JP5927177B2 - Die bonding agent - Google Patents
Die bonding agent Download PDFInfo
- Publication number
- JP5927177B2 JP5927177B2 JP2013502355A JP2013502355A JP5927177B2 JP 5927177 B2 JP5927177 B2 JP 5927177B2 JP 2013502355 A JP2013502355 A JP 2013502355A JP 2013502355 A JP2013502355 A JP 2013502355A JP 5927177 B2 JP5927177 B2 JP 5927177B2
- Authority
- JP
- Japan
- Prior art keywords
- silver
- component
- resin
- particles
- bonding agent
- 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.)
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- 239000007767 bonding agent Substances 0.000 title claims description 16
- 239000002245 particle Substances 0.000 claims description 103
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 96
- 229910052709 silver Inorganic materials 0.000 claims description 96
- 239000004332 silver Substances 0.000 claims description 96
- 229920000647 polyepoxide Polymers 0.000 claims description 49
- 239000003822 epoxy resin Substances 0.000 claims description 48
- -1 amine compound Chemical class 0.000 claims description 38
- 229920005989 resin Polymers 0.000 claims description 37
- 239000011347 resin Substances 0.000 claims description 37
- 239000011247 coating layer Substances 0.000 claims description 15
- 239000000919 ceramic Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 12
- 239000005011 phenolic resin Substances 0.000 claims description 12
- 229910052782 aluminium Inorganic materials 0.000 claims description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 11
- 239000011521 glass Substances 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 239000007822 coupling agent Substances 0.000 claims description 10
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 9
- 239000000194 fatty acid Substances 0.000 claims description 9
- 229930195729 fatty acid Natural products 0.000 claims description 9
- 229920001187 thermosetting polymer Polymers 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- 239000004925 Acrylic resin Substances 0.000 claims description 6
- PEEHTFAAVSWFBL-UHFFFAOYSA-N Maleimide Chemical compound O=C1NC(=O)C=C1 PEEHTFAAVSWFBL-UHFFFAOYSA-N 0.000 claims description 6
- 150000004665 fatty acids Chemical class 0.000 claims description 6
- 229920002803 thermoplastic polyurethane Polymers 0.000 claims description 6
- 229920000178 Acrylic resin Polymers 0.000 claims description 5
- 150000008065 acid anhydrides Chemical class 0.000 claims description 5
- 238000002356 laser light scattering Methods 0.000 claims description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 4
- 239000005642 Oleic acid Substances 0.000 claims description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 4
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- 150000004696 coordination complex Chemical class 0.000 claims description 3
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- 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 13
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- XQUPVDVFXZDTLT-UHFFFAOYSA-N 1-[4-[[4-(2,5-dioxopyrrol-1-yl)phenyl]methyl]phenyl]pyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C(C=C1)=CC=C1CC1=CC=C(N2C(C=CC2=O)=O)C=C1 XQUPVDVFXZDTLT-UHFFFAOYSA-N 0.000 description 4
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
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- KUAUJXBLDYVELT-UHFFFAOYSA-N 2-[[2,2-dimethyl-3-(oxiran-2-ylmethoxy)propoxy]methyl]oxirane Chemical compound C1OC1COCC(C)(C)COCC1CO1 KUAUJXBLDYVELT-UHFFFAOYSA-N 0.000 description 3
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- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
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- QYZFTMMPKCOTAN-UHFFFAOYSA-N n-[2-(2-hydroxyethylamino)ethyl]-2-[[1-[2-(2-hydroxyethylamino)ethylamino]-2-methyl-1-oxopropan-2-yl]diazenyl]-2-methylpropanamide Chemical compound OCCNCCNC(=O)C(C)(C)N=NC(C)(C)C(=O)NCCNCCO QYZFTMMPKCOTAN-UHFFFAOYSA-N 0.000 description 3
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- QEQBMZQFDDDTPN-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy benzenecarboperoxoate Chemical compound CC(C)(C)OOOC(=O)C1=CC=CC=C1 QEQBMZQFDDDTPN-UHFFFAOYSA-N 0.000 description 2
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- SYEWHONLFGZGLK-UHFFFAOYSA-N 2-[1,3-bis(oxiran-2-ylmethoxy)propan-2-yloxymethyl]oxirane Chemical compound C1OC1COCC(OCC1OC1)COCC1CO1 SYEWHONLFGZGLK-UHFFFAOYSA-N 0.000 description 2
- HDPLHDGYGLENEI-UHFFFAOYSA-N 2-[1-(oxiran-2-ylmethoxy)propan-2-yloxymethyl]oxirane Chemical compound C1OC1COC(C)COCC1CO1 HDPLHDGYGLENEI-UHFFFAOYSA-N 0.000 description 2
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- ULQMPOIOSDXIGC-UHFFFAOYSA-N [2,2-dimethyl-3-(2-methylprop-2-enoyloxy)propyl] 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC(C)(C)COC(=O)C(C)=C ULQMPOIOSDXIGC-UHFFFAOYSA-N 0.000 description 1
- LEPMNRDLCZJGTG-UHFFFAOYSA-N [2,2-dimethyl-3-(2-methylprop-2-enoyloxy)propyl] 2-methylprop-2-enoate;3-hydroxy-2,2-dimethylpropanoic acid Chemical compound OCC(C)(C)C(O)=O.CC(=C)C(=O)OCC(C)(C)COC(=O)C(C)=C LEPMNRDLCZJGTG-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
- URLYGBGJPQYXBN-UHFFFAOYSA-N [4-(hydroxymethyl)cyclohexyl]methyl prop-2-enoate Chemical compound OCC1CCC(COC(=O)C=C)CC1 URLYGBGJPQYXBN-UHFFFAOYSA-N 0.000 description 1
- MFIBZDZRPYQXOM-UHFFFAOYSA-N [dimethyl-[3-(oxiran-2-ylmethoxy)propyl]silyl]oxy-dimethyl-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound C1OC1COCCC[Si](C)(C)O[Si](C)(C)CCCOCC1CO1 MFIBZDZRPYQXOM-UHFFFAOYSA-N 0.000 description 1
- KYIKRXIYLAGAKQ-UHFFFAOYSA-N abcn Chemical compound C1CCCCC1(C#N)N=NC1(C#N)CCCCC1 KYIKRXIYLAGAKQ-UHFFFAOYSA-N 0.000 description 1
- ZGACYOKNEKDSNK-UHFFFAOYSA-N ac1mjht3 Chemical compound C1CC2(C)C3C(=O)OC(=O)C3C1(C(C)C)C=C2 ZGACYOKNEKDSNK-UHFFFAOYSA-N 0.000 description 1
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 125000003342 alkenyl group Chemical group 0.000 description 1
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 1
- KEBBHXFLBGHGMA-UHFFFAOYSA-K aluminum;4-ethyl-3-oxohexanoate Chemical compound [Al+3].CCC(CC)C(=O)CC([O-])=O.CCC(CC)C(=O)CC([O-])=O.CCC(CC)C(=O)CC([O-])=O KEBBHXFLBGHGMA-UHFFFAOYSA-K 0.000 description 1
- LIQDVINWFSWENU-UHFFFAOYSA-K aluminum;prop-2-enoate Chemical compound [Al+3].[O-]C(=O)C=C.[O-]C(=O)C=C.[O-]C(=O)C=C LIQDVINWFSWENU-UHFFFAOYSA-K 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 229940114079 arachidonic acid Drugs 0.000 description 1
- 235000021342 arachidonic acid Nutrition 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 150000004982 aromatic amines Chemical class 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 229940116226 behenic acid Drugs 0.000 description 1
- KIDIAQBVMKMQSF-UHFFFAOYSA-N benzoic acid;2,2-dimethylpropane-1,3-diol;prop-2-enoic acid Chemical compound OC(=O)C=C.OCC(C)(C)CO.OC(=O)C1=CC=CC=C1 KIDIAQBVMKMQSF-UHFFFAOYSA-N 0.000 description 1
- JGQFVRIQXUFPAH-UHFFFAOYSA-N beta-citronellol Natural products OCCC(C)CCCC(C)=C JGQFVRIQXUFPAH-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- IPHKNOWSJUHYSE-UHFFFAOYSA-N bis(oxiran-2-ylmethyl) 3-methylcyclohexane-1,2-dicarboxylate Chemical compound CC1CCCC(C(=O)OCC2OC2)C1C(=O)OCC1CO1 IPHKNOWSJUHYSE-UHFFFAOYSA-N 0.000 description 1
- XFUOBHWPTSIEOV-UHFFFAOYSA-N bis(oxiran-2-ylmethyl) cyclohexane-1,2-dicarboxylate Chemical compound C1CCCC(C(=O)OCC2OC2)C1C(=O)OCC1CO1 XFUOBHWPTSIEOV-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 235000000484 citronellol Nutrition 0.000 description 1
- 229920006026 co-polymeric resin Polymers 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 229930003836 cresol Natural products 0.000 description 1
- OZEHOHQZIRILDX-UHFFFAOYSA-N ctk1b7797 Chemical compound O=C1OC(=O)C2C1C1(C)CC2CC1 OZEHOHQZIRILDX-UHFFFAOYSA-N 0.000 description 1
- SPTHWAJJMLCAQF-UHFFFAOYSA-M ctk4f8481 Chemical compound [O-]O.CC(C)C1=CC=CC=C1C(C)C SPTHWAJJMLCAQF-UHFFFAOYSA-M 0.000 description 1
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 1
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 1
- 150000005690 diesters Chemical class 0.000 description 1
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 1
- XXJWXESWEXIICW-UHFFFAOYSA-N diethylene glycol monoethyl ether Chemical compound CCOCCOCCO XXJWXESWEXIICW-UHFFFAOYSA-N 0.000 description 1
- 229940075557 diethylene glycol monoethyl ether Drugs 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- XHWQYYPUYFYELO-UHFFFAOYSA-N ditridecyl phosphite Chemical compound CCCCCCCCCCCCCOP([O-])OCCCCCCCCCCCCC XHWQYYPUYFYELO-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 239000003759 ester based solvent Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 229940113087 geraniol Drugs 0.000 description 1
- VANNPISTIUFMLH-UHFFFAOYSA-N glutaric anhydride Chemical compound O=C1CCCC(=O)O1 VANNPISTIUFMLH-UHFFFAOYSA-N 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- WJRBRSLFGCUECM-UHFFFAOYSA-N hydantoin Chemical compound O=C1CNC(=O)N1 WJRBRSLFGCUECM-UHFFFAOYSA-N 0.000 description 1
- 229940091173 hydantoin Drugs 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 239000005453 ketone based solvent Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 229930007744 linalool Natural products 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 150000007974 melamines Chemical class 0.000 description 1
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- JAYXSROKFZAHRQ-UHFFFAOYSA-N n,n-bis(oxiran-2-ylmethyl)aniline Chemical compound C1OC1CN(C=1C=CC=CC=1)CC1CO1 JAYXSROKFZAHRQ-UHFFFAOYSA-N 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- NPFIXJIFUHTLRP-UHFFFAOYSA-N n-cyclohexyl-2-methylpropanamide Chemical compound CC(C)C(=O)NC1CCCCC1 NPFIXJIFUHTLRP-UHFFFAOYSA-N 0.000 description 1
- 125000001624 naphthyl group Chemical group 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- 239000004843 novolac epoxy resin Substances 0.000 description 1
- 229960002446 octanoic acid Drugs 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 125000000466 oxiranyl group Chemical group 0.000 description 1
- URLKBWYHVLBVBO-UHFFFAOYSA-N p-dimethylbenzene Natural products CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- NAKOELLGRBLZOF-UHFFFAOYSA-N phenoxybenzene;pyrrole-2,5-dione Chemical compound O=C1NC(=O)C=C1.O=C1NC(=O)C=C1.C=1C=CC=CC=1OC1=CC=CC=C1 NAKOELLGRBLZOF-UHFFFAOYSA-N 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- RINCXYDBBGOEEQ-UHFFFAOYSA-N succinic anhydride Chemical group O=C1CCC(=O)O1 RINCXYDBBGOEEQ-UHFFFAOYSA-N 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- 229940116411 terpineol Drugs 0.000 description 1
- NMOALOSNPWTWRH-UHFFFAOYSA-N tert-butyl 7,7-dimethyloctaneperoxoate Chemical compound CC(C)(C)CCCCCC(=O)OOC(C)(C)C NMOALOSNPWTWRH-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 150000004992 toluidines Chemical class 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- 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
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L101/00—Compositions of unspecified macromolecular compounds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/50—Assembly of semiconductor devices using processes or apparatus not provided for in a single one of the subgroups H01L21/06 - H01L21/326, e.g. sealing of a cap to a base of a container
- H01L21/52—Mounting semiconductor bodies in containers
Landscapes
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Conductive Materials (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Die Bonding (AREA)
Description
本発明は、回路パターンの形成又はダイボンディング剤として有用な導電性組成物に関する。 The present invention relates to a conductive composition useful as a circuit pattern forming or die bonding agent.
