JP5713905B2 - バルブメタル酸化物及びバルブメタル酸化物のアグロメレート粉末、及びその製造方法 - Google Patents
バルブメタル酸化物及びバルブメタル酸化物のアグロメレート粉末、及びその製造方法 Download PDFInfo
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- JP5713905B2 JP5713905B2 JP2011528274A JP2011528274A JP5713905B2 JP 5713905 B2 JP5713905 B2 JP 5713905B2 JP 2011528274 A JP2011528274 A JP 2011528274A JP 2011528274 A JP2011528274 A JP 2011528274A JP 5713905 B2 JP5713905 B2 JP 5713905B2
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- powder
- agglomerate
- niobium
- temperature
- valve metal
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- 238000004519 manufacturing process Methods 0.000 title claims description 21
- 229910044991 metal oxide Inorganic materials 0.000 title claims description 8
- 150000004706 metal oxides Chemical class 0.000 title claims description 8
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 44
- 239000010955 niobium Substances 0.000 claims description 41
- 229910052751 metal Inorganic materials 0.000 claims description 39
- 239000002184 metal Substances 0.000 claims description 39
- 229910052758 niobium Inorganic materials 0.000 claims description 37
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- 239000011148 porous material Substances 0.000 claims description 34
- 239000003990 capacitor Substances 0.000 claims description 31
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 21
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- 238000005245 sintering Methods 0.000 claims description 20
- 230000006835 compression Effects 0.000 claims description 19
- 238000007906 compression Methods 0.000 claims description 19
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 12
- 229910052715 tantalum Inorganic materials 0.000 claims description 12
- 238000003825 pressing Methods 0.000 claims description 11
- 239000001569 carbon dioxide Substances 0.000 claims description 9
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 9
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- 238000001035 drying Methods 0.000 claims description 6
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 3
- 229910001882 dioxygen Inorganic materials 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical class [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 3
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 claims description 2
- 150000003863 ammonium salts Chemical class 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
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- XQQPOQZGOKJHSN-UHFFFAOYSA-N N#[N+][O-].[Nb] Chemical compound N#[N+][O-].[Nb] XQQPOQZGOKJHSN-UHFFFAOYSA-N 0.000 claims 1
- 238000000354 decomposition reaction Methods 0.000 claims 1
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- 229910000484 niobium oxide Inorganic materials 0.000 claims 1
- 238000000859 sublimation Methods 0.000 claims 1
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- 229910001936 tantalum oxide Inorganic materials 0.000 claims 1
- 239000000203 mixture Substances 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
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- 239000001257 hydrogen Substances 0.000 description 7
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
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- 239000007864 aqueous solution Substances 0.000 description 6
- 229910052698 phosphorus Inorganic materials 0.000 description 6
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- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- 229910052804 chromium Inorganic materials 0.000 description 4
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- 229910052731 fluorine Inorganic materials 0.000 description 4
