CN1149296C - 阀金属组合物和方法 - Google Patents
阀金属组合物和方法 Download PDFInfo
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- CN1149296C CN1149296C CNB988054639A CN98805463A CN1149296C CN 1149296 C CN1149296 C CN 1149296C CN B988054639 A CNB988054639 A CN B988054639A CN 98805463 A CN98805463 A CN 98805463A CN 1149296 C CN1149296 C CN 1149296C
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- valve metal
- wire rod
- tantalum
- nickel
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 155
- 239000002184 metal Substances 0.000 title claims abstract description 155
- 238000000034 method Methods 0.000 title claims description 26
- 239000000203 mixture Substances 0.000 title description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 46
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 28
- 239000001301 oxygen Substances 0.000 claims abstract description 28
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000011248 coating agent Substances 0.000 claims abstract description 24
- 238000000576 coating method Methods 0.000 claims abstract description 24
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 23
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical group [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 9
- 239000011777 magnesium Substances 0.000 claims abstract description 9
- 150000003839 salts Chemical class 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 20
- 239000002250 absorbent Substances 0.000 claims description 17
- 230000002745 absorbent Effects 0.000 claims description 17
- 229910052715 tantalum Inorganic materials 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 6
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000005482 strain hardening Methods 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- VIESAWGOYVNHLV-UHFFFAOYSA-N 1,3-dihydropyrrol-2-one Chemical compound O=C1CC=CN1 VIESAWGOYVNHLV-UHFFFAOYSA-N 0.000 claims description 2
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 2
- 239000013543 active substance Substances 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000011575 calcium Substances 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 238000000935 solvent evaporation Methods 0.000 claims description 2
- 230000008719 thickening Effects 0.000 claims description 2
- 125000000129 anionic group Chemical group 0.000 claims 1
- 239000012752 auxiliary agent Substances 0.000 claims 1
- 239000007795 chemical reaction product Substances 0.000 claims 1
- 230000008018 melting Effects 0.000 claims 1
- 238000002844 melting Methods 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 25
