible for the additional frame 16 to be aligned relative to the basic frame 15 on the basis of other aspects . the window unit 30 , which can be seen from fig3 , has the window 31 and the frame 32 . the window 31 is , once again , designed as a laminated - glass window , which has the outer window part 31 . 1 and the inner window part 31 . 2 which are permanently connected to one another by means of the intermediate layer 31 . 3 . the frame 32 , once again , is of two - part design and is made up of the basic frame 35 and the additional frame 36 . the basic frame 35 has the abutment surface 37 which is directed toward the window 31 and is permanently connected to the underside 38 of the window 31 by means of the application of adhesive 39 . on the side which is directed toward the additional frame 36 , the basic frame 35 has the at least more or less planar connection surface 41 . the connection surface 42 of the additional frame 36 butts against said connection surface 41 . provided for the purpose of connecting the two frame parts 35 and 36 are connecting elements which are formed by coordinated profile sections , on the one hand , of the basic frame 35 and , on the other hand , of the additional frame 36 . on the basic frame 35 , this profile section is formed by a recess 43 which has a mushroom - shaped outline and is open in the direction of the additional frame 36 . on the additional frame 36 , the corresponding profile section is formed by a protrusion 44 which likewise has a mushroom - shaped outline , which is coordinated with the outline of the recess 43 . the profile sections 43 and 44 are provided at least in certain regions along the longitudinal extent of the frame parts 35 and 36 . they generally extend over the entire length of the periphery of the frame parts . the basic frame 35 is arranged on the window 31 such that its connection surface 41 is flush with the border of the window 31 , in particular with the border of the outer window part 31 . 1 . on account of the interengagement of the profile sections 43 and 44 , the additional frame 36 is fixed in its position relative to the basic frame 35 and the window 11 . however , if required , the additional frame 36 may be exchanged , e . g . for a frame part of a different material or else for a frame part of a different profile , in particular of different dimensions coordinated with differing dimensions of the window 11 and / or of the vehicle - body part 14 . | 1 |
hereinafter , it will be described about the present invention with reference to the accompanying drawings in detail . fig1 is a block diagram for controlling a pulse width of a column address select signal according to an embodiment of the present invention , which will be described as follows . when a corresponding mrs code is inputted in an external chip set 100 , a cl corresponding to the code is set in a mode register set 200 . for instance , the cl is approximately 2 ˜ 9 in a high frequency dram for a graphic so that it is assumed the cl as 2 ˜ 9 in the present invention . the set cl is inputted to a pulse width control unit 3 1 0 of a column address signal generation circuit 300 for generating a column address select signal . the cls inputted in the pulse width control unit 310 have their own delay time , respectively and then a delay pulse outputted thereof is generated as the column address select signal having an optimized pulse width in the pulse width control unit 310 . fig2 a and 2b are circuit diagrams of a column address select signal generation circuit in accordance with the present invention , which will be described as follows . a first inverter i 301 inverts a read column pulse casp 6 _rd , and a second inverter i 302 inverts an output of the first inverter i 301 . moreover , a third inverter i 303 inverts a write column pulse casp 6 _wt , and a fourth inverter i 304 inverts an output of the third inverter i 303 . furthermore , a first nand gate 301 inputs an internal column access pulse icasp 6 and a column activation pulse cast 12 x and then logically combines the two signals , and a fifth inverter i 305 inverts an output of the first nand gate 301 . a first nor gate 302 inputs outputs of the second , fourth , and fifth inverters i 302 , i 304 , i 305 and then logically combines them . a delay time for an output signal s 301 of the first nor gate 302 is decided by a plurality of delay means 303 , 304 , 305 alternatively operated by a plurality of switches sw 301 to sw 304 . a first latch 308 comprised of a second nand gate 306 and a third nand gate 307 latches the output signal s 301 of the first nor gate 302 and an output signal yi_width of the pulse width control unit 310 . here , the second nand gate 306 inputs the output signal s 301 of the first nand gate 302 and an output signal s 303 of the third nand gate 307 , and the third nand gate 307 inputs an output signal s 302 of the second nand gate 306 , the output signal yi_width of the pulse width control unit 310 , and a power - up signal pwrup . the pulse width control unit 310 inputs the plurality of cls applied from the mode register set 200 and controls a pulse width of the output signal s 302 of the second nand gate 306 according to the delay time by the cls . as a result , the output signal yi_width is outputted . the fourth nand gate 309 inputs the output signal s 302 of the first latch 308 and the output signal yi_width of the pulse width control unit 310 and then logically combines them . sixth to eighth inverters 1306 to 1308 invert and delay an output signal of the fourth nand gate 308 , to output a column address select signal yi . it will be explained of a method for driving the column address signal generation circuit according to the present invention constructed as described above . when the read column pulse casp 16 _rd or the write column pulse casp 6 _wt is applied to a high state , or the internal column access pulse icasp 6 and the column activation pulse cast 12 x are applied to a high state at the same time , the first nor gate 302 logically combines them , to output a low state pulse s 301 . the output pulse s 301 of the first nor gate 302 maintaining a low state is inputted into the second nand gate 306 of the first latch 308 , and the second nand gate 306 outputs a high state output signal s 302 . the output signal s 302 of the second nand gate 306 maintaining a high state is inputted into the third nand gate 307 and the pulse width control unit 310 . when the output signal s 302 of the first latch 308 is inputted , the pulse width control unit 310 sets a corresponding path according to the cl inputted from the mode register set . accordingly , the output signal yi_width of which the pulse width is controlled by passing through an appropriate delay time according to the cl , is outputted . in addition , the fourth nand gate 309 receives the output signal s 302 of the first latch 308 and the output signal yi_width of the pulse width control unit 310 and logically combines them to output a low state pulse . the output pulse of the fourth nand gate 309 maintaining a low state outputs a high state column address select signal yi through the sixth to eighth inverters i 306 to i 308 . on the other hand , the output signal of the pulse width control unit 310 is inputted into the third nand gate 307 with the output signal s 302 of the second nand gate 306 and the power - up signal pwrup and then is logically combined . the output signal s 303 of the third nand gate 307 is inputted into the second nand gate 306 . fig3 is a circuit diagram of the pulse width control unit of fig2 . the pulse width control unit according to the present invention is comprised of : a plurality of delay means 311 to 318 connected in series for delaying an input signal in ; a plurality of transmission gates t 311 to t 318 as a plurality of switching means for setting a delay path by being driven according to each cl which is inverted by each cl and inverters i 311 to i 318 ; and an inverter i 319 for inverting a signal delayed through each delay means 211 to 214 . the pulse width control unit constructed as described above controls a delay time of an output signal out by deciding a delay path according to the cl . for instance , when the cl set in the mode register set is 6 , only cl 6 is applied to a high state , and the other cls are all applied to a low state . the fourth transmission gate t 314 is turned on by the cl 6 applied to a high state and a signal inverted to a low state by the fourth inverter i 314 . accordingly , the input signal in is delayed through the first to fourth delay means 311 to 314 , and the delayed signal is inverted through the inverter i 319 , to be outputted as the output signal out . as the cl is decreased , the delay time is longer , which results in an increase of the pulse width . as aforementioned , it is possible to generate the pulse with a variable width according to the operation frequency by analogizing the operation frequency of the dram by means of using the cl set in a mode register set , and controlling the pulse width by means of a delay time according to the cl . therefore , the circuit for controlling the pulse width can be applied to a next generation standard dram such as a high speed ddr 2 or ddr 3 as well as a high speed graphic dram for supporting various cls . although the present invention has been described in connection with the embodiment of the present invention illustrated in the accompanying drawings , it is not limited thereto . it will be apparent to those skilled in the art that various substitutions , modifications and changes may be made thereto without departing from the scope and spirit of the invention . | 6 |
referring to the figures , fig1 illustrates a rotary - wing aircraft 2 incorporating a composite structure 4 ( fig5 ) according to an embodiment of the invention . while embodiments of the invention are shown and described with reference to a rotary - wing aircraft 2 and are particularly suited to a rotary - wing aircraft 2 , aspects of this invention can also be used in other configurations and / or machines such as , for example , automotive applications including commercial and military ground vehicles , building structures , construction applications such as infrastructure , cargo applications , oil and gas industrial applications , shipping applications including containers for rail , marine and aircraft , fixed - wing aircraft applications , non - rotary - aircraft applications , high speed compound rotary wing aircraft with supplemental translational thrust systems , dual contra - rotating , coaxial rotor system aircraft , turbo - props , tilt - rotors and tilt - wing aircraft . as illustrated in fig1 , rotary - wing aircraft 2 has a main rotor system 6 and includes an airframe 8 having an extending tail 10 which mounts a tail rotor system 12 , such as an anti - torque system . the main rotor system 6 is shown with a multiple of rotor blades 14 mounted to a rotor hub . the main rotor system 6 is driven about an axis of rotation r through a main gearbox by one or more engines 16 . the composite structure 4 of the present disclosure may be incorporated into the aircraft as part of the airframe 8 or any other internal or external part of the aircraft where high strength - to - weight ratios are desired . the composite structure 4 of the present disclosure may be assembled as a sandwich structure having a multiplicity of layers with a multiple of prepreg plies bonded together and co - cured at the same time through an autoclave process to form a multi - laminate assembly . the composite structure 4 may be manufactured in a single curing process using an autoclave processing but other processing techniques may be utilized . fig2 - 5 illustrate a composite structure 4 at various stages of a method for forming the composite structure according to one embodiment of the present disclosure . referring to fig2 , a core 18 is placed in tension or compression ( arrows a ) in at least one direction . the core 18 may be placed in tension or compression until it reaches a known dimension . for example , the core 18 may be stretched ( placed in tension ) until it reaches a dimension that is at or near 8 % larger than the original dimensions in the direction that the force has been applied . alternatively , the amount of tensile or compressive force exerted on the core 18 is known . when the desired parameter is reached , ( dimension of core , force applied , etc . ), the core 18 is held in place by a clamping device 20 . the core 18 may be any shape or thickness formed from material suitable for use as a lightweight , high - strength core of a composite structure . for example , the core may be formed from a kevlar ® honeycomb material having a density of 4 . 5 pcf or greater . as shown in fig3 , with the core 18 held in tension or compression by the clamping device 20 , a first layer 22 is applied to a first surface 18 a of the core 18 . in the illustrated example , a second surface 18 b of the core 18 remains exposed . the first layer 22 may be , for example , a film adhesive . in other examples , the first layer may comprise a plurality of plies that may include prepreg , fiber composites , low - resin films , additional adhesive films , and / or other features known in the art . referring to fig4 , the first layer 22 and the core 18 are then co - cured by application of heat from a heat source 24 . in some examples , the first layer 22 and the core 18 are partially cured . once the first layer 22 and the core 18 have been cured or partially cured , e . g ., for a predetermined amount of time at a predetermined temperature , the core 18 is released from the clamping device 20 . referring to fig5 , when the core 18 is placed in tension while the first layer 22 is applied , residual stresses from the forces applied to the core 18 ( see fig2 ) will typically cause the core 18 to bow in a convex direction with respect to the first surface 18 a , while a compressed core 18 will typically expand faster than the first layer 22 forming a concave shape at the first surface 18 a . if desired , a second layer 26 may then be applied to a second surface 18 b of the core 18 , opposite the first layer . as with the first layer 22 , the second layer 26 may comprise a plurality of plies . for example , the second layer 26 may include anti - saddling strips to prevent the core 18 from losing the desired shape over time . the second layer may 26 then be cured , or co - cured with the partially cured core 18 and first layer 22 . the resulting contoured shape of the sandwich composite structure 4 will vary with the chosen core material and the selection of the first layer 22 , and may be affected by the amount of curing . however , where the distribution of stresses throughout the core 18 is homogenous or substantially homogenous , the resulting shape shown in fig5 can be predicted . to improve the homogeneity of the residual stresses in the core 18 , the core material may be cured or partially cured prior to the application of the compressive or tensile forces . the method described herein is useful in the formation of composite structures comprising a core . in particular , the method is useful for forming composite structures where the core is stiff and difficult to place on a mandrel or in a mold . this allows the use of less expensive core materials currently available on the market while reducing the amount of defects and wasted material . in addition , the method of the present disclosure reduces the need for expensive tooling used to place the composite structure in a particular shape . the method described herein may be used on a composite structure , as described above , or on a portion of a composite structure . for example , where a particular structure comprises a complex curvature , different regions of the core may be placed in tension or compression and clamped into place . fig6 a illustrates another embodiment in which a core 18 has a first region 28 and a second region 30 . the first region 28 is placed in compression and the second region 30 is placed in tension . the core 18 is then held in placed by clamping devices 20 . a first portion 22 ′ of a first layer 22 is applied in the first region and a second portion 22 ″ of the first layer 22 is applied in the second region 30 . fig6 b shows the resulting composite structure 4 after applying heat to cure or partially cure the core 18 and the first layer 22 , releasing the clamping devices 20 , and applying the second layer 26 and applying additional heat . note that the curvature of the first region 28 is opposite the direction of the curvature of the second region 30 . other configurations are also possible . the regions of the core 18 may include flat regions . the various regions may be formed with curvatures in the same direction but varying by the extent of the curvature . while the invention has been described with reference to an exemplary embodiment or embodiments , it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention . in addition , many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from the essential scope thereof . also , in the drawings and the description , there have been disclosed exemplary embodiments of the invention and , although specific terms may have been employed , they are unless otherwise stated used in a generic and descriptive sense only and not for purposes of limitation , the scope of the invention therefore not being so limited . moreover , the use of the terms first , second , etc ., do not denote any order or importance , but rather the terms first , second , etc . are used to distinguish one element from another . furthermore , the use of the terms a , an , etc . do not denote a limitation of quantity , but rather denote the presence of at least one of the referenced item . | 1 |
fig1 shows a perspective view of an intelligent locker system , in accordance with certain preferred embodiments of the present invention . the intelligent locker system 20 includes a cabinet 22 having a plurality of locker openings 24 . each opening 24 is covered by a door 26 hingedly connected to the cabinet . the intelligent locker system also includes a central controller , commonly referred to by the assignee as a customer service station ( css ) 28 . in the particular embodiment shown in fig1 the intelligent locker system includes two vertically - extending columns of locker openings , each column having a series of vertically aligned openings . in the particular embodiment shown , the locker system has a first column of four locker openings , and a second column of three locker openings and one customer service station . the capacity of the locker system may be increased by adding another locker cabinet 22 to the left or right of that shown in fig1 . thus , additional locker cabinets 22 may be added to the system for increasing overall capacity . fig2 shows a front view of the customer service station 28 shown in fig1 . the customer service station 28 includes a video monitor 30 , a speaker 32 , and a series of keypads 34 for inputting information into the customer service station 28 . the customer service station 28 also includes an opening 36 for receiving money , such as coins or dollar bills . the opening 36 may also be adapted to receive magnetic cards , credit cards , smart cards or any other mode of making payment to the system . the customer service station 28 also preferably includes a biometric scanning device 38 used to scan one or more biometric characteristics of a user . in the particular preferred embodiments shown in fig2 the biometric scanner 38 is used to scan the fingerprint of a user . in other embodiments , the scanner 38 may record other physical characteristics of a user , such as a user &# 39 ; s iris . the system may also identify the user by using a pin code , a smart card , a magnetic card , a bar code or an embedded chip . fig3 shows a top view of the intelligent locker system shown in fig1 . at each level of the locker cabinet 22 , a set of doors 40 a and 40 b are hingedly attached to cabinet 22 . the doors desirably open away from one another , and preferably selectively cover the cabinet openings 24 a and 24 b . a central wall 42 extends between each locker opening so as to define distinct locker areas 44 a and 44 b . each locker area is defined by central wall 42 , a portion of rear wall 46 and a sidewall 48 . as mentioned above , the pair of hingedly connected doors 40 a and 40 b are designed to open away from one another . first door 40 a is hingedly connected to cabinet 22 by hinge 50 a . similarly , second door 40 b is hingedly connected to cabinet 22 by hinge 50 b . each door 40 a , 40 b also may include a resilient or spring element that normally maintains the door in a slightly open position . thus , a potential user of the intelligent locker system can visually discern whether a particular locker opening is available for use . a depressible button 52 a , 52 b is located adjacent each locker opening 24 a , 24 b . as will be explained in more detail below , when button 52 is depressed , the customer service station 28 is alerted that a user is holding one of the locker doors 40 in a closed position . the intelligent locker system also includes an intelligent locking device 54 having a printed circuit board 56 with a microprocessor secured therein . the intelligent locking device 54 includes two sets of retractable bolts . the first set of retractable bolts unlocks and locks the door 40 a closable over the first locker area 44 a and the second set of retractable bolts unlocks and locks the door 40 b closable over the second locker area 44 b . fig4 shows a fragmentary front view of the intelligent locker system of the present invention . in particular , fig4 shows one level of the locker cabinet 22 including first locker opening 24 a and second locker opening 24 b . adjacent central wall 42 , each locker opening has a flange 58 a , 58 b for supporting depressible buttons 52 a and 52 b . the intelligent locker system includes intelligent locking device 54 secured inside central wall 42 . the intelligent locking device includes a light emitting element 60 that is preferably exposed at the front surface of the locker cabinet 22 . in certain preferred embodiments , the light emitting element 60 is a two - color led that informs users of the intelligent locker system whether a locker is unlocked , locked , or in the process of being unlocked or locked . in one particular preferred embodiment , when locker space 24 is available for use , the light emitting element 60 emits green light . however , when a user places articles within the space 24 and closes the door ( not shown ), the light emitting element 60 will emit a red light that flashes on and off . the red light will continue to flash until the user has deposited money into the customer service station 28 and entered the required authenticating information ( e . g ., biometric , pin code ) into the system . once the user has entered the necessary information at the customer service station 28 , the intelligent locking device 54 will lock the door and the light emitting element 60 will emit a solid red light , indicating that the door covering the locker space 24 is locked . the led 60 will continue to emit a solid red light until the authorized user interacts with the customer service station 28 to unlock the door . at that time , the light emitting element 60 will emit green light . fig5 shows a top , cross - sectional view of an intelligent locking device 54 , in accordance with certain preferred embodiments of the present invention . the intelligent locking device includes a smart card 56 with a microprocessor that controls operation of the device . the smart card 56 has at least one communication line 62 attached thereto for sending and receiving information related to opening and closing locker doors . the smart card 56 preferably has a program stored therein for operating the intelligent locking device . the intelligent locking device includes a first set of retractable bolts 64 , including forward bolt 64 a and rear bolt 64 b , and a second set of retractable bolts 66 , including forward bolt 66 a and rear bolt 66 b . a front wall 68 of the intelligent locking device 54 includes the light emitting element 60 . as mentioned above , light emitting element 60 is capable of emitting various colors of light , such as green , amber and red for indicating the locked / unlocked status of the locker . the light emitting element may provide a solid stream of light or may blink on and off . the intelligent locking device 54 also preferably includes a first motor and associated driver 70 a for opening and closing the first set of retractable bolts 64 , and a second motor 70 b and associated driver for opening and closing the second set of retractable bolts 66 . the light emitting element 60 , and the first and second motor 70 a and 70 b are preferably in communication with smart card 56 . the first and second sets of bolts 64 , 66 are preferably independent from one another . in other words , one set of bolts may be in the retracted or unlocked position while the other set of bolts may be in the extended or locked position . moreover , both sets of bolts may simultaneously be in the unlocked position or the locked position . in the particular embodiment shown in fig6 the first set of bolts 64 are retracted in the unlocked position , while the second set of bolts 66 are in the extended , locked position . the unlocked / locked status of the bolts 64 , 66 , is at all times relayed to smart card 56 which in turn relays the information to the customer service station ( not shown ) via communication line 62 . as a result , the customer service station is able to monitor the status of each locker opening . this information may be compiled by the customer service station and transmitted to a central location via a wide variety of communication channels , such as telephone lines . as a result , the operation of a plurality of intelligent locker systems at a plurality of different locations may be monitored at one central location . fig7 shows a front view of intelligent locking device 54 , including a first light emitting element 60 a linked with the position of the first set of retractable bolts 64 and a second light emitting element 60 b linked with the position of the second set of retractable bolts 66 . thus , the first led 60 a shows the lock / unlock status of the first set of bolts 64 while the second led 60 b shows the lock / unlock status of the second set of bolts 66 . fig8 shows a local area network ( lan ) 72 used to interconnect the plurality of intelligent locking devices 54 with the central controller or customer service station 28 . the intelligent locking devices 54 may be connected in series with one another and with the customer service station 28 via a first network line 72 . the intelligent locking devices 54 may also be connected in parallel with the customer service station 28 via communication lines 72 ′. in other preferred embodiments , fiber optic cables may replace the communications lines 72 , 72 ′. in still other embodiments , the intelligent locking devices 54 may communicate with the customer service station 28 via radio waves . using the local area network shown in fig8 the customer service station 28 for each intelligent locker system is able to monitor the status of each intelligent locking device 54 . the particular status for each intelligent locking device 54 is preferably compiled by the printed circuit board 56 disposed therein . this information is then periodically sent via communication lines 72 to the customer service station 28 . the customer service station 28 preferably stores this information in a memory device ( not shown ). the information may be sent to a central location that compiles information from many different locations . the information may be transmitted via an uplink 84 . the transmitted information may include the amount of money collected , the percentage of lockers in use , and whether any of the lockers require maintenance . referring to fig1 - 11 , in operation a user will approach a particular locker opening 24 b in order to store one or more articles in locker space 44 b . as mentioned above , in its normal position , door 40 b is preferably slightly ajar . door 40 b includes one or more openings or recesses 74 adapted to receive one of the retractable bolts 64 , 66 when the retractable bolts are extended . the intelligent locking device 54 shown in fig9 is a simplified view of the system does not show the printed circuit board and the motor and driving mechanism for opening and closing retractable bolt 66 . adjacent locker opening 24 b , depressible button 52 b is held by flange 76 . depressible button 52 is movable between an extended position and a depressed position . when door 40 b is closed , inner surface 78 of door 40 b abuts against depressible button 52 b so as to depress the button . upon being depressed , a signal is sent to the printed circuit board of the intelligent locking device 54 , thereby informing the printed circuit board that the door 40 b of locker opening 24 b has been closed . fig1 shows a fragmentary view of the locker immediately after door 40 b has been closed and button 52 has been depressed , but before retractable bolt 66 has move into the extended position for locking the door 40 b . when door 40 b is initially closed , inner surface 78 of door 40 b depresses button 52 b , thereby sending a signal to the printed circuit board of the intelligent locking device 54 , the signal indicating that door 40 b has been closed . after a predetermined period of time , such as approximately 2 - 10 seconds , the printed circuit board will send a signal to the motor 70 b to move the bolt 66 into the extended , locking position . referring to fig1 , as motor 70 b moves bolt 66 into the extended , locking position , bolt 66 slides into recess 74 formed in the edge of door 40 b . once the bolt 66 extends completely into the locked position , light emitting element 60 emits a solid red light , thereby providing a visual indicator that door 40 b has been locked . referring to fig1 - 11 , in other preferred embodiments of the present invention , a user of the intelligent locker system 20 will approach cabinet 22 . the user will observe whether one of the locker openings 24 is available for use . the user will then open the door 40 of the locker opening 24 and place articles for storage within the locker area 44 . a user may also confirm that a locker is open and available for use by referring to one of the light emitting elements of the intelligent locking device 54 . if the light emitting element is a particular color , such as green , the color provides a visual indication that the locker is available . each locker opening 24 preferably has its own light emitting element 60 assigned thereto . in other preferred embodiments , each locker has two or more light emitting elements 60 . after the user places the articles within the locker opening 24 , the user will close the door 40 so as to depress depressible button 52 . upon being depressed , a signal will be sent to the printed circuit board 56 of the intelligent locking device 54 that the locker door 40 is being held in a closed position . after approximately 2 - 10 seconds , the printed circuit board 56 will send a signal to motor 70 to move retractable bolts 64 into the extended , locking position . as the retractable bolts move into the locking position , the bolts will slide into the recess 74 formed at the edge of door 40 . at the same time , light emitting element 60 will change from emitting a solid green light to a flashing amber or red light . the printed circuit board 56 will then send a communication to the customer service station 28 that the particular door has been closed . the user will then proceed to the customer service station 28 shown in fig2 . the customer service station will ask the user which language the user prefers . the user will then touch the video screen 30 or enter information into the system using keys 34 . during the initial transaction , the customer service station may ask the user how long he or she desires to use the locker space . the customer service station will then calculate how much the user owes . this amount may be deposited in the form of coins or bills through slot 36 . slot 36 may also be adapted to receive credit cards , magnetic cards , smart cards or any other form of payment . the user will then submit biometric data or other authenticating data to the system . in one particular preferred embodiment , the user places a fingerprint over the biometric sensor 38 . the sensor 38 will then scan the fingertip pattern and record it within a memory device . once the initial transaction is complete , the extendable bolt of the intelligent locking device will remain in the locked position and the light emitting element 60 will transform from emitting a blinking red light to a solid red color . later , when the user desires to remove the stored articles from the locker , the user will approach the customer service station 28 . the user will place his or her fingerprint over the biometric scanner 38 so that the scanner may obtain a copy of the user &# 39 ; s fingerprint . in highly preferred embodiments , the fingerprint data includes information related to the electrical capacitance of the ridges and valleys of the fingerprint . the scanned fingerprint will then be compared with the fingerprint stored in the memory of the customer service station . the processor of the customer service station will associate the retrieved fingerprint with a particular locker number for that fingerprint . once a link or association has been made between the retrieved fingerprint and the locker associated therewith , the bolts of the intelligent locking device for that particular locker will retract , thereby unlocking the locker door 40 . at that time , the light emitting element 60 will change from emitting a solid red light to a solid green light . once the bolt ( s ) retract , the locker door 40 will return to its normally partially ajar orientation . the user may than proceed to the locker opening to remove the articles stored in the locker . although the above described embodiment utilizes a biometric scanner to obtain fingerprints , it is contemplated that other forms of identification may be used for opening and closing the lockers . for example , the biometric sensor 38 may scan another characteristic of a user &# 39 ; s body , such as scanning a user &# 39 ; s eye or other distinguishing feature of the body . the customer service station may also utilize pin codes , magnetic cards , embedded chips or other means for authenticating users . shown below are tables that detail message type and exchanges that form the implementation of the protocol . although the present invention has been described with reference to particular preferred embodiments , it is to be understood that the embodiments are merely illustrative of the principles and application of the present invention . for example , the system can be used for any type of enclosable space , such as a room or closet . the system may also be used in any type of environment where enclosed spaces must be locked and unlocked , such as offices , hotel rooms , storage facilities , post office boxes and the like . it is therefore to be understood that numerous modifications may be made to the preferred embodiments and that other arrangements may be devised without departing from the spirit and scope of the present invention as defined by the claims . | 6 |
the foregoing description of the specific embodiments will so fully reveal the general nature of the embodiments herein that others can , by applying current knowledge , readily modify and / or adapt for various applications such specific embodiments without departing from the generic concept and therefore , such adaptations and modifications should and are intended to be comprehended within the meaning and range of equivalents of the disclosed embodiments . it is to be understood that the phraseology or terminology employed herein is for the purpose of description and not of limitation . therefore , while the embodiments herein have been described in terms of preferred embodiments , those skilled in the art will recognize that the embodiments herein can be practiced with modification within the spirit and scope of the appended claims . as used herein , “ small ” vessel is small relative to the large un - stirred or less stirred reactors . “ small ” is to be quantified as that size in a given throughput which provides less than 10 minute residence time , preferably less than 5 minute , while sizes of other bigger vessels / reactors in the line with same throughput will be proportionate with the higher residence times as chosen . as used herein , the term “ vigorously ” stirred vessel means wherein the stirring speed of vessel is about 400 to about 1000 rpm . as used herein , the term “ additive ” includes all possible additives which may or may not react with monomer . in accordance with the present invention there is provided a continuous polymerization process for manufacturing a condensation polymer . the process comprising the following steps : first step is employing an assembly comprising at least one initial reactor vessel , at least one final reactor vessel and optionally at least one intermittent reactor vessel . second step is connecting said reactor vessels to each other through one or more transfer lines for leading the reactive materials from one vessel to another . third step is adding the reactant components to at least one of the initial reactor vessels . fourth step is optionally adding additives to any of said reactor vessels or in the transfer lines . fifth step is stirring the reactive materials relatively vigorously in the intermittent reactor vessel after the addition of the additives . typically , the step of vigorous stirring is carried out at a speed of about 400 to about 1000 rpm for a period less than 10 minutes , preferably less than 5 minutes . next step is optionally stirring the reactive materials relatively mildly in the initial reactor vessel . typically , the step of mild stirring is carried out at a speed less than 200 rpm . finally the intermediates are obtained from at least one of the intermittent reactor vessel and the reaction product is obtained from the final reactor vessel . in accordance with the present invention the polymerization is carried out at a temperature not lower than 285 deg c . the additive used in the polymerization process in accordance with the present invention is carbon black with a particle size within the range of about 0 . 02 to about 1 microns . in accordance with another embodiment of the present invention the additive is a co - monomer containing a sulphonic acid group and which is capable of attaching to a cationic dye . the co - monomer employed is at least one selected from the group consisting of 5 - sulfoisophthalic acid ( sipa ), 5 - sulfoisophthalic acid dimethyl ester ( sipm ), 5 - sulfoisophthalic acid diglycolate ( sipeg ) and alkali metal salts thereof . in accordance with another aspect of the present invention there is provided a condensation polymer made from said continuous polymerization process . in accordance with still another aspect of the present invention there is provided a yarn having filament breakage less than about 20 to about 30 % made from said continuous polymerization process of any of the preceding claims . in accordance with yet another aspect of the present invention there is provided a process for making a yarn from a condensation polymer wherein the spin pack pressure rise rate is attenuated by about 25 to about 35 %. in accordance with another aspect of the present invention there is provided a system for carrying out the continuous polymerization process comprising : a . at least one initial reactor vessel ; b . at least one final reactor vessel ; c . optionally at least one intermittent reactor vessel ; d . transfer lines for connecting the reactor vessels ; and e . vigorous stirring means fitted in at least one of the intermittent reactor vessel . typically , the system further comprises mild stirring means fitted in at least one of the initial reactor vessels . according to present invention , at least one vigorously stirred vessel ( intermittent reactor vessel ) is employed in a polymerization line that is otherwise devoid of reactors , to allow injection of additive solution in the oligomer while it is undergoing intense mixing . it works by immediate dispersion of the fluid additive into the oligomer , before the heat transfer from oligomer to additive droplet can cause freezing of oligomer at the interface of the additive fluid droplets . the stirring speed of vessel is about 400 to about 1000 rpm . reduction in the rate of pressure rise up to 25 % and reduction in the rate of broken filament during melt spinning up to 20 % is achieved due to uniformity in the product obtained by such mixing . this vessel eliminates need of any other moving parts in reactor and reduces expenditure . in one of the preferred embodiments a continuous polymerization process is provided to manufacture a semi - dull cationic dyeable polyalkylene terephthalate . particularly , a continuous polymerization process to manufacture a semi - dull cationic dyeable polyalkylene terephthalate where alkali metal salt of 5 - sulfoisophthalic acid dimethyl ester is converted to an alkali metal salt of 5 - sulfoisophthalic acid diglycolate through a tranesterification reaction in at least one of an excess alkylene glycol is provided . reduction in the rate of pressure rise during melt spinning , as well as reduction in broken filaments of textured yarn , is achieved while using cationic dyeable polyester is made in a continuous process that employs additive injection into oligomer in a stirred vessel . then the additive such as tio 2 slurry in a glycol is added into a purified terephthalic acid ( pta ) slurry in at least one glycol or into an oligomer formed . here , tio 2 is added first to the purified terephthalic acid slurry followed by addition of alkali metal salt of 5 - sulfoisophthalic acid diglycolate to said oligomer after the transesterification . the mole ratio of alkylene glycol to purified terephthalic acid is around 2 . an especially fine dispersion of pta - meg slurry ( obtained through an otherwise known centrifugal separation / recirculating system ) being added to pta - meg slurry , 20 % converted sipeg solution addition to molten oligomer undergoing intense mixing in highly agitated vessel in the continuous polymerization line . about 15 % to 45 % of converted solution of alkali metal salt of 5 - sulfoisophthalic acid diglycolate is injected into a oligomer transferline , alkali metal salt of 5 - sulfoisophthalic acid diglycolate undergoes mixing with oligomer in a stirring vessel placed within oligomer transfer line . about 10 to 100 ppm of phosphoric acid is added in the oligomer transfer line . use of phosphoric acid eliminates need of other additives like peg . elimination of addition of peg which is thermally sensitive , thereby enabling the use of higher polymerization temp (˜ 295 ° c .) and hence provides higher productivity . the stirring speed inside the vessel may be about 400 to about 1000 rpm . in another aspect polyalkylene terephthalate yarn made from a semi - dull cationic dyeable polyalkylene terephthalate is provided . the cationic dyeable polyalkylene terephthalate is manufactured through a continuous polymerization process , the process including : converting a alkali metal salt of 5 - sulfoisophthalic acid dimethyl ester to a alkali metal salt of 5 - sulfoisophthalic acid diglycolate through a transesterification reaction in at least one of excess alkylene glycol ; adding additive slurry in a glycol into a purified terephthalic acid ( pta ) slurry in at least one glycol or into an oligomer formed therefrom ; injecting about 15 % to 45 % of converted solution of the alkali metal salt of 5 - sulfoisophthalic acid diglycolate into a oligomer transferline wherein the alkali metal salt of 5 - sulfoisophthalic acid diglycolate undergoes mixing with the oligomer in a stirring vessel placed within the oligomer transfer line . in other possible embodiment , there can be additives which do not react with the monomer and hence do not convert into such a derivative as the glycolate but only remain soluble . in a further possible embodiment , there can also be additives which neither react nor dissolve in the monomer but some complex or may even remain as neutral slurry and added through the stirred vessel . in accordance with the preferred embodiment of the present invention carbon black slurry and small part of mono - ethylene glycol are added to oligomer at 290 deg c . in the small vessel at 400 - 1000 rpm vessel speed . this gives fine dispersion in high shear zone of stirred vessel by breaking the drop into small particles . in further embodiment , a cationic dyeable polyester manufactured using vigorously stirred small vessel is provided where spin pack pressure rise of only 5 bars / day for poy 128 / 72 is required and filament breakage is reduced to 10 per bobbin . while considerable emphasis has been placed herein on the specific features of the preferred embodiment , it will be appreciated that many additional features can be added and that many changes can be made in the preferred embodiment without departing from the principles of the invention . these and other changes in the preferred embodiment of the invention will be apparent to those skilled in the art from the disclosure herein , whereby it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the invention and not as a limitation . | 2 |
[ 0020 ] fig1 illustrates the manner of use of the present invention bag holder 10 , with a bag 20 mounted thereto . a grounds maintenance person 15 is illustrated in dashed lines . bag holder 10 is comprised of a hoop 25 which , in this embodiment , is formed as a substantially circular ring of approximately 18 inches in diameter , “ d ”, ( see fig2 ). the diameter of hoop 25 is selected so that the person &# 39 ; s arm 16 can easily reach across hoop 25 to a handle 30 . referring now to fig2 the rim of hoop 25 is approximately { fraction ( 5 / 16 )} inch in thickness , “ t ”, in the preferred embodiment . hoop 25 is preferably formed from a lightweight material or it could alternatively be formed from a metal material for greater strength , as long as the weight thereof is not excessive . a suitable lightweight material is polyvinyl plastic resin . hoop 25 could also be alternatively formed as a hollow tubular ring . handle 30 is fixedly connected to and depends from hoop 25 along a portion of the inner edge of hoop 25 to provide a thin , substantially flat member that is easily grasped by one hand 16 of person 15 . handle 30 is connected to hoop 25 by welding , screws , or other convenient means . as seen in fig1 hoop 25 is held in a secure relationship resting on or against the hip of person 15 with a first hand 16 on handle 30 thereby leaving the other hand 17 free . free hand 17 can be used to manipulate a trash pick up stick 18 , or other means to pick up items for deposit in bag 20 . [ 0023 ] fig2 clearly illustrates a top view of bag holder 10 of the present invention . handle 30 receives a pair of cords 45 , 46 of predetermined length , each of which is passed through a respective one of holes 40 , 41 in handle 30 . as more clearly seen in the enlarged , fragmentary detail section view of fig3 a first end of typical cord 46 passes through respective hole 41 in handle 30 . knot 50 , or other suitable means , is formed at the end of cord 46 for preventing cord 46 from being pulled through hole 41 . cords 45 , 46 are of sufficient length for each cord to reach approximately half way around the circumference of hoop 25 . cords 45 , 46 are located on opposed ends of handle 30 . a predetermined number ( typically three per cord ) of commercially available spring clips 55 are fixedly secured along the length of cords 45 , 46 . when not in use to secure bag 20 to hoop 25 , cords 45 , 46 and spring clips 55 hang from handle 30 . spring clips 55 are of sufficient size to clamp bag 20 to hoop 25 when invention bag holder 10 is in use . referring again to fig1 in using bag holder 10 , a person 15 will insert a bag 20 through the center of hoop 25 and fold a lip portion 20 a thereof over hoop 25 . lip portion 20 a is typically folded over hoop 25 by a length of three to ten inches . this three to ten inch lip , once bag 20 is filled and removed from hoop 25 , is used to close bag 20 . bag 20 can be knotted , closed with a tie , or closed with drawstrings provided in the mouth thereof for closing of bag 20 . once bag 20 has been mounted on hoop 25 so that three to ten inches laps over hoop 25 , cords 45 , 46 are situated and clips 55 are utilized to clip bag 20 to hoop 25 in several separated locations ( see fig1 ). referring again to fig1 person 15 will now hold bag holder 10 and bag 20 against his body and the other side , preferably at handle 30 , in his hand 16 . such positioning will situate bag 20 conveniently with an open top for inserting trash , yard debris , or other items being collected therein . once bag 20 is filled or the pick up job is completed , clips 55 are removed and remain suspended by cords 45 , 46 from handle 30 , and the top of bag 20 is then closed by conventional means . while not shown , it is within the scope of the invention to make hoop 25 with a larger or smaller diameter so that various size bags 20 can be accommodated . also , hoop 25 , rather than being circular in shape , could be formed elliptical , rectangular , or square , as long as a conventional bag could be mounted thereon as previously described . the above detailed description of a preferred embodiment of the bag holder invention has set forth the best mode contemplated by the inventor for carrying out the invention at the time of filing this application and is provided by way of example and not as a limitation . accordingly , various modifications and variations , obvious to a person of ordinary skill in the art to which it pertains , are deemed to lie within the scope and spirit of the invention as set forth in the following claims . | 1 |
fig1 shows a snow bicycle ( 10 ) according to a possible embodiment of the present invention . the bicycle ( 10 ) comprises a main frame ( 12 ) which may be , as illustrated , substantially similar to a conventional bicycle frame . this main frame ( 12 ) comprises a down tube ( 14 ), a seat tube ( 16 ) for supporting a seat ( 18 ), a front head tube ( 20 ) , handlebars ( 22 ) and a rear chain stay ( 24 ). the rear chain stay ( 24 ) comprises a left and a right pipe extending towards the rear . the main frame ( 12 ) may also comprise a lockable hinge ( 32 ) located on the down tube ( 14 ) for collapsing the main frame ( 12 ). the snow bicycle ( 10 ) is called as such because it is primarily designed for the winter season . however , it is possible to use the bicycle ( 10 ) during other seasons . for instance , it is possible to use the bicycle ( 10 ) on conventional dry pavement , mud or grass . it must be understood that the term &# 34 ; snow &# 34 ; should not be interpreted as being restrictive . the front of the main frame ( 12 ) is supported by a front steerable supporting assembly that is operatively connected to the head tube ( 20 ). this assembly is actuated by the user through the handlebars ( 22 ). depending on the nature of the ground on which the bicycle ( 10 ) will travel , it is possible to choose among a plurality of removable implements such as a ski assembly ( fig1 ), a single ice blade assembly ( fig5 ), a pair of opposite ice blades assembly ( fig6 ) and a wheel ( fig7 ). those implements will be described later . since the bicycle ( 10 ) is human - powered , it comprises a pedal drive assembly ( 34 ) operatively connected to the main frame ( 12 ). the pedal drive assembly ( 34 ) comprises opposite pedals ( 36 ) that are operatively connected to a pivot ( 38 ) located in the lower side of the main frame ( 12 ). the bicycle ( 10 ) further comprises a rear drive wheel unit ( 40 ) that is preferably removably connected to the main frame ( 12 ) for easing the storage or the transportation by hand . alternatively , one can construct the bicycle ( 10 ) without making the rear drive wheel unit ( 40 ) removable . the rear drive wheel unit ( 40 ) comprises a drive wheel frame ( 42 ) having two parallel sections ( 44 , 46 ) respectively aligned with the left and the right pipe of the chain stay ( 24 ). each section ( 44 , 46 ) comprises an oblique member ( 48 , 50 ) downwardly projecting towards the rear and a substantially horizontal member ( 52 , 54 ). the rear end of each horizontal member ( 52 , 54 ) is connected to a lower end of the corresponding oblique member ( 48 , 50 ). preferably , the left section ( 44 ) and the right section ( 46 ) are substantially symmetrical with reference to a vertical plane . the drive wheel frame ( 42 ) is removably connected to the chain stay ( 24 ). one possible way is to provide a plurality of slots ( 56 ) and corresponding fasteners ( 58 ). it is then possible to connect the upper end of the oblique members ( 48 , 50 ) to the chain stay ( 24 ) and to connect the front end of the horizontal members ( 52 , 54 ) to vertical side plates ( 30 ) that are extending downwardly and rigidly connected to the left pipe ( 26 ) or the right pipe ( 28 ), respectively . the drive wheel frame ( 42 ) further comprises a first longitudinally - oriented wheel ( 60 ) operatively connected between the two sections ( 44 , 46 ) by means of a pivot ( 62 ). then , a second longitudinally - oriented wheel ( 64 ) is provided and is operatively connected between the two sections ( 44 , 46 ) by means of a pivot ( 66 ). the second wheel ( 64 ) is longitudinally aligned with the first wheel ( 60 ) and an endless track belt ( 68 ) is winded around them . the front wheel ( 60 ) and the second wheel ( 64 ) have a substantially identical diameter so that the path of the track belt ( 68 ) be as uniform as possible during the rotation thereof . the track belt ( 68 ) comprises a tread design on its outer side ( 72 ) to improve the traction . it may also comprise studs ( not shown ). the tension in the track belt ( 68 ) may be adjusted by a screw mechanism ( 74 ) that moves the second wheel ( 64 ) longitudinally . two parallel sets of rollers are provided to support the rear of the frame when the bicycle ( 10 ) is on the ground . each set comprises a plurality of spaced - apart rollers ( 82 , 84 , 86 ) operatively connected to and extending downwardly from a respective horizontal member ( 52 , 54 ) by means of individual brackets ( 78 ) with corresponding pivots ( 80 ). each roller ( 82 , 84 , 86 ) is in engagement with the inner side ( 70 ) of the track belt ( 68 ) and is significantly smaller than the first ( 60 ) and the second wheel ( 64 ). an example of a suitable type of roller ( 82 , 84 , 86 ) is a roller such as used on an in - line skate . preferably , each set of rollers comprises a front roller ( 82 ) juxtaposed to the first wheel ( 60 ), which means that the roller ( 82 ) is laterally offset with the first wheel ( 60 ) and that the bottom of the first wheel ( 60 ) and the bottom of the roller ( 82 ) are substantially side - by - side . this allows the weight to be divided between the front rollers ( 82 ) and the first wheel ( 60 ). then , a rear roller ( 86 ) is juxtaposed to the second wheel ( 64 ) and at least one intermediary roller ( 84 ) is located between the corresponding front ( 82 ) and rear rollers ( 86 ) and substantially longitudinally aligned therewith . two intermediary rollers ( 84 ) are provided on each set in the preferred embodiment shown in fig1 and 2 . a transmission mechanism is used to mechanically connect the pedal drive assembly ( 34 ) to the second wheel ( 64 ). various arrangements are possible . preferably , the transmission mechanism comprises a set of at least two first sprocket gears ( 90 ) rigidly connected to the pedal drive assembly ( 34 ). a hub ( 88 ), operatively connected between the upper end of the oblique members ( 48 , 50 ), is provided to bear a second ( 92 ) and a third sprocket gear ( 94 ). a first sprocket chain ( 98 ) has one end winded around one of the first gears ( 90 ) and another end winded around the second gear ( 92 ). a front derailleur ( 102 ) may be used to selectively align the first chain ( 98 ) with one of the first gears ( 90 ). the user controls the front derailleur ( 102 ) with a lever ( 104 ) and through a corresponding cable ( 105 ). a fourth sprocket gear ( 96 ) is rigidly connected to and coaxial with the second wheel ( 64 ). then , a second sprocket chain ( 100 ) is winded around the third gear ( 94 ) and around the fourth gear ( 96 ) to complete the mechanical connection . preferably , a stretching means may be used for tensioning the first chain ( 98 ). this may be done by using a conventional rear derailleur ( 106 ) without the ability of shifting gears . a similar additional rear derailleur ( 107 ) may be provided for tensioning the second chain ( 100 ). a guarding device may be provided to prevent snow or ice debris from accumulating in front of the second wheel ( 64 ) and the rear rollers ( 86 ). preferably , the guarding device comprises an inverted v - shaped knife ( 108 ) operatively connected in front of the second wheel ( 64 ) between the horizontal members ( 52 , 54 ) by means of a pivot ( 110 ). the knife ( 108 ) pushes away snow or ice debris to help prevent a possible jam between the second wheel ( 64 ) and the track belt ( 68 ), or between the rear rollers ( 86 ) and the track belt ( 68 ). as aforesaid , it is possible to choose among a plurality of removable implements such as a ski assembly , a single ice blade assembly , opposite ice blades assembly and a wheel ( 126 ). the ski assembly is shown in fig1 . it may comprise a ski ( 112 ) and a leaf spring ( 114 ) to absorb the shocks . fig5 shows an example of a single ice blade assembly to be used on an icy surface . the blade ( 116 ) is connected to the conventional fork ( 21 ) that is steerable using the handlebars ( 22 ). the fork ( 21 ) comprises an upper tube ( 130 ) that is inserted upwardly in the head tube ( 20 ) and connected to the handlebars ( 22 ) by a fastener ( 132 ). the blade assembly may comprise a front shock absorber ( 117 ) to damp the irregularities of the ground while riding thereon . the upper end of the shock absorber ( 117 ) is removably connected to the fork ( 21 ) by means of a cotter pin . fig6 shows another possibility for the front steerable supporting assembly . it consists of an opposite ice blades assembly that comprises a transverse static bar ( 120 ) connected to the main frame ( 12 ) and two opposite and parallel ice blades ( 118 ) operatively connected to a respective end of the bar ( 120 ). a steering system ( 122 ) is provided to steer the ice blades ( 118 ). this system ( 122 ) comprises tie rods ( 124 ) connected to the handlebars ( 22 ) by means of the steering tube ( 130 ) inserted and pivoting in the head tube ( 20 ). the bar ( 120 ) is connected to the main frame ( 12 ) by a lower sleeve tube ( 132 ) connected to the lower part of the head tube ( 20 ) by a fastener ( 134 ), such as a cotter pin . the upper end of the steering tube ( 130 ) is connected to the handlebars ( 22 ) by means of a releasable fastener ( 136 ). fig7 shows a front wheel ( 126 ) operatively connected to the fork ( 21 ). this wheel ( 126 ) may always be transported on the bicycle ( 10 ) by connecting it to the main frame ( 12 ) using an appropriate rear attachment ( 128 ), as shown in fig1 . this may be very useful in case the ice or snow surface is discontinued . one may also use the wheel ( 126 ) permanently if desired . although a preferred embodiment of the invention has been described in detail herein and illustrated in the accompanying drawings , it is to be understood that the invention is not limited to this precise embodiment and that various changes and modifications may be effected therein without departing from the scope or spirit of the present invention . | 1 |
