US20060162822A1 - Capacitor-grade lead wires with increased tensile strength and hardness - Google Patents
Capacitor-grade lead wires with increased tensile strength and hardness Download PDFInfo
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- US20060162822A1 US20060162822A1 US11/388,107 US38810706A US2006162822A1 US 20060162822 A1 US20060162822 A1 US 20060162822A1 US 38810706 A US38810706 A US 38810706A US 2006162822 A1 US2006162822 A1 US 2006162822A1
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- niobium
- wire
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- powder
- silicon
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- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000010955 niobium Substances 0.000 claims abstract description 30
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 29
- 239000003990 capacitor Substances 0.000 claims abstract description 23
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 17
- 239000010703 silicon Substances 0.000 claims abstract description 17
- 238000005272 metallurgy Methods 0.000 claims abstract description 7
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 6
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims abstract description 4
- 239000002184 metal Substances 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 19
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 8
- BFRGSJVXBIWTCF-UHFFFAOYSA-N niobium monoxide Chemical compound [Nb]=O BFRGSJVXBIWTCF-UHFFFAOYSA-N 0.000 claims description 8
- GFUGMBIZUXZOAF-UHFFFAOYSA-N niobium zirconium Chemical compound [Zr].[Nb] GFUGMBIZUXZOAF-UHFFFAOYSA-N 0.000 claims description 8
- 239000000654 additive Substances 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000004845 hydriding Methods 0.000 claims description 3
- 238000003801 milling Methods 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 229910001093 Zr alloy Inorganic materials 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000005096 rolling process Methods 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 238000000137 annealing Methods 0.000 claims 2
- 238000003825 pressing Methods 0.000 claims 1
- 238000004663 powder metallurgy Methods 0.000 abstract description 8
- XBLPLLLUACTLJN-UHFFFAOYSA-N [Pb].[Zr].[Nb] Chemical compound [Pb].[Zr].[Nb] XBLPLLLUACTLJN-UHFFFAOYSA-N 0.000 abstract 1
- 238000002474 experimental method Methods 0.000 description 19
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 12
- 229910001257 Nb alloy Inorganic materials 0.000 description 9
- 238000005245 sintering Methods 0.000 description 9
- LIZIAPBBPRPPLV-UHFFFAOYSA-N niobium silicon Chemical compound [Si].[Nb] LIZIAPBBPRPPLV-UHFFFAOYSA-N 0.000 description 7
- 238000000429 assembly Methods 0.000 description 4
- 230000000712 assembly Effects 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 3
- 238000009694 cold isostatic pressing Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- PYLYNBWPKVWXJC-UHFFFAOYSA-N [Nb].[Pb] Chemical compound [Nb].[Pb] PYLYNBWPKVWXJC-UHFFFAOYSA-N 0.000 description 1
- 238000009795 derivation Methods 0.000 description 1
- 238000010294 electrolyte impregnation Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000003116 impacting effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/008—Terminals
- H01G9/012—Terminals specially adapted for solid capacitors
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
- H01G9/052—Sintered electrodes
- H01G9/0525—Powder therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
- H01G9/052—Sintered electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/15—Solid electrolytic capacitors
Definitions
- the invention relates generally to capacitor lead wires, more particularly to niobium lead wires usable with anode compacts of tantalum or niobium.
- the invention includes niobium powder metallurgy derived lead wires of niobium doped with silicon, preferably having improved strength and hardness without significant detriment to electrical leakage rating of the wire.
- Niobium and niobium alloy lead wires with melt source derivation have been used as capacitor lead wires.
- Pure niobium wires of melt process origin have low electrical leakage at sintering temperatures of 1150° C. and above.
- the wires are limited in tensile strength and hardness, which make them difficult to work with; this results in low production through put when bonding the wires to the capacitor anode compacts and/or in the course of sintering the compact or prolysis of solid electrolyte with the lead wire attached.
- Niobium alloys, such as niobium-zirconium have better tensile strength then pure niobium wires of melt process origin and acceptable electrical leakage above 1150° C. However above 1050° C. zirconium diffuses off the wire and contaminates the anode, making it unacceptable as a capacitor lead wire.