携帯電話、パソコン、車載用電子部品などの分野で、回路パターンの形成や、IC、LSIなどの半導体素子とリードフレーム又は基板とを接合させるボンディング材料として、導電性組成物は使用されている。例えば、導電回路は、スクリーン印刷などによって、導電性組成物を基板上に塗布した後、熱硬化させることによって形成することができる。また、半導体素子とリードフレーム又は基板との接合は、リードフレーム又は基板の所定の部位に、導電性組成物を塗布した後、半導体素子をマウントし、熱硬化させることによって行うことができる。 In the fields of mobile phones, personal computers, in-vehicle electronic components, etc., conductive compositions are used as bonding materials for forming circuit patterns and bonding semiconductor elements such as ICs and LSIs to lead frames or substrates. For example, the conductive circuit can be formed by applying a conductive composition on a substrate by screen printing or the like and then thermally curing the conductive composition. Further, the bonding between the semiconductor element and the lead frame or the substrate can be performed by applying a conductive composition to a predetermined part of the lead frame or the substrate, mounting the semiconductor element, and thermally curing the semiconductor element.
一般に、導電性組成物は、銀粒子を配合することにより、導電性を発現させるものであるが、近年では、より安価なニッケル粒子や銀メッキ粒子を配合しつつ、かつ接着性や導電性の点で良好な硬化膜をもたらしうる導電性組成物が求められている。この要望に応えるべく、銀被覆粒子を含む導電性組成物が提案されている(特許文献1〜3参照)。 In general, a conductive composition is one that develops conductivity by blending silver particles, but in recent years, while blending cheaper nickel particles and silver plating particles, it also has adhesiveness and conductivity. In view of the above, there is a demand for an electrically conductive composition that can provide a cured film. In order to meet this demand, conductive compositions containing silver-coated particles have been proposed (see Patent Documents 1 to 3).
しかしながら、特許文献1の導電性組成物は、チタン及び/又はジルコニウムを含む有機金属錯体の使用が必須であり、コストダウンに十分、寄与しうるものではない。また、特許文献2及び3の導電性組成物は、分子量3000以上のポリエステル樹脂/又は変性ポリエステル樹脂といった熱可塑性樹脂を用いており、高温時(260℃)に軟化するため、接着強度が大きく低下し、吸湿後リフローにおける信頼性を保つことが難しくなる。さらに、平均粒径/厚さが2以上とリン片化度の高いフレーク粉を用いているため、チップと基板の接合に使用した場合、フレークが何枚も重なって上下導通が得られ、ひいては接触抵抗が高く、また、銀と違ってコア材の周辺を電気が通るため導通経路が長く、総じて上下導通の抵抗値が高くなってしまう。さらに、平均粒径/厚さが2以上とリン片化度の高いフレーク粉は比表面積が大きく、均一に銀で被覆するには銀のコート率を上げる必要があり、効果的なコストダウンが見込めなくなってしまう。 However, the conductive composition of Patent Document 1 requires the use of an organometallic complex containing titanium and / or zirconium, and cannot sufficiently contribute to cost reduction. In addition, the conductive compositions of Patent Documents 2 and 3 use a thermoplastic resin such as a polyester resin having a molecular weight of 3000 or more and / or a modified polyester resin, and soften at a high temperature (260 ° C.). In addition, it becomes difficult to maintain reliability in reflow after moisture absorption. Furthermore, since flake powder having an average particle size / thickness of 2 or more and a high degree of flaming is used, when used for bonding a chip and a substrate, a plurality of flakes overlap to obtain vertical conduction, and consequently The contact resistance is high, and unlike silver, electricity passes through the periphery of the core material, so the conduction path is long, and the resistance value of vertical conduction is generally high. Furthermore, flake powder having a high average particle size / thickness of 2 or more and having a high degree of flaming has a large specific surface area. In order to uniformly coat with silver, it is necessary to increase the coating rate of silver, thus reducing the cost effectively. It will not be expected.
本発明は上記事情に鑑みてなされたものであって、コストダウンと、良好な接着性及び導電性の発現との両方を満足させる導電性組成物を提供することを目的とする。 This invention is made | formed in view of the said situation, Comprising: It aims at providing the electrically conductive composition which satisfies both cost reduction and favorable adhesiveness and expression of electroconductivity.
本発明者らは、鋭意研究を進めたところ、導電性組成物に、銀被覆セラミック粒子及び銀被覆ガラス粒子及び銀被覆アルミニウム粒子からなる群より選択され、かつ特定の形状を有するフレーク状の銀被覆粒子を配合することによって、接着性及び導電性の点で十分な硬化膜がもたらされることを発見し、本発明を完成させた。本発明では、相対的に安価な銀被覆粒子を使用しているため、コストダウンも同時に図ることができる。 As a result of extensive research, the present inventors have determined that the conductive composition is a flaky silver having a specific shape selected from the group consisting of silver-coated ceramic particles, silver-coated glass particles, and silver-coated aluminum particles. It has been discovered that blending the coated particles results in a cured film that is sufficient in terms of adhesion and conductivity, thus completing the present invention. In the present invention, since relatively inexpensive silver-coated particles are used, the cost can be reduced at the same time.
すなわち、本発明は、
(A)銀被覆セラミック粒子、銀被覆ガラス粒子及び銀被覆アルミニウム粒子からなる群より選択され、かつ、レーザ光散乱法により測定した体積平均粒子径D50が、1〜10μmであり、走査型電子顕微鏡観察により測定した平均厚みTが、0.3〜10μmであり、アスペクト比T/D50が、0.3〜1.0であるフレーク状の銀被覆粒子
(B)熱硬化性樹脂、並びに
(C)硬化剤
を含む、導電性組成物に関する。That is, the present invention
(A) A volume average particle diameter D50 selected from the group consisting of silver-coated ceramic particles, silver-coated glass particles and silver-coated aluminum particles and measured by a laser light scattering method is 1 to 10 μm, and a scanning electron microscope Flake-shaped silver-coated particles having an average thickness T measured by observation of 0.3 to 10 μm and an aspect ratio T / D50 of 0.3 to 1.0 (B) thermosetting resin, and (C ) It relates to a conductive composition containing a curing agent.
本発明によれば、コストダウンと、良好な接着性及び導電性の発現との両方を満足させる導電性組成物が提供される。 ADVANTAGE OF THE INVENTION According to this invention, the electrically conductive composition which satisfies both cost reduction and favorable adhesiveness and expression of electroconductivity is provided.
本発明の導電性組成物は、(A)銀被覆セラミック粒子、銀被覆ガラス粒子及び銀被覆アルミニウム粒子からなる群より選択され、かつ、レーザ光散乱法により測定した体積平均粒子径D50が、1〜10μmであり、走査型電子顕微鏡観察により測定した平均厚みTが、0.3〜10μmであり、アスペクト比T/D50が、0.3〜1.0であるフレーク状の銀被覆粒子を含む。(A)成分のフレーク状の銀被覆粒子は、単独でも、複数種を併用してもよい。 The conductive composition of the present invention is selected from the group consisting of (A) silver-coated ceramic particles, silver-coated glass particles, and silver-coated aluminum particles, and has a volume average particle diameter D50 measured by a laser light scattering method of 1 The average thickness T measured by observation with a scanning electron microscope is 0.3 to 10 μm, and the flaky silver-coated particles having an aspect ratio T / D50 of 0.3 to 1.0 are included. . The flaky silver-coated particles of the component (A) may be used alone or in combination of two or more.
(A)成分のフレーク状の銀被覆粒子のコアは、セラミック、ガラス又はアルミニウムからなる。セラミックとしては、アルミナ、炭化ケイ素、窒化ケイ素、チタン酸バリウム、窒化ホウ素、フェライト、ステアタイト、酸化亜鉛、ジルコニアが挙げられ、入手の自由度、粒径や形状のコントロールの自由度、コストの観点から、特にアルミナ、が好ましい。 The core of the flaky silver-coated particles (A) is made of ceramic, glass or aluminum. Examples of ceramics include alumina, silicon carbide, silicon nitride, barium titanate, boron nitride, ferrite, steatite, zinc oxide, and zirconia. Freedom to obtain, freedom to control particle size and shape, and cost In particular, alumina is preferable.
(A)成分のフレーク状の銀被覆粒子は、レーザ光散乱法により測定した体積平均粒子径D50が、1〜10μmのものである。D50がこの範囲にあると、導電性組成物の作業性がよく、例えば、内径100〜200μmのノズルを使用したディスペンスにおいても、ノズルの詰まりを起こす事無く、連続して吐出することが可能となる。また、半導体チップと基板との接合では、導電性組成物の膜厚が20〜30μmに設定されることが多いが、(A)成分の存在により膜厚が厚くなってチップの傾きを発生させることを回避することもできる。D50は、銀被覆粒子をミクロスパテラで2杯、300mlビーカーに採り、0.5%スルホコハク酸ナトリウムのジオクチルエステル溶液を50ml入れ、超音波ホモジナイザーで10分間分散し、光散乱解析タイプ粒度分布測定装置(コールターLS230(ベックマンコールター製)で測定することができる。50%の累積径の平均値をD50とする。 The flaky silver-coated particles (A) have a volume average particle diameter D50 measured by a laser light scattering method of 1 to 10 μm. When D50 is in this range, the workability of the conductive composition is good. For example, even in dispensing using a nozzle having an inner diameter of 100 to 200 μm, it is possible to discharge continuously without causing clogging of the nozzle. Become. Further, in the bonding between the semiconductor chip and the substrate, the film thickness of the conductive composition is often set to 20 to 30 μm, but the film thickness is increased due to the presence of the component (A), and the tilt of the chip is generated. This can also be avoided. D50 is a glass-coated particle with 2 cups of microspatella, taken in a 300 ml beaker, put 50 ml of 0.5% sodium sulfosuccinate dioctyl ester solution, and dispersed with an ultrasonic homogenizer for 10 minutes. (A Coulter LS230 (manufactured by Beckman Coulter)) The average value of 50% cumulative diameter is D50.
(A)成分のフレーク状の銀被覆粒子のD50は、1〜10μmであり、好ましくは3〜8μmである。 (A) D50 of the flaky silver coating particle of a component is 1-10 micrometers, Preferably it is 3-8 micrometers.
