JP2643520B2 - Silver-containing alloy powder and conductive paste using the powder - Google Patents
Silver-containing alloy powder and conductive paste using the powderInfo
- Publication number
- JP2643520B2 JP2643520B2 JP2041093A JP4109390A JP2643520B2 JP 2643520 B2 JP2643520 B2 JP 2643520B2 JP 2041093 A JP2041093 A JP 2041093A JP 4109390 A JP4109390 A JP 4109390A JP 2643520 B2 JP2643520 B2 JP 2643520B2
- Authority
- JP
- Japan
- Prior art keywords
- silver
- powder
- alloy powder
- containing alloy
- acid
- 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.)
- Expired - Lifetime
Links
- 239000000843 powder Substances 0.000 title claims description 76
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims description 64
- 229910052709 silver Inorganic materials 0.000 title claims description 59
- 239000004332 silver Substances 0.000 title claims description 58
- 239000000956 alloy Substances 0.000 title claims description 22
- 229910045601 alloy Inorganic materials 0.000 title claims description 22
- 229920005989 resin Polymers 0.000 claims description 26
- 239000011347 resin Substances 0.000 claims description 26
- 239000002245 particle Substances 0.000 claims description 20
- 239000000155 melt Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 14
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 13
- 229910052759 nickel Inorganic materials 0.000 claims description 13
- 229910052802 copper Inorganic materials 0.000 claims description 11
- -1 phenol compound Chemical class 0.000 claims description 11
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 10
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims description 9
- 239000011230 binding agent Substances 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 9
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- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 6
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- 239000000853 adhesive Substances 0.000 description 4
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- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 4
- 235000020661 alpha-linolenic acid Nutrition 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical compound C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229960004488 linolenic acid Drugs 0.000 description 4
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 description 4
- WQGWDDDVZFFDIG-UHFFFAOYSA-N pyrogallol Chemical compound OC1=CC=CC(O)=C1O WQGWDDDVZFFDIG-UHFFFAOYSA-N 0.000 description 4
- 239000004593 Epoxy Substances 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 3
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- KMNCBSZOIQAUFX-UHFFFAOYSA-N 2-ethoxy-1,2-diphenylethanone Chemical compound C=1C=CC=CC=1C(OCC)C(=O)C1=CC=CC=C1 KMNCBSZOIQAUFX-UHFFFAOYSA-N 0.000 description 1
- KFXTTZQGCNRYEN-UHFFFAOYSA-N 2-n-octadecylpropane-1,2-diamine Chemical compound CCCCCCCCCCCCCCCCCCNC(C)CN KFXTTZQGCNRYEN-UHFFFAOYSA-N 0.000 description 1
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- NDWUBGAGUCISDV-UHFFFAOYSA-N 4-hydroxybutyl prop-2-enoate Chemical compound OCCCCOC(=O)C=C NDWUBGAGUCISDV-UHFFFAOYSA-N 0.000 description 1
- GZVHEAJQGPRDLQ-UHFFFAOYSA-N 6-phenyl-1,3,5-triazine-2,4-diamine Chemical compound NC1=NC(N)=NC(C=2C=CC=CC=2)=N1 GZVHEAJQGPRDLQ-UHFFFAOYSA-N 0.000 description 1
- FIHBHSQYSYVZQE-UHFFFAOYSA-N 6-prop-2-enoyloxyhexyl prop-2-enoate Chemical compound C=CC(=O)OCCCCCCOC(=O)C=C FIHBHSQYSYVZQE-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- BQACOLQNOUYJCE-FYZZASKESA-N Abietic acid Natural products CC(C)C1=CC2=CC[C@]3(C)[C@](C)(CCC[C@@]3(C)C(=O)O)[C@H]2CC1 BQACOLQNOUYJCE-FYZZASKESA-N 0.000 description 1
- 229910001316 Ag alloy Inorganic materials 0.000 description 1
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- XNCOSPRUTUOJCJ-UHFFFAOYSA-N Biguanide Chemical compound NC(N)=NC(N)=N XNCOSPRUTUOJCJ-UHFFFAOYSA-N 0.000 description 1
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- MHZGKXUYDGKKIU-UHFFFAOYSA-N Decylamine Chemical compound CCCCCCCCCCN MHZGKXUYDGKKIU-UHFFFAOYSA-N 0.000 description 1
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- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical group C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
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- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 1
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- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- IWYDHOAUDWTVEP-UHFFFAOYSA-N R-2-phenyl-2-hydroxyacetic acid Natural products OC(=O)C(O)C1=CC=CC=C1 IWYDHOAUDWTVEP-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- BGNXCDMCOKJUMV-UHFFFAOYSA-N Tert-Butylhydroquinone Chemical compound CC(C)(C)C1=CC(O)=CC=C1O BGNXCDMCOKJUMV-UHFFFAOYSA-N 0.000 description 1
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- 229920002433 Vinyl chloride-vinyl acetate copolymer Polymers 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- MBHRHUJRKGNOKX-UHFFFAOYSA-N [(4,6-diamino-1,3,5-triazin-2-yl)amino]methanol Chemical class NC1=NC(N)=NC(NCO)=N1 MBHRHUJRKGNOKX-UHFFFAOYSA-N 0.000 description 1
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 description 1
- 231100000987 absorbed dose Toxicity 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 150000001241 acetals Chemical class 0.000 description 1
- 229920006397 acrylic thermoplastic Polymers 0.000 description 1
- 125000003647 acryloyl group Chemical group O=C([*])C([H])=C([H])[H] 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000002723 alicyclic group Chemical group 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229940051879 analgesics and antipyretics salicylic acid and derivative Drugs 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 150000001454 anthracenes Chemical class 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 150000004982 aromatic amines Chemical class 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- GCTPMLUUWLLESL-UHFFFAOYSA-N benzyl prop-2-enoate Chemical compound C=CC(=O)OCC1=CC=CC=C1 GCTPMLUUWLLESL-UHFFFAOYSA-N 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- KBCQNEMPPWEKJC-UHFFFAOYSA-N butan-1-ol;phenol Chemical class CCCCO.OC1=CC=CC=C1 KBCQNEMPPWEKJC-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 150000001733 carboxylic acid esters Chemical class 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- AJPXTSMULZANCB-UHFFFAOYSA-N chlorohydroquinone Chemical compound OC1=CC=C(O)C(Cl)=C1 AJPXTSMULZANCB-UHFFFAOYSA-N 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 229960004106 citric acid Drugs 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- KBLWLMPSVYBVDK-UHFFFAOYSA-N cyclohexyl prop-2-enoate Chemical compound C=CC(=O)OC1CCCCC1 KBLWLMPSVYBVDK-UHFFFAOYSA-N 0.000 description 1
- 125000004386 diacrylate group Chemical group 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- VPNOHCYAOXWMAR-UHFFFAOYSA-N docosan-1-amine Chemical compound CCCCCCCCCCCCCCCCCCCCCCN VPNOHCYAOXWMAR-UHFFFAOYSA-N 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000001227 electron beam curing Methods 0.000 description 1
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 description 1
- 239000005038 ethylene vinyl acetate Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000001530 fumaric acid Substances 0.000 description 1
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- QAMFBRUWYYMMGJ-UHFFFAOYSA-N hexafluoroacetylacetone Chemical compound FC(F)(F)C(=O)CC(=O)C(F)(F)F QAMFBRUWYYMMGJ-UHFFFAOYSA-N 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-M hexanoate Chemical compound CCCCCC([O-])=O FUZZWVXGSFPDMH-UHFFFAOYSA-M 0.000 description 1
- NWVVVBRKAWDGAB-UHFFFAOYSA-N hydroquinone methyl ether Natural products COC1=CC=C(O)C=C1 NWVVVBRKAWDGAB-UHFFFAOYSA-N 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 229960000448 lactic acid Drugs 0.000 description 1
- PBOSTUDLECTMNL-UHFFFAOYSA-N lauryl acrylate Chemical compound CCCCCCCCCCCCOC(=O)C=C PBOSTUDLECTMNL-UHFFFAOYSA-N 0.000 description 1
- 229910052745 lead Inorganic materials 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
- 229960002510 mandelic acid Drugs 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 125000005641 methacryl group Chemical group 0.000 description 1
- YDKNBNOOCSNPNS-UHFFFAOYSA-N methyl 1,3-benzoxazole-2-carboxylate Chemical compound C1=CC=C2OC(C(=O)OC)=NC2=C1 YDKNBNOOCSNPNS-UHFFFAOYSA-N 0.000 description 1
- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical compound OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229920003986 novolac Polymers 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000006072 paste Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- CUQCMXFWIMOWRP-UHFFFAOYSA-N phenyl biguanide Chemical compound NC(N)=NC(N)=NC1=CC=CC=C1 CUQCMXFWIMOWRP-UHFFFAOYSA-N 0.000 description 1
- LYXOWKPVTCPORE-UHFFFAOYSA-N phenyl-(4-phenylphenyl)methanone Chemical compound C=1C=C(C=2C=CC=CC=2)C=CC=1C(=O)C1=CC=CC=C1 LYXOWKPVTCPORE-UHFFFAOYSA-N 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920005668 polycarbonate resin Polymers 0.000 description 1
- 239000004431 polycarbonate resin Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229940068918 polyethylene glycol 400 Drugs 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000009719 polyimide resin Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 description 1
- FBCQUCJYYPMKRO-UHFFFAOYSA-N prop-2-enyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC=C FBCQUCJYYPMKRO-UHFFFAOYSA-N 0.000 description 1
- QTECDUFMBMSHKR-UHFFFAOYSA-N prop-2-enyl prop-2-enoate Chemical compound C=CCOC(=O)C=C QTECDUFMBMSHKR-UHFFFAOYSA-N 0.000 description 1
- HJWLCRVIBGQPNF-UHFFFAOYSA-N prop-2-enylbenzene Chemical compound C=CCC1=CC=CC=C1 HJWLCRVIBGQPNF-UHFFFAOYSA-N 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 229960001367 tartaric acid Drugs 0.000 description 1
- 239000004250 tert-Butylhydroquinone Substances 0.000 description 1
- 235000019281 tert-butylhydroquinone Nutrition 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
- H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L24/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L24/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
- H01L24/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は、導電性に優れ、かつ耐酸化性が良く、銀の
耐マイグレーション性に優れた特性を有する。安価な導
電性ペースト及び該ペーストを用いた導電体に関するも
のであり、電磁シールド、ICダイボンデイングペース
ト、コンデンサー電極、導電性接着剤、接点材料、導電
回路用ペースト、低抵抗体ペーストとして応用できる。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention has excellent conductivity, good oxidation resistance, and excellent silver migration resistance. The present invention relates to an inexpensive conductive paste and a conductor using the paste, and can be applied as an electromagnetic shield, an IC die bonding paste, a capacitor electrode, a conductive adhesive, a contact material, a conductive circuit paste, and a low-resistance paste.