the method and the system of the invention are shown schematically in the appended figures . fig1 thus shows an operator 10 who has encountered a problem during implementation of a welding or similar operation , for example a weld bead of poor quality or mediocre appearance . to solve his problem quickly , that is to say in such a way that the productivity of the welding process is not affected , or is affected as little as possible , the operator 10 can obtain an almost immediate solution to this problem in real time by virtue of the method of the invention , and by proceeding as follows . firstly , the operator indicates or selects the type of heat treatment process employed , for example a gas - shielded arc welding process , and indicates or selects , on the one hand , the type of technical problem that he has encountered and , on the other hand , one or more parameters relating to the configuration of the said welding process . if necessary , further technical information may be provided . these indications and / or selections may be made by means of a fixed or portable computer 1 or a telephone 11 provided with suitable acquisition means , such as a keyboard , a mouse or the like . the information from the operator is then transmitted , for example by a wire link 2 and / or a radio link 12 , to a data processing server 3 which makes it possible to process this information and which , after this processing , presents the user with one or more technical solutions to be applied so that his welding process is modified effectively , that is to say presents him with one or more items of corrective information , modifications or adjustments to be made to one or more configuration parameters of said heat treatment process so as to try to solve the technical problem encountered . this corrective information will be retransmitted to the operator via the aforementioned data transmission means . the operator has merely to modify his welding process , taking into account this corrective information , and thus eliminates the technical problem with which he was confronted . depending on the case , it will also be possible to use the method of the invention to give a welding practitioner the means of informing himself about a technique or a welding process with which he is not very familiar , to organize the welding - related knowledge so that it answers technical questions and interrogations or solves technical problems , and / or to illustrate these remarks with quantitative or teaching examples . more generally , the invention also relates to an information processing system intended to make it easier to obtain an answer to a question or a solution to a problem which might arise during a heat treatment operation . using a menu displayed on a computer screen , pocket organizer , portable telephone , watch , etc ., it is possible to activate a link , for example a hypertext link in a web page , to a database by means of the processor in this tool and the programs contained in its memory . this activation of one of the elements of a menu may also be accomplished , for example , by means of a mouse , a pointer on a touchscreen , a voice recognition system , etc . this link makes it possible to activate , through a wire or radio network , an information storage and processing tool . in this tool , the information is contained in files , for example , stored in memory on a hard disk , and operates using an executable installed on an information system , such as a computer , by means of elements such as a hard disk , a micro - processor and the random - access memory and other elements needed for any computer or information processing system to operate correctly . this executable , thanks to the processor , will search for the requested information in a database , for example the access ™ program from microsoft ™, of the hard disk , extract it or possible store it momentarily in the random - access memory , and then to send it back , via the same means as that for the request , to the user . the latter will then be able to display the reply on a screen on a portable or fixed computer , a mobile telephone , a pocket organizer or a watch , again with the aid of executables stored in the memory of the user station and operating by means of a programmed chip or processor . fig2 illustrates , moreover , the case of a problem arising during a gmaw welding operation , for example a problem with the feeding of the wire , although the wire feeder is operating correctly . the user , that is to say the welder , his foreman or the welding engineer , will start up the tool , using the method of the invention , on his portable computer , mobile telephone or pocket organizer . to do this , he will activate an executable programme using a mouse , a touchscreen or the like , which will send the command to the machine to start searching for one or more items of information in a central server via at least one wire or radio link . the executable in the server will then load the “ welding ” home page , which is transmitted to the user via the same means as previously . by clicking on the “ incidents and remedies ” hypertext link , the executable in the server station is again activated . this time , the hypertext link will make a database management executable fetch the desired information from the database ( s ) identified by the program and stored on the hard disk of the server or on another mobile storage means ( cd - rom , zip disk , etc .). the process of exchanging information between the user station and the server is similar to the previous one . through the successive choices ( clicks ) associated with the choice of the process , and with the description of its “ feed problem ” consumable wire incident , a list of corrective actions will be presented to the user , all this information being stored in a database on the hard disk or on a mobile storage medium such as a cd - rom . thus , given the rate of information exchanged by this mode of communication , the user will have had the solution to his problem very quickly and without leaving his workplace , whereas the conventional approach would have been either to find the person who could solve the problem , who is not necessarily available or present on the site , or to look for the solution to his problem in the technical reference works relating to welding , but with the risk of not finding a suitable solution or of finding an incomplete solution therein , and / or with the risk of wasting a great deal of time . in other words , the solution to the problem that has arisen could , in no case , be found as quickly . the system of the invention , consisting of a database , server stations and users provided with processors , in memory executable programs , databases and data processing tools , together with wire or radio links , makes it possible to solve a problem that has arisen during a heat treatment operation very quickly and on site . in the case of this example , resolution of the problem would pass , for example , through the following proposed solutions that the system of the invention would present to the operator almost instantly , namely : check if the proper type of wire feeder is used ; check the surface state of the wire ; clean the nozzle of the torch ; reduce the pressure of the brake on the wire spool ; check that the wire surface is not excessively oxidized ; check that the spool of wire is still properly spooled ; adjust the pressure of the feeder drive rolls ; check that the welding torch cables are not overly twisted ; use a push - pull system . it will be immediately understood that the method and the system according to the invention result in an appreciable gain in efficiency , when a welding process or the like is carried out by an operator , compared with the prior art . the invention also includes the remote control of the heat treatment process or device by the computer , once the operator has received and accepted the database proposal . in one such embodiment , a welding assistance method begins with the user supplying an information request to a remote computer database , the information request comprising ( a ) a first indication and / or selection by the user of a type of contemplated heat treatment process , ( b ) a second indication and / or selection by the user of at least one type of technical problem to be solved arising or likely to arise during implementation of the contemplated heat treatment process , and ( c ) a third indication and / or selection by the user of at least one parameter relating to a configuration of the contemplated heat treatment process . the database processes at least some of the first , second , and third indications or selections made by the user , and after processing , the database supplies information relating to the contemplated heat treatment process as a proposal to the user of at least some information relating to at least one modification or at least one adjustment to be made to at least one configuration parameter of the contemplated heat treatment process so as to solve , at least partly , the type of technical problem supplied by the user in the second indication . the user receives the information in the proposal , and , if acceptable to the user , the user accepts the information in the proposal . the user may of course not accept the information and may modify the solution by adding user information based on experience or other information . upon communicating the user &# 39 ; s acceptance of the information in the proposal to a computer ( as an authorization for the computer to act consistent with the accepted information in the proposal ), the computer sets , modifies or adjusts at least one parameter of the welding operation of the contemplated heat treatment process based on the information proposal accepted by the user ( and as modified ) thereby solving , at least partially , the type of technical problem supplied by the user . the embodiment includes the computer setting , modifying or adjusting of at least one parameter of the welding operation is operated by acting on the heat treatment device or facility . the invention contemplates that heat treatment process is from the group consisting of cutting processes , welding processes , marking processes , heat spraying processes and combinations thereof , and that an indication or a selection of the contemplated heat treatment process is made by the user via an interactive computer interface . in another embodiment , the user prior to beginning any heat treatment process , makes a query to the database . the query may be in the form of a first indication and / or selection by the user of a type of heat treatment process to be implemented , and a second indication and / or selection by the user of at least one parameter relating to the configuration of the heat treatment process , that has to be or is likely to be adjusted , modified or set , before or during implementation of the heat treatment process of the first indication . the database processes at least some of the first and second indications or selections made by the user , and provides a proposal to the user of at least some information relating to at least one modification or at least one setting to be made of at least the configuration parameter of the heat treatment process . the user accepts the information provided by the computer as a proposal , and thereafter , the computer sets , modifies or adjusts at least one parameter of the welding operation of the contemplated heat treatment process based on the information proposal accepted by the user . as in other embodiments , this embodiment includes the computer setting , modifying or adjusting of at least one parameter of the welding operation is operated by acting on the heat treatment device or facility . also , the type of contemplated heat treatment process is from the group consisting of cutting processes , welding processes , marking processes , heat spraying processes and combinations thereof , where an indication or a selection of the contemplated heat treatment process is made by the user via an interactive computer interface . a further embodiment includes a welding assistance method for a user to exploit information available at a remote computer welding database in a contemplated welding operation . the method begins with the user supplying an information request to a computer hosing a the database , the information request comprising ( a ) a first indication and / or selection by the user of a type of contemplated heat treatment process , ( b ) a second indication and / or selection by the user of at least one type of technical problem to be solved arising or likely to arise during implementation of the contemplated heat treatment process , and ( c ) a third indication and / or selection by the user of at least one parameter relating to a configuration of the contemplated heat treatment process . as in similar embodiments , the database processes at least some of the first , second , and third indications or selections made by the user , and processing ; the database supplies information relating to the contemplated heat treatment process as a proposal to the user of at least some information relating to at least one modification or at least one adjustment to be made to at least one configuration parameter of the contemplated heat treatment process so as to solve , at least partly , the type of technical problem supplied by the user in the second indication . the user receives and accepts the information in the proposal , authorizing a computer setting , modifying or adjusting at least one parameter of the welding operation of the contemplated heat treatment process based on the information proposal accepted by the user , the information proposal being completed by and / or combined with user experience and / or user information , thereby solving , at least partially , the type of technical problem supplied by the user . generally , the invention includes allowing an improved remote control of a thermal welding or cutting process , device or facility by combining problem diagnostic with user &# 39 ; s query the following steps . first , providing a remote computer database with welding and / or cutting information for allow for diagnosing or identifying a technical problem arising or likely to arise during the implementation of the welding or cutting process , or the use of the welding or cutting device or facility . the user supplying at least one information request to the database about the technical problem to be solved allows the database processing the information and proposing to the user a modification , setting or adjustment proposal to be made to at least one configuration parameter of the welding or cutting process , device or facility . the user , receiving the information in the proposal , accepts the information in the proposal and this acceptance triggers a computer setting , modifying or adjusting at least one parameter of the welding or cutting process , device or facility based on the information proposal accepted by the user thereby solving , at least partially , the technical problem diagnosed or identified . advantageously , the inventive method allows the user , in accepting the information in the proposal , to add further information based on user experience and / or user information . also , the diagnostic or identification may be made by the user or by the computer , taking advantage of the strengths of each . | 1 |
preferred embodiments of this invention are illustrated by the following non - limiting examples . the feedstock used for this test was an athabasca bitumen having the properties given in table 1 below : table 1______________________________________test value______________________________________api gravity , ° api 8 . 1relative density , kg · m . sup .- 3 ( 15 ° c .) 1013viscosity100 ° c ., cst 195 . 44130 ° c ., cst 58 . 25150 ° c ., cst 31 . 24distillation resid , 525 ° c +. wt % 52 . 4pentane insolubles , wt % 16 . 50toluene insolubles , wt % 0 . 82microcarbon residue , wt % 14 . 30carbon , wt % 83 . 30hydrogen , wt % 10 . 90sulphur , wt % 4 . 62ash , wt % 0 . 83nitrogen , wt % 0 . 56 ( 0 . 59 ) metals , ppmsi 1661al 1081fe 700ti 209v 197ca 130k 119ni 74na 68mg 67______________________________________ a feedstock was prepared in a hopper by mixing athabasca bitumen with a predetermined amount of molybdenum naphthenate . the feedstock was then mixed with pure hydrogen of a specified pressure at stp flow rate of about 840 l / l or 5 , 000 scf / bbl and pumped continuously up through a high pressure continuous flow tubular reactor system at an apparent liquid space velocity of 1 h - 1 . one experimental run was completed in eight hours including start - up and shutdown . at start - up , the system was first pressurized with hydrogen and under hydrogen flow heated to 300 ° c . then , while maintaining conditions , the feedstock was pumped in for one hour . subsequently , the temperature was elevated to a predetermined level in about 0 . 5 hour by supplying constant power to reactor heaters . the temperature level was then maintained for 4 . 5 hours during which changes in reactor temperature profiles were monitored and two liquid product samples were collected at 1 . 5 hours and 3 hours . at shutdown , the heaters were turned off and , when cooled to 390 ° c ., the reactor was isolated from the flow system and its fluid content was drained by using the pressure of the residual gas . thereafter , the entire solid residue of the reservoir was carefully collected . the reactor was operated at reactor temperatures between 420 ° and 480 ° c ., molybdenum naphthenate was added in amounts between 1 and 100 ppm and hydrogen pressures were monitored between about 7 and 24 mpa . the results obtained are shown in fig2 and 3 . the ability of an additive to suppress coke can be determined by finding the threshold point of coking . for a given feedstock oil , these points depend on operating conditions , i . e . temperature and pressure if flow rates are kept constant . when the experimental conditions are near the threshold of coking , coke just begins to form . therefore , the operation becomes more difficult and usually a very small amount of reactor coke deposit is found after shutdown . however , should a higher temperature or lower hydrogen pressure be used , substantially more coke would be found , often causing premature shutdown . an additive which is capable of suppressing coke will shift the threshold of coking to either higher temperatures or lower pressures . this is clearly shown in fig2 . the ability of an additive to suppress coke can thus be quantitatively described by using operating conditions as variables to reach the threshold of coking . for example , the relationship between temperature and additive concentration at constant pressure , or the relationship between hydrogen pressure and additive concentration at constant temperature can be used . the latter is shown in fig3 . an important difference between fig2 and 3 is that the only points marked by &# 34 ; t &# 34 ; emerge as threshold coking situations from fig2 whereas all points in fig3 pertain to the threshold of coking . fig3 illustrates the ability of molybdenum naphthenate to substitute hydrogen pressure in suppressing coke formation . thus , it will be seen that while about 24 mpa hydrogen is needed to suppress coke in the feedstock alone , only about 14 mpa was required in the presence of 3 ppm molybdenum and only about 12 mpa was necessary in the presence of 5 ppm molybdenum , when added as molybdenum naphthenate . the ability of this additive to suppress coke quickly diminishes with pressure and disappears at about 4 mpa . without exception , all yields obtained for the test carried out with less than 10 ppm molybdenum were indistinguishable when the feedstock oil alone was used . usually , the extent of hydrogenation , cracking and , especially , sulphur removal are enhanced as a consequence of the catalytic effect of molybdenum . it is evident that there was no other catalytic activity to associate with the presence of molybdenum except coke suppression . for a typical hydrocracking arrangement using either fixed or an ebullated catalyst bed , the catalyst requirement can be expressed in terms of the amount needed to process a given volume of feedstock in a given time . for molybdenum contained in commercial catalyst extrudates , pellets , etc . this requirement is typically within the order of magnitude of 10 - 1 to 10 - 2 kg . l - 1 . h - 1 . in this situation , 10 ppm of molybdenum mixed in the oil feedstock represents about 10 - 5 kg . l - 1 . h - 1 if the liquid space velocity were 1 h - 1 , which is 1 , 000 to 10 , 000 times less than typically required . it is believed that the coke precursor entities effected by molybdenum present in such low concentrations are very large relative to other typical molecules and that their participation in other than coke - forming reactions is minimal . the catalytic effect of molybdenum is therefore simply demonstrated by stabilizing these entities through hydrogen transfer so that they become less prone to further growth . it appears that such a mechanism may involve predominantly the very external surface of catalytic particles which is effectively supplied through the high dispersion . since the total surface area remains very small because of the low metal concentration , the catalytic effects , in the conventional sense , are insignificant . however , the coke suppression activity is still very significant and it is thus obvious that the conventional indicators , such as yields , would not reveal the particular activity found in the process of this invention . the reduced propensity for coke formation achieved by adding trace amounts of molybdenum naphthenate according to this invention allows an increase of reactor temperature , which in turn provides higher conversion than are possible without additives . alternatively , conversions which may be achieved only at high pressures of higher than about 21 mpa without additives may be achieved according to the present invention at medium or moderate pressures as low as 10 mpa . | 2 |
the present invention is a turbo - charcoal barbecue , designated as 10 in the drawings . fig1 shows a turbo - charcoal barbecue comprising an enclosure 11 most preferably constructed of heat resistant materials . the enclosure 11 is supported by two wheels 20 and two legs 22 for portability . as shown in fig2 the enclosure comprises a larger upper chamber 24 containing a flame blocking and heat flow regulating fire screen 28 , a grill 30 , and an adjustable and removable charcoal tray 32 that can be raised or lowered by a crank shaft system . a housing 34 abuts the back of the upper chamber 24 and contains a turbo unit 40 within its structure . the enclosure also comprises a smaller lower chamber 26 for collecting expended ash material . beneath the lower chamber 26 is two removable ash trays 36 . a lid or cover 38 makes up the top portion of the enclosed structure and contains a rotisserie ensemble . the larger upper chamber 24 contains a grill 30 that supports food and the grill 30 extends to all walls of the enclosure . fig4 shows how the grill 30 divides the upper chamber 24 into an operating space 42 and a hot air flow space 44 . the upper chamber 24 in fig3 contains a fire screen 28 that is rectangular in shape and sits on ledges attached to the back wall and both side walls . the grill 30 is located above the fire screen 28 and is attached to the walls of the enclosure in the same fashion . the fire screen 28 stops an inch or two short of attaching to the front wall of the enclosure to leave a space allowing hot air to flow downwards . the fire screen 28 in fig2 is perforated with small holes 46 designed to allow hot air through the fire screen 28 and block undesired flash flames caused by ignited briquets 48 . the small holes 46 are sized to allow even heating across the entire grill 30 . there is no need for a grease collector because fat drippings that come in contact with the hot fire screen 28 dissipate . the fire screen 28 can be removed for remote cleaning purposes . previously patented flame blocking structures redirect a vast amount of the heat flow around the edges of the heat plate and to the outer edges of the grill . the fire screen not only blocks flames directed to the grill , but allows the heat to flow through the plate and be evenly applied to the entire grill surface . the upper chamber 24 in fig3 contains a charcoal tray 32 that can be raised and lowered by a crank shaft system and can be removed through an opening 50 in the side wall of the enclosure via a trap door 52 to replenish briquets 48 . the crank shaft system comprises a charcoal plate 54 fitted to the shape of the upper chamber 24 , an elongated threaded crank shaft 56 , a mount 58 attached to the floor of the upper chamber 24 and a handle 62 attached to the lower end of the crank shaft 56 . the charcoal plate 54 is attached to a crank shaft 56 in a way that keeps the charcoal plate 54 from rotating but allows the charcoal plate 54 to be raised and lowered when the crank shaft 56 is turned . the top portion of the crank shaft system is located in the upper chamber 24 and extends down into the lower chamber 26 out through the bottom of the enclosure . the crank shaft 56 passes through a mount attached to the floor 60 of the upper chamber 24 which is also threaded and operates to move the shaft 56 up or down when turned . the elongated crank shaft 56 is threaded and can be turned by the crank by means of an attached handle 62 . the crank shaft system operates by movement of the crank handle 62 which causes the shaft 56 to move in the up and down position when the handle 62 of the crank 56 is turned in a clockwise or counter - clockwise direction . the charcoal tray 32 filled with ignited briquets 48 rests on the charcoal plate 54 which can be raised and lowered to control the intensity of heat source applied to the fire screen 28 . normally reducing the temperature of the heat source can diminish the effect of radiation heat transfer and leave the user with only relatively inefficient convection heating to grill the food . however , the recirculation of hot air within the enclosure improves heat transfer efficiency , even though the crank shaft has reduced the temperature of the heat source . the crank shaft system can raise the charcoal tray 32 / plate 54 complex to the opening 50 located within the side of the enclosure wall . a trap door 52 in fig2 is hinged to the outside of the side enclosure wall can be opened by a latch 64 which exposes an opening 50 shaped to allow the charcoal tray 32 to be removed from the charcoal plate 54 and be slid through such opening 50 . the charcoal tray 32 has a portion of one of its side wall 66 exposed to the opening 50 extending downwards from the charcoal tray 32 perpendicular to the tray &# 39 ; s bottom . a housing 34 abuts the back wall of the upper chamber 24 and contains a turbo unit 40 positioned in the lower section thereof . the housing 34 comprises a bottom surface 68 , a back wall 70 , a top wall 72 and side walls . a turbo unit 40 makes up the lower to mid section of the housing area . the turbo unit 40 comprises a motor 74 attached to the back wall 70 through an opening that rotates a fan 76 adjacent to the motor 74 . the fan 76 is cylindrically shaped and has a plurality of blades 78 emanating from the center of the fan 76 . the back wall 70 of the enclosure in the upper chamber 24 contains a hot air intake opening 88 shaped to the size of the fan 76 , and air outlet opening 80 . the turbo unit motor 74 can be operated at various speeds and the source of the power is either a battery 82 or from an electrical outlet using a transformer 82 . the battery or transformer 82 is affixed to the lower shelf 84 located at the bottom of the barbecue . wire mesh 86 is attached to the opening 88 on the inside of the back wall 70 adjacent to the fan 76 and functions to prevent big particles of charcoal from falling into the turbo unit 40 . the wire mesh 86 can be removed by sliding it up from holding brackets for remote cleaning . the wire mesh solves the problem of hot ash particles being distributed throughout the enclosure of the barbecue and from falling onto the food being grilled . a standard control switch 91 designed to adjust at variable speeds would be located beneath the side table 92 and is located at the front area of the barbecue 10 at a convenient level for the user . the control switch 91 has heat resistant wires and is connected to the turbo unit motor 74 , not shown . an adjustable hot air vent 90 system surrounds the outer edges of the rotating cylindrically shaped fan 76 and extends upwards and comprises the upper section of the housing . the back wall 70 of the enclosure in the upper chamber 24 contains a hot air output opening 80 shaped to the size of the adjustable hot air vents 90 . the vent openings in the vent system 90 are designed to be positioned to expel hot air parallel to the grill 30 surface and the vent 90 can be adjusted to an upward position to expel hot air into the cover or lid 38 cavity . normally heat is applied to meat cooked on a rotisserie shaft 96 from only the direction of the heat source . the vent system 90 in the present invention is designed to apply hot air from two directions onto the rotisserie shaft 96 . by the vent 90 adjusted in the upward direction , hot air can be applied to an additional position on the rotisserie shaft 96 to allow for faster roasting . fig3 and 4 shows a lid or cover 38 makes up the top portion of the enclosed barbecue structure and is held by hinges 98 . a handle 100 would be attached to the outer surface of the front wall of the barbecue 38 lid for opening and closing the lid 38 . a rotisserie ensemble is assembled above the grill 30 and attached to the side walls of the barbecue cover 38 by gripping prongs mounted thereon . the rotisserie shaft 96 is rotated by a motor 102 which may be of conventional construction and the source of power is either by a battery 82 or from an electrical outlet using a transformer 82 . the rotisserie shaft 96 is adjustable in height through guides 104 mounted within both side walls of the lid 38 . in fig2 the guide 104 operates as a male 106 and female 108 connection that locks together by fine teeth located on each connection . the guide 104 is rectangular in shape and positioned vertically within the side walls with horizontally spaced teeth grooves on one side of both the male 106 and female 108 connections . there is a rectangular shape opening 110 within the guide 104 . this opening 110 functions as the female 108 connection of the guide lock system . attached to the ends of the rotisserie shaft 96 is a rectangular male 106 connection with matching teeth grooves spaced apart to fit together with the female 108 connection . when the grooves of the male 106 and female 108 connection are fitted together , screws 112 within the complex can be tightened and the male 106 \ female 108 attachment will lock into place . to adjust the height of the rotisserie shaft 96 the users would loosen the screws 112 , adjust shaft 96 to desired height , then tighten screws 112 . in order for this appliance to be efficient the turbo - charcoal barbecue cover 38 must be closed at all times , except when turning or retrieving food within the enclosure . the cycle of hot air is the key to this process . this is an efficient barbecue 10 because the hot air underneath the charcoal tray 32 is utilized in the recirculation of hot air . normally the hot air just stays underneath and is never used . fig3 and 4 the path and cycle of the hot air when the vent 90 is in both the upward and downward positions . the adjustable hot air flow vent 90 in the turbo unit 40 allows for two different methods of hot air flow for cooking food products within the turbo - charcoal barbecue 10 . in fig3 the first method of hot air flow , wherein the air flow vent 90 is angled upward , is shown in phantom lines . alternatively , as illustrated in solid lines , the hot air flow vent 90 may be directed horizontally . considering the upward - directed air flow vent 90 , after the briquets 48 have been ignited , the control switch 91 for the turbo unit motor 74 would be turned to the desired speed . the turbo unit motor 74 rotates the cylindrically shaped fan 76 which draws heated air through the hot air intake opening 88 and from beneath the charcoal tray 32 where the ignited briquets 48 rest . this hot air is propelled into the adjustable hot air flow vent 90 which expels hot air through the hot air output opening 80 and towards the center of the lid 38 enclosure where the rotisserie shaft 96 would be located . at the same time , the hot air flow emanating from above the ignited briquets 48 would be directed towards the fire screen 28 and be equally distributed through small holes 46 within the fire screen 28 . as the hot air flow leaves the fire screen 28 it either goes towards the grill 30 or circulated back down beneath the charcoal tray 32 to be recirculated . the hot air flow that passes through the grill 30 is circulated around the rotisserie shaft 96 and flows together with the hot air flowing expelled from the hot air flow vent 90 . with this method of hot air flow , hot air is directed towards two different areas of food being rotated on the rotisserie shaft 96 by its own motor 102 . fig3 and 4 show the second method of hot air flow is shown only in solid lines and requires the hot air flow vent 90 to be adjusted in a position parallel to the grill surface 30 . after the briquets 48 have been ignited , the control switch 91 for the turbo unit motor 74 would be turned to the desired speed . the turbo unit motor 74 rotates the cylindrically shaped fan 76 which draws in heated air through the hot air intake opening 88 and from beneath the charcoal tray 32 where the ignited briquets 48 rest . this hot air is propelled into the adjustable hot air flow vent 48 which expels hot air through the hot air output opening 80 towards the surface of the grill 30 and into the area between the fire screen 28 and the grill 30 . at the same time , the hot air flow emanating from above the ignited briquets 48 would be directed towards the fire screen 28 and be equally distributed through small holes 46 within the fire screen 28 . as the hot air flow leaves the fire screen 28 it either goes towards the grill 30 or circulated back down beneath the charcoal tray 32 to be recirculated . the hot air flow above the grill 30 surface is circulated into the lid &# 39 ; s 38 enclosure and recirculates back onto the grill surface 30 . the hot air flowing between the grill 30 and the fire screen 28 joins with the hot air flowing from above the grill 30 and is directed downwardly beneath the charcoal tray 32 and in drawn back into the turbo unit fan 76 for recirculation . the achievement of uniformly cooked meat and the efficient use of fuel and energy would be obtained by the present invention . a heat resistant glass window 114 in fig4 is located within the front wall of the barbecue &# 39 ; s lid 38 . this functions to allow the user to monitor the food product being cooked without having to open the lid 38 . by keeping the lid 38 in the closed position as long as possible , aids in the efficient use of the barbecue 10 in recirculating its hot air and not allow hot air to be exhausted . fig2 shows a rectangular heat control slot 116 located within the top portion of the turbo - charcoal barbecue &# 39 ; s lid 38 has a cover slip 118 that slides over it . the purpose of the slot 116 is to release some of the hot air inside the if heat is to high in the barbecue &# 39 ; s 10 enclosure . also located on the lid 38 is a thermostat 120 that indicates the intensity of the heat inside the barbecue &# 39 ; s 10 enclosure . the thermostat , timer , heat control slot work together to aid in regulating the intensity of heat needed to properly grill foods . there are several shelves 92 shown in fig2 that extend out of the barbecue 10 and function as a table to hold items used in grilling and roasting . each side of the barbecue 10 has a shelf 92 extending outward . one shelf 92 would be positioned on the same side and directly below the trap door 52 which functions to support the door 52 in the open position and to hold the charcoal tray 32 when removed from the opening 50 . there would also be a small shelf 92 extending outwardly from the front of the barbecue 10 at a convenient working height for the user . a timer 122 would be located beneath one of the side shelves 92 and can be set to give warning sounds to indicate the length of time meat has been cooking in the barbecue . referring to fig3 the barbecue 10 also comprises a smaller lower chamber 26 for collecting expended ash material . the lower chamber 26 of the barbecue is approximately five times smaller than the upper chamber 24 . there is a metal floor 60 within the enclosure that separates the upper 24 and lower 26 chambers . shown in fig2 the metal floor 60 has right and left rectangular shaped openings 124 with downwardly sloped chutes 126 leading into the lower chamber 26 . attached beneath the lower chamber 26 is two removable ash trays 36 . ashes can be swept down the chutes 126 and the ash trays 36 may be slidingly removed for emptying out the expended ash material . obviously , this would necessitate affixing some type of hinge means . the turbo - charcoal barbecue 10 has two wheels 20 located on the left side for easy transport and a shelf 84 is located near the wheel to hold many items including a rechargeable battery or transformer 82 to power the turbo unit 40 and rotisserie motor 102 . it is to be understood that the present invention is not limited to the embodiment described above , but encompasses any and all embodiments within the scope of the following claims . | 0 |
those of ordinary skill in the art will realize that the following description of the present invention is illustrative only and is not intended to be in any way limiting . other embodiments of the invention will readily suggest themselves to such skilled persons from an examination of the within disclosure . a high speed , low skew , logic level converter of the present invention is shown in simplified form in fig1 . the converter is designed to translate a differential complementary pair of input signals at input node inp and inpi ( input and inverted input ) from a potential associated with cmos logic levels into a differential complementary pair of output signals at output node out and outi that are at potentials associated with ecl logic levels . it is contemplated that the potentials associated with out and outi may be developed by the converter at levels other than those related to ecl including , but not limited to gunning transceiver logic ( gtl ). the converter of the present invention includes two switching components , a first potential switch and a second current switch . the first potential switch formed by the pfets p 1 , p 2 , p 3 , and p 4 . the pfets are arranged into two branches , a first branch consisting of pfet p 1 in series with pfet p 3 , where the source of pfet p 1 is connected with vcc , and the drain of pfet p 3 is connected with a base potential . the gate of pfet p 1 is connected with the input inpi and the gate of pfet p 3 is connected with the input inp . symmetrically , a second branch consisting of pfet p 2 in series with pfet p 4 , where the source of pfet p 2 is connected with vcc , and the drain of fet p 3 is connected with the base potential . the gate of pfet p 2 is connected with the input inp and the gate of pfet p 4 is connected with the input inpi . the base potential of the two branches is defined by the constant current through resistor r 1 . resistor r 1 is connected with vcc and the collector of transistor q 3 , the emitter of transistor q 3 is connected via the resistor r 4 with gnd , hence forming a constant current source . a reference voltage on the basis of transistor q 3 allows to adjust the base potential . the ecl current switch consists of two transistors q 1 and q 2 , where the coupled emitters are connected with a current source . each of the collectors is connected via a resistor with vcc , q 1 with r 2 and q 2 with r 3 . the collector of transistor q 1 is the output out , and symmetrically , the collector of q 2 is the output outi . the current source connected with the two emitters of the transistors q 1 and q 2 is similar to the current source for the resistor r 1 . it consists of a transistor q 4 , where the emitter is connected via a resistor r 5 with gnd . the collector of transistor q 4 is connected with the two emitters of transistor q 1 and q 2 . a reference voltage on the basis of transistor q 4 allows to adjust the current . the outputs potentials of the first switching component , the potential switch are connected with the input of the ecl current switch . the drain of pfet p 1 is connected with the basis of transistor q 2 , and the drain of pfet p 2 is connected with the basis of transistor q 1 . assume node inp has low - potential and consequently inpi has high potential . then both pfets p 2 and p 3 are conducting and the other pfets p 1 and p 4 are closed . the base of transistor q 1 is now connected with vcc and the base of transistor q 2 has now the base potential of the potential switch . this has the effect that q 1 is open and q 2 is closed . the out potential is low , defined by the voltage on resistor r 2 . since transistor q 2 is closed , outi is connected via r 3 with vcc and is high . when inp changes to high potential and consequently inpi has low potential , the pfets p 2 and p 3 are closed , and pfets p 1 and p 4 are conducting . pfet p 1 connects the base of transistor q 2 with vcc and pfet p 4 connects the base of transistor q 1 with the potential defined by r 1 . the change process is very fast since the pfets only have to switch the base currents of transistor q 1 and q 2 . due to the change of the potentials on the bases of the transistors q 1 and q 2 , the ecl current switch changes the output potentials . the output load ( succeeding ecl circuit ) is shifted by the two bipolar transistors . this has the effect that the signal is changing very fast . this is illustrated by the diagram of fig2 . [ 0051 ] fig2 . provides an illustration of the advantage in using the converter of fig2 . specifically , of the waveforms shown , the line labeled with is the cmos - level signal supplied at input inp and the line labeled with is the cmos - level signal supplied at input inpi for a 3 . 3 - volt supplied system . the line labeled with shows the potential associated with output out and it can be seen that a change of a differential cmos - input potentials force a change of the differential ecl - output signal within 100 psec . a logic low at the input results in a logic low at the output and a logic high at the input results in a logic high at the output . thus , for the noted example of the present invention , a full - swinging cmos input can be translated into a differential pair of output signals having a differential of about 0 . 2 v . in summary , the converter accomplishes cmos - to differential - ecl translation of node inp and node inpi by changing the potential of node out and node outi . although illustrative presently preferred embodiments and applications of this invention are shown and described herein , many variations and modifications are possible which remain within the concept , scope , and spirit of the invention , and these variations would become clear to those of skill in the art after perusal of this application . for example , the current source for the ecl current switch as well as the base potential could be implemented using multiple reference voltages or multiple transistors . obviously the dual circuit ( n - type semiconductor ( n - channel ) fets with pnp transistors ) works similarly , etc . the invention , therefore , is not intended to be limited except in the spirit of the appended claims . | 7 |
in a first aspect , the invention is directed to compounds of general formula ( i ) for imaging bone metastases wherein r 1 is — ch 2 — f 18 , — ch 2 — ch 2 — f 18 or — ch 2 — ch 2 — ch 2 — f 18 and pharmaceutically acceptable salts thereof . invention encompasses also the single isomers , enantiomers , stereoisomers , stereoisomeric mixtures or mixtures of compounds of general formula ( i ). preferably , the invention is directed to compounds of general formula ( i ) for imaging bone metastases wherein r 1 is — ch 2 — f 18 or — ch 2 — ch 2 — f 18 and pharmaceutically acceptable salts thereof . in other word , the invention is directed to the use of compounds of general formula ( i ) for the manufacture of an imaging tracer for imaging bone metastases wherein r 1 is — ch 2 — f 18 , — ch 2 — ch 2 — f 18 , or — ch 2 — ch 2 — ch 2 — f 18 and pharmaceutically acceptable salts thereof . the invention is directed to compound of general formula ( i ) for use in the imaging bone metastases . preferably , the compound of formula ( i ) is a d - tyrosine derivative of formula ( d - i ) wherein r 1 is — ch 2 — f 18 , — ch 2 — ch 2 — f 18 , or — ch 2 — ch 2 — ch 2 — f 18 . more preferably , the compound of formula ( i ) is a d - tyrosine derivative of formula ( d - i ) wherein r 1 is — ch 2 — f 18 , or — ch 2 — ch 2 — f 18 . the invention is directed to compound of general formula ( d - i ) or r )- 2 - amino - 3 -( 4 -[ f - 18 ] fluoromethoxy - phenyl )- propionic acid for use in the imaging bone metastases . the imaging tracer is suitable for positron emission tomography ( pet ) or micropet . the imaging comprises the step of pet imaging and is optionally preceded or followed by a computed tomography ( ct ) imaging or magnetic resonance tomography ( mrt ) imaging . the imaging occurs in mammals . the invention is also directed to a method for imaging or diagnosis bone metastases comprising the steps : administering to a mammal an effective amount of compounds of general formula ( i ) or ( d - i ) or mixture there of , obtaining images of the mammal and assessing the images . and pharmaceutically acceptable salts thereof for the manufacture of an imaging tracer for imaging bone metastases . in a second aspect , the invention is directed to the use of compound of formula ( i ) for differentiating bone metastatic disease from bone non - metastatic disease in mammal . preferred embodiments disclosed above in respect of compound of formula ( i ) are included herein . the invention is also directed to a method for differentiating bone metastatic disease from bone non - metastatic disease in mammal by assessing image ( s ) obtained after administering to the mammal of an effective amount of compounds of general formula ( i ) or ( d - i ) or mixture there of . bone non - metastatic diseases are benign bone pathologies comprised from the group of back pains , focal changes in bones , trauma , reconstructive surgery , bone grafts , metabolic bone disease or osteoporosis . in a third aspect , the invention is directed to a composition comprising compounds of the general formula ( i ), ( d - i ), or mixture thereof and pharmaceutically acceptable carrier or diluent wherein the compounds of the general formula ( i ), ( d - i ) are imaging tracer for imaging bone metastases . the person skilled in the art is familiar with auxiliaries , vehicles , excipients , diluents , solvents , carriers or adjuvants which are suitable for the desired pharmaceutical formulations , preparations or compositions on account of his / her expert knowledge . the administration of the compounds , pharmaceutical compositions or combinations according to the invention is performed in any of the generally accepted modes of administration available in the art . intravenous deliveries are preferred . generally , the compositions according to the invention is administered such that the dose of the active compound for imaging is in the range of 37 mbq ( 1 mci ) to 740 mbq ( 20 mci ). in particular , a dose in the range from 150 mbq to 370 mbq will be used . in a fourth aspect , the present invention provides a kit comprising a sealed vial containing a predetermined quantity of a compound having general chemical formula ( i ) or ( d - i ) and suitable salts of inorganic or organic acids thereof , hydrates , complexes , esters , amides , and solvates thereof for imaging bone metastases . optionally the kit comprises a pharmaceutically acceptable carrier , diluent , excipient or adjuvant . the terms used in the present invention are defined below but are not limiting the invention scope . suitable salts of the compounds according to the invention include salts of mineral acids , carboxylic acids and sulphonic acids , for example salts of hydrochloric acid , hydrobromic acid , sulphuric acid , phosphoric acid , methanesulphonic acid , ethanesulphonic acid , toluenesulphonic acid , benzenesulphonic acid , naphthalene disulphonic acid , acetic acid , trifluoroacetic acid , propionic acid , lactic acid , tartaric acid , malic acid , citric acid , fumaric acid , maleic acid and benzoic acid . suitable salts of the compounds according to the invention also include salts of customary bases , such as , by way of example and by way of preference , alkali metal salts ( for example sodium salts and potassium salts ), alkaline earth metal salts ( for example calcium salts and magnesium salts ) and ammonium salts , derived from ammonia or organic amines having 1 to 16 carbon atoms , such as , by way of example and by way of preference , ethylamine , diethylamine , triethylamine , ethyldiisopropylamine , monoethanolamine , diethanolamine , triethanolamine , dicyclohexylamine , dimethylaminoethanol , procaine , dibenzylamine , n - methylmorpholine , arginine , lysine , ethylenediamine and n - methylpiperidine . unless otherwise specified , when referring to the compounds of formula the present invention per se as well as to any pharmaceutical composition thereof the present invention includes all of the hydrates , salts , and complexes . as used herein , the term “ carrier ” refers to microcrystalline cellulose , lactose , mannitol . as used herein , the term “ solvents ” refers to liquid polyethylene glycols , ethanol , corn oil , cottonseed oil , glycerol , isopropanol , mineral oil , oleic acid , peanut oil , purified water , water for injection , sterile water for injection and sterile water for irrigation . in this study , it was investigated the potential of d - fmt to image bone metastases in two mouse models . injection of 786 - o / luc cells and mda - mb231sa / luc cells into the arterial circulation resulted in the development of aggressive osteolytic lesions in bones within 62 ± 8 days for the 786 - o / luc cells and 20 ± 5 days for the mda - mb231sa / luc cells . due to the variety of cytokines and growth factors stored in bone , the skeleton provides a fertile environment for the growth of cancer cells ( 13 ). the tumor cells were primarily located within the bone and resulted in cortical destruction of bone . no soft tissue metastases ( kidneys , adrenal glands , heart , lungs ) were detected by bioluminescence imaging or by histomorphometry ( 14 ). a bone scan with [ f - 18 ]- fluoride was performed to validate the localization of the bone metastases . the 786 - o / luciferase ( luc ) cell line was generated by stable transfection with a prev cmv_luc2 vector . the cells were cultured in rpmi medium ( biochrom ag , berlin , germany ) containing 10 % heat - inactivated fcs ( biochrom ag ), 2 % glutamine ( ppa laboratories , pasching , austria ), 4 . 5 g / l glucose ( sigma - aldrich chemie gmbh , taufkirchen , germany ), 10 mm hepes ( biochrom ag ), 1 mm pyruvate ( biochrom ag ) and 50 μg / ml hygromycin b ( invitrogen ltd ; carlsbad , calif ., usa ). the mda - mb231 / luciferase ( luc ) cell line was generated by stable transfection with a prev cmv_luc2 vector . cells were cultivated in high - glucose dmem ( biochrom ag ) containing 10 % heat - inactivated fcs ( biochrom ag ), 2 % glutamine ( paa laboratories gmbh ), 1 % nonessential amino acids ( paa laboratories ) and 250 μg / ml hygromycin b ( invitrogen ltd .). 786 - o / luc cells and the mda - mb231sa / luc cells were harvested from subconfluent cell culture flasks and resuspended in pbs ( biochrom ag ) to a final concentration of 5 × 10 5 cells / 100 μl . for intracardiac inoculations , 5 - week - old female athymic nude mice ( harlan - winkelmann gmbh , borchen , germany ) were anesthetized with an intraperitoneal injection of 5 % rompun ( bayer healthcare ag , leverkusen , germany )/ 10 % ketavet ( pfizer , karlsruhe , germany ) in 0 . 9 % nacl at a dose of 0 . 1 ml / 10 g body weight . using an insulin syringe ( bd micro - fine + demi u - 100 , becton dickinson gmbh , heidelberg , germany ), 5 × 10 5 786 - o / luc cells in 100 μl pbs were inoculated into the left cardiac ventricle ( i . c .) of anesthetized mice . experiments were approved by the governmental review committee on animal care . tumor cell dissemination in bone was regularly monitored by bioluminescence imaging using a cooled ccd camera ( nightowl lb , berthold technologies , bad wildbad , germany ). the mice were injected intravenously with 100 μl luciferin ( 45 mg / ml in pbs , synchem ohg , felsberg / altenburg , germany ) and anesthetized with 1 - 3 % isoflurane ( curamed pharma gmbh , karlsruhe , germany ). the synthesis of d -[ f - 18 ]- fluoromethyl tyrosine ( d - fmt ) was performed by reacting [ f - 18 ]- fluoromethyl bromide with d - tyrosine as previously described by tsukada h , sato k , fukumoto d , nishiyama s , harada n , kakiuchi t . evaluation of d - isomers of o - 11c - methyl tyrosine and o - 18f - fluoromethyl tyrosine as tumor - imaging agents in tumor - bearing mice : comparison with l - and d - 11c - methionine . j nucl med . april 2006 ; 47 ( 4 ): 679 - 688 . in brief , the [ f - 18 ]- fluoride ( 34 . 2 gbq ) was immobilized on a preconditioned qma ( waters ) cartridge ( preconditioned with 5 ml 0 . 5m k 2 co 3 and 10 ml water ). the [ f - 18 ]- fluoride was eluted with a solution of k 2 co 3 ( 2 . 7 mg ) in 50 μl water and k222 ( 15 mg ) in 950 μl acetonitrile . this solution was dried at 120 ° c . under vacuum and a stream of nitrogen . additional acetonitrile ( 1 ml ) was added and the drying step was repeated . a solution of dibromomethane ( 100 μl ) in acetonitrile ( 900 μl ) was added and heated at 130 ° c . for 5 min . the reaction was cooled and the [ f - 18 ]- fluoromethylbromide was distilled under a nitrogen flow of 50 ml / min through 4 silica cartridges into a solution of d - tyrosine ( 3 mg ), with 10 % naoh ( 13 . 5 μl ) in dmso ( 1 ml ). this solution was heated at 110 ° c . for 5 min and then cooled to 40 ° c . the reaction mixture was purified by hplc ( synergi hydro rp 4p 250 × 10 mm ; 10 % acetonitrile in water at ph 2 ; flow 5 ml / min ). the product peak was collected , diluted with water ( ph 2 ) and passed through a c18 plus environmental spe . the spe was washed with water ph2 ( 5 ml ). the product was eluted with a 1 : 1 mixture of etoh and water ph2 ( 3 ml ). starting from 34 . 2 gbq [ f - 18 ]- fluoride , 3 . 2 gbq ( 15 % d . c .) with a specific activity of 49 gbq / μmol [ f - 18 ]- dfmt were obtained in a synthesis time of 71 minutes . 10 to 12 mbq [ f - 18 ]- fluoride or [ f - 18 ]- d - fmt were injected i . v . into the tail vein . 60 min after injection anesthesia was induced by isoflurane / o2 and twenty - minute micro - pet / computed tomography ( ct ) scans were obtained using an inveon micro pet / ct scanner ( siemens ). after the pet / ct measurement , the mice were sacrificed by an overdose of isoflurane / o2 . with the information from the pet images the bones which showed [ f - 18 ]- d - fmt were removed and fixed in 4 % neutral - buffered formalin for several days . after fixation , decalcification in immunocal containing formic acid and routine dehydration , the samples were embedded in paraffin , and 4 - 6 μm thick sections were stained with hematoxylin - eosin ( h & amp ; e ) for microscopical examination . an immunohistochemistry for the detection of pan - cytokeratin ( ae1 / ae3 , abcam # ab27988 , cambridge , uk ) which recognizes epitopes present in epithelial tissues was performed in order to discriminate the origin of the tumor cells : epithelial vs . nonepithelial . for differential demonstration of osteoid and collagen one slide was stained with masson goldner trichrome ( mgt ) which stains osteoid and collagen blue green . detection of bone metastases by [ f - 18 ]- d - fmt was pre - clinically investigated using the 786 - 0 / luc human renal cell adenocarcinoma bone metastasis mouse model . in in vitro experiments investigating the uptake of [ f - 18 ]- d - fmt into the 786 - o / luc cells , good uptake was observed reaching 12 . 8 % applied dose / 10 6 cells after 30 min . the luciferase gene transfected 786 - o cells offered a reliable tool for following bone metastases formation in vivo by whole - body bioluminescence imaging ( bli ) longitudinally . after the i . v . injection of luciferin , the luciferase containing 786 - o tumor cells catalyzed the oxidation of luciferin resulting in the appearance of bioluminescence . the detection of the bioluminescence by ccd camera was used for monitoring metastasis progression and showed spread of cancer cells in the regions of hind limbs , forelimbs , spine and skull . 51 days after the inoculation of the 786 - o / luc cells into the mice , pet / ct imaging was performed with [ f - 18 ]- fluoride ( fig1 right side ). the images showed high accumulation in multiple osteolytic lesions in the spine , skull , forelimbs and hind limbs indicating increased mineralization compared with the uptake in healthy bone with normal appearance . the same mouse was imaged 2 weeks later ( day 65 ) with [ f - 18 ]- d - fmt ( fig1 left side ). the same bone lesions previously visualized with [ f - 18 ]- fluoride were visible as well as additional lesions . thus , the localization of tumor cells monitored by [ f - 18 ]- d - fmt correlated with affected areas of the skeleton as visualized by the [ f - 18 ]- fluoride scan . there was also uptake into the pancreas of the mice . the calculation of % id / g values based on the suv was between 4 . 1 and 6 . 8 for the various lesions . the size of the metastases ranged from 1 . 5 mm to more than 7 mm in diameter . [ f - 18 ]- d - fmt showed no uptake into the healthy bone . reconstruction of the ct and pet images by surface rendering showed that there are parts of the bones missing where the tumor cells invaded the skeleton ( fig2 left ). the pet signal ( fig2 middle ) showed a very specific localization which fitted into the holes in the bones , if the two images were fused ( fig2 right ). even very small lesions as in the shoulder blade could be visualized by pet while the ct remained inconclusive . histologically the hematopoietic cell areas are wholly replaced by tumor tissue in the medullary cavity in all samples collected after the pet / ct imaging . the proliferating cells were large pleomorphic , with abounded cytoplasm and round dense nuclei , in other areas spindle - shaped cells separated by a moderate amount of collganous matrix were more predominant ( fig3 ). a moderate number of mitotic figures were present ( 0 - 3 at 40 ×). additionally , in some samples multinucleated giant cells were present . an essential feature of the tumors was that lysis of normal bone occurred simultaneously with the formation of new osteoid , which stained blue green with mtg ( fig3 ). the tumor cells were positive for pan - cytokeratin , which confirmed that they are of epithelial origin . in the experiments , it is clearly shown that [ f - 18 ]- d - fmt is able to detect bone metastases in a nude mouse model . the areas of the bone , which showed accumulation of [ f - 18 ]- d - fmt were removed and histologically examined . tumor cells were detected which had invaded the bones and which are most likely responsible for the [ f - 18 ]- d - fmt accumulation . in addition , tsukada et al ( tsukada h , sato k , fukumoto d , nishiyama s , harada n , kakiuchi t . evaluation of d - isomers of o - 11c - methyl tyrosine and o - 18f - fluoromethyl tyrosine as tumor - imaging agents in tumor - bearing mice : comparison with l - and d - 11c - methionine . j nucl med . april 2006 ; 47 ( 4 ): 679 - 688 .) it was demonstrated in a turpentine - induced inflammation model , that [ f - 18 ]- d - fmt shows no uptake in inflammatory muscle tissue whereas fdg was taken up in inflammatory muscle tissue . [ f - 18 ]- fluoride reflects an unspecific uptake into regenerating and remineralizing bone , also the larger bones ( spine , legs ) as well as the joints showed [ f - 18 ]- fluoride uptake . in contrast to [ f - 18 ]- fluoride , osteoblastic activity is not detected by [ f - 18 ]- d - fmt . comparison of the pet / ct scans of [ f - 18 ]- fluoride and the [ f - 18 ]- d - fmt scan showed that [ f - 18 ]- d - fmt accumulated in all bone metastases imaged by [ f - 18 ]- fluoride but not in bone wherein osteoblastic activity was showed with [ f - 18 ]- fluoride . 25 days after the inoculation of the mda - mb231sa / luc cells into the mice , pet / ct imaging was performed with [ f - 18 ]- d - fmt as a second bone metastases model using a breast carcinoma cell line mda - mb231sa / luc which is an established model for the formation of bone metastases ( mbalaviele g , dunstan c r , sasaki a , williams p j , mundy g r , yoneda t . e - cadherin expression in human breast cancer cells suppresses the development of osteolytic bone metastases in an experimental metastasis model . cancer res 1996 ; 56 : 4063 - 70 .). [ f - 18 ]- d - fmt also showed uptake into the bone metastases ( fig4 ). to conclude , [ f - 18 ]- d - fmt is useful for the detection of bone metastases . | 0 |
this disclosure provides for a power spectral characterization and the identification of available upstream frequency regions which would support communications . the present invention enables an automatic determination of how much rf power is available in a network for addition of additional services , and ingress power before a predetermined soft failure occurs . a soft failure is a degradation in signal quality which causes pre equalized errors to occur , but are within available limits of error correction , the intent being that there will be no noticeable impairment to the live services on a network . the test in the invention generally involves demodulation of a specified test qam carrier and measurement of its signal quality to determine impact caused by stressing the network . the methodology described in this invention instructs two docsis terminal devices ( cable modems or mtas ) to transmit simultaneously and measures the affects on a third communications channel , such as the mer ( mean error ratio ), ber ( bit error rate ), and per ( packet error rate ). subsequently , power is increased for the two docsis terminal devices until , an impact on the communicating channel is detected . that is , it monitors the affects of increasing power in the return - path of the cable network on an active communications signal and logs the total power added when said power begins to impact the performance of the communications channel . the approach detailed in this disclosure requires that the three docsis terminal devices reside on the same optical node . a methodology for isolating devices which reside on the same optical node is provided in a commonly assigned disclosure attorney docket no . bcs04122 , entitled method and apparatus for grouping terminal network devices filed on sep . 5 , 2006 and assigned u . s . ser . no . 11 / 470 , 034 . preferably , the power margin test should not occur in conjunction with other changes in the network , such as changing of optical routing , ingress level switching or any other routine or event that will likely cause rf levels to be unstable . adequate margin should also preferably be available in the network to allow the addition of 2 docsis channels . this margin may be determined by first estimating the total power of the current upstream loading via fft measurement , then adding a test channel at the same level of the cable modem channel and rerunning the fft . if total power increase is less than 3 db with cable modem and test channel loading combined then the system is still functioning in linear region and power addition from test channel is acceptable . otherwise the optical link may be overdriven . the margin test should be repeated by adding the second test signal . the fft should also be run with both test signals transmitting at the same time during the second test . preferably , an active return path is providing services at the time that the operator desires to associate ( group ) network elements according to common optical nodes . also , this test picks test frequency locations based upon avoiding interference of 2 nd order intermods on active data services . we are assuming adequate margin is available such that 3 rd order products are not a problem for the active services . also , the approach preferably uses docsis cable modems to generate test signals . therefore test signals will be one of the available docsis bandwidths ( 200 khz , 400 khz , 800 khz , 1600 khz , 3200 khz , 6400 khz ). preferably , the test will use 800 khz bandwidth due to narrow bandwidths minimize the amount of clean spectrum required within the return path , and because many modems have problems with the 400 and 200 khz widths . fig1 illustrates an exemplary network in which a plurality of terminal network elements 8 ( e . g . cable modems , set top boxes , televisions equipped with set top boxes , or any other element on a network such as an hfc network ) are connected to a cable modem termination system ( cmts ) 10 located in a headend 14 through nodes 12 and one or more taps ( not shown ). in an exemplary arrangement , headend 14 also contains an optical transceiver 16 which provides optical communications through an optical fiber to the plurality of nodes 12 . the cmts 10 connects to an ip or pstn network 6 . those of skill in the art will appreciate that there may be a plurality of nodes 12 connected to a headend , and a headend may contain a plurality of cmts units , each of which contain a plurality of receivers ( e . g . 8 receivers ) each of which communicate with a plurality ( e . g . 100 s ) of network elements 8 . the cmts 10 may also contain a spare receiver which is not continuously configured to network elements 8 , but may be selectively configured to network elements 8 . use of a spare receiver is described in commonly assigned patent application ser . no . 11 / 171066 , filed on jun . 30 , 2005 and titled automated monitoring of a network , herein incorporated by reference in its entirety . fig2 illustrates a logical architecture of an exemplary cmts 10 . as illustrated in fig2 , cmts 10 may contain a processing unit 100 which may access a ram 106 and a rom 104 , and may control the operation of the cmts 10 and rf communication signals to be sent by the network elements 8 to the cmts . processing unit 100 preferably contains a microprocessor 102 which may receive information , such as instructions and data , from a rom 104 or ram 106 . processing unit 100 is preferably connected to a display 108 , such as a crt or lcd display , which may display status information such as whether a station maintenance ( sm ) is being performed or an unregistered receiver is eligible for load balancing . an input keypad 110 may also be connected to processing unit 100 and may allow an operator to provide instructions , processing requests and / or data to processor 100 . a rf transceiver ( transmitter / receiver ) 20 preferably provides bi - directional communication with a plurality of network elements 8 through optical transceivers 16 , nodes 12 and a plurality of network taps ( not shown ). those of skill in the art will appreciate that cmts 10 may contain a plurality of rf transceivers , e . g . 8 rf transceivers and a spare rf transceiver . each rf transceiver may support over 100 network elements . rf transceiver 20 , such as a broadcom 3140 receiver ( transceiver ), is preferably used to acquire equalizer values and burst mean error ratio ( mer ) measurements , packet error rate ( per ) and bit error rate ( ber ). rf transceiver 20 may also include fft module 308 to support power measurements . the communication characteristics of each receiver 20 may be stored on rom 104 or ram 106 , or may be provided from an external source , such as headend 14 . ram 104 and / or rom 106 may also carry instructions for microprocessor 102 . fig3 illustrates an exemplary network element 8 , such as a cable modem . network element 8 preferably contains a processor 202 which may communicate with a ram 206 and rom 204 , and which controls the general operation of the network element , including the pre - equalization parameters and preamble lengths of communications sent by the network element in accordance with instructions from the cmts 10 . network element 8 also contains a transceiver ( which includes a transmitter and receiver ) which provides bidirectional rf communication with cmts 10 . network element 10 may also contain an equalizer unit which may equalize the communications to cmts 10 . network element 10 may also contain an attenuator 220 which may be controlled by microprocessor to attenuate signals to be transmitted to be within a desired power level . those of skill in the art will appreciate that the components of network element 8 have been illustrated separately only for discussion purposes and that various components may be combined in practice . fig4 illustrates further detail of an exemplary headend 14 . headend 14 preferably contains an optical transceiver 16 which preferably includes an optical receiver 316 configured to receive optical signals through an optical fiber from nodes 12 . a plurality of laser transmitters 312 provide downstream optical communications to nodes 12 through an optical fiber . a laser transmitter may be assigned to communicate with a single node . a fast fourier transform ( fft ) module 308 such as a broadcom 3140 receiver fft , identifies frequencies in the optical signals received and provides desired frequencies to power monitoring unit 310 . preferably , the fft supports different windows , and sample lengths ( 256 , 512 , 1024 , 2048 ) with an output of frequency of 0 - 81 . 92 mhz . minimum resolution results from maximum window length of 2048 samples and yields an fft cell resolution of 80 khz . cpu 30 preferably contains a microprocessor 301 which interacts with ram 306 and rom 304 and controls the operation of the headend unit and preferably implements the method illustrated in fig5 . upon receiving a downstream communication signal from a network element , via cmts 10 , cpu 30 preferably provides instructions to modulate one of the laser transmitters 312 to transmit the communication signal to nodes 12 . optical receivers 316 are preferably configured to monitor the optical signal transmitted by nodes 12 , such as by receiving a portion of the signal . optical receiver 316 preferably provides the monitored portion to the fft module 308 where intermods may be determined and power monitor unit 310 where the power level in a specific frequency ( such as the test frequency ) may be measured or the total power of the signal may be measured . an exemplary process for automatically determining the power margin available in the system on an optical node is illustrated in fig5 . as illustrated in step s 0 of fig5 , three network elements ne 1 , ne 2 and ne 3 are selected for to be used by two network elements in the process . preferably , the three modems are connected to the same hfc node and return laser , are currently idle , have sufficient ability to have their transmit power turned up by ( 15 ) db , and can be controlled remotely by the cmts to move to new frequencies at command and change their transmission power level . also in a preferred implementation , one of these selected network elements will be used to provide a modulated signal , such as a 16 qam , 2 . 56 msym / sec , which is used as the “ test signal ” for the power margin test . the other two network elements will be instructed to transmit on a channel which impacts the test signal , such as 800 khz qpsk channels , whose power is increased sufficiently to cause loading ( compression ) of the rf devices ( most likely the return laser transmitter ) in the system . ideally , we want to find two frequencies that network elements ne 1 and ne 2 could transmit on which would not produce a 2 nd order intermod at a third frequency to which network element ne 3 may be assigned . each of the three frequencies are preferably within the 5 - 42 mhz spectrum . the possible frequencies may be identified by a plurality of techniques , such as by empirically determining usable frequency regions for qpsk ( quadrature phase shift keying , also referred to as four qam ) transmission from a survey process . the communication frequencies ( f 1 and f 2 ) are preferably selected such that f 1 ± f 2 does not fall on f 3 and each of f 1 , f 2 and f 3 lies between 5 - 42 mhz . the three frequencies are also preferably selected such that second order products from these frequencies do not fall on desired traffic in the network , if possible . preferably , frequencies f 1 and f 2 can be activated as docsis upstream channels with default upstream cmts receive levels without causing any significant harm to any other active services . as illustrated in fig5 , the power of the frequency band , e . g . 5 - 42 mhz is measured , step s 2 . this measurement provides a reference baseline power of the frequency band , as illustrated in fig6 . in a preferred implementation , this measurement may be performed as an incremental power measurement of the band of interest ( 5 - 42 ) mhz and may be recorded showing amplitude vs . frequency for at least 10 times showing occupied frequency bands and periodicity of channels on the network . an estimation of the total network rf power vs . single channel power is may also be mathematically estimated from measured data . as illustrated in step s 4 of fig5 , network element 3 is assigned to frequency f 3 , which is used as the test frequency f ( t ), and the baseline error rates , such as mer , per and ber are measured . the error rate may be measured at the cmts by measuring the mer , per and ber , such as by using an equalizer contained in the cmts , not shown . the total power may be measured at the cmts , for example by measuring the received rf power at fft module 308 and power monitor module 301 . alternatively , power may be determined from the settings on attenuator 220 of network element 3 . as illustrated in step s 6 of fig5 , network element 1 is assigned to frequency f 1 and network element 2 is assigned to frequency f 2 . network elements 1 and 2 are instructed to simultaneously transmit at a predetermined power level pl 1 and pl 2 , respectively , while network element 3 transmits the modulated test signal , step s 8 . the error rate of the modulated test signal from network element 3 is measured and the total power of the frequency spectrum , e . g . 5 - 42 mhz is measured again . the error rate may be measured at the cmts by measuring the mer , per and ber , such as by using an equalizer contained in the cmts , not shown . the total power may be measured at the cmts , for example by measuring the received rf power at fft module 308 and power monitor module 301 . alternatively , power may be determined from the settings on attenuator 220 of network element 3 . pl 1 and pl 2 may be the same power level and may be at level l which was assigned as the nominal power level . in this step , network elements 1 and 2 are preferably instructed to perform a station maintenance ( sm ) burst at exactly the same time . those of skill in the art will appreciate that this may be done by lining up the minislots in the maps for the two upstream channels associated with network elements a and b . those of skill in the art will also appreciate that the map or maps data provide a schedule of time slots which allocates different network elements specific time intervals in which they are allowed to transmit data to the cmts . from a cmts software perspective , this should not be a complicated problem as the im broadcast intervals are already aligned across all channels within a single spectrum group . the fft processor should also be configured to trigger samples based upon the map minislot interval when the two sm bursts from the network elements will align . the combined power ( pc ) and the power of f 3 ( pf 3 ) are measured , as illustrated in step s 10 . it may be desirable to perform steps s 8 and s 10 several times to eliminate the possibility that a coincidental ingress happened at the exact same instance as the sm bursts . the cmts spare receiver may be used to make the error rate and power measurements to avoid impacting service provided to customers ,. alternatively , another receiver could be used to make the measurements by being taken “ off line ” or by adjusting for the impact caused by normal service . if the simultaneous transmission has not increased the power level in the fft cell at the test frequency ( f 3 ) to significantly impact the test signal , step s 12 , no , then in step s 18 , then the power level of network element 1 or 2 or both is increased and the process in steps s 8 and beyond is repeated . if the test signal from network element 3 is impacted , step s 12 yes , the power addition and power margin are calculated , step s 14 and logged in step s 16 . the mer , per and / or ber is measured at each incremental increase in power level and signals are increased until degradation in mer and more importantly a significant increase in per is noted . the cause of this impairment is loading ( compression ) of the rf devices ( most likely the return laser transmitter ) in the system from the power created by the transmissions of network elements 1 and 2 . the processes in fig5 may be implemented in hard wired devices , firmware or software running in a processor . a processing unit for a software or firmware implementation is preferably contained in the cmts . any of the processes illustrated in fig5 may be contained on a computer readable medium which may be read by microprocessor 301 . a computer readable medium may be any medium capable of carrying instructions to be performed by a microprocessor , including a cd disc , dvd disc , magnetic or optical disc , tape , silicon based removable or non - removable memory , packetized or non - packetized wireline or wireless transmission signals . the invention enables the technician or engineer to remotely characterize upstream total power margin quickly at a central location , such as the headened such as by using the motorola bsr64000 , rather than having to use external test equipment , such as the vector signal analyzer and deploying technicians to various locations within the cable plant without impacting active services . it also allows the mso to plan for future offerings and schedule needed maintenance by allowing him / her to periodically monitor this power margin . all measurements may be made through the use of the existing terminal devices ( specifically , docsis terminal devices such as mtas and cable modems ) as well as headend equipment ( specifically a docsis cmts ). those of skill in the art will appreciate that the techniques of this invention allows an operator to determine available power margin on a network without the need for placing test instrumentation remotely in the cable plant . in addition , the technique discloses in the invention does not require an operator or technician to be dispatched to remote locations in the hfc network . all measurements may be made through the use of the existing terminal devices ( specifically , docsis terminal devices such as mtas and cable modems ) as well as headend equipment ( specifically a docsis cmts ). accurate knowledge of available power margin will enable an operation to utilize the available resources of their network more efficiently , such as by adding additional network elements to portions of the network with a large power margin and shifting network elements away from portions with a small power margin to improve signal quality and network speed . | 7 |