(A)成分のフレーク状の銀被覆粒子は、走査型電子顕微鏡観察により測定した平均厚みTが、0.3〜10μmのものである。Tがこの範囲にあると、導電性組成物の作業性がよく、また、半導体チップと基板との接合で、(A)成分によってチップが傾くといった不都合が生じることも回避できる。平均厚みは、銀被覆粒子2gとエポキシ樹脂(Epoxy Resin20−8130−032(BUEHLER製))5gとエポキシ樹脂硬化剤(EPOXY HARDENER20−8132−008(BUEHLER製))1gを直径25mmのクリアカップに計り取り、ヘラを用いてよく混合し、室温で12時間静置後、硬化した樹脂を、クリアカップより取り出し、ミクロトームで面出し加工を行い、カーボン蒸着後、電界放射型走査型電子顕微鏡(JEOL製JSM−7500F)で1000倍又は2000倍の倍率で写真を撮影し、中心を通る最短辺を銀被覆の厚みとして測定し、測定個数50個の平均値を平均厚みTとする。 The flaky silver-coated particles (A) have an average thickness T measured by observation with a scanning electron microscope of 0.3 to 10 μm. When T is in this range, the workability of the conductive composition is good, and it is also possible to avoid the inconvenience that the chip is inclined due to the component (A) in joining the semiconductor chip and the substrate. The average thickness is 2 g of silver coated particles, 5 g of epoxy resin (Epoxy Resin 20-8130-032 (manufactured by BUEHLER)) and 1 g of epoxy resin curing agent (EPOXY HARDENER 20-8132-008 (manufactured by BUEHLER)) in a 25 mm diameter clear cup. Take out and mix well using a spatula, let stand at room temperature for 12 hours, then remove the cured resin from the clear cup, perform surface processing with a microtome, and after carbon deposition, a field emission scanning electron microscope (manufactured by JEOL) JSM-7500F) is photographed at a magnification of 1000 times or 2000 times, the shortest side passing through the center is measured as the thickness of the silver coating, and the average value of 50 measured numbers is defined as the average thickness T.
(A)成分のフレーク状の銀被覆粒子のTは、0.3〜10μmであり、好ましくは1〜8μmである。 T of the (A) component flaky silver-coated particles is 0.3 to 10 μm, preferably 1 to 8 μm.
(A)成分のフレーク状の銀被覆粒子は、アスペクト比T/D50が、0.3〜1.0のものである。アスペクト比T/D50がこの範囲にあると、半導体チップと基板を接合した場合、リン片化度の高いもの(すなわち、T/D50が0.3未満のもの)よりも、上下導通をとるための銀被覆粒子の存在数が少なく済み、それにより銀被覆粒子同士の接触抵抗を減らすことが可能になる。また、リン片化度の高いものは、コア材料の周辺を電気がとおるので導通経路が長いのに対し、本発明の銀被覆微粒子は導通経路が短く済むため、上下導通の抵抗値を下げることが可能となる。さらに、リン片化度の高いものよりも、シェアがかかった時の流動性の向上が見込め、ディスペンスの吐出性の向上といった作業性の向上も見込める。T/D50は、0.3〜1.0が好ましく、より好ましくは0.4〜1.0である。 The flaky silver-coated particles (A) have an aspect ratio T / D50 of 0.3 to 1.0. When the aspect ratio T / D50 is within this range, when the semiconductor chip and the substrate are joined, the semiconductor chip and the substrate are more conductive than the one having a higher degree of fragmentation (that is, the T / D50 is less than 0.3). The number of silver-coated particles can be reduced, thereby making it possible to reduce the contact resistance between the silver-coated particles. In addition, the one with a high degree of fragmentation has a long conduction path because electricity passes around the core material, whereas the silver-coated fine particles of the present invention require a short conduction path, thereby reducing the resistance value of vertical conduction. Is possible. In addition, it is expected to improve fluidity when the market share is higher than those with a high degree of fragmentation, and to improve workability such as improved dispensing performance. T / D50 is preferably 0.3 to 1.0, more preferably 0.4 to 1.0.
(A)成分のフレーク状の銀被覆粒子は、作業性(特に、ディスペンス時のノズル詰まりの抑制)及び半導体チップと基板との接合においてチップが傾くことを防止する観点から、最大粒径が40μm以下であることが好ましい。最大粒径は、光散乱解析タイプ粒度分布測定装置で測定した値とする。最大粒径は、より好ましくは、35μm以下であり、30μm以下がさらに好ましい。 The flaky silver-coated particles of component (A) have a maximum particle size of 40 μm from the viewpoint of workability (especially suppression of nozzle clogging during dispensing) and prevention of tip tilting in bonding between the semiconductor chip and the substrate. The following is preferable. The maximum particle size is a value measured with a light scattering analysis type particle size distribution measuring device. The maximum particle size is more preferably 35 μm or less, and further preferably 30 μm or less.
(A)成分のフレーク状の銀被覆粒子は、コア材への銀被覆率と導電性の観点から、銀被覆層が銀被覆粒子の全重量のうち、10〜60質量%が好ましく、より好ましくは20〜50質量%であり、さらに好ましくは20〜40質量%である。銀被覆層の重量は、銀被覆粒子の重量と、銀被覆層を硝酸に溶解させて、銀を除き、測定したコア材の重量から算出することができる。 The flaky silver-coated particles of the component (A) are preferably 10 to 60% by mass of the total weight of the silver-coated particles, more preferably from the viewpoint of silver coverage to the core material and conductivity. Is 20-50 mass%, More preferably, it is 20-40 mass%. The weight of the silver coating layer can be calculated from the weight of the silver coating particles and the core material measured by dissolving the silver coating layer in nitric acid and removing silver.
(A)成分のフレーク状の銀被覆粒子は、銀被覆層が均一に備わっていることが好ましく、銀被覆層が厚くなって、粒子全体の比重、ひいては導電性組成物の比重が大きくなり、導電性組成物を同一重量で塗布した時の体積を減少させることによる、効率の低下を回避し、かつ安定した導電性を得る観点から、銀被覆層の厚さは、好ましくは50〜300nmである。銀被覆層の厚みは、より好ましくは50〜200nmであり、さらに好ましくは80〜200nmであり、特に好ましくは80〜150nmである。銀被覆層の厚みは平均厚みTと同様なサンプルを作製し、電界放射型走査型電子顕微鏡(JEOL製JSM−7500F)で10000倍〜30000倍の倍率で測定することができる。 The flaky silver-coated particles of the component (A) are preferably provided with a uniform silver coating layer, the silver coating layer is thick, and the specific gravity of the entire particle, and hence the specific gravity of the conductive composition, is increased. The thickness of the silver coating layer is preferably 50 to 300 nm from the viewpoint of avoiding a decrease in efficiency by reducing the volume when the conductive composition is applied with the same weight and obtaining stable conductivity. is there. The thickness of the silver coating layer is more preferably 50 to 200 nm, still more preferably 80 to 200 nm, and particularly preferably 80 to 150 nm. The thickness of the silver coating layer can be measured by preparing a sample similar to the average thickness T and using a field emission scanning electron microscope (JSM-7500F manufactured by JEOL) at a magnification of 10,000 to 30,000 times.
(A)成分のフレーク状の銀被覆粒子は、コアとなるセラミック、ガラス、アルミニウム粒子に、無電解めっき、スパッリング、蒸着などの方法により銀を被覆させることにより得られる。 The flaky silver-coated particles of the component (A) can be obtained by coating the ceramic, glass, and aluminum particles serving as the core with silver by a method such as electroless plating, sparring, or vapor deposition.
(A)成分のフレーク状の銀被覆粒子は、ペースト化したときの安定性の点から、脂肪酸又はその塩、あるいはカップリング剤で表面処理されたものであることが好ましい。 The flaky silver-coated particles (A) are preferably those that have been surface-treated with a fatty acid or a salt thereof, or a coupling agent from the viewpoint of stability when formed into a paste.
脂肪酸としては、プロピオン酸、カプリル酸、ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸、ベヘン酸、アクリル酸、オレイン酸、リノール酸、アラキドン酸などが挙げられ、エポキシ樹脂、フェノール樹脂、アクリレート樹脂、イソシアネート樹脂、マレイミド樹脂との相溶性、濡れ性、樹脂への反応性の観点から、好ましくはオレイン酸、ステアリン酸である。脂肪酸塩としては、上記脂肪酸のリチウム、ナトリウム、カリウム、バリウム、マグネシウム、カルシウム、アルミニウム、鉄、コバルト、マンガン、鉛、亜鉛、スズ、ストロンチウム、ジルコニウム、銀、銅などの金属塩が挙げられ、エポキシ樹脂、フェノール樹脂、アクリレート樹脂、イソシアネート樹脂、マレイミド樹脂との相溶性、濡れ性、樹脂への反応性の観点から、好ましくはナトリウム塩である。 Examples of fatty acids include propionic acid, caprylic acid, lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, acrylic acid, oleic acid, linoleic acid, arachidonic acid, epoxy resin, phenolic resin, acrylate resin, From the viewpoint of compatibility with isocyanate resin and maleimide resin, wettability, and reactivity to resin, oleic acid and stearic acid are preferred. Examples of fatty acid salts include metal salts of the above fatty acids such as lithium, sodium, potassium, barium, magnesium, calcium, aluminum, iron, cobalt, manganese, lead, zinc, tin, strontium, zirconium, silver, copper, and epoxy. From the viewpoint of compatibility with resins, phenolic resins, acrylate resins, isocyanate resins, and maleimide resins, wettability, and reactivity to resins, sodium salts are preferred.
脂肪酸又は脂肪酸塩による表面処理方法としては、場合により加温したアルコールに脂肪酸又は脂肪酸塩を溶解し、そこに銀被覆粒子を添加して、一定時間撹拌を行なうことで処理する方法が挙げられる。 Examples of the surface treatment method using a fatty acid or a fatty acid salt include a method of dissolving a fatty acid or a fatty acid salt in an optionally heated alcohol, adding silver-coated particles thereto, and stirring the mixture for a certain period of time.
カップリング剤としては、シランカップリング剤、チタネート系カップリング剤、アルミニウム系カップリング剤などが挙げられ、エポキシ樹脂、フェノール樹脂、アクリレート樹脂、イソシアネート樹脂、マレイミド樹脂との相溶性、濡れ性、樹脂への反応性の観点から、好ましくはシランカップリング剤、チタネート系カップリング剤である。 Examples of coupling agents include silane coupling agents, titanate coupling agents, aluminum coupling agents, etc., compatibility with epoxy resins, phenol resins, acrylate resins, isocyanate resins, maleimide resins, wettability, resins From the viewpoint of reactivity to silane, a silane coupling agent and a titanate coupling agent are preferable.
カップリング剤による表面処理方法としては、銀被覆粒子をアトライターにて撹拌しているところに噴霧して処理する方法、アルコールにカップリング剤を溶解させ、そこに銀被覆粒子を添加して撹拌を行ない処理する方法が挙げられる。 As a surface treatment method using a coupling agent, a method in which silver-coated particles are sprayed onto an agitator where the particles are being agitated, the coupling agent is dissolved in alcohol, and silver-coated particles are added thereto and stirred. There is a method of performing and processing.
本発明の導電性組成物は、(B)熱硬化性樹脂を含む。(B)成分の熱硬化性樹脂は、特に限定されず、例えば、エポキシ樹脂、アクリル樹脂、シリコーン樹脂、ウレタン樹脂、マレイミド樹脂などが挙げられる。熱硬化性樹脂は、単独でも、複数種を併用してもよい。 The conductive composition of the present invention contains (B) a thermosetting resin. (B) The thermosetting resin of a component is not specifically limited, For example, an epoxy resin, an acrylic resin, a silicone resin, a urethane resin, a maleimide resin etc. are mentioned. A thermosetting resin may be individual or may use multiple types together.
