JP5630962B2 - 亜酸化ニオブ、亜酸化ニオブの製造方法ならびに亜酸化ニオブを含有するアノードを有するキャパシタ - Google Patents
亜酸化ニオブ、亜酸化ニオブの製造方法ならびに亜酸化ニオブを含有するアノードを有するキャパシタ Download PDFInfo
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- JP5630962B2 JP5630962B2 JP2009062289A JP2009062289A JP5630962B2 JP 5630962 B2 JP5630962 B2 JP 5630962B2 JP 2009062289 A JP2009062289 A JP 2009062289A JP 2009062289 A JP2009062289 A JP 2009062289A JP 5630962 B2 JP5630962 B2 JP 5630962B2
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- Prior art keywords
- niobium
- nbo
- niobium suboxide
- suboxide
- pentoxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000010955 niobium Substances 0.000 title claims description 49
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 title claims description 47
- 229910052758 niobium Inorganic materials 0.000 title claims description 43
- 239000003990 capacitor Substances 0.000 title claims description 17
- 238000004519 manufacturing process Methods 0.000 title description 15
- 229910052751 metal Inorganic materials 0.000 claims description 30
- 239000002184 metal Substances 0.000 claims description 30
- HFLAMWCKUFHSAZ-UHFFFAOYSA-N niobium dioxide Chemical compound O=[Nb]=O HFLAMWCKUFHSAZ-UHFFFAOYSA-N 0.000 claims description 28
- 239000000843 powder Substances 0.000 claims description 24
- 239000001257 hydrogen Substances 0.000 claims description 21
- 229910052739 hydrogen Inorganic materials 0.000 claims description 21
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 17
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 16
- 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 16
- 230000009467 reduction Effects 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 8
- 239000007858 starting material Substances 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 150000002431 hydrogen Chemical class 0.000 claims 1
- 239000011164 primary particle Substances 0.000 description 14
- 239000000203 mixture Substances 0.000 description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 9
- 239000001301 oxygen Substances 0.000 description 9
- 229910052760 oxygen Inorganic materials 0.000 description 9
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 7
- 239000013078 crystal Substances 0.000 description 7
- 229910052749 magnesium Inorganic materials 0.000 description 7
- 239000011777 magnesium Substances 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000000395 magnesium oxide Substances 0.000 description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 5
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- BJDGBXPQVFSQOZ-UHFFFAOYSA-N [O-2].[O-2].[Nb+4] Chemical group [O-2].[O-2].[Nb+4] BJDGBXPQVFSQOZ-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 238000011067 equilibration Methods 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 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
- 239000000047 product Substances 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910052715 tantalum Inorganic materials 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
- 230000007704 transition Effects 0.000 description 2
- 239000013585 weight reducing agent Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012705 liquid precursor 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
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 231100000989 no adverse effect Toxicity 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
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- WTKKCYNZRWIVKL-UHFFFAOYSA-N tantalum Chemical compound [Ta+5] WTKKCYNZRWIVKL-UHFFFAOYSA-N 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 239000003832 thermite Substances 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
Classifications
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Description
C=(F・ε)/(d・VF)
