JP4942090B2 - 球状ニッケル微小粒子の製造方法および異方性導電フィルム用導電粒子の製造方法 - Google Patents
球状ニッケル微小粒子の製造方法および異方性導電フィルム用導電粒子の製造方法 Download PDFInfo
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- JP4942090B2 JP4942090B2 JP2006278219A JP2006278219A JP4942090B2 JP 4942090 B2 JP4942090 B2 JP 4942090B2 JP 2006278219 A JP2006278219 A JP 2006278219A JP 2006278219 A JP2006278219 A JP 2006278219A JP 4942090 B2 JP4942090 B2 JP 4942090B2
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims description 148
- 239000002245 particle Substances 0.000 title claims description 92
- 229910052759 nickel Inorganic materials 0.000 title claims description 68
- 238000004519 manufacturing process Methods 0.000 title claims description 35
- 239000010419 fine particle Substances 0.000 title claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 78
- 239000011859 microparticle Substances 0.000 claims description 47
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 30
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 26
- 239000003638 chemical reducing agent Substances 0.000 claims description 26
- 230000009467 reduction Effects 0.000 claims description 24
- 150000002815 nickel Chemical class 0.000 claims description 21
- 238000001556 precipitation Methods 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 238000009826 distribution Methods 0.000 claims description 15
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 14
- 229910021529 ammonia Inorganic materials 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 239000008139 complexing agent Substances 0.000 claims description 9
- 239000003002 pH adjusting agent Substances 0.000 claims description 5
- 229920005646 polycarboxylate Polymers 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 2
- 238000007747 plating Methods 0.000 description 11
- 238000000034 method Methods 0.000 description 10
- 239000007789 gas Substances 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- 230000002829 reductive effect Effects 0.000 description 9
- 150000003839 salts Chemical class 0.000 description 9
- 239000012298 atmosphere Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 229910001453 nickel ion Inorganic materials 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 239000004033 plastic Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002923 metal particle Substances 0.000 description 3
- 229910052752 metalloid Inorganic materials 0.000 description 3
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 230000001186 cumulative effect Effects 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000011835 investigation Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241000080590 Niso Species 0.000 description 1
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- RJTANRZEWTUVMA-UHFFFAOYSA-N boron;n-methylmethanamine Chemical compound [B].CNC RJTANRZEWTUVMA-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- -1 for example Substances 0.000 description 1
- 238000009689 gas atomisation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229940078494 nickel acetate Drugs 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
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229940053662 nickel sulfate Drugs 0.000 description 1