- the invention relates to a process for making a capacitor grade silicone-doped niobium lead-wire comprising (a) forming a low oxygen niobium powder by hydriding a niobium ingot or a niobium bar and grinding or milling the ingot or the bar, and thereby making a powder having a Fisher Average Particle Diameter particle size range of less than about 150 microns, (b) dehyriding the powder, and optionally deoxidizing the powder, forming a low oxygen niobium powder, (c) blending the low oxygen niobium powder with a silicon additive powder and compacting the powder by cold isostatic pressing to a bar; (d) thermomechanically processing the bar into a rod, and (e) subjecting the rod to a combination of rolling and cold drawning steps, and forming the silicon doped wire.
- the invention also relates to a method made from such a process.
- the present invention includes a niobium wire made from powder metallurgy (P/M), containing a silicon additive of less than about 600 ppm.
- P/M powder metallurgy
- the amount of silicon ranges from about 150 to about 600 ppm.
- the amount of silicon ranges from about 150 to 300 ppm.
- the invention imparts a controlled, higher mechanical tensile strength in the niobium wire at finish diameter that exceeds capacitor-grade wire formed from niobium and niobium-zirconium alloys derived directly from ingot metallurgy (I/M).
- I/M ingot metallurgy
- the P/M source niobium has oxygen content below 400 ppm, even when silicon is added in an oxide form.
- the P/M derived niobium, and niobium-silicon wires also have increased hardness that exceeds hardness of capacitor-grade wire of I/M niobium and niobium-zirconium wires and electrical leakage within current specifications at sinter temperatures of about 1150° C. and above, or about 1250 and above.
- the P/M source material if sintered at well below about 1150° C. or 1250° C. and above, and/or attached to anode compacts sintered below about 1150° C. or below 1250° C. would have higher leakage. But at about 1150° C. or 1250° C. and above, the differences become minimal.
- FIG. 1 is a chart of the ultimate tensile strength as a function of wire diameter of select niobium and niobium alloy wire of the present invention derived from powder metallurgy compared to niobium and niobium alloy wire derived from ingot metallurgy;
- FIG. 2 is a chart of electrical DC leakage as a function of sintering temperature of select niobium and niobium alloy wire of the present invention derived from powder metallurgy compared to niobium and niobium alloy wire derived from ingot metallurgy;
- FIG. 3A-3F are side and front views of examples of capacitor lead wires bonded to anode compacts.
- FIG. 4 is a chart of electrical DC leakage as a function of sintering temperature of select niobium and niobium alloy wire of the present invention derived from powder metallurgy compared to niobium and niobium alloy wire derived from ingot metallurgy.
- Niobium powders are formed by hydriding an ingot or bar of niobium and grinding or otherwise milling the ingot or bar to create a powder at a size range of less than 150 microns FAPD (Fisher Average Particle Diameter), dehyriding and deoxidating.
- FAPD Fisher Average Particle Diameter
- the hydride-grind process as disclosed in U.S. Pat. No. 3,295,951 of Fincham et al and the deoxidation (with a combined dehydriding deoxidation) is described in U.S. Pat. No. 6,261,337 of Kumar, incorporated herein by reference in their entirety, both said patents are of common assignment with this application and Mr.
- the niobium powder preferably is attained with an oxygen level below 400 ppm, preferably below 200 ppm.
- a silicon additive powder is blended with the low oxygen niobium powder, compacted by cold isostatic pressing (at up to 60 KSI) to a preform billet for extrusion or sinter bar preferably yeilding a bar approximately 1.3 inches diameter.
- the bar is thermomechanically processed to a rod.
- the rod is then rolled (or swaged) and cold drawn, typically with a schedule of reductions and intermediate anneals as follows:
- the rod can be rolled (or swaged) and cold drawn, typically with a schedule of reductions and intermediate anneals as follows:
- the diameter of the wire made in accordance to the invention can range from about 0.005 inches to about 0.1 inches.
- the wire of the present invention can contain other additional ingredients such as other metals or ingredients typically added to niobium metal, such as tantalum, zirconium, titanium, or mixtures thereof. The types and amounts of these additional ingredients can be the same as those used with conventional niobium and would be known to those skilled in the art. TABLE 1 below lists the chemistry of the specimens used in certain Experiments 1-5 of silicon doped niobium wire of powder metallurgy origin as reduced to 0.5 inch diameter and 0.103 inch diameter.
- the niobium-silicon wire had a much higher tensile strength and hardness than the niobium-zirconium wire at about 0.050 inches diameter and below.
- FIGS. 3A-3F Side and front views of examples of niobium-silicon capacitor lead wires of the present invention bonded to anode compacts are illustrated in FIGS. 3A-3F .
- FIGS. 3A and 3B illustrate a niobium-silicon capacitor lead wire 10 butt welded to an anode compact 12 .