（従来技術） 従来、導電性を有する材料として、カーボン、銅、ア
ルミニウムや、銀、パラジウム等の貴金属、銀メッキ複
合粉が用いられており、これら導電性の粉末を有機バイ
ンダー、必要に応じて溶剤、添加剤を加え分散させたペ
ーストが公知である。(Prior art) Conventionally, noble metals such as carbon, copper, aluminum, silver, and palladium, and silver-plated composite powders have been used as conductive materials. These conductive powders are used as an organic binder, if necessary. Pastes in which a solvent and additives are added and dispersed are known.
（発明が解決しようとする課題） 公知導電性ペーストとして用いられているカーボン、
銅、ニッケル、銀及び貴金属粉、銀メッキ複合粉は、以
下の欠点がある。銅、ニッケルは、安価であるが、酸化
により塗膜の導電性が低下しやすい。また、銀は高価で
あり、電場中、特に高湿度下で銀がマイグレーションを
起こし、絶縁不良を起こし易い。銀メッキ粉末は、剥れ
が生じ易く、また銀のマイグレーションの問題がある。
カーボン粉末を用いたペーストは、導電性が悪いという
欠点を有している。また、銀と銅、ニッケルを機械的強
制結合により合成粉を作製する方法が開示されているが
（例えば、特開昭56−155259,57−98572号）、機械的強
制結合のため、銀のマイグレーションの防止効果に乏し
い欠点を有する。(Problem to be Solved by the Invention) Carbon used as a known conductive paste,
Copper, nickel, silver and noble metal powder, and silver-plated composite powder have the following disadvantages. Copper and nickel are inexpensive, but the oxidation tends to lower the conductivity of the coating film. Further, silver is expensive, and silver easily migrates in an electric field, particularly under high humidity, and easily causes insulation failure. The silver plating powder is liable to peel off and has a problem of silver migration.
Pastes using carbon powder have the disadvantage of poor conductivity. Also, a method of producing a synthetic powder by mechanically forcing silver with copper and nickel has been disclosed (for example, JP-A-56-155259, 57-98572). There is a disadvantage that the effect of preventing migration is poor.
（課題を解決するための手段） 本発明は、導電性に優れ、かつ長期にわたり耐酸化性
に優れ、銀マイグレーションを起こさない安価な銀含有
合金粉末ならび該粉末を用いた導電性ペーストに関する
ものである。(Means for Solving the Problems) The present invention relates to an inexpensive silver-containing alloy powder which is excellent in conductivity and excellent in oxidation resistance for a long time and does not cause silver migration, and a conductive paste using the powder. is there.
本発明に用いる銀含有合金粉末は、高圧アトマイズ法
により作製されるが、高圧水アトマイズ法、高圧ガスア
トマイズ法が好ましい。特に、先に同一出願人により出
願した特願平１−205569号において詳細に説明されてお
り、高圧ガスアトマイズ法を用いるのが好ましい。開示
内容によれば、該組成の銀とＭ（但しＭはCu,Fe,Co,Ni,
より選ばれた１種以上）を混合し、不活性ガス雰囲気
中、るつぼ中で高周波誘導加熱を用いて融解する。さら
に、るつぼ先端より融液を不活性ガス雰囲気中へ噴出す
る。噴出と同時に、高圧の不活性ガスを断熱膨張させて
発生した高速気流を融液に向かって噴出、アトマイズ化
し、急冷凝固する方法である。融液を急冷凝固する冷却
速度は102℃/sec以上が好ましく、103℃/sec以上がさら
に好ましく、104℃/sec以上が最も好ましい。ここで用
いられる不活性ガスとは、かかる組成の融液と全くか、
あるいは極めてゆるやかにしか反応しないガスを意味す
る。例えば、窒素、ヘリウム、アルゴン、それらの混合
物などが挙げられる。また、本発明で用いる銀含有合金
粉末の特性に影響を与えない程度であれば、若干の不純
物ガスが混じっていても構わない。The silver-containing alloy powder used in the present invention is produced by a high-pressure atomization method, and a high-pressure water atomization method and a high-pressure gas atomization method are preferable. In particular, as described in detail in Japanese Patent Application No. 1-205569 filed earlier by the same applicant, it is preferable to use a high-pressure gas atomizing method. According to the disclosure, silver having the above composition and M (where M is Cu, Fe, Co, Ni,
And at least one selected from the group consisting of a mixture selected from the group consisting of a mixture of at least one selected from the group consisting of: Further, the melt is jetted into the inert gas atmosphere from the crucible tip. Simultaneously with the jetting, a high-speed airflow generated by adiabatically expanding a high-pressure inert gas is jetted toward the melt, atomized, and rapidly solidified. The cooling rate for rapidly solidifying the melt is preferably 10 2 ° C / sec or more, more preferably 10 3 ° C / sec or more, and most preferably 10 4 ° C / sec or more. The inert gas used here is a melt having such a composition at all,
Alternatively, it means a gas that reacts only very slowly. For example, nitrogen, helium, argon, a mixture thereof, and the like can be given. Further, as long as the properties of the silver-containing alloy powder used in the present invention are not affected, a slight amount of impurity gas may be mixed.
ガスの圧力（膨張前）は、70kg/cm2G以上が好まし
く、100kg/cm2G以上がさらに好ましい。高速気流の速度
は、融液との衝突位置で100m/秒以上が好ましく、さら
に、30m/秒以上が好ましく、600m/秒以上が最も好まし
い。ガスと融液との質量比は２以上が好ましく、さらに
４以上が好ましい。The gas pressure (before expansion) is preferably 70 kg / cm 2 G or more, more preferably 100 kg / cm 2 G or more. The speed of the high-speed airflow at the collision position with the melt is preferably 100 m / sec or more, more preferably 30 m / sec or more, and most preferably 600 m / sec or more. The mass ratio of gas to melt is preferably 2 or more, more preferably 4 or more.
高圧水アトマイズ法としては、該組成の融液をるつぼ
先端より噴出する。噴出と同時に、ノズル先端より噴出
された融液に向かって、加圧された水をノズルより噴出
し、該組成の融液と衝突させ、微粒子化、急冷凝固す
る。この時、水の質量速度／融液質量速度比が10以上で
あるのが好ましく、40以上であるのがさらに好ましい。
また、水と融液との衝突位置における水の速度は80m/秒
以上が好ましく、さらに、100m/秒以上が好ましい。加
圧水をノズル先端より噴出する時の圧力は、50kg/cm2G
以上が好ましく、100kg/cm2G以上がさらに好ましい。In the high-pressure water atomizing method, a melt having the composition is jetted from the crucible tip. Simultaneously with the jetting, pressurized water is jetted from the nozzle toward the melt jetted from the nozzle tip, and collides with the melt having the composition to form fine particles and rapidly solidify. At this time, the ratio of the mass velocity of water to the mass velocity of the melt is preferably 10 or more, and more preferably 40 or more.
Further, the velocity of water at the collision position between water and the melt is preferably 80 m / sec or more, and more preferably 100 m / sec or more. The pressure when jetting pressurized water from the nozzle tip is 50 kg / cm 2 G
Or more, more preferably 100 kg / cm 2 G or more.
水アトマイズ法により作製された急冷凝固粉末は、不
規則形状のものが多く含まれるが、本発明では、球状粒
子の範疇に入る。この場合には、各粒子の長径を各粒子
の粒径とする。Although the rapidly solidified powder produced by the water atomizing method includes many irregularly shaped powders, it falls into the category of spherical particles in the present invention. In this case, the major axis of each particle is the particle diameter of each particle.
本発明の一般式AgxM1-x（但し、ＭはCu、Ni、Co、Fe
より選ばれた一種以上で、且つＭがCuを含有する場合に
は、Ni、Co、Feより選ばれた１種以上を含む）合金粉末
は、0.0005＜ｘ＜0.01（原子比）であるが、ｘが0.0005
未満では、充分な耐酸化性が得られず、高価な銀を用い
ることなどから0.0005＜ｘ＜0.005が好ましい。General formula Ag x M 1-x (where M is Cu, Ni, Co, Fe
When at least one selected from the group consisting of M and Cu contains Cu, the alloy powder contains at least one selected from the group consisting of Ni, Co, and Fe. , X is 0.0005
If less than 0.0005 <x <0.005, sufficient oxidation resistance cannot be obtained and expensive silver is used.
本発明で用いるCu、Ni、Fe、Coは、高い導電性を有す
るのみならず、特に、Ni、Fe,Coは磁気的特性に優れ、
電磁波シールド性がさらに向上できる利点がある。Cu, Ni, Fe, Co used in the present invention not only has high conductivity, in particular, Ni, Fe, Co are excellent in magnetic properties,
There is an advantage that the electromagnetic wave shielding property can be further improved.
本発明で用いられる銀含有合金粉末の平均粒子径は、
0.1〜100μｍであるが、球状の場合は、１〜30μｍが好
ましく、１〜10μｍが最も好ましい。鱗片状の場合に
は、平均径（長径と短径がある場合は両者の平均値）が
１ないし100μｍが好ましく、１ないし30μｍがさらに
好ましい。100μｍを超える場合には、印刷適性、チキ
ソトロピー、粘性が悪く、かえって導電性が悪く、ま
た、0.1μｍ未満では接触抵抗が増加し、かえって導電
性が劣る。粒径の小さいものを特に収率よく作製するた
めには、ガス圧は高い方が良く、100kg/cm2G以上が好ま
しく、また、ガス質量速度／液質量速度比が大きい方が
よく、４以上が好ましく、６以上がさらに好ましい。形
状は、球状、樹枝状、鱗片状及びそれらの混合物が用い
られるが、球状、鱗片状及びそれらの混合物がより好ま
しい。鱗片状粒子の形状は、径／厚みが３以上であるの
が好ましい。形状と粒径の測定値は走査型電子顕微鏡を
用い、視野中の100粉末の測定値の平均値を用いた。The average particle diameter of the silver-containing alloy powder used in the present invention,
Although it is 0.1 to 100 μm, in the case of a spherical shape, it is preferably 1 to 30 μm, most preferably 1 to 10 μm. In the case of a scaly shape, the average diameter (when there is a major axis and a minor axis, the average value of both) is preferably 1 to 100 μm, more preferably 1 to 30 μm. If it exceeds 100 μm, the printability, thixotropy and viscosity are poor, and the conductivity is rather poor. If it is less than 0.1 μm, the contact resistance increases and the conductivity is rather poor. In order to produce a material having a small particle size with a particularly high yield, the gas pressure is preferably high, and is preferably 100 kg / cm 2 G or more, and the gas mass velocity / liquid mass velocity ratio is preferably large. The above is preferable, and 6 or more is more preferable. As the shape, a spherical shape, a dendritic shape, a scale-like shape and a mixture thereof are used, and a spherical shape, a scale-like shape and a mixture thereof are more preferable. The shape of the scaly particles preferably has a diameter / thickness of 3 or more. The measured values of the shape and the particle size were measured using a scanning electron microscope, and the average value of the measured values of 100 powders in the visual field was used.