a method and apparatus for generating multimedia overviews of documents , referred to herein as multimedia thumbnails ( mmnails ), are described . in one embodiment , mmnails contain the most important visual and audible ( e . g ., keywords ) elements of a document and present these elements in both the spatial domain and the time dimension . an mmnail results from analyzing , selecting and synthesizing information considering constraints given by the output device ( e . g ., size of display , limited image rendering capability ) or constraints on an application ( e . g ., limited time span for playing audio ). in one embodiment , the multimedia overview generation process includes extracting multimedia information from still image documents ( visual and audible ), assigning of importance and time attributes to visual and audible information segments , and optimizing multimedia information for visual and audio channels given device and application constraints . thus , mmnails use both channels . depending on the device or user preference , one of the two channels may be preferred over the other . as a result , mmnails utilize both the visual and audio channel of the device to present an overview of the document in a limited display and in a limited time - frame , and reduce , and potentially minimize , the interaction required by the user . in contrast to prior art approaches , the original document may be a still image with no multimedia content attached . in the following description , numerous details are set forth , such as distances between components , types of molding , etc . it will be apparent , however , to one skilled in the art , that the present invention may be practiced without these specific details . in other instances , well - known structures and devices are shown in block diagram form , rather than in detail , in order to avoid obscuring the present invention . some portions of the detailed descriptions that follow are presented in terms of algorithms and symbolic representations of operations on data bits within a computer memory . these algorithmic descriptions and representations are the means used by those skilled in the data processing arts to most effectively convey the substance of their work to others skilled in the art . an algorithm is here , and generally , conceived to be a self - consistent sequence of steps leading to a desired result . the steps are those requiring physical manipulations of physical quantities . usually , though not necessarily , these quantities take the form of electrical or magnetic signals capable of being stored , transferred , combined , compared , and otherwise manipulated . it has proven convenient at times , principally for reasons of common usage , to refer to these signals as bits , values , elements , symbols , characters , terms , numbers , or the like . it should be borne in mind , however , that all of these and similar terms are to be associated with the appropriate physical quantities and are merely convenient labels applied to these quantities . unless specifically stated otherwise as apparent from the following discussion , it is appreciated that throughout the description , discussions utilizing terms such as “ processing ” or “ computing ” or “ calculating ” or “ determining ” or “ displaying ” or the like , refer to the action and processes of a computer system , or similar electronic computing device , that manipulates and transforms data represented as physical ( electronic ) quantities within the computer system &# 39 ; s registers and memories into other data similarly represented as physical quantities within the computer system memories or registers or other such information storage , transmission or display devices . the present invention also relates to apparatus for performing the operations herein . this apparatus may be specially constructed for the required purposes , or it may comprise a general - purpose computer selectively activated or reconfigured by a computer program stored in the computer . such a computer program may be stored in a computer readable storage medium , such as , but is not limited to , any type of disk including floppy disks , optical disks , cd - roms , and magnetic - optical disks , read - only memories ( roms ), random access memories ( rams ), eproms , eeproms , magnetic or optical cards , or any type of media suitable for storing electronic instructions , and each coupled to a computer system bus . the algorithms and displays presented herein are not inherently related to any particular computer or other apparatus . various general - purpose systems may be used with programs in accordance with the teachings herein , or it may prove convenient to construct more specialized apparatus to perform the required method steps . the required structure for a variety of these systems will appear from the description below . in addition , the present invention is not described with reference to any particular programming language . it will be appreciated that a variety of programming languages may be used to implement the teachings of the invention as described herein . a machine - readable medium includes any mechanism for storing or transmitting information in a form readable by a machine ( e . g ., a computer ). for example , a machine - readable medium includes read only memory (“ rom ”); random access memory (“ ram ”); magnetic disk storage media ; optical storage media ; flash memory devices ; electrical , optical , acoustical or other form of propagated signals ( e . g ., carrier waves , infrared signals , digital signals , etc . ); etc . fig1 is a flow diagram of one embodiment of a process for generating multimedia overviews of documents . the process is performed by processing logic that may comprise hardware ( e . g ., circuitry , dedicated logic , etc . ), software ( such as is run on a general purpose computer system or a dedicated machine ), or a combination of both . referring to fig1 , using an electronic version of a document ( not necessarily containing video or audio data ) and its metadata , the process begins by processing logic pre - processing the document and / or its metadata and determining visual focus points ( vfps ) and / or important audible document information ( adis ) ( processing block 101 ). given the vfps and the adi , along with device and application constraints ( e . g ., display size , a time constraint ), processing logic multimedia selects visual and / or audible information to be included in the output representation ( e . g ., a multimedia thumbnail ) ( processing block 102 ). in one embodiment , the selection is optimized to include the preferred visual and audible information in the output representation , where preferred information may include important information in the document , user preferred , important visual information ( e . g ., figures ), important semantic information ( e . g ., title ), key paragraphs ( output of a semantic analysis ), document context . important information may include resolution sensitive areas of a document . after selection , processing logic synthesizes the information into visual data ( for the visual channel , or representation ) and / or audio data ( for the audio channel , or representation ) to create a multimedia thumbnail ( processing block 103 ). thus , a thumbnail , in this context , may refer to a representation in which material from the document is presented visually and audibly . fig2 is a flow diagram of another embodiment of processing components for generating multimedia overviews of documents . in one embodiment , each of the modules comprises hardware ( e . g ., circuitry , dedicated logic , etc . ), software ( such as is run on a general purpose computer system or a dedicated machine ), or a combination of both . referring to fig2 , analyzer 203 receives document 201 and metadata 202 . metadata 202 may include author information and creation data , text ( e . g ., in a pdf file format where the text may be metadata and is overlayed with the document image ), an audio or video stream , urls , publication name , date , place , access information , encryption information , image and scan resolution , mpeg - 7 descriptors etc . in response to these inputs , analyzer 203 performs pre - processing on these inputs and generates outputs information indicative of one or more visual focus points in document 101 along with information indicative of audible information in the document . the audible information may be information that is important in document 201 and / or metadata 202 . in one embodiment , analyzer 203 comprises document pre - processing unit 203 a , metadata pre - processing unit 203 b , visual focus points identifier 203 c , and important audible document information identifies 203 d . in one embodiment , document pre - processing unit 203 a performs one or more of optical character recognition ( ocr ), layout analysis and extraction , jpeg 2000 compression and header extraction , document flow analysis , font extraction , face detection and recognition , graphics extraction , and music notes recognition , which is performed depending on the application . in one embodiment , document pre - processing unit 203 a includes expervision ocr software to perform layout analysis on characters and generates bounding boxes and associated attributes , such as font size and type . in another embodiment , bounding boxes of text zones and associated attributes are generated using scansoft software . in another embodiment , a semantic analysis of the text zone is performed in the manner described in aiello m ., monz , c ., todoran , l ., worring , m ., “ document understanding for a broad class of documents ,” international journal on document analysis and recognition ( ijdar ), vol . 5 ( 1 ), pp . 1 - 16 , 2002 , to determine semantic attributes such as , for example , title , heading , footer , and figure caption . metadata pre - processing unit 203 b may perform parsing and content gathering . for example , in one embodiment , metadata preprocessing unit 203 b , given an author &# 39 ; s name as metadata , extracts the author &# 39 ; s picture from the world wide web ( www ) ( which can be included in the mmnail later ). in one embodiment , metadata pre - processing unit 203 b performs xml parsing . after pre - processing , visual focus points identifier 203 c determines and extracts visual focus segments , while important audible document information identifier 103 d determines and extracts important audible data . in one embodiment , visual focus points identifier 203 c identifies visual focus points based on ocr and layout analysis results from pre - processing unit 203 a and / or xml parsing results from pre - processing unit 203 b . in one embodiment , visual focus points identifier 203 c performs analysis techniques set forth in u . s . patent application ser . no . 10 / 435 , 300 , entitled “ resolution sensitive layout of document regions ,” filed may 9 , 2003 , published jul . 29 , 2004 ( publication no . us 2004 / 0145593 a1 ) to identify text zones and attributes ( e . g ., importance and resolution attributes ) associated therewith . text zones , may include a title and captions , which are interpreted as segments . in one embodiment , visual focus points identifier 203 c determines the title and figures as well . in one embodiment , figures are segmented . in one embodiment , audible document information identifier 203 d identifies audible information in response to ocr and layout analysis results from pre - processing unit 203 a and / or xml parsing results from pre - processing unit 203 b . examples of visual focus segments include figures , titles , text in large fonts , pictures with people in them , etc . note that these visual focus points may be application dependent . also , attributes such as resolution and saliency attributes are associated with this data . the resolution may be specified as metadata . in one embodiment , these visual focus segments are determined in the same fashion as specified in u . s . patent application ser . no . 10 / 435 , 300 , entitled “ resolution sensitive layout of document regions ,” filed may 9 , 2003 , published jul . 29 , 2004 ( publication no . us 2004 / 0145593 a1 ). in another embodiment , the visual focus segments are determined in the same manner as described in le meur , o ., le callet , p ., barba , d ., thoreau , d ., “ performance assessment of a visual attention system entirely based on a human vision modeling ,” proceedings of icip 2004 , singapore , pp . 2327 - 2330 , 2004 . saliency may depend on the type of visual segment ( e . g ., text with large fonts may be more important than text with small fonts , or vice versa depending on the application ). the importance of these segments may be empirically determined for each application prior to mmnail generation . for example , an empirical study may find that the faces in figures and small text are the most important visual points in an application where the user assess the scan quality of a document . the salient points can also be found by using one of the document and image analysis techniques in the prior art . examples of audible information include titles , figure captions , keywords , and parsed meta data . attributes , e . g ., importance ( saliency ) and time attributes ( duration after synthesizing to speech ) are also attached to the audible information . importance of audible segments may depend on its type . for example , an empirical study may show that the document title and figure captions are the most important audible information in a document for a “ document summary application ”. some attributes of vfps and adis can be assigned using cross analysis . for example , the time attribute of a figure ( vfp ) can be assigned to be the same as the time attribute of the figure caption ( adi )). in one embodiment , audible document information identifier 203 d performs term frequency - inverse document frequency ( tfidf ) analysis to automatically determine keywords based on frequency , such as described in matsuo , y ., ishizuka , m .” keyword extraction from a single document using word co - occurrence statistical information , international journal on artificial intelligence tools , vol . 13 , no . 1 , pp . 157 - 169 , 2004 or key paragraphs as in fukumoto , f ., suzuki , y ., fukumoto , j ., “ an automatic extraction of key paragraphs based on context dependency ,” proceedings of fifth conference on applied natural language processing , pp . 291 - 298 , 1997 . for each keyword , audible document information identifier 203 d computes a time attribute as being the time it takes for a synthesizer to speak that keyword . in one embodiment , the time is computed by multiplying the number of characters by a speech - synthesizing constant , ssc . instead of figuring out audio time for each word , an approximation for this time is generated by having a constant ssc that is multiplied by the number of characters . ssc may be found by feeding a test text document , which has c n number of characters , to the synthesizer , measuring the time , t audio , that is required to play back the synthesized audio and dividing this time by the number of characters , ssc = t audio / c n . the ssc constant may change depending on the language choice , synthesizer that is used and the synthesizer options ( female vs male voice , accent type , talk speed , etc ). in a similar fashion , audible document information identifier 203 d computes time attributes for selected text zones , such as , for example , title , headings , and figure captions . each time attribute is correlated with its corresponding segment . for example , the figure caption time attribute is also correlated with the corresponding figure segment . in one embodiment , each audible information segment also carries an importance attribute that may reflect the visual importance ( based on font size and position on a page ) or reading order in case of text zone , the frequency of appearance in the case of keywords , or the visual importance attribute for figures and related figure captions . in one embodiment , the importance attribute is calculated in the same way as described in u . s . patent application ser . no . 10 / 435 , 300 , entitled “ resolution sensitive layout of document regions ,” filed may 9 , 2003 , published jul . 29 , 2004 ( publication no . us 2004 / 0145593 a1 ). the visual focus segments and important audible information are output to optimizer 204 . optimizer 204 receives the output from analyzer 203 , which includes the characterization of the visual and audible document information , and device characteristics , or one or more constraints ( e . g ., display size , available time span , user settings preference , and power capability of the device ), and computes a combination of visual and audible information that meets the device constraints and utilizes the capacity of information deliverable through the available output visual and audio channels . in this way , optimizer 204 operates as a selector , or selection mechanism . in one embodiment , in response to visual and audible information segments from analyzer 203 and other inputs such as the display size of the output device and the time span , l , which is the duration of final multimedia thumbnail , optimizer 204 performs an optimization algorithm . in one embodiment , given display resolution and multimedia thumbnail length l , the following pseudo - code is applied by optimizer 204 : sort figure captions based on the time attributes ( from short to long ) sort keywords based on their tfidf scores ( from high to low ) do linear packing of keywords based on their time attributes given first_page_hold + zoom_to_title the main function of the optimization algorithm is to first determine how many pages can be shown to the user , given each page is to be displayed on the display for 0 . 5 second , during the time span available . if the time left from the time span l is large enough after displaying each page , optimizer 204 allocates time for zooming on the title of the document . if the visual information channel is completely occupied during this time , the only other choice for information delivery is the audio channel , which is used by synthesized speech of keywords . if the time span for “ reading ” keywords is limited , a selection of the keyword list is performed following the keyword importance values , i . e . sorting the keyword list with respect to importance and computing the cut off after one or more keywords by optimizing the filling of the one - dimensional time span interval via a linear packing / filling order approach applied to the keywords &# 39 ; time attributes . if there is any time left after page flipping through the pages and title zooming , optimizer 204 sorts the captions of the figures based on their time attribute ( duration when their captions are synthesized to speech ) to fill the remaining available time . in one embodiment , optimizer 204 then applies a linear packing / filling order approach in a manner well - known in the art to the sorted time attributes to select which figures will be included in the multimedia thumbnail . still - image holding is applied to the selected figures of the document . during the occupation of the visual channel by image holding , the caption is “ spoken ” in the audio channel . after optimization , optimizer 204 re - orders the selected visual and audio segments with respect to the reading order . other optimizers may be used to maximize the joined communicated information in time span l and in the visual display of constrained size . synthesizer 205 composes the final multimedia thumbnail . in one embodiment , synthesizer 205 composes the final multimedia thumbnail by executing selected multimedia processing steps determined in optimizer 204 . in one embodiment , synthesizer 205 receives a file , such as , for example , a plain text file or xml file , having the list of processing steps . in another embodiment , the list of processing steps may be sent to synthesizer 205 by some other means such as , for example , through socket communication or corn object communication between two software modules . in yet another embodiment , the list of processing steps is passed as function parameters if both modules are in the same software . the multimedia processing steps may include the “ traditional ” image processing steps crop , scale , and paste , but also steps including a time component such as page flipping , pan , zoom , and speech & amp ; music synthesis . in one embodiment , synthesizer 205 comprises visual synthesizer 205 a , audio synthesizer 205 b , and synthesizer / composer 205 c . synthesizer 205 uses visual synthesis 205 a to synthesize the selected visual information into images and sequence of images , audio synthesizer 205 b to synthesize audible information into speech , and then synchronizer / composer 205 c to synchronize the two output channels ( audio and visual ) and compose multimedia thumbnail 220 . in one embodiment , for the visual composition including sequences of images ( without audio ) such as zoom and page flipping is performed using adobe aftereffects , while synchronizer / composer 205 c uses adobe premier . in one embodiment , audio synthesizer 205 b uses cmu speech synthesizing software ( festvox http :// festvox . org / voicedemos . html ) to create sound for the audible information . in one embodiment , synthesizer 205 does not include synchronizer / composer 205 c . in such a case , the output of synthesizer 205 may be output as two separate streams , one for audio and one for visual . the outputs of synchronizer / composer 205 c may be combined into a single file and may be separate audio and video channels . fig3 is a flow diagram of another embodiment of a process for processing documents . the process of fig3 is performed by processing logic which may comprise hardware ( e . g ., circuitry , dedicated logic , etc . ), software ( such as is run on a general purpose computer system or a dedicated machine ), or a combination of both . referring to fig3 , processing begins by processing logic identifying document information associated with a document ( e . g ., visual information , audible information , semantic information , etc .) ( processing block 301 ). after identifying the document information , processing logic converts the document information to information for one or more constrained time - based media channels ( processing block 302 ). in one embodiment , these media channels may be a visual channel , an audio channel , or a combination of both . the techniques described herein may be potentially useful for a number of applications . for example , the techniques may be used for document browsing for devices , such as mobile devices and multi - function peripherals ( mfps ). for example , when performing interactive document browsing on a mobile device , the document browsing can be re - defined , for example , instead of zoom and scroll , operations may include , play , pause , fast forward , speedup , and slowdown . in another mobile device application when performing document viewing and reviewing on mobile devices , the techniques set forth herein may be used to allow a longer version of the mmnail ( e . g ., 15 minutes long ) to be used to provide not only an overview but also understand the content of a document . this application seems to be suitable for devices with limited imaging capabilities , but preferred audio capability , such as cell phones . after browsing and viewing a document with a mobile device , in one embodiment , the mobile device sends it to a device ( e . g ., an mfp ) at another location to have the device perform other functions on the document ( e . g ., print the document ). in one mfp application , the techniques described herein may be used for document overview . for example , when a user is copying some documents at the mfp , as the pages are scanned , an automatically computed document overview may be displayed to the user , giving a person a head start in understanding the content of the document . an image processing algorithm performing enhancement of the document image inside an mfp may detect regions of problematic quality , such as low contrast , small font , halftone screen with characteristics interfering with the scan resolution , etc . an mmnail may be displayed on the copier display ( possibly without audio ) in order to have the user evaluating the quality of the scanned document ( i . e ., the scan quality ) and suggest different settings , e . g ., higher contrast , higher resolution . fig4 is a flow diagram of one embodiment of a process for performing document processing . the process may be performed by a processing logic that comprises hardware ( e . g ., circuitry , dedicated logic , etc . ), software ( such as is run on a general purpose computer system or a dedicated machine ), or a combination of both . referring to fig4 , the process begins by processing logic performing at least one imaging operation ( e . g ., scanning ) on a document ( processing block 401 ). after performing any imaging operations , processing logic identifies visual information in the document image . in one embodiment , processing logic identifies visual information by detecting regions of problematic quality . regions of problematic quality may include , for example , regions that have low contrast , small font , and a halftone screen characteristic that interferes with scan resolution . in another embodiment , the processing logic identifies visual information in the document by identifying resolution sensitive portions of an image . after identifying visual information , processing logic selects portions of the visual information for inclusion into a multi - media representation of the document ( processing block 403 ). in one embodiment , where processing logic identifies resolution sensitive portions of the image , processing logic selects the portions by zooming in , panning or titling the resolution sensitive portions . after selecting portions , processing logic displays the multimedia representation on a display to enable the review of the results of any imaging operation ( processing block 404 ). in one embodiment , after displaying the multimedia representation , processing logic receives an input to modify application of the imaging operation . in a translation application , the language for the audio channel can be selected by the user and audible information may be presented in language of choice . in this case , the optimizer functions differently for different languages since the length of the audio would be different . that is , the optimizer results depend on the language . in one embodiment , visual document text is altered . the visual document portion can be re - rendered in a different language . in one embodiment , the mmnail optimizations are computed on the fly , based on interactions provided by user . for example , if the user closes the audio channel , then other visual information may lead to different visual representation to accommodate this loss of information channel . in another example , if the user slows downs the visual channel ( e . g ., while driving a car ), information delivered through the audio channel may be altered . also , animation effects such as , for example , zoom and pan , may be available based on the computational constraints of the viewing device . in one embodiment , the mmnails are used to assist disabled people in perceiving document information . for example , visual impaired people may want to have small text in the form of audible information . in another example , color blind people may want some information on colors in a document be available as audible information in the audio channel . fig5 is a block diagram of an exemplary computer system that may perform one or more of the operations described herein . referring to fig5 , computer system 500 may comprise an exemplary client or server computer system . computer system 500 comprises a communication mechanism or bus 511 for communicating information , and a processor 512 coupled with bus 511 for processing information . processor 512 includes a microprocessor , but is not limited to a microprocessor , such as , for example , pentium processor , etc . system 500 further comprises a random access memory ( ram ), or other dynamic storage device 504 ( referred to as main memory ) coupled to bus 511 for storing information and instructions to be executed by processor 512 . main memory 504 also may be used for storing temporary variables or other intermediate information during execution of instructions by processor 512 . computer system 500 also comprises a read only memory ( rom ) and / or other static storage device 506 coupled to bus 511 for storing static information and instructions for processor 512 , and a data storage device 507 , such as a magnetic disk or optical disk and its corresponding disk drive . data storage device 507 is coupled to bus 511 for storing information and instructions . computer system 500 may further be coupled to a display device 521 , such as a cathode ray tube ( crt ) or liquid crystal display ( lcd ), coupled to bus 511 for displaying information to a computer user . an alphanumeric input device 522 , including alphanumeric and other keys , may also be coupled to bus 511 for communicating information and command selections to processor 512 . an additional user input device is cursor control 523 , such as a mouse , trackball , trackpad , stylus , or cursor direction keys , coupled to bus 511 for communicating direction information and command selections to processor 512 , and for controlling cursor movement on display 521 . another device that may be coupled to bus 511 is hard copy device 524 , which may be used for printing instructions , data , or other information on a medium such as paper , film , or similar types of media . furthermore , a sound recording and playback device , such as a speaker and / or microphone may optionally be coupled to bus 511 for audio interfacing with computer system 500 . another device that may be coupled to bus 511 is a wired / wireless communication capability 525 to communication to a phone or handheld palm device . note that any or all of the components of system 500 and associated hardware may be used in the present invention . however , it can be appreciated that other configurations of the computer system may include some or all of the devices . whereas many alterations and modifications of the present invention will no doubt become apparent to a person of ordinary skill in the art after having read the foregoing description , it is to be understood that any particular embodiment shown and described by way of illustration is in no way intended to be considered limiting . therefore , references to details of various embodiments are not intended to limit the scope of the claims that in them recite only those features regarded as essential to the invention . | 6 |
referring again to prior art fig2 a , clicking on the “ exterior front ” selection on the menu at the left side , initiates the downloading of the “ panoramic image of the exterior front view of the house from the server database , as noted under the “ bamboo . com / virtual tour ” logo at the center of the page . referring again to prior art fig2 b , when the downloading of the panoramic image is complete , the exterior scene of the home scrolls across the “ vr window ” on the computer screen . the buttons on the lower left corner of the vr window are control buttons activated by the computer mouse . by moving the cursor to the “ left ” arrow , and pressing down referring now to prior art fig2 c , clicking on the “ master bedroom ” selection on the menu at the left side of the page , causes the “ panoramic ” image of the master bedroom , to download from the site - server to the client / user &# 39 ; s computer screen . the scrolling and stopping functions are identical to those in fig2 b . the present invention relates to methods and apparatus to construct and display electronic / cyber / on - line showrooms , galleries , stores and malls to emulate the physical showrooms , galleries , stores , and malls . virtual reality ( vr ) shots with audio segments , and / or video films are made to visually , audibly , and contiguously present a show room , gallery , store , or object . each still picture 32 a of the vr shots or each frame 30 a , 30 b , 30 c , 30 d , 30 e , 30 f , 30 g , 30 h , and 30 i of the video film is given a unique frame address within the vr packet address . thus , each picture 32 a or each frame 30 a , 30 b , 30 c , 30 d , 30 e , 30 f , 30 g , 30 h , and 30 i is identifiable via the address of the packet and the address of the frame 30 a , 30 b , 30 c , 30 d , 30 e , 30 f , 30 g , 30 h , and 30 i . each significant and unique object 32 in the vr data packet , is given an unique identification , indexed by the area 50 the unique object 32 occupies in the frames 30 a , 30 b , 30 c , 30 d , 30 e , 30 f , 30 g , 30 h , and 30 i or pictures 32 a containing the object . links are assigned to that unique object 32 , which may appear in multiple frames , such that detailed information ( such as graphical , vr , video , audio , or textual descriptions ) related to the object 32 addressed by the links , can be retrieved from the database external to the vr data packet , on demand , such as when the object 32 in the proximity frames is “ clicked ,” from any of the proximity frames . clicking on a particular object 32 in a frame 30 a , 30 b , 30 c , 30 d , 30 e , 30 f , 30 g , 30 h , and 30 i , or in any of the proximity frames 30 b , 30 c , 30 d , 30 e , 30 f , 30 g , and 30 h in a vr presentation of a show room , gallery , or store , would select the link / links associated with the particular object 32 clicked , and store the links in a file on the client / use computer . multiple objects can be “ clicked ,”— i . e ., selected , within a vr presentation . when the viewing and the selection process is completed , and the collection of “ clicked ” links is submitted to the server , by clicking a “ submit ” button , all data , whether video , audio , vr , graphics , or textual , addressed by the links submitted are brought from the server database to the client / user / user computer with reference to each selected object . fig3 a shows the central scene about a primary object 32 , venus of milo of a virtual reality presentation of a museum hall . the small buttons 25 at the lower left corner scrolls the panoramic scene of the hall to the left , right , up , down , and zoom - in and pan - out . a selected set of nine frames 30 a , 30 b , 30 c , 30 d , 30 e , 30 f , 30 g , 30 h , and 30 i around the primary object 32 in this example , are shown in fig3 b . the limit of the conventional virtual reality of the known - art is here . there is no interaction or linking mechanism from inside the virtual reality images , such as these frames , to data outside of the vr packet . in fig3 b , there are nine virtual reality frames 30 a , 30 b , 30 c , 30 d , 30 d , 30 f , 30 g , 30 h , and 30 i around the primary object 32 in the hall , scanning from the left of the object through the object , to the right of the object , each assigned its unique frame identity in the present invention . in our implementation , each frame 30 a , 30 b , 30 c , 30 d , 30 e , 30 f , 30 g , 30 h , and 30 i in the virtual reality data packet is given an identification . a primary object 32 that appears in multiple proximity frames would be “ cut out ” from the rest of each frame , or the scene , and given a unique identification , and assigned a link , or a collection of links , to link to external data storage space that stores data associated with the object 32 . the primary object 32 appearing on several proximity frames , such as from fig3 b — frame 30 b through frame 30 h , would be identified as one object , and given the same set of links . a rectangular area 50 closely surrounding the object 32 in all of the proximity frames is cut as shown in fig3 c , and marked out and separated from the rest of the frame in order to be assigned a separate and unique identity to the object 32 . this is done for frame 30 b through frame 30 h in fig3 b . the rectangular area 50 in all 7 frames 30 b , 30 c , 30 d , 30 e , 30 f , 30 g , and 30 h are assigned the same identity representing the object 32 , and the same links to the memory space external to the virtual reality frames , containing the detailed information related to the object 32 . clicking within the rectangular area 50 in all 7 frames 30 b , 30 c , 30 d , 30 e , 30 f , 30 g and 30 h results in linking to the same set of data . fig3 d shows frames , video , or vr can all be linked and called on demand . in this example , the enlarged still image 32 a in fig3 d is further linked to another virtual reality data packet that presents the object in 360 - degree rotation . referring now to fig3 e , clicking the “ virtual reality55 button 70 in fig3 d , brings the “ rotating ” virtual reality data packet of the object , with the control buttons 25 at the lower left corner . fig3 f shows the 12 of the standard 36 frames 80 a , 80 b , 80 c , 80 d , 80 e , 80 f , 80 g , 80 h , 80 i , 80 j , 80 k and 801 shot from equally spaced angles , 360 - degrees around the object . when the number of shots and the speed of sequentially “ flashing in55 the still images into the viewing window are compatible , human eyes perceive that the object rotates on the viewing window . a larger number of shots would permit a smoother and slower rotation . the invention enables practical and actionable commerce applications of virtual reality and video casting or screaming technologies on the web , for example , in displaying objects in show rooms , galleries , stores , or stores in malls , shopping centers , or on main streets in a “ real life55 , in addition to conventional categorization , search , and listing presentations in the convention web stores and galleries . the current invention enables object images to be linked to additional textual , audio , graphical , video , or vr data stored in the database outside of the virtual reality or video data packet . clicking on the image of a sofa in such an “ active virtual reality55 show room of this invention for example , of an interior furnishing show room , would deposit the links associated with the image to a temporary file . when the entire vr or video presentation is viewed , and the selection of multiple interested objects shown in the vr presentation is completed , the collection of links of the objects selected is submitted to the server from the client / user computer , to retrieve data addressed by the submitted links , including but not limited to detailed audio or textual descriptions , additional graphics or vr presentations , pricing information and ordering / or buying submission mechanism , sorted and presented by each object at command . the present invention is implemented using software which can be written in many programming languages , or implemented with many web - page generation tools . the present invention can be used on a global or local computer network , on a personal computer , on viewable storage media such as a cd rom , on a wireless telephone , on a wireless personal assistant such as a palm pilot ®, or on any type of wired or wireless device that enables digitally stored information to be viewed on a display device . also , information displayed and viewed using the present invention can be printed , stored to other storage medium , and electronically mailed to third parties . numerous modifications to and alternative embodiments of the present invention will be apparent to those skilled to the art in view of the foregoing description . accordingly , this description is to be construed as illustrative only and is for the purpose of teaching those skilled in the art the best mode of carrying out the invention . details of the structure may be varied substantially without departing from the spirit of the invention and the exclusive use of all modifications which come within the scope of the appended claims is reserved . | 6 |
in an exemplary embodiment , a shaft adapter system is provided for providing multiple club lie and face angles . the lie angle 2 of a club 3 is the angle 2 between a horizontal surface 4 on which a club is laying and a longitudinal axis 5 of the club shaft 14 when a center portion 6 of a face 7 of the club head 10 is lying on such horizontal surface , as for example shown in fig1 . the face angle 8 is the angle between a plane 9 through the longitudinal axis 5 of the club shaft and a plane 11 tangent a hitting portion of the club face 7 , as for example shown in fig2 a , 2 b , and 2 c . in an exemplary system , a club head 10 is provided having a hosel opening 12 formed there - through to allow for coupling of a golf club shaft 14 , as for example shown in fig3 and fig6 b , 6 c and 6 d . in an exemplary embodiment , the opening 12 is formed having a section 15 having an inner surface 16 having a polygonal shape ( fig3 ). in an exemplary embodiment , the polygonal shape is an octagonal shape . a shaft adapter 20 is provided having a length having a first section 22 which in an exemplary embodiment defines a hosel , a second section 24 extending from the hosel having a polygonal outer surface shape complementary to the polygonal shape of the club head hosel opening inner surface 16 , as for example shown in fig4 . instead of a polygonal outer surface , the second section 24 may have longitudinal ridges 26 formed on the outer surface of the second section which are spaced apart , as for example shown in fig5 a and 5b . each ridge emulates an angular edge 27 of a polygon . for example , instead of an octagonal outer surface , a cylindrical outer surface with eight evenly spaced apart longitudinal ridges 26 may be used . the polygonal shaped outer surface section or the section with ridges of the shaft adapter is sized so that it can mate with the polygonal shaped inner surface 16 of the hosel opening such that the polygonal outer surface section or surface with ridges of the shaft adapter is prevented from rotating relative to the polygonal shaped opening . a third section 30 may extend from the second section of the shaft adapter as for example shown in fig4 , 5 a , 5 b and 6 . instead of the inner surface 16 of the club head hosel opening having a polygonal shape , in another exemplary embodiment , the inner surface may be cylindrical with grooves 28 extending radially and longitudinally to accommodate the ridges 26 or angular edges 27 of the second section 24 of the shaft adapter as for example shown in fig6 a . the shaft adapter is placed inside the club head opening 12 such that the angular edges or ridges of the shaft adapter are accommodated by the angular edges 31 or the grooves 28 of the club head opening 12 . two bores are defined in the shaft adapter . a first bore 32 is formed through the first section defining the hosel onto which is attached to the club shaft . the first bore is formed at an angle relative to a longitudinal axis of the shaft adapter as for example shown in fig7 . in other words , the longitudinal axis 36 of the first bore is at an angle 38 relative to the longitudinal axis 40 of the shaft adapter as for example shown in fig7 . in an exemplary embodiment , the angle 38 is 2 °. a second threaded bore 42 is defined in the shaft adapter along the shaft adapter longitudinal axis and extends to an opposite end of the shaft adapter opposite the first bore . a golf club shaft 14 is fitted and attached to the first bore . in an exemplary embodiment , the shaft is adhered to the first bore using an adhesive such as an epoxy . in another exemplary embodiment , the first bore is threaded and the shaft is threaded into the first bore . in yet a further exemplary embodiment , the shaft adapter is integral with the shaft . in other words , the shaft adapter is defined at the end of the shaft such that it only has the first bore . in an exemplary embodiment , a lip 44 extends from the inner surface below the section 15 of the club hosel opening 12 , as for example shown in fig8 . the lip narrows the opening 12 such that the shaft adapter can not displace axially past the lip . the shaft adapter with shaft is placed in the hosel opening 12 such that its second section 24 with the polygonal outer surface or ridges mates with the section 15 of the opening having the polygonal inner surface or depressions and the first section 22 of the shaft adapter defines the hosel of the club . a fastener 46 having a head 48 is positioned from the opposite side of the opening 12 and threaded into the threaded second bore 42 , such that the lip is sandwiched between the fastener head and the shaft adapter . in an exemplary embodiment , the fastener head 48 has an outer surface diameter which is greater than an inner surface diameter of the lip 44 . in this regard , as the fastener is threaded into the shaft adapter second bore , it pulls the shaft adapter towards the lip such that when the fastener is tightened onto the adapter , the lip retains the adapter in an axial direction and the fastener and shaft adapter sandwich the lip . since the first bore which accommodates the shaft is formed at an angle relative to the shaft adapter , rotating the orientation of the shaft adapter relative to the hosel opening 12 formed on the club will change the orientation of the shaft relative to the opening . in this regard , by rotating the adapter relative to the opening formed on the club head , the lie and face angle positions of the club may be changed . in an exemplary embodiment , a marker 50 may be provided at an outer surface of the shaft adapter in line with an angular edge 27 or ridge 26 . the marker serves as an indicator . for example , if the marker is positioned along the top angular edge or depression in the club head opening 12 , the club head will have predetermined lie and face angles . by orienting and installing the adapter into the club head opening such that the indicator is positioned along the different angular edges 31 or grooves 28 of the hosel opening , different lie and face angles are provided , as for example indicated in fig9 . in an exemplary embodiment , the fastener 46 is threaded onto the shaft adapter such that it tightens against the shaft adapter by being rotated in counter clockwise fashion . in another exemplary embodiment , the fastener may be tightened by being rotated in a clockwise fashion . the fastener may have a hexagonal depression which accepts an allen wrench for tightening . other types of fasteners may also be used . in other exemplary embodiments , the club head opening first section may have multiple grooves other than eight or may have a polygonal shape other than octagonal . for example , the inner surface of the first section of the club head hosel opening as well as the second section outer surface of the shaft adapter may be hexagonal , heptagonal , or decagonal , etc . in addition , the angle 38 between the longitudinal axis of the shaft adapter and the first threaded bore which accepts the shaft may be formed at different angles other than 2 °, as for example , 1 °, 3 °, etc . so that different lie and face angles may be provided by rotating the shaft adapter relative to the club opening . the angle of the first bore relative to the shaft adapter affects the angle of the shaft while the orientation of the shaft adapter relative to the head effects the orientation of the shaft angle relative to the head . in use , a club maker would be able to carry a single club head and using a shaft adapter will be able to form a club having a desired lie and face angle for a particular user by rotating , i . e ., orienting and positioning the shaft adapter to an appropriate orientation , as for example by lining the indicator with the appropriate club head hosel opening angular edge so as to align the adapter first bore with attached club shaft at a particular angle orientation . in an exemplary embodiment , the club maker may carry a single head having a hosel opening and multiple adapters each having the first bore formed at different angles relative to each shaft adapter longitudinal axis . in this regard , the club maker can make a club head having many different lie and face angles . moreover , as a player &# 39 ; s game progresses , or a player is simply looking for a change in clubs , the shaft adapter can be removed and re - inserted in another orientation to alter the lie and / or face angles of the club . such re - orientation of the shaft adapter can also provide directional help as one &# 39 ; s swing changes . in this regard , the inventive system allows a single club to grow with the owner &# 39 ; s game without becoming obsolete like many clubs in the market . the adapters may be sold separately and attached to any of the multitude of popular shafts available today creating a nearly limitless number of filling possibilities . for example , with three different lofted heads and eight shafts with adapters which are able to be configured in eight different positions , a club maker can produce 192 unique drivers with very limited inventories . although the present invention has been described and illustrated in respect to an exemplary embodiments , it is to be understood that it is not to be so limited , since changes and modifications may be made therein which are within the full intended scope of the this invention as hereinafter claimed . | 0 |
fig1 shows a block diagram of an automatic focusing ( af ) single lens reflex camera to which the present invention is applied . the af single lens reflex camera includes a camera body 11 , and a taking lens 51 which is detachably attached to the camera body 11 . a large part of a bundle of light rays transmitted through the taking lens 51 of the camera body 11 is reflected by a main mirror 13 towards a pentagonal prism 15 which constitutes a finder optical system . a part of the reflected light is made incident upon a light receiving element ( not shown ) of a photometering ic 17 . the incident light transmitted through the lens 53 is partly transmitted through a half mirror portion 14 of the main mirror 13 and is reflected downwardly by an auxiliary mirror 19 to be made incident on an object distance measuring ccd sensor unit 21 . the light receiving element provided in the photometering ic 17 outputs electrical signals corresponding to the quantity of light received thereby . analogue output signals are logarithmically compressed in the photometering ic 17 and sent to a main cpu 35 through a peripheral control circuit 23 to be converted to digital signals in the cpu 35 . the main cpu 35 calculates optimum exposure factors ( i . e ., shutter speed and / or diaphragm value ) in accordance with an object brightness and film sensitivity , and so on . as a result , a releasing operation is carried out ( i . e ., shutter mechanism 25 and diaphragm mechanism 27 are driven ) in accordance with the optimum shutter speed and diaphragm value to expose the film . when the releasing operation is effected , the peripheral control circuit 23 drives a mirror motor 31 through a motor driving circuit 29 to effect an up - down movement of the main mirror 13 . upon completion of exposure , a winding motor 33 is driven to wind the film . the object distance measuring ccd sensor unit 21 comprises a phase difference detecting type sensor having a beam splitter for splitting a bundle of light rays ( object light ) and ccd line sensors which receives the respective split beams and integrates them ( i . e ., photoelectric conversion and accumulation of electric charges ). the object distance measuring ccd sensor unit 21 outputs the integration data by the ccd line sensors to the main cpu 35 as a control means . the object distance measuring ccd sensor unit 21 is driven and controlled by the main cpu 35 and the peripheral control circuit 23 . the ccd sensor unit 21 has a monitoring element through which the peripheral control circuit 23 detects the brightness of an object to be photographed , so that the integration time is varied in accordance with the object brightness . the main cpu 35 performs a predetermined calculation ( prediction calculation ) to calculate the amount of defocus in accordance with the integration data output from the photometering ccd sensor unit 21 , to thereby obtain the direction of rotation and the number of revolutions ( i . e ., number of pulses of an encoder 41 ) of the af motor 39 in accordance with the defocus amount . as a result , the main cpu 35 drives the af motor 39 through the af motor drive circuit 37 in accordance with the direction of rotation and the number of pulses of the af motor 39 thus obtained . the main cpu 35 detects and counts the number of pulses output by the encoder 41 in accordance with the rotation of the af motor 39 and stops the af motor 39 when the counted value reaches the number of pulses . the main cpu 35 normally drives the af motor 39 by dc control , and maintains the af motor 39 at low constant speed ( constant speed control ) in accordance with the interval of the pulses output from the encoder 41 . the rotation of the af motor 39 is transmitted to the taking lens 41 through a joint 47 provided on a mount of the camera body 11 and a joint 57 provided on a mount of the taking lens 51 to be connected to the joint 47 . &# 34 ; dc control &# 34 ;, referred to above , is indicative of the af motor 39 being driven by a substantially direct current . &# 34 ; constant speed control &# 34 ;, referred to above , is indicative of the af motor 39 being driven at a constant speed . &# 34 ; dc control &# 34 ; and &# 34 ; constant speed control &# 34 ; are realized by a pwm control ( pulse width modulation ) control circuit in the illustrated embodiment . the main cpu 35 is connected to a photometering switch sws which is turned on when a release button ( not shown ) is depressed half way , a release switch swr which is turned on when the release button is fully depressed by , an automatic focusing switch swaf , and a main switch swm which is actuated to turn on and off a power source connected to the main cpu 35 and the peripheral elements , etc . the main cpu 35 indicates the set af , exposure value , photographic modes , shutter speed , diaphragm value , etc ., in indicator unit 45 which is usually provided on an outer surface of the camera body 11 and within the field of view of a finder . the main cpu 35 serves not only as a control means for generally controlling the whole camera system , but also as a focus detecting means and a moving object judging ( checking ) means . the main cpu 35 constitutes an object distance measuring means together with the ccd sensor unit 21 and the peripheral control circuit 23 , etc ., and a lens driving means together with the af motor 39 etc ., respectively . the taking lens 51 includes a focus adjusting mechanism 55 for moving a focusing lens unit ( group ) 53 in the optical axis direction , the lens joint 57 provided on the lens mount of the taking lens and connected to the body joint 47 of the camera body 11 to transmit the rotation of the af motor 39 to the focus adjusting mechanism 55 , and a lens cpu 61 for calculating necessary data of the taking lens 51 . the lens cpu 61 is connected to the peripheral control circuit 23 of the camera body 11 through a group of electrical contacts 59 and 49 , so that data communication between the main cpu 35 and the lens cpu 61 is effected through the peripheral control circuit 23 . the data sent from the lens cpu 61 to the peripheral control circuit 23 includes an open diaphragm value , maximum diaphragm value , focal length , and k value , etc . the k value represents the number of pulses of the encoder 41 ( i . e ., number of revolutions of the af motor 39 ) necessary for moving the image plane formed by the taking lens by a predetermined unit displacement ( e . g ., 1 mm ). the following discussion will be directed to the af operation with reference to fig2 through 9 . the af operation of the single lens reflex camera starts when the photometering switch sws is turned on . in the af operation , the photometering ccd sensor unit 21 commences a first integration . thereafter , the main cpu 35 calculates the amount of defocus and the number of drive pulses in accordance with the integration data . consequently , the af motor 39 is driven in accordance with the number of drive pulses thus obtained . in the illustrated embodiment , the af mode functions in the same way that the normal af mode functions when the object is still , and functions as the above - mentioned moving object predicting af mode when the object moves . furthermore , the af mode also includes an af single mode in which the focused state is locked when no object moves , and a focus priority af mode in which release can be effected only in the focused state . the operation prior to the moving object tracing af operation ( i . e ., moving object predicting af mode ) is as follows ( fig2 and 3 ). the graphs of fig2 and 3 show the relationship between the position of an object image plane and the position of a plane equivalent to a film plane ( focal position ), with respect to the position ( reference position ) of the focusing lens 53 when the moving object approaches the camera . in fig2 and 3 , &# 34 ; i &# 34 ; designates the integration operation , &# 34 ; o &# 34 ; the calculation operation and &# 34 ; m &# 34 ; the movement of the lens ( lens driving operation ), respectively . when control enters the af operation after the photometering switch sws is turned on , the lens ( i . e ., the af motor 39 ) is driven in accordance with the displacement ( i . e ., number of drive pulses ) obtained by the first integration operation i and calculation c . in the illustrated embodiment , as a result of the first integration and calculation after the photometering switch sws is turned on , if the defocus amount ( i . e ., number of drive pulses ) is above a predetermined value , the integration operation and calculation are repeated during the movement ( drive ) of the lens . if the defocus amount becomes smaller than the predetermined value during the repeated integration and calculation , the subsequent integration operation and calculation are stopped , and the lens is moved in accordance with the number of drive pulses obtained by the latest integration operation and calculation . the integration operation and calculation will also be referred to as an object distance measuring operation hereinafter . upon completion of the first lens driving operation , the integration operation and calculation are again effected to check whether the object is in - focus . if the object is in - focus , the object may be considered still , with a slight possibility that the object is moving . to compensate for the slight possibility that the object is moving , the object distance measuring operation is effected after the lapse of a predetermined time and if necessary , the lens is driven . if the main routine is interrupted by the operation of the release switch swr during the predetermined time , release is effected . if there is no interruption , the object distance measuring operation and the lens driving operation are repeated while the photometering switch sws is on . if a focused state is not attained during a predetermined number of repeated object distance measuring operations and lens driving operations ( e . g ., three times ), the object is deemed to be a moving object , and control enters the moving object predicting af mode routine ( fig3 ). in an alternative embodiment , the object distance measuring operation and the lens driving operation are repeated , while the photometering switch sws is on , and if a focused state is not attained during the three consecutive object distance measuring operations and lens driving operations after the object is once focused , control enters the moving object predicting af mode routine ( fig3 ). the moving object predicting af mode routine will be discussed below . fig4 and 5 are graphs showing the operation in the moving object