- FIGS. 3C and 3D illustrate a niobium-silicon capacitor lead wire 10 imbedded for a length 14 within compact 12 .
- FIGS. 3E and 3F illustrated yet another attachment technique of welding the lead wire 10 to the top 16 of the compact 12 .
- the lead wire 10 of any of FIGS. 3A-3F and/or the compact 12 of any such figures can be circular or flat (ribbon form) or other shapes.
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
Abstract
Description
- The invention relates generally to capacitor lead wires, more particularly to niobium lead wires usable with anode compacts of tantalum or niobium. The invention includes niobium powder metallurgy derived lead wires of niobium doped with silicon, preferably having improved strength and hardness without significant detriment to electrical leakage rating of the wire.
- Niobium and niobium alloy lead wires with melt source derivation have been used as capacitor lead wires. Pure niobium wires of melt process origin have low electrical leakage at sintering temperatures of 1150° C. and above. However the wires are limited in tensile strength and hardness, which make them difficult to work with; this results in low production through put when bonding the wires to the capacitor anode compacts and/or in the course of sintering the compact or prolysis of solid electrolyte with the lead wire attached. Niobium alloys, such as niobium-zirconium have better tensile strength then pure niobium wires of melt process origin and acceptable electrical leakage above 1150° C. However above 1050° C. zirconium diffuses off the wire and contaminates the anode, making it unacceptable as a capacitor lead wire.
- It is an object of the present invention to improve chemical, mechanical, metallurgical, and functional consistency of capacitor grade lead wires.
- It is a further object of the present invention to reduce sintering and bonding problems.
- It is yet a further object of the present invention to improve niobium wire to overcome the above-described disadvantages without significantly impacting the electrical properties of the wire and wire-anode assembly.
- The invention relates to a process for making a capacitor grade silicone-doped niobium lead-wire comprising (a) forming a low oxygen niobium powder by hydriding a niobium ingot or a niobium bar and grinding or milling the ingot or the bar, and thereby making a powder having a Fisher Average Particle Diameter particle size range of less than about 150 microns, (b) dehyriding the powder, and optionally deoxidizing the powder, forming a low oxygen niobium powder, (c) blending the low oxygen niobium powder with a silicon additive powder and compacting the powder by cold isostatic pressing to a bar; (d) thermomechanically processing the bar into a rod, and (e) subjecting the rod to a combination of rolling and cold drawning steps, and forming the silicon doped wire. The invention also relates to a method made from such a process.
- The present invention includes a niobium wire made from powder metallurgy (P/M), containing a silicon additive of less than about 600 ppm. Generally, the amount of silicon ranges from about 150 to about 600 ppm. Preferably, the amount of silicon ranges from about 150 to 300 ppm. The invention imparts a controlled, higher mechanical tensile strength in the niobium wire at finish diameter that exceeds capacitor-grade wire formed from niobium and niobium-zirconium alloys derived directly from ingot metallurgy (I/M). Preferably too the P/M source niobium has oxygen content below 400 ppm, even when silicon is added in an oxide form. The P/M derived niobium, and niobium-silicon wires also have increased hardness that exceeds hardness of capacitor-grade wire of I/M niobium and niobium-zirconium wires and electrical leakage within current specifications at sinter temperatures of about 1150° C. and above, or about 1250 and above. The P/M source material if sintered at well below about 1150° C. or 1250° C. and above, and/or attached to anode compacts sintered below about 1150° C. or below 1250° C. would have higher leakage. But at about 1150° C. or 1250° C. and above, the differences become minimal.
- It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are intended to provide further explanation of the present invention as described.
