JP4670653B2 - ニッケル微粒子の製造方法 - Google Patents
ニッケル微粒子の製造方法 Download PDFInfo
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- JP4670653B2 JP4670653B2 JP2006012893A JP2006012893A JP4670653B2 JP 4670653 B2 JP4670653 B2 JP 4670653B2 JP 2006012893 A JP2006012893 A JP 2006012893A JP 2006012893 A JP2006012893 A JP 2006012893A JP 4670653 B2 JP4670653 B2 JP 4670653B2
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- fine particles
- nickel fine
- nickel
- sulfur
- sulfate
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims description 174
- 229910052759 nickel Inorganic materials 0.000 title claims description 89
- 239000010419 fine particle Substances 0.000 title claims description 80
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 23
- 229910052717 sulfur Inorganic materials 0.000 claims description 23
- 239000011593 sulfur Substances 0.000 claims description 23
- 239000002245 particle Substances 0.000 claims description 11
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 7
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 7
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical group [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 2
- 235000011151 potassium sulphates Nutrition 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical class OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 2
- WWILHZQYNPQALT-UHFFFAOYSA-N 2-methyl-2-morpholin-4-ylpropanal Chemical compound O=CC(C)(C)N1CCOCC1 WWILHZQYNPQALT-UHFFFAOYSA-N 0.000 claims 1
- 239000011859 microparticle Substances 0.000 claims 1
- 150000003464 sulfur compounds Chemical class 0.000 description 19
- 238000000034 method Methods 0.000 description 16
- 239000000243 solution Substances 0.000 description 15
- 239000000919 ceramic Substances 0.000 description 11
- 238000010304 firing Methods 0.000 description 11
- 239000003985 ceramic capacitor Substances 0.000 description 10
- 238000005245 sintering Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 150000002815 nickel Chemical class 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- -1 nickel hydrogen Chemical class 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000007847 structural defect Effects 0.000 description 2
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 description 2
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- GTKOIJNHZXHJIQ-UHFFFAOYSA-N [N].S Chemical compound [N].S GTKOIJNHZXHJIQ-UHFFFAOYSA-N 0.000 description 1
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 1
- HIVLDXAAFGCOFU-UHFFFAOYSA-N ammonium hydrosulfide Chemical compound [NH4+].[SH-] HIVLDXAAFGCOFU-UHFFFAOYSA-N 0.000 description 1
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 239000012461 cellulose resin Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 description 1
- 229910000342 sodium bisulfate Inorganic materials 0.000 description 1
- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 229940116411 terpineol Drugs 0.000 description 1
- 230000000930 thermomechanical effect Effects 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
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- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Powder Metallurgy (AREA)
- Battery Electrode And Active Subsutance (AREA)
Description
(株)堀場製作所製レーザー回折式粒度分布測定装置LA−500を用いて測定した。(ニッケル微粒子の含有する硫黄量)
誘導結合プラズマ分析(ICP)にて求めた。