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- 238000010438 heat treatment Methods 0.000 description 4
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- 239000011777 magnesium Substances 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 4
- WPCMRGJTLPITMF-UHFFFAOYSA-I niobium(5+);pentahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[Nb+5] WPCMRGJTLPITMF-UHFFFAOYSA-I 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- 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 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 3
- 229910052753 mercury Inorganic materials 0.000 description 3
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 239000007784 solid electrolyte Substances 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000010405 anode material Substances 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
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- 238000011109 contamination Methods 0.000 description 2
- 238000006392 deoxygenation reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 2
- 238000007580 dry-mixing Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
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- 239000007788 liquid Substances 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- HFLAMWCKUFHSAZ-UHFFFAOYSA-N niobium dioxide Chemical compound O=[Nb]=O HFLAMWCKUFHSAZ-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- AOLPZAHRYHXPLR-UHFFFAOYSA-I pentafluoroniobium Chemical compound F[Nb](F)(F)(F)F AOLPZAHRYHXPLR-UHFFFAOYSA-I 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
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- YRGLXIVYESZPLQ-UHFFFAOYSA-I tantalum pentafluoride Chemical compound F[Ta](F)(F)(F)F YRGLXIVYESZPLQ-UHFFFAOYSA-I 0.000 description 2
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 229910001257 Nb alloy Inorganic materials 0.000 description 1
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 description 1
- 229910001362 Ta alloys Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000002902 bimodal effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
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- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
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- 150000004820 halides Chemical class 0.000 description 1
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- 238000005470 impregnation Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
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- 239000000395 magnesium oxide Substances 0.000 description 1
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- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 1
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- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Images
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
- B22F3/1121—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
- B22F3/1134—Inorganic fillers
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- 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
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/148—Agglomerating
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
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- 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
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- 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
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- H01G9/04—Electrodes or formation of dielectric layers thereon
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- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/24—Obtaining niobium or tantalum