-
FIG. 1 is a chart of the ultimate tensile strength as a function of wire diameter of select niobium and niobium alloy wire of the present invention derived from powder metallurgy compared to niobium and niobium alloy wire derived from ingot metallurgy; -
FIG. 2 is a chart of electrical DC leakage as a function of sintering temperature of select niobium and niobium alloy wire of the present invention derived from powder metallurgy compared to niobium and niobium alloy wire derived from ingot metallurgy; -
FIG. 3A-3F are side and front views of examples of capacitor lead wires bonded to anode compacts; and -
FIG. 4 is a chart of electrical DC leakage as a function of sintering temperature of select niobium and niobium alloy wire of the present invention derived from powder metallurgy compared to niobium and niobium alloy wire derived from ingot metallurgy. - One of the preferred embodiments of the invention is a lead wire of silicone-doped niobium made as follows. Niobium powders are formed by hydriding an ingot or bar of niobium and grinding or otherwise milling the ingot or bar to create a powder at a size range of less than 150 microns FAPD (Fisher Average Particle Diameter), dehyriding and deoxidating. The hydride-grind process as disclosed in U.S. Pat. No. 3,295,951 of Fincham et al and the deoxidation (with a combined dehydriding deoxidation) is described in U.S. Pat. No. 6,261,337 of Kumar, incorporated herein by reference in their entirety, both said patents are of common assignment with this application and Mr. Kumar as a joint inventor of the present invention. The niobium powder preferably is attained with an oxygen level below 400 ppm, preferably below 200 ppm. A silicon additive powder is blended with the low oxygen niobium powder, compacted by cold isostatic pressing (at up to 60 KSI) to a preform billet for extrusion or sinter bar preferably yeilding a bar approximately 1.3 inches diameter. The bar is thermomechanically processed to a rod. The rod is then rolled (or swaged) and cold drawn, typically with a schedule of reductions and intermediate anneals as follows:
- Annealed at 2500° F. for 1.5 hours;
- Rolled to 0.440 inches diameter;
- Annealed at 2500° F. for 1.5 hours;
- Reduced to 0.103 inches diameter;
- Drawn to 0.0346 inches diameter wire;
- Drawn to a finish diameter.
- Stated in general terms, the rod can be rolled (or swaged) and cold drawn, typically with a schedule of reductions and intermediate anneals as follows:
- Annealed at a temperature ranging from about 2100° F. to about 2700° F. for a time ranging from about 0.5 hours to about 2.0 hours;
- Rolled from a diameter ranging from about 1 inch to about 0.25 inches diameter;
- Annealed at a temperature ranging from about 2100 to about 2700° F. for a time ranging from about 0.5 hours to about 2.0 hours;
- Reduced from about 1 inch to about to 0.075 inches diameter;
- Drawn to a finish diameter.
- The diameter of the wire made in accordance to the invention can range from about 0.005 inches to about 0.1 inches. The wire of the present invention can contain other additional ingredients such as other metals or ingredients typically added to niobium metal, such as tantalum, zirconium, titanium, or mixtures thereof. The types and amounts of these additional ingredients can be the same as those used with conventional niobium and would be known to those skilled in the art. TABLE 1 below lists the chemistry of the specimens used in certain Experiments 1-5 of silicon doped niobium wire of powder metallurgy origin as reduced to 0.5 inch diameter and 0.103 inch diameter.
TABLE 1 PPM C O N Mg Al Si Ti Cr Fe Ni Cu Zr Mo Ta W Experiment # 1 ½″ 88 646 47 114 20 25 20 108 655 157 10 10 20 1388 200 Experiment # 2½″ 90 301 42 106 20 158 20 99 574 133 16 10 20 8374 200 Experiment # 3½″ 54 322 60 120 0.5 13 6.1 45 225 44 4 5 1 3000 5 Experiment # 4½″ 142 358 60 120 1.1 161 5.3 50 255 53 3.5 5 1 10000 7.1 Experiment # 5½″ 58 329 72 95 2.7 306 5.5 45 230 53 7 5 1 20000 7.5 Experiment # 1.103″ 63 173 31 110 2 23 2 140 500 130 4 5 11 1000 55 Experiment # 2.103″ 71 180 28 105 3 163 2 150 675 150 6.4 5 11 10000 85 Experiment # 3.103″ 57 262 49 85 5.2 12 7.5 65 100 55 1.9 5 1 5000 6.8 Experiment # 4.103″ 79 291 52 100 4.1 162 6.1 63 130 65 2.2 5 1 10000 5.7 Experiment # 5.103″ 61 282 59 80 2.8 294 4.9 63 70 55 1.9 5 1 10000 6.5 - Wires were prepared from the silicon master blends presented in Experiments 1-5 of TABLE 1, and sample were taken at various size milestones and tested for tensile strength and hardness (Rockwell hardness B scale, HRB). I/M derived niobium-zirconium wires (prior art) were also tested similarly.