鱗片状粉を得るには、本発明の銀合金粉末を公知な方
法で機械的に変形させるのがよい。例えば、スタンプミ
ル、ボールミル、振動式ボールミル等の方法が好まし
い。中でも振動式ボールミルを用いるのが好ましい。振
動式ボールミルを用いる場合には、不活性あるいは還元
性雰囲気中で実施するのが好ましく、かつ、不活性液体
中で実施するのがさらに好ましい。不活性液体として
は、ミネラルスピリット、ソルベントナフサ等の有機溶
媒があげられる。不活性液体の量は、１ないし1000ml/g
粉末が好ましい。この際、公知の分散助剤を加えても良
い。In order to obtain a scaly powder, the silver alloy powder of the present invention is preferably mechanically deformed by a known method. For example, a method such as a stamp mill, a ball mill, and a vibration ball mill is preferable. Among them, it is preferable to use a vibrating ball mill. When a vibrating ball mill is used, it is preferably carried out in an inert or reducing atmosphere, and more preferably in an inert liquid. Examples of the inert liquid include organic solvents such as mineral spirits and solvent naphtha. The amount of inert liquid is 1 to 1000ml / g
Powders are preferred. At this time, a known dispersing aid may be added.
本発明で用いる銀含有合金粉末は一般式AgxM1-x（但
し、ＭはCu、Ni、Co、Feより選ばれた一種以上で、且つ
ＭがCuを含有する場合には、Ni、Co、Feより選ばれた１
種以上を含む、0.0005＜ｘ＜0.01、原子比）であるが、
必要に応じて、Al、Zn、Sn、Pb、Si、Mn、Bi、Mo、Cr、
Ir、Nb、Sb、Ｂ、Ｐ、Mg、Li、Ｃ、Na、Ba、Ti、In、A
u、Pd、Pt、Rh、Ru、Zr、Hf、Ｙ、などの金属、半金
属、及びそれらの化合物を添加してても構わない。The silver-containing alloy powder used in the present invention has a general formula Ag x M 1-x (where M is at least one selected from Cu, Ni, Co, and Fe, and when M contains Cu, Ni, 1 selected from Co, Fe
0.0005 <x <0.01, atomic ratio)
If necessary, Al, Zn, Sn, Pb, Si, Mn, Bi, Mo, Cr,
Ir, Nb, Sb, B, P, Mg, Li, C, Na, Ba, Ti, In, A
Metals such as u, Pd, Pt, Rh, Ru, Zr, Hf, and Y, metalloids, and compounds thereof may be added.
本発明の銀含有合金粉末をペーストとして使用する場
合には、有機バインダーを用いるのが好適である（この
ようなものは、通常導電性ペーストと呼ばれるが、使い
道により導電性塗料、導電性接着剤と呼ばれることもあ
り、いずれの場合も本発明の範疇に入る）。有機バイン
ダーを用いる場合は、銀含有合金粉末は主として鱗片状
からなることが導電性の面から好ましい。When the silver-containing alloy powder of the present invention is used as a paste, it is preferable to use an organic binder (this is usually called a conductive paste, but depending on the use, a conductive paint, a conductive adhesive, etc.). , And both cases fall within the scope of the present invention). When an organic binder is used, it is preferable that the silver-containing alloy powder mainly has a flaky shape from the viewpoint of conductivity.
本発明に用いる有機バインダーとしては、熱可塑性樹
脂、光硬化性樹脂、電子線硬化性樹脂、熱硬化性樹脂よ
り選ばれた１種以上であるが、熱可塑性樹脂としては、
例えば、熱可塑性アクリル樹脂、アルキッド樹脂、塩化
ビニル樹脂、ウレタン樹脂、ポリエステル樹脂、塩化ビ
ニル−酢酸ビニル共重合体、酢酸ビニル樹脂、エチレン
−酢酸ビニル共重合体、ポリカーボネート樹脂、スチレ
ン系樹脂などが挙げられる。中でも、熱可塑性アクリル
樹脂が好ましい。また、熱硬化性樹脂としては、エポキ
シ樹脂、フェノール樹脂、メラミン樹脂、アルキッド樹
脂、ポリウレタン樹脂、ポリエステル樹脂、熱硬化性ア
クリル樹脂、ポリイミド樹脂、メラミンアルキッド樹脂
及びそれらの変性樹脂の１種以上の組合せがあげられ
る。中でも、エポキシ樹脂、フェノール樹脂の１種、或
は２種以上の組合せが好ましい。エポキシ樹脂として
は、分子量380〜8000のビスフェノールＡ型エポキシ樹
脂、ノボラツク型エポキシ樹脂、ブロム化ビスフェノー
ルＡ型エポキシ樹脂、脂環式エポキシ樹脂あるいはそれ
らの変性樹脂、脂肪酸変性樹脂などがあげられる。フェ
ノール樹脂としては、ノボラック型、レゾール型のフェ
ノール樹脂、ロジ変性フェノール樹脂を単独或はエポキ
シ樹脂の架橋剤として用いるのが好ましい。As the organic binder used in the present invention, a thermoplastic resin, a photocurable resin, an electron beam curable resin, one or more selected from thermosetting resins, as the thermoplastic resin,
For example, thermoplastic acrylic resin, alkyd resin, vinyl chloride resin, urethane resin, polyester resin, vinyl chloride-vinyl acetate copolymer, vinyl acetate resin, ethylene-vinyl acetate copolymer, polycarbonate resin, styrene resin and the like. Can be Among them, a thermoplastic acrylic resin is preferable. In addition, as the thermosetting resin, epoxy resin, phenol resin, melamine resin, alkyd resin, polyurethane resin, polyester resin, thermosetting acrylic resin, polyimide resin, melamine alkyd resin and a combination of one or more modified resins thereof Is raised. Among them, one type of epoxy resin and phenol resin, or a combination of two or more types is preferable. Examples of the epoxy resin include a bisphenol A type epoxy resin having a molecular weight of 380 to 8000, a novolak type epoxy resin, a brominated bisphenol A type epoxy resin, an alicyclic epoxy resin, a modified resin thereof, and a fatty acid modified resin. As the phenol resin, it is preferable to use a novolak-type or resol-type phenol resin or a rho-modified phenol resin alone or as a crosslinking agent for an epoxy resin.
メラミン樹脂としては、例えばメチロール化メラミン
樹脂あるいはアルキル化メチロールメラミン樹脂等をエ
ポキシ樹脂の架橋剤として混ぜ合わせて用いるのが好ま
しい。エポキシ樹脂の熱硬化剤としては、必要に応じて
有機ポリアミン、無水物、ジシアンジアミド、ベンゾグ
アナミン、ビグアニド、アルキルフェニルビグアニド、
ヂフェニルビグアニド、三ふっかほう素などの公知の硬
化剤などが用いられる。As the melamine resin, for example, it is preferable to use a mixture of a methylolated melamine resin or an alkylated methylolmelamine resin as a crosslinking agent for an epoxy resin. As a thermosetting agent for the epoxy resin, as necessary, an organic polyamine, an anhydride, dicyandiamide, benzoguanamine, biguanide, alkylphenyl biguanide,
A known curing agent such as ヂ phenylbiguanide and trifluorboron is used.
本発明の導電性ペーストは、銀含有合金粉末100重量
部に対して、有機バインダー５〜100重量部を有する
が、５重量部未満の場合は、塗膜中の導電性金属粉末を
結合させておくに充分な樹脂量がなく、導電性、機械的
強度を低下させる。また、100重量部を越える場合に
は、導電性金属の量が足りず、充分な導電性が得られな
い。好ましくは、10〜50重量部である。The conductive paste of the present invention, based on 100 parts by weight of the silver-containing alloy powder, has 5 to 100 parts by weight of an organic binder, but if less than 5 parts by weight, binds the conductive metal powder in the coating film. Insufficient amount of resin to keep, lowers conductivity and mechanical strength. On the other hand, when the amount exceeds 100 parts by weight, the amount of the conductive metal is insufficient, and sufficient conductivity cannot be obtained. Preferably, it is 10 to 50 parts by weight.
本発明の導電性ペーストを用いる場合、必要に応じて
溶剤を用いることができる。溶剤の量としては、銀含有
合金粉末と有機バインダーの合計100重量部に対して０
〜100重量部を含有することが好ましい。When using the conductive paste of the present invention, a solvent can be used if necessary. The amount of the solvent is 0 to 100 parts by weight of the total of the silver-containing alloy powder and the organic binder.
It is preferable to contain 100100 parts by weight.
本発明で用いることのできる溶剤としては、樹脂によ
って異なるが、公知の溶剤で構わない。例えば、トルエ
ン、キシレンなどの芳香族類、メチルエチルケトン、メ
チルイソブチルケトンなどのケトン類、酢酸ブチル、酢
酸エチルなどのエステル、ブチルセロソルブ、エチルセ
ロソルブなどのセロソルブ類、α−テルペノール、イソ
プロパノール、ブタノールなどのアルコール類、フェノ
ール、クロルフェノール等のフェノール類、ブチルカル
ビトール、ブチルカルビトールアセテートを１種以上含
むものなどが好ましく、銀含有合金粉末と有機バインダ
ー合計100重合部に対して０〜100重量部を含有させるの
がよい。100重量部を越える場合には、印刷時ににじみ
等が生じ導電性を損ねる。１〜50重量部が好ましい。The solvent that can be used in the present invention varies depending on the resin, but may be a known solvent. For example, aromatics such as toluene and xylene, ketones such as methyl ethyl ketone and methyl isobutyl ketone, esters such as butyl acetate and ethyl acetate, cellosolves such as butyl cellosolve and ethyl cellosolve, alcohols such as α-terpenol, isopropanol and butanol Phenols such as phenol and chlorophenol, butyl carbitol, those containing one or more butyl carbitol acetate, and the like are preferable, and the silver-containing alloy powder and the organic binder are contained in an amount of 0 to 100 parts by weight based on 100 polymer parts in total. Is good. If the amount exceeds 100 parts by weight, bleeding or the like occurs at the time of printing, and the conductivity is impaired. 1 to 50 parts by weight is preferred.