-
- 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
- Y10T29/00—Metal working
- Y10T29/49—Method of mechanical manufacture
- Y10T29/49002—Electrical device making
-
- 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
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
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- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Metallurgy (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Description
A)前駆体粒子の製造
V1:
脱イオン水100lの容器(Vorlage)に、15時間にわたってH2NbF7水溶液75l/hを連続的に、Nb81g/l及び9%のNH3水溶液75l/hという濃度で加え、その結果、pH値は7.6±0.4である。溶液の温度は、63℃に保つ。得られた懸濁液は、圧力濾過ヌッチェによって濾別し、3%のNH3水溶液で、そして引き続き脱イオン水で洗浄する。得られる湿った水酸化ニオブ(V)を24時間、100℃で、乾燥トレーで乾燥させる。得られる水酸化ニオブ(V)は、比表面積が201m2/gであり、球状の形状を有する。
エトキシドニオブ(V)溶液100体積部に、脱イオン水40体積部を撹拌しながら添加する。沈殿した水酸化ニオブ(V)(ニオブ酸)は、ヌッチェを介して濾別し、脱イオン水で洗浄する。引き続き、水酸化ニオブ(V)を17時間、100℃で乾燥させる。この粉末は、比表面積が130m2/gであり、不規則な形状である。
前駆体粒子V1を4時間、500℃で空気中でか焼し、そしてそれからジェットミルでD90が<10μm(超音波処理無しのマスターサイザー)に粉砕する。比表面積が89m2/gのNb2O5が得られる。
脱イオン水100lの容器に、30時間にわたってH2TaF7水溶液75l/hを連続的に、Ta155.7g/l及び9%のNH3水溶液75l/hという濃度で入れ、この際にpH値は7.6±0.4であり、溶液の温度は69℃に維持する。濾別、NH3溶液及び脱イオン水での洗浄、24時間100℃での乾燥後、比表面積が106m2/gの球形状をした水酸化タンタル(V)が得られる。
前駆体粒子V4を2時間、500℃で空気中でか焼し、ジェットミルでD90<10μmに粉砕する。比表面積が83m2/gのTa2O5が得られる。
焼結された五酸化物粉末P1〜P14を製造するため、表1、コラム1に記載した前駆体を使用する。
五酸化物粉末P1〜P14を、五酸化ニオブの場合には、1300℃で水素により二酸化ニオブに還元後、900℃で輸送ガスとしてのアルゴン下、マグネシウム蒸気による還元により6時間、冷却、不活性化、300μm未満へのふるい分け、8%の硫酸による酸化マグネシウムの除去、及び脱イオン水による中性洗浄によって、金属粉末M1〜M14にする。表2には、BET比表面積、マスターサイザー後のD50値(超音波処理無し)と、鉄、クロム及びニッケル、フッ素及び塩素、並びにナトリウム及びカリウムの不純物含分の合計が記載されている。
ニオブ亜酸化物粉末を製造するために、それぞれ表3のコラム1に記載された五酸化ニオブを、表3のコラム2に記載されたニオブ金属の三倍の化学量論、及びコラム3に記載された細孔形成剤(金属と五酸化物に対して20質量%)と乾燥混合し、75barで圧縮し、そして600℃で3時間にわたって細孔形成剤を除去するために温度処理する。
粉末M1〜M8、及びM10〜M14を、脱酸素化のためにそれぞれ、8質量%(ニオブ金属粉末)若しくは5質量%(タンタル金属粉末)のマグネシウム片と混合し、そして燐100ppmドープのために充分な量でNH4H2PO4溶液を混合し、そしてアルゴン下で2時間、850℃に加熱し、冷却して不活性化し、そして<300μmにふるい分けする。粉末M9の2つの試料は850℃及び750℃の温度で脱酸素化し、以降M9a、及びM9bと呼ぶ。表4及び5には、BET比表面積、マスターサイザー後のD50値(超音波処理無し)、鉄、クロム及びニッケル、フッ素及び塩素、並びにナトリウム及びカリウムの不純物含分の合計が記載されている。さらに、圧縮係数α、及び滑り係数η(以下で定義する)、並びに滑り係数η×BET表面積の積が記載されている。
脱酸素化された金属粉末D1〜D14及びニオブ亜酸化物粉末S1〜S8から、直径3.6mm、長さ3.6mmのアノード体を、プレス形態で組み込まれるタンタル線材のために、厚さ0.3mmから、表4、5、及び6に記載された圧縮密度(g/cm3)で圧縮し、引き続き高真空下で20分にわたって表に記載された温度で焼結する。
Claims (13)
- BET比表面積(m2/g)×滑り係数ηの積が0.33〜0.75、好適には0.45〜0.58であり、圧縮係数が0.07超である、ニオブ亜酸化物アグロメレート粉末。
- BET比表面積(m2/g)×滑り係数ηの積が0.62〜0.95、好適には0.65〜0.86であり、圧縮係数が0.08超である、タンタルアグロメレート粉末。
- BET比表面積(m2/g)×滑り係数ηの積が0.38〜0.8、好適には0.42〜0.6であり、圧縮係数が0.08超である、ニオブアグロメレート粉末。
- プレス密度2.8g/cm3にプレスし、1340℃以上の温度で20分間の焼結後に、見かけ密度が88%超、好適には90%超、とりわけ好適には92%超のアノード体が製造可能な、請求項1に記載のニオブ亜酸化物アグロメレート粉末を含有する、コンデンサアノード焼結体。
- プレス密度5g/cm3超にプレスし、1250℃以上の温度で20分間の焼結後に、見かけ密度が92%超のアノード体が製造可能な、請求項2に記載のタンタルアグロメレート粉末を含有する、コンデンサアノード焼結体。
- 請求項1から3までのいずれか1項に記載のアグロメレート粉末の製造方法において、
アグロメレート粉末の前駆体粒子を微粒子状細孔形成剤と混合し、圧縮によって高多孔性の接着結合された前駆体粒子のアグロメレートを生成し、350℃〜600℃に徐熱することにより、細孔形成剤を熱により除去し、接着結合されたアグロメレートを、焼結橋形成に充分な温度及び所要時間の温度処理に供し、この少なくとも部分的に焼結されたアグロメレートを、バルブメタル及び/又はバルブメタル亜酸化物のアグロメレート粉末にさらに加工することを特徴とする、前記製造方法。 - 細孔形成剤として、蒸発温度、昇華温度、又は分解温度が600℃未満のアンモニウム塩を使用することを特徴とする、請求項6に記載の方法。
- 細孔形成剤として、微粒子状の塩化アンモニウム及び/又はシュウ酸アンモニウムを使用することを特徴とする、請求項7に記載の方法。
- 細孔形成剤を、前駆体化合物の体積に対して10〜90体積%の量で使用することを特徴とする、請求項6から8のいずれか1項に記載の方法。
- 請求項1から3までのいずれか1項に記載のアグロメレート粉末の製造方法において、
バルブメタルの、又はニオブ及び/又はタンタルの酸化物、水酸化物、及び水和五酸化物から成る群から選択されるアグロメレート粉末の前駆体粒子を、過酸化水素又は二酸化炭素含有水の中でスラリー化し、乾燥によって酸素ガス若しくは二酸化炭素を放出させながら水を除去し、その結果、高多孔性の接着結合された前駆体粒子のアグロメレートが生成され、この接着結合されたアグロメレートを、焼結橋形成に充分な温度及び所要時間の温度処理に供し、この少なくとも部分的に焼結されたアグロメレートを、バルブメタル及び/又はバルブメタル酸化物のアグロメレート粉末にさらに加工することを特徴とする、前記製造方法。 - 前駆体粒子が、80m2/g超、好適には100m2/g超の比表面積を有することを特徴とする、請求項6から10のいずれか1項に記載の方法。
- 請求項1から3までのいずれか1項に記載のアグロメレート粉末のプレスと焼結により製造される、コンデンサアノード。