上記式中、Fはキャパシタ表面積を表し、εは誘電率を表し、dは化成電圧のVあたりの絶縁層の厚さを表し、かつVFは化成電圧を表す。誘電率εは五酸化タンタルまたは五酸化ニオブに関してそれぞれ27.6または41であるが、しかし化成電圧dのボルトあたりの膜厚における成長は16.6または25Å/Vであるので、いずれの五酸化物もそれぞれほぼ同じ比ε/d=1.64または1.69を有する。従って両方の五酸化物をベースとするキャパシタは、アノード構造が同じ形状寸法であれば、同じ静電容量を有する。質量に対する比静電容量に関する詳細における些細な違いは、Nb、NbOx(0.7<x<1.3、特に0.95<x<1.1)およびTaの異なった密度により生じる。従ってNbおよびNbOxから製造されるアノード構造は、たとえば1グラムの軽量化も優先される移動電話において使用される場合に軽量化の利点を有する。コストの側面に関してNbOxはNbよりも好ましい。というのもアノード構造の体積の幾分かは酸素によるものだからである。
2Nb2O5+3Nb→5NbO (1)
従ってこの方法は高純度の市販の五酸化ニオブを使用し、かつ該ニオブを高純度のニオブ金属と、いずれも粉末形で理論量に相応させて混合し、かつこれらを、有利には水素を10%まで含有する水素含有雰囲気下で800〜1600℃で数時間処理することを含む。五酸化物および金属の両方にとって、酸素平衡が行われた後で、1μm以下またはわずかにこれを上回る(最小の)断面寸法の所望の一次粒径に相応する一次粒径を有することが有利である。
NbO2+Nb→2NbO (2)
により記載される亜酸化ニオブを製造する。
a)二酸化ニオブNbOyの製造
メッシュ幅300μmのふるいに通過させ、直径約0.7μmの一次粒径およびBET(ASTM D3663)により測定して2.4m2/gの比表面積を有する部分的に凝集した、高純度の球形の五酸化ニオブを使用した。
a)で得られた二酸化ニオブの部を反応器中のニオブワイヤのメッシュの上に装入した。二酸化物の酸素含有率に対して理論量の1.1倍のマグネシウムを炉中のメッシュの下に装入した。反応器をアルゴンで下から上へとパージした。次いで反応器を1050℃に加熱した。8時間後に反応器を冷却し、かつ空気をゆっくり導入して金属表面を不動態化した。
b)で得られたニオブ粉末43質量部およびa)で得られた二酸化ニオブ粉末57質量部を混合し、かつるつぼに導入して縁まで満たした。次いでるつぼを、アルゴン85体積%および水素15体積%からなる気体混合物によりパージされる炉中で2.5時間かけて1380℃に加熱した。
そのつどc)による亜酸化ニオブ粉末103mgを、ニオブ接触ワイヤを取り囲むようにプレス成形金型へ導入し、次いでプレス成形して2.8g/cm3の圧縮密度を有するプレス成形体を形成した。
a)二酸化ニオブNbOyの製造:
使用される出発材料は、<300μmまでふるいをかけた後にBET(ASTM D3663)により測定して2.3m2の比表面積を有する、部分的に凝集させた、高純度の実質的に球形のNb2O5であった。このNb2O5の部を水素流下に60分間で1000℃から1450℃へと上昇する温度で組成NbO2.02の酸化物へと還元させ、かつ次いで1450℃で200分間維持した。二酸化物の比表面積は0.32m2/gであり、かつレーザー回折(ASTM B822)により測定した粒径分布は67μmのD10値、176μmのD50値および284μmのD90値を有していた。
a)で製造した二酸化ニオブの部を反応器中のワイヤメッシュ上に装入し、かつ該ワイヤメッシュの下に理論量の1.2倍(二酸化ニオブのO含有率に対する)のマグネシウムを含有するるつぼをおいた。次いで反応器をアルゴン流下に4時間、900℃に加熱し、この期間の間にマグネシウムを気化させ、かつその上の二酸化ニオブを金属ニオブへと還元した。冷却および不動態化の後、硫酸次いで水により繰り返し洗浄することによって、形成された酸化マグネシウムを形成されたニオブ金属から除去した。
1.従来技術による方法:
b)で製造されるニオブ金属の半分を質量比1:0.95でa)に記載したNb2O5と混合し、かつ次いで炉中で67ミリバール絶対の水素分圧下に3時間、1400℃に加熱した。次いで粉末をメッシュ幅300μmのふるいに通過させた。この方法で得られた亜酸化ニオブ(「粉末A」)は、組成NbO1.01および0.95〜1.1μmの一次粒径(SEM画像から目視で測定)を有していた。比表面積は1.07m2/gであり、かつレーザー回折により測定したD10値は71μm、D50値は165μmおよびD90値は263μmであった。
b)で製造したニオブ金属の残りの半分を質量比1:1.34でa)で製造したNbO2.02の部と混合し、かつ次いで炉中で67ミリバール絶対の水素分圧下に2時間、1210℃に加熱した。得られた亜酸化ニオブ(「粉末B」)は組成NbO0.98および1.13m2/gの比表面積を有していた。SEM画像から目視により測定した一次粒径は平均して1.0μmであり、かつレーザー回折から測定した粒径分布によりD10値は62μm、D50値は158μmおよびD90値は269μmであった。
粉末A:65s/25g、
粉末B:26s/25g。
Claims (4)
- 出発材料である式NbOy[式中、1.8<y<2.1]の二酸化ニオブと、理論量のニオブ金属とを水素の存在下で反応させることによる、式NbOx[式中、0.7<x<1.3]の亜酸化ニオブの製造方法であって、前記二酸化ニオブNbOyを、水素流中での五酸化ニオブの還元により製造し、かつ反応を50〜1100ミリバールの水素分圧で行うことを特徴とする前記方法。
- 水素流が水蒸気不含になるまで前記反応を実施することを特徴とする、請求項1記載の方法。
- ASTM B213により40s/25g超60s/25g以下の流動性を有する、式NbOx[式中、0.7<x<1.3]の亜酸化ニオブ。
- 請求項3記載の亜酸化ニオブの粉末を焼結することにより得られるアノードを有するキャパシタ。
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PT1505611E (pt) * | 2003-07-22 | 2012-01-12 | Starck H C Gmbh | Método para a produção de condensadores |
DE10333156A1 (de) * | 2003-07-22 | 2005-02-24 | H.C. Starck Gmbh | Verfahren zur Herstellung von Niobsuboxid |
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Also Published As
Publication number | Publication date |
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KR101129764B1 (ko) | 2012-03-26 |
JP2009143804A (ja) | 2009-07-02 |
CN1576234A (zh) | 2005-02-09 |
TWI355424B (en) | 2012-01-01 |
CN100404428C (zh) | 2008-07-23 |
TW200516157A (en) | 2005-05-16 |
DE10333156A1 (de) | 2005-02-24 |
CN101298340A (zh) | 2008-11-05 |
EP2078699A1 (de) | 2009-07-15 |
KR20050011700A (ko) | 2005-01-29 |
EP1508550A1 (de) | 2005-02-23 |
DE502004009299D1 (de) | 2009-05-20 |
MXPA04007024A (es) | 2005-03-23 |
US20050019581A1 (en) | 2005-01-27 |
BRPI0402986A (pt) | 2005-05-24 |
ZA200405851B (en) | 2005-09-28 |
EP1508550B1 (de) | 2009-04-08 |
US7341705B2 (en) | 2008-03-11 |
US20090242853A1 (en) | 2009-10-01 |
RU2363660C2 (ru) | 2009-08-10 |
AU2004203208B2 (en) | 2009-07-23 |
PH12008000260A1 (en) | 2006-03-07 |
IL163104A (en) | 2007-10-31 |
AU2004203208A1 (en) | 2005-02-10 |
JP4317091B2 (ja) | 2009-08-19 |
JP2005041774A (ja) | 2005-02-17 |
RU2004122053A (ru) | 2006-01-27 |
PT1508550E (pt) | 2009-05-22 |
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