JP2010118334A - 導電性粉体及びそれを含む導電性材料並びに導電性粒子の製造方法 - Google Patents
導電性粉体及びそれを含む導電性材料並びに導電性粒子の製造方法 Download PDFInfo
- Publication number
- JP2010118334A JP2010118334A JP2009220045A JP2009220045A JP2010118334A JP 2010118334 A JP2010118334 A JP 2010118334A JP 2009220045 A JP2009220045 A JP 2009220045A JP 2009220045 A JP2009220045 A JP 2009220045A JP 2010118334 A JP2010118334 A JP 2010118334A
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- Prior art keywords
- nickel
- particles
- conductive
- core
- conductive powder
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- 150000001298 alcohols Chemical class 0.000 description 1
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- 150000005215 alkyl ethers Chemical class 0.000 description 1
- 125000005037 alkyl phenyl group Chemical group 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- QUDWYFHPNIMBFC-UHFFFAOYSA-N bis(prop-2-enyl) benzene-1,2-dicarboxylate Chemical compound C=CCOC(=O)C1=CC=CC=C1C(=O)OCC=C QUDWYFHPNIMBFC-UHFFFAOYSA-N 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- RJTANRZEWTUVMA-UHFFFAOYSA-N boron;n-methylmethanamine Chemical compound [B].CNC RJTANRZEWTUVMA-UHFFFAOYSA-N 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- DQXBYHZEEUGOBF-UHFFFAOYSA-N but-3-enoic acid;ethene Chemical class C=C.OC(=O)CC=C DQXBYHZEEUGOBF-UHFFFAOYSA-N 0.000 description 1
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
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- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- YACLQRRMGMJLJV-UHFFFAOYSA-N chloroprene Chemical class ClC(=C)C=C YACLQRRMGMJLJV-UHFFFAOYSA-N 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000000805 composite resin Substances 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000002526 disodium citrate Substances 0.000 description 1
- 235000019262 disodium citrate Nutrition 0.000 description 1
- CEYULKASIQJZGP-UHFFFAOYSA-L disodium;2-(carboxymethyl)-2-hydroxybutanedioate Chemical compound [Na+].[Na+].[O-]C(=O)CC(O)(C(=O)O)CC([O-])=O CEYULKASIQJZGP-UHFFFAOYSA-L 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
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- 125000003700 epoxy group Chemical group 0.000 description 1
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- 230000007717 exclusion Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 description 1
- 239000000174 gluconic acid Substances 0.000 description 1
- 235000012208 gluconic acid Nutrition 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 1
- 229960004275 glycolic acid Drugs 0.000 description 1
- 150000002343 gold Chemical class 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
