JP2008542174A - 無機化合物 - Google Patents
無機化合物 Download PDFInfo
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- JP2008542174A JP2008542174A JP2008514010A JP2008514010A JP2008542174A JP 2008542174 A JP2008542174 A JP 2008542174A JP 2008514010 A JP2008514010 A JP 2008514010A JP 2008514010 A JP2008514010 A JP 2008514010A JP 2008542174 A JP2008542174 A JP 2008542174A
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- niobium
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- niobium suboxide
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- 150000002484 inorganic compounds Chemical class 0.000 title 1
- 229910010272 inorganic material Inorganic materials 0.000 title 1
- 239000000843 powder Substances 0.000 claims abstract description 93
- 239000010955 niobium Substances 0.000 claims abstract description 79
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 67
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 64
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000003990 capacitor Substances 0.000 claims abstract description 32
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 239000013078 crystal Substances 0.000 claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims description 32
- 239000002184 metal Substances 0.000 claims description 32
- 239000002243 precursor Substances 0.000 claims description 24
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 12
- 239000001301 oxygen Substances 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 12
- 239000012298 atmosphere Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 9
- 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 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 229910000484 niobium oxide Inorganic materials 0.000 claims description 7
- 239000011164 primary particle Substances 0.000 claims description 6
- 238000009826 distribution Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- 239000011777 magnesium Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 9
- 239000001257 hydrogen Substances 0.000 description 9
- 229910052739 hydrogen Inorganic materials 0.000 description 9
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 8
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 229910052786 argon Inorganic materials 0.000 description 7
- 239000000395 magnesium oxide Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 229910052749 magnesium Inorganic materials 0.000 description 6
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 4
- 229910052715 tantalum Inorganic materials 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- CFJRGWXELQQLSA-UHFFFAOYSA-N azanylidyneniobium Chemical compound [Nb]#N CFJRGWXELQQLSA-UHFFFAOYSA-N 0.000 description 3
- 238000007323 disproportionation reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 238000002411 thermogravimetry Methods 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression 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
- 238000011835 investigation Methods 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- HFLAMWCKUFHSAZ-UHFFFAOYSA-N niobium dioxide Chemical compound O=[Nb]=O HFLAMWCKUFHSAZ-UHFFFAOYSA-N 0.000 description 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 2
- WPCMRGJTLPITMF-UHFFFAOYSA-I niobium(5+);pentahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[Nb+5] WPCMRGJTLPITMF-UHFFFAOYSA-I 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 238000005121 nitriding Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 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 2