- 請求項12に記載のコンデンサアノードを含む、コンデンサ。
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DE102008048614.0 | 2008-09-23 | ||
DE102008048614A DE102008048614A1 (de) | 2008-09-23 | 2008-09-23 | Ventilmetall-und Ventilmetalloxid-Agglomeratpulver und Verfahren zu deren Herstellung |
PCT/EP2009/060912 WO2010034577A1 (de) | 2008-09-23 | 2009-08-25 | Ventilmetall- und ventilmetalloxid-agglomeratpulver und verfahren zu deren herstellung |
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EP (1) | EP2329507B1 (ja) |
JP (1) | JP5713905B2 (ja) |
KR (1) | KR101712678B1 (ja) |
CN (3) | CN102891018B (ja) |
BR (1) | BRPI0918987A2 (ja) |
DE (1) | DE102008048614A1 (ja) |
IL (2) | IL211461A (ja) |
MX (2) | MX351911B (ja) |
PT (1) | PT2329507T (ja) |
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DE102008048614A1 (de) * | 2008-09-23 | 2010-04-01 | H.C. Starck Gmbh | Ventilmetall-und Ventilmetalloxid-Agglomeratpulver und Verfahren zu deren Herstellung |
CN104039483B (zh) | 2011-12-30 | 2017-03-01 | 思高博塔公司 | 涂层组合物 |
US11130205B2 (en) | 2014-06-09 | 2021-09-28 | Oerlikon Metco (Us) Inc. | Crack resistant hardfacing alloys |
EP3234209A4 (en) | 2014-12-16 | 2018-07-18 | Scoperta, Inc. | Tough and wear resistant ferrous alloys containing multiple hardphases |
JP6512297B2 (ja) * | 2015-08-12 | 2019-05-15 | 株式会社村田製作所 | コンデンサおよびその製造方法 |
CA2997367C (en) | 2015-09-04 | 2023-10-03 | Scoperta, Inc. | Chromium free and low-chromium wear resistant alloys |
KR102389784B1 (ko) * | 2018-03-05 | 2022-04-22 | 글로벌 어드밴스드 메탈스 유에스에이, 아이엔씨. | 구형 분말을 함유하는 애노드 및 커패시터 |
AU2019363613A1 (en) | 2018-10-26 | 2021-05-20 | Oerlikon Metco (Us) Inc. | Corrosion and wear resistant nickel based alloys |
DE102019000906A1 (de) * | 2019-02-08 | 2020-08-13 | Taniobis Gmbh | Pulver auf Basis von Niobzinnverbindungen für die Herstellung von supraleitenden Bauteilen |
CN110261459A (zh) * | 2019-06-17 | 2019-09-20 | 北京科技大学 | 一种用于控制气氛中极低氧含量并测量其氧分压的装置 |
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CZ302792B6 (cs) * | 1997-02-19 | 2011-11-09 | H.C. Starck Gmbh. | Práškový tantal, zpusob jeho výroby a z nej získatelné anody a kondenzátory |
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WO2000067936A1 (en) | 1998-05-06 | 2000-11-16 | H.C. Starck, Inc. | Metal powders produced by the reduction of the oxides with gaseous magnesium |
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DE102008048614A1 (de) * | 2008-09-23 | 2010-04-01 | H.C. Starck Gmbh | Ventilmetall-und Ventilmetalloxid-Agglomeratpulver und Verfahren zu deren Herstellung |
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JP2012503343A (ja) | 2012-02-02 |
US9466433B2 (en) | 2016-10-11 |
TWI463510B (zh) | 2014-12-01 |
MX368351B (es) | 2019-09-30 |
US20110170238A1 (en) | 2011-07-14 |
MX351911B (es) | 2017-11-03 |
BRPI0918987A2 (pt) | 2015-12-01 |
MX2011002698A (es) | 2011-04-05 |
EP2329507B1 (de) | 2017-06-07 |
EP2329507A1 (de) | 2011-06-08 |
CN102881460B (zh) | 2017-05-17 |
RU2011115873A (ru) | 2012-10-27 |
IL211461A (en) | 2016-06-30 |
PT2329507T (pt) | 2017-07-19 |
IL245817A0 (en) | 2016-06-30 |
CN102881460A (zh) | 2013-01-16 |
TW201027578A (en) | 2010-07-16 |
RU2542866C9 (ru) | 2015-11-20 |
US20150162137A1 (en) | 2015-06-11 |
US8995112B2 (en) | 2015-03-31 |
KR101712678B1 (ko) | 2017-03-06 |
WO2010034577A1 (de) | 2010-04-01 |
CN102165545A (zh) | 2011-08-24 |
RU2542866C2 (ru) | 2015-02-27 |
CN102165545B (zh) | 2017-03-15 |
IL211461A0 (en) | 2011-05-31 |
KR20110063512A (ko) | 2011-06-10 |
IL245817B (en) | 2018-07-31 |
CN102891018A (zh) | 2013-01-23 |
DE102008048614A1 (de) | 2010-04-01 |
CN102891018B (zh) | 2016-12-21 |
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