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000000654 additive Substances 0.000 abstract description 3
- 230000000996 additive effect Effects 0.000 abstract description 3
- 239000003990 capacitor Substances 0.000 abstract description 3
- 239000012266 salt solution Substances 0.000 abstract description 3
- 150000001450 anions Chemical class 0.000 abstract 1
- 239000008188 pellet Substances 0.000 abstract 1
- 230000002093 peripheral effect Effects 0.000 abstract 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 8
- 238000005245 sintering Methods 0.000 description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 229910052758 niobium Inorganic materials 0.000 description 5
- 239000010955 niobium Substances 0.000 description 5
- -1 sulfate radical Chemical class 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 4
- 238000007669 thermal treatment Methods 0.000 description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 241000370738 Chlorion Species 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 238000007743 anodising Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000006261 foam material Substances 0.000 description 2
- 239000003966 growth inhibitor Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 2
- 150000002926 oxygen Chemical class 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910001257 Nb alloy Inorganic materials 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 241001074085 Scophthalmus aquosus Species 0.000 description 1
- 229910001362 Ta alloys Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
- 150000001241 acetals Chemical class 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 description 1
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 description 1
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 description 1
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 description 1
- 229910001026 inconel Inorganic materials 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- YPJKMVATUPSWOH-UHFFFAOYSA-N nitrooxidanyl Chemical compound [O][N+]([O-])=O YPJKMVATUPSWOH-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 238000005491 wire drawing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S148/00—Metal treatment
- Y10S148/902—Metal treatment having portions of differing metallurgical properties or characteristics
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/12—All metal or with adjacent metals
- Y10T428/12458—All metal or with adjacent metals having composition, density, or hardness gradient
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/12—All metal or with adjacent metals
- Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
- Y10T428/12771—Transition metal-base component