- 239000012071 phase Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000000126 substance Substances 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
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910052782 aluminium 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
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000012705 liquid precursor Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 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
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000002821 niobium Chemical class 0.000 description 1
- -1 nitrogen-containing compound Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 239000005518 polymer electrolyte Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
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Classifications
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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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- 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
- C01P2006/10—Solid density
-
- 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
-
- 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
-
- 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
- C01P2006/80—Compositional purity
-
- 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
- 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
-
- 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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- Microelectronics & Electronic Packaging (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Powder Metallurgy (AREA)
- Saccharide Compounds (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Catalysts (AREA)
- Valve Device For Special Equipments (AREA)
- Oscillators With Electromechanical Resonators (AREA)
Abstract
Description
C=(F・ε)/(d・VF)
[式中、Fは前記キャパシタの活性表面積であり、εは五酸化物層の誘電率であり、dは化成電圧1ボルトあたりの絶縁性の五酸化物層の厚さであり、かつVFは化成電圧である]により計算される。五酸化タンタル及び五酸化ニオブについて、前記比ε/dはほぼ等しい(それぞれ1.64及び1.96)が、ε(それぞれ27.6及び41)及びd(それぞれ16.6及び25A/V)はかなり異なる。従って、同じ幾何学構造を有する五酸化物の両方をベースとするキャパシタは同じキャパシタンスを有する。質量当たりの比キャパシタンスは、それぞれNb、NbOx及びTaの異なる密度のために異なる。従って、Nb又はNbOxのキャリア(アノード)構造は、重量の低減が課題の一つである携帯電話で使用する場合に、重量を節約するという利点を有する。コストに関してNbOxはNbよりも適していて、その際、酸素からアノード構造の体積の一部を提供される。
このニオブ金属前駆体は、有利に極めて純粋なNb2O5から還元により得られる。これは、アルミノテルミット還元(aluminothermic reduction)により、つまりNb2O5/Al混合物を点火し、それから酸化アルミニウムを洗い落とし、電子ビーム加熱によりニオブ金属を精製することにより行うことができる。こうして得られたニオブ金属インゴットを、公知の方法で水素の拡散により脆化し、粉砕することにより、チップ状の粒子形状を有する粉末にすることができる。
A1: NH4OH水溶液の添加によりH2NbO7水溶液から沈殿させ、前記沈殿物を分離し、乾燥し、1100℃で空気中で焼成することにより得られる高純度のNb2O5は次の分析データを有する:
Al:1ppm
Cr:<0.3ppm
C:<10pp
Fe:<0.5ppm
K:0.6ppm
Mg:<1ppm
Mn:<0.1ppm
Mo:<0.3ppm
Na:3ppm
Ni:<0.2ppm
Si:14ppm
スコット密度:12.2g/inch3。
Al:2ppm
Cr:<2ppm
C: 12ppm
Fe:<2ppm
K:1ppm
Mo:54ppm
Na:4ppm
Ni:<2ppm
N:<300ppm
O:26.79%
Si:14ppm
BET:0.17m2/g
スコット密度:23.6g/inch3。
Cr:<2ppm
C:<10ppm
Fe:<2ppm
K:1ppm
Mg:28.14%
Mo:41ppm
Na:2ppm
Ni:<2ppm
N:<300ppm
O:18.74%
Si:7ppm。
Al:3ppm
Cr:<2ppm
C:<10ppm
Fe:<2ppm
K:1ppm
H:344ppm
Mg:750ppm
Mo:75ppm
Na:3ppm
Ni:<2ppm
N:<300ppm
O:1.65%
Si:8ppm
BET:4.52m2/g。
実施例1(比較)
前駆体A4(Nb)53.98質量%及び前駆体A1(Nb2O5)46.02質量%を均質に混合し、水素雰囲気中で1400℃に加熱する。この生成物の特性を表1に示す。