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- 239000003112 inhibitor Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229920000554 ionomer Polymers 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000006078 metal deactivator Substances 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 229910001463 metal phosphate Inorganic materials 0.000 description 1
- 229910052914 metal silicate Inorganic materials 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000000025 natural resin Substances 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 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
- 150000004767 nitrides Chemical class 0.000 description 1
- 125000002560 nitrile group Chemical group 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 239000006179 pH buffering agent Substances 0.000 description 1
- 150000002941 palladium compounds Chemical class 0.000 description 1
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical compound [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920000768 polyamine Chemical class 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 229920001083 polybutene Polymers 0.000 description 1
- 229920006267 polyester film Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920001289 polyvinyl ether Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 1
- 229960001755 resorcinol Drugs 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- HELHAJAZNSDZJO-OLXYHTOASA-L sodium L-tartrate Chemical compound [Na+].[Na+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O HELHAJAZNSDZJO-OLXYHTOASA-L 0.000 description 1
- 239000001433 sodium tartrate Substances 0.000 description 1
- 229960002167 sodium tartrate Drugs 0.000 description 1
- 235000011004 sodium tartrates Nutrition 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 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
- 229920002554 vinyl polymer Polymers 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
-
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/18—Non-metallic particles coated with metal
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1635—Composition of the substrate
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1646—Characteristics of the product obtained
- C23C18/165—Multilayered product
- C23C18/1651—Two or more layers only obtained by electroless plating
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
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Abstract
【解決手段】芯材粒子の表面に、ニッケル又はニッケル合金皮膜が形成された導電性粒子からなる導電性粉体である。導電性粒子は、前記皮膜の表面から突出し、かつ該皮膜と連続体になっている、アスペクト比が1以上の突起部を多数有している。アスペクト比が1以上の前記突起部の割合は、全突起部の数に対して40%以上である。導電性粉体においては、導電性粒子のうち、一次粒子が占める重量が、導電性粉体の重量に対して85重量%以上である。
【選択図】図1
Description
前記導電性粒子は、前記皮膜の表面から突出し、かつ該皮膜と連続体になっている、アスペクト比が1以上の突起部を多数有し、
アスペクト比が1以上の前記突起部の割合が、全突起部の数に対して40%以上であり、
前記導電性粉体においては、前記導電性粒子のうち、一次粒子が占める重量が、導電性粉体の重量に対して85重量%以上であることを特徴とする導電性粉体を提供するものである。