- Y10T428/12806—Refractory [Group IVB, VB, or VIB] metal-base component
- Y10T428/12819—Group VB metal-base component
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Powder Metallurgy (AREA)
Abstract
最好在边缘区域具有第二金属的阀金属制品，如线材，板材或粉材，通过用金属添加物的盐溶液涂敷阀金属并在吸氧剂的存在下加热处理，以从阀金属除去氧和形成金属添加物的金属盐的阴离子而制造。对于钽线材，优选的第二金属是镍。优选的吸氧剂是镁。含镍的钽线材用于提高电解电容器生产中对烧结的压制钽粉片的结合。
Description
发明背景
阀金属(Valve metals)，如钽和铌以稳定的氧化物层为特征，已具有有用的性能，如耐蚀性和电阻，这使这些金属有各种用途，如电解电容器中的阳极材料和某些腐蚀环境中的结构材料。该氧化物层可阻碍阀金属结合，例如阻碍压制阀金属粉末烧结成结合到阀金属引线或接头的片上。当使用细小阀金属粉末获得更高电容时，使用低烧结温度以防止暴露在烧结温度下的表面积过分损失。此外，当在压制粉末中获得满意的颗粒与颗粒结合时，在低烧结温度时颗粒与接线结合可能不完全，以使烧结片在电容器的制造或使用时容易拉脱引线或接头。
发明简述
本发明提供包含第二种金属的阀金属，该第二金属最好在或接近阀金属的边缘部分比在阀金属内部更加富集。这种阀金属可呈各种形式，如线材、包括箔的板材，或包括片状、球状或角状粉末的粒状物。在这些形式中，阀金属中的第二金属富集在阀金属成形物或阀金属制品的边缘。本发明阀金属线材用于电解电容器用阳极的制造，以在该线材与阀金属粉末烧结片之间提供高的结合强度。本发明阀金属板材同样用于形成烧结的阀金属粉末阳极上的接头。
本发明还提供阀金属中添加第二金属的方法，它包括：
(a)用含有第二金属的溶液涂敷阀金属表面；
(b)在吸氧剂的存在下，在足以从所述阀金属中除去氧和能在阀金属边缘区域对阀金属提供第二金属的温度下加热该阀金属和涂层。优选的是，在或接近阀金属的表面提供该第二金属，如在边缘区域，以改进阀金属的表面性能。
具体方案的详述
本文使用的术语“阀金属”指的是钽、铌、包括钽和铌合金的阀金属合金和包含晶粒生长抑制剂，如带有至多约1000ppm的硅或氧化钇的钽，带有锆的铌等的阀金属。与优选富集在边缘区域的第二金属不同，其它阀金属的添加物，如晶粒生长抑制剂和合金元素都是更均匀地分散在整个阀金属中。
本文使用的术语“第二金属”指的是不均匀分散在阀金属中的阀金属的金属组分。使用的第二金属可在周期表IVB、VB、VIB、VIIB和VIII族中选择，它包括钽、铌、镍、钛、锆、钨和铁。对于要结合到烧结钽粉末上的钽产品来说镍是优选的第二金属。
在本发明方法中通过用第二金属的化合物涂敷阀金属表面并在吸氧剂存在下，在足以从阀金属上除去氧并在该阀金属边缘区域能提供该金属的温度下加热该已涂敷的阀金属而将第二金属添加到阀金属中。该吸气剂在除去该涂层中与第二金属有关的阴离子也是有效的。这种方法尤其是用于制造带有第二金属的阀金属线材、粉材和板材。
当使用这种含第二金属的线材作为制备粒化阀金属粉末的烧结阳极用的引线时，可在烧结粉末和引线之间获得高结合强度。预料这种带有对于钽粉最好在低温，如小于1500℃或更低，如在1200-1400℃范围内烧结的阀金属粉末的线材是有用的。
期望阳极片与本发明阳极引线结合的改进将降低(由此改进)该阳极对起动冲击电流的敏感性。然而不希望受理论的限制，我们知道，如果粉末和引线之间的接点形成不良，由此总横截面小的话，则当放电电路开始通电时所存在的起动冲击电流能引起钽电容器破坏。高瞬时电流不得不通过不良的接点，引起高的电流密度和引线与阳极内表面区的电阻加热。该高电流密度和产生的热可引起电容器破坏，甚至可能引起阀金属片着火。由本发明提供的改进的引线与片的结合预期可降低因电流冲击引起的破坏产生。
本发明阀金属板材也预料可用于制造高电容的阀金属粉末的烧结阳极接头。这样，本发明优选的产品是具有改进表面性能，如对阀金属粉末烧结体的结合的第二金属的阀金属线材和板材。该引线直径通常在约100-1000微米(μm)的范围内；板材可以较薄，如约为50μm，并甚至可以是更薄的箔。本发明含第二金属的粉末可用作连接阀金属零件或低温烧结阀金属粉末的结合剂或仅提供金属添加物，如掺杂物到阀金属边缘区域。
由本发明提供的优选的线材和板材具有富集在阀金属产品边缘区域的第二金属，其中边缘区域的厚度取决于第二金属进入阀金属的扩散速度。影响扩散的因素预期可包括第二金属在涂层的每单位表面积的浓度和时间与温度，在该温度下将阀金属进行像暴露在吸氧剂场合下的热处理。在许多情况下最好使富集第二金属的边缘区域尽可能的薄，以提供阀金属的改进的表面性能，而不影响阀金属的整体性能。富集第二金属的薄边缘区域的另一个优点是在使用高表面性能后第二金属的浓度可降低到最小水平，如通过热处理使第二金属易于扩散到第二金属浓度低(如果有)的阀金属体中，如扩散到线材的芯区域或板材的中心区域。本发明优选的情况下富集第二金属的边缘区域可以是离表面1-2微米之内。对于某些用途，边缘区域的第二金属浓度可至多约1％(重量)或更多。基于产品中阀金属的总重量，第二金属的体浓度可在2-2000ppm的范围内。对于某些用途，第二金属的体浓度可为5-200ppm。对于另一些用途，第二金属的体浓度可为5-50ppm。
可将本发明阀金属线材退火(55000-90000psi)(385-540MPa)，不退火的-半硬质(105000-160000)(735-1120MPa)或不退火-硬质(130000-215000psi)(910-1505MPa)。
对于钽有用的第二金属是稳定和耐腐蚀的镍。在钽线材中使用的镍量最好为可提供高性能，即对烧结阀金属粉末的高结合性，同时对成品阳极的电性能不利影响最小的最小量。本发明的优点是，当加热烧结时第二金属，如镍的浓度开始在边缘区域较高，以使粉末易于结合到线材；随着烧结的继续第二金属趋向于从表面扩散到线材的中心，以使边缘区域具有低浓度，以使对电解电容器的电性能没有不利影响。
