JP4451760B2 - 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 - Google Patents
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 Download PDFInfo
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- JP4451760B2 JP4451760B2 JP2004324868A JP2004324868A JP4451760B2 JP 4451760 B2 JP4451760 B2 JP 4451760B2 JP 2004324868 A JP2004324868 A JP 2004324868A JP 2004324868 A JP2004324868 A JP 2004324868A JP 4451760 B2 JP4451760 B2 JP 4451760B2
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- 239000002245 particle Substances 0.000 title claims description 72
- 239000010419 fine particle Substances 0.000 title claims description 34
- 238000004519 manufacturing process Methods 0.000 title claims description 17
- 239000007864 aqueous solution Substances 0.000 claims description 40
- 239000011859 microparticle Substances 0.000 claims description 40
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 30
- 239000002344 surface layer Substances 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 238000001556 precipitation Methods 0.000 claims description 15
- 239000003638 chemical reducing agent Substances 0.000 claims description 12
- 229910052698 phosphorus Inorganic materials 0.000 claims description 10
- 230000009467 reduction Effects 0.000 claims description 9
- 150000002815 nickel Chemical class 0.000 claims description 8
- 239000003002 pH adjusting agent Substances 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 7
- 239000006179 pH buffering agent Substances 0.000 claims description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 6
- 239000011574 phosphorus Substances 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 230000000977 initiatory effect Effects 0.000 claims 1
- 239000002184 metal Substances 0.000 description 26
- 229910052751 metal Inorganic materials 0.000 description 26
- 238000010438 heat treatment Methods 0.000 description 22
- 239000000203 mixture Substances 0.000 description 18
- 238000009826 distribution Methods 0.000 description 16
- 238000000034 method Methods 0.000 description 13
- 239000000243 solution Substances 0.000 description 13
- 229910000765 intermetallic Inorganic materials 0.000 description 12
- 238000006722 reduction reaction Methods 0.000 description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 239000012298 atmosphere Substances 0.000 description 9
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 9
- 230000002829 reductive effect Effects 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000003917 TEM image Methods 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- 150000003839 salts Chemical class 0.000 description 7
- 238000007747 plating Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 229910001873 dinitrogen Inorganic materials 0.000 description 5
- 238000009413 insulation Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 229910052752 metalloid Inorganic materials 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 229930185605 Bisphenol Natural products 0.000 description 3
- 229920002799 BoPET Polymers 0.000 description 3
- 239000006087 Silane Coupling Agent Substances 0.000 description 3
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 3
- 230000005587 bubbling Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 239000012266 salt solution Substances 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- SIGUVTURIMRFDD-UHFFFAOYSA-M sodium dioxidophosphanium Chemical compound [Na+].[O-][PH2]=O SIGUVTURIMRFDD-UHFFFAOYSA-M 0.000 description 3
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000012212 insulator Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 239000001632 sodium acetate Substances 0.000 description 2
- 235000017281 sodium acetate Nutrition 0.000 description 2
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002788 crimping Methods 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 239000013081 microcrystal Substances 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
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000006174 pH buffer Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- KOUDKOMXLMXFKX-UHFFFAOYSA-N sodium oxido(oxo)phosphanium hydrate Chemical compound O.[Na+].[O-][PH+]=O KOUDKOMXLMXFKX-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/08—Other phosphides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Powder Metallurgy (AREA)
- Non-Insulated Conductors (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