前駆体A4(Nb)を、1.5倍の化学量論的量のマグネシウム(酸素含有量に対して)及びNH4Clの5.4質量部(Nb100部当たり)と均質に混合し、反応器中に置く。次いで、前記反応器をアルゴンですすぎ、700℃に90分間加熱した。前記反応器を冷却した後に、不動態化のために空気をゆっくりと充填する。硫酸で洗浄し、すすいだ後に、窒素でドープされたニオブ金属が得られ、これは窒素9600〜10500ppm(平均で9871ppm)を含有する。酸素含有量は6724ppmである。
実施例2を繰り返すが、NH4Clの添加を8.2質量部に増加させる。このニオブ粉末は14730ppmの平均窒素含有量を有する。酸素含有量は6538ppmである。この亜酸化物の生成物の特性を表1に示す。
前駆体A4(Nb)53.95質量部と前駆体A1(Nb2O5)46.05質量部とを均質に混合し、反応器中に置く。この反応器をアルゴンですすぎ、500℃に加熱する。その後に、前記反応器を3回80%Ar/20%N混合物でそれぞれ30分間すすぐ。この後に、粉末混合物を1450℃に水素雰囲気中で加熱する。この生成物の特性を表1に示す。この粉末のX線回折パターンを図2に示す。明らかに、矢印で示された2Θ=38.5°でのNb2N(101)ピークを確認することができる。
前駆体A3(MgO含有Nb)を窒素ガスで630℃で窒化し、その後に酸化マグネシウム及び残留するマグネシウム金属を15%硫酸で洗浄することにより除去する。生じるニオブ金属の酸素含有量は1.6質量%であり、窒素含有量は8515ppmである。
前駆体A2(NbO2)を反応器中のニオブワイヤから製造されたスクリーン上に置く。このスクリーンの下方にはNbO2の酸素含有量に対して1.05倍の化学量論的量のマグネシウムを含有する坩堝がある。アルゴンは、反応器の底部に連続的に導入され、反応器の上部から排出される。次いで、この反応器を約950℃に加熱する。マグネシウムの消費後に前記反応器を575℃に冷却し、窒素を3時間導入する。冷却し、不動態化し及び酸化マグネシウム及び残留マグネシウム金属を除去した後に、窒素でドープしたニオブ金属が得られ、これはNbOに変換するために使用することができる。
実施例1(比較)、2及び3のそれぞれの粉末50gを、150×30mmのアレイで0.1mmの厚さのニオブシート上に配置した。この粉末アレイを一端で点火し、完全に燃焼する時間を測定した(空気中で)。
実施例2の粉末:燃焼時間6分25秒、
実施例3の粉末:燃焼時間8分10秒。
実施例1の試料及び実施例2の試料を、空気中で25℃から600℃に加熱し、質量の増加を熱重量分析(TGA)により測定した。同時に、それと共に生じる熱流を、DSC法により測定した。図4は、実施例1(比較)の粉末についてのそれぞれの曲線を示し、図5は、実施例2の粉末についてのそれぞれの曲線を示す。この図中で、それぞれ時間(水平方向のスケールはそれぞれ0〜50及び60sec)に関して、曲線Aは温度(左内側のスケールは0〜600℃)を表し、曲線Bは質量%(左外側のスケールは95〜125%)を示し、曲線Cは質量で補正した熱流(左側のスケールは0〜120W/g)を表す。両方の試料は、約200℃より上で僅かな熱の上昇で僅かな質量の増大を示す。約450℃までの質量の増大及び発熱性の熱は両方の試料について極めて類似している。約450℃より上で、窒素不含の試料は、重量の急激な増加及び対応する熱の著しい上昇を生じる(図5)、他方で窒素含有試料については、熱の上昇及び重量の増加率は、発熱性のピークなしで450℃より上でも適度である。
実施例1(比較)及び実施例2のNbOx粉末をそれぞれ、軸方向に配置されたタンタルワイヤの周囲で、4.1mmの直径及び4.2mmの長さを有する円筒形の圧縮モジュール内に充填する。この粉末を、2.8g/cm3の密度を有する圧粉体に圧縮する。この圧粉体をニオブタブレット上に置き、10-8barの真空中で20分の保持時間で1460℃に加熱する。
このアノードを85℃の温度で0.1%のリン酸水溶液(導電率8600μS/cm)中に浸漬し、電圧が急激に低下する(破壊電圧)まで化成のために150mAの定電流を供給する。実施例1(比較)の粉末から製造されたアノードは、96Vで急激な電圧の低下が生じるが、実施例2の粉末から製造されたアノードは、104Vで急激な電圧の低下が生じる。
工業生産ラインで、キャパシタを実施例1(比較)の粉末並びに実施例2の粉末から製造した。この粉末を、直径4.2mm及び長さ4.1mmの圧縮モジュール中で、中央に配置されたタンタルワイヤの周囲で、2.8g/cm3の圧縮密度で圧縮する。この圧粉体を10-8barの真空中で焼結させる。このアノード構造は16Vの化成電圧で陽極酸化され、MnO2カソードを設ける。このアノードを、以後に示されているように一定温度でかつ使用電圧の交流で運転する。50個のキャパシタをそれぞれ並列で次の試験で運転した。
Claims (15)
- 500〜20000ppmのバルク窒素含有量を有する亜酸化ニオブ粒子を有する、亜酸化ニオブ粉末。
- 窒素含有量が1000〜8000ppm、有利に3000〜5000ppmである、請求項1記載の亜酸化ニオブ粉末。
- 窒素が、少なくとも部分的に、Nb2N結晶又は酸窒化ニオブ結晶の形で存在する、請求項1又は2記載の亜酸化ニオブ粉末。
- Nb2N結晶は、CuKα−X線照射において約38.5°の2シータ角でピークを生じるために十分なサイズを有する、請求項3記載の亜酸化ニオブ粉末。
- 約2Θ=38.5°でのNb2Nピークの高さは、2Θ=30°でのNbOピークの高さの2〜25%である、請求項4記載の亜酸化ニオブ粉末。
- 約2Θ=38.5°でのCuKα1−ピークは0.05〜0.2°の半値幅を有する、請求項1から5までのいずれか1項記載の亜酸化ニオブ粉末。
- 粉末は、ASTM B 822により測定して、50〜90μmのD10値、150〜210μmのD50値、250〜350μmのD90値により特徴付けられる粒度分布を有する、請求項1から6までのいずれか1項記載の亜酸化ニオブ粉末。
- 亜酸化ニオブ粉末粒子は、0.1〜1.5μm、有利に0.3〜1.0μmの平均径の一次粒子のアグロメラートである、請求項1から7までのいずれか1項記載の亜酸化ニオブ粉末。
- 亜酸化ニオブは組成NbOx(0.7<x<1.3)を有する、請求項1から8までのいずれか1項記載の亜酸化ニオブ粉末。
- 1<x<1.033である、請求項8記載の亜酸化ニオブ粉末。
- 酸素含有量が14.5〜15.1質量%である、請求項1から10までのいずれか1項記載の亜酸化ニオブ粉末。
- 粉末50gを厚さ0.1mmのニオブシート上に150×30mmの範囲内で配置して、一端で点火する場合に、5分より長い燃焼時間を有する、請求項1から11までのいずれか1項記載の亜酸化ニオブ粉末。
- 電解キャパシタの製造のための、請求項1から12までのいずれか1項記載の亜酸化ニオブ粉末の使用。
- ニオブ金属粉末前駆体から式NbOx(式中、0.7<x<1.3)の酸化ニオブ粉末を製造する方法において、ニオブ金属前駆体を、酸化ニオブに変換する前に窒化することを特徴とする、酸化ニオブ粉末の製造方法。
- 窒化されたニオブ金属をより高く酸化された酸化ニオブと混合し、還元雰囲気中で酸素濃度の均等化のために十分な温度にかつ十分な時間で加熱することによりNbOxに変換することを特徴とする、請求項14記載の方法。
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US8824122B2 (en) * | 2010-11-01 | 2014-09-02 | Avx Corporation | Solid electrolytic capacitor for use in high voltage and high temperature applications |
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