本発明の導電性ペースト中の銀含有合金粉末の分散性
を向上させるため、粉末表面の金属酸化物を除去あるい
は還元するなどのため添加剤を加えるのが良い。本発明
で用いる添加剤としては、飽和脂肪酸、不飽和脂肪酸、
飽和脂肪酸の金属塩、不飽和脂肪酸の金属塩、高級脂肪
族アミン、有機チタネート化合物、有機リン化合物、ヒ
ドロキノン及びその誘導体、オキシカルボン酸、オキシ
ジカルボン酸、金属キレート形成剤、フェノール化合
物、Ｌ−アスコルビン酸誘導体、アントラセン及びその
誘導体、ロジンより選ばれた１種以上である。飽和、不
飽和脂肪酸としては、炭素数６以上が好ましく、炭素数
15〜18の樹脂酸およびそれらの金属塩がさらに好まし
い。例えば、ステアリン酸、パルミチン酸、リノール
酸、リノレン酸、オレイン酸、エライジン酸）、脂肪酸
ジカルボン酸としてアジピン酸、ピメリン酸、スペリン
酸、セバシン酸、マレイン酸、フマル酸、オキシカルボ
ン酸として例えば、りんご酸、グルコール酸、グリセリ
ン酸、乳酸、酒石酸、クエン酸、マンデル酸、サリチル
酸及びその誘導体があげられる。金属塩を構成する金属
としては、リチウム、ナトリウム、カリウム、マグネシ
ウム、カルシウム、バリウム、亜鉛、銅、銀、鉄、ニッ
ケル等が好ましい。In order to improve the dispersibility of the silver-containing alloy powder in the conductive paste of the present invention, it is preferable to add an additive for removing or reducing the metal oxide on the surface of the powder. As the additives used in the present invention, saturated fatty acids, unsaturated fatty acids,
Metal salts of saturated fatty acids, metal salts of unsaturated fatty acids, higher aliphatic amines, organic titanate compounds, organic phosphorus compounds, hydroquinone and its derivatives, oxycarboxylic acids, oxydicarboxylic acids, metal chelating agents, phenol compounds, L-ascorbin At least one selected from acid derivatives, anthracene and its derivatives, and rosin. The saturated or unsaturated fatty acid preferably has 6 or more carbon atoms.
More preferred are 15-18 resin acids and their metal salts. For example, stearic acid, palmitic acid, linoleic acid, linolenic acid, oleic acid, elaidic acid), adipic acid, pimelic acid, spearic acid, sebacic acid, maleic acid, fatty acid dicarboxylic acid, fumaric acid, and oxycarboxylic acid such as apple Acids, glycolic acid, glyceric acid, lactic acid, tartaric acid, citric acid, mandelic acid, salicylic acid and derivatives thereof. As the metal constituting the metal salt, lithium, sodium, potassium, magnesium, calcium, barium, zinc, copper, silver, iron, nickel and the like are preferable.
高級脂肪族アミンとしては、溶剤に可溶の炭素数８〜
22のものが好ましく、例えば、ステアリルアミン、パル
ミチルアミン、ベヘニルアミン、セチルアミン、オクチ
ルアミン、デシルアミン、ラウリルアミンのような飽和
モノアミン、不飽和アミンとしてはオレイルアミン、ジ
アミンとしてはステアリルプロピレンジアミン、オレイ
ルプロピレンジアミンなどが挙げられる。As the higher aliphatic amine, a solvent-soluble carbon number of 8 to
22 are preferred, for example, stearylamine, palmitylamine, behenylamine, cetylamine, octylamine, decylamine, saturated monoamines such as laurylamine, unsaturated amines as oleylamine, diamines as stearylpropylenediamine, oleylpropylenediamine And the like.
金属キレート形成剤としては、モノエタノールアミ
ン、ジエタノールアミン、トリエタノールアミン、エチ
レンジアミン、トリエチレンテトラミンなどや、アセチ
ルアセトン、トリフルオルアセチルアセトン、ヘキサフ
ルオルアセチルアセトン、ベンゾイルアセトンなどが挙
げられる。Examples of the metal chelate forming agent include monoethanolamine, diethanolamine, triethanolamine, ethylenediamine, triethylenetetramine and the like, acetylacetone, trifluoroacetylacetone, hexafluoroacetylacetone, benzoylacetone and the like.
フェノール化合物、ヒドロキノン誘導体としては、例
えば、フェノール、ハイドロキノン、カテコール、２−
メチルハイドロキノン、tert−ブチルハイドロキノン、
クロルハイドロキノン、フェニルハイドロキノン、ピロ
ガロール、1,2,4−ベンゼントリオールなどが挙げられ
る。Examples of phenol compounds and hydroquinone derivatives include phenol, hydroquinone, catechol,
Methylhydroquinone, tert-butylhydroquinone,
Chlorhydroquinone, phenylhydroquinone, pyrogallol, 1,2,4-benzenetriol and the like can be mentioned.
有機チタン化合物としては、R1−Ti−（R2）３（式中
R1は炭素数１〜４、好ましくは炭素数１〜３のアルコキ
シ基、R2は炭素数１〜20、好ましくは炭素数２〜18のカ
ルボン酸エステル）があげられ、例えば、イソプロピル
トリイソステアロイルチタネート、イソプロピルトリオ
クタノイルチタネートなどが挙げられる。As the organic titanium compound, R 1 —Ti— (R 2 ) 3 (wherein
R 1 is an alkoxy group having 1 to 4 carbon atoms, preferably 1 to 3 carbon atoms, and R 2 is a carboxylic acid ester having 1 to 20 carbon atoms, preferably 2 to 18 carbon atoms. Examples include stearoyl titanate and isopropyltrioctanoyl titanate.
アントラセン及びアントラセン誘導体としては、例え
ば、アントラセンカルボン酸があげられる。Anthracene and anthracene derivatives include, for example, anthracene carboxylic acid.
ロジンとしては、アビエチン酸、あるいは、アビエチ
ン酸誘導体が好ましい。例えば、部分水添ロジン、完全
水添ロジン、エステル化ロジン、マレイン化ロジン、不
均化ロジン、重合ロジンなどの変性ロジンなどが挙げら
れる。As rosin, abietic acid or an abietic acid derivative is preferable. For example, modified rosins such as partially hydrogenated rosin, fully hydrogenated rosin, esterified rosin, maleated rosin, disproportionated rosin, and polymerized rosin are exemplified.
Ｌ−アスコルビン酸及びその誘導体としては、例え
ば、Ｌ−アスコルビン酸、Ｌ−アスコルビン酸ジパルミ
テート、Ｌ−アスコルビン酸−６−ステアレートなどが
挙げられるが、特に、エステル、アセタール類、ケタノ
ール類などが好ましい。Examples of L-ascorbic acid and its derivatives include, for example, L-ascorbic acid, L-ascorbic acid dipalmitate, L-ascorbic acid-6-stearate and the like, and particularly preferred are esters, acetals, ketanols and the like. .
添加剤の量としては、銀含有合金粉末100重量部に対
して、前記添加剤の１種以上を0.1〜25重量部添加する
のが良い。好ましくは、0.1〜10重量部であり、さらに
0.1〜５重量部が好ましい。As for the amount of the additive, it is preferable to add 0.1 to 25 parts by weight of one or more of the above additives to 100 parts by weight of the silver-containing alloy powder. Preferably, it is 0.1 to 10 parts by weight, furthermore
0.1 to 5 parts by weight is preferred.
本発明の導電性ペーストに用いる銀含有合金粉末は、
接点抵抗の低く、高い導電性を有するものであり、ま
た、銀が合金化しているために、銀のマイグレション防
止効果に優れる。さらに、前述の添加剤を加えること
で、分散性、導電性を向上できる効果がある。Silver-containing alloy powder used in the conductive paste of the present invention,
It has low contact resistance and high conductivity, and is excellent in the effect of preventing silver migration because silver is alloyed. Further, by adding the above-mentioned additives, there is an effect that dispersibility and conductivity can be improved.
本発明で用いることのできる光硬化性樹脂としては、
紫外線硬化性樹脂、可視光線光硬化性樹脂が挙げられる
が、紫外線硬化性樹脂が好ましい。紫外線硬化性樹脂を
用いる場合には、光重合性オリゴマー、光重合体モノマ
ーを光開始剤、光開始助剤とともに用いるのが良い。As the photocurable resin that can be used in the present invention,
An ultraviolet curable resin and a visible light curable resin may be mentioned, and an ultraviolet curable resin is preferable. When using an ultraviolet curable resin, it is preferable to use a photopolymerizable oligomer and a photopolymer monomer together with a photoinitiator and a photoinitiator.
光重合性オリゴマーとは、低分子量反応性分子（数百
から数千）で、ポリエステル、エポキシ，ウレタンなど
の骨格に官能基としてアクリル基、メタアクリル基が２
つ以上付加したものであり、例えば、エポキシアクリレ
ート、ウレタンアクリレート、ポリエステルアクリレー
ト、ポリエーテルアクリレートが挙げられる。Photopolymerizable oligomers are low-molecular-weight reactive molecules (several hundreds to thousands) having two functional groups, such as polyester, epoxy, or urethane, having acryl groups and methacryl groups as functional groups.
One or more are added, for example, epoxy acrylate, urethane acrylate, polyester acrylate, and polyether acrylate.