predicting af mode , by way of example . when a defocus amount dp ( i . e ., number of pulses ) is obtained by the calculation c in accordance with the integration operation i , which is performed when the object is a moving object , the lens is driven ( lens drive m ) in accordance with the defocus amount dp . upon completion of the lens drive m , the integration operation i 1 ( i1 ) is carried out again to calculate a defocus pulse number dp 1 ( dp1 ). thereafter , moving speed ( moving object following speed ) s of the object image plane is calculated by calculation c 1 ( c1 ) in accordance with time t 1 between an intermediate point of preceding integration operation i and an intermediate point of the present integration operation i 1 . thereafter , to make the object image plane coincident with the film plane within a short space of time , constant speed control m 1 ( multiplied speed lens driving operation ) is effected in time t 1 ( t1 ) at a speed several times ( e . g . two times that of ) the moving object following speed s . while integration operation i 2 is performed after a doubled lens driving operation m 1 ( m1 ) is completed , constant speed control ( lens driving operation ) m 2 is effected at a moving object following speed s 1 . the moving speed of the object image plane corresponds to the speed of the movement of the object image plane , formed by the taking lens 51 , in the optical axis direction . upon completion of the integration operation i 2 , the lens drive m 2 is finished , and calculation c 2 is performed . in the calculation c 2 , the moving object following speed s 2 , of the object image plane is calculated in accordance with the defocus pulse number dp 2 , the calculated moving pulse number mp 1 of the moving object , and the time t 2 between the integration operations i 1 and i 2 . consequently , the multiplied speed lens drive m 3 is performed at a speed two times the moving object following speed s 2 for the time t 2 in which the calculation c 2 has been effected . when multiplied lens drive m 3 is completed , integral i 3 commences . during the integration operations i 3 , multiplied lens drive m 4 is performed at a moving object following speed s 3 . the focusing lens 53 may move beyond the focal position due to the double speed lens drive . for example , in fig4 the excess displacement is represented by defocus pulse number dp 3 in the double speed lens drive m 3 . if the excess displacement ( defocus pulse number dp 3 ) is below a predetermined value ; it can be considered that the object is continuing to move . accordingly , multiplied speed lens drive m 5 is performed at a double speed of the moving object following speed s 3 after calculation c 3 is finished . conversely , the excess displacement ( defocus pulse number dp 3 ) may be larger than the predetermined value . there are several cases that may have caused this , for example , the moving speed of the object may have been decreased , the object may have stopped moving , or the direction of the movement of the object may have changed , etc . in these cases , a checking operation is performed without effecting the lens driving operation , for example , as shown in fig5 . in fig5 if the excess defocus pulse number dp 4 above the predetermined value is obtained by integration operation i 4 , no operation ( lens driving operation ) is effected for time t 4 which has been required for calculation c 4 . thereafter , upon commencement of subsequent integration operation i 5 , tracing ( following ) lens drive m 7 is effected at object following speed s 3 obtained in the preceding calculation c 4 . if defocus pulse number dp 5 within the predetermined value is obtained , by integration operation i 5 , the tracing af operation ( i . e ., normal multiplied speed lens driving operation ) is performed . if an object image cannot be brought within the focus range , even by the two checking operations in which a multiplied lens driving operation is not effected , and since it is considered that either the speed of the object has decelerated , the object has stopped moving , or the direction of the movement of the object has changed , control is returned from the moving object predicting af mode to the normal af mode , as shown in fig2 . as can be seen from the foregoing , the change in state ( i . e ., direction , speed , etc .) of the moving object can be detected by the two checking operations of the focus state . although the twice checking operations are repeated in the illustrated embodiment , the number is not limited to two and can be more than two . furthermore , it is possible to realize a modified construction in which a tracing lens driving operation is not effected in the checking operations . the moving object following speed s can be calculated as follows ( fig4 and 5 ). the first moving object following speed s 1 is obtained by the equation below , in accordance with the defocus pulse number dp 1 obtained by the first integration operation i 1 and the time t 1 between the intermediate point of the preceding integration operation i and the intermediate point of the present integration operation i 1 : ## equ1 ## wherein x 1 ( x1 ) is an output cycle ( ms ) of the pulses generated by the encoder 41 . the moving object following speed s 1 is substantially or approximately equal to the moving speed of the object image plane . the multiplied lens drive m 1 is carried out at a speed ( 2 · dp 1 / t 1 ), two times the moving object following speed s 1 thus obtained , during the time t 1 , corresponding to the integration operation time ( interval ) t 1 , so that the focusing lens 53 is moved to the vicinity of the focal position at high speed . thereafter , the tracing lens drive m 2 is effected at the moving object following speed s 1 during the integration operation i 2 to follow the movement of the moving object . during the trace of the movement of the moving object , moving object tracing speed sn is obtained as follows : first , a lens drive pulse number mp 1 corresponding to the displacement which is obtained on the assumption that the object continues moving at the moving object tracing speed s 2 in time t 2 between the intermediate point of the preceding integration operation i 1 and the intermediate point of the present integral i 2 is obtained by equation 3 below : thereafter , output cycle x 2 of the af pulse corresponding to the object tracing speed s 2 is first obtained in accordance with time t 2 between the intermediate point of the preceding integration operation i 1 and the intermediate point of the present integration operation i 2 , the pulse number mp 1 which is assumed to correspond to the displacement within the time t 2 , and the present defocus pulse number dp 2 . the object tracing speed s 2 is then obtained , as follows : ## equ2 ## the lens drive m 2 is effected at a speed twice that of the object following speed s 2 for time t 2 required for the calculation c 2 . after the lens drive m 2 at double speed is finished , the lens drive m 3 is effected at the moving object following speed s 2 for the time period of integration operation i 3 to follow the movement of the moving object . note that the defocus pulse number dp is represented by a scalar value in the calculations mentioned above , the sign (+ or -) depending on a front focus or rear focus . accordingly , in the case of an excess displacement , the pulse number mp 1 corresponding to the displacement within the time t 2 is subtracted by the present defocus pulse number dp 2 . for example , ## equ3 ## repeated calculations of the equations 6 , 7 , and 8 mentioned above and the lens driving operation and the integration operations in accordance with the calculation results make it possible to follow the movement of the object as shown in the drawings . in the illustrated embodiments , since the calculated moving pulse number mp n - 1 ( mpn - 1 ) of the object image and the calculated defocus pulse number dp n ( dpn ) are absolute numbers , ( mp n - 1 ± dp n ) in equation 7 is replaced by ( mp n - 1 + dp n and ( mp n - 1 - dp n ) or ( mpn - 1 - dpn ) in the case of a rear focus and a front focus , respectively . as can be understood from the above discussion , after the calculation is finished , the lens is driven at the speed two times the moving object following speed that is s 1 for the time required for the calculation . this is because the image plane must be moved by the displacement corresponding to the movement of the moving object after the lens driving operation has stopped and before the subsequent lens driving operation is completed . namely , the relationship defined by s n ×( lens stop period + lens driving period )=( lens driving speed × lens driving period ) can be obtained by an easier calculation . therefore , it is possible to drive the lens at a different object following speed , provided that the above relationship is satisfied . the operation when the release switch swr is turned on during the moving object predicting af mode operation is discussed below with reference to fig6 . generally speaking , since the mirror is moved up after the release switch is turned on in a single lens reflex camera , a certain amount of time is required before the film is actually exposed after the release switch is turned on . this is referred to as release time lag rtl . in the case of a moving object , since the object continues to move during the release time lag rtl ( i . e ., after the release switch swr is turned on and before the exposure commences ), it is preferable to continuously drive the lens to follow the movement of the object . to this end , in the illustrated embodiment , whether the release switch swr is turned on is checked at the completion of the necessary calculations . if the release switch swr is turned on , the lens drive m 3 is performed at a speed that is twice the moving object following speed s 3 for the calculation time t 3 plus the release time lag rtl , so that the focusing lens 53 is initially moved in the optical axis direction by an additional ( excess ) displacement corresponding to the release time lag rtl . upon completion of the double speed lens drive m 5 , the photometering calculation and the upward movement of the mirror are effected , so that the diaphragm is adjusted to a calculated value , and the shutter mechanism 25 is driven at the calculated shutter speed . the above - mentioned operations are operations in which the object approaches the camera . if the focusing lens is initially moved through the excess displacement , for an object moving away from the camera , as mentioned above , a &# 34 ; rear focus &# 34 ; occurs . since the depth of field decreases as the object distance decreases , a &# 34 ; front focus &# 34 ; is preferable to a rear focus . furthermore , in the case of where the object is moving away from the camera , the moving speed of the image plane gradually decreases , provided that the moving velocity of the object is constant . in view of these phenomena in the present invention , in case of the object is moving away from the camera , the lens is driven at the multiplied speed for a time equal to half the time as in case of the object approaching the camera . namely , in fig7 the lens driving operation is effected at a speed that is twice the object following speed s 3 for a time equal to half the calculation time t 4 plus the release time lag rtl , i . e ., the time defined by ( t 4 + rtl )/ 2 . the main operation of the present embodiment will be discussed below in more detail , with reference to fig8 through 15 . the operation is performed by the main cpu 35 in accordance with the program stored in the internal rom 35a thereof . data , such as constants or parameters necessary to conduct the calculations , are stored in the e 2 prom 43 . fig8 shows a main routine of the main operation of the main cpu 35 . when the main switch swm is turned on , control enters the main routine in fig8 . first , at step s101 , the system of the main cpu 3 , 5 including various ports and the memory , etc ., is initialized . thereafter , a power down operation is performed to reduce unnecessary electrical power consumption ( step s103 ). at step s105 , whether the photometering switch sws is turned on is checked ( step s105 ). the power down operation is retained and the checking operations are repeated until the photometering switch sws is turned on . if the photometering switch sws is turned on , a reference timer 35c ( fig1 ) starts , and the states of the switches , such as the af switch swaf are checked ( steps s107 , s109 ). thereafter , data communication with the lens cpu 61 is carried out to receive lens data , such as an open diaphragm value a maximum diaphragm value , a focal length , and a k value data , etc ., at step s111 . the photometer data is inputted to the main cpu 35 from the photometering ic 17 , so that the shutter speed and the diaphragm value are calculated , based on the photometer data and the film sensitivity , etc ., in accordance with a predetermined algorithm ( step s113 ). the calculated shutter speed and the diaphragm value thus obtained are indicated in the indicator unit 45 at step s115 . thereafter , the af operation is performed . every time the set time , of the reference timer 35c has expired during the repeating of the operations of steps s109 through s119 , the main routine is interrupted by the reference timer routine , which is shown in fig9 . in the reference timer routine shown in fig9 a loop time is counted and the states of the photometering switch sws , and the release switch swr are inputted ( steps s121 and s123 ). after the photometering switch has been checked , the release switch swr is checked after an operation for detecting terminal , which will be discussed hereinafter with reference to fig1 . if the release switch swr is turned off or if the release switch swr is turned on but a permission signal of the release is not issued , for example , if the object is not focused in the focus priority mode , control is returned to the step prior to the interruption by the reference timer routine ( steps s125 and s127 ). if the release switch swr is turned on and release is permitted , the release is performed . during the release operation , the mirror motor 31 is driven to move the mirror up and the diaphragm mechanism 27 is driven to adjust the diaphragm value to the calculated value obtained at step s113 ( steps s131 and s133 ). upon completion of the upward movement of the mirror , the exposure mechanism 25 is driven to effect the exposure at the shutter speed calculated at step s113 ( steps s135 , s137 ). when the exposure is finished , the mirror motor 31 is driven to move the mirror down and the film winding motor 33 is driven to wind the film by one frame ( step s139 ). thereafter , control is returned to step s107 . the following discussion will be directed to the af operation according to an embodiment of the present invention , with reference to fig1 through 13 . first , whether the focus mode is the af mode or the mf mode ( manual focus mode ) is checked ( step s201 ). if the mode is the mf mode , control jumps to step s211 . the af mode and the mf mode referred to above are the automatic focus adjusting mode , and the manual focus adjusting mode in which the focus is adjusted by a photographer , respectively . when control enters , the af operation routine in the af mode for the first time since an integration operation is not performed , it is not in an af lock state ( i . e ., af lock flag is &# 34 ; 0 &# 34 ;), the object is not in - focus ( i . e . an in - focus flag is &# 34 ; 0 &# 34 ;) and a reintegration flag is &# 34 ; 0 &# 34 ;, control jumps to step s211 ( steps s203 , s205 , s209 ). in the second operation or operation subsequent thereto , if the af lock flag is &# 34 ; 1 &# 34 ;, control jumps to the step for performing the af lock operation . if the af lock flag is &# 34 ; 0 &# 34 ;, and if the object is focused , i . e ., if a predetermined time has elapsed after the object is once focused , the af lock flag is set at &# 34 ; 1 &# 34 ;, and the reintegration operation is performed ( steps s203 , s205 and s207 ). if the object is not in - focus , but the operation is the second af operation or the operation subsequent thereto , since the reintegration flag is &# 34 ; 1 &# 34 ;, the reintegration operation is carried out ( steps s203 , s205 and s209 ). if the operation is the first af operation , or the focus mode is the manual focus mode , control proceeds to step s211 ( steps s201 , s203 , s205 , s209 ). whether or not the af operation is being performed is checked at step s211 , and whether or not the mf operation is being performed is checked at step s213 , respectively . if the operation is performed in the af mode ( first af operation ), control proceeds to step s231 , and if the operation is performed , not in the af mode but in the mf mode , the object distance measuring operation and focus state indication operation are effected ( steps s215 through s227 ). at step s215 , the integration and calculation operations are carried out . thereafter , whether the calculation results are effective is checked at step s217 . if the calculation results are effective , and if the object is in - focus , the in - focus state is indicated by lighting a focus indicating led ( not shown ) of the indicator unit 45 . in addition thereto , an electronic buzzer ( pvc ) 46 is sounded to alert the photographer of the in - focus state ( step s219 ). if the object is out - of - focus , an indication operation is not effected . if the object contrast is low and the operation is the first operation of the routine , control jumps to step s229 , and if the operation is not the first af operation at low object contrast , whether or not the object is in - focus is checked ( steps s221 and s223 ). if the object is in - focus , the release permission flag is set at &# 34 ; 1 &# 34 ; and control proceeds to step s229 ( steps s223 and s225 ). conversely , if the object is not in - focus , the secondary in - focus width ( focal range ) flag is cleared and the focus , release permission flag and the af lock flag are cleared . the indication of the indicator unit 45 and the operation of the buzzer 46 are stopped ( steps s223 and s227 ), and control proceeds to step s229 . if the calculation results are not effective , the secondary focal width is cleared , and the in - focus , release permission flag , and the af lock flag are cleared . thereafter , the indication of the indicator unit 45 and the operation of the buzzer 46 are stopped ( steps s217 and s227 ). thereafter , control proceeds to step s229 , in which the loop time is checked . if a predetermined loop time has not elapsed , control is returned to step s211 to repeat the operations mentioned above . if a predetermined loop time has elapsed , control is returned to step s109 of the main routine . if the operation is determined to be the af operation at step s211 , control proceeds to step s231 to enter the af operation routine . at step s231 , the integration and calculation operations are effected . thereafter , whether the calculation results are effective is checked at step s233 . if the calculation results are effective , control jumps to step s261 , in which the focus state is checked . conversely , if the calculation results are not effective , whether the mode is an auxiliary light emission mode is checked ( step s233 ). in the auxiliary light emission mode , infrared auxiliary light ( contrast pattern ) is emitted towards the object from an auxiliary light emitter ( not shown ) when the brightness of the object is smaller than a predetermined value . in the auxiliary light emission mode , since it is difficult to follow the movement of the moving object , a moving object predicting mode forbidding flag is set ( step s237 ). thereafter , the auxiliary light is emitted and the integration and calculation are effected . thereafter , the calculation results are checked ( steps s239 and s241 ). if the calculation results are effective , control proceeds to step s261 in which the focus state is checked . conversely , if the calculation results are not effective , control proceeds to step s243 . if the mode is not the auxiliary light emission mode , control jumps steps s237 through s241 and goes to step s243 . the steps following s243 involve a search integration operation . at step s243 , the af motor 39 is driven by the dc control , since effective calculation results were not obtained . thereafter , the search integration and calculation are effected to detect the focal point at step s245 . the calculation results are checked at step s247 . if the calculation results are not effective , the search integration and calculation are effected again , and if the calculation results are effective , control proceeds to step s373 to check the driving direction ( step s245 and s247 ). fig1 a and 11b show the sub - routine of the reintegration and focus check operation . reintegration is a second integration operation or an integration operation subsequent thereto . in the reintegration operation , the reintegration flag is set to &# 34 ; 1 &# 34 ;. the integration and the calculation for obtaining the defocus amount are effected ( steps s251 , s253 ). thereafter , based upon a determination in step s255 , if the calculation results of the defocus amount are not effective , control proceeds to an afng operation , and if the calculation results are effective , control proceeds to an in - focus check operation . in the in - focus state checking operation , whether the object is in focus is checked . if the object is in - focus , the focus indicating led of the indicator unit 45 is lit and the electronic buzzer ( pcv ) 46 is actuated ( step s261 ). conversely , if the object is out - of - focus , no operation is effected . thereafter , at step s263 , if the object is out - of - focus for the first time at a low object contrast , control is returned to step s251 , and the integration operations , etc ., are carried out . if the object is not out - of - focus at a low object contrast at step s263 , if it is in - focus at s265 , and if the mode is not a moving object predicting mode , af release permission flag is set at &# 34 ; 1 &# 34 ; ( steps s263 , s265 , s267 and s269 ). if the mode is not the af lock mode ( i . e ., if the af lock flag is not set in step 271 ), control proceeds to step s273 . namely , the af lock flag is set in the first operation after the object is in - focus , and if the af lock flag has already been set , the operation is the second operation or the operation subsequent thereto ( steps s271 , s273 ). control then proceeds to an af lock operation ( step s283 ). if the af lock flag is set at &# 34 ; 1 &# 34 ; at step s273 , control does not proceed for a predetermined period of time in which the operation may be interrupted by the release operation , provided that the object contrast is high and the moving object prediction forbidding flag is &# 34 ; 0 &# 34 ;. if no interruption occurs within the predetermined time , the af release permission flag is cleared to forbid the releasing , and the af lock flag is cleared to permit the af operation ( steps s275 , s277 , s279 and s281 ). thereafter , the af lock operation starts . when the loop time has elapsed , control is returned to step s109 in the main routine ( step s283 ). if the object contrast is not high , or the moving object prediction forbidding flag is set at 1 , control immediately proceeds to the af lock operation without waiting for a predetermined time ( i . e . operation interruption by the release operation ). the preceding is shown at steps s275 , s277 , s283 . in the af lock operation , once the object is focused , an af operation is not performed while the photometering switch sws is turned on . in the focus checking operation at step s265 , if the object is out - of - focus , the control skips to step s285 to check whether the mode is the moving object predicting mode . if the mode is not the moving object predicting mode , control proceeds to step s301 ( i . e ., moving object checking operation ), and if the mode is the moving object predicting mode , the control proceeds to step s321 . in the moving object checking operation where it is checked whether the object is the moving object ( fig2 and 3 ), the secondary focal width flag , the focus flag , the release permission flag and the af lock flag are cleared and the focus indicating led of the indicator unit 45 and the electronic buzzer ( pvc ) 46 are turned off ( step s301 ). thereafter , if the reintegration flag is cleared at step s303 , control jumps to the pulse number calculation operation and if the reintegration flag is set , control proceeds to step s305 in which the direction of the present movement of the lens is compared with the direction of the previous movement thereof ( step s305 ). if the directions of the movements are identical to each other , the moving object judging counter is decremented by one , provided that the object contrast is high and the moving object prediction forbidding flag is cleared ( steps s307 , s309 , s311 and s313 ). note that the initial value of the moving object judging counter is &# 34 ; 3 &# 34 ; in the illustrated embodiment . conversely , if the direction of the present movement of the lens is not identical to the direction of the previous movement thereof at step s305 , the object contrast is not high , or the moving object prediction forbidding flag is set at &# 34 ; 1 &# 34 ;, control jumps to a pulse number calculation operation , without performing the counting operation ( steps s307 , s309 and s311 ). after the moving object judging counter is decremented by one , it is checked if the counted value is 0 . if so , the moving mode predicting mode flag is set and the moving object judging counter is reset ( steps s315 , s317 and s319 ). thereafter , the pulse number calculation operation is performed . if the counted value is not 0 , control proceeds directly to the pulse number calculation operation ( step s315 ). if the mode is the moving object predicting mode at step s285 , the focus flag , the release permission flag and the af lock flag are cleared , and the focus indicating led of the indicator unit 45 and the electronic buzzer 46 are turned off ( step s321 ). thereafter , the defocus pulse number is calculated in accordance with the result of the latest integration operation at step s253 . the defocus pulse number thus obtained is a value for the object at an intermediate point of the integration operation time . thereafter , the speed ( following speed ) of the movement of the object is calculated in accordance with the calculated pulse number for the movement of the object , the present defocus pulse number , and the integration operation time between the intermediate points of the integration operations . upon completion of the calculation , the object following flag , which is indicative of the object being traced , is set at 1 ( steps s325 and s327 ). thereafter , the defocus pulse number is set in counter 35d , so that the operation for controlling the af motor speed constant is commenced ( steps s329 and s331 ). if the mode is the moving object predicting mode within the focusing range at step s267 , control proceeds to step s323 . the following discussion will be directed to the operation which is effected when the result of the af calculation operation is void ( afng operation ), with reference to the flow chart shown in fig1 d . the afng operation is also performed as a part of &# 34 ; terminal operation &# 34 ;, which performed when the focusing lens reaches the telephoto or wide extremity . when the result of the af calculation operation is void the , in - focus indication led 46 is effected to emit light in a blinking manner to inform the photographer that it is impossible to focus ( s341 ). then , the reintegration flag is set . the ae calculation operation is performed if the loop time has elapsed after the loop time is checked . the control returns to the reintegration operation if the loop time has not elapsed ( s342 , s343 ). the following discussion will be directed to the calculation of pulse number and backlash drive , with reference to fig1 a and 12b . the pulse calculation calculates the number of pulses corresponding to the defocus amount and the number of pulses necessary to eliminate backlash . the backlash drive referred to is indicative of the driving of internal gears of the af motor 39 , the joints 47 and 57 , and the lens driving mechanism 55 to eliminate backlash , for example , when the direction of the driving operation of the af motor 39 changes . in the illustrated embodiment , the backlash driving operation is separately carried out prior to the driving operation based on the defocus amount . in the pulse calculation , first , the defocus pulse number is calculated . if the direction of the driving operation is different from that of the previous driving operation , the backlash pulse quantity is calculated , and the backlash drive flag is set at 1 ( steps s351 and s353 ). the backlash pulse quantity referred to is indicative of the pulse number and direction necessary to remove the backlash . the backlash value of the camera body 11 is stored in the e 2 prom 43 , and the backlash value of the taking lens 51 is stored in the rom of the lens cpu 61 and can be stored in the ram 35b of the main cpu 35 through the peripheral control circuit 23 by the data communication . if the backlash drive flag is not set , the defocus pulse number is set as the af pulse number in the counter and if the backlash drive flag is set , the backlash pulse number is set as the af pulse number in the counter , respectively . thereafter , the dc drive of the af motor 39 is commenced ( steps s355 and s357 ). if the backlash drive flag is cleared , and if the mode is not the moving object predicting mode ( i . e . the moving object predicting mode flag is cleared ), the value of the counter is compared with a predetermined pulse number ( steps s363 and s365 ). if the counted value is above the predetermined pulse number , the moving object prediction mode is cleared ( s367 ) and an overlap integration operation is commenced to calculate the defocus amount ( steps s367 and s369 ). the overlap integration operation referred to is indicative of an integration operation being executed during the lens driving operation . after the defocus amount is calculated , whether the defocus amount is effective is checked at step s371 . if the defocus amount is ineffective , control is returned to step s363 and if the defocus amount is effective , control proceeds to a direction of movement check operation ( steps s373 ˜ s377 ). in the direction checking operation , whether the focal position is before or after the object image position and within a predetermined range ( allowance ) is checked in accordance with the defocus amount ( steps s373 , and s375 ). if the focal position is before the object image position and out of the predetermined range of the defocus pulse number is calculated in accordance with the defocus amount calculated at step s369 , and then , the calculated number is set in the counter ( steps s375 and s377 ). thereafter , control is returned to step s363 . if the focal position is beyond the object image position , or within the predetermined range , the af motor 39 is braked to stop the driving operation of the taking lens . thereafter , control is returned to the reintegration operation ( steps s375 and s379 ). the braking of the af motor 39 is indicative of a short circuit of the input terminals of the af motor 39 in the illustrated embodiment . if the backlash driving operation is necessary , the mode is the object moving predicting mode , or the counted value is smaller than the predetermined pulse number , the counted value of the af pulse counter is compared with the predetermined pulse number . control does not proceed until the af counter value is smaller than the predetermined pulse number ( steps s359 ˜ s365 , s381 and s383 ). if the af pulse counter value is smaller than the predetermined pulse number , the af motor 39 is braked when the mode is not the backlash drive mode . thereafter , a constant speed control operation commences ( steps s385 and s387 ). in the case of the backlash drive mode , the af pulse number is compared with the predetermined pulse number . if the af pulse number is smaller than the predetermined pulse number , the af motor 39 is braked , so that control proceeds to the constant speed control ( steps s389 , s391 , s387 ). the backlash driving operation is performed by the constant speed control . if the af pulse number is larger than the predetermined pulse number , control does not proceed until the dc drive , for eliminating backlash , is finished . upon completion of the dc drive , the af motor 39 is braked , so that the backlash drive flag is cleared to finish the backlash driving operation ( steps s391 , s393 , s395 and s397 ). thereafter , control is returned to step s355 . in the case that the predetermined pulse numbers in s365 , s383 and s391 are p 1 , p 2 , and p 3 , the following relationship is satisfied : p 1 & gt ; p 2 = p 3 . the defocus pulse number is set in the af pulse counter , so that the lens driving operation for the normal af operation is performed . thus , the backlash driving operation is carried out prior to the defocus driving operation . furthermore , if the backlash pulse number is larger than a predetermined value , the backlash driving operation is performed by the dc drive within an extremely short space of time , and if the backlash pulse number is smaller than a predetermined value , the backlash driving operation is performed by the constant speed driving operation so as not to exceed the predetermined backlash . the following discussion will be directed to constant speed control , with reference to fig1 a and 13b . constant speed control involves the control of the af motor 39 at a constant speed . in the illustrated embodiment , the main cpu 35 controls the af motor 39 so as to rotate the same at a predetermined constant speed in accordance with the pulse interval output from the encoder 41 . in a preferred embodiment , the af motor 39 is rotated at a constant speed equal to or twice the moving speed s of the object image . in the constant speed control operation , x n is set as the constant speed control time ( pulse width ) and the counter for the constant speed control is set ( step s401 ). thereafter , if the moving object is being traced , a double speed 2sn twice the constant speed sn is set ( steps s403 and s405 ). if the integration operation is effected , the constant speed sn is set to trace the moving object at the tracing speed , and control then proceeds to step s411 . if no integral is effected , control proceeds directly to step s411 ( steps s407 and s409 ). at step s411 , it is checked if the object is being traced and integration is underway . if the object is being traced and the integration is underway , control jumps to step s459 to check for the completion of integration . conversely , if neither the object is being traced nor the integration is underway , control proceeds to step s413 ( step s411 ). at step s413 , whether the constant speed control time has elapsed is checked . when the constant speed control time has elapsed , the counter for the constant speed control is reset , then the terminal point detecting timer is counted ( s414 , s415 ). if the constant speed control time has elapsed , control proceeds to step s415 where it is checked whether the focusing lens has come to a terminal point . thereafter , if the af motor is being driven , control returns to step s411 . if the af motor is not being driven , the drive af motor operation is carried out at step s419 and control is returned to step s401 . conversely , if constant speed control time has not elapsed , control proceeds to step s421 . at step s421 , whether the af pulses are outputted from the encoder 41 is checked . if af pulses are not outputted , control is returned to step s411 , and if af pulses are outputted , control proceeds to step s423 , respectively . at step s423 , whether the count of the pulses is completed when not in the moving object tracing mode , or the drive time for following the moving object has elapsed when in the moving object tracing mode is checked . if the count of the pulses is completed , or the drive time has elapsed , the braking operation is effected . if neither the count of the pulses is completed , nor the drive time has elapsed , control proceeds to step s425 ( steps s423 , s437 and s425 ). at step s425 , whether the focusing lens 53 reaches the terminal point is checked and the terminal point detecting timer is reset . thereafter , whether the counted value of the af pulse counter is below a certain the speed switching pulse number is checked . if the counted value is below the speed switching pulse number , the drive speed is switched to low speed , and then , the af motor 39 is braked . thereafter , control proceeds to step s433 ( steps s427 , s429 , s431 ). at step s433 , whether the af motor 39 is driven is checked . if the af motor 39 is driven , the af motor 39 is braked . thereafter , control is returned to step s401 . conversely , if the af motor 39 is not driven , control is directly returned to step s401 . if the count of the pulse number is finished or the drive time has elapsed at step s423 , the af motor 39 is braked at step s437 . thereafter , whether the af lock flag in the moving object predicting mode is set is checked . if the af lock flag is set , the af release permission flag is set . thereafter , control proceeds to the release operation ( steps s439 , s441 and s443 ). if the mode is not the moving object predicting mode , or the af lock flag is cleared , whether or not backlash drive is effected , that is , whether the drive at present is backlash drive is checked ( step s445 ). if backlash drive is effected , control proceeds to the backlash drive completion operation ( s397 ). if backlash drive is not effected , the reintegration flag is set and the loop time is checked . if the loop time has elapsed , control is returned to step s109 . if loop time has not elapsed , control proceeds to the reintegration operation ( steps s445 , s446 and s447 ). fig1 c shows a start integration operation in which ccd data is inputted , and an integration operation is performed by a defocus calculation ( s215 , s231 , and s253 ). in the reintegration operation , the initialization for integration and calculation is effected . thereafter , integration commences and the integration flag is set ( steps s451 , s453 and s455 ). if the moving object is traced , control jumps to step s401 ( i . e ., constant speed control operation ), and if the moving object is not being traced , whether or not integration is finished is checked ( steps s457 and s459 ). if integration is not completed , control proceeds to step s461 to check whether the integration time is longer than a predetermined time . if the integration time is longer than the predetermined time , the moving object predicting mode forbidding flag is set at step s463 , since the object brightness is considered to be small . conversely , if the integration time is shorter than the predetermined time , control proceeds to step s465 . if the moving object is not traced at s465 , control is returned to step s459 to wait for the completion of integration ( steps s459 ˜ s465 ). if the moving object is traced at s465 , control is returned to step s413 . when integration is completed ( step s459 ), and if the object is being traced ( step s467 ), the af motor 39 is braked . thereafter , the integration data is inputted from the object distance measuring sensor unit 21 to determine the defocus amount . after that , control is returned to the step that is subsequent to the step at which integration starts ( steps s467 , s469 , s471 and s473 ). if the object is not being traced at step s467 , step s469 is skipped and control goes to step s471 . the following discussion will be directed to the determination of defocus amount which is performed at step s473 , with reference to fig1 . first , the calculation and check of contrast are effected ( step s501 ). in the calculation of contrast , the sum of the differences of the integration data of the adjoining light receiving portions in the ccd object measuring sensor unit are calculated . after that , whether the contrast is high enough to calculate the phase difference is checked ( step s503 ). if the contrast is low , control is returned , and if the contrast is sufficiently high , the calculation of the phase difference is effected ( steps s503 and s505 ). at step s505 , the phase difference is calculated , for example , by a correlation method or the like . in step s507 , if the mode is a 10 bit select mode , control proceeds to step s551 ( 10 bit select operation ), and if the mode is not the 10 bit select mode , control proceeds to step s509 . when control first enters this routine , the mode is not the 10 bit select mode . accordindly , control proceeds to step s509 . the 10 bit select mode referred to is indicative of an operation in which , if a correlation ( identity ) of the integration data between a comparative portion and a reference portion of the ccd line sensor is not satisfactory , a plurality of 10 bit areas are successively selected from among the comparative portion and the reference portion of the ccd line sensor to obtain high correlative areas . at step s509 , whether the calculation results of the phase difference are effective is checked . if the calculation results of the phase difference are not effective , control is returned . conversely , if the calculation results are effective , the correlation is checked ( steps s509 and s511 ). if the correlation is good , a calculation of the defocus amount is carried out ( steps s511 and s530 ). if the first out - of - focus flag at a low contrast flag is set , and the defocus amount is smaller than a predetermined value , the defocus amount determined by the present calculation is compared with that determined by the previous calculation ( steps s533 , s535 , s537 ). if the present defocus amount is smaller than the previous defocus amount , the present defocus amount is set as an effective value , and the defocus ok flag is set ( steps s539 , s541 and s543 ). thereafter , control is returned . if the first out - of - focus flag at a low contrast flag is not set , the present defocus amount is effective , so that the defocus ok flag is set ( steps s533 , s541 and s543 ). thereafter , control is returned . even if the first out - of - focus at low contrast flag is set , if the defocus amount is larger than a predetermined value , the previous defocus amount is made effective , and then , the defocus ok flag is set ( steps s533 , s535 and s543 ). thereafter , control is returned . even if the first out - of - focus flag at a low contrast is set and the defocus amount is less than a predetermined value , if the previous defocus amount is smaller than the present defocus amount , the previous defocus amount is retained . thereafter , the defocus ok flag is set ( steps s533 , s535 , s537 , s539 and s543 ). thereafter , control is returned . as can be understood from the above discussion , if the object contrast is low , a smaller defocus amount is selected from those of the present and previous defocus amounts , a malfunction due to a possible measurement error , for example , an unsteady blinking of the indication of the in - focus state or a failure to operate the af motor 39 does not occur . if there is a poor correlation in the integration data at step s511 , the searching flag is checked at step s513 . since the flag is &# 34 ; 0 &# 34 ; when control first comes to this operation a continuation of the calculation for the phase difference is performed at step s515 . if the result of the calculation for the phase difference is effective , control goes back to step s511 , and if not effective , the searching flag is set . control then goes back to step s505 ( s517 and s519 ). after the searching flag has been set , control proceeds from step s513 to step s521 and , the phase deviation is compared with a reference value ( step s521 ). if the phase deviation is smaller than the reference value , the contrast is checked ( steps s521 and s523 ). if the contrast is low , control proceeds to step s530 . if the contrast is high , the 10 bit select mode flag and the moving object predicting mode forbidding flag are set to select the first 10 bits . thereafter , the number of checking operations is set ( the number is 4 in the illustrated embodiment ). thereafter , control is returned to step s505 ( steps s523 , s525 , s527 and s529 ). if the 10 bit select mode flag is set , control proceeds to step s551 ( 10 bit select operation ) from step s507 . in the 10 bit select operation , whether the effective defocus amount based on the selected 10 bits is obtained by one operation is checked . if so , and if the contrast is more than twice the previous contrast , the 10 bit select defocus ok flag is cleared to make the previous data null . thereafter , control proceeds to step s559 ( steps s551 , s553 , s555 and s557 ). if the 10 bit select defocus amount is not obtained at step s551 , control proceeds to step s559 directly . if the contrast is lower than the previous contrast , control proceeds to step s571 , since the presently selected 10 bit data is not used ( steps s551 and s555 ). if the present contrast is greater than the previous contrast , but less than twice the previous contrast , control proceeds to step s559 without clearing the 10 bit select defocus ok flag ( steps s551 ˜ s557 ). at step s559 , if the calculation result of the phase difference is effective , the defocus calculation is performed , provided that there is a good correlation ( steps s559 , s561 and s563 ). after the defocus calculation , the bit select defocus ok flag is checked ( step s565 ). if the 10 bit select defocus ok flag is set , the smaller of the present defocus amount and the previous defocus amount , i . e ., a smaller defocus amount is selected ( step s565 , s567 ). thereafter , the 10 bit select ok flag is set and control proceeds to step s571 ( s569 ). if the 10 bit select defocus ok flag has been cleared , control proceeds directly to step s569 and the flag is then set ( steps s565 , s569 ). thereafter , control proceeds to step s571 ( steps s565 , s567 , and s569 ). if the calculation result of the phase difference is not effective , or the correlation is bad , control proceeds to step s571 without calculating the defocus amount ( steps s559 and s561 ). at step s571 , the subsequent 10 bits are selected . thereafter , the counter that counts the number of 10 bit select checking operations is decremented by one . if the counter value is not 0 , control is returned to step s505 . the operations from step s551 to step s575 are repeated until the counter value is 0 ( steps s573 and s575 ). the initial value of the counter is set at &# 34 ; 4 &# 34 ; in the illustrated embodiment . if the counter value is 0 , control proceeds to step s533 ( i . e ., the operation that prevents the unsteady flicker at low contrast ), on the condition that the 10 bit select defocus ok flag is set . if no 10 bit select defocus ok flag is set , the 10 bit select mode flag is cleared ( steps s575 , s577 and s579 ). thereafter , control is returned . thus , the integration data can be selected from the bit group of the ccd sensors having good correlation by the operations of steps s505 , s507 , s551 ˜ s575 . although the bit number is 10 ( 10 bits ) in the illustrated embodiment , the number is not limited to 10 . the tracing speed of the moving object is calculated as follows , with respect to fig1 . first , time t n between the intermediate point of the previous integration and the intermediate point of the present integration is calculated ( step s601 ). the reason that the intermediate point of the integration is used as a reference point is that the integration time varies depending on the object brightness . if the object is not traced , that is , it is the first time control comes to this operation after the moving object tracing mode has been set , the speed s 1 of the movement of the object image from time t 1 and the defocus pulse number dp 1 is calculated in accordance with equations 1 and 2 . thereafter , t 1 is set at the object tracing time ( i . e ., constant speed control time , and control is returned ( step s605 and s606 ). if the object is being traced , that is , it is the first time control comes to this operation after the moving object tracing mode has been set , the number of pulses mp n - 1 in which the object image would move within time t n from time t n and speed s n - 1 in accordance with equation 3 is calculated ( step s607 ). the suffix &# 34 ; n - 1 &# 34 ; mentioned above refers to a variable of the previous integration , calculation or driving operation , whereas &# 34 ; n &# 34 ; stands for a current value . thereafter , the direction of the present movement of the focusing lens is compared with that of the previous movement thereof . if the directions are identical to each other , the over displacement flag ( i . e ., over displacement of the focusing lens beyond an intended position ) is cleared . thereafter , the pulse number mp n - 1 is added to the present defocus pulse number dpn . control then proceeds to step s617 ( i . e ., tracing speed correcting operation in fig1 c ) ( steps s609 , s611 , s613 and s615 ). if the directions of movement of the focusing lens are different from each other , control proceeds to step s637 , since it can be considered that the moving speed of the object image is decreased or the object image is stopped at an extreme position beyond the intended position , or that the direction of the movement thereof is changed ( steps s609 and s611 ). if an error occurs , i . e ., if it is impossible to detect the difference in the direction of the movement of the focusing lens , the moving object predicting mode flag is cleared and control proceeds to the reintegration operation ( steps s611 , s613 and s655 ). in the tracing speed correcting calculation 1 , the object tracing speed s n is obtained by the following formula ( step s617 ); ## equ4 ## thereafter , the object tracing time ( sum of the integration data input time and the calculation time ) c n is set at step s621 . if the object is in - focus ( step s623 ) and the release switch swr is turned on ( step s625 ), the af lock flag is set ( step s627 ). thereafter , the time lag correcting time ( i . e ., the object tracing time c n plus the time corresponding to the release time lag ) is calculated at step s629 . if the object moves away from the camera , the constant speed control time is set to be half the time lag correcting time ( step s633 ). if the object approaches the camera , the constant speed control time is set to be identical to the time lag correcting time ( step s635 ). if the object is out - of - focus , or if the release switch swr is not turned on , even if the object is in - focus ( steps s623 and s625 ), control proceeds to step s635 to continue the tracing operation , so that the constant speed control time is set to be identical to the object tracing time c n ( step s635 ). if the direction of the present movement of the focusing lens is different from that of the previous movement , whether ( mp n - 1 - dp n ) is positive or negative is checked at step s637 . if ( mp n - 1 - dp n )≧ 0 , the value of ( mp n - 1 - dp n ) is calculated at step s639 . thereafter , the correcting calculation of the tracing speed s n is effected based on the following equations and the state of the release switch swr is checked ( step s641 ). ## equ5 ## if the object is in - focus at step s643 , the over displacement flag representing the over displacement of the focusing lens is cleared ( step s645 ). if the object is out - of - focus at step s643 , or if ( mp n - 1 - dp n )& lt ; 0 at step s637 , whether the over displacement flag has been set is checked ( step s647 ). if the over displacement flag has not been set , it is set at step s649 . thereafter , the calculation time c n is set at step s651 . control then waits for the calculation time c n and proceeds with reintegration . if the over displacement flag has been set at step s647 , the moving object predicting mode flag is cleared at step s655 . fig1 shows the focus checking operation . in this operation , the focus range ( width ) is expanded to increase the permissibility range of the releasing operation when the object is traced . first , the predetermined focus range ( i . e . predetermined defocus amount ) is maintained if the mode is not the moving object predicting mode . if the mode is the moving object predicting mode , the focus range is expanded ( enlarged ). thereafter , whether the present defocus amount is smaller than a predetermined value is checked ( steps s701 , s703 and s705 ). if the present defocus amount is larger than a predetermined value ( which is larger than the focus width ), the first out - of - focus at low contrast flag is reset at step s719 . if the defocus amount is smaller than a predetermined value , and the object is in - focus ( within the focus width ), the in - focus flag is set . thereafter , the first out - of - focus at a low contrast flag is cleared . thereafter , the focus indicating led of the indicator unit 45 is illuminated , and the electronic buzzer ( pcv ) 46 is sounded ( steps s705 , s707 , s709 , s711 and s713 ). if the af operation is effected , a predetermined focus range ( width ) corresponding to the moving speed of the object image is set to check the moving object . conversely , if the af operation is not effected , control is directly returned ( steps s715 and s717 ). if the defocus amount is larger than a predetermined focus width of s707 and smaller than the predetermined value of step s705 , the operation to prevent the unsteady blinking at a low contrast is carried out . if the first out - of - focus flag at a low contrast has been set , or even if it has not been set , but the mode is the moving object predicting mode , the first out - of - focus at a low contrast flag is cleared and control is returned ( steps s721 , s723 and s719 ). if the first out - of - focus at low contrast flag has been cleared at step s271 , the mode is not the moving object predicting mode , and the mode is the auxiliary light emission mode , control is directly returned ( steps s721 , s723 and s725 ). if the mode is not the auxiliary light emission mode , and the 10 bit select mode flag is set , the first out - of - focus at low contrast flag is set ( steps s727 and s733 ). even if the mode is not the 10 bit select mode , if the integration operation time is longer than a predetermined time , control is directly returned ( steps s727 and s729 ). even if the integration operation time is shorter than a predetermined time , if the contrast is not low , the control is directly returned . if the contrast is low , the first out - of - focus at low contrast flag is set . thereafter , control is returned ( steps s729 , s731 and s733 ). if the contrast is high , control is directly returned ( step s731 ). as can be seen from the above discussion , when control enters this routine for the first time , if the object is out - of - focus , and the contrast is low , the first out - of - focus flag at a low contrast is set . as a result , even if the focus state is switched from the in - focus state to the out - of - focus state , the out - of - focus indication operation ( step s301 ) is not effected at the first out - of - focus state . accordingly , an unsteady blinking of the indication lamp does not occur . although the out - of - focus state is indicated when the two consecutive out - of - focus states occur in the illustrated embodiment , the number of the occurrence of the out - of - focus state is not limited to two , and can be , for example , three or more than three . the operations when the focusing lens group 53 reaches a closet extremity ( i . e ., shortest focal position ) and a farthest extremity ( i . e ., infinite focal position ) will be discussed below with reference to fig1 . in this operation , when the arrival of the focusing lens group 53 to the terminal points ( i . e ., two extremities ) or the impossibility of the drive of the focusing lens group 53 by some reason is detected , the af motor 39 is stopped . whether the af motor 39 is driven is checked . if the af motor is not driven , control proceeds to step s791 to perform a terminal point detecting timer resetting operation . if the pulse interruption flag is set ( i . e ., the encoder 41 outputs the pulses ) during the driving of the af motor 39 , a terminal point checking operation is carried out ( step s771 ). conversely , if the pulse interruption flag is not set ( i . e ., pulse is not issued ), control proceeds to step s755 ( i . e ., counting operation of the terminal point detecting timer ). in the terminal point , detecting timer counting operation , the af motor 39 is stopped when no pulse is outputted from the encoder 41 for a predetermined time during the driving of the af motor 39 , since it is assumed that the focusing lens group 53 is at one of the extremities of the focusing lens group 53 can not move . first , the pulse flag which represents the presence of the pulse at the terminal point pawdt is cleared , and the terminal point detecting timer count flag which indicates that the counting operation of the timer is being effected , is set . the counting operation of the timer is decreased ( step s755 , s757 and s759 ). if the counted number is 0 , it is detected that the focusing lens group has come to the terminal point and control goes to the terminal process operation . if the counted number is not 0 , control is returned ( step s801 ). the following discussion will be directed to the operation which is performed when the time of the terminal point detecting timer is up , with reference to the flow chart regarding terminal operation shown in fig1 d . in the terminal operation , the af motor is first braked to a stop ( step s345 ). then , when the result of the calculation is effective while the af motor is being driven , control goes to step s342 in the afng operation to set the reintegration operation . then , the ae calculation operation is performed if the loop time has expired . control goes back to the reintegration operation if the loop time has not expired ( steps s346 , s342 , s343 ). when the result of calculation is not effective in step s347 and the driving direction is reversed , control proceeds to the afng operation ( step 341 ) and the operations of steps s341 - s343 are performed ( s346 , s347 , s341 ). if the driving direction is determined not to be reversed in step s347 , control proceeds to step s348 to reverse the driving direction prior to going to a search reintegration operation . in the terminal point checking operation , the terminal point of the focusing lens group 53 is detected by the change of the pulses outputted from the encoder 41 . in this operation , the pulse interrupting flag is cleared ( step s771 ) of fig7 . thereafter , the counting operation of the terminal point detecting timer is checked ( step s775 ). if counting is not effected , or if the pulse flag pawdt is set during the counting operation , control proceeds to the terminal point detecting times resetting operation ( step s791 ). if the pulse flag pawdt is not set during the counting operation , the pulse flag pawdt is set . thereafter , if the constant speed pulse flag pawdt is set . thereafter , if the constant speed control is effected , control is returned . but , if constant speed control is not effected , control proceeds to step s757 ( steps s777 , s779 and s781 ). the timer resetting operation is effected to initialize the data regarding the detection of the terminal point . in this operation , the timer count flag and the pulse flag pawdt are cleared , and the terminal point detecting timer data is set ( steps s791 , s793 and s795 ). the second embodiment of the moving object predicting af operation will be discussed below with reference to fig1 and 19 . in the second embodiment , the constant speed control continues even during the calculation . namely , the lens driving speed corresponding to the moving speed of the object image is calculated , and the tracing speed is corrected by the integration while driving the focusing lens group at the constant speed identical to the calculated speed . the basic principle of the second embodiment is the same as that of the first embodiment , except that the constant speed control is effected during the necessary calculation in the second embodiment . to this end ( i . e ., constant speed control in parallel with the necessary calculation ), the cpu 36 is provided to control the motor driving ic 37 in the second embodiment . first , the dc lens drive m is effected in accordance with the defocus pulse dp when the mode is the moving object predicting mode . upon completion of the dc lens drive m , the integration operation i 1 is carried out . in the calculation c 1 , the speed , s 1 of the movement of the object image in the period of time t 1 between the intermediate point of the integration operation i and the intermediate point of the integration operation i 1 is calculated by equations 1 and 2 mentioned above , so that the lens driving time can be obtained by the following equation 9 : consequently , the lens drive m 1 is performed at a constant speed that is identical to the triple speed of the tracing speed s 1 for the drive time calculated by the equation 9 . as a result of the lens drive m 1 at the constant speed control , the focusing lens group 53 is moved to the vicinity of the focal position within a short space of time . the effect substantially similar to that obtained by the driving operation at the speed twice the moving speed s 1 of the object image for the time ( t 1 + i 1 / 2 + c 1 ) is also obtained by the lens driving operation at triple speed . upon the completion of the lens drive m 1 at the triple speed , the integration operation i 2 and the calculation c 2 are effected while performing the constant speed drive m 2 at the tracing speed s 1 . in the calculation c 2 , the pulse number mp 1 corresponding to the displacement of the object image on the assumption that the object image moves at the tracing speed s 1 for the time t 2 between the intermediate point of the previous integration operation i 1 and the intermediate point of the present integration operation i 2 is calculated based on equation 3 ( mp 1 = t 2 × s 1 ) mentioned above . thereafter , the moving speed s 2 of the object image for the time t 2 is obtained by the following equations , similar to equations 4 and 5 mentioned above : ## equ6 ## the lens drive m 3 at the constant tracing speed s 2 continues during the integration operation i 3 and the calculation c 3 . thereafter , similar to the foregoing , the tracing speed s n is obtained in accordance with the pulse number mp n - 1 ( mp n - 1 = t n × s n - z ), corresponding to the displacement of the object which would move at speed s n - 1 within the time t n . the lens drive m n + 1 continues at the constant tracing speed s n during the integration operation i n + 1 and the calculation c n + 1 . the tracing control as mentioned above ensures that the moving object is substantially always kept in - focus . if the release switch is turned on during the tracing operation , the constant speed control is effected at the tracing speed s n obtained in the previous calculation while the mirror is in an upward position . the focusing lens group stops before the shutter leading curtain moves ( fig1 ). thus , the object is substantially in - focus when the leading curtain starts to move ( i . e ., when the exposure commences ). fig2 ( 20a - 20c ) and 21 ( 21a - 21b ) show flow charts of the second tracing operation of the moving object . in this embodiment , the operations shown in fig8 - 14c and 17 mentioned above and 20b , 20c , 21a , 21b are performed by the main cpu 35 , whereas the operation for calculation of the moving object tracing speed 2 , shown in fig2 a , and the operation of starting integration , shown in fig2 , are performed by a sub cpu 36 at the same time as the main cpu 35 operation . in the second embodiment , the reintegration operation shown in fig1 c has been performed at step s253 in the reintegration operation shown in fig1 a before the moving object prediction mode flag is set . when the moving object prediction mode flag has been set , the reintegration operation shown in fig2 is performed . further , when the moving object prediction mode flag has been set , steps s326 and s325 are skipped to perform the defocus pulse calculation at the middle point of integration which is equivalent to step s323 , before the calculation for the moving object tracing speed at step s921 in the reintegration operation . first , time t n between the intermediate point of the previous integration operation and the intermediate point of the present integration operation is calculated ( step s801 ). thereafter , whether the object is being traced is checked at step s803 . if the object is not traced , that is , if the object has not yet been traced , since it is the first time for the control to come to this operation , after the control had entered the moving object tracing mode , the speed s 1 of the object image movement is calculated with the t 1 and dp 1 values ( step s805 ). thereafter , {( t 1 + i 1 / 2 + c )/ 2 } is set as the object tracing time ( i . e ., constant speed control time . if the object is traced and the calculation is the first calculation during tracing operation , that is , if the object has already been traced once , since it is the second time for the control to come to this this operation , the pulse number mp 1 corresponding to the displacement of the object image within the time t 2 is calculated with the t 2 and s values . after the second calculation , the pulse number mp n - 1 corresponding to the displacement of the object image within time t n is calculated with the t n and s n - 1 values ( steps s803 , s807 , s809 , s811 ). thereafter , the direction of the present movement of the focusing lens group 53 is compared with the direction of the previous movement at step s813 . if the directions are identical to each other , the over displacement flag is cleared and the calculated pulse number mp n - 1 is added to the present defocus pulse number dp n ( steps s813 , s815 , s818 and s819 ). thereafter , control proceeds to step s821 ( i . e ., tracing speed correcting calculation 2 ). conversely , if the directions of movement of the focusing lens group are different from each other ( as determined in step s813 ), it is assumed