(B)成分の熱硬化性樹脂は、ダイボンディング剤に求められる接着性、硬化性、耐熱性の点から、エポキシ樹脂が好ましい。エポキシ樹脂は、常温で液状であることが好ましいが、常温で固体のものであっても、他の液状のエポキシ樹脂又は希釈剤により希釈し、液状で用いることができる。エポキシ樹脂としては、具体的には、ビスフェノールA型エポキシ樹脂、臭素化ビスフェノールA型エポキシ樹脂、ビスフェノールF型エポキシ樹脂、ビフェニル型エポキシ樹脂、ノボラック型エポキシ樹脂、脂環式エポキシ樹脂、ナフタレン型エポキシ樹脂、エーテル系又はポリエーテル系エポキシ樹脂(例えば、ポリオキシプロピレンビスフェノールAジグリシジルエーテルのようなポリオキシプロピレン変性エポキシ樹脂)、オキシラン環含有ポリブタジエン、ダイマー酸のエピクロルヒドリンによるジグリシジルエステル化変性物、エポキシ基を有するポリブタジエン化合物、シリコーンエポキシコポリマー樹脂、アミノフェノール型エポキシ樹脂(例えば、N,N−ビス(2,3−エポキシプロピル)−4−(2,3−エポキシプロピルオキシ)アニリン)などが例示される。 The thermosetting resin as component (B) is preferably an epoxy resin from the viewpoint of adhesiveness, curability and heat resistance required for the die bonding agent. The epoxy resin is preferably liquid at normal temperature, but even if it is solid at normal temperature, it can be diluted with another liquid epoxy resin or diluent and used in liquid form. Specific examples of epoxy resins include bisphenol A type epoxy resins, brominated bisphenol A type epoxy resins, bisphenol F type epoxy resins, biphenyl type epoxy resins, novolac type epoxy resins, alicyclic epoxy resins, and naphthalene type epoxy resins. , Ether-based or polyether-based epoxy resins (for example, polyoxypropylene-modified epoxy resins such as polyoxypropylene bisphenol A diglycidyl ether), oxirane ring-containing polybutadiene, diglycidyl esterified modified products of dimer acid with epichlorohydrin, epoxy groups A polybutadiene compound having a molecular weight, a silicone epoxy copolymer resin, an aminophenol type epoxy resin (for example, N, N-bis (2,3-epoxypropyl) -4- (2,3-epoxypropylene) Piruokishi) aniline), and the like.
特に、液状であるエポキシ樹脂としては、ビスフェノールA型エポキシ樹脂の平均分子量が約400以下のもの;p−グリシジルオキシフェニルジメチルトリスビスフェノールAジグリシジルエーテルのような分岐状多官能ビスフェノールA型エポキシ樹脂;ビスフェノールF型エポキシ樹脂;フェノールノボラック型エポキシ樹脂の平均分子量が約570以下のもの;ビニル(3,4−シクロヘキセン)ジオキシド、3,4−エポキシシクロヘキシルカルボン酸(3,4−エポキシシクロヘキシル)メチル、アジピン酸ビス(3,4−エポキシ−6−メチルシクロヘキシルメチル)、2−(3,4−エポキシシクロヘキシル)5,1−スピロ(3,4−エポキシシクロヘキシル)−m−ジオキサンのような脂環式エポキシ樹脂;3,3’,5,5’−テトラメチル−4,4’−ジグリシジルオキシビフェニルのようなビフェニル型エポキシ樹脂;ヘキサヒドロフタル酸ジグリシジル、3−メチルヘキサヒドロフタル酸ジグリシジル、ヘキサヒドロテレフタル酸ジグリシジルネオデカン酸グリシジルエステルのようなグリシジルエステル型エポキシ樹脂;ジグリシジルアニリン、ジグリシジルトルイジン、トリグリシジル−p−アミノフェノール、テトラグリシジル−m−キシリレンジアミン、テトラグリシジルビス(アミノメチル)シクロヘキサンのようなグリシジルアミン型エポキシ樹脂;並びに1,3−ジグリシジル−5−メチル−5−エチルヒダントインのようなヒダントイン型エポキシ樹脂;ナフタレン環含有エポキシ樹脂が例示される。また、1,3−ビス(3−グリシドキシプロピル)−1,1,3,3−テトラメチルジシロキサンのようなシリコーン骨格をもつエポキシ樹脂も使用することができる。さらに、(ポリ)エチレングリコールジグリシジルエーテル、(ポリ)プロピレングリコールジグリシジルエーテル、ブタンジオールグリシジルエーテル、ネオペンチルグリコールジグリシジルエーテル、1,4−シクロへキサンジメタノールジグリシジルエーテル、1,6−ヘキサンジオールジグリシジルエーテル、p−tert―ブチルフェニルグリシジルエーテル、ジシクロペンタジエンジメタノールジグリシジルエーテル、トリメチロールプロパンのグリシジルエーテル、ポリテトラメチレンエーテルグリコールのジグリシジルエーテル、ダイマー酸ジグリシジルエーテルとポリプロビレングリコールのジグリシジルエーテル、グリセリンジグリシジルエーテル、ネオペンチルグリコールジグリシジルエーテル、1,4−フェニルジメタノールジグリシジルエーテルのようなジエポキシド化合物;トリメチロールプロパントリグリシジルエーテル、グリセリントリグリシジルエーテルのようなトリエポキシド化合物なども例示される。 In particular, the liquid epoxy resin has a bisphenol A type epoxy resin having an average molecular weight of about 400 or less; a branched polyfunctional bisphenol A type epoxy resin such as p-glycidyloxyphenyldimethyltrisbisphenol A diglycidyl ether; Bisphenol F type epoxy resin; phenol novolak type epoxy resin having an average molecular weight of about 570 or less; vinyl (3,4-cyclohexene) dioxide, 3,4-epoxycyclohexylcarboxylic acid (3,4-epoxycyclohexyl) methyl, adipine Cycloaliphatic epoxies such as bis (3,4-epoxy-6-methylcyclohexylmethyl) acid, 2- (3,4-epoxycyclohexyl) 5,1-spiro (3,4-epoxycyclohexyl) -m-dioxane Resin; 3, 3 ', Biphenyl type epoxy resin such as 5,5'-tetramethyl-4,4'-diglycidyloxybiphenyl; diglycidyl hexahydrophthalate, diglycidyl 3-methylhexahydrophthalate, diglycidyl neodecanoate glycidyl ester of hexahydroterephthalate Glycidyl ester type epoxy resins such as: diglycidyl aniline, diglycidyl toluidine, triglycidyl-p-aminophenol, tetraglycidyl-m-xylylenediamine, tetraglycidyl bis (aminomethyl) cyclohexane; And hydantoin type epoxy resins such as 1,3-diglycidyl-5-methyl-5-ethylhydantoin; naphthalene ring-containing epoxy resins. Moreover, an epoxy resin having a silicone skeleton such as 1,3-bis (3-glycidoxypropyl) -1,1,3,3-tetramethyldisiloxane can also be used. Furthermore, (poly) ethylene glycol diglycidyl ether, (poly) propylene glycol diglycidyl ether, butanediol glycidyl ether, neopentyl glycol diglycidyl ether, 1,4-cyclohexane dimethanol diglycidyl ether, 1,6-hexane Diol diglycidyl ether, p-tert-butylphenyl glycidyl ether, dicyclopentadiene dimethanol diglycidyl ether, glycidyl ether of trimethylolpropane, diglycidyl ether of polytetramethylene ether glycol, diglycidyl ether of dimer acid and polypropylene glycol Glycidyl ether, glycerin diglycidyl ether, neopentyl glycol diglycidyl ether, 1,4-phenyldi Diepoxide compounds such as ethanol diglycidyl ether; trimethylolpropane triglycidyl ether, also like triepoxide compounds such as glycerin triglycidyl ether and the like.
エポキシ樹脂は、常温で固体ないし超高粘性のエポキシ樹脂を併用することも可能であり、そのようなエポキシ樹脂として、高分子量のビスフェノールA型エポキシ樹脂、ノボラックエポキシ樹脂、テトラブロモビスフェノールA型エポキシ樹脂、ジシクロペンタジエン型エポキシ樹脂、イソシアネート変性エポキシ樹脂、フルオレン型エポキシ樹脂、ビフェニルアラルキルエポキシ樹脂などが例示される。これらは、常温で液体であるエポキシ樹脂及び/又は希釈剤と組み合わせて、流動性を調節して使用することができる。 The epoxy resin can be used in combination with a solid or ultra-high viscosity epoxy resin at room temperature, and as such an epoxy resin, a high molecular weight bisphenol A type epoxy resin, a novolac epoxy resin, a tetrabromobisphenol A type epoxy resin. And dicyclopentadiene type epoxy resin, isocyanate-modified epoxy resin, fluorene type epoxy resin, biphenyl aralkyl epoxy resin and the like. These can be used in combination with an epoxy resin and / or a diluent that is liquid at room temperature to adjust fluidity.
常温で固体ないし超高粘性であるエポキシ樹脂を用いる場合、低粘度のエポキシ樹脂、例えば、(ポリ)エチレングリコールジグリシジルエーテル、(ポリ)プロピレングリコールジグリシジルエーテル、ブタンジオールグリシジルエーテル、ネオペンチルグリコールジグリシジルエーテル、1,4−シクロへキサンジメタノールジグリシジルエーテル、1,6−ヘキサンジオールジグリシジルエーテル、p−tert―ブチルフェニルグリシジルエーテル、ジシクロペンタジエンジメタノールジグリシジルエーテル、トリメチロールプロパンのグリシジルエーテル、ポリテトラメチレンエーテルグリコールのジグリシジルエーテル、ダイマー酸ジグリシジルエーテルとポリプロビレングリコールのジグリシジルエーテル、グリセリンジグリシジルエーテル、ネオペンチルグリコールジグリシジルエーテル、1,4−フェニルジメタノールジグリシジルエーテルのようなジエポキシド化合物;トリメチロールプロパントリグリシジルエーテル、グリセリントリグリシジルエーテルのようなトリエポキシド化合物などと組み合わせることが好ましい。 When using an epoxy resin that is solid or ultra-highly viscous at room temperature, low-viscosity epoxy resins such as (poly) ethylene glycol diglycidyl ether, (poly) propylene glycol diglycidyl ether, butanediol glycidyl ether, neopentyl glycol diester Glycidyl ether, 1,4-cyclohexanedimethanol diglycidyl ether, 1,6-hexanediol diglycidyl ether, p-tert-butylphenylglycidyl ether, dicyclopentadiene dimethanol diglycidyl ether, glycidyl ether of trimethylolpropane Diglycidyl ether of polytetramethylene ether glycol, diglycidyl ether of dimer acid and diglycidyl ether of polypropylene glycol, glycerin diglycol Jill ether, neopentyl glycol diglycidyl ether, a diepoxide compound such as 1,4-phenyl-dimethanol diglycidyl ether; trimethylolpropane triglycidyl ether, be combined with such triepoxide compounds such as glycerin triglycidyl ether preferable.