光重合性モノマーとしては、アクリロイル基（CH2＝C
OCO−）またはメタアクリロイル基（CH2＝Ｃ（CH3）CO
−）を１分子あたり１個または２個以上を持つものであ
り、１個持つ単官能アクリレート（メタ）、２個以上持
つ多官能アクリレート、その他ビニル基（CH2＝CH−）
を持つものが好ましい。単官能アクリレートとしては、
例えば、アリルアクリレート、アリルメタアクリレー
ト、ベンジルアクリレート（メタ）、イソボニルアクリ
レート、シクロヘキシルアクリレート（メタ）、N,N−
ジメチルアミノエチルアクリレート、グリシジルメタア
クリレート、ラウリルアクリレート、ポリエチレングリ
コール90メタアクリレート、トリフロロエチルメタアク
リレートなどがある。多官能アクリレートとしては、例
えば、1,4ブタンジオールアクリレート、1,6ヘキサンジ
オールジアクリレート、ジエチレングリコールジアクリ
レート、ネオペンチルグリコールジアクリレート、ポリ
エチレングリコール400ジアクリレート、トリプロピレ
ングリコールジアクリレート、ビスフェノールＡジエト
キシジアクリレート、テトラエチレングリコールジアク
リレート、トリメチロールプロパントリアクリレート、
ペンタエリスリトールトリアクリレートなどがあげられ
る。As the photopolymerizable monomer, an acryloyl group (CH 2 CC
OCO-) or a methacryloyl group (CH 2 ＣC (CH 3 ) CO
-) a are those having one or two or more per molecule, one with a monofunctional acrylate (meth), polyfunctional acrylate having two or more other vinyl group (CH 2 = CH-)
Are preferred. As a monofunctional acrylate,
For example, allyl acrylate, allyl methacrylate, benzyl acrylate (meth), isobonyl acrylate, cyclohexyl acrylate (meth), N, N-
Examples include dimethylaminoethyl acrylate, glycidyl methacrylate, lauryl acrylate, polyethylene glycol 90 methacrylate, and trifluoroethyl methacrylate. Examples of the polyfunctional acrylate include 1,4 butanediol acrylate, 1,6 hexanediol diacrylate, diethylene glycol diacrylate, neopentyl glycol diacrylate, polyethylene glycol 400 diacrylate, tripropylene glycol diacrylate, and bisphenol A diethoxy diacrylate. Acrylate, tetraethylene glycol diacrylate, trimethylolpropane triacrylate,
Pentaerythritol triacrylate and the like.
ビニル基を有する反応性モノマーとしては、例えば、
スチレン、ビニルトルエン、酢酸ビニル、Ｎ−ビニルピ
ロリドンなどの単官能モノマーが使用できる。As the reactive monomer having a vinyl group, for example,
Monofunctional monomers such as styrene, vinyltoluene, vinyl acetate and N-vinylpyrrolidone can be used.
前記オリゴマー、モノマーとともに用いられる光開始
剤は、紫外線を吸収してラジカルを発生しやすくなる物
質が好ましく、アセトフェノン系、チオキサンソン系、
ベンゾイン系、パーオキサイド系の公知の光開始剤が使
用できる。例えば、ジエトキシアセトフェノン、４−フ
ェノキシジクロロアセトフエノン、ベンゾイン、ベンゾ
インエチルエーテル、ベンゾイニソプロピルエーテル、
ベンジルジメチルケタール、ベンゾフェノン、４−フェ
ニルベンゾフェノン、アクリル化ベンゾフェノン、チオ
キサンソン、２−クロルチオキサンソン、ベンジル、２
−エチルアンスラキノンなどがあげられる。The oligomer, the photoinitiator used together with the monomer is preferably a substance that easily absorbs ultraviolet rays to generate radicals, acetophenone, thioxanthone,
Known benzoin-based and peroxide-based photoinitiators can be used. For example, diethoxyacetophenone, 4-phenoxydichloroacetophenone, benzoin, benzoin ethyl ether, benzoinisopropyl ether,
Benzyl dimethyl ketal, benzophenone, 4-phenylbenzophenone, acrylated benzophenone, thioxanthone, 2-chlorothioxanthone, benzyl,
-Ethylanthraquinone and the like.
また、本発明で用いることのできる光開始助剤として
は、それ自身は紫外線照射により活性化はしないが、光
開始剤とともに使用すると、光開始単独よりも開始反応
が促進され、硬化反応を効率的にするものであり、脂肪
族、芳香族のアミの公知の光開始助剤が使用できる、例
えば、トリエタノールアミン、Ｎ−メチルジエタノール
アミン、ミヒラーケトン、4,4′−ジエチルアミノフェ
ノンなどの公知の光開始助剤が使用できる。In addition, the photoinitiator, which can be used in the present invention, does not activate itself by irradiation with ultraviolet light, but when used with a photoinitiator, the initiation reaction is accelerated more than the photoinitiation alone, and the curing reaction is more efficient A known photoinitiator of an aliphatic or aromatic amine can be used, for example, a known photoinitiator such as triethanolamine, N-methyldiethanolamine, Michler's ketone, and 4,4'-diethylaminophenone. A starting aid can be used.
本発明の導電性ペーストを用いる際に、公知の粘度調
整剤、希釈剤、沈降防止剤、レベリング剤、泡消剤、シ
ランカップリング剤、チタンカップリング剤等の添加剤
を適宜配合しても良いことは言うまでもない。When using the conductive paste of the present invention, well-known additives such as a viscosity modifier, a diluent, an anti-settling agent, a leveling agent, a defoaming agent, a silane coupling agent, and a titanium coupling agent may be appropriately compounded. Needless to say, it's good.
硬化方法としては、例えば、室温あるいはそれ以上、
好ましくは40〜80℃でロールコーターで塗布された光硬
化性樹脂組成物塗膜を水銀ランプ等の紫外線発生装置を
光源として照射する。光源としては公知の装置で構わな
いが、100W/cm程度で充分である。照射時間としては、
数秒から数十秒程度で充分である。As a curing method, for example, room temperature or higher,
The coating film of the photocurable resin composition applied by a roll coater is preferably irradiated at 40 to 80 ° C. using a UV generator such as a mercury lamp as a light source. As the light source, a known device may be used, but about 100 W / cm is sufficient. As the irradiation time,
A few seconds to several tens of seconds are sufficient.
また、電子線硬化性樹脂としては、前記の光硬化性樹
脂（光重合性オリゴマー、光重合性モノマー）を用いる
ことができる。電子線で硬化する場合には、高電圧で加
速した電子はエネルギーが大きく、光に比較して物質透
過性が大きいため硬化能力が大きく、しかも室温で硬化
でき、光硬化より電子線硬化の方がより好ましい。ま
た、前記オリゴマー、モノマーは電子線を吸収して、イ
オン、ラジカルを発生するため、光開始剤、光開始助剤
は原則として必要ない。電子線硬化方法は、公知の方法
で構わない。たとえば、塗膜圧100μｍ以下程度であれ
ば、150kVの加速電圧があれば充分であり、吸収線量と
しては、5Mradであれば充分であり、公知の方法が使用
できる。In addition, as the electron beam-curable resin, the above-described photocurable resin (photopolymerizable oligomer, photopolymerizable monomer) can be used. When cured by electron beam, electrons accelerated by high voltage have high energy, have high material permeability compared to light, and therefore have high curing ability, and can be cured at room temperature. Is more preferred. In addition, since the oligomer and the monomer absorb an electron beam to generate ions and radicals, a photoinitiator and a photoinitiator are not required in principle. The electron beam curing method may be a known method. For example, if the coating film pressure is about 100 μm or less, an acceleration voltage of 150 kV is sufficient, and the absorbed dose is 5 Mrad, and a known method can be used.
本発明の導電性ペーストを電子回路、電子機器など
に、素子間の導線、導電性接着剤、電磁波シールド膜と
して応用する場合、スクリーン印刷、スプレー法、刷
毛、バーコート法、ドクターブレード法などの印刷、塗
布法などの公知な方法で良い。When the conductive paste of the present invention is applied to an electronic circuit, electronic equipment, etc., as a conductive wire between elements, a conductive adhesive, an electromagnetic wave shielding film, screen printing, spraying, brushing, bar coating, doctor blade method, etc. A known method such as printing and coating may be used.
本発明の導電性ペーストからなる塗膜の導電性は、４
端子法を用いて測定した。また、銀のマイグレーション
は、1mm間隔に塗布した２本の塗膜（幅10mm、長さ30m
m）を作製し、0.2mlの水滴を塗膜間に滴かし、（この
時、水滴が２本の塗膜のどちらにも充分接触するように
する）、直流の電圧5Vを２本の塗膜に印可し、塗膜間に
流れる直流電流を測定する。電流値が100μＡを越える
場合を銀がマイグレーションが生じたものとする。The conductivity of the coating film made of the conductive paste of the present invention is 4
It was measured using the terminal method. In addition, the migration of silver was measured using two coatings (width 10 mm, length 30 m) applied at 1 mm intervals.
m), and a 0.2 ml water droplet is dropped between the coating films (at this time, the water droplet is in sufficient contact with either of the two coating films), and a DC voltage of 5 V is applied to the two coating films. Apply to the coatings and measure the DC current flowing between the coatings. When the current value exceeds 100 μA, it is assumed that silver migration has occurred.
（発明の効果） 本発明は、導電性に優れ、長期にわたり耐酸化性が良
く、銀のマイグレーションが起こらない、極少量の銀を
含む安価な銀含有合金粉末及び該粉末を用いた導電性ペ
ースト、導電体を供するものであり、電子回路用導体、
導電性接着剤、電磁シールドペースト、コンデンサー電
極用ペースト、低抵抗用ペースト及びそれらを用いた導
電体として使用できる。(Effects of the Invention) The present invention provides an inexpensive silver-containing alloy powder containing a very small amount of silver, which has excellent conductivity, has good oxidation resistance over a long period of time, and does not cause migration of silver, and a conductive paste using the powder. , To provide conductors, conductors for electronic circuits,
It can be used as a conductive adhesive, an electromagnetic shield paste, a paste for capacitor electrodes, a paste for low resistance, and a conductor using them.
（実施例） 以下、実施例と比較例によって本発明を具体的に説明
する。(Examples) Hereinafter, the present invention will be specifically described with reference to Examples and Comparative Examples.
実施例１ 銅粉（純度99.9％以上、高純度化学製）630g、銀粉
（純度99.9％以上、ミツワ化学製）3gを混合し、黒鉛る
つぼ（BNノズル付き）に入れ、アルゴン雰囲気中で高周
波誘導加熱により溶融し、1400℃まで加熱した。この融
液をアルゴン大気圧下でノズルより30秒間で噴出した。
同時に、ボンベ入りアルゴンガス（ボンベ圧力150気
圧）3NTPm3を噴出する融液に向かって周囲のノズルより
噴出した（ガス線速度300m/秒）。この時、ガス質量速
度／融液質量速度比は8.46であった。Example 1 A mixture of 630 g of copper powder (purity 99.9% or more, manufactured by High-Purity Chemical) and 3 g of silver powder (purity 99.9% or more, manufactured by Mitsuwa Chemical) was placed in a graphite crucible (with a BN nozzle), and high-frequency induction was performed in an argon atmosphere. It was melted by heating and heated to 1400 ° C. This melt was ejected from the nozzle for 30 seconds under argon atmospheric pressure.
At the same time, 3NTPm 3 of argon gas in a cylinder (cylinder pressure 150 atm) was ejected from the surrounding nozzle toward the ejected melt (gas linear velocity 300m / sec). At this time, the ratio of gas mass velocity / melt mass velocity was 8.46.