TABLE 2 Prior Art Nb PM Nb PM Nb PM Nb PM Nb PM NbZr Exp. # 1 Exp. # 2Exp. # 3Exp. # 4Exp. # 5Ingot (25 ppm) (150 ppm) (10 ppm) (150 ppm) (300 ppm) Size Hardness Tensil Hardness Tensil Hardness Tensil Hardness Tensil Hardness Tensil Hardness Tensil In HRB KSI HRB KSI HRB KSI HRB KSI HRB KSI HRB KSI 0.6 83.7 73 74.3 75.7 76.5 80.2 0.42 82.4 74.9 73.2 36.7 39.7 43.1 0.266 89.8 74.4 71 74.3 76.9 79.1 0.166 89.1 74.5 76.6 79.9 81 81.1 0.107 87.7 72 81 82 82.5 84.7 0.103 79.2 85.6 86.1 84.4 86.4 87.5 0.0933 68.5 41 80.8 53 76.9 55.6 0.0845 72.3 47 78.7 57.1 79.5 58.32 0.0765 71.6 47.2 81.4 59.72 82.7 62.5 0.0693 72.7 52.8 83.4 62.12 82.4 64.86 0.0627 75.4 55 82.4 68.3 83.7 69.9 0.0568 75.4 55.9 85 72.53 84.3 75.1 0.0514 76.9 62.5 83.7 75.6 85.4 77.7 89 119.88 91.5 122.28 98 125.94 0.0465 77.2 64.4 84 76.1 86.3 78.7 87 124.65 90.5 130.17 96.8 132.48 0.0422 78.3 66.7 85.4 81.28 84.7 82.7 92.5 126.05 91.7 133.49 97.4 132.83 0.0382 79 65.5 86.5 83.5 85.8 84.2 88.3 131.23 93.2 138.43 97.6 137.2 0.0344 85 70.31 88.5 89 85.6 87.7 90 130.57 92.5 143.76 97.5 139.88 0.02878 83.7 71.22 86.5 93.8 87.1 94.6 93 133.74 94.2 142.57 99.6 141.34 0.02634 84.7 72.21 88.5 95.2 88.5 96.3 96.7 150.2 99.7 154.8 99.7 174.64 0.02431 85 72.93 89 101 89.5 99.7 96.4 168.63 98 180.61 98.1 182.2 0.0223 87.3 74.63 89 99.3 89.9 103.3 99.3 178.14 99.4 180.66 100.3 182.4 0.02062 87.6 75.88 90.5 103.4 91.4 106.8 98.8 188.97 100.2 206.86 99.7 192.47 0.01995 87.8 83.56 90.7 112.32 90.7 114.98 99.7 164.45 100.2 172.85 102 158.6 0.0173 85 82.30 90.1 116.8 90.5 117.66 100.5 168.54 101.5 179.12 101.6 166.84 0.01537 86.8 73.36 91 119.56 91.2 121 99.7 172.73 103.6 182.28 102.2 172.94 0.01334 87.8 73.36 90.6 126.95 91 128.43 100 176.76 104.6 187.1 102.2 179.5 - As can be seen from the results in TABLE 2 and
FIG. 1 , the niobium-silicon wire had a much higher tensile strength and hardness than the niobium-zirconium wire at about 0.050 inches diameter and below. - Also, electrical leakage tests (40 volts at 90%) were conducted for wire (wire-anode assemblies in capacitor test conditions) or anodes with select silicon master blends (
Experiments # 1 and #2) and presented inFIG. 2 . The tests were conducted for anode assemblies with lead wires made at various sintering temperatures. As can be seen from the results in TABLE 3 below andFIG. 2 , the niobium-silicon wire is acceptable for use at sintering temperatures of 1250° C. and above, but not lower, complying with the current tantalum capacitor grade wire specification leakage of 0.6 μA/in2 at 1250° C.TABLE 3 (@1250° C.) Leakage μA/in2 niobium ingot 0.1 niobium-zirconium 0.25 Experiment # 10.35 Experiment # 20.6 Specification 0.6 - Side and front views of examples of niobium-silicon capacitor lead wires of the present invention bonded to anode compacts are illustrated in
FIGS. 3A-3F .FIGS. 3A and 3B illustrate a niobium-siliconcapacitor lead wire 10 butt welded to ananode compact 12.FIGS. 3C and 3D illustrate a niobium-siliconcapacitor lead wire 10 imbedded for alength 14 withincompact 12.FIGS. 3E and 3F illustrated yet another attachment technique of welding thelead wire 10 to the top 16 of the compact 12. Thelead wire 10 of any ofFIGS. 3A-3F and/or the compact 12 of any such figures can be circular or flat (ribbon form) or other shapes. - Also, electrical leakage tests (40 volts at 90%) were conducted for wire (wire-anode assemblies in capacitor test conditions) or anodes with select silicon master blends (
Experiments # FIG. 4 . The tests were conducted for anode assemblies with lead wires made at various sintering temperatures. As can be seen from the results in TABLE 4 below andFIG. 4 , the niobium-silicon wire is acceptable for use at sintering temperatures of 1150° C. and above, but not lower, complying with the current tantalum capacitor grade wire specification leakage of 0.6 μA/in2 at 1150° C.TABLE 4 (@1150° C.) Leakage μA/in2 niobium ingot 0.1 niobium-zirconium 0.25 Experiment # 30.09 Experiment # 40.118 Experiment # 50.103 Specification 0.6 - Artifacts of electrolyte impregnation and pyrolysis cathode attachment and packaging all well known to those skilled in the art are omitted from the figures for convenience of illustration
- Other embodiments of the present invention will be apparent to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. It is intended that the specification and examples be considered as exemplary only.