that the moving speed of the object has decreased , the object has stopped , or the direction of movement of the object image has changed , resulting in a displacement beyond the intended position . accordingly , control proceeds to step s833 . if the direction cannot be detected , for example , by an unexpected error , the moving object predicting mode flag is cleared . thereafter , control proceeds to the reintegration operation ( steps s815 , s817 and s849 ). in a tracing speed correcting calculation 2 , the object tracing speed s n is obtained by the following formula ( step s821 ): ## equ7 ## if the object is in - focus and the release switch swr is turned on , the af lock , flag and the af release permission flag are set . thereafter , control is returned ( steps s825 , s827 , s829 and s831 ). if the object is out - in - focus or the release switch swr is not turned on , control is directly returned ( steps s825 and s827 ). if the directions of the present movement of the focusing lens is different from that of the previous movement , whether ( mp n - 1 - dp n ) is positive or negative is checked . if ( mp n - 1 - dp n )≧ 0 , tracing speed sn is obtained by the following equations ( steps s815 , s833 , s835 and s837 ): ## equ8 ## if the object is in - focus at step s839 , the over displacement flag representing the over displacement of the focusing lens is cleared ( steps s839 , s841 ). if the object is out - of - focus at step s643 , or if ( mp n - 1 - dp n )& lt ; 0 at step s833 , whether or not the over displacement flag is set is checked ( step s843 ). if the over displacement flag has been set , the moving object predicting mode flag is cleared at step s849 , since the over displacement occurs for the second time . namely , if the over displacement ( excess displacement ) of the focusing lens group takes place , this may be caused by an error . this is because when the two over displacements occur , the moving object predicting mode flag is cleared . alternatively , it is possible to clear the moving object predicting mode flag by one over displacement or more than two over displacements . if an over displacement flag is not set at step s647 , it is set at step s845 , since the over displacement occurs for the first time . thereafter , integration data is input and the calculation time c n is set . control then waits for calculation time c n and proceeds to the an integration operation ( steps s843 , s845 and s847 ). the following discussion will be directed to another constant speed control , with reference to fig2 a and 21b . the pulse duration x n is set in step s851 . thereafter , if the moving object is being traced , the tracing speed s n ( 1 / x n ) is set ( steps s853 , s855 ). if the object is traced , and if the operation is the first operation after the tracing operation commences , the triple speed 3s n of the tracing speed s n is reset ( steps s857 , s859 ). but , if the operation is the second or subsequent operation , resetting of the tracing speed is not effected ( steps s853 , s855 , s857 ). if the calculation is completed ( i . e ., calculation completion flag = 1 ), data , such as af pulse , tracing speed s n , etc ., is input and set . thereafter , the calculation completion flag is cleared ( steps s861 , s863 and s865 ). thereafter , control returns to step s851 . if the calculation is not finished ( i . e ., calculation completion flag = 0 ), whether the constant speed control time has elapsed is checked at step s867 . if the constant speed control time has elapsed , the terminal point detecting counter begins counting . if the af motor 39 is driven , control is returned to step s861 ( steps s867 , s869 and s871 ). if the af motor 39 is not driven , the af motor 39 starts and control returns to step s851 ( steps s871 and s873 ). if the constant speed control time has not elapsed , whether the af pulses are outputted is checked ( steps s867 and s875 ). if there is no output of the af pulses , control is returned to step s861 , and if the pulses are outputted , control proceeds to step s877 . at step s877 , whether the upward movement of the mirror is completed is checked . if the upward movement of the mirror is completed , the af motor 39 is braked and stopped ( steps s877 and s878 ). conversely , if the upward movement of the mirror is not completed , whether the count of the af pulses is completed is checked ( step s879 ). if the count is finished , the af motor 39 is stopped . thereafter , the loop time is checked . if the loop time has elapsed , the af operation is effected . if the loop time has not elapsed , control proceeds to the reintegration operation ( steps s879 , s881 and s883 ). if the counting operation of the af pulses is not finished in step s8879 the checking operation of the terminal point and the setting of the terminal point detecting timer are effected ( step s885 ) thereafter , whether the value of the af pulse counter is below the speed switching pulse number is checked ( steps s879 , s885 , s887 ). if the value of the af pulse counter is below the speed switching pulse number , the speed control is switched to a low speed control and the af motor 39 is braked . thereafter , control proceeds to step s893 . conversely , if the value of the af pulse counter is not smaller than the speed switching pulse number , control directly proceeds to step s893 ( steps s887 , s889 and s891 ). at step s893 , whether the af motor 39 is driven is checked . if the af motor 39 is not driven , control is directly returned to step s851 . conversely , if the af motor 39 is driven , the af motor 39 is braked . thereafter , control is returned to step s851 ( step s895 ). in the subroutine of the reintegration operation , the reintegration operation commences after initialization , and the reintegration operation flag is set ( steps s901 , s903 and s905 ). the integration operation time is checked until the integration operation is completed ( steps s907 and s909 ). if the integration operation time is longer than a predetermined time , the object is too dark to be photographed . accordingly , the moving object predicting mode forbidding flag is set ( steps s909 and s911 ). if the integration operation is finished , the integral data is inputted to calculate the defocus amount ( steps s907 , s909 and s911 ). if the calculation result is effective and the mode is the moving object predicting mode , the object tracing speed is calculated . thereafter , the calculation completion flag is set . thereafter , control proceeds to step s925 . if the calculation result is not effective , control is returned to step s901 ( steps s919 , s921 and s923 ). at step s925 , whether or not the af release permission flag is set is checked . if the af release permission flag is not set , control is returned to step s901 , and if the af release permission flag is set , control proceeds to the release operation . as can be understood from the above discussion , since the focusing lens group 53 is driven by a constant speed control during the integration and calculation , as shown in fig1 and 19 , the moving object can be precisely kept in focus . according to the present invention , even if the object is once in - focus , if the object is out of focus in the af operation at a predetermined time later , it is assumed that the object is moving . accordingly , the movement of the object can be detected even when the object is accidentally in - focus , for example , in the case that the object approaching the camera is focused with the focusing lens group moving from a near focal position to a far focal position . although the object is judged to be a moving object when three consecutive out - of - focus states are detected in the af operation after the object is once in - focus , as in the illustrated embodiment , the number of out - of - focus states to be detected is not limited to three . furthermore , it is possible to judge the moving object when more than one discontinuous or consecutive out - of - focus state is detected in the af operation after the detection of one in - focus state . as can be seen from the above discussion , according to the present invention , when the focus judging means determines that the object is in - focus , the object distance measuring means and the lens driving means are actuated after the lapse of a predetermined time . thereafter , if the focus judging means determines that the object is out - of - focus more than one time , the object is considered to be a moving object . consequently , the moving object can be detected even if the object continues moving after it is once focused or the focusing lens is moved in the direction opposite to the direction of movement of the object , thereby bringing the object into focus . furthermore , according to the present invention , when the object moves , the focusing lens group is moved at a speed corresponding to the speed of movement of the object image . accordingly , the moving object can be precisely brought into in focus . furthermore , if the object is a moving object , the measurement of the defocus amount and the calculation of the speed of movement of the object image are repeatedly effected , and the lens driving means drives the focusing lens group at the latest tracing speed during the measurement or the calculation . consequently , the in - focus state can always be substantially maintained . according to the present invention , since the focusing lens group is driven at the same speed as the speed of movement of the object image until the exposure commences , the exposure can be effected in the in - focus state . in addition to the foregoing , according to the present invention , if the object contrast is low , the defocus amount for the object is temporarily stored and the object distance is again measured , so that the defocus amount obtained by the re - measurement is compared with the stored defocus amount . as a result , a smaller defocus amount is selected and little or no measurement error occurs . namely , there is little or no possibility that the moving object , which is in - focus , is determined to be out - of - focus , thus resulting in the elimination of unsteady blinking of the focus state indication light . furthermore , if there is a backlash , since the focusing lens groups is driven to compensate for the displacement corresponding to the backlash , independently of the driving operation based on the defocus amount the calculation for obtaining the sum of the displacement based on the backlash and the displacement based on the defocus amount is not necessary , thereby simplifying the calculation . according to the present invention , the lens driving speed for the defocus amount varies depending on the displacement of the focusing lens group . namely , if there is a large displacement , the driving speed is increased to shorten the drive time . if there is a small displacement , the driving speed is decreased to prevent the focusing lens group from moving beyond the intended position ( over displacement ). | 6 |
a high voltage battery charger in accordance with the present invention includes a plurality of series - connected or parallel - connected low - voltage output stages with current regulation , automatic current and voltage sharing , and reconfigurable output voltage and current . with reference to the drawings , fig3 shows a full - bridge ( buck - based ) high voltage smps battery charger 30 with multiple low - voltage output stage circuits 31 . a multi - winding high frequency transformer 32 , with a primary 33 and multiple secondaries 34 coupled to the primary , is used to supply the output stages . the output stages can be series - connected , as shown in fig3 or parallel - connected , as shown in fig4 to realize the desired output voltage and current level . although a single transformer with multiple secondaries is preferred , multiple transformers may be utilized , each with a single primary and one or more secondaries . the series - connected configuration of fig3 can be utilized to realize high voltage / low current output while the parallel - connected configuration of fig4 can be utilized to realize low voltage / high current output . for both configurations , ac input power from an ac source ( e . g ., ac power mains ) is supplied to input terminals 35 . the ac power is converted to a dc voltage on dc bus lines 36 by a rectifier 38 ( e . g ., a full bridge of diodes ) and a filter capacitor 39 to form a dc source , and the voltage on the dc bus lines 36 is inverted to an ac voltage and then applied to the primary 33 of the transformer 32 by a buck - based dc to ac converter ( inverter ) 41 . in a preferred embodiment , the inverter 41 is formed of controlled switching devices 42 ( e . g . mosfets ) arranged in a bridge configuration . the ac output of the inverter 41 is coupled to the primary 33 of the transformer 32 through a dc blocking capacitor 43 . each of the output stages 31 include a rectification circuit 44 , which may comprise , for example , full wave bridge rectifiers formed of diodes 45 , and a low - pass l - c filter , formed of an output filter inductor 47 and an output capacitor 48 . other types of rectifiers may also be used . the battery charger in accordance with the present invention can use lower voltage rated diodes in the rectification circuit than are required by conventional chargers . for example , for a 800v / 10a charger , two low voltage series - connected output stages 31 can be used , instead of a conventional high voltage single stage , to realize the desired high voltage output . if a snubber circuit is used , the voltage rating of the rectifier diodes 45 is only 600v instead of 1200v . since reverse recovery losses are lower for 600v diodes than for 1200v diodes , a charger that can use the lower voltage rating diodes is more efficient and will allow operation at a switching frequency higher than that of a conventional charger . the higher switching frequency permits smaller magnetic and capacitive components and thereby enables increased charger power density . in the present invention , the charger configurations of fig3 and 4 are controlled to ensure balancing of voltage on the output capacitors 48 of each output stage 31 in the series - connected configuration of fig3 and to ensure sharing and balancing of the current in each of the output inductors 47 in the parallel - connected configuration of fig4 . further , the charger in accordance with the invention may be controlled to implement both constant - voltage and constant - current charging methods . a preferred controller in accordance with the present invention meets such objectives by closing a current control loop around the charger . the feedback current signal may consist , for example , of the weighted average of the individual output currents of each output stage . an outer voltage loop can be then used to regulate the output voltage of the charger . for exemplification , fig5 shows a full - bridge high voltage smps charger 30 having two series - connected output stages 31 and current and voltage feedback control loops . the current feedback signal , io_sum , is composed of the sum , at 50 , of the two output inductor currents io 1 and io 2 obtained from current sensors 49 . the voltage feedback signal , vo , is the sum , at 51 , of the output voltages of each output stage , namely vo 1 and vo 2 , which is available at the output terminals 52 for charging a battery . the voltage feedback scaling factor , kv , is used at 53 to scale the nominal output voltage level across the output terminals 52 to the control signal level . the outer voltage loop is closed and a proportional - integral ( pi ) compensation network 55 can be used to regulate the output voltage to the desired level , namely vo_limit . this allows the charger to implement the constant - voltage method . the pi network 55 generates a current command for the inner current loop , io_ref . in order to implement the constant - current method , a current limiter circuit 57 is used , the output of which is the current command , io_ref , up to and capped by io_limit . if the current command , io_ref , is lower than io_limit the charger will be in constant - voltage mode . on the other hand , if the current command , io_ref , is higher than io_limit the charger will be in constant - current mode . the current limiter 57 output signal is provided to a summing junction 62 which subtracts the signal io_sum from the current limiter output signal to provide a signal io_err . io_err is provided as the input to another pi compensation network 60 that is used as part of the current loop to regulate the charger current to the desired level . a pwm controller and gate drive 65 , e . g ., the unitrode uc3525pwm control ic , can be used to generate the required pwm control and gate drive levels to drive the gate controlled power devices 42 of the inverter 41 at a relatively high switching frequency , e . g ., 50 khz , with the pwm controller controlling the duty cycle of the output voltage waveform of the type v p illustrated in fig2 . the frequency of the pwm modulated output voltage from the inverter 41 can be at a selected high frequency , typically above 1 khz and preferably around 50 khz , to allow use of a relatively small and less costly transformer 32 . it is desired that , although the controller regulates the average current of both output stages , leaving the individual currents unregulated , current balancing is ensured , i . e ., that the individual currents are well balanced . in addition , it is also desired that , although the controller regulates the total output voltage , the individual output voltages across each of the output capacitors 48 , vo 1 and vo 2 , are also balanced . these two conditions can be met in the present invention with the use of a buck - based converter topology , such as the forward , half - bridge , or the full - bridge , with average ( or total ) current and voltage loops closed around the charger . the current feedback signal is effectively composed of the average value of all output currents for the series - connected configuration and the sum for the parallel - connected configuration but the current feedback signal effectively represents the average of the output inductor currents since the sum of the currents is proportional to the average current . the voltage feedback signal is the effective charger output voltage across the output terminals 52 in either configuration . to demonstrate the automatic current and voltage balancing feature of the invention , the full - bridge high voltage charger of the type shown in fig3 and 5 having two series - connected output stages may be considered . the equivalent circuits for both output stages during the power delivery mode and the freewheeling mode are shown in fig6 and 7 , respectively . in response to a disturbance causing the current , e . g . io 1 , flowing in one of the output inductors , e . g . lo 1 , to increase , the current loop will act to accelerate the return to the balanced state . if this current disturbance occurs while the charger is in constant - current mode , the output current feedback level , which is the sum of both output current stages , will increase , causing the current loop to reduce the duty cycle of the converter . this will cause the effective secondary voltages to decrease and will further cause both io 1 and io 2 to decrease . however , since the increase in io 1 will cause a corresponding increase in vo 1 , the output current io 1 will decrease at a higher rate than io 2 will . the same effect will happen if the disturbance in the output current , io 1 occurs when the charger is in constant - voltage mode . in that case , the increase in io 1 will cause the output voltage feedback level to increase . this will prompt the voltage loop to decrease the charger duty cycle command , causing the effective secondary voltages to decrease . again , this will cause both io 1 and io 2 to decrease , with io 1 decreasing at a higher rate than io 2 decreases because vo 1 is greater than vo 2 . the result is automatic average voltage and average current balancing between respective inductor currents and capacitor voltages without the need for any active control of the individual currents or voltages . another advantage of the present invention is the ease of reconfiguration between series - connected and parallel - connected operation . fig8 illustrates a charger in accordance with the invention with two output stages 31 connected in parallel . other than reconfiguring the physical connection of the output capacitors 48 , the control loops do not need to be changed from the circuit of fig5 except for the voltage feedback scaling factor , kv , applied at 53 . the voltage feedback scaling factor kv for the series - connected configuration will be half of that factor for the parallel - connected configuration in a case having two secondary windings and two output stages 31 . in the battery charger 30 of the present invention , adjusting the voltage feedback scaling factor during reconfiguration can be carried out , for example , by switching between pre - defined resistor values , or alternatively , by adjusting a potentiometer . in this way , none of the command levels or the compensation networks in the controller need to change . it is seen that the circuit of fig8 utilizes the same controller as that of fig5 reconfigured by the scaling factor kv for parallel - connected operation . as an example of the series / parallel reconfiguration of the invention , if the 800v / 10 a two - stage series - connected charger is reconfigured by connecting the output stages 31 and the output capacitors 48 in parallel , a 400v / 20a charger is obtained . this reconfiguration flexibility allows one charger configuration to be used for both types of chargers , which simplifies the assembly process and minimizes changes between product lines . the invention can be further extended to encompass more than two series - connected or parallel - connected output capacitors 48 . for example , a 400v charger may be configured using three series - connected output stages with each output capacitor supplying 133 . 3v . this allows the use of schottky diodes as the diodes 45 having minimal or no reverse recovery . however , the benefit of reducing reverse recovery losses in the rectifier diodes 45 must be balanced with the addition of more output stages 31 . the battery charger in accordance with the present invention is also suitable for arrangement in alternative network combinations , such as , for example , in the parallel combination of two series - connected strings of output stages 31 with output capacitors 48 , wherein the respective ends of the two strings of stages 31 are connected in parallel . a corresponding adjustment to the voltage feedback scaling factor , kv , at the scaling block 53 , is all that is necessary to complete the reconfiguration for charging within a suitable voltage and current range for this arrangement . since the current feedback signal for both the series - connected and parallel - connected configuration is the sum of the individual output currents , a single hall - effect current sensor can be used for the current sensors 47 . to obtain the sum of the output currents , the individual output current paths ( wires ) from each stage are looped through the same sensor . fig9 shows a preferred arrangement for sensing the total current for a series - connected high voltage smps charger using a hall - effect sensor 70 . in this embodiment , there is no need for a summation circuit in the controller . note that the same current sum is used in the feedback loop of the parallel - connected configuration , which further simplifies configuring the charger for either series or parallel operation . an example of the implementation of the control loops is shown in fig1 . if a hall - effect current sensor 70 is used as in fig9 a current sense resistor , rsi , is used to generate a voltage feedback level at the output of an amplifier u 1 ( acting as the summer 50 ), corresponding to the sum of the output currents . the output voltage is fed back through a differential amplifier u 2 , providing the scaling function 53 , where the voltage feedback scaling factor , kv , is set by the ratio of resistors rsvf to rsvi . the voltage p 1 loop 55 is configured using an amplifier u 3 , as well as resistors rvi , rvf , and capacitor cvf . the limiter 57 is realized using a simple minimum detector using diodes d 1 and d 2 , and a resistor rd connected to vcc . finally , the current p 1 loop 60 is configured using an amplifier u 4 , as well as resistors rii , rif , and a capacitor cif . the foregoing circuit implementation is for purposes of illustration , and it is understood that any suitable implementation may be utilized . for example , as an alternative , the controller can be a microprocessor or dsp that digitally process the signals using digital circuits alone or in combination with software . as noted above , the invention may be implemented using any suitable circuit topology , including various buck - based dc - to - ac converters and rectification circuits . for example only , various converter and rectification circuit topologies that may be used are illustrated in fig1 - 15 . in each of these views , a single output stage 31 is shown , it being understood that multiple similar output stages would be utilized in accordance with the invention . fig1 illustrates a full - bridge buck - based dc - to - ac converter 41 and an output stage 31 with a push - pull rectification circuit 44 having two diodes 75 and 76 and a center tapped transformer secondary 34 . fig1 illustrates a topology with a buck - based dc - to - ac converter 41 having two controlled switching devices 77 and 78 and two capacitors 80 and 81 , and a full - bridge rectification circuit 44 . fig1 illustrates a topology having a half - bridge buck - based dc - to - ac converter 41 as in fig1 , and a push - pull rectifier 44 as in fig1 . fig1 illustrates a forward buck - based dc - to - ac converter 41 having a single switch 85 , and a half - wave rectification circuit 44 having two diodes 86 and 87 . fig1 illustrates a forward buck - based topology with a dc - to - ac converter 41 having two switches 90 and 91 and two diodes 92 and 93 , and a half - wave rectification circuit 44 with two diodes 86 and 87 as in fig1 . it is understood that the invention is not confined to the particular embodiments set forth herein as illustrative , but embraces all such forms thereof as come within the scope of the following claims . | 7 |
referring now more specifically to the drawings , and to fig1 a and 1b in particular , numeral 10 designates generally the improved sawmill assembly , shown here in a fully operational mode . the sequence of operation can most easily be explained with reference to these figures , 1a and 1b , and processing of the logs occurs from left to right , as viewed in the drawings . this type of sawmill assembly is sometimes termed a &# 34 ; breakdown machine &# 34 ; in that its main function is to slice the outer rounded slabs off of the sides of the log , leaving a square or rectangular central cant . the log is thus &# 34 ; broken down &# 34 ;, the cant being further processed into lumber by a gang saw or other device . the slabs cut from the outer perimeter may be either ground into sawdust or processed through a &# 34 ; chipper &# 34 ; to make mulch . thus , the present assembly includes a rigid framework 12 which is substantially open , elongated , and rectangular in shape . the framework includes a pair of spaced , longitudinally extending &# 34 ; i &# 34 ; beams 14 , which are connected by a plurality of transverse &# 34 ; i &# 34 ; beams 16 to provide a base for the assembly . a plurality of generally vertical support members 18 are secured either to the longitudinal beams or the transverse beams and in general , support a raised , log conveying central track . the log conveying track is charcterized also by a pair of spaced , longitudinally extending upper &# 34 ; i &# 34 ; beams 20 , which are also generally parallel to one another . upper transverse support members 22 are connected to beams 20 where necessary to support additional platforms or work stations , such as members 22 in fig1 b . the functions and what particular stations are supported by these support members 22 will be described more fully hereinafter . at the extreme left hand side , as viewed in fig1 a , is a station for feeding logs from a laterally extending conveyor , ( not shown ) to a gate means 24 , which includes a plurality of pivotally mounted gate members 26 . the operator utilizes the gate means to feed , one at a time , logs l to the conveying track of the present sawmill assembly . extending the length of the present assembly , substantially in the center thereof , is a variable speed conveyor means 28 which includes endless flexible elements such as chains 30 . these central chains are disposed on sprockets 32 which are in turn mounted on shafts 34 for rotation in suitable pillow block bearings 36 or the like . the conveyor means includes a suitable tensioning mechanism such as that designated by numeral 38 in fig1 b , which is used to adjust and maintain the proper tension on the chains . in general , the logs are conveyed by the chain drive through the present sawmill assembly , the chain being routed , on the return run , along or near the bottom of the main frame 12 with additional chain tensioning mechanisms 38 being provided as required , based on the length of the run . an auxiliary conveying means , designated generally by numeral 40 is provided on the downstream side of the second set of saw blades . this conveying means includes a set of chains 42 , mounted on sprockets 44 which are suitably mounted forrotation . the chains 42 convey the finished central cant through a splitter 46 , a gang saw ( not shown ) or to another suitable finishing step . the auxiliary conveyor will be explained in greater detail hereinbelow . as shown in fig1 a and 1b , the invention includes a double set of linearly spaced cutting stations to break down the logs into square or rectangular central cants . in both cutting stations , the saw blades 60 are movable laterally in and out to pare off only the least necessary amount of wood , thereby maximizing the yield from each log . guide means , such as plates 61 are provided on each side of the track , downstream from the saw blades , to ensure the axial alignment of the log being cut . the blade carriage assemblies 62 are mounted on transverse rods 64 with ball bushings ( not shown ) and the lateral movements are controlled hydraulically through lines 66 and automatic control valves ( not shown ), disposed beneath the carriage and connected to a suitable hydraulic pump and reservoir ( not shown ). as the logs are moved through the saws , the slabs cut from the sides of the logs are directed to spaced , parallel , continuous conveyors 68 which transport the slabs to a suitable trough or bin where they may be collected for further processing . as can be seen in fig1 a and 1b , each blade carriage assembly has two motors 70 which are electrically operated and run sheaves 72 which are in turn connected through couplings ( not shown ) to the blades . the slab conveyors 68 are hydraulically operated , with motors 74 connected to the conveyors and to hyraulic lines 76 , the lines 76 being supplied from the same reservoir and pump as is used for jogging the blade carriages . referring still to fig1 a and 1b , it is seen that as many as five logs may be processed simultaneously , with the processing occurring essentially continuously , that is , as soon as a log has passed through the first set of saw blades , another can be loaded from the gate means 24 to the main conveying track . the chains 30 of the conveyor are provided with radially extending abutment means or lugs 78 , shown in fig2 a through 2d . the lugs are movable from one link to another on the chain and the processing operation is set up on a timed schedule to facilitate the continuous flow desired , by mounting the lugs a certain defined distance apart depending on conditions such as the length and type of log being processed . as a log is released to the conveyor from gate means 24 , the operator adjusts the spacing of the blades , and a lug pushes the log through the first cutting station . this station has , in addition to blades 60 , a toothed pressure roller 80 which holds the log down with a hydraulic piston and cylinder 81 and helps to ensure a smooth cut . a guard 101 is provided as a shield against wood chips dislodged during the cutting operation . as the log passes through the first set of saws , slabs are trimmed from each side and deposited on conveyors 68 which transport the slabs away from the operations area . the log is propelled forwardly by the lug 78 in the chain 30 and by rollers 82 to an inclined and inwardly sloping ramp 84 . the log rides up the ramp and as it rolls off on the uncut , rounded side , is caused to rotate ninety degrees to rest on one of the now flattened sides . the log is then further propelled by rollers 82 to the position shown in fig2 a . at this point , the log is engaged by an upper log engaging and propelling means , such as overhead roller 88 . roller 88 is mounted on an arm 90 which is pivotally attached to upright 18 . the roller is driven by a hydraulic motor 92 which drives rotor 94 . the rotor in turn drives roller 88 through a chain 96 or similar arrangement . the elevation of arm 90 is in part controlled by the height of the log , and in part by a hydraulic cylinder 98 , both the cylinder and motor 92 being supplied with hydraulic fluid through lines 100 . roller 88 has radially extending projections such as spikes 102 which engage the log and propel it forward to the position shown in fig2 b . as shown , the front end of the log is pushed under a smooth surfaced pressure roller 104 . this roller 104 is mounted on arm 106 which is pivotally attached to a croww beam 108 , extending between uprights 18 . pressure on the arm and roller 104 is maintained by a hydraulic cylinder 110 , cylinders 110 and 98 being mounted on transverse frame members 120 . as roller 104 is lifted by the end of the log , the arm 106 trips a limit switch 122 which activates cylinder 98 to raise the arm 90 and its spiked roller 88 . here , fig2 b and 3a show the same positioning of the equipment . with the log now esting on platform 86 , a dual set of centering arms 124 are activated through hydraulic cylinders 126 as shown in fig2 c and 3b . the centering arms are connected at their base by rotatably mounted and meshed gears 128 which move the opposed arms simultaneously to center the log . the log at this point is still being held by roller 104 at its lead end , thus contact with the log is being made at five points , the roller and the four arms , making the centering operation both quick and precise . having cnetered the log , the arms 124 are returned to their open position by cylinders 126 , shown in fig3 c . during this time , the operator can also set the spacing of the second set of saw blades by jogging the blade carriage . as the centering operation proceeds , and proceeding in sequence from fig2 a through 2d , lug 78 on chain 30 can be seen advanced toward the log , having been timed and set in a desired position , depending on the approximate length of the logs being cut . the lug reaches the centered log in virtual sequence with the retraction of the centering arms . the log is then propelled through the second set of saw blades , as shown in fig2 d , pressure being maintained on the log by roller 104 . this provides a squared or rectangular central cant , suitable for processing into lumber . as with the first set of saw blades , a guard 101 is provided , mounted to frame member 108 , to deflect chips dislodged during the sawing operation . the remaining two slabs cut from the sides of the log are deflected and conveyed by the side conveyor belts 68 to a waiting trough or bin beneath the frame . returning to fig1 a and 1b , the squared or rectangular central cant is conveyed on chain 30 either directly off of the sawmill assembly or to an auxiliary splitter or gang saw . the operator controls this further procesing depending on the sizes desired . an elongated bar means 140 is provided downstream from the second set of saw blades . the bar is slidably mounted and laterally movable on rods 142 which are supported by struts 144 connected to beam 20 . hydraulic actuator 146 controls the lateral movement of the bar , which is selectively operated to move the cant to conveyor 40 . the present assembly thus provides essentially continuous processing of logs . the operation can be run by a single operator and the various advantages over sawmills which can only process a single log at a time are believed to be evident . the use and operation of the present tandem sawmill assembly have been fully described in conjunction with the description of the structural features . the invention is capable of processing eight to ten foot logs at a rate of approximately nine per minute , depending partly on the length of the logs being cut , thus providing a significant advantage over the prior art . while an embodiment of a tandem sawmill assembly has been shown and described in detail herein , various changes and modifications may be made without departing from the scope of the present invention . | 8 |
certain optical discs , such as dvds , consist of two plastic halves (“ substrates ”), which are metallized and bound together with an interstitial bonding layer . it would be desirable to use an interstitial layer between the two substrates to interfere with the reading laser in order to inhibit reading of the disc . this would result in a disc that is more difficult to defeat , as the two halves of the optical disc would protect the interfering layer . using an interstitial layer as the interfering layer still allows triggering the process of disc expiration . for example , polycarbonate , which is typically used to manufacture dvd substrates , allows the propagation of oxygen that could reach the interstitial reactive layer and trigger a reaction that causes the expiration of the disc . furthermore , it would be desirable to use the bonding layer itself as the interfering layer , for example by changing the chemical composition of the bonding layer through the incorporation of a reactive substance . this could simplify the manufacturing of limited - play optical discs because no additional layers would be introduced , and attempting to defeat the limited - play mechanism by removing this layer could destroy the optical disc itself , as the bonding layer is critical to the integrity of the optical disc . however , in certain types of optical discs , such as a dvd - 5 , the bonding layer is not in the optical path . fig2 illustrates a cross sectional view of the layers typical of a dvd - 5 construct . thus while the bonding layer could play part in an expiration process for a dvd - 5 that does not rely on direct interference with the reading laser ( e . g ., by corroding the reflective metal layer that is in contact with the bonding layer ), it would not be possible to make this type of disc expire by transitioning the bonding layer to a state that prevents the reading laser from reading the data on the disc . since it is often desirable to make the disc unplayable by means of a process that interferes with the reading laser , it is desirable to have a disc similar to a dvd - 5 where the interstitial bonding layer is in the optical path . in limited use optical discs where the expiration process relies on interference with the reading laser , the data encoding structures ( such as metallized pits on a polycarbonate substrate ) typically are preserved in an expired disc , although the reading laser is prevented from reading the encoded information . as long as these data structures are present , there is always the possibility of the disc being defeated by enabling the reading laser to access the information . it would thus be desirable to have additional mechanisms that prevent recovery of the data , such as permanently erasing the data by compromising the integrity of the data structures on the optical disc . these , and other , goals and embodiments of the invention will be better appreciated and understood when considered in conjunction with the following description and the accompanying drawings . it should be understood , however , that the following description , while indicating preferred embodiments of the invention and numerous specific details thereof , is given by way of illustration and not of limitation . many changes and modifications may be made within the scope of the invention without departing from the spirit thereof , and the invention includes all such modifications . a clear conception of the advantages and features constituting the present invention , and of the components and operation of model systems provided with the invention , will become more readily apparent by referring to the exemplary , and therefore non - limiting , embodiments illustrated in the drawings accompanying and forming a part of this specification . it should be noted that the features illustrated in the drawings are not necessarily drawn to scale . we now describe the different aspects of the current invention , and several corresponding embodiments and examples . dvds are the most common optical discs used for distribution of movies . dvds are made from two bonded plastic substrates , typically referred to as l 0 for the bottom substrate and l 1 for the top substrate , where “ top ” and “ bottom ” refer to a dvd in a playing position where it is read from the bottom , as is the common convention . these substrates are molded from materials such as polycarbonate , acrylic , or polyolefine , which is injected in a molten form to a mold and pressed against a stamper . the process of creating the physical stampers used in replicating the dvd substrates is referred to as mastering . the following procedure is used , which is illustrated in fig1 : 1 . float glass blank 5 is polished and coated with a primer 10 to enhance adhesion with the photo resist layer 15 . 2 . photo resist coating 15 is applied , baked , and then exposed to the laser for recording . the formatted data signal is used to modulate the cutting laser of a laser beam recorder ( lbr ) machine which creates pits 20 in the glass disc . 3 . the exposed glass is then developed leaving pits 20 and lands 25 across the surface . 4 . this “ glass master ” then has a thin ( 110 nm ) metal layer sputter - applied to make the surface conductive for electroplating . 5 . the glass master is then placed into an electroplating solution where nickel is formed to the desired thickness . ( typically 0 . 300 mm ). 6 . this “ metal father ” ( or “ father stamper 30 ”) is then separated from the glass master 35 and cleaned . at this step , the metal father 30 could be used for the molding process , but if the part gets destroyed or damaged in replication , the entire process must be repeated . 7 . therefore , most manufacturers will grow “ metal mothers ” ( or “ mother stampers 40 ”), which are negatives of the father 30 . typically , four mother stampers 40 can be grown from one father 30 without quality degradation , and from each mother 40 , up to 8 stampers (“ sons 45 ”) can be grown . 8 . stampers get sent to replication facilities and mothers 40 are stored for reorders or replacement parts . in the case of a dvd - 5 , which is a single layer disc illustrated in fig2 , the l 0 substrate 100 is covered with a thin reflective layer 105 of aluminum by a sputtering process . this creates a metallic coating between 60 and 100 angstroms thick ( the l 0 layer ). the l 0 substrate 100 is then bonded 110 to a blank l 1 substrate 110 , as illustrated in fig3 . for a dvd - 9 , which is a two - layer disc , the l 0 layer is formed as a very thin , semi - reflective metal layer , and is typically made of gold . a fully reflective aluminum layer is formed on the l 1 substrate ( the l 1 layer ). the two substrates are subsequently bonded with appropriate adhesive material , which forms a transparent bonding layer , to form the dvd - 9 disc . as seen in the dvd family illustration in fig4 , a dvd disc may contain either one or two information layers for each substrate , resulting to different types of disc capacities , such as dvd - 5 200 ( single sided , single layer , 4 . 7 gbyte capacity ), dvd - 9 205 ( single sided , dual layer , 8 . 5 gbyte capacity ), dvd - 10 210 ( double sided , single layer , 9 . 4 gbyte capacity ), dvd - 14 ( double sided , one side single layer , one side dual layer , 13 . 2 gbyte capacity ), and dvd - 18 215 ( double sided , dual layer , 17 gbyte capacity ). a dual layer disc such as a dvd - 9 205 must conform to the “ dvd specifications for read - only disc , part 1 physical specifications version 1 . 0 ”, which require the following : 1 . total disc thickness , including bonding layer 110 , spacer ( s ) and label ( s ), shall be 1 . 20 mm + 0 . 30 mm /− 0 . 06 mm 2 . index of refraction ( ri ) of the transparent substrate shall be 1 . 55 +/− 0 . 10 the index of refraction of the spacer shall be ( ri of the substrate +/− 0 . 10 ) 3 . thickness of the transparent substrate is specified as a function of its index of refraction . typically with polycarbonate at ri = 1 . 56 , the thickness values for the disc substrate would be 0 . 57 mm ˜ 0 . 63 mm ( see fig5 a and 5b ) there is no specification for the dvd - 5 200 and dvd - 10 210 spacer layer ( bonding layer 110 ), as long as the total disc thickness conforms to the dvd specification and the half discs ( molded substrates ) conform to ri related specifications as above . the information in dvds is encoded in the pits 20 and lands 25 ( data areas that are not pits ) that are molded into the substrates and subsequently are metallized to form the corresponding data layer . the pits and the lands are organized in a spiral track , which , in the case of a dvd - 5 200 , is read in a clockwise direction beginning at the inside of the disc and proceeding towards the outside of the disc . the reference area of the disc that is not occupied by data is used for tracking of the reading laser . the reading laser , which has a wavelength of 630 - 650 nanometers in vacuum , is focused on the l 0 layer 100 of a dvd - 5 200 or dvd - 9 205 , or on the l 1 layer 115 of a dvd - 9 by penetrating through the semi - reflective l 0 layer 100 , and it is reflected back to a photo detector . during transitions from a pit 20 to a land 25 or vice versa , interference patterns develop , which are detected by the photo detector and result in changes in its electrical output . these changes in the electrical output of the photo detector allow the player to read the information recorded on the dvd . dual - layer discs , such as dvd - 9s 205 , typically utilize one of two methods for read - out of the disc information : a dual - layer parallel track path ( ptp ) disc 299 will have a lead - in 300 and a lead - out 305 area on both layers , as illustrated in fig6 . for each layer , the lead - in 300 area is located at the inner radius of the disc , and lead - out 305 area is located at the outer radius of the disc . this layout structure is comparable with the layout of the single layer 320 disc . reading of the data is done , as in a dvd - 5 , 200 from the inner radius of the disc to the outer radius , for both layers . with proper authoring of the content on the disc , the ptp method can allow quick access from layer to layer , for example in order to provide background information and commentary in one track along with the movie in the other track . a dual - layer opposite track path ( otp ) 325 disc , also illustrated in fig6 , offers the possibility of seamless continuation of the playback from the l 0 100 to the l 1 115 layer . the first information layer ( l 0 ) 100 starts with a lead - in area at the inner radius of the disc and ends with a so - called middle area 330 at the outer radius . the second information layer starts with a middle area 330 at the outer radius and ends with a lead - out 300 area at the inner radius of the disc . reading the data 335 stored on the disc will start at the inner radius of the first information layer and proceed until the middle area 330 of this layer is reached . then a switch over to the middle area in the second information layer is made , in order to continue reading of the data from the outer radius up to the lead - out 305 area in the inner radius of the second layer ( l 1 ) 115 . one embodiment of the present invention is an optical disc similar to a dvd - 5 where , unlike a standard dvd - 5 , the interstitial layer 400 typically used as the bonding layer 401 is in the optical path 405 of the reading laser ( e . g ., see fig7 ). in one embodiment of the present invention ( labeled below as “ special dvd - 5 design # 1 ”), this disc is manufactured by inverting the reflective layer 410 of a standard dvd - 5 , and reading the information through the non - information - bearing substrate 415 and the bonding layer 401 . in another embodiment of the present invention ( labeled below as “ special dvd - 5 design # 2 ”), the direction of the spiral track is inverted during mastering , the information bearing substrate is flipped “ upside down ”, and the information is read through the non - information bearing substrate 415 and the bonding layer 401 . in this type of optical disc , the bonding layer 401 is an integral part of the optical path 405 of the reading laser . even though the structure of the “ special dvd - 5 ” disc described herein differs from a standard dvd - 5 , a player would play this disc as if it were a standard dvd - 5 . this embodiment of the present invention has significant advantages in terms of allowing the manufacturing of a low - cost “ limited - play ” optical disc that is resistant to attempts to defeat it . in particular , because it does not incorporate any additional layers compared to a standard dvd - 5 , it can be manufactured on equipment designed to manufacture dvd - 5 discs with minimal changes to that equipment . furthermore , because the bonding layer 401 is in the optical path , 405 modifying that layer to interfere with the reading of data in response to a predetermined stimulus results in a disc that is very difficult to defeat , as the interfering layer 400 is protected by the two substrates 415 and 420 , respectively of the optical disc . for example , grinding the interfering layer 400 off the disc is impractical , as it would most likely destroy the disc . similarly , attempting to compromise the bonding / interfering layer in other ways is likely to destroy the structural integrity of the optical disc . we now describe in detail the manufacturing of three embodiments of the current invention , which we label as “ special dvd - 5 ” designs 1 , 2 and 3 . in one embodiment of the invention , the above process is modified by using the mother stamper to replicate the l 1 disc substrate 420 . fig3 shows how the stamper or father is used to mold a normal single layer dvd - 5 substrate . fig8 illustrates manufacturing this embodiment of the current invention by using the mother stamper 40 and creating a disc with the bonding layer 401 in the optical path 405 . in a normally molded standard dvd - 5 information is encoded on the l 0 100 side with “ pits ” 20 and “ lands ” 25 molded on the l 0 substrate 100 and metallized with a reflective metal coating , 105 as illustrated in fig2 , fig3 and fig9 . in one embodiment of the current invention , the mother stamper 40 is used to mold the l 1 side 420 as shown in fig8 . this side is subsequently metallized and bonded with a blank l 0 substrate , 415 leaving the bonding layer 401 in the optical path , 405 as shown in fig1 . using the specified layer thickness of 0 . 055 mm +/− 0 . 015 , the thickness of the l 0 substrate 100 is targeted at 0 . 55 mm ˜ 0 . 57 during molding , to yield a focal length of the disc thickness ( including the bonding layer ) consistent with standard dvd specifications , allowing the player to be in the normal focusing range for reading a l 0 layer 100 . thus the player interprets the disc as a standard single layer dvd - 5 . field experience has shown that spacer layer thickness can be maintained at 0 . 045 ˜ 0 . 065 mm consistently in production . this controlled variation in production along with the reduced thickness of the molded disc keeps the focus and optics within the specifications set by the dvd licensing authority and the hardware manufacturers . for the replication facility , most applications would remain unchanged in the actual pressing and bonding portions of production . the main areas of change would be in the lbr ( laser beam recording ) and developing areas of mastering . typically , masters are cut with larger pit volumes to compensate for plastic shrinkage and replication inefficiencies . the ratio of pit to land areas on a disc is measured by a term called asymmetry . because asymmetry is a ratio of pit to land area , and because for each pit area , typically defined by i 3 to i 14 pit , there is an equal and opposite land area i 3 to i 14 land , typically it is easier for manufacturers to target a positive asymmetry ( larger pit area ) to account for loses in replication to the plastic substrate . for example , the master may be cut with a positive 10 ˜ 12 % for asymmetry , while the end result from molding may be 5 ˜ 7 %. the specification for the disc substrate is : − 0 . 05 ≦ asymmetry ≦+ 0 . 15 . in the case of dvd discs , a positive asymmetry represents a larger pit volume compared with the land area . for this embodiment of the invention , it may be desirable to change the asymmetry set point on the lbr to produce a higher asymmetry value on the father stamper while subsequently increasing the asymmetry on the mother stamper used for molding . asymmetry can be changed on the master by modifying the power of exposure , focusing intensity and offset , developing time / endpoint detection , or baseline ( control of how fast the laser diode cuts the laser exposure beam off between exposure ). there are many other possible ways to control asymmetry , but the basic process or set point control would be the easiest to implement . this process of molding from the mother stamper would also eliminate the need to grow additional stampers and the subsequent yield loses attributed to the family process . in this embodiment of the invention , the pits 20 are molded in the l 1 layer 420 using a mother stamper , 40 and as a result the surface of the pits 20 is elevated relative to the reference plane 450 of the l 1 layer 420 as illustrated in fig1 . this reference plane 450 is typically used for tracking by the disc player ( tracking area ). by contrast , in a normal dvd - 5 the pits 20 are molded as cavities in the l 0 substrate 100 as illustrated in fig9 . using the common convention of describing a disc as if it is in a play position where it is read from the bottom , and a convention that we will follow hereinafter unless otherwise specified , in a normal dvd - 5 the pits 20 are lower than the reference plane 450 , while the lands 25 are at the reference plane 450 ( see fig9 ). in the embodiment of the invention described above the blank l 0 substrate 415 and the bonding layer 401 are below the l 1 substrate 420 in the optical path 405 of the reading laser , and the surface of the pits 20 in the l 1 substrate 420 is below the reference plane 450 while the lands 25 are at the reference plane 450 ( see fig1 ). note that this construction requires the pits 25 to be molded in an unconventional way ( they protrude from the reference plane 450 of the disc ), which is achieved by molding the l 1 substrate 420 from a mother stamper 40 . fig1 shows an atomic force microscope ( afm ) image of a father stamper 30 for a dvd - 5 , fig1 shows an afm image of the corresponding mother stamper 40 , and fig1 shows an afm image of the l 1 layer of a special dvd - 5 design # 1 , molded from the mother stamper 40 . this molding required for this embodiment of the invention can present certain challenges . in a typical injection molding process , the polymer material flows around the pits 20 on the stamper , which are raised from the reference plane 450 . this is easier than to mold from the mother , where the polymer material must flow into cavities that will form the pits 20 on the separated part . as the material flows over the surface of the mother stamper 40 , the molecular chains cool off through contact with the relatively colder reference surface of the stamper . after the mold is completely filled , then pressure must be applied to bend and force the cooler polymer material into the pit 20 cavities . although this method is capable to reproduce discs within the specifications of a standard dvd - 5 configuration , the molding process is more difficult . however , one skilled in the art can address such challenges by adjusting the process characteristics of the molding machine , e . g ., by increasing mold surface temperature and cycle time . alternatively appropriate materials with higher melt flow rate could be used , such as pmma or high melt flow rate polycarbonate . for example , general electric &# 39 ; s spoq research grade polycarbonate has twice the melt flow rate of standard grade polycarbonate . as long as the index of refraction ( ri ) of the bonding adhesive used is approximately equal to the ri of the l 0 substrate 415 , the thickness of the bonding layer 401 is uniform , and the thickness of the l 0 substrate 415 has been adjusted to compensate for the presence of the bonding layer 401 in the optical path 405 of the reading layer , the player will not be able to distinguish special dvd - 5 design # 1 from a standard dvd - 5 . experience has shown that playable discs can be manufactured even without these adjustments , because most players will play discs that do not fully conform to the dvd specification , as long as the departure from the specification is not excessive . a father stamper 30 was mastered with slightly increased symmetry ( positive asymmetry = larger pits 20 compared to lands 25 ). the asymmetry can be increased or decreased many ways . the simplest method and the one used for this design , was to increase the development time ( endpoint detection set point ) to overdevelop the pits 20 . by lengthening the development process , the pit volume surrounding , that which was exposed , will increase in volume causing a shift to positive asymmetry . a mother stamper 40 was grown from the father stamper 30 as with a normal family process . disc substrates were molded from the mother stamper 40 , taking advantage of the larger indentation caused by the positive asymmetry . the larger pits 20 that resulted from molding with the mother 40 helped to compensate for the additional shrinkage of the pit 20 , which is now an extremity to the body of the substrate , rather than a cavity as in the standard molding process . typically , the molten plastic flows around the pits 20 in a normal ( father 30 or son 45 ) stamper like a river flows around a hill . as the level rises , the hill or the pit 20 will be covered . as the molten plastic flows across the cooler stamper surface , a skin layer forms right on the surface that acts as a heat insulator . this allows for the plastic to maintain its flow rate necessary to form the pit volume without undue stress or cooling . in the case of special dvd - 5 design # 1 , the plastic has to flow into the indentations of the mother stamper 40 , rather than around the bumps of a father / son stamper 30 and 45 respectively . this is difficult because as the plastic flows across the surface of the mother stamper 40 , it again forms a skin layer on the surface . then as the mold volume increases with continued injection and packing / holding time , the molten plastic must be forced into the indentation . because this skin layer is solidified typically below the glass transitional temperature of the plastic , the material does not free flow into the indentation . because the pit - forming plastic in the l 1 substrate 420 of special dvd - 5 design # 1 is not in the optical path of the reading laser , the material can be filled with greater force without the concern for birefringence and residual stress , although there is a limit to the pressure due to warping ( tilt ) caused by excessive packing pressure on the plastic . in this example , the combination of larger indentations in the mother stamper 40 as well as increased mold temperatures assisted in replicating the desired pits 20 . typically , in direct water injection systems for the mold heating and cooling , safety interlocks of 120 ° c . max temperature limit the temperature of the water . by using a 50 / 50 solution of glycol and water , the temperature can be effectively run at a max temperature of 130 ° c . this added temperature assists in keeping the skin layer in the molten state , close to its glass transition temperature , which facilitates the replication of l 1 substrates 420 for special dvd - 5 design # 1 . also , the mother stamper 40 must be filled quickly with molten plastic in order to prevent skinning on the surface . l 1 substrates 420 were molded as above using a mother stamper 40 . fig1 shows an atomic force microscope ( afm ) image of an l 1 layer 420 molded from a mother stamper 40 . fig1 and 12 show afm images of the father 30 and mother 40 stampers used in the process . for these discs to be formed , it was necessary to raise the melt temperature from 360 ° c . to 390 ° c . while maintaining a mold temperature of 121 ° c . compared to the standard of around 100 ° c . the clamp force was set at maximum of 30 tons and the filling time was decreased from 0 . 13 to 0 . 09 seconds . these parameters were adjusted until the proper pit 20 formations were achieved . the molded l 1 substrates 420 were bonded using optical grade uv curable dvd adhesives , as used in dvd - 9 production , to blank l 0 substrates 415 , to manufacture design # 1 of the special dvd - 5 . l 0 substrates 415 were molded at a thickness of 0 . 55 ˜ 0 . 57 mm ( i . e ., 30 ˜ 50 micron thinner than standard dvd halves ) to compensate for the bonding layer in the optical path , thus preserving the same focal depth for the information - carrying layer as in a standard dvd - 5 . the electronics of optical media drives , including dvd players , are typically designed to read the information contained in a layer on the disc by identifying the interference patterns caused by the transitions from a “ land ” 25 to a “ pit ” 20 in that layer . the pits 20 are often molded with a height approximately equal to , and typically somewhat less than , one quarter of the wavelength of the reading laser . for example , in dvds the typical wavelength of the reading laser is 635 - 650 nanometers ( in vacuum ), or 410 - 420 nm in a material with ri = 1 . 55 ( which is typical of the materials used to manufacture the dvd substrates ), and thus the height of the pits in a standard dvd - 5 should be approximately 100 - 105 nanometers . consequently , a transition from a land 25 to a pit 20 or vice versa corresponds to a change to the path of the reading laser of approximately one half wavelength , or a phase change of approximately 180 degrees . two identical waves with a phase difference of 180 degrees will interfere with each other and cancel out , and the electronics of the optical drive are designed to detect the resulting interference patterns . using the standard convention of the disc being read from below , in a standard dvd - 5 the surface of the pits 20 is below the surface of the land 25 , and a transition from a land 25 to a pit 20 is a “ down ” transition , while a transition from a pit 20 to a land 25 is an “ up ” transition . if the height of the pits 20 is one quarter of the wavelength of the reading laser then a transition from a land 25 to a pit 20 in a standard dvd - 5 is a “ down ” transition that corresponds to a phase change of + 180 degrees , and a transition from a pit to a land 25 is an “ up ” transition that corresponds to a phase change of − 180 degrees . if an “ up ” and a “ down ” transition differ by 360 degrees , as in the case described above , their effects will be identical . one implication of this is that the pits 20 of a dvd - 5 could be molded in the opposite direction , i . e ., with the pit surface approximately one quarter wavelength above the land 25 surface , and the electronics of the optical disc player are unlikely to be influenced by whether a detected transition is in the “ up ” or “ down ” direction , i . e . whether a pit 20 area is higher or lower than the land 25 area . in a standard dvd - 5 , the laser pick up will read through the l 0 substrate 100 focusing on the pits 20 aligned in a spiral track . the rotation of the disc would be in the counterclockwise direction ( as seen from the side of the reading laser ), and the spiral track would be in the clockwise direction . given that the pit 20 direction can be reversed without changing the electrical signal seen by the player , in another embodiment of the current invention the pits 20 are molded as depressions 500 into the l 1 substrate 420 , by employing a normal ( father / son ) dvd - 5 stamper 30 / 45 , as illustrated in fig1 . the direction of the spiral track is reversed during mastering , as the disc will be read from the side of the bonding layer 401 , rather than through the substrate as in a standard dvd - 5 . the resulting disc has information encoded as a dvd - 5 , although the pits 20 are formed in the l 1 layer 420 : the surfaces of the pits 20 are above the surfaces of the lands 25 , and the lands 25 are at the reference plane of the l 1 layer 420 , as illustrated in fig1 . the pit 20 width , length , height , and shape give the corresponding hf signals needed to decode the data on the dvd . the signals are encoded utilizing an eight - to - fourteen modulation ( efm ) signal . the pit 20 edges and slopes of the sidewalls serve to distinguish the logical transition of 0 &# 39 ; s and 1 &# 39 ; s . this results in pit 20 length units measured as 3 units long to 14 units long , which set the frequency limits of the efm signal , read from the disc . this measurement is commonly referred to as 3t - 14t signal with t referring to a period of time . as long as the pits 20 are replicated in standard fashion , the player will still be able to distinguish the pit 20 start and end position , while reading from the reverse side , to correctly identify its data identity . in many circumstances this will be the preferred embodiment of the invention , as it does not require molding from the mother stamper 40 , as is the case with special dvd - 5 design # 1 above . the actual height of the pits 20 in a standard dvd - 5 is typically somewhat less than one quarter wavelength of the reading laser . this is intended to avoid complete cancellation of the reflected laser during a pit - to - land transition , which facilitates the functioning of player electronics . for example , a value of 0 . 