得られた粉末を走査型電子顕微鏡で観察したところ球
状（平均粒径20μｍ）であった。また、濃硝酸に粒子の
一部を溶解し、ICPにより平均の銀濃度を測定したとこ
ろ、〔Ag/（Ag＋Cu）、原子比〕ｘは0.00279であった。
得られた粉末のうち10μｍ粒径以下の粉体10gをミネラ
ルスピリット100ml中、窒素雰囲気中で、5mmΦのステン
レスボールを充填した、振動式ボールミル中で展延し
た。得られた鱗片状粉末の平均径は25μｍ、平均厚さ１
μｍであった。この粉末のうち10μｍ以下の隣片状粉末
9gを市販のアクリル系熱可塑性樹脂3g、トルエン3g、リ
ノール酸0.45gよりなる液に分散し、ガラスエポキシ樹
脂基板上に塗布し、50℃,1日大気中乾燥した。硬化後の
膜を段差計を用いて測定したところ、膜厚は、20μｍで
あった。４端子法を用いて測定した体積抵抗率は、3.5
×10-4Ω・cmであった。この膜を60℃、湿度90％の大気
中に2000時間放置したところ、体積抵抗率は殆ど変化し
なかった。また、銀のマイグレーション試験のために、
幅10mm、長さ30mm、膜間隔1mmの塗膜を２本同様に作製
した。この２本の膜間に0.2mlの水滴を落し、5V（DC）
の直流電圧を２分間印可した。塗膜、塗膜間とも外観上
の変化は見られなかった。Observation of the obtained powder with a scanning electron microscope revealed that the powder was spherical (average particle size: 20 μm). When a part of the particles was dissolved in concentrated nitric acid and the average silver concentration was measured by ICP, [Ag / (Ag + Cu), atomic ratio] x was 0.00279.
Among the obtained powders, 10 g of powder having a particle diameter of 10 μm or less was spread in a mineral ball in a vibrating ball mill filled with stainless balls of 5 mmφ in a nitrogen atmosphere in a nitrogen atmosphere. The average diameter of the obtained scaly powder is 25 μm and the average thickness is 1
μm. Neighboring flake powder of 10μm or less of this powder
9 g was dispersed in a liquid composed of 3 g of a commercially available acrylic thermoplastic resin, 3 g of toluene, and 0.45 g of linoleic acid, applied on a glass epoxy resin substrate, and dried in the air at 50 ° C. for one day. When the film after curing was measured using a step meter, the film thickness was 20 μm. The volume resistivity measured using the four-terminal method is 3.5
× 10 −4 Ω · cm. When this film was left in the air at 60 ° C. and 90% humidity for 2000 hours, the volume resistivity hardly changed. Also, for the silver migration test,
Two coating films having a width of 10 mm, a length of 30 mm, and a film interval of 1 mm were similarly prepared. Drop 0.2 ml of water between the two membranes and apply 5V (DC)
Was applied for 2 minutes. No change in appearance was observed between the coating films.
本発明で示される銀のマイグレーションの有無につい
ては、前記マイグレーション試験において、直流電流値
が100μＡを越える場合をもって銀のマイグレーション
が生じたものとする。以下の実施例、比較例についても
同様に判断する。Regarding the presence or absence of silver migration shown in the present invention, it is assumed that silver migration has occurred when the DC current value exceeds 100 μA in the migration test. The same applies to the following examples and comparative examples.
実施例２ 実施例１で得られた10μｍ以下の鱗片状粉末9gとエポ
キシ樹脂（AER661）1g、メラミン樹脂2g、ブチルカルビ
トール3g、リノレン酸0.45g、ピロカテコール0.4gをよ
く混合し、ガラスエポキシ樹脂基板上へ塗布した。塗布
後、160℃、大気中30分間加熱硬化した。硬化後の膜厚2
0μｍ、体積抵抗率は、２×10-4Ω・cmであり、60℃、9
0％湿度、2000期間放置でも体積抵抗率の変化は認めら
れなかった。また、実施例１と同様にして銀のマイグレ
ーション試験をしたところ、銀のマイグレーションは殆
ど認められなかった。Example 2 9 g of the flaky powder of 10 μm or less obtained in Example 1, 1 g of an epoxy resin (AER661), 2 g of a melamine resin, 3 g of butyl carbitol, 0.45 g of linolenic acid, and 0.4 g of pyrocatechol were mixed well, and then mixed with glass epoxy. It was applied on a resin substrate. After the application, it was cured by heating at 160 ° C. for 30 minutes in the atmosphere. Film thickness after curing 2
0 μm, volume resistivity is 2 × 10 −4 Ω · cm, 60 ° C., 9
No change in volume resistivity was observed even after leaving it at 0% humidity for 2000 periods. When a silver migration test was performed in the same manner as in Example 1, almost no silver migration was recognized.
実施例３ 実施例１で得られた鱗片状粉末のうち10μｍ以下の粉
末11gとエポキシ樹脂（AER331）1g、エポキシ樹脂（AER
337）2g、ジシアンジアミド0.03g、ハイドロキノン0.
2gを混ぜ合わせ同様にしてガラスエポキシ樹脂基板上へ
塗布した。塗膜の厚さは、18μｍであった。得られた塗
膜を150℃、大気中20分間加熱硬化した。硬化後の膜の
体積抵抗率は、６×10-4Ω・cmであった。さらに、、60
℃、90％湿度中2000時間放置したところ、体積抵抗率
は、殆ど変化しなかった。また、銀のマイグレーション
試験を実施例１と同様にして行ったところ銀のマイグレ
ーションは殆ど認められなかった。Example 3 Of the scaly powder obtained in Example 1, 11 g of powder having a size of 10 μm or less, 1 g of epoxy resin (AER331), and epoxy resin (AER
337) 2 g, dicyandiamide 0.03 g, hydroquinone 0.
2 g were mixed and coated on a glass epoxy resin substrate in the same manner. The thickness of the coating film was 18 μm. The obtained coating film was cured by heating at 150 ° C. in the air for 20 minutes. The volume resistivity of the cured film was 6 × 10 −4 Ω · cm. In addition, 60
When left for 2000 hours at 90 ° C. and 90% humidity, the volume resistivity hardly changed. When a silver migration test was conducted in the same manner as in Example 1, almost no silver migration was recognized.
実施例４ 銅粉（純度99.9％以上、高純度化学製）630gと銀粉
（純度99.9％以上、みつわ化学製）1gを実施例１と同様
にして黒鉛るつぼ中アルゴン雰囲気下で1500℃まで溶解
した。溶解後、黒鉛ルツボの先端に取り付けたBNノズル
より、アルゴン雰囲気中へ25秒間で噴出した。噴出と同
時に、オボンベ入りアルゴンガス（ボンベ圧力130気
圧）2.2NTPm3を噴出する融液に向けて周囲のノズルから
噴出した（ガス線速度200m/秒）。この時のガス質量速
度／融液質量速度比は6.2であった。得られた粉末は平
均粒径15μｍの球状であった。得られた粉末の10μｍ以
下10gをミネラルスプリット100ml、窒素雰囲気下、振動
式ボールミルを用いて展延した。平均粒径19μｍ、厚さ
１μｍの鱗片状粉末が得られた。また、ICPにより測定
したところ、粉末の〔Ag/（Ag＋Cu）、原子比〕ｘは0.0
00932であった。Example 4 630 g of copper powder (purity 99.9% or more, manufactured by High Purity Chemical) and 1 g of silver powder (purity 99.9% or more, manufactured by Mitsuwa Chemical) were dissolved in a graphite crucible up to 1500 ° C. in an argon atmosphere in the same manner as in Example 1. . After dissolution, it was jetted into an argon atmosphere for 25 seconds from a BN nozzle attached to the tip of a graphite crucible. Jetting the same time, it was ejected from the periphery of the nozzle toward the melt ejecting Obonbe containing argon gas (cylinder pressure 130 atmospheres) 2.2NTPm 3 (gas linear velocity 200 meters / sec). At this time, the gas mass velocity / melt mass velocity ratio was 6.2. The obtained powder was spherical with an average particle size of 15 μm. 10 g of the obtained powder having a particle size of 10 μm or less was spread using a vibrating ball mill under a nitrogen atmosphere in 100 ml of a mineral split. A flaky powder having an average particle size of 19 μm and a thickness of 1 μm was obtained. Also, when measured by ICP, [Ag / (Ag + Cu), atomic ratio] x of the powder was 0.0
00932.
得られた、鱗片状粉末のうち10μｍ以下の粉末9gとフ
ェノール樹脂（CJ1004）4g、ブチルカルビトール2g、メ
チルエチルケトン2g、アントラセン0.05、ステアリルア
ミン0.05g、ピロカテコール0.1gを混合し、ガラスエポ
キシ樹脂基板状へ塗布した。塗膜膜は、22μｍであっ
た。得られた塗膜を140℃、１時間大気中加熱硬化し
た。A glass epoxy resin substrate was prepared by mixing 9 g of the obtained scaly powder with a particle size of 10 μm or less, 4 g of phenol resin (CJ1004), 2 g of butyl carbitol, 2 g of methyl ethyl ketone, 0.05 anthracene, 0.05 g of stearylamine, and 0.1 g of pyrocatechol. It was applied to the shape. The coating film was 22 μm. The obtained coating film was heated and cured in air at 140 ° C. for 1 hour.
硬化後の塗膜の体積抵抗率は、3.5×10-4Ω・cmであ
り、60℃、90％湿度2000時間放置しても体積抵抗率は殆
ど変化しなかった。また、実施例１と同様にして、銀の
マイグレーションを試験したところ、マイグレーション
は殆ど認められなかった。The volume resistivity of the cured coating film was 3.5 × 10 −4 Ω · cm, and the volume resistivity did not substantially change even after being left at 60 ° C. and 90% humidity for 2000 hours. When the migration of silver was tested in the same manner as in Example 1, almost no migration was recognized.
実施例５ ニッケル粉末（純度99.9％以上、みつわ化学製）630
g、銀粉末（純度99.9％以上、みつわ化学製）10gとをBN
（ボロンナイトライド）ルツボにいれ、高周波誘導加熱
を用いて1650℃まで溶解した。溶解後、るつぼの先端に
取り付けたBNノズルにより、アルゴン大気圧下へ融液を
30秒間で噴出した。噴出と同時に、ボンベ入りアルゴン
ガス（ボンベ圧150気圧）3NTPm3を周囲のノズルより融
液に向かって噴出した。この時、ガス質量速度／液質量
速度比は8.3であった（ガス線速度320m/秒）。Example 5 Nickel powder (purity 99.9% or more, manufactured by Mitsuwa Chemical) 630
g, silver powder (purity 99.9% or more, manufactured by Mitsuwa Chemical) 10 g and BN
(Boron nitride) It was put in a crucible and melted to 1650 ° C. using high-frequency induction heating. After dissolution, the melt is brought to atmospheric pressure with argon using a BN nozzle attached to the tip of the crucible.