Claims (9)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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US11/388,107 US20060162822A1 (en) | 2003-01-21 | 2006-03-23 | Capacitor-grade lead wires with increased tensile strength and hardness |
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
PCT/US2003/001822 WO2004003949A1 (en) | 2002-01-24 | 2003-01-21 | Capacitor-grade lead wires with increased tensile strength and hardness |
US10/498,174 US7056470B2 (en) | 2002-01-24 | 2003-01-21 | Capacitor-grade lead wires with increased tensile strength and hardness |
WOPCT/US03/01822 | 2003-01-21 | ||
US11/388,107 US20060162822A1 (en) | 2003-01-21 | 2006-03-23 | Capacitor-grade lead wires with increased tensile strength and hardness |
Related Parent Applications (1)
Application Number | Title | Priority Date | Filing Date |
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US10/498,174 Division US7056470B2 (en) | 2002-01-24 | 2003-01-21 | Capacitor-grade lead wires with increased tensile strength and hardness |
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US20060162822A1 true US20060162822A1 (en) | 2006-07-27 |
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US11/388,107 Abandoned US20060162822A1 (en) | 2003-01-21 | 2006-03-23 | Capacitor-grade lead wires with increased tensile strength and hardness |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20100211147A1 (en) * | 2009-02-19 | 2010-08-19 | W. C. Heraeus Gmbh | Electrically conducting materials, leads, and cables for stimulation electrodes |
US20190287730A1 (en) * | 2018-03-15 | 2019-09-19 | Kemet Electronics Corporation | Method to Reduce Anode Lead Wire Embrittlement in Capacitors |
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US3295951A (en) * | 1965-02-02 | 1967-01-03 | Nat Res Corp | Production of metals |
US4235629A (en) * | 1977-10-17 | 1980-11-25 | Fansteel Inc. | Method for producing an embrittlement-resistant tantalum wire |
US6261337B1 (en) * | 1999-08-19 | 2001-07-17 | Prabhat Kumar | Low oxygen refractory metal powder for powder metallurgy |
US6269536B1 (en) * | 1996-03-28 | 2001-08-07 | H.C. Starck, Inc. | Production of low oxygen metal wire |
US6402066B1 (en) * | 1999-03-19 | 2002-06-11 | Cabot Corporation | Method of making niobium and other metal powders |
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US3295951A (en) * | 1965-02-02 | 1967-01-03 | Nat Res Corp | Production of metals |
US4235629A (en) * | 1977-10-17 | 1980-11-25 | Fansteel Inc. | Method for producing an embrittlement-resistant tantalum wire |
US6269536B1 (en) * | 1996-03-28 | 2001-08-07 | H.C. Starck, Inc. | Production of low oxygen metal wire |
US6402066B1 (en) * | 1999-03-19 | 2002-06-11 | Cabot Corporation | Method of making niobium and other metal powders |
US6261337B1 (en) * | 1999-08-19 | 2001-07-17 | Prabhat Kumar | Low oxygen refractory metal powder for powder metallurgy |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20100211147A1 (en) * | 2009-02-19 | 2010-08-19 | W. C. Heraeus Gmbh | Electrically conducting materials, leads, and cables for stimulation electrodes |
DE102009009557A1 (en) * | 2009-02-19 | 2010-09-02 | W.C. Heraeus Gmbh | Electrically conductive materials, leads and cables for stimulation electrodes |
US20190287730A1 (en) * | 2018-03-15 | 2019-09-19 | Kemet Electronics Corporation | Method to Reduce Anode Lead Wire Embrittlement in Capacitors |
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