88 *( laser wavelength )/ 4 is sometimes recommended , i . e . approximately 90 nanometers for a material with ri = 1 . 55 . thus it may be desirable to mold the pit 20 surfaces in this embodiment of the current invention somewhat higher than one quarter the wavelength of the reading laser , so that the change in the path of the reading laser during a transition from a land 25 to a pit 20 in the special dvd - 5 design # 2 will be exactly one wavelength longer than the corresponding change in a standard dvd - 5 . for example , if the reading laser wavelength is 650 nanometers ( i . e ., 420 nm in a polycarbonate substrate of ri = 1 . 55 ), and the pits in a standard dvd - 5 are 90 nanometers , the pits 20 in this embodiment ( special dvd - 5 design # 2 ) can be molded at 120 nanometers , i . e ., one half wavelength ( 210 nm ) from the position of the pit 20 surface in design # 1 . a special stamper for molding l 1 substrates 420 for special dvd - 5 design # 2 was produced through a modified mastering process , where the direction of rotation of the laser beam recorder turntable was reversed during the cutting process , resulting in a spiral tracking path in the opposite direction from that in a normal dvd - 5 . this stamper was produced by forcing the turntable to rotate in the reverse direction from cutting a normal dvd - 5 , while the content information was fed to the laser beam recorder as a dvd - 5 image . the scanning velocity that is normally preset for dvd formats was manually set to the velocity of 3 . 49 m / s typical in dvd - 5 mastering . l 1 substrates 420 were then molded on standard molding machines set up for dvd - 5 fabrication . some of the molded l 1 substrates 420 were bonded using optical grade uv curable dvd adhesives to blank l 0 substrates 415 , to manufacture design # 2 of the special dvd - 5 . as in example 1 , the l 0 substrates 415 were molded at a thickness of 0 . 55 ˜ 0 . 57 mm ( i . e ., 30 ˜ 50 micron thinner than standard dvd halves ) to compensate for the bonding layer 401 in the optical path , thus preserving the same focal depth for the information - carrying layer as in a standard dvd - 5 . to bond the discs , the machines were placed into a dvd - 9 production mode and the semi - reflective metallizer for the l 0 layer was taken offline . then the cure time was adjusted to compensate for the decrease in cure exposure needed due to the missing semi - reflective layer . curing was basically set for a dvd - 5 disc , and the disc was flipped to cure through the l 0 layer . this function is typically reserved for dvd - 9 production . the discs were then tested with a koch dvd testing system and played in four different dvd players . they performed indistinguishably from regular dvd - 5 discs , as illustrated in fig2 and 22 . also , the discs played with no errors in an additional three dvd players and two dvd - rom drives . some of the molded substrates were used to manufacture discs with a reactive bonding layer ( see example 9 ). the electronics of optical media drives , including dvd players , can be designed to read the information contained in a layer on the disc by identifying pits 20 and lands 25 in that layer based on the absolute and / or relative elevation of these pits 20 and lands 25 , thus distinguishing between an “ up ” and a “ down ” transition in the information encoding layer , but without being influenced by the elevation of the pits 20 and lands 25 relative to the reference plane 450 of the layer . thus in another embodiment of the current invention , during mastering the direction of the spiral track is reversed and also the pits 20 and lands 25 are reversed , so that the pits 20 become lands 25 on the resulting stamper 30 , and lands 25 become pits 555 . the l 1 substrate 420 is then molded by employing 550 a normal ( father ) stamper 30 and is bonded to a blank l 0 substrate 415 . the resulting disc has information encoded as a dvd - 5 , the relative elevation of pits and lands , and the “ up ” and “ down ” transitions in the information encoding layer , are identical to a dvd - 5 . specifically , the surface of the pits is below the surface of the lands . however , while in a standard dvd - 5 the surface of the lands is at the reference plane of the l 0 layer , in this embodiment it is the surface of the lands 560 ( corresponding to pits on a standard dvd - 5 ) that is at the reference plane of the l 1 layer , with the pits 565 ( corresponding to lands on a regular dvd - 5 ) being above this reference plane , as illustrated in fig1 . another embodiment of the present invention is having a reactive material incorporated in an interstitial layer . in one embodiment , the interstitial layer is the bonding layer of the disc . in one embodiment of the invention , the stimulus triggering the reaction is exposure to atmospheric oxygen . upon exposure to oxygen , a reactive material , e . g ., leuco methylene blue , which is essentially colorless , is oxidized to form an opaque or semi - opaque layer ( e . g ., the deep blue dye , methylene blue ). data storage media with the opaque / semi - opaque layer can no longer be played in media players . by adjusting the time it takes to turn opaque , this method can be used to provide limited - play data storage media having the desired life for the given application . the reactive layer , which comprises both a carrier and a reactive material , should initially have sufficient transmission to enable data retrieval by the data storage media device , and subsequently form a layer which inhibits data retrieval by that device ( e . g ., which absorbs a sufficient amount of light i . e ., incident and / or reflected light ) at the wavelength of the laser in the given device ). typically a layer that allows an initial percent reflectivity from the reflective layer of about 50 % or greater can be employed , with an initial percent reflectivity of about 65 % or greater preferred , and an initial percent reflection of about 75 % or greater more preferred . once the media has been exposed to oxygen , e . g ., air , for a desired period of time ( e . g ., the desired allowable play time of the media ), the layer preferably comprises a percent reflectivity of about 45 % or less , with about 30 % or less preferred , about 20 % or less more preferred , and about 15 % or less especially preferred . possible reactive materials include oxygen sensitive leuco or reduced forms of methylene blue , brilliant cresyl blue , basic blue 3 , methylene green , taylor &# 39 ; s blue , meldola &# 39 ; s blue , new methylene blue , thionin , nile blue , celestine blue , and toluidine 0 , as well as reaction products and combinations comprising at least one of the foregoing material ; the structures of which are set forth below : a method of synthesis of leucomethylene blue and the oxygen dependent reoxidation to form the colored form of the methylene blue dye is shown below : in addition to the above reactive materials , numerous other dyes and light blocking materials , can be synthesized to operate to render the data storage media limited play . for example , some other possible reactive materials can be found in u . s . pat . no . 4 , 404 , 257 , hereafter incorporated by reference , and u . s . pat . no . 5 , 815 , 484 , hereafter incorporated by reference . the reactive materials can further comprise a mixture comprising at least one of any of the above mentioned reactive materials . the reactive material is preferably mixed with a carrier for deposition on and / or impregnation into at least a portion of the surface of the substrate . possible carriers comprise the thermoplastic acrylic polymers , polyester resins , epoxy resins , polythiolenes , uv curable organic resins , polyurethanes , thermosettable acrylic polymers , alkyds , vinyl resins and the like , as well as combinations comprising at least one of the foregoing carriers . polyesters include , for example the reaction products of aliphatic dicarboxylic acids including , e . g ., fumaric or maleic acid with glycols , such as ethyleneglycol , propyleneglycol , neopentylglycol , and the like , as well as reaction products and mixtures comprising at least one of the foregoing . some epoxy resins , which can be the used as the organic resin , include monomeric , dimeric , oligomeric , or polymeric epoxy material containing one or a plurality of epoxy functional groups . for example , reaction products of bis phenol - a and epichlorohydrin , or the epichlorohydrin with phenol - formaldehyde resins , and the like . other organic resins can be in the form of mixtures of polyolefin and polythiols , such as shown by kehr et al , u . s . pat . nos . 3 , 697 , 395 and 3 , 697 , 402 , hereafter incorporated by reference . optionally , the reactive layer can be applied to the substrate using various coating techniques such as painting , dipping , spraying , spin coating , screen printing , and the like . for example , the reactive layer can be mixed with a relatively volatile solvent , preferably an organic solvent , which is substantially inert towards the polycarbonate , i . e ., will not attack and adversely affect the polycarbonate , but which is capable of dissolving the carrier . examples of some suitable organic solvents include ethylene glycol diacetate , butoxyethanol , the lower alkanols , and the like . for surface coatings , the reactive layer may also optionally contain various additives such as flatting agents , surface active agents , thixotropic agents , and the like , and reaction products and combinations comprising at least one of the foregoing additives . the thickness of the reactive layer is dependent upon the particular reactive material employed , the concentration thereof in the reactive layer , and the desired absorption characteristics of the layer both initially and after a desired period of time . one embodiment of the present invention is the use of blocked forms of the reactive compounds in the reactive layer . these compounds will unblock within a predetermined time period after the disc is manufactured or packaged , and typically before the disc is used by the consumer . this is desirable when the stimulus that triggers the reaction that causes the disc to become unplayable ( e . g ., atmospheric oxygen ) can trigger this reaction during the manufacturing of the disc , and thus measures need to be taken so that the reactive compound is not activated during the manufacturing of the disc . for example , in the case of oxygen triggered reactions , unless a blocked form of the reactive compound is used , manufacturing may need to take place in an oxygen free environment , such as a nitrogen atmosphere . one embodiment of the present invention comprises the idea of using a chemically blocked reactive substance for the purpose of producing optical discs that become unplayable after being exposed to oxygen , a specific such blocked leuco dye , a method of preparing this leuco dye precursor , a formulation including this leuco dye precursor which permits the deblocking and oxidation of the leuco dye precursor at acceptable rates , methods of applying this formulation to optical discs both on the surface of optical discs and as bonding layers for optical discs , the use of bases to increase the rate of methylene blue generation in blocked leuco dye - containing layers in or on optical discs , and the use of silyllaating agents such as hexamethyldisilazane to stabilize the blocked leuco dye in coating fluids . in one embodiment of the invention , to manufacture an optical disc that becomes unplayable after being removed from its package ( a “ limited - play disc ”), the disc incorporates a reactive layer with a composition containing a leuco dye which oxidizes to a colored dye which absorbs light at the wavelength of the reading laser of an optical disc player , preventing enough of the reading laser light from being reflected off the disc to render the disc unplayable . the oxidation of the leuco dye can be initiated by exposure of the coating containing the dye to atmospheric oxygen , which diffuses through the coating to oxidize the leuco dye molecules . one problem with putting such a coating on the surface of the disc is the possibility of the coating being removed by a consumer to make the disc permanently playable . another problem with putting such a coating on the surface of an optical disc is that this requires an additional step in the disc manufacturing process , entailing higher cost , special tooling for production equipment , and inevitably lower manufacturing yields . finally , the oxygen - sensitive fluid used to make such a coating is difficult to handle because of its oxygen sensitivity . in some methods of coating a leuco - dye - containing fluid on the surface of an optical disc , some of which were described above , the coating is solvent based and the solvent must evaporate to yield a hard coat containing the leuco dye and any other components required , typically bound in a polymer matrix . there are several disadvantages to such a solvent coating . first , most of the solvent based fluid is spun off of the disc during a spin coating manufacturing process and is difficult or impossible to recover due to solvent evaporation , which both wastes fluid ( increasing the cost of the process ) and fouls the coating equipment . second , evaporation of the solvent takes time , which reduces the rate at which such coated discs can be manufactured and thereby increases the cost of the process . third , the solvent vapors emitted by the coated disc during the coating and drying process must be vented from the manufacturing equipment , increasing the cost of the installed equipment and presenting process and environmental obstacles to disc replicators considering adopting this manufacturing process . all of the problems discussed in the previous two paragraphs could be avoided if the leuco dye could be coated in a solventless , light or radiation cured ( hereafter called generically “ uv - cured ”) layer , and if this layer could be the same as the optical disc bonding layer that is used to bond the two substrates which compose certain types of optical disc , such as a dvd . the major obstacle to creating such a system is that many leuco dyes , and in particular leucomethylene blue ( hereafter “ lmb ”, which has been used by the present inventors to render dvds unplayable in a solvent - based , surface coated system ), inhibit both radical and cationic polymerization reactions of the type used to cure uv - curable monomers such as the acrylates that are commonly used as adhesives for bonding dvd substrates . the oxidized dyes ( including methylene blue ) also are inhibitors of such polymerization reactions . so putting a leuco dye ( which will inevitably contain some of the oxidized , colored dye ) in a uv - curable composition will either prevent the uv - curing from taking place , or slow the uv - curing and make the process much less economical by reducing the rate at which discs can be manufactured . moreover , the process of uv - curing can result in some of the leuco dye becoming oxidized if any oxygen or other oxidizing agent is present in the layer to be cured , resulting in a product prematurely containing oxidized dye which may interfere with the readability of the disc or change the rate at which it becomes unreadable after exposure to oxygen . chemically blocked ( sometimes called “ protected ”) leuco dyes ( also called “ leuco dye precursors ”) are known and have been used for decades in applications such as “ carbonless copy paper ”. in particular , blocked versions of leucomethylene blue are known and have been used in such applications , and one such compound at least , benzoyl - leucomethylene blue ( blmb ), is commercially available . however , we have found that blmb does not deblock easily enough to yield an acceptable limited play dvd product . other blocked leucomethylene blue compounds share this problem , or deblock too easily such that oxidizable leucomethylene blue is generated in the coating fluid before it is desired . we have found that triisopropylsilyloxycarbonylleucomethylene blue ( hereafter “ tipsoclmb ”), whose structure and exemplary synthesis are illustrated in fig1 and described in example 4 , has the following desirable properties for use in creating limited - play dvds : 1 . it is readily synthesized in two steps from commercially available starting materials . by isolating and purifying the boc - lmb produced in the first step as shown in fig1 , the tipsoclmb is prepared from a pure compound rather than from the typically very impure methylene blue . 2 . it can be incorporated into an acrylate formulation described in example 5 in which it is stable ( to conversion to oxidized methylene blue ) for at least several weeks at temperatures below 0 c ., allowing coating formulations to be prepared at one facility and shipped to another facility for dvd manufacturing if desired . 3 . it can be deblocked in a period of a week or less , presumably by a hydrolysis reaction involving water or other nucleophiles which can either be provided in the acrylate formulation or be absorbed from the atmosphere in which the dvd is manufactured or in the dvd packaging material . 4 . the deblocked lmb is stable ( to oxidation to methylene blue ) in the absence of oxygen . the rate at which the deblocked lmb oxidizes in the presence of oxygen can be controlled by controlling the effective ph of the coating formulation . it is known in the art that the rate of oxidation of lmb increases as the ph of its environment increases . thus the rate of oxidation can be increased by the addition of basic substances that are soluble in the matrix containing deblocked or blocked lmb and which do not react with the matrix or substrate used . one such basic compound is dabco ( 1 , 4 - diazabicyclo [ 2 . 2 . 2 ] octane ), an amine . other amines may be added or substituted . further , the addition of a strong protic acid such as camphorsulfonic acid decreases the rate of lmb oxidation in a polymer film . 5 . in the absence of water or other nucleophiles , it is a stable solid which can be stored after synthesis for at least several months , even in the presence of oxygen . acrylate - based coating fluids containing tipsoclmb can be handled in the presence of oxygen until the deblocking reaction has taken place , which reaction is slow enough that the handling of the coating fluid during the dvd manufacturing process can be done in normal ( undried ) air and is not difficult . in a 2 - liter separatory funnel was dissolved 60 . 0 g of sodium hydrosulfite ( sodium dithionite , na 2 s 2 o 4 ) in 300 ml cold distilled water . to this solution was added 60 . 0 g methylene blue ( dark green powder ) from several different bottles , and the separatory funnel was stoppered and shaken vigorously over a 30 - minute period , during which time the dark green solids gradually form a tan suspension of insoluble leucomethylene blue . to this suspension was added three 60 - ml portions of 10 % aqueous sodium hydroxide solution with vigorous shaking after each addition . some heat is evolved , and a lighter suspension results . after allowing the mixture to stand for a short while to cool , 700 ml methylene chloride was added and the separatory funnel was stoppered and shaken to dissolve the solids . an amber organic layer began to separate below an emulsion . an additional portion of 60 ml aqueous naoh was added , the stoppered funnel was shaken , and the emulsion was allowed to stand for 30 - 60 minutes to separate into two liquid phases . alternatively , fresh na 2 s 2 o 4 and reasonably pure methylene blue may be used to result in a faster and cleaner phase separation . to a 1 - liter , 3 - necked , round - bottomed flask equipped with a magnetic stirrer and nitrogen inlet inside a fluted adapter ( aldrich z11 , 563 - 0 ) packed with 1 . 5 sheets of crumpled small kimwipe ® tissues ( 11 × 21 cm ) was added 81 . 0 ml di - tert - butyldicarbonate ( boc 2 o ) diluted with 25 ml methylene chloride . after stirring under nitrogen for 5 - 10 minutes , 3 . 0 g of 4 -( dimethylamino ) pyridine ( dmap ) was added followed by dropwise addition of the leucomethylene blue solution from the separatory funnel and through the fluted kimwipe - containing tube . the stem of the separatory funnel was connected to the fluted tube through a one - holed rubber stopper so that the addition was performed under nitrogen . gas evolution ( co 2 ) began immediately . after two hours , the addition was completed to give a dusty green reaction mixture that was stirred overnight under nitrogen at room temperature . on the following morning , the dusty green reaction mixture was arranged for atmospheric distillation . about 550 ml ch 2 cl 2 was distilled off and replaced with 300 ml hexanes . a gray - blue solid separated out . distillation was continued until the head temperature reached about 55 ° c . the mixture was allowed to cool ; then the solid was collected by filtration through a sintered glass funnel . the solid was washed with hexanes ( 2 × 50 ml ) to remove excess boc 2 o , and then it was washed with methanol ( amount unspecified , 4 × 50 ml estimate ) to remove unreacted and oxidized leucomethylene blue until the wash liquid was only faintly blue . the resulting gray solid was dried in air and then under vacuum at room temperature . thin layer chromatography analysis on a 5 × 10 cm whatman k5f silica gel plate eluting with 5 % acetone in methylene chloride showed a faint blue spot at the origin , a very weak spot at r f = 0 . 58 , and a large product spot at r f = 0 . 63 . the initially colorless product spot became dark blue upon standing in air , and rapidly when heated in a 120 ° c . oven . repetition of this reaction at the same scale resulted in a yield of 48 . 0 g ( 78 %). to a 500 - ml , 3 - necked , round - bottomed flask equipped with a magnetic stirrer , addition funnel , and condenser under a nitrogen bubbler was dissolved 35 . 61 g boclmb in 200 ml methylene chloride to give a blue solution . to this solution was added 26 . 0 ml 2 , 6 - lutidine followed by dropwise addition of 39 . 0 ml of triisopropylsilyl trifluoromethanesulfonate ( tipsotf ) over a 15 minute time period . the green - blue reaction mixture was then stirred under reflux for 6 hours . tlc analysis ( k5f silica , 5 % acetone / ch 2 cl 2 ) showed only a small amount of boclmb starting material present at r f = 0 . 67 with a large product spot at r f = 0 . 74 . the reaction mixture was then stirred overnight at room temperature under nitrogen . on the next morning , the green - blue clear reaction mixture was again stirred under reflux for one hour . tlc analysis still indicated that a trace of boclmb or similar r f impurity was present . the solution was then concentrated on a rotary evaporator under vacuum to remove most of the methylene chloride , resulting in a dark green - blue syrup . after addition of 200 ml hexanes , the mixture was stirred by hand to effect the separation of a blue - gray solid . upon heating this mixture under reflux with continued hand stirring , the tipsoclmb product dissolved in the hot hexanes leaving behind a dark blue salt residue as a melt or crusty solid . the hot hexanes solution was decanted from the residue , and the residue was further extracted with 60 ml boiling hexanes . the combined hot hexanes extract ( green in color ) was allowed to cool slightly and was then filtered through a 1 . 5 cm - thick layer of celite to obtain a clear , pale tan filtrate . after washing the celite twice with 30 ml portions of hot hexanes , the combined filtrate (˜ 320 ml volume ) was placed in the freezer ( about − 20 ° c .) overnight . on the following morning , an off - white solid with a greenish cast was observed to have crystallized . the mixture was filtered cold , and the product was washed with cold hexanes ( 2 × 50 ml ), sucked dry , and dried under vacuum at room temperature to an off - white solid . yield : 33 . 3 g ( 75 %). ( mw of tipsoclmb = 485 . 77 ) the melting point from an earlier run was 121 - 123 ° c . tlc analysis ( k5f silica , 3 % acetone / ch 2 cl 2 ) showed very weak spots at the origin and at r f = 0 . 53 ( probably unreactied boclmb ) with the main spot at r f = 0 . 61 that is initially colorless and becomes dark blue upon standing at room temperature for several hours , or in a 120 ° c . oven for a few minutes . examples 5 and 6 illustrate how tipsoclmb can be incorporated in a coating fluid that can be uv - cured to create a reactive layer containing tipsoclmb . example 7 illustrates how the above technique can produce an interstitial reactive layer , which allows the special dvd - 5 designs 1 , 2 and 3 to be used to manufacture expiring optical discs . example 8 illustrates how tipsoclmb deblocks and becomes oxygen sensitive lmb in either a surface or an interstitial layer . when exposed to oxygen , the lmb oxidizes into methylene blue , as illustrated by the increasing cyan density in fig1 ; methylene blue strongly absorbs light in the 650 nm wavelength , as illustrated in fig1 . the tipsoclmb , irgacure 819 , and dabco are weighed into a brown glass bottle , a stir bar is added , the cd - 501 is poured in to the proper weight , and the hmdz is added by syringe . dry nitrogen is blown into the bottle for a few minutes and the bottle is capped and the cap covered by parafilm . the contents are stirred at room temperature for at least two hours to dissolve the solids . if not all of the material is used , blow the bottle with nitrogen , cap and seal with parafilm , and store in a freezer ; warm the bottle before opening to prevent water from condensing in the bottle . a dvd clear half disk ( an unmetalized 0 . 6 mm thick and 120 mm diameter polycarbonate disc ) or a full dvd ( two layers bonded together , back to back with a adhesive ) is centered on a laboratory spin coating turntable rotating at roughly 60 rpm &# 39 ; s . a 4 ml solution from example # 5 is then applied uniformly in a circular ring by a syringe at about a 34 to 40 mm diameter from the center of the disc . the spin speed is then rapidly increased to about 200 rpm for about 15 seconds , resulting in a coating of acrylate / tipsoclmb fluid about five μm thick . the spinning is slowed ; excess fluid wiped off of the edge of the disk with a tissue and base solvent , if available , and then removed to a lab bench . at this point , the disc is subjected to about five flashes from a norlite 400 xenon flash lamp at its max setting . the time between flashes is dictated by the charging of the flash lamp , but should be sufficient as to not induce added stress from heat generated in the cure ( typically about 5 seconds ). this process will yield a clear , uncolored , fully cured acrylate film . other disks are also prepared with similar acrylate formulations that contain either no dabco or 10 × the amount of dabco described in example 5 . a dvd half disk is centered data side up on the turntable as stated above . the turntable is held stationary while the fluid is dispensed on the data side in a manner creating drops with a syringe roughly 3 ˜ 5 mm round . these are evenly spaced about 3 mm apart on a diameter of 30 ˜ 40 mm . the disc to be bonded is then placed data side facing the solution and slightly bowed away from the bottom disc by the edges . the disc will be lowered at an angle until the first contact point between a fluid drop and top disc occurs . we do not want to place the top disc immediately on the bottom because of entrapped air and subsequent bubbles . therefore , to get a more uniform capillary flow , we can rotate the disc in a clockwise rotation while keeping it slightly bent under light pressure until each of the fluid drops begins to form a capillary bridge ring . once the capillary ring is completed , the top disc can be released and the capillary action will continue . we can wait for the capillary flow to cover the surface , or we can spin the disc at 100 rpm &# 39 ; s until the material at least reaches the maximum od diameter . at this point the turntable can be turned on and rotated at about 500 rpm &# 39 ; s for 5 seconds . this will level the spacer layer ( adhesive layer ) and remove excess material from the od . the disc edge can then be wiped and the disc will then be uv cured . it is important that prior to curing , the disc halves be aligned as close as possible to avoid center hole misalignment an subsequent play back problems . at this point , the disc is subjected to about 20 ˜ 30 flashes from a norlite 400 xenon flash lamp at its max setting . the time between flashes is dictated by the charging of the flash lamp , but should be sufficient as to not induce added stress from heat generated in the cure ( typically 5 seconds ). this process will yield a clear , uncolored , fully cured acrylate film . other disks are prepared with similar acrylate formulations that contain either no dabco or 10 × the amount of dabco described in example 5 . deblocking and oxidation of tipsoclmb in surface and sandwich - coated disks , and the effect of a base included in the coating formulation disks prepared as described in examples 6 and 7 were cut into six ‘ chips ’ each and the chips were stored in either dry nitrogen , dry air , or room air ( average rh about 30 %) and their cyan reflectance densities were recorded periodically with an x - rite 504 densitometer ( the samples stored in nitrogen were only tested at the start and end of the experiment as they were visibly unchanged and it was desired to minimize their exposure to oxygen ). in all cases the samples stored in nitrogen showed no methylene blue ( mb ) generation , as expected . incorporating 1 , 4 - diazabicyclo [ 2 . 2 . 2 ] octane ( dabco ) into an acrylate formulation at 1 . 0 equivalent with respect to the tipsoclmb gave very significant acceleration of the deblocking / oxidation rate compared to a control ( fig1 ), while a higher concentration of this compound was actually less effective . in general the open samples ( those with the tipsoclmb layer coated on top of a dvd half without any cover ) generated mb only slightly faster than the sandwich structures , indicating that deblocking and oxidation of the lmb is not significantly limited by the transfer of either water or oxygen through an unmetallized 0 . 6 mm polycarbonate layer . rather , the deblocking of the tipsoclmb is likely to be rate - limiting in these systems . the control samples without any added base shows noticeably faster mb generation in room air than in dry air , suggesting that moisture in the air speeds deblocking in this sample . example 9 illustrates how a reactive bonding layer was incorporated into special dvd - 5 design # 2 , thus manufacturing a disc that was normally playable like a dvd - 5 and subsequently became unplayable . incorporating tipsoclmb into a special dvd - 5 design # 2 bonding layer a set of experiments was performed to test whether a formulation containing tipsoclmb , irgacure - 819 , dabco , 1 , 1 , 1 , 3 , 3 , 3 - hexamethyldisilazane ( as a fluid stabilizer ), and sartomer cd - 501 acrylate monomer could be used as a dvd adhesive to produce playable dvds . using the formulation described in example 5 , filtered through a 1 . 0 μm glass syringe filter , the fluid was syringed onto either clear or metallized special dvd - 5 design # 2 halves manufactured as in example 2 . a dvd half disk is centered data side up on the turntable as stated above . the turntable is held stationary while the fluid is dispensed on the data side in a manner by creating drops with a syringe roughly 3 ˜ 5 mm round . these are evenly spaced circularly about a diameter of 30 ˜ 40 mm . the disc to be bonded is then placed data side facing the solution and slightly bowed away from the bottom disc by the edges . the disc will be lowered at an angle until the first contact point between the fluid and top disc occurs . we do not want to place the top disc immediately on the bottom because of entrapped air and subsequent bubbles . therefore , to get a more uniform capillary flow , we can rotate the disc in a clockwise rotation while keeping it slightly bent under light pressure until each of the fluid drops begins to form a capillary bridge ring . once the capillary ring is completed , the top disc can be released and the capillary action will continue . we can wait for the capillary flow to cover the surface , or we can spin the disc at 100 rpm until the material reaches the maximum od diameter . at this point the turntable can be turned up and rotated at about 500 rpm &# 39 ; s for 5 seconds to thin out the adhesive and achieve a resulting 50 μm adhesive films ( determined by profilometry ). this will level the spacer layer ( adhesive layer ) and remove excess material from the od . the disc edge can then be wiped and then the disc uv cured . it is important that prior to curing , the disc halves be aligned as close as possible to avoid center hole misalignment an subsequent play back problems . at this point , the disc is subjected to about 20 ˜ 30 flashes from a norlite 400 xenon flash lamp at its max setting . the time between flashes is dictated by the charging of the flash lamp , but should be sufficient as to not induce added stress from heat generated in the cure ( typically 5 seconds ). this process will yield a clear , uncolored , fully cured acrylate film that plays on the dvd test player . the discs were manufactured under normal ambient conditions , and were subsequently put in a nitrogen box for 3 - 4 days , to remove the oxygen dissolved in the substrates ( which would take an estimated 12 - 20 hours ), and to allow tipsoclmb to unblock into lmb ( which would take 2 - 3 days ). the special dvd - 5 design # 2 discs were subsequently removed from the nitrogen box and were measured for reflectivity at the 650 nm wavelength as a function of time . the discs were clear and playable for 12 - 16 hours after which time they turned dark blue within 24 hours and became unplayable with reflectivities under 2 % at 650 nm . as seen in the dvd family illustration in fig4 , in a dual layer optical disc designed to read multiple layers from one side , the spacer ( bonding ) layer is in the optical path . in the case of dual layer dvds , the given specification for this spacer layer thickness is 0 . 055 +/− 0 . 015 mm . the thickness of the substrate for a dual layer dvd with optical path bonding is typically 0 . 55 mm ˜ 0 . 64 mm . incorporating a reactive compound inhibiting the reading laser in the bonding layer 800 of either type of dual - layer disc would only inhibit the player from reading the l 1 layer 805 , as the bonding layer 800 is not in the optical path for reading the l 0 layer 810 . furthermore , the metal 815 in the l 0 layer 810 might act as a barrier preventing a predetermined stimulus such as moisture or oxygen to permeate to the reactive compound in the bonding layer 800 in a controllable manner . one method around this potential problem would be as follows . typically , when a player or a drive begins reading a disc , it looks for the table of contents or information area in the lead - in area for the l 0 layer 810 ( see fig6 ). when authoring the disc , it is possible to have the l 0 lead - in 820 area contain commands to directly access the l 1 layer 805 . in order to be able to read the l 0 layer 810 to direct the play sequence to the l 1 805 , we would have to metallize the l 0 side 810 . this would then possibly interfere with the reactive adhesive material 800 causing unstable or uncontrolled kinetics of reaction that would be dependent on the permeability of the metal layer . one approach around this would be to change the metallizer masking for the l 0 semi - reflective layer 800 , which is typically run out to 58 mm to 59 mm radius on the disc , to something closer to the lead - in or information data area on the l 0 . to facilitate activation of the reactive material 800 , e . g ., when the activating stimulus is oxygen or moisture that might be prevented from reaching the reactive bonding layer 800 because of the l 0 metal layer 820 , part of the l 0 layer 810 can be masked during metallization , so that part of the reactive layer will be easier to expose to the stimulus and thus the corresponding part of the l 0 layer will be disabled . these discs would have a partially metallized l 0 layer 810 , as illustrated in fig2 . for example , if only the lead - in area or program start portion of the l 0 layer 810 is metallized , the player is able to read the lead - in data , and is able to access the information stored on l 1 layer 805 . as only a small area on the l 0 layer 810 would be metallized , a substantial part of the reactive bonding layer would be in direct contact with the l 0 substrate 810 , which is typically permeable by stimuli such as oxygen or moisture . when the reactive bonding layer responds to the appropriate stimuli and starts interfering with the reading laser , the player is no longer able to access the corresponding part of the l 1 layer 805 . another embodiment of the present invention is utilizing authoring techniques , such as sequencing and branching commands to be executed by the optical media player , to ensure that making a certain part of a disc unplayable will interfere with playing other parts of the disc , or the entire disc . the part of the disc made unplayable for this purpose may be in the single layer of a one - layer disc , or in any of the layers of a multi - layer disc . for example , one embodiment of this invention consists of a dvd - 9 authored so that making a certain part of the l 1 layer unplayable would interfere with playing other parts of the disc , or the entirety of the disc . for example , reading the l 0 layer lead - in area would direct the player to access a part of the l 1 layer that would become unreadable when the reactive layer starts interfering with the reading laser , which would cause the disc to be inoperable . a dvd - 9 disc can be authored so that all or part of the l 1 layer is essential in order to play any information on l 0 and / or l 1 . for example each chapter on the disc can be authored so that it requires reading certain information on l 1 before proceeding . in another embodiment of this invention , activation of the reactive material is facilitated by controlling the deposition of the l 0 layer . for example , fast deposition of a gold or silver or silicon l 0 layer through sputtering is known to result in grainy dendritic formations that are easier to penetrate by oxygen and moisture . also , a thinner l 0 layer can be deposited , which is easier to penetrate by oxygen and moisture . while depositing grainy or thin l 0 layers may be unacceptable for a permanent , archival quality disc , it is often adequate for a limited use , expiring disc . a dvd - 9 with parallel track path encoding can have two distinctly different layers for play back . in the encoding or data mastering process , the lead - in area normally found on the l 0 disc , can have information telling the reading players to read from either or both layers on the disc . therefore , for this example using a reactive bonding material , the reactive layer could prevent play back from the l 1 layer while not affecting the l 0 . for this example corresponding l 0 and l 1 masters were manufactured , and l 0 and l 1 substrates were normally molded and metallized . the dvd halves were bonded as in example 9 above using an adhesive containing the formulation tipsoclmb , irgacure - 819 , dabco , 1 , 1 , 1 , 3 , 3 , 3 - hexamethyldisilazane ( as a fluid stabilizer ), and sartomer cd - 501 acrylate monomer described in example 5 . the solution was filtered through a 1 . 0 - μm glass syringe filter . a dvd half disk is centered data side up on the turntable as stated above . the turntable is held stationary while the fluid is dispensed on the data side in a manner by creating drops with a syringe roughly 3 ˜ 5 mm round . these are evenly spaced circularly about a diameter of 30 ˜ 40 mm . the disc to be bonded is then placed data side facing the solution and slightly bowed away from the bottom disc by the edges . the disc will be lowered at an angle until the first contact point between the fluid and top disc occurs . we do not want to place the top disc immediately on the bottom because of entrapped air and subsequent bubbles . therefore , to get a more uniform capillary flow , we can rotate the disc in a clockwise rotation while keeping it slightly bent under light pressure until each of the fluid drops begins to form a capillary bridge ring . once the capillary ring is completed , the top disc can be released and the capillary action will continue . we can wait for the capillary flow to cover the surface , or we can spin the disc at 100 rpm until the material reaches the maximum od diameter . at this point the turntable can be turned up and rotated at about 500 rpm &# 39 ; s for 5 seconds to thin out the adhesive and achieve a resulting 50 μm adhesive films ( determined by profilometry ). this will level the spacer layer ( adhesive layer ) and remove excess material from the od . the disc edge can then be wiped and then the disc uv cured . it is important that prior to curing , the disc halves be aligned as close as possible to avoid center hole misalignment an subsequent play back problems . at this point , the disc is subjected to about 20 ˜ 30 flashes from a norlite 400 xenon flash lamp at its max setting . the time between flashes is dictated by the charging of the flash lamp , but should be sufficient as to not induce added stress from heat generated in the cure ( typically 5 seconds ). this process will yield a clear , uncolored , fully cured acrylate film that plays on the dvd test player . the discs were manufactured under normal ambient conditions , and were subsequently put in a nitrogen box for 7 days , to remove the oxygen dissolved in the substrates ( which would take an estimated 12 - 20 hours ), and to allow tipsoclmb to unblock into lmb ( which was estimated to take up to 5 - 6 days ). the discs were subsequently removed from the nitrogen box and were normally playable on both the l 0 and l 1 layer for 2 - 3 days on a pioneer player . after 7 days of exposure to ambient oxygen , the discs became unplayable on the l 1 layer , although they would play normally on the l 0 layer . as in example 10 above , dvd - 9 master tapes were generated with the data area being identified on layer l 1 and the l 0 layer serving only to provide the lead - in and subsequent table of contents relating to the disc type and information . during play back , the l 0 lead - in would instruct the disc to read from the l 1 data side . in this case , we would not have to metalize the entire surface of the l 0 layer because there is no information to be read outside of the lead - in area . therefore , dvd - 9 master tapes were produced with lead - in and command information on l 0 and data area on l 1 . typically , the metalizer masking covers areas from 25 mm through 118 mm diameters on both layers . being as the lead - in area data covers the diameters of 25 . 2 mm to a maximum of 48 mm , and the subsequent information area starts at no less than 48 mm diameter , the metalizer masking can be reduced to cover the lead - in only . this would allow a reflective signal to read the lead - in on the l 0 layer and then switch to the l 1 layer for data playback without having to read through additional semi - reflective metal . in this example , we manufactured donut - masking plates that dropped into the metalizer od mask assembly . by registering the masking from the od , we are able to reduce the metalized diameter to an area allowing lead - in playback . we extended the mask just outside of the lead - in 48 mm diameter in order to compensate for eccentricity tolerance with the masking position . additionally , in order to prevent a reflective spike from the transition of clear disc area to metalized disc area when reading the l 1 layer , the edge of the masking was slightly raised above the disc to cause a shadowing or tapered layer uniformity . this would cause a gradual focusing compensation rather than a large “ speed bump ” effect causing its radial noise and focusing error to fall out of specification and perhaps jump track . the resulting dvd - 9 halves were bonded as in example 10 . the dvd - 9s constructed were tested for playability in a pioneer dvd player and in a dvd - rom drive , and were subsequently put in a nitrogen box for 7 days , so that the tipsoclmb would unblock into lmb . the discs were subsequently removed from the nitrogen box and were clear and playable for 12 - 16 hours , and turned dark blue within 24 hours after that , becoming unplayable . the discs were effectively prevented from having information read from either l 0 or l 1 . preferably , the data quality of the disc should remain high for the intended period of use and then decay rapidly resulting in a rapid degradation of the ability to read data off the optical disc . one benefit of this embodiment of the present invention is that for a broad class of stimuli , such as those requiring diffusion of a substance through a barrier layer , incorporating the reactive material in an interstitial layer results in substantial advantages regarding the timing characteristics of the reaction . one method of achieving the above mentioned desirable timing characteristics is to use a reactive interstitial material between the disc substrates , as described earlier , which reacts with a substance that needs to diffuse through the substrates of the disc . for example , if the reactive material is sensitive to oxygen , there will be an extended period in which there will be no reaction while the oxygen diffuses through the disc substrates . once oxygen reaches the reactive layer , the resulting reaction can be fast , resulting in rapid expiration of the disc . when oxygen is used as the diffusing substance , it may be necessary to remove oxygen that dissolves in the disc during the different stages of its manufacture . this can be done , for example , by storing the discs in a vacuum or in an oxygen free environment for an appropriate period of time . it has been established theoretically and experimentally that 24 hours is an adequate period to extricate oxygen dissolved in a 0 . 6 mm thick polycarbonate disc substrate . alternatively , if a blocked reactive material is used as described earlier , an oxygen scavenging material , such as iron or an organometallic compound , can be used to extricate oxygen from the optical disc before the blocked reactive material unblocks . this method has several manufacturing advantages ; for example , it can avoid oxygen extrication during manufacturing of the disc by including the oxygen scavenging material in the packaging of the disc , which allows the extrication of the oxygen to take place after the disc is manufactured and packaged . another means for controlling the timing of the expiration of the disc is to include in or adjacent to the reactive layer a finite , controlled quantity of an appropriate protective substance , such as an antioxidant in the case that the reactive layer reacts with oxygen . the protective substance would prevent the reactions that cause the disc to expire until such time as the anti - oxidant was consumed , at which time the disc would rapidly degrade and become unplayable . for example , an organometallic compound that reacts with oxygen can be packaged with the disc to protect the disc from oxidation while in the package . alternatively , the organometallic compound can be incorporated into the substrate , thus continuing to protect the metal layer for a period of time after the package has been opened . depletion of a protective substance could be combined with diffusion of the triggering substance through the substrate of the disc , to result in longer delays before the disc expires , or to enable finer control of the characteristics of the expiration process , such as the steepness of reflectivity degradation . alternatively , the protective substance may be a reducing agent which may be incorporated into the reactive bonding layer itself . in an experiment in which the concentration of tlmb was also varied and shown to have an effect , the play time was shown to be more greatly affected by varying the amount of stannous ethylhexanoate reducing agent ( see table i ). dvd - 5 discs were made using a tipsoclmb - containing adhesive formulation , and deblocked in an oxygen - free atmosphere for 48 hours at 60 ° c . at that time the discs were exposed to ambient room air and the rate of methylene blue color development was quantified with an x - rite reflection densitometer . the short play time was chosen to be the time at which the cyan density increased by 0 . 35 , which roughly corresponds to a playability cutoff at 45 % reflectance as typified by a low quality dvd player . the long play time was chosen to be the time at which the cyan density increased by 0 . 85 , which roughly corresponds to a playability cutoff at 10 % reflectance as typified by a high quality dvd player . the most likely mechanism for this extended play is reduction of the initially formed methylene blue dye back to the leuco form until most of the reducing agent is consumed . alternate mechanisms , such as the stannous compound acting as a primary oxygen scavenger to consume oxygen before the leuco dye is affected , are also possible . the mobility within the cured matrix is expected to have a significant effect upon the reduction rate ; indeed , the calculated glass transition temperature ( tg ) of the monomers used in this example is − 34 ° c . in such a soft matrix , adequate molecular mobility should exist to allow molecular contact of reducing agent and dye molecules . alternate reducing agents might include other sn ( ii ) compounds which would be soluble in the uv cure formulation , such as acetylacetonate chelates , fatty alpha - aminoacid chelates and salts ; soluble iron ( ii ) compounds , such as fatty carboxylates and chelates such as acetylacetonates ; ascorbic acid and its derivatives such as ascorbyl palmitate ; hydroquinones , such as 2 , 5 - di - tert - amylhydroquinone ; alkylhydroxylamines ; hydrazines ; dithionates with a solubilizing counterion ; reducing saccharides such as glucose ; alpha - hydroxyketones , such as acetol ; appropriately substituted boron and silicon hydrides . although many of these materials are difficultly soluble in current active adhesive formulations , a more expeditious choice of monomers and oligimers might allow the use of one of these alternate reducing agents while still providing good adhesive and dye stabilization properties . future generations of optical discs and players are typically developed to offer increased performance for consumers and other users of the technology . for example , dvds offer increased storage capacity compared to cds , and the next generation of “ blue laser ” dvds will offer improved capacity compared to today &# 39 ; s dvds . subsequent generations of optical storage media , such as the “ dvr ” format currently under development , will have even greater capacity and performance . optical media players are typically engineered with the ability to play previous generations of discs . for example , while cd players employ a laser with a wavelength of 780 nanometers to read cds , dvd players typically employ their reading laser with a wavelength of 650 nanometers to read cd discs . the next generation dvds (“ blue laser dvds ”) is designed to be read with a laser with a wavelength of 450 - 460 nanometers ; the “ dvr ” format will use lasers emitting around 405 nm . future generation players are likely to be able to read current dvds with their 450 - 460 nanometer or 405 nanometer lasers . dyes used to inhibit the reading laser in current optical disc players are typically designed to interfere with the reading laser employed by these players ; such dyes , however , may not interfere with the reading laser future players , which is likely to have a shorter wavelength . the implication is that expired discs , even though they may not play in the current generation of players , they may become playable when future generation players become available . dyes used to inhibit the reading laser in current dvd players are typically designed to interfere with a 650 nanometer reading laser ; such dyes , however , may not interfere with a reading laser in the 450 - 460 nanometer range . for example , methylene blue , which is one of the read inhibit dyes proposed in smith et al , while strongly absorbent in the 650 nanometer wavelength , it is essentially transparent in the 450 - 460 nanometer range ( see fig1 ). the implication is that expired dvds may play in blue laser dvd players . another embodiment of the present invention is an optical disc that will not play in future generation players , thus preventing an expired disc from becoming playable when future generation players ( e . g ., blue laser dvd players ) become available . this can be accomplished by incorporating in the optical path of the disc a selectively interfering layer that will interfere with the reading laser of future generation players , and thus will inhibit reading of the disc in such players . such a layer can be designed by incorporating a dye or pigment that does not interfere with the reading laser in a certain type of players , but does interfere with the reading laser in other types of players ( or will change to become interfering in response to a predetermined stimulus ). for example , acridine yellow [ 135 - 49 - 9 ], is essentially transparent at the 635 - 650 nanometer wavelength but strongly absorbs at the 450 - 460 and 405 nanometer wavelengths ( absorption max in ethanol at 462 nm , molar absorptivity = 37 , 000 m − 1 cm − 1 ). alternatively 9 , 10 - bis ( phenylethynyl ) anthracene [ 10075 - 85 - 1 ] also does not absorb at all in the 635 - 650 nanometer range , but is strongly absorbent in the 450 - 460 and 405 nanometer range ( absorbance max 455 nm in cyclohexane , molar absorptivity 33 , 000 m − 1 cm − 1 ). other classes of dyes and pigments that can be used for blocking blue laser light ( at either 450 - 460 or 405 nm ) include aromatic hydrocarbons , azo dyes , cyanines , polymethines , carotinoids , hemicyanines ,, styryls , quinaldines , coumarins , di - and triarylmethines , anthraquinones , nitro and nitrosos . as mentioned above , methylene blue is essentially transparent at the 450 - 460 nanometer wavelengths , but strongly absorbs at the 635 - 650 nanometer range . in one embodiment of the current invention , the selectively interfering layer is a dedicated layer in the optical path of the reading laser . in another embodiment , which is likely to be the preferred embodiment because it does not introduce an additional design element for the optical disc , the selectively interfering layer is combined with another element of the disc , such as the substrate or the reactive layer . for example , this could be accomplished by mixing an appropriate dye or pigment , such as acridine yellow [ 135 - 49 - 9 ] or 9 , 10 - bis ( phenylethynyl ) anthracene [ 10075 - 85 - 1 ], with the polycarbonate or other polymer used to mold the substrate of the disc , or with the reactive layer in an expiring disc , such as the bonding layer in the special dvd - 5 designs described earlier . another embodiment of the present invention is combining the mechanism ( s ) that prevent reading of the optical disc by inhibiting the reading laser with additional mechanism ( s ) for preventing recovery of the information encoded in the data structures on the disc . these additional mechanism ( s ) can be designed with less accurate control of the timing of their activation than the mechanism ( s ) that work by inhibiting the reading laser . thus it may be desirable to combine the mechanism that controls expiration of the optical disc by interfering with the reading laser with additional mechanism ( s ) that permanently prevent the recovery of the data on the optical disc . for example , a disc may become unplayable by transitioning a layer in the optical path from transparent to opaque in a controlled time period , for example approximately 24 hours after a predetermined stimulus , such as removing the disc from its packaging . in addition , a secondary mechanism could corrode the metal layer on the disc , such mechanism acting over a longer period of time , such as 1 - 2 weeks , and being triggered by the same or a different stimulus . additional mechanisms may also be employed , such as an additive that degrades the polycarbonate material from which the disc is composed , which process can be triggered by the same stimulus ( such as exposure to ambient air ), or a different stimulus ( such as the centrifugal forces generated when a disc is played in a cd or dvd player ). other triggering stimuli for these backup mechanisms can include various constituents of air , light , physical motion , and time from manufacturing or packaging . many other mechanisms are possible . one method of accomplishing this is to deposit a layer of metallic silver separated from the information bearing aluminum layer by a material incorporated for this purpose , or by an existing material , such as the bonding layer or one of the substrates of the optical disc . this silver layer can be above or below the aluminum layer , and if it is below ( and thus in the optical path of the reading laser ) it needs to be sufficiently transparent initially so that the reading laser can read the information on the aluminum layer . in one embodiment of the invention , a dvd - 9 disc is manufactured with a reactive bonding layer consisting of a material with appropriate dielectric properties , and with appropriate selection of metals for l 0 and l 1 . for example , l 0 can be made of silver and l 1 can be made of aluminum . when a silver layer and an aluminum layer are separated by an appropriate dielectric material , then upon exposure to oxygen the silver serves as a cathode , on which o 2 is reduced , and aluminum serves as an anode . corrosion is fast only if a short develops between the silver and the aluminum layers . the development of the short results from the growth of a silver dendrite through the separating material . to grow the dendrite through the separating material it is desirable to use a material that has some ionic conductivity . several likely separating materials consist of or contain polyacrylate . if the polyacrylate is slightly hydrolyzed , or if it is , for example , a 2 - hydroxyethylacrylate copolymer , there will be some ionic conductivity . preferred are co - polymers of poly ( acrylonitrile ), or of poly ( 4 - vinylpyridine ), or of poly ( 1 - vinylimidazole ). all of these should conduct silver , copper or thallium ions ( ag + cu + or tl + ). thallium is less preferred due to its toxicity . ag + is reduced by aluminum , which is oxidized ( if ag + is mobile in the lacquer , which is designed to conduct ag + ) a silver dendrite starts growing from the aluminum to the silver . when the two layers are shorted , the “ switch ” between a battery &# 39 ; s ( al ) anode and ( ag ) cathode is closed . corrosion is rapid and catastrophic . one skilled in the art will recognize that other similar metals may be substituted for al and ag in this example . alternatively , other ways of permanently corroding data layers via the reactive layer can be employed . for example , certain embodiments of this invention may have a bonding layer that promotes the corrosion of the reflective metal layer or may involve the diffusion of some substance from the bonding layer to the reflective layer ( s ). in other embodiments , the additional mechanisms will not be part of the bonding material . for example , a precursor of a corrosive substance may be deposited adjacent to the metal layer . when oxygen or some other appropriate substance diffuses through the substrate and reaches the corrosive precursor , a reaction could be initiated that results in producing a corrosive substance that over a period of time permanently destroys the data structures on the disc . alternatively , the material in the substrate of the disc , such as polycarbonate , could be engineered so that it degrades over a period of time , thus making the disc unusable . such substances and reactions are known to the skilled in the art . another composition that performs a similar function is one in which the substrate itself is modified over time . the modification of the substrate could cause it to change its optical qualities , thereby degrading the signal reaching the reader . these optical qualities could include its index of refraction or its transparency . moreover , the modification of the substrate could cause the underlying metal layer to change its optical properties , as described above . in this way , a time - sensitive substrate and / or lacquer could be combined with a reflective layer that becomes non - reflective . the transparency of a polymer film can be changed by any of the following : reaction of the film with water ; reaction of the film with oxygen ; or crystallization of the polymer , meaning increased alignment of polymer molecules in the film . as an example , a substrate could be chosen that is changed by components in air such as oxygen or water . for example , oxygen could oxidize the substrate , causing a change in its transparency or its index of refraction . alternatively , the substrate could be designed to absorb water in the air , causing it to swell and change its optical properties . another example is that the substrate could change its permeability to oxygen over time , thereby permitting the oxidation of the metallic layer . in the later case , the overall time sensitivity of the optical media could be a function of the properties of both the substrate and / or lacquer and the reflective layer . the substrate or the metallic layer could also be made sensitive to specific wavelengths of light . exposure to these wavelengths would cause a change in the optical qualities of the layer , thereby degrading the signal reaching the reader . examples include photodepolymerization of the substrate ; photogeneration of acid ; photogeneration of singlet oxygen ; and unzipping of the polymers ( e . g ., fissure of cross linking hydrogen bonds ). incorporation of light - activated catalysts into the substrate or the metallic layer can assist in this process . accordingly , the present invention has been described at some degree of particularity directed to the exemplary embodiments of the present invention . it should be appreciated , though , that the present invention is defined by the following claims construed in light of the prior art so that modifications or changes may be made to the exemplary embodiments of the present invention without departing from the inventive concepts contained herein . | 6 |