アクリル樹脂としては、ネオペンチルグリコールジメタクリレート、1,6−ヘキサンジオールジメタクリレート、1,9−ノナンジオールジメタクリレート、1,10−デカンジオールジメタクリレート、ジメチロール−トリシクロデカンジメタクリレート、トリメチロールプロパントリメタクリレート、2−ヒドロキシ−3−アクリロイルオキシプロピルメタクリレート、ヒドロキシピバリン酸ネオペンチルグリコールジメタクリレート、2−メタクリロイルオキシエチルリン酸エステル、2−ヒドロキシエチルメタクリレート、2−ヒドロキシプロピルメタクリレート、2−ヒドロキシブチルメタクリレート、2−メタクリロイルオキシエチル−コハク酸、グリセリンジメタクリレート、2−メタクリロイルオキシエチル−フタル酸、γ−ブチロラクトンメタクリレート、2−メチル−2−アダマンチルメタクリレート、2−エチル−2−アダマンチルメタクリレート、エトシキ化シクロヘキサンジメタノールジメタクリレート又はそれらのアクリレート、1,4−シクロヘキサンジメタノールモノアクリレート、メトキシジプロピレングリコールアクリレート、ネオペンチルグリコールアクリル酸安息香酸エステル、ビスフェノールAのプロピレンオキサイド変性ジアクリレート、ペンタエリスリトールトリアクリレートなどが挙げられる。 Examples of acrylic resins include neopentyl glycol dimethacrylate, 1,6-hexanediol dimethacrylate, 1,9-nonanediol dimethacrylate, 1,10-decanediol dimethacrylate, dimethylol-tricyclodecane dimethacrylate, trimethylolpropane triacrylate. Methacrylate, 2-hydroxy-3-acryloyloxypropyl methacrylate, hydroxypivalate neopentyl glycol dimethacrylate, 2-methacryloyloxyethyl phosphate ester, 2-hydroxyethyl methacrylate, 2-hydroxypropyl methacrylate, 2-hydroxybutyl methacrylate, 2 -Methacryloyloxyethyl-succinic acid, glycerin dimethacrylate, 2-methacryloyloxyethyl-phthalic acid, -Butyrolactone methacrylate, 2-methyl-2-adamantyl methacrylate, 2-ethyl-2-adamantyl methacrylate, ethoxylated cyclohexanedimethanol dimethacrylate or acrylates thereof, 1,4-cyclohexanedimethanol monoacrylate, methoxydipropylene glycol acrylate, Neopentyl glycol acrylic acid benzoate, propylene oxide modified diacrylate of bisphenol A, pentaerythritol triacrylate and the like.
シリコーン樹脂としては、エポキシ変性ポリシロキサン、脂環式エポキシ変性ポリシロキサン、カルビノール変性ポリシロキサン、カルボキシル変性ポリシロキサン、モノアミン変性ポリシロキサン、ジアミン変性ポリシロキサン、ハイドロジェン変性ポリシロキサン、メルカプト変性ポリシロキサン、メタクリル変性ポリシロキサン、ジオール変性ポリシロキサンが挙げられる。 Examples of silicone resins include epoxy-modified polysiloxane, alicyclic epoxy-modified polysiloxane, carbinol-modified polysiloxane, carboxyl-modified polysiloxane, monoamine-modified polysiloxane, diamine-modified polysiloxane, hydrogen-modified polysiloxane, mercapto-modified polysiloxane, Examples include methacryl-modified polysiloxane and diol-modified polysiloxane.
ウレタン樹脂としては、イソシアネート樹脂、イソシアネート基をεカプロラクタムなどでブロックしたイソシアネート樹脂、エポキシ変性ウレタン樹脂、メタクリレート変性ウレタン樹脂、アクリレート変性ウレタン樹脂が挙げられる。
マレイミド樹脂としては、ビスマレイミド樹脂(4,4’−ジフェニルメタンビスマレイミド、m−フェニレンビスマレイミド、ビスフェノールA型ジフェニルエーテルビスマレイミド、3,3’−ジメチル−5,5’−ジエチル4,4’−ジフェニルメタンビスマレイミド、4−メチル−1,3−フェニレンビスマレイミド、1,6−ビスマレイミド−(2,2,4−トリメチル)ヘキサン)、モノマレイミド樹脂(N−フェニルマレイミド、N−シクロヘキシルマレイミド、o−メチルフェニルマレイミド、p−ヒドロキシフェニルマレイミド、p−カルボキシフェニルマレイミド、N−ドデシルマレイミド)が挙げられる。Examples of the urethane resin include isocyanate resins, isocyanate resins whose isocyanate groups are blocked with ε-caprolactam, epoxy-modified urethane resins, methacrylate-modified urethane resins, and acrylate-modified urethane resins.
As the maleimide resin, bismaleimide resin (4,4′-diphenylmethane bismaleimide, m-phenylene bismaleimide, bisphenol A type diphenyl ether bismaleimide, 3,3′-dimethyl-5,5′-diethyl 4,4′-diphenylmethane is used. Bismaleimide, 4-methyl-1,3-phenylenebismaleimide, 1,6-bismaleimide- (2,2,4-trimethyl) hexane), monomaleimide resin (N-phenylmaleimide, N-cyclohexylmaleimide, o- Methylphenylmaleimide, p-hydroxyphenylmaleimide, p-carboxyphenylmaleimide, N-dodecylmaleimide).
本発明の導電性組成物は、(C)硬化剤を含む。硬化剤は、熱硬化性樹脂との組み合わせで、適宜、選択することができ、例えば、フェノール樹脂、アミン系化合物、酸無水物、過酸化物、金属錯体、アゾ化合物などが挙げられる。硬化剤は、単独でも、複数種を併用してもよい。 The conductive composition of the present invention contains (C) a curing agent. A hardening | curing agent can be suitably selected with a combination with a thermosetting resin, for example, a phenol resin, an amine compound, an acid anhydride, a peroxide, a metal complex, an azo compound etc. are mentioned. A hardening | curing agent may be individual or may use multiple types together.
フェノール樹脂としては、ビスフェノールF型フェノール樹脂、アリルフェノール樹脂、フェノールノボラック樹脂、クレゾールノボラック樹脂、ナフトール変性フェノール樹脂、ジシクロペンタジエン変性フェノール樹脂、p−キシレン変性フェノール樹脂などが挙げられる。 Examples of the phenol resin include bisphenol F type phenol resin, allyl phenol resin, phenol novolac resin, cresol novolac resin, naphthol modified phenol resin, dicyclopentadiene modified phenol resin, p-xylene modified phenol resin and the like.
アミン系化合物としては、脂肪族ポリアミン、芳香族アミン、変性ポリアミン(例えば、ポリアミノアミド、ポリアミノイミド、ポリアミノエステル、ポリアミノ尿素、ポリエーテル変性アミンなど)、第三級アミン化合物、イミダゾール化合物(例えば、2−メチルイミダゾール、2−フェニルイミダゾール、2−フェニル−4−メチルイミダゾール、2−フェニル−4−メチル−5−ヒドロキシメチルイミダゾール、2−ウンデシルイミダゾール、2−ヘプタデシルイミダゾール、2,2−ジアミノ−6−[2’−メチルイミダゾリル−(1’)]−エチル−s−トリアジンなど)、ヒドラジド化合物、ジシアンアミド化合物、メラミン化合物などが挙げられる。 Examples of amine compounds include aliphatic polyamines, aromatic amines, modified polyamines (eg, polyaminoamides, polyaminoimides, polyaminoesters, polyaminoureas, polyether-modified amines), tertiary amine compounds, and imidazole compounds (eg, 2 -Methylimidazole, 2-phenylimidazole, 2-phenyl-4-methylimidazole, 2-phenyl-4-methyl-5-hydroxymethylimidazole, 2-undecylimidazole, 2-heptadecylimidazole, 2,2-diamino- 6- [2′-methylimidazolyl- (1 ′)]-ethyl-s-triazine, etc.), hydrazide compounds, dicyanamide compounds, melamine compounds and the like.
酸無水物としては、メチルテトラヒドロフタル酸無水物、メチルヘキサヒドロフタル酸無水物、アルキル化テトラヒドロフタル酸無水物、ヘキサヒドロフタル酸無水物、メチルハイミック酸無水物、アルケニル基で置換されたコハク酸無水物、メチルナジック酸無水物、グルタル酸無水物などが例示される。中でも、2,4−ジエチルペンタン二酸無水物、3,4−ジメチル−6−(2−メチル−1−プロペニル)−1,2,3,6−テトラヒドロフタル酸無水物、1−イソプロピル−4−メチル−ビシクロ[2.2.2]オクト−5−エン−2,3−ジカルボン酸無水物、ノルボルナン−2,3−ジカルボン酸無水物、メチルノルボルナン−2,3−ジカルボン酸無水物、水素化メチルナジック酸無水物、アルケニル基で置換されたコハク酸無水物、ジエチルグルタル酸無水物が挙げられる。 Examples of acid anhydrides include methyltetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, alkylated tetrahydrophthalic anhydride, hexahydrophthalic anhydride, methylheimic acid anhydride, and alkenyl-substituted succinic acid. Examples include acid anhydride, methyl nadic acid anhydride, glutaric acid anhydride and the like. Among them, 2,4-diethylpentanedioic anhydride, 3,4-dimethyl-6- (2-methyl-1-propenyl) -1,2,3,6-tetrahydrophthalic anhydride, 1-isopropyl-4 -Methyl-bicyclo [2.2.2] oct-5-ene-2,3-dicarboxylic acid anhydride, norbornane-2,3-dicarboxylic acid anhydride, methylnorbornane-2,3-dicarboxylic acid anhydride, hydrogen Methyl nadic acid anhydride, succinic acid anhydride substituted with an alkenyl group, and diethyl glutaric acid anhydride.
過酸化物としては、1,1,3,3−テトラメチルブチルパーオキシ2−エチルヘキサナート、t−ブチルパーオキシベンゾエート、t−ブチルパーオキシネオデカノエート、クミルパーオキシネオデカノエート、1,1,3,3−テトラメチルブチルパーオキシネオデカノエート、t−ブチルパーオキシベンゾエート、ジクミルパーオキサイド、ジ−t−ブチルパーオキサイド、ジ−t−ヘキシルパーオキサイド、ジ(2−t−ブチルパーオキシイソプロピル)ベンゼン、2,2−ジ(4,4−ジ−(ブチルパーオキシ)シクロヘキシル)プロパン、p−メンタンハイドロパーオキサイド、ジイソプロピルベンゼンハイドロパーオキサイド、1,1,3,3−テトラメチルブチルハイドロパーオキサイド、クメンハイドロパーオキサイド、1,1−ジ(t−ブチルパーオキシ)シクロヘキサン、シクロヘキサノンパーオキサイド、1,1−ジ(t−ヘキシルパーオキシ)シクロヘキサンが挙げられる。 Peroxides include 1,1,3,3-tetramethylbutylperoxy 2-ethylhexanate, t-butylperoxybenzoate, t-butylperoxyneodecanoate, cumylperoxyneodecanoate, 1,1,3,3-tetramethylbutylperoxyneodecanoate, t-butylperoxybenzoate, dicumyl peroxide, di-t-butyl peroxide, di-t-hexyl peroxide, di (2- t-butylperoxyisopropyl) benzene, 2,2-di (4,4-di- (butylperoxy) cyclohexyl) propane, p-menthane hydroperoxide, diisopropylbenzene hydroperoxide, 1,1,3,3 -Tetramethylbutyl hydroperoxide, cumene hydroperoxide, 1 1,1-di (t-butylperoxy) cyclohexane, cyclohexanone peroxide, 1,1-di (t-hexylperoxy) cyclohexane.
金属錯体としては、アルキルアセトアセテートアルミニウムジイソプロピレート、アルミニウムトリス(アセチルアセトネート)、アクリル酸アルミニウム、アルミニウムビスエチルアセトアセテートジイソプロピレート、2−エチルヘキサン酸マグネシウムが挙げられる。 Examples of the metal complex include alkyl acetoacetate aluminum diisopropylate, aluminum tris (acetylacetonate), aluminum acrylate, aluminum bisethylacetoacetate diisopropylate, and magnesium 2-ethylhexanoate.