It erupted in 30 seconds. Simultaneously with the ejection, 3NTPm 3 of argon gas in a cylinder (cylinder pressure 150 atm) was ejected from the surrounding nozzle toward the melt. At this time, the gas mass velocity / liquid mass velocity ratio was 8.3 (gas linear velocity 320 m / sec).
得られた粉末は、平均径23μｍの球状粉であった。ま
た、ICPにより測定したところ、〔Ag/（Ag＋Cu）〕ｘは
0.00917であった。得られた粉末の中10μｍ以下の粉末1
0gを100mlのミネラルスピリットとともに、振動式ボー
ルミル中で展延した。得られた粉末は、平均径20μｍ、
厚さ1.5μｍの鱗片状であった。得られた鱗片状粉末の
中10μｍ以下の粉末9gを実施例１で使用したアクリル樹
脂3g、エチルセロソルブ1g、トルエン2g、フェノール0.
1g,パルミチン酸0.15gとよく混合し、ガラスエポキシ樹
脂基板上へ塗布した。塗布後、50℃、１日大気中で乾燥
した。The obtained powder was a spherical powder having an average diameter of 23 μm. [Ag / (Ag + Cu)] x was measured by ICP.
It was 0.00917. Powder 1 of 10 μm or less in the obtained powder 1
0 g was spread in a vibrating ball mill with 100 ml of mineral spirits. The resulting powder has an average diameter of 20 μm,
It was scale-like with a thickness of 1.5 μm. 9 g of powder having a size of 10 μm or less in the obtained flaky powder was 3 g of the acrylic resin used in Example 1, 1 g of ethyl cellosolve, 2 g of toluene, and 0.1 g of phenol.
1 g and palmitic acid 0.15 g were mixed well and applied on a glass epoxy resin substrate. After the application, it was dried at 50 ° C. for one day in the air.
硬化後の塗膜は19μｍ、体積抵抗率は、３×10-4Ω・
cmであった。また、60℃,90％湿度中2000時間放置後の
体積抵抗率は、殆ど変化なかった。さらに、銀のマイグ
レーション試験を行ったところ、銀のマイグレーション
は認められなかった。The cured film has a thickness of 19 μm and a volume resistivity of 3 × 10 −4 Ω ·
cm. In addition, the volume resistivity after leaving at 60 ° C. and 90% humidity for 2000 hours hardly changed. Further, when a silver migration test was performed, no silver migration was recognized.
実施例６ 銅粉（純度99.9％以上、高純度化学製）500g、ニッケ
ル粉（純度99.95％以上、みつわ化学製）30g、銀粉（純
度99.9％以上、みつわ化学製）6gとを混合し、BN（ボロ
ンナイトライド）ルツボ中で高周波誘導加熱を用いて15
50℃に溶解した。溶解後、ルツボ先端に取り付けたBNノ
ズルより溶液をアルゴン大気圧下へ40秒で噴出した。噴
出と同時に、ボンベ入りアルゴンガス（ボンベ圧130気
圧）3NTPm3を融液に向かって噴出した。この時、ガス質
量速度／液質量速度比は9.9であった（ガス線速度260m/
秒）。得られた粉末は、平均粒径16μｍの球状粉末であ
った。ICPで測定したところ、〔Ag/（Ag＋Cu）〕ｘは0.
00658であった。Example 6 500 g of copper powder (purity 99.9% or higher, manufactured by High Purity Chemical), 30 g of nickel powder (purity 99.95% or more, manufactured by Mitsuwa Chemical), and 6 g of silver powder (purity 99.9% or higher, manufactured by Mitsuwa Chemical) were mixed with BN. (Boron nitride) Using high frequency induction heating in a crucible
Dissolved at 50 ° C. After dissolution, the solution was ejected from the BN nozzle attached to the crucible tip under argon atmospheric pressure in 40 seconds. Jetting the same time, a bottled argon gas (cylinder pressure 130 atmospheres) 3NTPm 3 jetted toward the melt. At this time, the gas mass velocity / liquid mass velocity ratio was 9.9 (gas linear velocity 260 m /
Seconds). The obtained powder was a spherical powder having an average particle size of 16 μm. When measured by ICP, [Ag / (Ag + Cu)] x was 0.
00658.
得られた球状粉末のうち、10μｍ以下10gをのミネラ
ルスピリット100mlとともに、振動式ボールミルで展延
した。得られた粉末は、鱗片状で平均粒径14μｍ、厚さ
２μｍであった。このうち、10μｍ以下の鱗片粉6gと10
μｍ以下の球状粉3gとを混合し、さらに、エポキシ（AE
R661）1g,メラミン（日立化成メラミン27）2g、ブチル
カルビトール3g、ピロガロール0.3g,ピロカテコール0.3
g,リノレン酸0.3gと混合し、実施例１と同様に、ガラス
エポキシ樹脂基板上へ塗布した。塗布膜を150℃、30分
間大気中で加熱硬化した。硬化後の膜厚は21μｍであ
り、体積抵抗率は、２×10-4Ω・cmであった。硬化後の
塗膜を60℃,90％湿度中で放置したところ、体積抵抗率
は、殆ど変かなかった。また、銀のマイグレーション試
験を同様にして行ったところ、銀のマイグレーションは
殆ど認められなかった。Of the obtained spherical powder, 10 g of 10 μm or less together with 100 ml of mineral spirit was spread by a vibrating ball mill. The resulting powder was scaly and had an average particle size of 14 μm and a thickness of 2 μm. Of these, 6 g of scale powder of 10 μm or less and 10 g
3 g of spherical powder of less than μm and mix with epoxy (AE
R661) 1 g, melamine (Hitachi Chemical Melamine 27) 2 g, butyl carbitol 3 g, pyrogallol 0.3 g, pyrocatechol 0.3
g, and 0.3 g of linolenic acid, and applied to a glass epoxy resin substrate in the same manner as in Example 1. The coating film was cured by heating at 150 ° C. for 30 minutes in the atmosphere. The film thickness after curing was 21 μm, and the volume resistivity was 2 × 10 −4 Ω · cm. When the cured coating film was allowed to stand at 60 ° C. and 90% humidity, the volume resistivity hardly changed. When a silver migration test was performed in the same manner, almost no silver migration was recognized.
実施例７ 銅粉（純度99.9％以上、高純度化学製）500g、鉄粉
（純度99.9％以上、高純度化学製）15g、コバルト粉
（純度99.95％以上、みつわ化学製）15g、銀粉（純度9
9.9％以上、みつわ化学製）6gを混合し、BNるつぼ中、
アルゴン雰囲気下で1750℃まで溶解した。溶解後、るつ
ぼ先端に取り付けたBNノズルよりアルゴン雰囲気中へ30
秒で噴出した。噴出と同時に、周囲に取り付けたBNノズ
ルより融液に向かってボンベ入りアルゴンガス（ボンベ
圧150気圧）4NTPm3を噴出した（ガス線速度350m/秒）。
この時、ガス質量速度／液質量速度比は12.9であった。
得られた粉末は、平均粒径18μｍの球状粉であった。IC
Pで測定したところ、Ag/（Ag＋Cu＋Fe＋Co）（原子比）
ｘは0.0066であった。このうち10μｍ以下の粉末10gを
ミネラルスピリット100mlとともに振動式ボールミルを
用いて展延した。得られた粉末は、平均径18μｍ、厚さ
1.9μｍの鱗片状粉末であった。このうち10μｍ以下の
鱗片粉9gと熱可塑性アクリル樹脂3g,トルエン、2g,ブチ
ルセロソルブ1g、パルミチン酸0.5とを混合し、ガラス
エポキシ樹脂基板上へ塗布した。塗膜を50℃、大気中１
日乾燥した。乾燥後の塗膜の膜厚は、19μｍであり、体
積抵抗率は２×10-4Ω・cmであった。乾燥後の塗膜を60
℃、90％湿度中2000時間放置したが、体積抵抗率は殆ど
変化なかった。また、銀のマイグレーション試験をした
ところ、銀のマイグレーションは殆ど認められなかっ
た。Example 7 Copper powder (purity 99.9% or more, high purity chemical) 500g, iron powder (purity 99.9% or more, high purity chemical) 15g, cobalt powder (purity 99.95% or more, Mitsuwa Chemical) 15g, silver powder (purity) 9
9.9% or more, manufactured by Mitsuwa Chemical)
It melted to 1750 ° C under an argon atmosphere. After dissolution, put into the argon atmosphere from the BN nozzle attached to the crucible tip.
Erupted in seconds. Jetting the same time, it was ejected Bottled argon gas (cylinder pressure 150 atmospheres) 4NTPm 3 towards the melt from BN nozzle mounted around (the gas linear velocity 350 meters / sec).
At this time, the ratio of gas mass velocity / liquid mass velocity was 12.9.
The obtained powder was a spherical powder having an average particle size of 18 μm. I c
When measured with P, Ag / (Ag + Cu + Fe + Co) (atomic ratio)
x was 0.0066. Among them, 10 g of powder having a size of 10 μm or less was spread using a vibrating ball mill together with 100 ml of mineral spirit. The obtained powder has an average diameter of 18 μm and thickness
It was a 1.9 μm scaly powder. Among them, 9 g of flake powder of 10 μm or less, 3 g of thermoplastic acrylic resin, 2 g of toluene, 1 g of butyl cellosolve, and 0.5 of palmitic acid were mixed and applied onto a glass epoxy resin substrate. Apply the coating film at 50 ℃ in air 1
Sun dried. The thickness of the dried coating film was 19 μm, and the volume resistivity was 2 × 10 −4 Ω · cm. 60 coats after drying
After being left for 2000 hours at 90 ° C. and 90% humidity, the volume resistivity hardly changed. When a silver migration test was performed, almost no silver migration was recognized.
（比較例） 比較例１ 実施例１と同様にして得られた鱗片状粉末の中10μｍ
以下9gと実施例１で用いたアクリル樹脂20g、トルエン6
g、リノール酸0.9gとを混ぜ合わせ、実施例１と同様に
してガラスエポキシ樹脂基板上へ塗布し、塗膜を50℃、
大気中１日乾燥した。乾燥後の体積抵抗率は、６×103
Ω・cmと高かった。(Comparative Example) Comparative Example 1 10 μm in scaly powder obtained in the same manner as in Example 1.