in general , this invention comprises materials and methods for improving the adhesive strength of adhesives , coatings and composites to biological substrates . the terms &# 34 ; adhesives , coatings and composites &# 34 ; are taken to mean any composition that can be stored in either a single or multi - component form , is used to adhere , cover , adorn , replace , or otherwise protect a surface , and can be polymerized by one or more of a variety of free radical - type initiation processes . examples of such materials are ( 1 ) two - component ( powder and liquid ) artificial fingernail prosthesis formulations , which polymerize through a peroxide / tertiary amine type initiation ; ( 2 ) one component , glass / resin dental compositions , which are polymerized by actinic ( visible and / or ultraviolet ) light activation of a photoinitiator , together with an optional tertiary amine ; and ( 3 ) ultraviolet and visible light cured , unfilled or filled , coatings and adhesives used to attach and / or cover natural or artificial fingernails ; similar compositions are utilized for the reparation of livestock hooves that have become split or cracked . although not limited to the above types of adhesives , coatings and composites , the three categories listed are those compositions that show marked improvement in adhesive strength through the practice of the present invention . the most preferred inventive method for pretreating the surfaces to be adhered to comprises contacting the surface with a non - aqueous solution of a methacryloyloxyethyl maleate ( herein referred to as mahema ), and allowing the non - aqueous solvent to completely evaporate . then , the adhesive , coating or composite is allowed to contact the treated surface and polymerized through free radical mechanisms . the preferred concentration of mahema in the non - aqueous solvent is from about one percent to about 30 percent , and the most preferred concentration is about 5 to 20 percent . differences in the porosity and surface free energy of the substrate will have a bearing on the optimal mahema concentration for each individual surface to be &# 34 ; primed &# 34 ;. in general , following the complete evaporation of the carrier solvent , the treated substrate should appear relatively dry . treated surfaces that appear shiny and wet tend to have a thick layer of residual mahema , which can act as a boundary layer and lead to decreased adhesive strength . mahema was prepared by heating together 1 mole of maleic anhydride and in slight excess of 1 mole of 2 - hydroxyethyl methacrylate together with about 200 ppm of the monomethyl ether of hydroquinone as a stabilizer against premature polymerization . in addition 500 ppm of triethylamine was included in the reaction mixture as a catalyst for the addition reaction . upon cooling , a slightly yellow , moderately viscous liquid is obtained , having a refractive index of 1 . 484 ( at 20 degrees c .) and a brookfield viscosity ( at 23 degrees c .) of 470 cps . this liquid was stored in amber glass bottles until further use . the structure of mahema is as follows : ## str3 ## care must be taken during the heating process above to keep the reaction process at or below about 80 - 90 degrees c . to avoid premature polymerization due to the methacrylate group . alternatively , mahema may be synthesized in the solvent carrier to be used in the practice of this invention . for example , the properly calculated amounts of maleic anhydride and 2 - hydroxyethyl methacrylate may be added to ethyl acetate to provide the desired final concentration of mahema in situ . attention must be paid to this method of synthesizing mahema , in that certain solvents , such as isopropyl alcohol , can compete with the 2 - hydroxyethyl methacrylate for addition to the anhydride group of maleic anhydride . proteinaceous substrates were tested to demonstrate the adhesive strength improvement caused by the adhesion promoting compositions of this invention . the differences in the adhesive strength provided by pretreating the substrate with the present invention relative to prior art systems are shown . solutions ranging from one to 30 percent mahema in anhydrous ethyl acetate were prepared and packaged in amber glass bottles with a polyethylene brush cap for application to the surfaces to be tested . in order to test the extent of adhesion improvement by the mahema solutions on keratinaceous substrates , cattle hooves were chosen due to their availability and ease of handling during tensile adhesive strength testing . flat sections of cattle hooves were prepared with the hoof fibers running parallel to the surface to be tested . the hoof surface was then abraded with a fine grit sandpaper and subsequently rinsed with water and allowed to dry thoroughly . the abraded and rinsed hoof surface was then treated with the mahema solution , being brushed on and allowing the ethyl acetate to evaporate completely . the surface of the hoof at this point appeared dry and slightly glossy . a stainless steel cylinder with a tapered bore and an access port was then contacted to the treated hoof surface perpendicularly . the following formulation was mixed , poured into the testing cylinder through the access port , and allowed to polymerize . this assembly was allowed to age at room temperature for 24 hours and subsequently tested for tensile adhesive strength in an instron tensile strength tester model 1011 ( instron corp , quincy , ma ) at a crosshead speed of 0 . 1 mm / minute . ratio of liquid a : powder b is approximately 1 : 3 in the final mixture . ______________________________________ no . mahema % avg . adh . * adh . range ** measurements______________________________________0 240 110 - 330 51 570 400 - 670 52 720 460 - 790 53 780 600 - 840 54 800 690 - 880 55 870 810 - 910 58 080 940 - 1170 510 1410 1250 - 1500 513 1840 1610 - 1990 516 2320 1980 - 2500 520 2450 2020 - 2610 525 2030 1880 - 2150 530 1490 1200 - 1780 5______________________________________ * average adhesion in psi ( lbs per sq . inch ) ** adhesion range in psi ( lbs per sq . inch ) the adhesion promoting capabilities of the maleic anhydride addition reaction products of this invention were compared to those of other known and / or potential adhesion promoters . all compounds tested had at least one carboxylic group and at least one unsaturated group capable of participating in free radical type polymerizations . each promoter is listed below , together with it &# 39 ; s concentration , solvent ( if any ), substrate appearance , and tensile adhesive strength as described in example 1 . ______________________________________adhesion promoter conc . solvent avg . adh . sup . 3______________________________________methacrylic acid 20 % ethyl acetate 680methacrylic acid 100 % none 1250acrylic acid 20 % ethyl acetate 820acrylic acid 100 % none 1500mahema . sup . 4 20 % ethyl acetate 2510pmdm . sup . 1 5 % acetone 1110pmdm . sup . 1 20 % acetone 730maleic acid 20 % ethyl acetate 300mahpma . sup . 2 , 4 20 % ethyl acetate 2480______________________________________ . sup . 1 pyromellitic dianhydride / 2hydroxyethyl methacrylate adduct ( ref . patent no . 4 , 521 , 550 ) . sup . 2 maleic anhydride / 2hydroxypropyl methacrylate adduct . sup . 3 average adhesion in psi ( lbs per sq . inch ) . sup . 4 invented compositions it is anticipated that just about any substrate comprised entirely or in part of protein will be adhered to better by pretreatment of the substrate surface with the compositions of this invention . the preceding disclosure has demonstrated the improved adhesion of a free - radical initiated composition to keratin substrates treated with mahema and other cyclic anhydride addition reaction products as previously described . it is believed that substrates such as fingernails , hooves , bone , ivory , leather , dentin , enamel , and other partially or wholly proteinaceous materials will show the adhesion - promoted benefits of the present inventive compositions . | 0 |
the present invention may be a system , a method , and / or a computer program product . the computer program product may include a computer readable storage medium ( or media ) having computer readable program instructions thereon for causing a processor to carry out aspects of the present invention . the computer readable storage medium can be a tangible device that can retain and store instructions for use by an instruction execution device . the computer readable storage medium may be , for example , but is not limited to , an electronic storage device , a magnetic storage device , an optical storage device , an electromagnetic storage device , a semiconductor storage device , or any suitable combination of the foregoing . a non - exhaustive list of more specific examples of the computer readable storage medium includes the following : a portable computer diskette , a hard disk , a random access memory ( ram ), a read - only memory ( rom ), an erasable programmable read - only memory ( eprom or flash memory ), a static random access memory ( sram ), a portable compact disc read - only memory ( cd - rom ), a digital versatile disk ( dvd ), a memory stick , a floppy disk , a mechanically encoded device such as punch - cards or raised structures in a groove having instructions recorded thereon , and any suitable combination of the foregoing . a computer readable storage medium , as used herein , is not to be construed as being transitory signals per se , such as radio waves or other freely propagating electromagnetic waves , electromagnetic waves propagating through a waveguide or other transmission media ( e . g ., light pulses passing through a fiber - optic cable ), or electrical signals transmitted through a wire . computer readable program instructions described herein can be downloaded to respective computing / processing devices from a computer readable storage medium or to an external computer or external storage device via a network , for example , the internet , a local area network , a wide area network and / or a wireless network . the network may comprise copper transmission cables , optical transmission fibers , wireless transmission , routers , firewalls , switches , gateway computers and / or edge servers . a network adapter card or network interface in each computing / processing device receives computer readable program instructions from the network and forwards the computer readable program instructions for storage in a computer readable storage medium within the respective computing / processing device . computer readable program instructions for carrying out operations of the present invention may be assembler instructions , instruction - set - architecture ( isa ) instructions , machine instructions , machine dependent instructions , microcode , firmware instructions , state - setting data , or either source code or object code written in any combination of one or more programming languages , including an object oriented programming language such as smalltalk , c ++ or the like , and conventional procedural programming languages , such as the “ c ” programming language or similar programming languages . the computer readable program instructions may execute entirely on the user &# 39 ; s computer , partly on the user &# 39 ; s computer , as a stand - alone software package , partly on the user &# 39 ; s computer and partly on a remote computer or entirely on the remote computer or server . in the latter scenario , the remote computer may be connected to the user &# 39 ; s computer through any type of network , including a local area network ( lan ) or a wide area network ( wan ), or the connection may be made to an external computer ( for example , through the internet using an internet service provider ). in some embodiments , electronic circuitry including , for example , programmable logic circuitry , field - programmable gate arrays ( fpga ), or programmable logic arrays ( pla ) may execute the computer readable program instructions by utilizing state information of the computer readable program instructions to personalize the electronic circuitry , in order to perform aspects of the present invention . aspects of the present invention are described herein with reference to flowchart illustrations and / or block diagrams of methods , apparatus ( systems ), and computer program products according to embodiments of the invention . it will be understood that each block of the flowchart illustrations and / or block diagrams , and combinations of blocks in the flowchart illustrations and / or block diagrams , can be implemented by computer readable program instructions . these computer readable program instructions may be provided to a processor of a general purpose computer , special purpose computer , or other programmable data processing apparatus to produce a machine , such that the instructions , which execute via the processor of the computer or other programmable data processing apparatus , create means for implementing the functions / acts specified in the flowchart and / or block diagram block or blocks . these computer readable program instructions may also be stored in a computer readable storage medium that can direct a computer , a programmable data processing apparatus , and / or other devices to function in a particular manner , such that the computer readable storage medium having instructions stored therein comprises an article of manufacture including instructions which implement aspects of the function / act specified in the flowchart and / or block diagram block or blocks . the computer readable program instructions may also be loaded onto a computer , other programmable data processing apparatus , or other device to cause a series of operational steps to be performed on the computer , other programmable apparatus or other device to produce a computer implemented process , such that the instructions which execute on the computer , other programmable apparatus , or other device implement the functions / acts specified in the flowchart and / or block diagram block or blocks . the flowchart and block diagrams in the figures illustrate the architecture , functionality , and operation of possible implementations of systems , methods , and computer program products according to various embodiments of the present invention . in this regard , each block in the flowchart or block diagrams may represent a module , segment , or portion of instructions , which comprises one or more executable instructions for implementing the specified logical function ( s ). in some alternative implementations , the functions noted in the block may occur out of the order noted in the figures . for example , two blocks shown in succession may , in fact , be executed substantially concurrently , or the blocks may sometimes be executed in the reverse order , depending upon the functionality involved . it will also be noted that each block of the block diagrams and / or flowchart illustration , and combinations of blocks in the block diagrams and / or flowchart illustration , can be implemented by special purpose hardware - based systems that perform the specified functions or acts or carry out combinations of special purpose hardware and computer instructions . the programs described herein are identified based upon the application for which they are implemented in a specific embodiment of the invention . however , it should be appreciated that any particular program nomenclature herein is used merely for convenience , and thus the invention should not be limited to use solely in any specific application identified and / or implied by such nomenclature . it is to be noted that the term ( s ) “ smalltalk ” and the like may be subject to trademark rights in various jurisdictions throughout the world and are used here only in reference to the products or services properly denominated by the marks to the extent that such trademark rights may exist . the present invention will now be described in detail with reference to the figures . fig1 illustrates a distributed data processing system , generally designated 100 , according to one embodiment of the present invention . in the illustrated embodiment , distributed data processing system 100 comprises computing device 101 and server computers 102 , 120 , and 122 interconnected through network 103 . computing device 101 may be any electronic device or computing system capable of receiving input from a user , executing program instructions , and communicating with another computer through a network . in a preferred embodiment , computing device 101 is a mobile computing device , such as a personal digital assistant or smart phone , and is wirelessly connected to network 103 by wi - fi or cellular technology . computing device 101 includes message interpreter 104 and query unfolding program 108 . embodiments of the present invention recognize that using a third party to interpret a request and write a syntactically correct query can increase cost and decrease efficiency . embodiments of the present invention further recognize that a report can be quite comprehensive , and running a full report for one small piece of information is often inefficient . additionally , a report may not exist that returns the desired information or an individual may simply not have access to such reports . as such , embodiments of the present invention provide a method , program product , and system for composing or receiving a user or high level query or request for data in an improper form and , utilizing stored query templates and known terms , converting ( unfolding ) the user query into a query understandable by a computer system . towards that end , computing device 101 may execute message interpreter 104 , which is a routine or program that takes the user query and fits it to the nearest query template from a list of known query templates 106 . the query , now in a template format , is passed to query unfolding program 108 which examines all terms that are not predefined from the template and determines whether these are known terms , for example by comparing them to terms in business glossary 110 . business glossary 110 may associate each known term to one or more business definitions ( including attribute names of stored data ), business rules ( e . g ., constraints limiting sought attributes , rules of structure and syntax for a query , etc . ), and locations ( e . g ., proper databases , servers , etc .). appropriate rules , definitions , and / or locations may be substituted and / or added into the query for the associated term . the unfolded query is subsequently submitted to the appropriate server computer as determined by determined location information , here depicted as server computer 102 . server computer 102 may be , for example , a server computer system such as a management server , a web server , or any other electronic device or computing system capable of receiving and sending data and executing program instructions . alternatively , server computer 102 may represent a computing system utilizing clustered computers and components to act as a single pool of seamless resources when accessed through network 103 . this is a common implementation for data centers and cloud computing applications . in one embodiment , the unfolded query received by server computer 102 , is now in an understandable format for the server computer , and the server computer merely processes the query and returns results . however , embodiments of the present invention recognize that storage capacity and other resources on computing device 101 may be limited , especially when compared to the resources on server computer 102 . as such , in a preferred embodiment , the unfolded query received by server computer 102 , though in a format that is nearer to a syntactically correct query , is further unfolded or expanded on server computer 102 . in the depicted example , a second instance of query unfolding program 108 operates on server computer 102 , using a local , and perhaps more comprehensive , business glossary 112 . again appropriate associations discovered in the business glossary are substituted into the query . the resulting query can now be executed , and is passed to query handler 114 , which is a routine or program that processes queries , to identify target repositories , databases , etc . ( e . g ., storage locations 116 ) and perform the query . the results may be processed by result handler 118 , which may send the results to computing device 101 , or alternatively , may forward the results to an interested third party ( e . g ., a client requesting the data ). a person of ordinary skill in the art will recognize that in alternate embodiments , the determined location information on computing device 101 may indicate that the unfolded query should be sent to multiple server computers , e . g ., server computers 102 , 120 , and 122 . similarly , based on the involved data storage details , the initial high level query or request may be split into multiple queries and submitted to different servers for processing . results received from result handler 118 on server computer 102 and corresponding result handler functionalities on server computers 120 and 122 would be compiled and presented to a user by a result handling functionality ( not depicted ) on computing device 101 . network 103 may include connections , such as wire , wireless communication links , or fiber optic cables . in the depicted example , network 103 is the internet representing a worldwide collection of networks and gateways that use the transmission control protocol / internet protocol suite of protocols to communicate with one another . network 103 may also be implemented as a number of different types of networks , such as an intranet , a local area network ( lan ), or a wide area network ( wan ). computing device 101 and server computer 102 each maintain respective system components . exemplary components for these systems are illustrated in fig4 . fig2 is a flowchart depicting the operational steps of message interpreter 104 for fitting a natural language query to a known query template . message interpreter 104 begins by receiving text or a message intended as a query ( step 202 ). in one embodiment , message interpreter 104 may receive the text directly from a user of computing device 101 . in another embodiment , computing device 101 may receive a message from a third party and direct the message to message interpreter 104 . for example , the user of computing device 101 may have a client that requests information related to the user &# 39 ; s business . where computing device 101 is a smart phone , the client request may come in the form of a text message , a voice message , or even during a phone conversation . a text message can be sent directly to message interpreter 104 . alternatively , a voice message or recorded conversation can be converted to text using known speech recognition programs , and the converted text can be sent to message interpreter 104 . subsequent to receiving pertinent text , message interpreter 104 searches the text for key words related to queries ( step 204 ). as a threshold matter , in one embodiment , message interpreter 104 determines whether the received text or message is meant to be a query at all . in one exemplary implementation , the text of a message is searched for key words indicative of a query ( e . g ., “ provide ,” “ please provide ,” “ i need ,” “ send me ,” etc .). if it is determined that the text is a query , message interpreter 104 may search for words and / or phrases within the text that match words and / or phrases ( or their equivalents ) found in a list of query templates . for example , one query template might read : “ select & lt ; attribute & gt ; from & lt ; location & gt ;* where & lt ; constraints & gt ;* and & lt ; constraints & gt ;* and & lt ; constraints & gt ;.” the “*” represents optional components of the query that may be filled . a more basic template might look like : “ provide & lt ; attribute & gt ; of & lt ; attribute & gt ; in & lt ; attribute & gt ;.” a series of such templates may exist and each of the key words ( query words ) and their equivalents may be searched for . a query word like “ select ” may have a list of equivalent words such as “ provide ,” “ get ,” “ send ,” etc . “ from ” might have the equivalent “ of .” “ in ” might have defined equivalents “ between ,” “ within ,” “ from & lt ; date & gt ; to & lt ; date & gt ;,” etc . in one embodiment , a “& lt ; constraint & gt ;” marker might be associated with query words that indicate that the constraint should be replaced by the word / phrase that follows the word . for example , “ where ” might be a query word defined as a known constraint limitation . if “ where ” is found in text , the word or phrase following “ where ” may be substituted into a & lt ; constraint & gt ; placeholder . similarly , “ in ” might indicate that the subsequent term should be substituted into a & lt ; constraint & gt ; placeholder . query templates may be predefined in the system or may be created by a user of the system to match the specific requirements of the user &# 39 ; s organization . message interpreter 104 matches the text to the nearest query template from the list of query templates ( step 206 ) and formats the text to fit the query template ( step 208 ). for example , terms can be replaced with equivalent terms from the query template and clauses may be rearranged to follow a specific order . take for example , the text “ provide top 3 high value customers of abc_bank in first quarter .” the nearest query template may be “ select & lt ; attribute & gt ; from & lt ; location & gt ;* where & lt ; constraints & gt ;* and & lt ; constraints & gt ;* and & lt ; constraint & gt ;”. subsequent to fitting the query to the query template , the query reads : “ select top 3 high value customers from abc bank * where & lt ; constraints & gt ;* and & lt ; constraints & gt ; and in first quarter ” ( with “ in first quarter ” replacing one of the optional & lt ; constraints & gt ;). the query , now formed to the nearest template , may be forwarded to query unfolding program 108 . in another embodiment , to form the initial user query , when the user is composing the query , the user may be presented with a plurality of query templates from which he can compose the query . in such a manner , the user query is already formed to a query template and may be forwarded to query unfolding program 108 . fig3 depicts the operational steps of query unfolding program 108 for building into the query accurate terms , constraints , and locations , in accordance with an illustrative embodiment . in an exemplary embodiment , query unfolding program 108 receives the text / query in the format of a query template ( step 302 ). query unfolding program 108 moves to and examines the first word or phrase of the query ( step 304 ) and determines whether the word or phrase is provided by , or part of , the original query template ( decision 306 ). for example , the words “ select ,” “ get ,” “ move ,” “ from ,” etc . may be terms specific to a query template with predefined actions or associations already defined for such terms . if the word is provided by the template ( yes branch of decision 306 ), query unfolding program 108 skips the word or phrase and moves to the next word or phrase ( step 307 ). if the word or phrase is not a predefined term from a query template ( no branch of decision 306 ), query unfolding program 108 determines whether the word or phrase is located in the business glossary , e . g ., business glossary 110 or business glossary 112 ( decision 308 ). the business glossary contains known business terms and corresponding definitions , rules , and / or locations . for example , the business glossary can store business vocabulary and associations . within the business glossary , categories and terms can be defined , as well as custom attributes and values . a person of ordinary skill in the art will understand that while in one embodiment all vocabulary and associations may be stored in a single database or repository , in other embodiments , terms may be linked to appropriate associations in other databases . in an exemplary embodiment , the business glossary connects business glossary terms to individual instances of metadata called “ information assets ,” or “ assets .” an information asset is a piece of information that is of value to an organization and can have relationships , dependencies , or both with other information assets . one example of an asset is an implemented data resource such as a database table . hence , a term in the business glossary may be linked to a specific attribute value found in a specific database table . in this manner , business terms found in the business glossary can indicate attribute names and locations , constraints ( e . g ., filters and other limiting clauses ), organizational rules , and other pertinent information and definitions . in one embodiment , the business glossary organizes metadata or information assets into categories corresponding to specific terms . the corresponding terms can relate to the assets that are stored in a metadata repository or to external assets according to the standards and practices of an enterprise . words or phrases captured by query unfolding program 108 can be searched for in the business glossary for information such as a category corresponding to the term , context , status , abbreviations , related terms , synonyms , assigned assets , and other attributes . if query unfolding program 108 does not locate the word or phrase in the business glossary ( no branch of decision 308 ), query unfolding program 108 moves to the next word or phrase ( step 307 ). alternatively , if query unfolding program does locate the word or phrase in the business glossary ( yes branch of decision 308 ), query unfolding program 108 replaces the word or phrase with any applicable corresponding definition , rule , and / or location ( step 310 ). query unfolding program 108 may add in additional constraints or reorganize the query based on discovered rules . in some embodiments , different rules may apply depending on the query template used . query unfolding program 108 determines whether there are more words or phrases ( decision 312 ) and if there are , moves to the next word or phrase ( step 307 ). if there are no more words or phrases , query unfolding program 108 finishes constructing the query ( step 314 ), for example , by completing any remaining reorganization required by business rules or removing any unfilled optional terms from the query , and submits the query ( step 316 ). if query unfolding program 108 is an instance running on a client device such as computing device 101 , the query is submitted to the applicable server computer ( or computers ) such as server computer 102 . at server computer 102 , if the query is complete , server computer 102 may run the query and submit the results . if the query is not complete , server computer 102 may run its own instance of query unfolding program 108 utilizing a different and / or larger business glossary , e . g ., business glossary 112 . take for example the first examplary query from above : “ provide top 3 high value customers of abc_bank in first quarter .” the nearest query template was “ select & lt ; attribute & gt ; from & lt ; location & gt ;* where & lt ; constraints & gt ;* and & lt ; constraints & gt ;* and & lt ; constraints & gt ;,” which computing device 101 translated to “ select top 3 high value customers from abc bank * where & lt ; constraints & gt ;* and & lt ; constraints & gt ;* and in first quarter .” as depicted , the query words designated with a “*” are optional and may still be filled if subsequently discovered rules supply applicable terms . “ select ” is a word from the query template and in this example is ignored . in another embodiment , all words and phrases are searched for in the business glossary including query words , which would either not be found or would be listed as a query verb and remain unchanged . query unfolding program 108 on computing device 101 moves to the next word or phrase . for discussion purposes , query unfolding program 108 does not locate “ top 3 ” and leaves it unchanged . query unfolding program 108 locates the term “ high value customer ” in the business glossary in an attributes category with “ high value customer ” defined as a customer detail (“ cust_details ”). a business rule associated with the term specifies a constraint that a high value customer is one who has a balance of more than one hundred thousand dollars ( balance_amount & gt ; 100000 ). the corresponding terms are replaced with these values . the unfolding query now reads : “ select top 3 cust_details from abc bank where balance_amount & gt ; 100000 * and & lt ; constraints & gt ; and in first quarter .” moving to the next word , “ from ” is a query word and remains in place . query unfolding program 108 locates the next word , “ abc_bank ,” in the business glossary . a resource location asset for “ abc_bank ” is a database table defined as “ cust_abc_bank_tbl ,” which is substituted for “ abc_bank .” this is governed by the associated definition or business rule in the business glossary . query unfolding program 108 continues to check subsequent words and phrases . the optional constraint is ignored . the term “ in first quarter ” is found in a “ dates ” category with an associated definition / rule of “ trans_date between 1 - jan - 2011 and 28 - mar - 2011 .” the definition may be substituted for the term “ in first quarter .” after all words and phrases have been checked and necessary replacements met , optional constraints are removed . the query now reads : “ select top 3 cust_details from cust_abc_bank_tbl where balance_amount & gt ; 100000 and trans_date between 1 - jan - 2011 and 28_mar — 2011 .” the query may now be run or submitted to the server containing “ cust_abc_bank_tbl ” to be run . in this example , the query is submitted to the applicable server ( e . g ., server computer 102 ) and is incomplete . the process is repeated on server computer 102 with each word and phrase examined for matches in a different business glossary . though “ cust_details ” could , in one embodiment , be the name of a single searchable attribute in a database , in another embodiment , an attribute substituted in at a client device may be further broken down at the server computer . for example , “ cust_details ” might be further defined as “ cust . name ” and “ cust . address ” based on definitions at the server computer . the phrase “ top 3 ” may be matched to a phrase in the server &# 39 ; s business glossary such as “ top n .” the business rules associated with the term “ top n ” may specify that the parameters should be a transaction amount ( trans_amount ) and that the query should be nested n times to fetch the higher transaction amounts . based on the located definitions and rules , the final query could be : “ select cust . name , cust . address from cust_abc_bnk_tbl as c1 where ( select count ( trans_amount ) from cust_abc_bnk_tbl as c2 where c1 . trans_amount & gt ; c2 . trans_amount )& gt ; 3 and balance_amount & gt ; 100000 and trans_date between 1 - jan - 2011 and 28_mar — 2011 ”. though the process described above fits the query to the nearest query template prior to comparing terms to the business glossary , a person of ordinary skill in the art will recognize that in other embodiments the words or phrases may be searched for in the business glossary first . unfolding and substituting correct terms and determining categories to which the terms belong may in some instances be helpful in matching the query to the closest query template . in another embodiment still , each word or phrase may be compared to both the query templates and the business glossary as the text is being parsed . in such an embodiment , the list of potential query templates may be reduced as each word or phrase is examined . fig4 depicts a block diagram of components of a computing system , such as computing device 101 or server computer 102 in accordance with an illustrative embodiment . it should be appreciated that fig4 provides only an illustration of one implementation and does not imply any limitations with regard to the environment in which different embodiments may be implemented . many modifications to the depicted environment may be made . the computing system includes communications fabric 402 , which provides communications between computer processor ( s ) 404 , memory 406 , persistent storage 408 , communications unit 410 , and input / output ( i / o ) interface ( s ) 412 . memory 406 and persistent storage 408 are examples of computer - readable tangible storage devices and media . memory 406 may be , for example , one or more random access memories ( ram ) 414 , cache memory 416 , or any other suitable volatile or non - volatile storage device . message interpreter 104 and query unfolding program 108 on computing device 101 , for example , may be stored in persistent storage 408 for execution by one or more of the respective computer processors 404 via one or more memories of memory 406 . in the embodiment illustrated in fig4 , persistent storage 408 includes flash memory . alternatively , or in addition to , persistent storage 408 may include a magnetic disk storage device of an internal hard drive , a solid state drive , a semiconductor storage device , read - only memory ( rom ), eprom , or any other computer - readable tangible storage device that is capable of storing program instructions or digital information . the media used by persistent storage 408 may also be removable . for example , a removable hard drive may be used for persistent storage 408 . other examples include an optical or magnetic disk that is inserted into a drive for transfer onto another storage device that is also a part of persistent storage 408 , or other removable storage devices such as a thumb drive or smart card . communications unit 410 , in these examples , provides for communications with other data processing systems or devices . in these examples , communications unit 410 includes one or more network interface cards . communications unit 410 may provide communications through the use of either or both physical and wireless communications links . in another embodiment still , the computing system may be devoid of communications unit 410 . message interpreter 104 and query unfolding program 108 may be downloaded to persistent storage 408 through communications unit 410 . i / o interface ( s ) 412 allows for input and output of data with other devices that may be connected to the computing system . for example , i / o interface 412 may provide a connection to external devices 418 such as a keyboard , keypad , a touch screen , and / or some other suitable input device . i / o interface ( s ) may also connect to a display 420 . display 420 provides a mechanism to display data to a user and may be , for example , a computer monitor . the programs described herein are identified based upon the application for which they are implemented in a specific embodiment of the invention . however , it should be appreciated that any particular program nomenclature herein is used merely for convenience , and thus the invention should not be limited to use solely in any specific application identified and / or implied by such nomenclature . the flowchart and block diagrams in the figures illustrate the architecture , functionality , and operation of possible implementations of systems , methods and computer program products according to various embodiments of the present invention . in this regard , each block in the flowchart or block diagrams may represent a module , segment , or portion of code , which comprises one or more executable instructions for implementing the specified logical function ( s ). it should also be noted that , in some alternative implementations , the functions noted in the block may occur out of the order noted in the figures . for example , two blocks shown in succession may , in fact , be executed substantially concurrently , or the blocks may sometimes be executed in the reverse order , depending upon the functionality involved . it will also be noted that each block of the block diagrams and / or flowchart illustration , and combinations of blocks in the block diagrams and / or flowchart illustration , can be implemented by special purpose hardware - based systems that perform the specified functions or acts , or combinations of special purpose hardware and computer instructions . | 6 |
the various embodiments of the present invention and their advantages are best understood by referring to fig1 through 7 of the drawings . the elements of the drawings are not necessarily to scale , emphasis instead being placed upon clearly illustrating the principles of the invention . throughout the drawings , like numerals are used for like and corresponding parts of the various drawings . this invention may be provided in other specific forms and embodiments without departing from the essential characteristics as described herein . the embodiments described above are to be considered in all aspects as illustrative only and not restrictive in any manner . the following claims rather than the foregoing description indicate the scope of the invention . fig1 depicts an exemplary stair safety apparatus 10 comprising a bar member 11 , a wrist band 13 , and an elastic or stretchable cord 15 connecting the bar member 11 and the wrist band 13 so the apparatus is worn around a user &# 39 ; s wrist . the bar member 11 comprises a rigid core with an outer surface of a high friction material , for example , rubber or similar polymeric substance . preferably , the outer surface further comprises a plurality of circumferential ribs 12 that lay roughly perpendicular to the longitudinal axis of the bar member 11 . the cord 15 may be a helical stretch cord , as depicted , or may be any suitable elastic line . fig2 through 4 illustrate the use of the stair safety apparatus 10 where the apparatus 10 , worn by a user 14 , is suspended between a stair rail 16 and the wall 18 to which the stair rail is mounted . if a user falls as he or she transits the stair way , the bar member 11 becomes wedged between the wall and the stair rail ( fig4 ), and the cord is pulled tight by the weight of the user . the friction between the outer surface of the bar member 11 and the wall helps to prevent the bar member 11 from disengaging from is wedged position . it will be appreciated that the bar member 11 should be long enough to engage both the wall and the stair rail , and the cord 15 should be long enough , in a stretched position , to prevent a user from toppling when a stumble occurs . with reference now to fig5 , an embodiment of the stair safety apparatus includes a hollow bar member 21 defining a chamber 22 in which is retained an alarm device 23 . the alarm device 23 may be connected to a line 25 having an end attached to the cord 15 . when a user falls and the cord 15 is pulled tight , the line 25 is also pulled and triggering activation of the alarm device 23 . an alai device 23 suitable for use in this embodiment is exemplified by the personal keychain alarm device model no . 51208 offered by general electric co . as shown in fig6 a & amp ; 6b , such an alarm device 23 may include a pin 27 attached to the line 25 , which is configured to activate an audible alarm when removed from the alarm device 23 , which occurs when the line is pulled along with the cord 15 when a user falls on the stairs as described above . in another embodiment , shown with reference to fig7 a and 7b , the bar member 31 comprises two pieces 33 a , b , wherein a first piece 33 a is formed to include a boss 35 . the second piece 33 b is formed with a chamber 32 for receiving the boss 35 . in this way , the bar member 31 may be separated into pieces for convenient storage and re - attached for use . as described above and shown in the associated drawings , the present invention comprises a stair safety apparatus . while particular embodiments of the invention have been described , it will be understood , however , that the invention is not limited thereto , since modifications may be made by those skilled in the art , particularly in light of the foregoing teachings . it is , therefore , contemplated by the appended claims to cover any such modifications that incorporate those features or those improvements that embody the spirit and scope of the present invention . | 0 |
referring now to fig1 , 2 and 4 of the drawings , a refractory repair dispenser device 10 of the invention can be seen used to repair the interior refractory lining wall surface w within a furnace f while in operation . the repair device 10 is more specifically adapted to be used in conjunction with a source s of refractory patch material m . such refractory patch material m source s is well established and known within the art in which an acquiesce granular mix of refractory material is supplied under pressure to an outlet . accordingly , no further description is required under the enabling disclosure requirement that has been well established in which apparatus or processes that are common and well understood within the art need not be described in detail , only referred thereto . the dispensing device 10 of the invention has a main elongated cylindrical body 11 having a threaded end cap 12 or equivalent registerably positioned within the perimeter of its dispensing end at 13 . the end cap 12 is preferably of the same outer diameter as that of the cylindrical body 11 for smooth withdrawal during the repair process which will be described in greater detail hereinafter . the cylinder body member 11 is adapted to be removably secured to the source s of refractory patch material m by a connecting couple 14 which may be of any corresponding configuration to match the respective source s of refractory patch material m , as noted . a plurality of injection nozzle assemblies 15 are positioned within and dispensing end portion 16 in cylinder 13 in longitudinally and radially spaced relation to one another as best seen in fig3 of the drawings . each of the nozzle assemblies 15 are formed from a short open ended tubular element 17 that extends angularly through an opening in the cylindrical wall 18 , as best seen in fig2 of the drawings . the tubular elements 17 are correspondingly flush with the outer cylindrical surface 19 of the cylindrical wall 18 and extend inwardly midway into the cylindrical body member 11 &# 39 ; s interior at 20 . the length and angular orientation of each of the tubular elements 17 imparts a reverse directional outlet stream of refractory patch material m therefrom as illustrated by multiple flow arrows 21 . the reverse directional outlet stream flows 21 are critical to the success of the repair illustrated in fig4 and 5 of the drawings as follows . once an area for repair at 22 has been identified by detecting a “ hot spot ” hs on the outside surface 23 of an outer steel furnace wall 24 , a small access opening is cut at 25 therein . the repair device 10 interconnected to the source s of refractory patch material m is inserted through the cut - out at 24 into the furnace f to a distance equal to that of the existing refractory wall w . the refractory patch material m is then supplied under pressure through the interior 20 of the cylindrical body member 11 and into the respective open ends at 25 of the tubular elements 17 . the nozzles 15 so formed direct the outlet flows 21 back towards the interior surface of the furnace wall 23 filling in the area for repair 22 in the refractory lining wall w . this undirectional concentration of directed refractory patch material m assures that a proper repair is being made with little waste and undirected material being dispensed and lost within the confines of the furnace f . as the nozzle 15 &# 39 ; s directs the flow of the refractory patch material m back towards the refractory wall w , the repair material m is deposited within the repair area building up thereagainst as seen in fig4 of the drawings . the repair device 10 of the invention is then slowly pulled out of the furnace f through the opening at 24 continuing to dispense refractory patch material m imparting a self - sealing action is achieved assuring that the access opening at 24 is effectively sealed with refractory patch material m in one simple repair action . by the positioning of the multiple nozzles 15 and the angular inclination of their tube elements 17 , a conical spray pattern is achieved about the cylindrical body member 11 assuring a complete accurate patch to the interior refractory wall surface w . the refractory patch material m will dry and harden forming a heat resistance liner patch equal to that of the original refractory brick lining wall w typically used in such installations . it will thus be seen that a new and novel refractory furnace repair device has been illustrated and described and it will be apparent to those skilled in the art that various changes and modifications may be made thereto without departing from the spirit of the invention . therefore i claim : | 5 |
when a ferrite magnetic powder is incorporated in a binder at a high filling factor and the result is kneaded , the large shearing load it receives during the kneading and ensuing molding imparts strain to the ferrite crystals . the bond magnet after molding is therefore lowered in coercivity relative to the ferrite powder before molding . the inventors conducted extensive research and experimentation in search of a way to mitigate this decline in coercivity and learned that by using fine and coarse powders within a different range from that taught by reference , the decline in coercivity at molding of a bond magnet can be made slight . ferrite magnetic powder comes in varying compositions and grain forms . when produced by the dry method , the sequence of the processes is generally : starting material blending → pelletizing → firing → pulverizing → washing → dewatering / drying → crushing → annealing → product . the final “ annealing ” step is conducted for relieving crystal strain arising during pulverizing after firing ( and also during crushing after drying ), because the crystal strain occurring during pulverizing and crushing degrades the magnetic properties , particularly coercivity . after annealing , the ferrite magnetic powder including alkaline - earth metal constituent has a ph of 10 - 12 . this makes its compatibility with binder poor and has a large adverse effect on the viscosity and fluidity of the powder - binder compound . it is therefore preferable to lower the powder ph of the annealed ferrite magnetic powder . methods available for lowering the powder ph include that of suspending the magnetic powder in water , stirring it well and , as circumstances require , adding a mineral acid to the suspension , and that of stirring the magnetic powder and carbon dioxide gas in the presence of moisture ( water ). when the ferrite magnetic powder is used to produce a bond magnet , the filling factor with respect to the binder can be increased by optimizing the ratio between fine and coarse powders as taught by reference . however , while this makes it possible to obtain high magnetic force , it unavoidably results in the coercivity maintained by the ferrite magnetic powder being lowered at the time of bond magnet molding . the inventors carried out a series of experiments with regard to this point and learned that the decline in coercivity at molding becomes slight when fine powder and coarse powder are mixed within a prescribed ratio range different from the levels taught as preferable by reference . the decline in coercivity at molding of a bond magnet can be assessed by a molding test consisting of the steps ( 1 )-( 4 ) set out earlier . when the mixed powder of fine and coarse powders according to the present invention set out above is used , the value obtained by subtracting the coercivity of the molded product acquired in the molding test from the coercivity of the magnetic powder specimen before molding is 600 oe or less . the annealing can be conducted before blending the fine and coarse powders but is more conveniently conducted after . the annealing relieves the strain arising within the crystal grains when the fine and coarse powders are obtained by pulverization in the course of production . an annealing temperature of 800 - 1100 ° c . is preferable . at lower than 800 ° c ., the effect of the annealing does not reach a sufficient level , resulting in low coercivity and saturation magnetization . at higher than 1100 ° c ., firing proceeds to degrade compression density and orientation . iron oxide and strontium carbonate were weighed out and mixed at a mole ratio of 1 : 5 . 5 . the mixture was pelletized using water , dried and then fired for two hours at 950 ° c . in an electric furnace . the fired product was pulverized in a hammer mill ( marketed as sample mill ) and further wet - pulverized in a wet pulverizer ( marketed as wetmill ) to obtain a fine powder of an average particle diameter of 0 . 59 μm . iron oxide and strontium carbonate were weighed out and mixed at a mole ratio of 1 : 5 . 75 . the mixture was pelletized using water , dried and then fired for four hours at 1290 ° c . in an electric furnace . the fired product was pulverized in the sample mill to obtain a coarse powder of an average particle diameter of 3 . 3 μm . the fine powder , 30 wt %, and the coarse powder , 70 wt %, were blended by the wet method , filtered , washed with water , dried , crushed and fired ( annealed ) for one hour at 990 ° c . in an electric furnace . the powder ph of the fired product was adjusted using carbon dioxide gas and water . a strontium ferrite powder of the following description was obtained as the final dry powder product . the specific surface area shown is that by bet and the compression density value is that under compression at a force of 1 ton / cm 2 . average particle diameter : 1 . 17 μm specific surface area : 2 . 23 m 2 / g compression density : 3 . 50 g / cm 2 powder ph : 9 . 4 powder ihc : 3707 ( oe ) under stirring in a mixer ( sample mill sk - m10 , kyoritsu - rikou co ., ltd . ), 90 parts by weight of the strontium ferrite powder obtained in ( 3 ) was surface treated with 0 . 4 parts by weight of silane coupling agent ( a - 1122 , nihonunica corporation ), mixed with 9 . 48 parts by weight of nylon 6 powder ( p - 1010 , ube industries , ltd . ), and further added with 0 . 12 parts by weight of lubricant ( calcium stearate ). the obtained mixture was formed into kneaded pellets of an average diameter of about 2 mm at 230 ° c . using a kneader ( laboplus mill biaxial batch kneader , toyoseiki co ., ltd .) and then injection molded at a temperature of 290 ° c . and molding pressure of 85 kgf / cm 2 under a magnetic field orientation of 10 koe to obtain a 15 mm diameter × 8 mm height cylindrical anisotropic bond magnet . the magnetic properties of the magnet were measured with a bh tracer . it had a maximum energy product ( bh ) max of 2 . 20 mgoe and an ihc of 3308 oe . the decline in coercivity ihc between that before molding and that of the molded product was thus 399 oe . the properties of the ferrite powder and the properties of the bond magnet obtained in this example are summarized in tables 1 and 2 . a strontium ferrite powder was produced under the same conditions as in example 1 , except that 100 wt % of coarse powder was used with no addition of fine powder . specifically , only the coarse powder obtained in ( 2 ) of example 1 was wet - pulverized , filtered , washed , dried , crushed and fired ( annealed ) for 1 hour at 990 ° c . the powder ph of the fired product was adjusted using carbon dioxide gas and water to obtain a strontium ferrite powder of an average particle diameter of 1 . 49 μm as the final dry powder product . the obtained powder was used to fabricate a bond magnet as in example 1 , and the properties of the ferrite powder and bond magnet were assessed as in example 1 . the results of the assessment are shown in tables 1 and 2 in comparison with those of example 1 . as shown in table 2 , the decline in coercivity ihc between that before molding and that of the molded product was 1041 oe . iron oxide and strontium carbonate were weighed out at a mole ratio of 1 : 5 . 75 and mixed with the additives . the mixture was pelletized using water , dried and then fired for four hours at 1290 ° c . in an electric furnace . the fired product was pulverized in a hammer mill ( marketed as sample mill ) and further wet - pulverized in a wet pulverizer ( marketed as wetmill ) to obtain a fine powder of an average particle diameter of 1 . 20 μm . iron oxide and strontium carbonate were weighed out at a mole ratio of 1 : 5 . 75 and mixed with the additives . the mixture was pelletized using water , dried and then fired for four hours at 1290 ° c . in an electric furnace . the fired product was pulverized in the sample mill to obtain a coarse powder of an average particle diameter of 4 . 4 μm . the fine powder , 30 wt %, and the coarse powder , 70 wt %, were blended by the wet method , filtered , washed with water , dried , crushed and fired ( annealed ) for one hour at 990 ° c . in an electric furnace . the powder ph of the fired product was adjusted using carbon dioxide gas and water . a strontium ferrite powder of an average particle diameter of 1 . 44 μm was obtained as the final dry powder product the obtained powder was used to fabricate a bond magnet as in example 1 , and the properties of the ferrite powder and bond magnet were assessed as in example 1 . the results of the assessment are shown in tables 1 and 2 . as shown in table 2 , the decline in coercivity ihc between that before molding and that of the molded product was 811 oe . as can be seen from the results shown in tables 1 and 2 , the bond magnet of example 1 has about the same molding density , residual flux density and maximum energy product as those of comparative examples 1 and 2 . however , its difference in coercivity between before and after molding is , at 399 oe , well within 600 oe , in contrast to the high differences of 1041 oe and 811 oe for those of comparative examples 1 and 2 . the decline in coercivity at the time of bond magnet molding is thus smaller in the case of the ferrite magnetic powder of example 1 than in the case of the ferrite magnetic powders of comparative examples 1 and 2 . as is clear from the foregoing explanation , the present invention provides a ferrite magnetic powder for bond magnet that experiences only small decrease in coercivity when molded into a bond magnet and that , as such , is useful in applications requiring high coercivity . | 2 |
fig4 shows a flowchart of the method used to acquire timing and synchronization between a mobile station and a base station using the proposed wcdma perch channel structure in accordance with an embodiment of the invention . the method starts with the step of sampling the downconverted input signal over one or more slots . as described in the discussion of fig1 , each wcdma frame contains 16 slots , each slot being 2560 chips long . the psc sequence is transmitted in the first 256 chips of each slot . in order to synchronize the acquisition system to the slot timing of the received signal , the primary synchronization code ( psc ) sequence is correlated with the data received over a first period f 1 . this step 102 is shown with a formula psc ( f 1 )=& gt ; psc 1 , indicating that samples collected over slots in frame period number one are used to correlate with the psc sequence to arrive at a first estimate of slot timing , psc 1 . in an exemplary embodiment of the invention , the psc slot timing estimate is formed by accumulating samples over multiple slot periods . this is accomplished by using a slot sample buffer large enough to hold sampled data for one slot period , and then adding the subsequent samples collected over the following slot periods . for example , if the received signal is sampled at half - chip intervals , a slot sample buffer having 5120 sample bins would be used to perform psc slot timing estimation . after storing 5120 for the first slot period being estimated into each of the 5120 sample bins , each sample collected over the second slot period is added to a corresponding bin . in this way , bin 1 would contain the sum of samples s 1 + s 5121 + s 10241 and so forth . since the psc sequence is constant , and is transmitted in the same place in each slot , this “ soft combining ” accumulation method results in a better estimate than is possible over a single slot period . in the preferred embodiment , the correlation between received samples and the psc sequence is measured using a digital matched filter . for example , if the samples received during 16 consecutive slot periods are accumulated into 5120 half - chip sample bins , a psc digital matched filter is used to measure correlation of the 512 - sample psc sequence with each of the 5120 possible 512 - bin groupings . the 5120 - bin slot sample buffer is implemented as a circular buffer that allows wrap around addressing to generate digital matched filtering correlation energies at all possible offsets within the slot period . for example , to create a 512 - bin period with an offset of 5100 , the matched filter would be correlated with the bin numbers 5100 to 5120 , followed by bins 1 through 491 . though the invention is described here using digital matched filters , one skilled in the art will appreciate that other forms of correlation , such as analog matched filters or multiply - and - integrate circuits could also be used without departing from the present invention . in the preferred embodiment of the present invention , the sampling step entails complex sampling as is well known in the art . other forms of sampling , including but not limited to real sampling , could also be used without departing from the present invention . in the preferred embodiment of the invention , the samples are collected at half - chip intervals . a received 256 - chip psc sequence , therefore , would be represented within 512 sample intervals . in using complex samples , the received sample stream would be evaluated for correlation over 1024 samples , 512 in - phase ( i ) samples , and 512 quadrature - phase ( q ) samples . in the preferred embodiment of the invention , the first period f 1 , during which data is accumulated and used for psc synchronization , is a full frame period ( 16 slot ). the first period f 1 , however , could be any number of slot periods , including fewer than 16 slots or any multiple of 16 slots , without departing from the present invention . step 104 shows the processing performed on samples received during a second period f 2 which follows step 102 . in step 104 , slot timing from estimate psc 1 is used to decode the secondary synchronization code ( ssc ) information , as indicated by the formula “ ssc ( f 2 , psc 1 )=& gt ; ssc 1 ”. decoding the ssc code word is a two - stage process consisting of decoding the ssc symbol residing in each slot , and then decoding the ssc code word from the generated ssc symbols . the first stage of decoding ssc symbols is performed based on the assumption that the available slot timing estimate is correct . in an exemplary embodiment of the invention for a wcdma system , slot timing estimate psc 1 is used to establish the location of the first 256 chips of each of the sixteen slots in every frame . over period f 2 , the samples for each of the sixteen 256 - chip periods are accumulated into ssc sample accumulation buffers . in an exemplary embodiment of the invention , period f 2 is an integer multiple of frame periods in length . in the case of wcdma , the sixteen 256 - chip buffers may be implemented as a single , 4095 - chip buffer divided into sixteen sections . the accumulated sample values in each buffer or buffer section are then matched against the possible transmitted ssc code symbols . in the case of wcdma , there are seventeen different possible 256 - chip ssc code symbols . for the ssc symbol in each slot , the ssc symbol sequence having the highest degree of correlation with the values in the corresponding ssc sample accumulation buffer is selected as the most - likely ssc code symbol . the second stage of ssc decoding is identifying the ssc code word from the estimated ssc code symbols . in wcdma , the ssc code words are selected from a comma - free subset of a reed - solomon block code . the sixteen selected ssc code symbols are resolved to a reed - solomon code word , which is then shifted as necessary to equate to one of the comma - free subset allowed . the number of shifts necessary are used to identify frame timing ( which slot comes first ), and the ssc code word identified identifies the group identification ( gi ). in the preferred embodiment of the invention , the psc sample values received during the second period f 2 are accumulated into the slot sample buffer already containing the accumulated samples received during first period f 1 . this means that , during step 104 , as indicated by the formula “ psc ( f 2 , f 1 )=& gt ; psc 2 ”, psc 2 is derived from samples collected over both periods f 1 and f 2 . in an alternate embodiment , the slot sample buffer is cleared at the beginning of period f 2 , so that psc 2 is formed using samples from period f 2 . after completing step 104 , psc 1 is compared with new estimate psc 2 in step 106 . if psc 1 is equal to psc 2 , then psc 1 is deemed valid for use in slot timing . if psc 1 is not yet deemed valid in step 106 , then ssc 1 , which was generated based on slot timing in psc 1 , is questionable and is not yet used for frame timing estimation . if it is determined that psc 1 is questionable ( not equal to psc 2 ), step 108 is performed , wherein data from a third period f 3 is used to estimate received data . in this step , as indicated by the formula “ ssc ( f 3 , psc 2 )=& gt ; ssc 2 ”, data received during a third period f 3 is used to form ssc 2 , a second estimate of the ssc code word . in addition , during step 108 , an additional estimate of slot timing is made , based on data received in the third period f 3 , to generate psc 3 . as in step 104 , the accumulated samples used to generate the previous estimate psc 2 are utilized in generation of psc 3 . again , an alternative embodiment creates psc 3 based on samples received during period f 3 only . one skilled in the art will appreciate that the number of successive unchanged psc estimates required by the validity test may be more than the two described without use of inventive faculties . for example , three or four identical ssc slot timing estimates in a row may be required before the ssc slot timing estimate is considered valid . additionally , pilot channel data is decoded from data received during period f 3 , based on the frame timing and group identification provided from ssc 1 , to form pilot offset estimate pilot 1 . in determining pilot channel offset , received samples are only correlated against the 16 pilot offsets specified by the group identification ( gi ) associated with ssc 1 . at step 110 , psc 1 is compared with new estimate psc 3 . if psc 1 is equal to psc 3 , then psc 1 is deemed valid for use in slot timing . if psc 1 is deemed valid , then ssc 1 , which based its slot timing on psc 1 , is evaluated and tested for validity in step 112 . in an exemplary embodiment , the ssc validation in step 112 is based on the number of ssc symbol errors detected during the formation of ssc 1 . these symbol errors are measured by counting the number of symbols decoded during the first stage of ssc decoding which do not agree with the symbols of the nearest ssc code word decoded in the second stage . if this number of symbol disagreements ( also called hamming distance ) is greater than a predetermined value , ssc 1 is deemed invalid . in another embodiment of the invention , step 112 uses a combination of hamming distance and the correlation energies of the decoded ssc symbols to determine whether the confidence level of a ssc decoding rises to the level required for validity . if ssc 1 is deemed valid in step 112 , then pilot 1 is used as an estimate of pilot offset in step 114 . in an alternative embodiment of the invention , no maximum is placed on the allowable number of symbol errors received in conjunction with ssc estimations . the best estimate of received ssc code word is immediately used , and steps 112 and 128 are omitted . in the preferred embodiment of the invention , a correlation strength metric is generated for each decoded ssc symbol . this correlation strength metric is a measure of the degree of correlation between the estimated transmitted symbol value and the received signal , and is generated during the first stage of the two - stage ssc decoding method described above . the correlation strength metrics , along with the estimated received symbols , are used as input for the chase algorithm to determine the received ssc code word . the chase algorithm is an improved method of performing “ soft decision ” decoding of block codes , and was described in an article by david chase in “ ieee transactions on information theory , vol . it - 18 , no . 