アゾ化合物としては、2,2’−アゾビス(4−メトキシ−2,4−ジメチルバレロニトリル)、2,2’−アゾビス(2,4−ジメチルバレロニトリル)、1,1’−アゾビス(シクロヘキサン−1−カルボニトリル)、2,2’−アゾビス{2−メチル−N−[2−(1−ヒドロキシブチル)]プロピオンアミド}、2,2’−アゾビス[2−メチル−N−(2−ヒドロキシエチル)プロピオンアミド]、2,2’−アゾビス[N−(2−プロペニル)−2−メチルプロピオンアミド]、2,2’−アゾビス(N−シクロヘキシル−2−メチルプロピオンアミド、2,2’−アゾビス[2−(2−イミダゾリン−2−イル)プロパンが挙げられる。 Examples of the azo compound include 2,2′-azobis (4-methoxy-2,4-dimethylvaleronitrile), 2,2′-azobis (2,4-dimethylvaleronitrile), 1,1′-azobis (cyclohexane- 1-carbonitrile), 2,2′-azobis {2-methyl-N- [2- (1-hydroxybutyl)] propionamide}, 2,2′-azobis [2-methyl-N- (2-hydroxy) Ethyl) propionamide], 2,2′-azobis [N- (2-propenyl) -2-methylpropionamide], 2,2′-azobis (N-cyclohexyl-2-methylpropionamide, 2,2′- And azobis [2- (2-imidazolin-2-yl) propane.
導電性組成物をダイボンディング剤として使用する場合、ブリードの抑制、良好な高温強度や吸湿後の高温強度の低下抑制、及び低い吸水率が望まれる。なかでも、ブリードの発生はモールド剤とリードフレームの剥離を誘発する可能性があり、パッケージの信頼性の点から重要である。これらの観点から、(B)成分として、エポキシ樹脂、アクリル樹脂、かつ(C)成分として、フェノール樹脂、アミン系化合物、過酸化物の組み合わせが好ましい。 When the conductive composition is used as a die bonding agent, suppression of bleed, good high temperature strength, suppression of decrease in high temperature strength after moisture absorption, and low water absorption are desired. In particular, the occurrence of bleed may induce peeling of the molding agent and the lead frame, which is important from the viewpoint of package reliability. From these viewpoints, as the component (B), an epoxy resin, an acrylic resin, and as the component (C), a combination of a phenol resin, an amine compound, and a peroxide is preferable.
(A)成分、(B)成分及び(C)成分は、これらの合計を100質量部とした場合、(A)成分は、導電性と弾性率の点から、40〜80質量部であることが好ましく、より好ましくは50〜75質量部であり、さらに好ましくは50〜65質量部である。(B)成分は、ディスペンス時の流動性やブリード、接着強度、吸水率の点から、10〜58質量部であることが好ましく、より好ましくは 22〜42質量部である。(C)成分は、ボイド、ブリード、硬化性、接着強度の点から、2〜10質量部であることが好ましく、より好ましくは3〜8質量部である。 When (A) component, (B) component, and (C) component make these total 100 mass parts, (A) component shall be 40-80 mass parts from the point of electroconductivity and an elasticity modulus. Is more preferable, More preferably, it is 50-75 mass parts, More preferably, it is 50-65 mass parts. (B) It is preferable that it is 10-58 mass parts from the point of the fluidity | liquidity at the time of dispensing, bleeding, adhesive strength, and a water absorption rate, More preferably, it is 22-42 mass parts. (C) It is preferable that it is 2-10 mass parts from a point of a void, a bleed, sclerosis | hardenability, and adhesive strength, More preferably, it is 3-8 mass parts.
本発明の導電性組成物には、(A)成分以外の導電粒子を配合してもよい。(A)成分以外の導電粒子は、全導電粒子((A)成分の銀被覆粒子及び(A)成分以外の導電粒子)中、合計で50質量%以下であることが好ましく、より好ましくは30質量%以下であり、もっとも好ましくは導電粒子として(A)成分の銀被覆粒子のみを使用することである。(A)成分以外の導電粒子としては、球状の銀被覆セラミック粒子、銀被覆ガラス粒子、銀被覆アルミニウム粒子を使用することができる。球状の銀被覆粒子のコアは、セラミック、ガラス又はアルミニウムからなることが好ましい。セラミックとしては、アルミナ、炭化ケイ素、窒化ケイ素、チタン酸バリウム、窒化ホウ素、フェライト、ステアタイト、酸化亜鉛、ジルコニアが挙げられ、入手の自由度、粒径や形状のコントロールの自由度、コストの観点の点から、特にアルミナが好ましい。球状の銀被覆粒子は、レーザ光散乱法により測定した体積平均粒子径D50が、1〜20μmのものが好ましく、より好ましくは、2〜15μmである。球状の銀被覆粒子は、コア材への銀被覆率と導電性の観点の点から、銀被覆層が球状の銀被覆粒子の全重量のうち、10〜50質量%が好ましく、より好ましくは、15〜40質量%である。球状の銀被覆粒子は、銀被覆層が均一に備わっていることが好ましく、厚みは、銀被覆層が厚くなって、粒子全体の比重、ひいては導電性組成物の比重が大きくなり、導電性組成物を同一重量で塗布した時の体積を減少させることによる、効率の低下を回避し、かつ安定した導電性を得る観点の点から、好ましくは50〜300nmである。銀被覆層の厚みは、より好ましくは50〜200nmであり、さらに好ましくは70〜150nmである。 You may mix | blend electrically conductive particles other than (A) component with the electrically conductive composition of this invention. The total amount of the conductive particles other than the component (A) is preferably 50% by mass or less, more preferably 30% in total in all the conductive particles (the silver-coated particles of the component (A) and the conductive particles other than the component (A)). Most preferably, only the silver-coated particles of component (A) are used as the conductive particles. As the conductive particles other than the component (A), spherical silver-coated ceramic particles, silver-coated glass particles, and silver-coated aluminum particles can be used. The core of the spherical silver-coated particles is preferably made of ceramic, glass or aluminum. Examples of ceramics include alumina, silicon carbide, silicon nitride, barium titanate, boron nitride, ferrite, steatite, zinc oxide, and zirconia. Freedom to obtain, freedom to control particle size and shape, and cost From this point, alumina is particularly preferable. The spherical silver-coated particles preferably have a volume average particle diameter D50 measured by a laser light scattering method of 1 to 20 μm, more preferably 2 to 15 μm. The spherical silver-coated particles are preferably 10 to 50% by mass of the total weight of the silver-coated particles having a spherical silver coating layer, more preferably, from the viewpoint of silver coverage on the core material and conductivity. 15 to 40% by mass. Spherical silver-coated particles preferably have a uniform silver coating layer, and the thickness of the silver coating layer increases, and the specific gravity of the entire particle, and hence the specific gravity of the conductive composition, increases. The thickness is preferably 50 to 300 nm from the viewpoint of avoiding a decrease in efficiency caused by reducing the volume when an object is applied with the same weight and obtaining stable conductivity. The thickness of the silver coating layer is more preferably 50 to 200 nm, still more preferably 70 to 150 nm.
(A)成分以外の導電粒子としては、銀粒子、銅粒子、ニッケル粒子、パラジウム粒子、インジウム粒子、錫粒子、亜鉛粒子、ビスマス粒子又はそれらの合金を使用することもできる。形状は、特に限定されない。 As the conductive particles other than the component (A), silver particles, copper particles, nickel particles, palladium particles, indium particles, tin particles, zinc particles, bismuth particles, or alloys thereof can also be used. The shape is not particularly limited.
本発明の導電性組成物には、溶剤を配合してもよい。溶剤は、特に限定されず、例えば、エチレングリコール、プロピレングリコール、ジヒドロターピネオールなどのアルコール系溶剤;トルエン、キシレン、エチルベンゼン、ジエチルベンゼン、イソプロピルベンゼン、アミルベンゼン、p−シメン、テトラリン及び石油系芳香族炭化水素混合物などの芳香族炭化水素系溶剤;テルピネオール、リナロール、ゲラニオール、シトロネロールなどのテルペンアルコール;エチレングリコールモノエチルエーテル、エチレングリコールモノブチルエーテル、プロピレングリコールモノメチルエーテル、プロピレングリコールモノエチルエーテル、プロピレングリコールモノ−n−ブチルエーテル、プロピレングリコールモノ−tert−ブチルエーテル、ジエチレングリコールモノエチルエーテル、ジエチレングリコ−ルモノブチルエーテル、ジプロピレングリコールモノメチルエーテル、ジプロピレングリコールモノブチルエーテル、トリプロピレングリコールモノメチルエーテルなどのエーテルアルコール系溶剤;メチルイソブチルケトンなどのケトン系溶剤;並びにエチレングリコールモノメチルエーテルアセテート、エチレングリコールモノエチルエーテルアセテート、エチレングリコールモノブチルエーテルアセテート、プロピレングリコールモノメチルエーテルアセテート、プロピレングリコールモノエチルエーテルアセテートなどのエステル系溶剤、水などが挙げられる。溶剤は、単独でも、複数種を併用してもよい。 You may mix | blend a solvent with the electroconductive composition of this invention. The solvent is not particularly limited, and examples thereof include alcohol solvents such as ethylene glycol, propylene glycol, dihydroterpineol; toluene, xylene, ethylbenzene, diethylbenzene, isopropylbenzene, amylbenzene, p-cymene, tetralin, and petroleum aromatic hydrocarbons. Aromatic hydrocarbon solvents such as mixtures; Terpene alcohols such as terpineol, linalool, geraniol, citronellol; ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, propylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol mono-n- Butyl ether, propylene glycol mono-tert-butyl ether, diethylene glycol monoethyl ether, die Ether alcohol solvents such as tylene glycol monobutyl ether, dipropylene glycol monomethyl ether, dipropylene glycol monobutyl ether, tripropylene glycol monomethyl ether; ketone solvents such as methyl isobutyl ketone; and ethylene glycol monomethyl ether acetate, ethylene glycol monoethyl ether Examples thereof include ester solvents such as acetate, ethylene glycol monobutyl ether acetate, propylene glycol monomethyl ether acetate, and propylene glycol monoethyl ether acetate, and water. A solvent may be individual or may use multiple types together.
さらに、本発明の導電性組成物には、本発明の所定の効果を損なわない範囲で、無機充填剤(例えば、ヒュームドシリカ、炭酸カルシウム、タルクなど)、カップリング剤(例えば、γ−グリシドキシプロピルトリメトキシシランなどのシランカップリング剤、テトラオクチルビス(ジトリデシルホスファイト)チタネートなどのチタネートカップリング剤など)、シランモノマー(例えば、トリス(3−(トリメトキシシリル)プロピル)イソシアヌレート)、可塑剤(例えば、カルボキシル基末端ポリブタジエン‐アクリロニトリルなどのコポリマー、シリコーンゴム、シリコーンゴムパウダー、シリコーンレジンパウダー、アクリル樹脂パウダーなどの樹脂パウダー)、難燃剤、酸化防止剤、消泡剤などを配合することができる。 Furthermore, the conductive composition of the present invention includes an inorganic filler (for example, fumed silica, calcium carbonate, talc, etc.) and a coupling agent (for example, γ-glycerin) within the range that does not impair the predetermined effects of the present invention. Silane coupling agents such as Sidoxypropyltrimethoxysilane, Titanate coupling agents such as Tetraoctylbis (ditridecylphosphite) titanate), Silane monomers (for example, tris (3- (trimethoxysilyl) propyl) isocyanurate ), Plasticizer (for example, copolymer such as carboxyl group-terminated polybutadiene-acrylonitrile, silicone rubber, silicone rubber powder, silicone resin powder, resin powder such as acrylic resin powder), flame retardant, antioxidant, antifoaming agent, etc. can do.