A工程において得られた、ニッケル初期薄膜層を有する前記芯材粒子、及び前記分散剤を含む水性スラリーを、該分散剤の分散効果が発現するpH範囲に維持しつつ、該水性スラリーに、1時間当たりのニッケルの析出量が25〜100nmとなる量に相当する量のニッケルイオン及び還元剤を経時的に添加して、該水性スラリー中にニッケルの核粒子を生成させるとともに、生成した核粒子を前記芯材粒子に付着させて、付着した核粒子を起点として該核粒子を成長させ、アスペクト比が1以上の突起を形成するB工程とを具備することを特徴とする導電性粒子の製造方法を提供するものである。
変動係数(%)=(標準偏差/平均粒径)×100 (1)
この変動係数が大きいことは分布に幅があることを示し、一方、変動係数が小さいことは粒度分布がシャープであることを示す。本発明では、芯材粒子として、この変動係数が30%以下、特に20%以下、とりわけ10%以下のものを使用することが好ましい。この理由は、本発明の導電性粒子を異方導電フィルム中の導電粒子として用いた場合に、接続に有効な寄与割合が高くなるという利点があるからである。
式(2)で示されるF及びSは、微小圧縮試験機MCTM−500((株)島津製作所製)で測定したときの、それぞれ該微球体の10%圧縮変形における荷重値(kgf)及び圧縮変位(mm)であり、Rは該微球体の半径(mm)である。
(1)A工程
表1に示す粒径を有し、真比重が1.1の球状スチレン−シリカ複合樹脂〔(株)日本触媒製、商品名ソリオスター〕を芯材粒子として用いた。その40gを、400mLのコンディショナー水溶液(ローム・アンド・ハース電子材料製の「クリーナーコンディショナー231」)に攪拌しながら投入した。コンディショナー水溶液の濃度は40ml/Lであった。引き続き、液温60℃で超音波を与えながら30分間攪拌して芯材粒子の表面改質及び分散処理を行った。水溶液をろ過し、一回リパルプ水洗した芯材粒子を200mLのスラリーにした。このスラリーへ塩化第一錫水溶液200mlを投入した。この水溶液の濃度は5×10-3mol/Lであった。常温で5分攪拌し、錫イオンを芯材粒子の表面に吸着させる感受性化処理を行った。引き続き水溶液をろ過し、1回リパルプ水洗した。次いで芯材粒子を400mlのスラリーにし、60℃に維持した。超音波を併用してスラリーを攪拌しながら、0.11mol/Lの塩化パラジウム水溶液2mLを添加した。そのままの攪拌状態を5分間維持させ、芯材粒子の表面にパラジウムイオンを捕捉させる活性化処理を行った。
224g/L硫酸ニッケル水溶液と、210g/Lの次亜リン酸ナトリウム及び80g/Lの水酸化ナトリウムを含む混合水溶液とをそれぞれ300mL用い、これらをA工程で得られた芯材粒子のスラリーに、定量ポンプによって連続的に分別添加し、無電解めっきB工程を開始した。添加速度はいずれも2.5mL/分とした。本工程の具体的な条件を表3に示す。液を全量添加した後、70℃の温度を保持しながら5分攪拌を継続した。次いで液をろ過し、ろ過物を3回洗浄した後、100℃の真空乾燥機で乾燥してニッケル−リン合金皮膜を有する導電性粒子を得た。実施例3において得られた導電性粒子の走査型電子顕微鏡(SEM)像を図1に示した。同図から明らかなように、導電性粒子におけるニッケル皮膜と突起部とは連続体になっている。
表1及び表3に示す条件でA工程及びB工程を行う以外は実施例1と同様にして導電性粒子を得た。ただし、実施例19のB工程においては、硫酸ニッケル水溶液と、次亜リン酸ナトリウム及び水酸化ナトリウムを含む混合水溶液の添加量をそれぞれ230mLとした。また実施例20のB工程においては、硫酸ニッケル水溶液と、次亜リン酸ナトリウム及び水酸化ナトリウムを含む混合水溶液の添加量をそれぞれ390mLとした。また実施例21ないし23の硫酸ニッケル水溶液と、次亜リン酸ナトリウム及び水酸化ナトリウムを含む混合水溶液の添加量及び滴下速度はそれぞれ150、225、600mL、1.3、1.9、5.0mL/分とした。このようにして、ニッケル−リン合金皮膜を有する導電性粒子を得た。
10g/LのEDTA−4Na、10g/Lのクエン酸―2Na及び2.9g/Lのシアン化金カリウム(Auとして2.0g/L)からなる無電解金めっき液を調製した。この金めっき液2リットルを79℃に加熱し、これを攪拌しながら、実施例2で得られた導電性粒子10gを添加した。これによって粒子の表面に無電解めっき処理を行った。処理時間は20分とした。処理の完了後、液をろ過し、ろ過物を3回リパルプした。次いで110℃の真空乾燥機で乾燥した。このようにして、ニッケル−リン合金皮膜上に金めっき被覆処理を施した。
10g/LのEDTA−2Na、10g/Lのクエン酸2Na及び20g/Lのテトラアンミンパラジウム塩酸塩(Pd(NH3)4Cl2)溶液(パラジウムとして2g/L)、カルボキシメチルセルロース(分子量250000、エーテル化度0.9)100ppmからなる無電解パラジウムめっき液を調製した。このパラジウムめっき液0.65リットル(実施例25)、1.3リットル(実施例16)、2.6リットル(実施例27)を70℃に加熱し、これを攪拌しながら、実施例2で得られた導電性粒子10gを添加した。これによって粒子の表面に置換型の無電解めっき処理を行った。処理時間は60分とした。処理の完了後、液をろ過し、ろ過物を3回リパルプした。次いで110℃の真空乾燥機で乾燥した。このようにして、ニッケル−リン合金皮膜上にパラジウムめっき被覆処理を施した。パラジウム皮膜中にリンは含まれていなかった。
表1及び表3に示す条件でA工程及びB工程を行う以外は実施例1と同様にして、ニッケル―リン合金皮膜を有する導電性粒子を得た。ただし、比較例3のB工程においては、硫酸ニッケル水溶液と、次亜リン酸ナトリウム及び水酸化ナトリウムを含む混合水溶液の添加量をそれぞれ230mLとした。また比較例5ないし6の硫酸ニッケル水溶液と、次亜リン酸ナトリウム及び水酸化ナトリウムを含む混合水溶液の添加量及び滴下速度はそれぞれ38、1200mL、0.3、10.0mL/分とした。比較例1において得られた導電性粒子のSEM像を図2に示した。
比較例2で製造した導電性粒子に、実施例24と同様の金めっき被覆処理を施した。