1 , january 1972 ”. the use of the chase algorithm provides improvement in ssc decoding accuracy of as much as 2 db for additive white gaussian ( awgn ) channels , and 6 – 8 db for fading channels . if psc 1 is deemed invalid at step 110 , then psc 2 is compared with new estimate psc 3 in step 116 . if psc 2 is not equal to psc 3 , then psc 2 is deemed invalid or questionable for slot timing . in the preferred embodiment of the invention , if samples collected over periods f 1 , f 2 , and f 3 have been accumulated into the psc slot sample buffer at step 116 , but a good slot timing estimate has still not been obtained , the process resets and starts over at step 118 , returning to step 102 . if , at step 116 , psc 2 is equal to psc 3 , then psc 2 is deemed valid for slot timing . if psc 2 is deemed valid , then ssc 2 , which based its slot timing on psc 2 , is evaluated in step 122 . in the preferred embodiment of the invention , step 122 uses the same ssc evaluation methods as step 112 . if ssc 2 is deemed valid in step 122 , then ssc 2 is used in step 124 to decode pilot channel data from data received during a fourth period f 4 . the pilot 2 data decoded in step 124 is then made available for use in step 126 . if , after evaluating the validity of psc 1 at step 106 , psc 1 is determined to be valid , then ssc 1 is evaluated for validity in step 128 . in the preferred embodiment of the invention , step 128 uses the same ssc evaluation methods as step 112 . if ssc 1 is deemed invalid during step 128 , then data received during a third period f 3 is used in step 120 to generate another ssc estimate , ssc 2 . though step 120 is shown in the figure as using psc 2 to generate ssc 2 , psc 1 could be used in step 120 to obtain the same result . after step 120 , the resulting ssc 2 is evaluated in step 122 , which has already been described above . if , in step 128 , ssc 1 is deemed valid for use in frame timing , then ssc 1 is used with data received during a third period f 3 to decode the pilot information in step 130 . the product of step 130 is pilot 1 , which is subsequently made available for use by the system in step 132 . period f 3 is one or more frames in length . in steps 108 and 120 , alternative embodiments of the invention add symbol estimates collected during periods f 2 and f 3 in generating ssc 2 . in other words , ssc 1 is used strengthen the estimate ssc 2 . in other alternate embodiments of the invention , evaluation of the validity of a psc slot timing estimate in steps 106 , 110 , and 116 is performed by evaluating the degree of correlation resulting from the matched filtering used to generate psc estimates . for example , when half - chip samples are used , then each slot period contains 5120 samples , which are accumulated into 5120 sample bins . the psc sequence is correlated at each of the 5120 possible offsets to yield a set of 5120 correlation energies . the highest correlation energy is the psc best estimate energy , and the slot timing offset corresponding to that correlation energy is the psc best estimate offset . in order to be considered a valid reference for ssc decoding , the psc best estimate energy is compared to the next - highest of the remaining 5119 correlation energies . as the samples of additional slots are accumulated into the accumulation buffer , the psc best estimate energy rises farther and farther above all other correlation energies . in one embodiment of the invention , the psc best estimate offset is deemed reliable only if the psc best estimate energy exceeds the next highest correlation energy by a predetermined threshold multiplier , for example 6 db . the timing of the received psc code may be such that it results in high correlation energies in two or three adjacent offsets . recognizing this possibility , an alternative embodiment of the invention compares the psc best estimate energy only to offsets which are not immediately adjacent to the psc best estimate offset . in an exemplary implementation of this method , the four highest correlation energies and their offsets are saved as all offsets are correlated to the psc sequence , and the psc best estimate energy is compared to the next highest correlation energy which does not belong to an adjacent offset . another alternative embodiment of the invention is useful where the autocorrelation function of the psc sequence followed by 2304 chips of zeroes has an identifiable envelope . in this embodiment , the correlation energies of all offsets are stored into a correlation energy buffer . in an exemplary implementation using half - chip sampling , the correlation energy buffer would hold 5120 correlation energies . the set of correlation energies is then matched with the autocorrelation function of the psc sequence followed by 2304 chips of zeroes . the offset having the contour closest to this autocorrelation function is the psc best estimate offset . fig5 shows a flowchart of another method of acquire timing and synchronization between a mobile station and a base station using the proposed wcdma perch channel structure in accordance with an embodiment of the invention . the method starts with the step 150 of clearing sample accumulation buffers used to accumulate psc and ssc samples , setting each bin of each buffer to zero . samples later received are added to the values already in the bins . the psc sample accumulation buffer stores enough samples to accumulate an entire slot period of 2560 chips . the ssc sample accumulation buffer stores enough samples to accumulate the first 256 chips of 16 consecutive slots . the ssc sample accumulation buffer has enough bins , therefore , to store 4096 chips worth of samples . after the psc and ssc buffers are cleared 150 , a first set of samples is received and accumulated 152 into the psc sample accumulation buffer . in the preferred embodiment of the invention , a full frame ( 16 slots ) of samples are accumulated into the psc buffer . the sample accumulation 152 is performed as described above in step 102 . the psc sequence is then correlated against the contents of the psc buffer to generate slot timing estimate psc 1 154 . the correlation of the psc sequence to values in the psc buffer is done in any of the ways described above . in step 156 , slot timing estimate psc 1 is used to accumulate samples into the ssc sample accumulation buffer . as described above , each sample is accumulated into a psc buffer bin according to its time offset within its slot . not all samples are accumulated into the ssc buffer , however . based on slot timing from estimate psc 1 , only samples collected during the first 256 chips of each slot are saved into the ssc buffer . because the transmitted ssc symbols differ from slot to slot , the sample bins of the ssc buffer are broken into sixteen 256 - chip regions , into which the collected samples are accumulated . if the slot timing provided by psc 1 is accurate , each 256 - chip region will contain accumulated samples for one slot &# 39 ; s ssc symbol period . because the value of ssc buffer contents depend on the accuracy of psc 1 , and to conserve computational resources , the ssc decoding of the ssc buffer contents may be delayed or postponed until psc 1 is shown to be valid . at the same time that ssc samples are accumulated in step 156 , samples are also accumulated into the psc sample accumulation buffer . in step 160 , the contents of the psc buffer are again analyzed for correlation to the psc sequence , resulting in slot timing estimate psc 2 . in this way , psc 2 is generated from all of the samples accumulated in steps 152 and 156 . at step 164 , slot estimate psc 1 is compared with slot estimate psc 2 . if the two estimates are not equal , then psc 1 is assumed to be inaccurate . the ssc estimate generated using psc 1 is discarded by setting the contents of ssc sample accumulation buffer to zero 162 . slot timing estimate psc 1 is updated to be equal to psc 2 158 , and processing continues from step 156 . subsequent ssc estimates will be generated according to slot timing from the new slot timing estimate . in recognition that slight oscillator drift may cause the psc estimate to change slightly without completely invalidating ssc accumulation , an alternative embodiment of the invention continues to accumulate ssc samples if the psc estimate changes at step 164 by a chip or less . in the preferred embodiment of the invention , sampling is performed at half - chip intervals . in such an implementation , psc sample accumulation buffer has 5120 sample bins , and ssc accumulation buffer has 8192 sample bins . in step 164 , if psc 1 differs from psc 2 by only a half - chip ( one sample bin ), then step 162 is skipped , and step 158 is executed immediately after step 164 . in other words , the ssc buffer is not cleared , but the slot timing index , to be used in subsequent ssc sample accumulation , is updated . also evaluated at step 164 is the number of frames which have been accumulated into the psc sample accumulation buffer . if a predetermined number of frames , for example 10 , have elapsed with no apparent stabilization in the psc slot timing estimate , the psc sample accumulation buffer is cleared ( filled with zeroes ) and processing optionally continues at step 152 or aborts . the validity of psc 1 and psc 2 are further evaluated using one of the methods described above in conjunction with steps 106 , 110 , and 116 . in one embodiment of the invention , step 160 includes saving the second - highest correlation energy as well as psc 2 . at step 166 , psc 2 is evaluated for validity by comparing it to the correlation energies of other offsets . a psc slot timing estimate is deemed valid only if its correlation energy exceeds the correlation of every other offset by a predetermined amount , for example 6 db . in another embodiment of the invention , step 160 includes saving the four highest correlation energies as well as their offsets . at step 166 , a psc slot timing estimate is deemed valid only if its correlation energy exceeds the correlation of every other non - adjacent offset by a predetermined amount , for example 6 db . in another alternative embodiment of the invention , the correlation energies for all offsets are stored into a correlation energy buffer at step 160 . at step 166 , a psc slot timing estimate is deemed valid only if the values stored in the correlation energy buffer evaluated at that offset most closely match the autocorrelation function of the psc sequence followed by 2304 chips of zeroes . the ssc samples stored using a psc slot timing estimate are not decoded unless the psc slot timing estimate is deemed valid . if , at step 166 , psc 2 is deemed invalid , then processing continues from step 156 , so that the psc estimate can be strengthened by further sample accumulation . if , at step 166 , psc 2 is deemed valid , then the decoding of ssc and pilot information continue in step 168 . in one embodiment of the invention , the ssc code word is decoded in step 168 using the aforementioned chase algorithm . the first time an ssc code word is decoded , there may not be a sufficient degree of confidence in it to call it valid . subsequent samples are accumulated into the ssc sample buffer until the ssc code word is decoded and validated . just in case the ssc code word is later found to be valid , the pilot offset is estimated based on the best guess of the ssc information at the same time that additional ssc samples are being accumulated . after a valid ssc code word has been decoded in step 168 , the pilot offset generated in step 168 is evaluated in step 170 . if the pilot offset was generated based on the ssc code word eventually found to be valid , then the pilot offset measured in step 168 is used 174 . if the ssc code word decoded was not used to generate the pilot offset available at step 170 , then the pilot offset is decoded in step 172 based on the valid ssc code word . after the pilot offset is decoded in step 172 , it is ready for use in step 174 . in another embodiment of the invention , a frame sample accumulation buffer ( large enough to hold accumulated samples over an entire frame ) is used for decoding of psc , ssc and pilot information . samples are accumulated over enough frame periods that psc , ssc , and pilot may be decoded with high confidence . once the slot timing is established , the buffer may be organized into 16 slots . the accumulated samples in the first 256 chips of each buffer slot are immediately analyzed to decode the ssc code word . once the ssc code word has been decoded , the pilot offset is decoded from the last 1280 chips of each buffer slot . the samples from additional frame periods may be accumulated in the buffer as necessary to generate valid psc , ssc , and pilot information . psc and ssc decoding techniques described above , including use of psc correlation and autocorrelation , ssc symbol correlation energy measurement and the chase algorithm for decoding the ssc , are equally applicable to this frame accumulation method . this method requires a rather sizeable sample accumulation buffer ( 81 , 920 bins if half - chip samples are used ), but allows decoding of psc , ssc , and pilot information in a small number of frames ( theoretically as little as 10 milliseconds ). in an alternative embodiment , a pilot sample accumulation buffer large enough to accumulate samples for the portion of each slot in a frame period containing the pilot code is used for decoding pilot information . in the case of wcdma , the pilot sample accumulation buffer is divided into sixteen sections of 1280 chips . sample accumulation in this buffer may begin as soon as a psc slot timing estimate is generated . if the psc slot timing estimate used for pilot sample accumulation changes , the pilot sample accumulation buffer is cleared , and pilot sample accumulation resumes based on the new psc slot timing estimate . or , in an alternative embodiment , the pilot sample accumulation buffer is only cleared if the psc estimate changes by more than one sample offset . once the ssc code word is successfully decoded , hence identifying the frame timing and group identification , the sections in the pilot sample accumulation buffer are immediately correlated with the gold code offsets indicated by the ssc &# 39 ; s group identification . no further sample periods are needed beyond those required to decode the ssc code word . fig6 shows a high - level block diagram of a receiver configured in accordance with an embodiment of the invention . the apparatus depicted allows parallel processing of received samples based on the potential correctness of early psc and ssc estimates . the signals carrying primary synchronization code ( psc ), secondary synchronization code ( ssc ), and pilot information are received at antenna 202 , and are downconverted , complex pn despread , and complex sampled in receiver ( rcvr ) 204 . the resultant stream of complex samples are sent to psc detector 206 , ssc detector 208 , and pilot detector 210 . psc detector 206 , ssc detector 208 , and pilot detector 210 are also operably coupled to control processor 212 . control processor 212 sends control signals to psc detector 206 , ssc detector 208 , and pilot detector 210 commanding them to begin searching for a pilot signal or to abort a search in progress . psc detector 206 evaluates the samples received from receiver 202 over several slot periods to generate an estimate of slot timing . the operations performed by psc detector 206 are the same as the operations used to generate psc slot timing estimates as described above in conjunction with steps 102 , 104 , and 108 . psc detector 206 provides ssc detector 208 with the psc slot timing estimates through the connection shown . at the same time that psc detector 206 is generating additional slot timing estimates , ssc detector 208 uses slot timing estimates already generated by psc detector 206 to decode the ssc code word from subsequent samples provided by receiver 204 . the operations performed by ssc detector 208 are the same as the ssc operations described above in conjunction with steps 104 , 108 , and 120 . ssc detector 208 provides pilot detector 210 with frame timing estimates through the connection shown . at the same time that ssc detector continues to decode subsequent ssc samples , pilot detector 210 uses frame timing and group identification information provided by ssc detector 208 to estimate the pilot channel offset using subsequent samples provided by receiver 204 . the operations performed by pilot detector 210 are the same as the pilot offset determination operations described above in conjunction with steps 108 , 124 , and 130 . fig7 is a detailed block diagram of a preferred embodiment of psc detector 206 . in an exemplary embodiment of the invention , slot sample accumulators 304 are implemented as first - in first - out ( fifo ) buffers , having one sample bin for each of the sample positions in a single slot period . for example , half - chip samples would require a 5120 - sample slot buffer . at the beginning of channel acquisition , slot sample accumulators 304 are cleared upon receiving a command or signal from control processor 212 . thereafter , each time a sample with a slot offset is received at summing block 302 , it is added to the value for that slot offset retrieved from accumulator 304 . the resultant sum is stored into the sample bin associated with that slot offset within accumulator 304 . summing block 302 a and accumulator 304 a receive in - phase ( i ) samples and accumulate i values in the sample bins of accumulator 304 a . summing block 302 b and accumulator 304 b receive quadrature - phase ( q ) samples and accumulate q values in the sample bins of accumulator 304 b . in an embodiment of the invention which accumulates samples over entire frame periods , slot sample accumulators 304 are large enough to accumulate the number of samples in an entire frame period . in the case of half - chip samples , this means that slot sample accumulators 304 each have 81 , 920 bins . after accumulating samples over several slot periods , matched filter 310 is provided with sample bin values from accumulators 304 and measures psc sequence correlation throughout the sample bin regions . in the preferred embodiment of the invention , samples are accumulated over multiple frame periods ( 16 slots each in the case of wcdma ). matched filter 310 measures a real and imaginary correlation energy value for each possible slot timing offset . in the case where half - chip samples are used in a wcdma system , this would result in 5120 real and 5120 imaginary correlation energy values . as described for step 102 , the sample bins are used as a circular , or wrap - around buffer when evaluating offsets close to the end of the buffer . for example , to create a 512 - sample period with an offset of 5100 , values from bin numbers 5100 to 5120 , followed by bins 1 through 491 would be used as input to digital matched filter 310 . the real and imaginary correlation energies for each slot offset generated by matched filter 310 are provided to complex - to - scalar converter block 312 . as indicated in the figure , converter block 312 takes the real and imaginary components for each offset and combines them according to equation ( 2 ): r =√{ square root over ( x r 2 + x i 2 )}, ( 2 ) where x r is the real component of the correlation energy for a slot offset , x i is the imaginary component of the correlation energy for the slot offset , and r is the scalar magnitude of the correlation energy vector for the slot offset . the set of scalar correlation energy values generated by complex - to - scalar converter block 312 are provided to slot timing decision module 314 , which identifies the most likely psc slot boundary offset by selecting the offset with the greatest correlation . the determination of validity of a psc may be done using the methods previously described for steps 106 , 110 , and 116 . slot timing decision module 314 generates a slot timing signal , which is provided to ssc detector 208 . as described above , in an embodiment of the invention which compares the complete set of correlation energies with an autocorrelation envelope of the psc sequence , slot timing decision module 314 includes a correlation energy buffer having the same number of bins as a slot sample accumulator 304 . fig8 is a detailed block diagram of a preferred embodiment of ssc detector 208 . i and q samples from receiver 204 are received by ssc sample buffer 402 , along with the slot timing signal provided by psc detector 206 . ssc sample buffer 402 collects samples for the one symbol per slot which is expected to contain ssc symbols . in wcdma , for example , ssc symbols are transmitted in the first 256 chips , and therefore in the first symbol position of each slot . the i and q samples collected over the ssc symbol period are provided to ssc symbol correlator 404 , which determines which of the possible ssc symbols has the highest correlation energy to the samples in the ssc symbol period . in an exemplary embodiment in which the ssc symbols are walsh codes , ssc symbol correlator 404 is a fast hadamard transform ( fht ) module . ssc symbol correlator 404 generates decoded ssc symbols and provides them to ssc decoder 406 . when ssc decoder 406 has been provided with one ssc symbol for each slot in a frame period , ssc decoder 406 performs block decoding of the ssc code word to determine group identification ( gi ) and frame timing . as discussed above , wcdma uses a comma - free ssc code , which enables the identification of slot position within a frame from the symbols of the decoded ssc code word . the decoded ssc code word also uniquely identifies the one of sixteen group identification ( gi ) values for use in subsequent pilot channel decoding . both the frame timing signal and gi generated by ssc decoder 406 are provided to pilot detector 210 . in the preferred embodiment of the invention , ssc symbol correlator 404 also generates a correlation strength metric for each decoded ssc symbol , and provides this metric to ssc decoder 406 . in the preferred embodiment of the invention , ssc decoder 406 is a reed - solomon decoder . the correlation strength metrics provided by ssc symbol correlator 404 allow ssc decoder 406 to perform a “ soft decision ” decoding of the ssc code word in accordance with the aforementioned chase algorithm . fig9 is a detailed block diagram of an exemplary embodiment of pilot detector 210 . i and q samples from receiver 204 are received by pilot sample buffer 502 , along with the frame timing signal provided by ssc detector 208 . pilot sample buffer 502 collects samples for the portions of each slot expected to contain pilot data . in wcdma , for example , pilot data is transmitted in the latter half , or the last 1280 chips , of each slot . the i and q samples collected by pilot sample buffer 502 are provided to pilot correlator 504 , which determines the offset of the pilot gold code in relation to the start of each frame . pilot correlator 504 is also provided with group identification ( gi ) information so that it may be configured to search for only the pilot offsets within the identified group . in wcdma , for example , each group associated with a gi value contains only 16 of the 32 * 16 possible pilot offsets . in an alternative embodiment of the invention , pilot sample buffer 502 is implemented as an accumulator for combining samples of subsequent frame periods with those already collected . this allows an increasingly strong set of sample values used to generate a pilot offsets with a higher degree of confidence . the previous description of the preferred embodiments is provided to enable any person skilled in the art to make or use the present invention . the various modifications to these embodiments will be readily apparent to those skilled in the art , and the generic principles defined herein may be applied to other embodiments without the use of the inventive faculty . thus , the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein . | 7 |
all illustrations of the drawings are for the purpose of describing selected versions of the present invention and are not intended to limit the scope of the present invention . the present invention is a method of naturally decomposing chewing gum so that a piece of gum is not left in a dried - out harden state on an unwanted area . the present invention allows the piece of gum to start decomposing as a user chews on the piece of gum within their mouth . the present invention helps to mitigate the effects of irresponsible disposal and helps to accelerate biodegradation for the piece of gum that makes it into the recycling stream . as can be seen in fig1 and 2 , the present invention enhances a piece of gum by implementing the following components : a quantity of chewing - gum base , a quantity of biological organisms , a quantity of salvia , and an enclosing kneader . the quantity of chewing - gum base allows for the piece of chewing gum to have its kneadable texture . the quantity of chewing - gum base can be composed of other traditional chewing - gum ingredients such as flavorings . for the present invention , the quantity of chewing - gum base is made of , but is not limited to , either a chicle base or a glycerin base . the quantity of biological organisms is used to naturally decompose the quantity of chewing - gum base as the user is chewing on the piece of gum within their mouth . thus , the quantity of biological organisms is infused throughout the quantity of chewing - gum base ( step a ). in addition , the quantity of salvia is used to activate the quantity of biological organisms and consequently needs to be retained within the enclosing kneader ( step b ). the enclosing kneader preferably is the user &# 39 ; s mouth . the present invention also avoids or limits additional additives for a piece of gum so that the piece of gum is more easily decomposed by the present invention . as can be seen in fig2 , an overall process is followed by the method of the present invention in order to ensure that the present invention is able to naturally decompose chewing gum . the overall process begins by masticating the quantity of salvia into the quantity of chewing - gum base by placing the quantity of chewing - gum base into the enclosing kneader ( step c ), which allows the quantity of salvia to be integrated into the quantity of chewing - gum base and to make physical contact with the quantity of biological organisms . this physical contact between the quantity of saliva and the quantity of biological organisms is used to activate the quantity of biological organisms so that the quantity of biological organisms begins to decompose the quantity of chewing - gum base . thus , the overall process proceeds by executing a biodegradation process for the quantity of chewing - gum base with the quantity of biological organisms ( step d ) as the quantity of biological organisms is activated through contact with the quantity of saliva during step c . the type of biodegradation process that is used to decompose the quantity of chewing - gum base depends of the kind of biological organism that is initially infused into the quantity of chewing - gum base . in addition , if the quantity of chewing - gum base is removed from the enclosing kneader , then the overall process concludes by accelerating the biodegradation process for the quantity of chewing - gum ( step e ). the biodegradation process is accelerated for the quantity of chewing - gum base because the quantity of chewing - gum base is aerated outside of the enclosing kneader . typically , step e occurs when the user removes the piece of gum from their mouth . the present invention can use different types of biological organisms in order to naturally decompose chewing gum . one type of biological organism that can be used with the present invention is a type of fungus , which have been traditionally used to ferment food products . moreover , a preferably type of fungus is aspergillus oryzae , which is more palpable than other kinds of fungus . aspergillus oryzae has been a popular type of fungus in fermenting food products such as soy sauce , jiang / miso , fermented black soybeans , and grain - based wines ( e . g . sake , amazake , and li ). another type of biological organism that can be used with the present invention is a type of bacteria , which would be able to decompose the quantity of chewing - gum base without risking the user &# 39 ; s health . in one embodiment of the present invention , the biodegradation process described in step d would be executed with the following set of steps in order to naturally decompose chewing gum . this embodiment of the biodegradation process preferably uses aspergillus oryzae or another similar type of fungus as the quantity of biological substance . the first step in this embodiment of the biodegradation process is to produce enzymes with the quantity of biological organisms during step d . the enzymes allow or assist the present invention in naturally decomposing a piece of gum . the enzymes are produced because the quantity of chewing - gum base typically includes sugars for flavoring . when the quantity of biological organisms consumes the sugars within the quantity of chewing - gum base , the quantity of biological organisms produces those enzymes as byproducts . some of those enzymes can be , but is not limited to , amylases , proteases , lipases , tanninase , and combinations thereof . the second step in this embodiment of the biodegradation process is to decompose macromolecules of the quantity of chewing - gum base into its constituent parts with those enzymes . for the chewing - gum base , some of its constituent parts can be , but is not limited to , dextrin , glucose , peptides , amino acids , fatty acid chains , and combinations thereof . in some embodiments of the present invention , a plurality of pockets is integrated throughout the quantity of chewing - gum base . the plurality of pockets is a pragmatic means of housing the quantity of biological organisms within the quantity of chewing - gum base until the user begins knead the quantity of chewing - gum base within their mouth . in addition , the plurality of pockets is integrated throughout the quantity of chewing - gum base so that the quantity of biological organisms is evenly distributed throughout the quantity of chewing - gum base . consequently , the quantity of biological organisms is able to decompose the entire quantity of chewing - gum base instead of a fraction of the chewing - gum base . although the invention has been explained in relation to its preferred embodiment , it is to be understood that many other possible modifications and variations can be made without departing from the spirit and scope of the invention as hereinafter claimed . | 0 |
for the purpose of detecting hpv , it is first of all necessary to remove biopsy or smear material . this is taken up in 500 μl of melting buffer ( 0 . 1 m edta ; 0 . 05 m tris , ph 8 . 0 ; 0 . 5 % sds ). 2 . 5 μl of proteinase k ( 20 mg / ml ) are then added to this and the solution is incubated at 55 ° c . for from 24 to 48 hours . this is then followed by two extractions with phenol ( phenol : chcl 3 : isoamyl alcohol = 25 : 24 : 1 ). the preparation is mixed , not vortexed , incubated for 2 - 5 min . ( rotated with inversion ), and , after that , centrifuged at 14 000 rpm for 5 min . there then follows an extraction with chcl 3 / isoamyl alcohol ( 24 : 1 ) and incubation for 2 - 5 min and , after that , a centrifugation at 14 000 rpm for 5 min . 1 / 10 of the preparation volume of 7 . 5 m ammonium acetate is then added and the preparation is mixed and incubated at 55 ° c . for from 2 to 4 hrs . the preparation is then precipitated with ethanol at − 20 ° c . overnight . the dna which has been extracted in this way is subsequently used in a pcr reaction . 0 . 25 μl , 1 μl , 2 . 5 μl and 5 μl of the extracted quantity of dna are used for this purpose ( without the concentration being determined ); additions : primer 1 : 100 ng , primer 2 : 100 or 200 ng , dntps : in each case 10 mm ; 5 μl of taq polymerase buffer ( 10 - fold , without mgcl 2 ); 7 μl of mgcl 2 ( 25 mm stock solution , corresponds to 3 . 6 mm ); 0 . 4 μl of taq gold polymerase ( corresponds to 2 units ). the preparation is made up to a total volume of 50 μl . the pcr is performed in an mj - research thermocycler ( ptc 200 ); set heating rate : 1 ° c ./ sec . the pcr amplification takes place over 40 cycles [ 10 min . 95 ° c . ( heating , only in the first cycle ); 30 sec . 95 ° c . ; 30 sec . 55 ° c . ; 1 min . 72 ° c . ; 5 min . 72 ° c . ( cooling , only in the last cycle )]. for the purpose of nonspecifically detecting an hpv infection ( screening ), preference is given to using the sequences seq id no . 1 ( forward ) and seq id no . 2 ( backward ) as the primer pair ( 100 ng in each case ). the nucleotide sequences of these primers , and their position in the hpv genome ( hpv16 as an example ) are : if this is to be followed by a typing , for example by means of dna sequencing , preference is then given to using the sequences seq id no . 1 ( forward ) and seq id no . 3 ( backward ; 200 ng ) as the primer pair : where y is a pyrimidine ( t or c ), x is amino ( a or c ) and r is a purine ( g or a ). in the case of the backward primers seq id nos . 2 and 3 , the positions which are given are those of the anticoding dna strand , to which these primers are reverse and complementary . the sequencing of the amplificate from example 2 , for the purpose of identifying the hpv type , is carried out using the abi big dye terminator cycle sequencing ready reaction kit containing ampli - taq and using 200 ng of primer seq id no . 1 or seq id no . 3 and the pcr amplification preparation . this latter has previously been concentrated and purified through microcon 100 columns ( millipore ). approx . 50 % of the purified preparation is used for the sequencing . the sequencing pcr reaction is carried out in accordance with the following conditions : 10 sec . 96 ° c ., 5 sec . 55 ° c ., 4 min . 60 ° c ., 30 cycles , with a heating rate of 1 ° c ./ sec . there then follows a precipitation with 0 . 3 m sodium acetate and 2 . 5 times the volume of ethanol . the pellet is taken up in 25 μl of tsr ( template suppression reagent from abi ), incubated at 90 ° c . for 2 min . and , after that , brought to 4 ° c . for 2 min . and subsequently kept at room temperature . the capillary electrophoresis is carried out with the aid of the abi prism 310 automated sequencing appliance and using a 47 cm capillary ( diameter 50 μm ), and is analyzed using the abi 310 genetic analyser program . the polymer employed is the abi polymer pop 6 ( performance optimized polymer 6 ). when the primers seq id no . 1 and seq id . no . 3 are used , this typing can identify the following hpv types : hpv1 to hpv8 hpv10 to hpv19 hpv21 to hpv28 hpv30 to hpv38 hpv40 hpv42 hpv44 to hpv47 hpv51 to hpv54 hpv56 to hpv60 hpv65 to hpv67 hpv70 hpv72 to hpv73 hpv82 to hpv83 analogous results are obtained when the pcr primer pair . seq id no . 1 and seq id no . 2 is used . due to the smaller amplification product , it is not possible to differentiate between the following hpv types : using a nucleotide sequence from the hpv e1 open reading frame in fig1 , the hpv genome is depicted , by way of examples by the hpv16 genome , which is 7 905 bp in length . the genome is divided into three sections : a noncoding region ( lcr , long control region ), an e ( early ) region , which encodes the “ early genes ”, and an l ( late ) region , which encodes the “ late genes ”. the position indicators show the position of the open reading frames . according to the invention , one or more nucleotide sequences from the e1 open reading frame , which encodes an atp - dependent dna helicase , is / are used for detecting hpv such that all the hpv types are thereby detected . it is possible to use such sequences in the form of hybridization probes or also of pcr primers , etc . an hpv infection in the anogenital region , in particular in connection with a disease of the uterine cervix , comes particularly into consideration in this regard . the e1 region is characterized by a high degree of conservation within the known hpv types . the e1 region is therefore particularly suitable for detecting any hpv infection . it has been found that , due to greater variations in the sequence between the different hpv types , falsely negative results can be obtained when the l1 open reading frame is used for detecting hpv . using the e1 region minimizes this risk of erroneous detection . however , the e1 region can also be used for typing the hpv ; the inventor has found that the small differences in sequence are then , surprisingly , sufficient for this purpose . quantitative pcr using the primer pair seq id no . 1 and seq id no . 3 the lightcycler ™ is employed to detect the hpv33 genome using the primer pair seq id no . 1 and seq id no . 3 . for this , ten - fold lc - dna master hybridization fast - start probe - mix ( without mgcl 2 ) is used in accordance with the manufacturer &# 39 ; s instructions and the final concentration of mgcl 2 is adjusted to 4 mm . the quantity of hpv33 dna employed was 30 ng , while the two primers were in each case used in a range from 0 . 45 to 0 . 9 μm . the pcr amplification was carried out in accordance with the following protocol : initial denaturation at 95 ° c ., 10 minutes amplification ( 50 cycles ) of in each case 95 ° c ., 10 seconds , 55 ° c ., 15 seconds and 72 ° c ., 15 seconds . cooling took place at 40 ° c . for 1 minute . in all the steps but one , the heating rates were in each case 20 ° c ./ second ; in the 72 ° c . step from the amplification , the rates were in each case 5 ° c ./ second . using the dye cyber ™ green i , which binds to double - stranded dna , it was possible to demonstrate , as compared with using an hpv plasmid standard , that this method had a sensitivity which still enabled only ten copies of hpv genome per sample to be detected . two sequence - specific dna probes which were labeled with different dyes were used in another test . the sequences of the two probes are selected such that they are hybridized to the target sequence of the amplified dna segment in such a way that the 3 ′ end of one of the probes lies in close proximity to the 5 ′ end of the other probe , with the two dyes being brought close to each other . one of the dyes is a donor dye and is excited by a short - wave - length light source , whereupon it emits fluorescent light at a somewhat longer wavelength . when the two dyes are located close to each other , the energy emitted by the donor dye excites the acceptor dye , which is located on the second hybridization probe and emits a fluorescent light at another wavelength . the 3 ′ probe was labeled with the dye lc - red640 and the 5 ′ probe was labeled with the dye fitc . both the probes were used in a range from 0 . 15 to 0 . 25 μm . the pcr amplification took place in accordance with the manufacturer &# 39 ; s protocol ; in this case , too , it was possible to demonstrate an achievable sensitivity of 10 genome copies per sample employed . comparison between the primer pairs gp5 +/ gp6 + and seq id no . 1 / seq id no . 3 , and the hybrid capture method various cervical smears were investigated for the presence of hpv using the hybrid capture ii hpv dna test supplied by digene corporation , gaithersburg , md ., usa ; this test indicated that 15 samples were high - risk hpv - positive while 24 were high - risk hpv - negative . these samples were also examined for hpv using the primer pair seq id no . 1 and seq id no . 3 and the pcr reaction shown in example 2 . in parallel , these samples were also examined using the gp5 +/ gp6 + primer pair and the reaction conditions specified in the jacobs et al . publication , loc . cit . while eleven out of the 15 hcii high - risk hpv - positive samples were positive with gp5 +/ gp6 +, all 15 of the samples were positive with seq id no . 1 / seq id no . 3 . of the 24 hcii high - risk hpv - negative samples , a further two samples were positive with gp5 +/ gp6 + while as many as seven samples were positive with seq id no . 1 / seq id no . 3 . in all the cases apart from one in which a positive finding was made using seq id no . 1 / seq id no . 3 , it was possible to identify the hpv type which was present by directly sequencing the amplificates . in the case of the total of 13 samples which were positive using gp5 +/ gp6 +, it was only possible to do this in seven cases since patient samples were found to give rise to multiple bands in the gel , something which appeared to point to nonspecific amplificates of cellular genes . in two out of these seven cases the result differed from that which was obtained using seq id no . 1 / seq id no . 3 . the hpv types which were found in this experiment using seq id no . 1 / seq id no . 3 were : 2a , 16 , 18 , 31 , 32 , 33 , 35 , 42 , 45 , 51 , 53 and 72 . these comparative experiments demonstrate that the primer pair seq id no . 1 / seq id no . 3 is markedly more sensitive than the hybrid capture method or a method which uses the gp5 +/ gp6 + probes . in comparison to seq id no . 1 / seq id no . 3 , gp5 +/ gp6 + showed nine falsely negative samples whereas , when compared with seq id no . 1 / seq id no . 3 , the hybrid capture method showed seven falsely negative samples . | 2 |
the objective of the present invention is to provide an equipment that solves the drawbacks associated with those body thermoregulation devices known in the art and , in detail , to provide a body thermoregulation device that features reduced dimensions , high heat transmission energy efficiency and that is applied to the user &# 39 ; s wrist in order to transmit or extract heat . another objective of the present invention is to provide a body thermoregulation device equipped with a body temperature display element that allows the user to adjust the temperature of the body following the display and evaluation of the body &# 39 ; s instantaneous temperature . a further objective of the present invention is to allow for relaxation of the skin by reducing stress and increasing the feeling of wellness thus bringing the energy fields into balance . these and further objectives are achieved by the body thermoregulation device , described below in a preferred embodiment which is not limited by further developments to the patent , with the aid of the attached drawings which illustrate , respectively : fig1 an exploded view of the body thermoregulation device referred to in the present invention ; fig2 a sectional view of the body thermoregulation device referred to in the present invention ; fig3 a view of the body thermoregulation device display . with reference to the attached figures , the device representing the present invention and relating to a body thermoregulation device 1 consists of a case 2 within which are inserted in sequence , starting from the base 22 , a plate made of highly thermally conductive material 3 which is equipped with a temperature sensor 9 , a thermal conduction interface 5 a , a peltier cell 4 , a second thermal conduction interface 5 b , a heat sink 7 , a display 10 which is mounted on a lid 12 which allows for hermetic closure of the case 2 and which is equipped with a glass window 13 designed to protect the display 10 . again , within the case 2 , there are to be found an electronic circuit board 6 and one or more batteries 8 for supplying power to the device 1 ; moreover , said case 2 is held in position by a strap 11 in such a way that the device 1 encircles the wrist w of the user . finally , the case 2 and lid 12 feature holes 24 for locating control buttons 25 that are operatively connected to the electronic circuit board 6 in order to interact with the latter for the setting or modification of the device operating parameters . with reference to the attached figures , the case 2 may furthermore present an opening 21 at its base whose shape corresponds to that of the bottom projection 31 which is positioned on the face 3 a of the plate 3 , said plate being made of highly thermally conductive material . the thickness of said bottom projection 31 coincides with the thickness of the base 22 of the case 2 . the plate 3 made of highly thermally conductive material transmits the heat from the peltier cell 4 to the skin , or vice versa . to this aim , the plate 3 is made of highly thermally conductivity material , such as aluminium for example , and is in contact with the skin , by which means heat exchange occurs whenever the device 1 is worn . in the absence of the opening 21 , the base 22 of the case 2 may be closed and placed in contact with a face 4 a of the peltier cell 4 . in order to increase heat exchange , thermal conduction interfaces 5 a and 5 b may be present which serve to enclose the peltier cell 4 ; in particular the interfaces 5 a and 5 b are designed to increase the thermal exchange between the peltier cell 4 and the plate 3 , made of highly thermally conductive material , and between the peltier cell 4 and the heat sink 7 , the latter also being in contact with the peltier cell 4 . as previously mentioned , the peltier cell 4 is a thermoelectric device comprising a plurality of “ peltier ” effect junctions which together constitute a solid state heat pump , wherein one surface absorbs heat while the other produces it and the direction in which the heat is transferred depends on the direction of the continuous current applied across the cell itself . the electronic circuit board 6 comprises all of the components required in order to correctly manage the operation of the device . therefore it is operatively connected to the display 10 , temperature sensor 9 , peltier cell 4 , control buttons 25 and is powered by the battery 8 . the electronic circuit board performs the following tasks : by means of the sensor 9 it measures the skin temperature and stores the measured value in memory , it performs algebraic and comparison operations , it activates the peltier cell 4 resulting in heat exchange , and sends temperature and functional information to the display 10 . the electronic circuit board 6 is also capable of interpreting control signals derived from the buttons 25 . the display 10 reveals all of the information relating to the operation of the device including the temperature measured , information about the current date and time , as per a common digital clock , and allows for programming of the thermal functions . more specifically , the display 10 reveals the following information : time 101 , date 102 , reference skin temperature 103 , instantaneous skin temperature 104 , battery charge level 105 , thermal function state ( on / off ) and thermal function mode ( heating / cooling ) 106 and the minimum 107 and maximum 108 temperatures . furthermore , the display 10 is programmed in such a way as to vary its colour as a function of the reference temperature and as a function of the thermal function mode . the heat sink 7 allows some of the heat produced by the peltier cell 4 to be dissipated toward the outside of the device 1 . once placed in position on the wrist and activated , for a predetermined period of time “ t ”, lasting 10 hours for example , the body thermoregulation device 1 begins a preliminary body temperature acquisition phase during which period the skin temperature is measured every “ n ” intervals over a predetermined duration of time “ t1 ”, such as for example on the hour during the 10 hours of the learning phase . the reference temperature measurement phase is managed by the electronic circuit board 6 which , to this aim , stores in memory the values measured by the temperature sensor 9 , said sensor being in contact with the skin . at the end of the temperature acquisition phase , the electronic circuit board 6 calculates the average temperature ( also referred to as the reference temperature “ tr ”) whose value 103 is then revealed on the display 10 . the reference temperature tr , which is the average of the temperatures measured during the period t of the acquisition phase , is constantly updated by further temperature measurements occurring at a predetermined time interval “ t2 ”, for example after every hour from the last reference temperature tr measurement event . therefore , in the example above , the new reference temperature tr will be the result of the average of the temperatures measured over the last 10 hours excluding the most chronologically distant measurement and including instead the most recent measurement . the device 1 thus constantly updates the reference temperature tr during use . other then when the device is placed in position on the wrist and activated , the reference temperature tr acquisition phase can also be manually initiated via a reset button . during said reference temperature tr acquisition phase , in order to allow for stabilisation of the temperature at the plate 3 made of highly thermally conductive material of the device 1 with respect to that of the skin , the peltier cell 4 thermal heat transfer function is deactivated . moreover , at this stage , an icon 106 appears on the display 10 , for example an hourglass , indicating that the device 1 is occupied with the reference temperature acquisition phase . when the device is not worn , the reference temperature and minimum / maximum temperature calculation process carried out by the electronic circuit board 6 is interrupted ; the device will start making measurements again when it is once more in position on the wrist . to this aim there is a sensor 111 on the strap 11 that the electronic circuit board 6 uses to detect whether or not the device 1 is being worn . whenever the strap 11 is closed , a reactivation request or else a thermal function request will appear on the display 10 . the strap 11 can furthermore take the form of a strap with a velcro 112 , buckle or deployante buckle closure element . skin temperature measurements can also be performed manually by means of a dedicated control button 25 . the body thermoregulation device 1 features two operating modes : a first mode that aims to maintain the body temperature close to the reference temperature tr , and a second mode that can only be activated when the first mode is deactivated and that causes the peltier cell to be activated cyclically over a given time interval “ t4 ”. said cyclic activation can be programmed to either only heat or only cool the surface of the skin which is in contact with the bottom of the plate 3 . an “ automatic ” mode is also included wherein the device 1 alternately heats and then cools for a predetermined period of time . in order to avoid false temperature measurements , when the peltier cell 4 is active and simultaneously a reference temperature measurement is being performed at the end of the temperature range “ t1 ”, then before the temperature measurement is carried out by means of the temperature sensor 9 the electronic circuit board 6 first disables the peltier cell 4 . the device also features a button 25 which allows the user to reset the reference temperature “ tr ” at any time thereby restarting the reference temperature learning phase . as mentioned previously , the device features two operating modes , in the first case after the previously set time interval “ t3 ” has elapsed the electronic circuit board 6 , by means of the temperature sensor 9 , performs an instantaneous temperature measurement “ ts ”, whose resulting value 104 also appears on the display 10 , and compares it with the reference temperature “ tr ”. if the difference is greater or less than a given hysteresis value ( e . g . a default value of 0 . 5 ° c . that can be manually set with increments of 0 . 5 ° c . to 2 ° c .) the electronic circuit board 6 will activate the peltier cell 4 as a function of heating or cooling so as to rebalance the body temperature . the peltier cell 4 thermal functions will only be deactivated when the measured temperature ts is re - established , or else returns to within the hysteresis value set for the reference temperature ts = tr . alternatively to the first thermal operating mode , the electronic circuit board 6 can control the device 1 in such a way that after a predetermined number of hours the peltier cell 4 is activated for a given period of time “ t4 ”. in this operating mode the device firstly heats for a given duration and then , after a time interval , the device cools for the same duration . alternatively , the device can be set for a single heating or cooling cycle that will last for a manually preset duration . in this operating mode the new temperature to be reached and maintained becomes the preset temperature “ tp ” which may be n - degrees higher or lower , up to the maximum difference in temperature guaranteed by the device . to this end the preset temperature “ tp ”, as chosen by the user , is set by means of the control buttons 25 that the device 1 features . following this logic the thermal functionality automatically turns off after a given interval at which point the temperature to be maintained returns to that of the reference temperature tr . a schematic example is given of the operating phases of the device together with the defined time intervals : 0 ) the reference temperature tr learning phase has a total duration t of 10 hours during which the temperature is measured at every interval t1 ( i . e . on the hour ), at which point in time the peltier cell 4 is turned off so as not to influence the measurement itself . 1 ) once the reference temperature tr has been calculated , then at each successive interval t2 , after 2 seconds for example , the instantaneous temperature ts is measured and used to maintain the reference temperature tr ( tr = ts ) by means of appropriately activating the peltier cell 4 . 2 ) after a predetermined time interval , for example 55 minutes , the peltier cell is then deactivated . 3 ) after a further fixed time interval , for example 5 minutes , a temperature measurement is made in order to update the average calculated over the preceding 10 hours , i . e . the reference temperature tr , at which point the display is updated with the most recently measured temperature ts 104 and with the new reference temperature tr 103 . 4 ) if for example two hours have passed since the last activation of the peltier cell 4 , and the device 1 thermal operating mode is set such that the peltier cell 4 is cyclically activated after a set number of hours for a predetermined period of time , then the device either continues from phase five or else recommences from phase one . 5 ) the peltier cell 4 is activated in order to either heat or cool with a maximum temperature difference of 3 degrees thus returning the set temperature to the reference temperature tr for example . 6 ) at each successive interval t1 , after 2 seconds for example , the instantaneous temperature ts is measured and used to maintain the reference temperature tr by means of appropriately activating the peltier cell 4 . 7 ) after a predetermined time interval , for example 55 minutes , the peltier cell is then deactivated . 8 ) after a further fixed time interval , for example 5 minutes , a temperature measurement is made in order to update the average calculated over the preceding 10 hours , i . e . the reference temperature tr , at which point the display is updated with the most recently measured temperature ts 104 and with the new reference temperature tr 103 and then the device recommences from phase four . the time interval durations t , t1 and t2 , the number of intervals n and the temperature tr are illustrative and may be different than those described and set by the user . | 0 |
referring to fig1 , a processor - based system 10 may be coupled to a standby system 12 . in one embodiment of the present invention , the processor - based system 10 and the standby system 12 may be contained within the same housing . thus , the user may not appreciate that two distinct processor - based systems are provided . the processor - based system 10 may be any conventional computer system , including a laptop or portable computer system operable from a battery . the processor - based system 10 may include a real time clock ( rtc ) 14 and an information manager application 16 such as a personal information manager ( pim ) application . a driver 20 may drive a speaker 22 in accordance with one embodiment of the present invention . an application program 24 may act as an interface between the application 16 and the standby system 12 . while the present invention is described in connection with an embodiment in which a personal information management ( pim ) application utilized , the present application is applicable to systems which involve time sensitive data which may come in a variety of different types of information including time information and time sensitive alerts as additional examples . thus , it is not essential that the information be associated with a pim application in particular . the standby system 12 may be coupled to the processor - based system 10 by an appropriate link . in embodiments in which separate housings are utilized for the systems 10 and 12 , a tethered connection may be provided between the systems 10 and 12 . in other embodiments , the systems 10 and 12 may be coupled by a airwave communication link , such as a infrared link , a radio link or a cellular telephone link . in some embodiments of the present invention , the standby system 12 may use the same power supply as the system 12 . in the case where the processor - based system 10 is run from a battery , the standby system 12 may also be operated from the same battery . in addition , in some embodiments , the standby system 12 may be coupled to the real time clock 14 of the processor - based system 10 so that timing is synchronized between the two systems . the processor - based system 10 may store an application 16 , such as a scheduler , a calendar or the like which may receive time sensitive data such as the time for appointments , telephone calls or the like . the application 16 may be user programmed to give a visible or audible alert at a preprogrammed time . in order to ensure that this information is always available for notification to the user , the application 16 information may be transferred to the standby system 12 . this transfer of application 16 information may be implemented in a variety of ways . it may be implemented automatically in response to an indication that the processor - based system 10 is about to be powered off . alternatively , every time a given type of information is stored on the processor - based system 10 in association with the application 16 , that information may be automatically transferred to the standby system 12 . for example , whenever the user sets an alert to audibly or visibly notify the user of a given event , information about that alert may automatically be transferred to the standby system 12 . as still another embodiment , the information associated with the application 16 may automatically be transferred at periodic intervals to the standby system 12 . in each case , the expectation is that by automatically transferring the time sensitive data from the processor - based system 10 to the system 12 , upon power off of the system 10 , the data may still be available on the system 12 . the system 12 may include a display 18 in one embodiment of the present invention that may be operated even when the processor - based system 10 is in its power off state . in addition , the standby system 12 may operate the driver 20 and speaker 22 to provide an audible indication , at a predetermined time , in keeping with the information provided by the application 16 . in other embodiments of the present invention , the standby system 12 may include its own speaker 22 . through the standby system 12 that is always powered on , the user may be notified of an important activity or event that is stored in his or her application 16 . alternatively , the system 12 may be automatically powered on whenever the processor - based system 10 is about to be powered off . thus , one of the two systems 10 or 12 is always in a powered on state ready to provide time sensitive data , in one embodiment of the invention . referring to fig2 , in accordance with one embodiment of the present invention , software 24 may be stored on the processor - based system 10 , for example a hard disk drive . the flow begins by determining when a power off state is about to occur as indicated in diamond 26 . in such case , any active application 16 task may be transferred to the standby system 12 as indicated in block 28 . thus , events of a particular type may automatically be transferred from the system 10 to the system 12 prior to shut down of the system 10 . the software 24 may extract time sensitive alerts from pim applications in one embodiment of the invention . for example , pre - programmed alerts which are designed to notify the user of a given event may be transferred to the standby system 12 prior to shut off . after transferring the information , the processor - based system 10 may proceed to a power off state , as indicated in block 30 . in other embodiments of the present invention , as described previously , the transfer of time sensitive data to the standby system 12 may be done automatically whenever events of a certain type are preprogrammed . alternatively , the data may be periodically automatically transferred to the standby system 12 . in some embodiments of the present invention , the power consumption of the standby system 12 may be considerably less than that encountered with the overall system 10 . thus , power may be reasonably conserved . turning now to fig3 , software 32 may be stored on the standby system 12 in accordance with one embodiment of the present invention . the software 32 may monitor for pim application 16 information , as indicated in diamond 34 . when pim information or other time sensitive data is transferred , the standby system 12 may be activated automatically . the system 12 may compare the time of the time sensitive data , such as a pim alert , contained in a queue containing one or more time sensitive events , to the information about the current time from the real time clock 14 , as indicated in block 36 . when there is a match , as indicated in diamond 38 , an audio or visible display may be activated as indicated in block 40 . in one such case , an image of the calendar , produced by the pim application 16 , may be displayed on a display 18 or a sound may be produced , for example from the speaker 22 , to alert the user ( block 42 ). after a time out is reached , as indicated in diamond 44 , the flow may be terminated . turning next to fig4 , in accordance with one embodiment of the present invention , the system 10 may be a laptop or portable computer which includes within its housing the system 10 and the standby system 12 . the laptop may include a display portion 46 that folds onto a keyboard portion 48 . the display 18 may be provided on the exterior of the housing of the system 10 , for example on the portion 46 . thus , even though the system 10 is in its closed configuration and is powered off , the user may be notified , for example through the display 18 on the exterior of the housing , of alerts and other time sensitive events . in accordance with one embodiment of the present invention , the standby system 12 may be implemented by a microcontroller 50 which is coupled to the display 18 and to a storage 52 , as shown in fig5 . for example , in one embodiment of the present invention , the storage 52 may store the software 32 . the microcontroller 50 may also be coupled to an interface 53 which in turn may be coupled to the processor - based system 10 . in this way , the systems 10 and 12 may exchange information such as the real time clock information , pim information and signals to the processor - based system 10 and speaker 22 . in one embodiment of the present invention the system 12 may be a cellular telephone linked to the user &# 39 ; s personal computer . on the opposite end of the spectrum , the system 12 may be a server . for example , the system 12 may be an internet server . when the user is about to turn off his or her computer system 10 , for example before going on a trip , the user &# 39 ; s time sensitive data may automatically be transferred to a web site operated by the server . the user can then access the time sensitive data , once stored on the web site , from a computer different from the one originally used to record the pim information . referring to fig6 , the display 18 , in accordance with one embodiment of the present invention , may display a graphical user interface 56 such as a calendar . thus , a plurality of times may be displayed , with a particular meeting time 58 highlighted . in one embodiment user definable information may be scrolled across the display 18 . thus , by exporting the time sensitive data from the application 16 , the user is provided with a portion of his or her overall calendar and given a visual warning of the timed event . turning finally to fig7 , the processor - based system 10 may include a processor 60 coupled to an interface 62 such as a bridge . the interface 62 may be coupled to a system memory 64 and a display controller 66 . a display 68 may be coupled to a controller 66 . an interface 70 may be coupled to the interface 62 as well as to a system bus 72 . the real time clock may be part of the interface 70 . the system bus 72 may be coupled to a storage medium 74 , storing the software 76 for example that implements the pim functions and the software 24 . in addition , the interface 70 may be coupled to a secondary bus 78 coupled to the interface 80 . the interface 80 is coupled to the standby system 12 through its interface 53 . the secondary bus 78 may also couple a bios storage 82 . the software 24 may be part of the bios software stored on the bios storage 82 . the storage 74 may define a time sensitive data queue , controlled for example by the application 24 , for storing a plurality of time sensitive alerts in accordance with one embodiment to the present invention . the queue may be in the form of a content addressable memory ( cam ) with each location associated with a tag indicative of a particular time for action . the queue may be searched to find alerts having a tag indicative of a time that matches the current time , for example obtained from the real time clock . the application 24 may be responsible for gathering time sensitive data from the application 16 , prioritizing that data , ordering the data in the queue and running the queue . the application 24 may also notify the user when the last alert in the queue has been completed . in some cases , the queue depth may be exceeded , for example because the number of timed entries exceeds the capacity of the queue . in such cases , a notification may be provided to the user that the queue depth has been exceeded and that additional entries may not be accepted . this may be accomplished for example , by a suitable graphical user interface . in some embodiments of the present invention , it may advantageous to provide the ability to mute the audible notification so that the user is not disturbed when the user is in a meeting or the like . in such cases , the user may enter a command through the processor - based system 10 which mutes any audible alerts until the mute is released . in addition , it may be desirable to provide a interrupt which allows the user to enter a code into the processor - based system 10 to turn off the on - going display , on the display 18 , of an alert or upcoming timed event . in addition it may be desirable in some cases to turn off the display 18 at any time when the processor - based system 10 is operational to avoid duplicative indications of time sensitive data . while the program 24 is illustrated as being an application program , it may also be implemented as part of an operating system . the program 24 may also be part of a personal information manager application as well . while the present invention has been described with respect to a limited number of embodiments , those skilled in the art will appreciate numerous modifications and variations therefrom . it is intended that the appended claims cover all such modifications and variations as fall within the true spirit and scope of this present invention . | 6 |
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