- Chemically Coating (AREA)
Description
ホスフィン酸ナトリウム一水和物を純水1.5×10−2(m3)に溶解し、1.8(kmol/m3)の濃度のホスフィン酸ナトリウム水溶液とし、この水溶液を窒素ガス(流量0.3(m3/h))でバブリングしながら343(K)に加熱保持して、リンを含む還元剤水溶液を得た。
リンを含む還元剤水溶液としてホスフィン酸ナトリウム1.8(kmol/m3)の水溶液を1.5×10−2(m3)作製した。硫酸ニッケル0.6(kmol/m3)のニッケル塩水溶液1.5×10−2(m3)を準備し、pH緩衝剤のマレイン酸0.3(kmol/m3)とpH調整剤の水酸化ナトリウム1.55(kmol/m3)とを含む混合水溶液1.5×10−2(m3)を準備し、ニッケル塩水溶液と混合水溶液とを撹拌混合して金属塩水溶液を3.0×10−2(m3)作製した。上の還元剤水溶液と金属塩水溶液を窒素ガス雰囲気下で343(K)に撹拌加熱し、実施例1と同様な方法により、加熱処理までを行ない球状NiP微小粒子を製造した。なお、混合した時のpHは7.5であった。レーザー回折散乱法により、粒径の分布を確認したところd50値が6.8μm、(d90−d10)/d50値が0.63であり、図9のSEM写真に示す球状NiP微小粒子を得た。なお、その断面構造は、結晶質構造を有する中心部と、非晶質構造を有する表層部とからなりかつ、その表層部にはNiP金属間化合物が存在していることを、確認できた。
特許文献1に従い、ホスフィン酸ナトリウム1.8(kmol/m3)水溶液と、水酸化ナトリウム0.6(kmol/m3)および酢酸ナトリウム0.5(kmol/m3)の混合水溶液を、それぞれ2.5×10−4(m3)作製し、ウォーターバス中で加熱撹拌しながら2液を混合して還元剤水溶液とし、窒素ガスを流してバブリングを行なって、水溶液の温度が343±1(K)となるように調整した。
Claims (2)
- ニッケル塩の水溶液と、pH調整剤およびpH緩衝剤の混合水溶液と、リンを含む還元剤水溶液とを混合して還元析出反応させて、Niを主体にPを含む球状NiP微小粒子を製造する方法において、
これらの水溶液を混合して還元析出反応を開始させる時のpHが7.3以上のアルカリ性になるように調整し、還元析出反応させて、結晶構造を有する中心部と、非晶質からなりP含有量が中心部のP含有量よりも高い表層部とからなる球状NiP微小粒子を析出させ、得られた球状NiP微小粒子に300℃から550℃の温度で加熱処理を行なうことを特徴とする球状NiP微小粒子の製造方法。 - 請求項1に記載の球状NiP微小粒子の製造方法で得た球状NiP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。
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2004324868A JP4451760B2 (ja) | 2004-11-09 | 2004-11-09 | 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 |
KR1020050105862A KR100880742B1 (ko) | 2004-11-09 | 2005-11-07 | 구상 NiP 미소 입자 및 그 제조방법과, 이방성 도전필름용 도전 입자 |
TW094139054A TWI339140B (en) | 2004-11-09 | 2005-11-08 | Fabricating method of ball-shaped nip micro particle and fabricating method of conductive particle for anisotropic conductive film |
Applications Claiming Priority (1)
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JP2004324868A JP4451760B2 (ja) | 2004-11-09 | 2004-11-09 | 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 |
Publications (2)
Publication Number | Publication Date |
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JP2006131978A JP2006131978A (ja) | 2006-05-25 |
JP4451760B2 true JP4451760B2 (ja) | 2010-04-14 |
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JP2004324868A Active JP4451760B2 (ja) | 2004-11-09 | 2004-11-09 | 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 |
Country Status (3)
Country | Link |
---|---|
JP (1) | JP4451760B2 (ja) |
KR (1) | KR100880742B1 (ja) |
TW (1) | TWI339140B (ja) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2023090525A1 (ko) * | 2021-11-16 | 2023-05-25 | 덕산하이메탈(주) | 도전입자, 도전재료 및 접속 구조체 |
Families Citing this family (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP4942090B2 (ja) * | 2006-10-12 | 2012-05-30 | 秋田県 | 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 |
JP5327582B2 (ja) * | 2007-10-18 | 2013-10-30 | 日立金属株式会社 | 還元析出型球状NiP微小粒子およびその製造方法 |
JP5943019B2 (ja) | 2014-02-26 | 2016-06-29 | 日立金属株式会社 | 導電性粒子、導電性粉体、導電性高分子組成物および異方性導電シート |
WO2015141485A1 (ja) * | 2014-03-17 | 2015-09-24 | 日立金属株式会社 | 触媒用Pd粒子および触媒用Pd粉体、触媒用Pd粒子の製造方法 |
JP6443732B2 (ja) * | 2014-10-24 | 2018-12-26 | 日立金属株式会社 | 導電性粒子、導電性粉体、導電性高分子組成物および異方性導電シート |
WO2022210217A1 (ja) * | 2021-03-30 | 2022-10-06 | 日立金属株式会社 | 導電性金属粒子の製造方法および導電性金属粒子 |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5474623A (en) * | 1993-05-28 | 1995-12-12 | Rhone-Poulenc Inc. | Magnetically anisotropic spherical powder and method of making same |
JPH10317021A (ja) * | 1997-05-22 | 1998-12-02 | Akita Pref Gov Shigen Gijutsu Kaihatsu Kiko | 球状アモルファスCo−Ni−P三元合金粉末およびその製造法 |
JP2001279306A (ja) * | 2000-03-30 | 2001-10-10 | Akita Pref Gov Shigen Gijutsu Kaihatsu Kiko | 球状Ni−Pアモルファス金属粉末の製法 |
JP4524727B2 (ja) * | 2000-04-26 | 2010-08-18 | 日立金属株式会社 | 異方性導電膜用Ni合金粒およびその製造方法 |
JP4088137B2 (ja) * | 2002-11-13 | 2008-05-21 | 積水化学工業株式会社 | 導電性微粒子および異方導電材料 |
-
2004
- 2004-11-09 JP JP2004324868A patent/JP4451760B2/ja active Active
-
2005
- 2005-11-07 KR KR1020050105862A patent/KR100880742B1/ko active IP Right Grant
- 2005-11-08 TW TW094139054A patent/TWI339140B/zh active
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2023090525A1 (ko) * | 2021-11-16 | 2023-05-25 | 덕산하이메탈(주) | 도전입자, 도전재료 및 접속 구조체 |
Also Published As
Publication number | Publication date |
---|---|
TW200616736A (en) | 2006-06-01 |
KR100880742B1 (ko) | 2009-02-02 |
TWI339140B (en) | 2011-03-21 |
JP2006131978A (ja) | 2006-05-25 |
KR20060052506A (ko) | 2006-05-19 |
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