CN115305022B - Epoxy resin electronic pouring sealant and preparation method and application thereof - Google Patents
Epoxy resin electronic pouring sealant and preparation method and application thereof Download PDFInfo
- Publication number
- CN115305022B CN115305022B CN202211054965.XA CN202211054965A CN115305022B CN 115305022 B CN115305022 B CN 115305022B CN 202211054965 A CN202211054965 A CN 202211054965A CN 115305022 B CN115305022 B CN 115305022B
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- CN
- China
- Prior art keywords
- epoxy resin
- parts
- agent
- byk
- pouring sealant
- 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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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 78
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 78
- 239000000565 sealant Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000000945 filler Substances 0.000 claims abstract description 26
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
- 239000003999 initiator Substances 0.000 claims abstract description 12
- 239000003086 colorant Substances 0.000 claims abstract description 8
- 239000007822 coupling agent Substances 0.000 claims abstract description 7
- 239000002270 dispersing agent Substances 0.000 claims abstract description 7
- 238000004806 packaging method and process Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000012745 toughening agent Substances 0.000 claims abstract description 7
- 239000004014 plasticizer Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims abstract description 4
- -1 alkyl peroxides Chemical class 0.000 claims description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 24
- 239000000853 adhesive Substances 0.000 claims description 11
- 230000001070 adhesive effect Effects 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- 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 claims description 8
- 239000002518 antifoaming agent Substances 0.000 claims description 8
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 6
- 239000003085 diluting agent Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 229920000570 polyether Polymers 0.000 claims description 6
- 125000002723 alicyclic group Chemical group 0.000 claims description 5
- AFEQENGXSMURHA-UHFFFAOYSA-N oxiran-2-ylmethanamine Chemical compound NCC1CO1 AFEQENGXSMURHA-UHFFFAOYSA-N 0.000 claims description 5
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 5
- PSFDAYXWBWRTSM-UHFFFAOYSA-N 1-prop-2-enylpyrrole-2,5-dione Chemical compound C=CCN1C(=O)C=CC1=O PSFDAYXWBWRTSM-UHFFFAOYSA-N 0.000 claims description 4
- 239000004593 Epoxy Substances 0.000 claims description 4
- PEEHTFAAVSWFBL-UHFFFAOYSA-N Maleimide Chemical compound O=C1NC(=O)C=C1 PEEHTFAAVSWFBL-UHFFFAOYSA-N 0.000 claims description 4
- 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 claims description 4
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims description 4
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 4
- 239000000178 monomer Substances 0.000 claims description 4
- 238000004382 potting Methods 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 3
- WJRBRSLFGCUECM-UHFFFAOYSA-N hydantoin Chemical group O=C1CNC(=O)N1 WJRBRSLFGCUECM-UHFFFAOYSA-N 0.000 claims description 3
- CIRMGZKUSBCWRL-LHLOQNFPSA-N (e)-10-[2-(7-carboxyheptyl)-5,6-dihexylcyclohex-3-en-1-yl]dec-9-enoic acid Chemical compound CCCCCCC1C=CC(CCCCCCCC(O)=O)C(\C=C\CCCCCCCC(O)=O)C1CCCCCC CIRMGZKUSBCWRL-LHLOQNFPSA-N 0.000 claims description 2
- AOBIOSPNXBMOAT-UHFFFAOYSA-N 2-[2-(oxiran-2-ylmethoxy)ethoxymethyl]oxirane Chemical compound C1OC1COCCOCC1CO1 AOBIOSPNXBMOAT-UHFFFAOYSA-N 0.000 claims description 2
- 239000004944 Liquid Silicone Rubber Substances 0.000 claims description 2
- 229920000459 Nitrile rubber Polymers 0.000 claims description 2
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims description 2
- 239000004842 bisphenol F epoxy resin Substances 0.000 claims description 2
- 125000001951 carbamoylamino group Chemical group C(N)(=O)N* 0.000 claims description 2
- 239000004359 castor oil Substances 0.000 claims description 2
- 235000019438 castor oil Nutrition 0.000 claims description 2
- 238000006757 chemical reactions by type Methods 0.000 claims description 2
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 2
- 125000003700 epoxy group Chemical group 0.000 claims description 2
- 239000005350 fused silica glass Substances 0.000 claims description 2
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 239000004843 novolac epoxy resin Substances 0.000 claims description 2