本発明の導電性組成物は、(A)成分、(B)成分及び(C)成分、並びに場合により溶剤などの任意成分を、例えば、3本ロールやプラネタリーミキサー、ライカイ機を用いて、混合することによって、ペースト状の導電性組成物を製造することができる。なお、上記各成分を混合する順番は任意であり、同時に混合してもよいし、逐次混合でもよい。 The conductive composition of the present invention is composed of (A) component, (B) component and (C) component, and optionally optional components such as a solvent, for example, using a three roll, planetary mixer, or likai machine. By mixing, a paste-like conductive composition can be produced. In addition, the order which mixes said each component is arbitrary, may be mixed simultaneously and may be mixed sequentially.
次に、上記のようにして得られた導電性組成物を、所望の対象(例えば、基板など)に塗布した後、加熱して熱硬化させることにより硬化膜を形成することができる。 Next, after applying the conductive composition obtained as described above to a desired object (for example, a substrate or the like), a cured film can be formed by heating and thermosetting.
塗布方法は、特に限定されず、例えば、ディスペンス、ジェットディスペンス、孔版印刷、スクリーン印刷、ピン転写、スタンピングなどが挙げられる。 The coating method is not particularly limited, and examples thereof include dispensing, jet dispensing, stencil printing, screen printing, pin transfer, and stamping.
加熱温度は、例えば、120〜200℃とすることができ、より好ましくは150〜175℃であり、加熱時間は、例えば、1〜120時間とすることができ、好ましくは、30〜60時間である。 The heating temperature can be, for example, 120 to 200 ° C., more preferably 150 to 175 ° C., and the heating time can be, for example, 1 to 120 hours, preferably 30 to 60 hours. is there.
本発明の導電性組成物を、基板(例えば、LTCCなどのセラミック基板やガラス・エポキシ基板)上に塗布した後、熱硬化させることによって、導電回路を形成することができる。また、本発明の導電性組成物は、ダイボンディング剤として使用することもできる。例えば、本発明の導電性組成物からなるダイボンディング剤を、リードフレーム又は基板(例えば、Bare Cuリードフレーム、AgめっきCuリードフレーム、PPF、Agめっき42アロイフレーム)の所定の部位に塗布した後、半導体素子をマウントし、熱硬化させて、リードフレーム又は基板と、半導体素子とを接合させることができる。 A conductive circuit can be formed by applying the conductive composition of the present invention on a substrate (for example, a ceramic substrate such as LTCC or a glass / epoxy substrate) and then thermally curing it. The conductive composition of the present invention can also be used as a die bonding agent. For example, after applying the die bonding agent made of the conductive composition of the present invention to a predetermined part of a lead frame or a substrate (for example, Bare Cu lead frame, Ag plated Cu lead frame, PPF, Ag plated 42 alloy frame). The semiconductor element can be mounted and thermally cured to bond the lead frame or the substrate and the semiconductor element.
このようにして得られた硬化膜は、十分な導電性(例えば比抵抗値が1×10−2Ω・cm以下)を示す。また、基板との間の接着性(接着強度、接着抵抗値)も良好である。The cured film thus obtained exhibits sufficient conductivity (for example, a specific resistance value of 1 × 10 −2 Ω · cm or less). Moreover, the adhesiveness (adhesion strength, adhesion resistance value) between the substrates is also good.
以下、本発明の実施例について説明するが、本発明はこれらに限定されるものではない。 Examples of the present invention will be described below, but the present invention is not limited thereto.
表1及び2に示す各成分を、3本ロールを用いて混合し、実施例及び比較例の各導電性組成物を調製した。 Each component shown in Table 1 and 2 was mixed using 3 rolls, and each electrically conductive composition of an Example and a comparative example was prepared.
実施例・比較例の各導電性組成物について、特性の測定を行った。結果を表1及び2に示す。
〔比抵抗の測定〕
アルミナ基板(120mm×20mm、厚み1.6mm)に、図1−1のようなパターンになるように、ステンレスマスク(200メッシュ、レジスト20μm)を用いて、実施例・比較例の各導電性組成物をスクリーン印刷した。次に、150℃±5℃に保持された送風乾燥機で30分間加熱して、硬化膜を形成した試料を得た。試料の硬化膜の両端の抵抗値X(Ω)を、4261ALCRメーター(YHP社製)を用いて測定した。
アルミナ基板1上の導電性組成物の硬化膜2の厚みZ(μm)を、表面粗さ形状測定機サーフコム590A(東京精密社製 表面粗さ形状測定機)を用いて測定した(図1−2参照)。
比抵抗値ρ(Ω・cm)を、次式により算出した。
ρ = (0.1/7.1)×X×Z×10-4 (Ω・cm)
試料2個の測定値から平均値を算出し、比抵抗の値とした。The characteristics of each conductive composition of Examples and Comparative Examples were measured. The results are shown in Tables 1 and 2.
[Measurement of resistivity]
Each conductive composition of Examples and Comparative Examples using an alumina substrate (120 mm × 20 mm, thickness 1.6 mm) and a stainless mask (200 mesh, resist 20 μm) so as to have a pattern as shown in FIG. The object was screen printed. Next, it heated for 30 minutes with the ventilation drying machine hold | maintained at 150 degreeC +/- 5 degreeC, and the sample which formed the cured film was obtained. The resistance value X (Ω) at both ends of the cured film of the sample was measured using a 4261ALCR meter (manufactured by YHP).
The thickness Z (μm) of the cured film 2 of the conductive composition on the alumina substrate 1 was measured using a surface roughness profile measuring machine Surfcom 590A (surface roughness profile measuring machine manufactured by Tokyo Seimitsu Co., Ltd.) (FIG. 1− 2).
The specific resistance value ρ (Ω · cm) was calculated by the following equation.
ρ = (0.1 / 7.1) × X × Z × 10 −4 (Ω · cm)
The average value was calculated from the measured values of the two samples, and used as the specific resistance value.
〔接触抵抗値〕
メタルマスク(厚さ:70μm)を用いて、膜厚:7〜15μmのAg厚膜電極3を備えた25.4±0.1mm□のアルミナ基板4上(図2−1参照)に、図2−2のようなパターンになるように、メタルマスク(厚さ70μm)を用いて、実施例・比較例の各導電性組成物5をスクリーン印刷した。スクリーン印刷は、メタルスキージ(スキージ圧力100kPa、スキージ20mm/s、基板−マスク間ギャップ0mm、スキージ角度60°、版離れ速度0.05mm/s)を使用して行った。
導電性組成物5に接触するようにして、AgPd電極の3216型コンデンサ部品(コンデンサ電極6)を搭載し(図2−3)、部品に均等に1.0±0.5Nの荷重を加えて、試料を得た。
恒温槽にて、所定の硬化条件(150℃へ30分で昇温させ、150℃で30分保持)で導電性組成物を硬化させた。
試料のコンデンサ電極6上部と導電性組成物5の塗布部より周囲1mm以内の導体(基板電極)間の抵抗値を4端子法にて測定した(図2−4参照)。電流源の測定電流値は10±0.5mAとした。
試料8個の測定値から平均値を算出し、接触抵抗の値とした。[Contact resistance value]
Using a metal mask (thickness: 70 μm) on the 25.4 ± 0.1 mm square alumina substrate 4 (see FIG. 2-1) provided with an Ag thick film electrode 3 having a thickness of 7 to 15 μm, Each conductive composition 5 of Examples and Comparative Examples was screen-printed using a metal mask (thickness 70 μm) so as to have a pattern like 2-2. Screen printing was performed using a metal squeegee (squeegee pressure 100 kPa, squeegee 20 mm / s, substrate-mask gap 0 mm, squeegee angle 60 °, plate separation speed 0.05 mm / s).
An AgPd electrode 3216 type capacitor component (capacitor electrode 6) is mounted so as to be in contact with the conductive composition 5 (FIG. 2-3), and a load of 1.0 ± 0.5 N is uniformly applied to the component. A sample was obtained.
In a thermostatic bath, the conductive composition was cured under predetermined curing conditions (heated to 150 ° C. in 30 minutes and held at 150 ° C. for 30 minutes).
The resistance value between the conductor (substrate electrode) within 1 mm from the upper part of the sample capacitor electrode 6 and the coated portion of the conductive composition 5 was measured by a four-terminal method (see FIG. 2-4). The measured current value of the current source was 10 ± 0.5 mA.
The average value was calculated from the measured values of 8 samples and used as the value of contact resistance.
〔接着強度の測定〕
1.5mm□×40μmtとなるパターンを、10個形成できるスクリーンマスクを用いて、各導電性組成物をBare Cuリードフレームにスクリーン印刷した。
2mm□シリコンチップをシリコン面が導電性組成物に接触するようにして、10個マウントした。
恒温槽にて、所定の硬化条件(150℃へ30分で昇温させ、150℃で30分保持)で硬化させた。
得られた試料を、強度試験機 MODEL-1605HTP(アイコーエンジニアリング社製)を用いて側面から突き、シリコンチップが剥がれた時の数値を読み取った。測定は、側面から突く際のテストスピード12±1mm/分、常温(25±5℃)で行った。(Measurement of adhesive strength)
Each conductive composition was screen-printed on a Bare Cu lead frame using a screen mask capable of forming 10 patterns of 1.5 mm □ × 40 μmt.
Ten 2 mm square silicon chips were mounted so that the silicon surface was in contact with the conductive composition.
In a thermostatic bath, curing was performed under predetermined curing conditions (heating to 150 ° C. in 30 minutes and holding at 150 ° C. for 30 minutes).
The obtained sample was struck from the side surface using a strength tester MODEL-1605HTP (manufactured by Aiko Engineering Co., Ltd.), and the numerical value when the silicon chip was peeled was read. The measurement was performed at a normal speed (25 ± 5 ° C.) at a test speed of 12 ± 1 mm / min when protruding from the side.
〔粘度変化〕
E型粘度計 TVE-22Hを用い、ローター 3°コーンR9.7 を用いた。
実施例・比較例の各導電性組成物を、テルモ社製シリンジを用いて0.3ml吸い上げ、粘度計のカップの中心部に塗布した。カップを粘度計に装着し、恒温槽を用いて25℃に保ち、10分間放置した。0.5rpmで3分後の粘度を測定した(V1)。
実施例・比較例の各導電性組成物をシリンジに充填後、25℃、湿度50%の環境下、24時間放置した。各導電性組成物をシリンジを用いて0.3ml吸い上げ、粘度計のカップの中心部に塗布した。カップを粘度計に装着し、恒温槽を用いて25℃に保ち、10分間放置した。0.5rpmで3分後の粘度を測定した(V2)。
粘度の変化率を、次式により算出した。
粘度変化率(%)=(V2−V1)/V1×100[Viscosity change]
An E-type viscometer TVE-22H was used, and a rotor 3 ° cone R9.7 was used.
Each conductive composition of Examples and Comparative Examples was sucked up by 0.3 ml using a Terumo syringe and applied to the center of the cup of the viscometer. The cup was attached to a viscometer, kept at 25 ° C. using a thermostatic bath, and allowed to stand for 10 minutes. The viscosity after 3 minutes at 0.5 rpm was measured (V1).
Each conductive composition of Examples and Comparative Examples was filled in a syringe and then left for 24 hours in an environment of 25 ° C. and 50% humidity. 0.3 ml of each conductive composition was sucked up using a syringe and applied to the center of the viscometer cup. The cup was attached to a viscometer, kept at 25 ° C. using a thermostatic bath, and allowed to stand for 10 minutes. The viscosity after 3 minutes at 0.5 rpm was measured (V2).