在本发明方法中优选通过使用含有第二金属的可溶性盐的溶液来形成均匀的第二金属涂层。可将这样的溶液涂敷到阀金属的氧钝化的表面上。该金属溶液可使用有机或水溶液。对于该第二金属的可溶性盐的实用阴离子包括氯离子、硫酸根、碳酸根和硝酸根、实用的有机溶剂包括丙酮、二甲苯、甲醇、乙腈、二氯甲烷、N-吡咯烷酮、二甲亚砜、二甲基乙酰胺、二甲基甲酰胺、甲基乙基酮、乙二醇乙醚等。为有助于在表面形成和保持均匀的涂层，该溶液最好还包括辅助剂，如通常在涂层中采用的粘合剂、增稠剂、调节剂、表面活性剂等。实用的辅助粘合剂包括聚碳酸亚丙基酯、羟基丙基甲基纤维素、聚乙烯醇、聚乙烯醇缩丁醛和聚合胶乳；优选的辅助粘合剂是聚碳酸亚丙基酯。第二金属和辅助剂的浓度取决于可应用的均匀涂层的厚度和所希望的第二金属浓度。该溶液可通过任何已知的方法，如喷涂、刷涂、浸渍等而对阀金属涂敷。对于线材涂层实用的操作包括通过用该溶液饱和的多孔介质或通过该溶液的槽而拉拔该线材。通过使溶液蒸发和/或凝固，如胶凝或交联粘合辅助剂而将该涂层固定。对于线材上固定涂层的实用方法是通过一个对流加热区拉拔该已涂敷的线材，以促使溶剂去除。实用的对流加热区可以是一个带有与室中线材运动方向并流或逆流的加热气流的竖式或卧式管状室。
在本发明方法中，将第二金属化合物涂层固定后，在吸氧剂的存在下，在足以从阀金属除去氧化物层和使阀金属中第二金属还原的温度下加热阀金属产品。实用的吸氧剂是具有对氧比对阀金属更大亲合力的材料。该吸氧剂包括镁、钙、钠、铝、碳、钛和钻。如当第二金属是钛或锆时该吸气剂还必须具有对氧比对第二金属有更高的亲合力。该吸氧剂还可有效地从第二金属盐中获取阴离子。当使用氯化镍作第二金属盐时，镁是优选的吸氧剂。当产品是线材时，该线材可宽松地绕在线轴上，如阀金属线轴上，以使绕轴的线材暴露到含有吸气材料的气相中。该产品最好暴露于真空炉中的吸气材料中，真空炉抽空空气中的氧，并在惰性气体相，如在含氩的气相中有相对高的吸氧剂和镁蒸汽浓度。当镁用作吸氧剂时，除去阀金属表面氧的实用的温度约为800℃。从阀金属除去氧的工艺在本文参考引用的US专利3647420、4722756、4960471和5241481中均可找到。
按本发明制造的阀金属线材一般通过带有吸氧剂的热处理而软化，该软化线材的拉伸强度常常不能满足用来制造电解电容器用阀金属阳极的引线。热处理和使该线材硬化的淬火一般是不利于在电容器操作中使用，由于在这些处理中捕获氧。现已发现，本发明含第二金属的阀金属线材的表面和边缘区域是耐用的，与许多表面涂层不同，可允许将该线材拉拔到减小的直径，并可有效地冷加工该线材，以对电容器引线用途提供足够的强度。在第二金属盐涂层不均匀涂敷，如成条纹的情况下，将产生一些第二金属浓度低的边缘区域，则在拉拔前对线材涂敷氧化物层是有用的，可使拉模磨损减至最小。
上述工艺也可变化，以对阀金属粉末，如尺寸约1-10微米的粉末中提供第二金属。例如，可用第二金属盐溶液涂敷阀金属粉末并干燥，如在流化床中。这样的金属盐涂敷的阀金属粉末可用吸氧剂处理，以使在阀金属粉末中形成第二金属。实用的本发明阀金属粉末可包括含镍的钽粉和含铌的钽粉与含钽的铌粉。含镍的钽粉可用作钽部件的结合剂。含钽的铌粉末可使铌粉具有高的电性能。
下面的实施例说明本发明的一些情况。
实施例1
通过在200ml甲醇中溶解32.4g的氯化镍六水合物并将氯化镍/甲醇溶液慢慢添加到800ml的5重量％聚碳酸亚丙基酯的丙酮溶液中而制备含0.8重量％镍的溶液，上述丙酮溶液是通过将丙酮添加到20wt％从PAC Polymers，Allentown，Pennsylvania购得的QPAC-40-M聚碳酸亚丙基酯的溶液中而制备的。使线材通过用8.0重量％镍溶液饱和的泡沫材料，然后使线材通过带有并流的热空气的一段因康镍合金管以促进溶剂蒸发而涂敷直径约710μm的钽线材。将该具有干燥涂层的线材松绕在钽线轴上并将一些镁粉放在真空炉中的钽容器中。该镁粉的量要足以从钽(线材、线轴和容器)中除去表面氧和从涂层中除去氯离子。从炉中排出空气并用低压(约13Pa)氩气取代。在2小时期间内使温度升高到925℃，以使汽化的镁和已涂敷的线材的表面接触。炉冷后，将空气引入炉中，取出线材并在约20％硝酸和2％氢氟酸的混合酸槽中酸洗，以除去残余的镁、氧化镁和氯化镁。通过热处理使线材软化并使其拉伸强度为530兆帕(MPa)(77000psi)。该线材的全分析表明总镍含量为45ppm。虽然该线材没有镍涂层，但镍量相当于319埃厚的镍表面层。对该线材表面到约1.5-2微米深进行的SEM分析表明，存在镍和钽。将该线材再卷绕并拉拔到直径240微米，以提供拉伸强度为1190MPa(173000psi)的加工硬化线材。该拉拔线材表面的SEM分析也表明镍和钽的存在。通过X-射线分析该线材表面的表面绘图表明钽和镍均匀分散。将已处理的拉拔线材的盘卷在与类似于制备电解电容器中压制钽粉末的烧结片阳极化的条件下进行阳极化。当电流供到浸渍在0.13重量％磷酸中的拉拔线材盘卷时，酸中的气泡表明通过线材表面上的氧化钽短路，防止氧化层的形成。将该线材的另一个盘卷加热到1300℃30分钟，以模拟钽粉末压片的烧结条件。在0.13重量％磷酸中在93℃将已热处理的线材用升高到线端电压为200伏的恒定电流阳极化30分钟，线端电压保持5.5分钟。将阳极化的线材盘卷浸渍在25℃。0.1％磷酸中，并供给180伏电压2分钟，对于阳极化的线材盘卷的直流电流泄漏在0.25-1毫安/厘米2(约1.5-7毫安/英寸2)的范围内。对于对照钽线材(没有第二金属)直流电流泄漏为约0.04毫安/厘米2。
实施例2
以实施例1的方法制造含镍钽线材，只是用泡沫材料对竖直悬挂线材来涂敷镍盐溶液。该线材通过拉拔到直径250微米而加工硬化，并用作电解电容器的烧结钽粉阳极中的引线。在该引线末端周围模压钽粉并将带有压制钽粉的该引线在普通制造条件下烧结。通过从烧结片拉拔该引线来试验结合到引线的粉末质量。按照本发明线材的含镍引线从烧结片拉脱所使用的力要比使用标准钽线材时需要的力大50％。
Claims (19)
1.一种含有镍的钽线材，其中在所述钽材料中镍的浓度在或接近所述钽线材的表面更大，其中镍的存在量为2-2000ppm。
2.按照权利要求1的钽线材，其中，镍的量与钽总量之比在5-200ppm之间。