実施例及び比較例で得られた導電性粒子の粒径、ニッケル皮膜の厚み、金皮膜の厚み、パラジウム皮膜の厚み、表面状態、ニッケル皮膜の密着性及び導電性をそれぞれ測定・評価した。また、更に金めっきを施したものは、金皮膜の密着性、パラジウムめっきを施したものは、パラジウム皮膜の密着性を評価した。各物性評価は次の方法によって行った。また、突起部のアスペクト比、アスペクト比が1以上である突起部の割合、及び導電性粉体における一次粒子が占める割合、導電性粒子の粒径をそれぞれ上述の方法で測定した。それらの結果を表4及び表5に示す。
導電性粒子を王水に浸漬してニッケル皮膜を溶解し、皮膜成分をICP又は化学分析し、以下の式(1)、(2)からニッケル皮膜の厚みを算出した。
A=[(r+t)3―r3]d1/r3d2 (1)
A=W/(100−W) (2)
式中、rは芯材粒子の半径(μm)、tはニッケル皮膜の厚み、d1はニッケル皮膜の比重、d2は芯材粒子の比重、Wはニッケル含有率(重量%)である。
導電性粒子を王水に浸漬して、金又はパラジウム皮膜とニッケル皮膜とを溶解し、皮膜成分をICP分析又は化学分析した。そして、以下の(3)及び(4)から金又はパラジウム皮膜の厚みを算出した。
B=[(r+t+u)3−(r+t)3]d3/(r+t)3d4 (3)
B=X(100−X) (4)
式中、uは金又はパラジウム皮膜の厚み、d3は金又はパラジウム皮膜の比重、d4はNi品の比重、Xは金又はパラジウムの含有率(重量%)である。ここで、Ni品の比重d4は計算式を使用して算出する。比重は以下の(5)の計算式を用いて算出した。
d4=100/[(W/d1)+(100−W)/d2] (5)
式中、d1はニッケル皮膜の比重、d2は芯材粒子の比重、Wはニッケル含有率(重量%)である。
SEMを用い、導電性粒子を30000倍に拡大して10視野を観察し、導電性粒子1個が有する突起部の個数の平均値を算出した。10〜100個を○、10以下を△とした。また、ニッケルが異常析出した場合を×とした。異常析出とは、例えばニッケルが芯材粒子の表面に析出せず、液中に単独析出する場合等を言う。
100mLのビーカーに導電性粒子2g及び直径1mmのジルコニアビーズ90gを入れ、更にトルエンを10mL入れた。攪拌装置で10分攪拌した後、ジルコニアビーズとスラリーを分離し乾燥させた。乾燥後の導電性粒子をSEMを用いて2000倍に拡大して10視野を観察し、攪拌によって生じた剥離片の個数の平均値を算出した。剥離片の個数10個未満を○とし、10〜30個を△、30個超を×とした。
エポキシ樹脂100部、硬化剤150部、トルエン70部を混合し、絶縁性接着剤を調製した。これに導電性粒子15部を配合してペーストを得た。バーコーターを用い、このペーストをシリコーン処理ポリエステルフィルム上に塗布し乾燥させた。得られた塗工フィルムを用い、全面をアルミニウムで蒸着したガラスと50μmピッチに銅パターンを形成したポリイミドフィルム基板との間の接続を行った。そして電極間の導通抵抗を測定することで、導電性粒子の導電性を評価した。評価は抵抗値2Ω以下を○とし、2〜5Ωを△、5Ω以上を×とした。また、ショート発生の有無も表に併記した。
Claims (7)
- 芯材粒子の表面に、ニッケル又はニッケル合金皮膜が形成された導電性粒子からなる導電性粉体であって、
前記導電性粒子は、前記皮膜の表面から突出し、かつ該皮膜と連続体になっている、アスペクト比が1以上の突起部を多数有し、
アスペクト比が1以上の前記突起部の割合が、全突起部の数に対して40%以上であり、
前記導電性粉体においては、前記導電性粒子のうち、一次粒子が占める重量が、導電性粉体の重量に対して85重量%以上であることを特徴とする導電性粉体。 - 前記芯材粒子の平均粒径が1〜3μmである請求項1記載の導電性粉体。
- 前記突起部を含む前記皮膜の表面を金又はパラジウムで被覆した請求項1又は2記載の導電性粉体。
- 請求項1ないし3のいずれかに記載の導電性粉体と絶縁性樹脂とを含む導電性材料。
- 分散剤及びニッケルイオンを含む無電解めっき浴と、表面に貴金属が担持された芯材粒子とを混合して、該芯材粒子の表面にニッケル初期薄膜層を形成するに際し、ニッケルイオンの濃度が0.0001〜0.008モル/リットルに調整された該無電解めっき浴1リットルに対して、表面積の総和が1〜15m2となるような量の該芯材粒子を用いるA工程と、
A工程において得られた、ニッケル初期薄膜層を有する前記芯材粒子、及び前記分散剤を含む水性スラリーを、該分散剤の分散効果が発現するpH範囲に維持しつつ、該水性スラリーに、1時間当たりのニッケルの析出量が25〜100nmとなる量に相当する量のニッケルイオン及び還元剤を経時的に添加して、該水性スラリー中にニッケルの核粒子を生成させるとともに、生成した核粒子を前記芯材粒子に付着させて、付着した核粒子を起点として該核粒子を成長させ、アスペクト比が1以上の突起部を形成するB工程とを具備することを特徴とする導電性粒子の製造方法。 - ニッケル初期薄膜層の厚みが0.1〜10nmとなるようにA工程を行う請求項5記載の製造方法。
- 前記分散剤として、非イオン界面活性剤、両性イオン界面活性剤又は水溶性高分子を用いる請求項5又は6記載の製造方法。
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JP2004296322A (ja) * | 2003-03-27 | 2004-10-21 | Sekisui Chem Co Ltd | 導電性微粒子及び液晶表示素子 |
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Also Published As
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JP4746116B2 (ja) | 2011-08-10 |
TWI479508B (zh) | 2015-04-01 |
KR101594639B1 (ko) | 2016-02-16 |
CN102187405A (zh) | 2011-09-14 |
WO2010044388A1 (ja) | 2010-04-22 |
TW201021054A (en) | 2010-06-01 |
KR20110069811A (ko) | 2011-06-23 |
CN102187405B (zh) | 2013-01-02 |
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