The following 9 g, the acrylic resin 20 g used in Example 1, and toluene 6
g, and linoleic acid 0.9 g, and applied to a glass epoxy resin substrate in the same manner as in Example 1.
Dried in air for one day. The volume resistivity after drying is 6 × 10 3
It was as high as Ω · cm.
比較例２ 実施例１と同様にして得られた鱗片状粉末の中10μｍ
以下9gと実施例１で用いたアクリル樹脂0.1g、トルエン
3g,エチルセロソルブ3g、リノール酸5gとを混合し、実
施例１と同様にしてガラスエポイキシ樹脂基板上へ塗布
した。塗膜を50℃、大気中１日乾燥した。乾燥後の塗膜
の体積抵抗率は、６×105Ω・cmと高かった。Comparative Example 2 10 μm in a scaly powder obtained in the same manner as in Example 1.
The following 9 g, 0.1 g of the acrylic resin used in Example 1, and toluene
3 g, 3 g of ethyl cellosolve and 5 g of linoleic acid were mixed and applied on a glass epoxy resin substrate in the same manner as in Example 1. The coating was dried at 50 ° C. in air for one day. The volume resistivity of the dried coating film was as high as 6 × 10 5 Ω · cm.
比較例３ 市販の電解銅粉末（平均粒径15μｍ）10gと実施例１
で用いたアクリル樹脂4g、トルエン3g,エチルセロソル
ブ2g、リノレン酸0.2gとを混合し、実施例１と同様にし
てガラスエポキシ樹脂基板上へ塗布した。塗膜を50℃，
大気中１日乾燥した。乾燥後の塗膜の体積抵抗率は、し
た。３×10-3Ω・cmであり、60℃,90％湿度中2000時間
放置したところ、体積抵抗率が初期体積抵抗率の15倍に
増加していた。Comparative Example 3 10 g of commercially available electrolytic copper powder (average particle size: 15 μm) and Example 1
4 g of the acrylic resin, 3 g of toluene, 2 g of ethyl cellosolve, and 0.2 g of linolenic acid used in the above were mixed and applied to the glass epoxy resin substrate in the same manner as in Example 1. Apply the coating at 50 ℃
Dried in air for one day. The volume resistivity of the dried coating film was determined. It was 3 × 10 −3 Ω · cm, and when left at 60 ° C. and 90% humidity for 2000 hours, the volume resistivity increased to 15 times the initial volume resistivity.
比較例４ 市販の銀粉末（平均粒径２μｍ）10gと実施例１で用
いたアクリル樹脂4g、トルエン2g,エチルセロソルブ2
g、リノール酸0.1gとを混合し、実施例１と同様にして
ガラスエポキシ樹脂基板上へ塗布した。塗膜を50℃、大
気中１日乾燥した。乾燥後の塗膜厚は21μｍ、体積抵抗
率は、１×10-4Ω・cmであった。しかし、銀のマイグレ
ーション試験したところ、10秒ほどで銀のマイグレーシ
ョンが起こり（電流値＞100μＡ）、塗膜間に銀が析出
した。Comparative Example 4 10 g of commercially available silver powder (average particle size 2 μm), 4 g of the acrylic resin used in Example 1, 2 g of toluene, and 2 g of ethyl cellosolve 2
g and linoleic acid 0.1 g were mixed and applied on a glass epoxy resin substrate in the same manner as in Example 1. The coating was dried at 50 ° C. in air for one day. After drying, the film thickness was 21 μm and the volume resistivity was 1 × 10 −4 Ω · cm. However, a silver migration test revealed that silver migration occurred in about 10 seconds (current value> 100 μA), and silver was deposited between the coating films.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｃ２２Ｃ 9/00 Ｃ２２Ｃ 9/00 19/00 19/00 Ｑ 38/00 ３０２ 38/00 ３０２Ｚ Ｈ０１Ｂ 1/00 9459−5Ｌ Ｈ０１Ｂ 1/00 Ｊ 1/22 1/22 Ａ Ｈ０５Ｋ 9/00 Ｈ０５Ｋ 9/00 Ｘ ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 6 Identification number Office reference number FI Technical indication location C22C 9/00 C22C 9/00 19/00 19/00 Q 38/00 302 38/00 302Z H01B 1 / 009459-5L H01B 1/00 J 1/22 1/22 A H05K 9/00 H05K 9/00 X
Claims (6)
eより選ばれた一種以上で、且つＭがCuを含有する場合
には、Ni、Co、Feより選ばれた１種以上を含む、0.0005
＜ｘ＜0.01、原子比）で表され、且つかかる組成の融液
を高圧アトマイズ法を用いて急冷凝固して得られる銀含
有合金粉末。[Claim 1] The general formula Ag x M 1-x (where M is Cu, Ni, Co, F
e, at least one selected from e, and when M contains Cu, contains at least one selected from Ni, Co, Fe;
<X <0.01, atomic ratio), and a silver-containing alloy powder obtained by rapidly solidifying a melt having such a composition using a high-pressure atomization method.
ズ法が、高圧水アトマイズ法域は高圧ガスアトマイズ法
より選ばれた１種以上であることを特徴とする第１項記
載の銀含有合金粉末。2. The silver-containing alloy powder according to claim 1, wherein the high-pressure atomization method according to claim 1 has at least one selected from a high-pressure gas atomization method in a high-pressure water atomization method. .
粉末の平均粒子径が0.1μｍ〜100μｍである球状、樹板
状、鱗片状或いはそれらの１種以上の混合物であること
を特徴とする第１または２項記載の銀含有合金粉末。3. The silver-containing alloy powder according to claim 1 or 2, wherein the silver-containing alloy powder has a mean particle size of 0.1 μm to 100 μm, which is spherical, tree-like, scale-like, or a mixture of at least one of them. 3. The silver-containing alloy powder according to claim 1 or 2,
載の銀含有粉末100重量部に対して有機バインダー５〜1
00重量部を有する導電性ペースト。4. An organic binder 5-1 based on 100 parts by weight of the silver-containing powder according to any one of claims 1 to 3.
Conductive paste having 00 parts by weight.
ーが熱可塑性樹脂、光硬化性、電子線硬化性、あるいは
熱硬化性樹脂より選ばれた１種以上であることを特徴と
する第４項記載の導電性ペースト。5. The method according to claim 4, wherein the organic binder is at least one selected from the group consisting of a thermoplastic resin, a photocurable resin, an electron beam curable resin, and a thermosetting resin. 5. The conductive paste according to claim 4.
性ペーストに対して、飽和脂肪酸、不飽和脂肪酸、飽和
脂肪酸の金属塩、不飽和脂肪酸の金属塩、高級脂肪族ア
ミン、有機チタネート化合物、有機リン化合物、ヒドロ
キノン誘導体、オキシカルボン酸、オキシジカルボン
酸、金属キレート形成剤、フェノール化合物、Ｌ−アス
コルビン酸誘導体、アントラセン及びその誘導体、ロジ
ンより選ばれた１種以上を銀含有合金粉末100重量部に
対して0.1〜25重量部を含有させたことを特徴とする導
電性ペースト。6. The conductive paste according to claim 4 or 5, wherein a saturated fatty acid, an unsaturated fatty acid, a metal salt of a saturated fatty acid, a metal salt of an unsaturated fatty acid, a higher aliphatic amine, and an organic titanate are used. A silver-containing alloy powder containing at least one selected from a compound, an organic phosphorus compound, a hydroquinone derivative, an oxycarboxylic acid, an oxydicarboxylic acid, a metal chelating agent, a phenol compound, an L-ascorbic acid derivative, anthracene and its derivatives, and a rosin; A conductive paste containing 0.1 to 25 parts by weight with respect to parts by weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2041093A JP2643520B2 (en) | 1990-02-23 | 1990-02-23 | Silver-containing alloy powder and conductive paste using the powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2041093A JP2643520B2 (en) | 1990-02-23 | 1990-02-23 | Silver-containing alloy powder and conductive paste using the powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03247702A JPH03247702A (en) | 1991-11-05 |
| JP2643520B2 true JP2643520B2 (en) | 1997-08-20 |
Family
ID=12598864
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2041093A Expired - Lifetime JP2643520B2 (en) | 1990-02-23 | 1990-02-23 | Silver-containing alloy powder and conductive paste using the powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2643520B2 (en) |
Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5136365A (en) * | 1990-09-27 | 1992-08-04 | Motorola, Inc. | Anisotropic conductive adhesive and encapsulant material |
| US5840432A (en) * | 1995-02-13 | 1998-11-24 | Hitachi Chemical Company, Ltd. | Electroconductive paste |
| US6487774B1 (en) | 1998-01-22 | 2002-12-03 | Matsushita Electric Industrial Co., Ltd. | Method of forming an electronic component using ink |
| JP4507378B2 (en) * | 2000-10-02 | 2010-07-21 | 株式会社村田製作所 | Method for producing multilayer ceramic electronic component and conductive paste |
| JP2002197921A (en) * | 2000-12-26 | 2002-07-12 | Toppan Forms Co Ltd | Electron beam curing conductive paste, conductor circuit using it, and ic media having antenna part formed with electron beam curing conductive paste |
| JP2002197435A (en) * | 2000-12-27 | 2002-07-12 | Toppan Forms Co Ltd | Method for forming antenna circuit for non-contacting ic medium using electron beam and the medium provided with the circuit |
| CA2359347A1 (en) | 2001-10-18 | 2003-04-18 | Cesur Celik | Laminated ceramic capacitor internal electrode material |
| JP4380145B2 (en) * | 2002-11-20 | 2009-12-09 | 株式会社村田製作所 | Method for manufacturing conductive paste and ceramic electronic component |
| JP5405814B2 (en) * | 2007-12-28 | 2014-02-05 | 三井金属鉱業株式会社 | Copper powder for conductive paste and conductive paste |
| JP6855292B2 (en) * | 2016-03-16 | 2021-04-07 | Ｄｏｗａエレクトロニクス株式会社 | Ag-Cu alloy powder and its manufacturing method |
| CN114786453A (en) * | 2022-04-02 | 2022-07-22 | 昆明理工大学 | Mg-Li alloy/silicon steel plate electromagnetic shielding material and preparation method thereof |
| KR20230161994A (en) * | 2022-05-18 | 2023-11-28 | 미쓰이금속광업주식회사 | Copper powder and its production method |
| CN115213419A (en) * | 2022-07-12 | 2022-10-21 | 贵州越达增材材料科技有限公司 | Silver powder manufacturing method |
-
1990
- 1990-02-23 JP JP2041093A patent/JP2643520B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03247702A (en) | 1991-11-05 |
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