3.按照权利要求2的钽线材，其中，镍的量与钽总量之比在5-50ppm之间。
4.按照权利要求1的钽线材，其极限拉抻强度大于830MPa。
5.一种将第二金属添加到阀金属的方法，它包括：
(a)用所述第二金属的溶液涂敷阀金属表面；
(b)在吸氧剂存在下，在足以从阀金属除去氧和能在阀金属边缘区域对阀金属提供第二金属的温度下加热阀金属和涂层；
其中所述第二金属是镍，所述阀金属是钽的线材。
6.按照权利要求5的方法，其中，所述涂敷包括将在一种溶剂中的第二金属的盐溶液涂敷到阀金属表面并使溶剂蒸发。
7.按照权利要求5的方法，进一步包括用酸溶液处理含第二金属的阀金属，以除去残余吸氧剂和吸气剂与氧和盐的阴离子的反应产物。
8.按照权利要求5的方法，其中，所述的阀金属为通过拉伸线材到更小的直径以加工硬化的线材形式。
9.按照权利要求5的方法，其中通过该方法，其结果为所述第二金属熔化在该阀金属中。
10.按照权利要求5的方法，其中具有所述第二金属的所述阀金属在所述阀金属的边缘区域呈线材状。
11.按照权利要求5的方法，其中第二金属的存在量为2-2000ppm。
12.按照权利要求6的方法，其中所述的溶剂是有机溶剂。
13.按照权利要求5的方法，其中所述的溶液是有机溶液。
14.按照权利要求5的方法，其中所述的溶液是水溶液。
15.按照权利要求6的方法，其中所述的溶剂是丙酮、二甲苯、甲醇、乙腈、二氯甲烷、N-吡咯烷酮、二甲基亚砜、二甲基乙酰胺、二甲基甲酰胺、甲乙酮、或乙二醇乙基醚。
16.按照权利要求5的方法，其中所述的溶液含有所述的第二金属和助剂、增稠剂、流平剂、表面活性剂、或其组合。
17.按照权利要求5的方法，其中所述的吸氧剂是镁、钙、钠、铝、碳、钛或锆。
18，按照权利要求5的方法，其中所述的吸氧剂是镁。
19.按照权利要求5的方法，其中所述的阀金属和涂层暴露于真空炉中的吸氧剂下。
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1997
- 1997-04-26 US US08/845,736 patent/US6051326A/en not_active Expired - Fee Related
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1998
- 1998-04-23 EP EP98918612A patent/EP0977899A1/en not_active Withdrawn
- 1998-04-23 RU RU99124811/02A patent/RU2224808C2/ru not_active IP Right Cessation
- 1998-04-23 JP JP54711998A patent/JP2002514268A/ja active Pending
- 1998-04-23 AU AU71508/98A patent/AU7150898A/en not_active Abandoned
- 1998-04-23 IL IL13256398A patent/IL132563A0/xx not_active IP Right Cessation
- 1998-04-23 CN CNB988054639A patent/CN1149296C/zh not_active Expired - Fee Related
- 1998-04-23 BR BR9815473-7A patent/BR9815473A/pt not_active IP Right Cessation
- 1998-04-23 KR KR19997009908A patent/KR20010012119A/ko not_active Application Discontinuation
- 1998-04-23 WO PCT/US1998/008170 patent/WO1998049356A1/en not_active Application Discontinuation
- 1998-04-24 TW TW087106356A patent/TW398016B/zh not_active IP Right Cessation
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- 1999-10-25 US US09/426,020 patent/US6231689B1/en not_active Expired - Lifetime
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111524707A (zh) * | 2020-04-28 | 2020-08-11 | 北京安邦特资源技术有限公司 | 钽电容器阳极引线用复合丝材及制备方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| US6517645B2 (en) | 2003-02-11 |
| KR20010012119A (ko) | 2001-02-15 |
| RU2224808C2 (ru) | 2004-02-27 |
| CN1257552A (zh) | 2000-06-21 |
| TW398016B (en) | 2000-07-11 |
| IL132563A0 (en) | 2001-03-19 |
| AU7150898A (en) | 1998-11-24 |
| US20010030005A1 (en) | 2001-10-18 |
| EP0977899A1 (en) | 2000-02-09 |
| WO1998049356A1 (en) | 1998-11-05 |
| JP2002514268A (ja) | 2002-05-14 |
| US6051326A (en) | 2000-04-18 |
| BR9815473A (pt) | 2002-02-19 |
| US6231689B1 (en) | 2001-05-15 |
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