ターピネオールに溶解したエチルセルロースをバインダーとして用い、3本ロールを用いて分散、乾燥、粉砕し、500μmの篩を通した後、造粒して試料を調製した。この試料を直径5mmの円柱状ペレットに成形した。セイコー電子工業(株)製TMA320型熱機械式分析装置を用いて、2体積%水素−窒素ガス中、上記試料を5℃/分の速度で1200℃まで昇温し、温度に対する重量変化率を測定して、試料の収縮開始温度と1000℃における収縮率を求めた。
湿式法で製造した平均粒径0.18μmの球状のニッケル微粒子をその0.2重量%に相当する硫黄を含有する硫酸アンモニウム水溶液に加え、5分間攪拌して、スラリーとした後、温風循環型乾燥機に入れ、加熱乾燥し、蒸発乾固させた。このようにして得たニッケル微粒子の有する硫黄量は0.199重量%であった。また、このニッケル微粒子の温度に対する重量変化率を図1に示し、試料の収縮開始温度と1000℃における収縮率を表1に示す。
湿式法で製造した平均粒径0.18μmの球状のニッケル微粒子のスラリーにこのニッケル微粒子に対して0.8重量%に相当する硫黄を含有する硫酸アンモニウム水溶液を加え、5分間攪拌した後、温風循環型乾燥機に入れ、加熱乾燥し、蒸発乾固させた。このようにして得たニッケル微粒子の有する硫黄量は、0.795重量%であった。また、このニッケル微粒子の温度に対する重量変化率を図1に示し、試料の収縮開始温度と1000℃における収縮率を表1に示す。
湿式法で製造した平均粒径0.18μmの球状のニッケル微粒子のスラリーにこのニッケル微粒子に対して0.08重量%に相当する硫黄を含有する硫酸アンモニウム水溶液を加え、5分間攪拌した後、温風循環型乾燥機に入れ、加熱乾燥し、蒸発乾固させた。このようにして得たニッケル微粒子の有する硫黄量は、0.077重量%であった。また、このニッケル微粒子の温度に対する重量変化率を図1に示し、試料の収縮開始温度と1000℃における収縮率を表1に示す。
実施例1で用いたニッケル微粒子に硫酸アンモニウム水溶液による処理を行うことなく、温度に対する重量変化率を測定した。結果を図1に示す。また、このニッケル微粒子の収縮開始温度と1000℃における収縮率を表1に示す。
実施例1で用いたニッケル微粒子を耐圧容器に入れ、これに0.04体積%硫化水素−窒素ガスを1時間導入し、2時間経過した後、ニッケル微粒子を耐圧容器から取り出してニッケル微粒子の有する硫黄量を分析したところ、0.082重量%であった。また、このニッケル微粒子の温度に対する重量変化率を図1に示し、収縮開始温度と1000℃における収縮率を表1に示す。
Claims (3)
- ニッケル微粒子を硫酸塩の水溶液で湿式処理して、ニッケル微粒子に対して0.05〜1.0重量%の範囲の硫黄を含有させることを特徴とするニッケル微粒子の製造方法。
- ニッケル微粒子を硫酸塩の水溶液で湿式処理した後、蒸発乾固させる請求項1に記載のニッケル微粒子の製造方法。
- 硫酸塩が硫酸ナトリウム、硫酸水素アンモニウム、硫酸カリウム又は硫酸アンモニウムである請求項1又は2に記載のニッケル微粒子の製造方法。
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JP2007191771A JP2007191771A (ja) | 2007-08-02 |
JP4670653B2 true JP4670653B2 (ja) | 2011-04-13 |
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Families Citing this family (12)
Publication number | Priority date | Publication date | Assignee | Title |
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JP5067312B2 (ja) * | 2008-08-18 | 2012-11-07 | 住友金属鉱山株式会社 | ニッケル粉末とその製造方法 |
JP2010053409A (ja) * | 2008-08-28 | 2010-03-11 | Sumitomo Electric Ind Ltd | 金属粉末の製造方法および金属粉末、導電性ペースト、積層セラミックコンデンサ |
JP5574154B2 (ja) * | 2010-01-25 | 2014-08-20 | 住友金属鉱山株式会社 | ニッケル粉末およびその製造方法 |
JP5768322B2 (ja) * | 2010-03-19 | 2015-08-26 | 住友金属鉱山株式会社 | ニッケル微粉及びその製造方法 |
JP2011252194A (ja) * | 2010-06-01 | 2011-12-15 | Murata Mfg Co Ltd | 金属粉末とその製造方法および金属粉末を用いた導電性ペーストとそれを用いた積層セラミック電子部品 |
KR20120049026A (ko) * | 2010-11-08 | 2012-05-16 | 삼성전기주식회사 | 황이 코팅된 금속 파우더, 이를 이용한 내부전극용 페이스트, 적층 세라믹 전자부품 및 그 제조방법 |
JP5724822B2 (ja) * | 2011-10-21 | 2015-05-27 | 堺化学工業株式会社 | 含硫黄ニッケル微粒子の製造方法 |
JP5958749B2 (ja) * | 2012-06-22 | 2016-08-02 | 株式会社村田製作所 | 金属粉末の製造方法 |
JP2013067865A (ja) * | 2012-11-12 | 2013-04-18 | Sumitomo Electric Ind Ltd | 金属粉末、導電性ペースト及び積層セラミックコンデンサ |
JP5962562B2 (ja) * | 2013-03-22 | 2016-08-03 | 住友金属鉱山株式会社 | ニッケル粉末とその製造方法 |
JP5826204B2 (ja) * | 2013-03-26 | 2015-12-02 | 大陽日酸株式会社 | 金属微粒子の製造方法 |
JP2014231643A (ja) * | 2014-07-14 | 2014-12-11 | 住友電気工業株式会社 | 金属粉末の製造方法、金属粉末及び積層セラミックコンデンサ用導電性ペースト |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2003055704A (ja) * | 2001-08-13 | 2003-02-26 | Toshiba Corp | 水素吸蔵合金粉末、水素吸蔵合金改質方法、二次電池、ハイブリッドカー及び電気自動車 |
WO2005123307A1 (ja) * | 2004-06-16 | 2005-12-29 | Toho Titanium Co., Ltd. | ニッケル粉末およびその製造方法 |
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Patent Citations (2)
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JP2003055704A (ja) * | 2001-08-13 | 2003-02-26 | Toshiba Corp | 水素吸蔵合金粉末、水素吸蔵合金改質方法、二次電池、ハイブリッドカー及び電気自動車 |
WO2005123307A1 (ja) * | 2004-06-16 | 2005-12-29 | Toho Titanium Co., Ltd. | ニッケル粉末およびその製造方法 |
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