The rate of change in viscosity was calculated by the following formula.
Viscosity change rate (%) = (V2−V1) / V1 × 100
〔D50の測定〕
D50は、銀被覆粒子をミクロスパテラで2杯、300mlビーカーに採り、0.5%スルホコハク酸ナトリウムのジオクチルエステル溶液を50ml入れ、超音波ホモジナイザーで10分間分散し、光散乱解析タイプ粒度分布測定装置(コールターLS230(ベックマンコールター製)で測定することができる。50%の累積径の平均値をD50とする。[Measurement of D50]
D50 is a glass-coated particle with 2 cups of microspatella, taken in a 300 ml beaker, put 50 ml of 0.5% sodium sulfosuccinate dioctyl ester solution, and dispersed with an ultrasonic homogenizer for 10 minutes. (A Coulter LS230 (manufactured by Beckman Coulter)) The average value of 50% cumulative diameter is D50.
〔平均厚みTの測定〕
平均厚みは、銀被覆粒子2gとエポキシ樹脂(Epoxy Resin20−8130−032(BUEHLER製))5gとエポキシ樹脂硬化剤(EPOXY HARDENER20−8132−008(BUEHLER製))1gを直径25mmのクリアカップに計り取り、ヘラを用いてよく混合し、室温で12時間静置後、硬化した樹脂を、クリアカップより取り出し、ミクロトームで面出し加工を行い、カーボン蒸着後、電界放射型走査型電子顕微鏡(JEOL製JSM−7500F)で1000倍又は2000倍の倍率で写真を撮影し、中心を通る最短辺を銀被覆の厚みとして測定し、測定個数50個の平均値を平均厚みTとする。[Measurement of average thickness T]
The average thickness is 2 g of silver coated particles, 5 g of epoxy resin (Epoxy Resin 20-8130-032 (manufactured by BUEHLER)) and 1 g of epoxy resin curing agent (EPOXY HARDENER 20-8132-008 (manufactured by BUEHLER)) in a 25 mm diameter clear cup. Take out and mix well using a spatula, let stand at room temperature for 12 hours, then remove the cured resin from the clear cup, perform surface processing with a microtome, and after carbon deposition, a field emission scanning electron microscope (manufactured by JEOL) JSM-7500F) is photographed at a magnification of 1000 times or 2000 times, the shortest side passing through the center is measured as the thickness of the silver coating, and the average value of 50 measured numbers is defined as the average thickness T.
〔銀被覆層の重量〕
銀被覆粒子の重量と、銀被覆層を硝酸に溶解させて、銀を除き、測定したコア材の重量から算出した値である。[Weight of silver coating layer]
It is a value calculated from the weight of the silver-coated particles and the core material measured by dissolving the silver-coated layer in nitric acid and removing silver.
〔銀被覆層の厚み〕
平均厚みTと同様なサンプルを作製し、電界放射型走査型電子顕微鏡(JEOL製JSM−7500F)で10000倍〜30000倍の倍率で測定して求めた値である。[Thickness of silver coating layer]
It is a value obtained by preparing a sample similar to the average thickness T, and measuring it at a magnification of 10,000 to 30,000 times with a field emission scanning electron microscope (JSM-7500F manufactured by JEOL).
表1及び2中の樹脂、硬化剤及びその他の成分は、以下のとおりである。
樹脂1:ビスフェノールF型エポキシ樹脂
ビスフェノールF型エポキシ樹脂(エポキシ当量:160〜175)
樹脂2:アミノフェノール型エポキシ樹脂
N,N−ビス(2,3−エポキシプロピル)−4−(2,3−エポキシプロピルオキシ)アニリン
樹脂3:PO変性エポキシ樹脂
ポリオキシプロピレンビスフェノールAジグリシジルエーテル(エポキシ当量250〜270)
樹脂4:ビスマレイミド樹脂
1,6−ビスマレイミド−(2,2,4−トリメチル)ヘキサン
硬化剤1:ポリオキシプロピレンジアミン
H2N−SH(CH3)CH2[OCH2CH(CH3)]xNH2
x=33.1、活性水素当量:514
フィラー1:ヒュームドシリカ
ポリジメチルシロキサン処理ヒュームドシリカ
体積基準平均粒径:0.25μmThe resins, curing agents and other components in Tables 1 and 2 are as follows.
Resin 1: Bisphenol F type epoxy resin Bisphenol F type epoxy resin (epoxy equivalent: 160 to 175)
Resin 2: Aminophenol type epoxy resin N, N-bis (2,3-epoxypropyl) -4- (2,3-epoxypropyloxy) aniline resin 3: PO modified epoxy resin Polyoxypropylene bisphenol A diglycidyl ether ( Epoxy equivalent 250-270)
Resin 4: Bismaleimide resin 1,6-Bismaleimide- (2,2,4-trimethyl) hexane curing agent 1: Polyoxypropylenediamine H 2 N—SH (CH 3 ) CH 2 [OCH 2 CH (CH 3 ) ] XNH 2
x = 33.1, active hydrogen equivalent: 514
Filler 1: Fumed silica Polydimethylsiloxane-treated fumed silica Volume-based average particle size: 0.25 μm
図3−1は、銀被覆粒子1の倍率5000倍のSEM写真であり、図3−2は、平均厚みを測定するため、銀被覆粒子1を水溶性エポキシ樹脂に配合して、硬化させた硬化物の断面のSEM写真である。 FIG. 3A is an SEM photograph at a magnification of 5000 times of the silver-coated particles 1, and FIG. 3-2 is a graph illustrating the measurement of the average thickness. It is a SEM photograph of the section of hardened material.
表1より、本発明のフレーク状の銀被覆粒子を使用した実施例1〜6は、いずれも、比抵抗値及び接触抵抗値が小さく、接着強度にも優れていた。なかでも、オレイン酸処理した銀粒子を使用した実施例3〜6は、粘度変化が少なく、導電性組成物の安定性においても優れていた。
一方、アスペクト比が小さい銀被覆粒子を使用した比較例1は、比抵抗値、接触抵抗値に劣っていた。
表2の実施例7〜9より、熱硬化性樹脂系を変更しても、本発明のフレーク状の銀被覆粒子が有効であり、銀被覆粒子の量を変更しても、本発明のフレーク状の銀被覆粒子が有効であることがわかる。また、表2の実施例10及び11により、(A)成分の銀被覆粒子が、導電性組成物((A)成分、(B)成分及び(C)成分)の合計100質量部に対して、75質量部含まれると、若干接着強度が劣る傾向が見られた。また、表2の実施例14及び15により、(A)成分の銀被覆層が銀被覆粒子の全重量のうち、50〜60質量%の場合においても、比抵抗値及び接触抵抗値が小さく、接着強度にも優れていた。実施例15により、アスペクト比T/D50が1.0の球状の銀被覆粒子を使用した場合には、接触抵抗の点で若干劣る傾向が見られた。From Table 1, all of Examples 1 to 6 using the flaky silver-coated particles of the present invention had small specific resistance values and contact resistance values, and were excellent in adhesive strength. Among these, Examples 3 to 6 using silver particles treated with oleic acid had little change in viscosity and were excellent in the stability of the conductive composition.
On the other hand, Comparative Example 1 using silver-coated particles having a small aspect ratio was inferior in specific resistance value and contact resistance value.
From Examples 7 to 9 in Table 2, even if the thermosetting resin system is changed, the flaky silver-coated particles of the present invention are effective, and even if the amount of silver-coated particles is changed, the flakes of the present invention It can be seen that the silver-coated particles are effective. Moreover, according to Examples 10 and 11 in Table 2, the silver-coated particles of the (A) component are based on 100 parts by mass in total of the conductive composition (the (A) component, the (B) component, and the (C) component). When 75 parts by mass was contained, the adhesive strength was slightly inferior. Further, according to Examples 14 and 15 of Table 2, the specific resistance value and the contact resistance value are small even when the silver coating layer of the component (A) is 50 to 60% by mass in the total weight of the silver-coated particles, The adhesive strength was also excellent. According to Example 15, when spherical silver-coated particles having an aspect ratio T / D50 of 1.0 were used, a tendency to be slightly inferior in terms of contact resistance was observed.
本発明によれば、コストダウンと、良好な接着性及び導電性の発現との両方を満足させる導電性組成物が提供される。本発明の導電性組成物は、導電回路の形成、ダイボンディング剤として有用である。 ADVANTAGE OF THE INVENTION According to this invention, the electrically conductive composition which satisfies both cost reduction and favorable adhesiveness and expression of electroconductivity is provided. The conductive composition of the present invention is useful as a conductive circuit formation and die bonding agent.
Claims (9)
(B)熱硬化性樹脂、並びに
(C)硬化剤
を含む、ダイボンディング剤。 (A) The volume average particle diameter D50 measured by the laser light scattering method is 1 to 10 μm, the average thickness T measured by scanning electron microscope observation is 0.3 to 10 μm, and the aspect ratio T / D50 is Flaky silver-coated ceramic particles 0.3 to 1.0,
(B) A thermosetting resin, and (C) a die bonding agent containing a curing agent .
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JP5925556B2 (en) * | 2012-03-29 | 2016-05-25 | Dowaエレクトロニクス株式会社 | Silver-coated flaky glass powder and method for producing the same |
JP6219042B2 (en) * | 2013-03-14 | 2017-10-25 | コスモ石油ルブリカンツ株式会社 | High thermal conductive epoxy resin composition |
TWI500737B (en) * | 2013-05-06 | 2015-09-21 | Chi Mei Corp | Conductive adhesive |
KR101618093B1 (en) * | 2014-03-17 | 2016-05-09 | 주식회사 상보 | A Conductive Paste Composition for Forming Conductive Thin Film on a Flexible Substrate and a method for producing the same |
JP6614127B2 (en) * | 2015-01-14 | 2019-12-04 | 東洋紡株式会社 | Conductive silver paste |
CN107406747B (en) * | 2015-03-02 | 2020-09-11 | 三键有限公司 | Heat-curable conductive adhesive |
MY190140A (en) * | 2015-04-16 | 2022-03-30 | Furukawa Electric Co Ltd | Electrically conductive adhesive film and dicing die bonding film |
JP2017008160A (en) * | 2015-06-18 | 2017-01-12 | 京セラ株式会社 | Method of producing die bonding paste and die bonding paste |
JP6729143B2 (en) * | 2015-10-29 | 2020-07-22 | 三菱マテリアル株式会社 | Resin composition, bonded body and semiconductor device |
CN108350105B (en) * | 2015-11-26 | 2020-10-13 | 三键有限公司 | Thermosetting composition and conductive adhesive using same |
CN107633894A (en) * | 2016-07-19 | 2018-01-26 | 翌骅实业股份有限公司 | The conducting resinl and its manufacture method and solar cell module of tool modification metallic |
WO2018087858A1 (en) * | 2016-11-10 | 2018-05-17 | 京セラ株式会社 | Semiconductor-bonding resin composition, semiconductor-bonding sheet, and semiconductor device using semiconductor-bonding sheet |
CN107424964A (en) * | 2017-07-27 | 2017-12-01 | 武汉市三选科技有限公司 | Underfill constituent and its bottom filling method of use and Electronic Assemblies component |
EP3664106A4 (en) * | 2017-08-03 | 2021-05-05 | Powdertech Co., Ltd. | Composite particles, powder, resin composition and moulded body |
JP2020139020A (en) * | 2019-02-27 | 2020-09-03 | ナミックス株式会社 | Conductive adhesive |
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