- RRIWRJBSCGCBID-UHFFFAOYSA-L nickel sulfate hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-]S([O-])(=O)=O RRIWRJBSCGCBID-UHFFFAOYSA-L 0.000 description 1
- 229940116202 nickel sulfate hexahydrate Drugs 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 239000006174 pH buffer Substances 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- NIWMEUWZZDPUEQ-UHFFFAOYSA-M sodium;azane;hydroxide Chemical compound N.[OH-].[Na+] NIWMEUWZZDPUEQ-UHFFFAOYSA-M 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
- Non-Insulated Conductors (AREA)
Description
純水に塩化ニッケル六水和物を溶解して、0.6(kmol/m3)のニッケル塩水溶液を5(dm3)作製した。一方で、純水に水酸化ナトリウムと25%アンモニア水をそれぞれ、0.7(kmol/m3)、1.0(kmol/m3)の濃度で溶解したpH調整水溶液を5(dm3)作製した。上記2つの水溶液をよく撹拌混合して、10(dm3)の混合水溶液とした。続いて、該混合水溶液に対して、2.0(質量%)のポリカルボン酸塩を混合し、外部ヒータで加熱しながら200(min−1)の回転速度で撹拌混合を続け、343(K)±1(K)で保持した。この時の混合水溶液のpHを測定すると、10.6の値を示した。
硫酸ニッケル六水和物により、0.6(kmol/m3)のニッケル塩水溶液を5(dm3)作製した。また、水酸化ナトリウム0.9(kmol/m3)と25%アンモニア水0.75(kmol/m3)とで、5(dm3)のpH調整水溶液を作製し、上記2つの水溶液を混ぜ合わせて混合水溶液とした。そして、該混合水溶液に対して、2.0(質量%)のポリカルボン酸塩を混合し、外部ヒータで加熱しながら200(min−1)の回転速度で撹拌混合を続け、333(K)±1(K)で保持を行ない、pHを測定したところ11.5であった。
混合水溶液を作製する際のpH調整水溶液については、それの水酸化ナトリウム濃度を1.1(kmol/m3)とし、アンモニアの添加を行なわなかったことと、この混合水溶液1(L)に対し混合する還元剤水溶液中のヒドラジン一水和物を2.6(mol)とした以外は、本発明例2と同じ条件で、ニッケル微小粒子を作製した。なお、該混合水溶液にポリカルボン酸塩を混合した際の上記pHは11.3であった。そして、得られたニッケル微小粒子について、粒度分布とSEM観察を行なった結果、粒子径d50は21.9μm、d90は38.2μmで、d10は8.2μmであり、粒度分布[(d90−d10)/d50]は1.37であった。そして、SEMで外観を確認したところ、図5の通り、個々の1次粒子のサイズは0.5〜5μmのバラツキがあり、粒子同士が連結されて大きな塊状(2次粒子)となっていた。
Claims (7)
- ニッケル塩の水溶液と、pH調整剤および錯化剤を含んだpH調整水溶液と、還元剤水溶液とを混合して還元析出反応させ、球状ニッケル微小粒子を製造する方法であって、pH調整剤には水酸化ナトリウムおよび/または水酸化カリウムを使用し、錯化剤にはアンモニアを使用し、かつpH調整水溶液に占める水酸化ナトリウムおよび/または水酸化カリウム濃度を0.05〜1.3(kmol/m3)、アンモニア濃度を0.5〜2.0(kmol/m3)とし、ニッケル塩の水溶液とpH調整水溶液の混合水溶液には、該混合水溶液に対して、0.05〜6(質量%)のポリカルボン酸および/またはポリカルボン酸塩を混合することを特徴とする球状ニッケル微小粒子の製造方法。
- ニッケル塩の水溶液に占めるニッケル塩の濃度が、0.1〜3.0(kmol/m3)であることを特徴とする請求項1に記載の球状ニッケル微小粒子の製造方法。
- 還元剤水溶液には、ニッケル塩の水溶液とpH調整水溶液の混合水溶液1(L)に対して、0.5〜7(mol)のヒドラジンおよび/またはヒドラジン一水和物を混合することを特徴とする請求項1または2に記載の球状ニッケル微小粒子の製造方法。
- 還元析出反応を開始させる時のpHが8超のアルカリ性になるように調整することを特徴とする請求項1ないし3のいずれかに記載の球状ニッケル微小粒子の製造方法。
- 球状ニッケル微小粒子は、結晶質構造を有し、粒子径がd 50 :1〜10μmでありかつ、粒度分布が[(d 90 −d 10 )/d 50 ]≦1.0(d 90 、d 10 、d 50 :積算分布曲線において、90体積%、10体積%、50体積%を示す粒子径)であることを特徴とする請求項1ないし4のいずれかに記載の球状ニッケル微小粒子の製造方法。
- 還元析出反応によって得られた球状ニッケル微小粒子に、573(K)以上の加熱処理を行なうことを特徴とする請求項1ないし5のいずれかに記載の球状ニッケル微小粒子の製造方法。
- 請求項1ないし6のいずれかによって製造された球状ニッケル微小粒子の表面に、Auを被覆することを特徴とする異方性導電フィルム用導電粒子の製造方法。
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JP2010043345A (ja) * | 2008-08-18 | 2010-02-25 | Sumitomo Electric Ind Ltd | ニッケル粉末またはニッケルを主成分とする合金粉末およびその製造方法、導電性ペースト、並びに積層セラミックコンデンサ |
JP7344550B2 (ja) * | 2018-12-19 | 2023-09-14 | ユニチカ株式会社 | 鉄ニッケルナノワイヤーの製造方法 |
CN116441528B (zh) * | 2023-03-07 | 2023-09-29 | 畅的新材料科技(上海)有限公司 | 一种超细球状镍粉及其制备方法 |
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JP2003221610A (ja) * | 2002-01-31 | 2003-08-08 | Murata Mfg Co Ltd | ニッケル粉末の製造方法及びニッケル粉末 |
JP2003306659A (ja) * | 2002-04-16 | 2003-10-31 | Tokuriki Kagaku Kenkyusho:Kk | 導電性接着剤 |
JP4451760B2 (ja) * | 2004-11-09 | 2010-04-14 | 財団法人秋田県資源技術開発機構 | 球状NiP微小粒子の製造方法および異方性導電フィルム用導電粒子の製造方法 |
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