- 150000002903 organophosphorus compounds Chemical class 0.000 claims description 2
- 125000005375 organosiloxane group Chemical group 0.000 claims description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 2
- 229920000728 polyester Polymers 0.000 claims description 2
- 229920001451 polypropylene glycol Polymers 0.000 claims description 2
- 229920002545 silicone oil Polymers 0.000 claims description 2
- 229920002379 silicone rubber Polymers 0.000 claims description 2
- 150000003623 transition metal compounds Chemical class 0.000 claims description 2
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 claims 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- 125000003668 acetyloxy group Chemical group [H]C([H])([H])C(=O)O[*] 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 239000013530 defoamer Substances 0.000 abstract description 5
- 238000003860 storage Methods 0.000 abstract description 5
- 239000012752 auxiliary agent Substances 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 238000001723 curing Methods 0.000 description 25
- 239000003292 glue Substances 0.000 description 13
- 239000002994 raw material Substances 0.000 description 10
- JJRDRFZYKKFYMO-UHFFFAOYSA-N 2-methyl-2-(2-methylbutan-2-ylperoxy)butane Chemical compound CCC(C)(C)OOC(C)(C)CC JJRDRFZYKKFYMO-UHFFFAOYSA-N 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- NECRQCBKTGZNMH-UHFFFAOYSA-N 3,5-dimethylhex-1-yn-3-ol Chemical compound CC(C)CC(C)(O)C#C NECRQCBKTGZNMH-UHFFFAOYSA-N 0.000 description 4
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 4
- 229920003192 poly(bis maleimide) Polymers 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- SJMYWORNLPSJQO-UHFFFAOYSA-N tert-butyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC(C)(C)C SJMYWORNLPSJQO-UHFFFAOYSA-N 0.000 description 4
- 229920001187 thermosetting polymer Polymers 0.000 description 4
- PMMYEEVYMWASQN-DMTCNVIQSA-N Hydroxyproline Chemical compound O[C@H]1CN[C@H](C(O)=O)C1 PMMYEEVYMWASQN-DMTCNVIQSA-N 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- FVQMJJQUGGVLEP-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy 2-ethylhexaneperoxoate Chemical compound CCCCC(CC)C(=O)OOOC(C)(C)C FVQMJJQUGGVLEP-UHFFFAOYSA-N 0.000 description 2
- 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
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 description 2
- HIDBROSJWZYGSZ-UHFFFAOYSA-N 1-phenylpyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C1=CC=CC=C1 HIDBROSJWZYGSZ-UHFFFAOYSA-N 0.000 description 2
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 2
- HFCUBKYHMMPGBY-UHFFFAOYSA-N 2-methoxyethyl prop-2-enoate Chemical compound COCCOC(=O)C=C HFCUBKYHMMPGBY-UHFFFAOYSA-N 0.000 description 2
- IFXDUNDBQDXPQZ-UHFFFAOYSA-N 2-methylbutan-2-yl 2-ethylhexaneperoxoate Chemical compound CCCCC(CC)C(=O)OOC(C)(C)CC IFXDUNDBQDXPQZ-UHFFFAOYSA-N 0.000 description 2
- RFSCGDQQLKVJEJ-UHFFFAOYSA-N 2-methylbutan-2-yl benzenecarboperoxoate Chemical compound CCC(C)(C)OOC(=O)C1=CC=CC=C1 RFSCGDQQLKVJEJ-UHFFFAOYSA-N 0.000 description 2
- FSGAMPVWQZPGJF-UHFFFAOYSA-N 2-methylbutan-2-yl ethaneperoxoate Chemical compound CCC(C)(C)OOC(C)=O FSGAMPVWQZPGJF-UHFFFAOYSA-N 0.000 description 2
- CFVWNXQPGQOHRJ-UHFFFAOYSA-N 2-methylpropyl prop-2-enoate Chemical compound CC(C)COC(=O)C=C CFVWNXQPGQOHRJ-UHFFFAOYSA-N 0.000 description 2
- BIKSKRPHKQWJCW-UHFFFAOYSA-N 3,4-dibromopyrrole-2,5-dione Chemical compound BrC1=C(Br)C(=O)NC1=O BIKSKRPHKQWJCW-UHFFFAOYSA-N 0.000 description 2
- GNSFRPWPOGYVLO-UHFFFAOYSA-N 3-hydroxypropyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCCO GNSFRPWPOGYVLO-UHFFFAOYSA-N 0.000 description 2
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 description 2
- 239000006087 Silane Coupling Agent Substances 0.000 description 2
- 239000004305 biphenyl Substances 0.000 description 2
- 235000010290 biphenyl Nutrition 0.000 description 2
- 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 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
- 239000011353 cycloaliphatic epoxy resin Substances 0.000 description 2
- OIWOHHBRDFKZNC-UHFFFAOYSA-N cyclohexyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1CCCCC1 OIWOHHBRDFKZNC-UHFFFAOYSA-N 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 230000009477 glass transition Effects 0.000 description 2
- 150000002460 imidazoles Chemical class 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 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 2
- 239000000203 mixture Substances 0.000 description 2
- SEEYREPSKCQBBF-UHFFFAOYSA-N n-methylmaleimide Chemical compound CN1C(=O)C=CC1=O SEEYREPSKCQBBF-UHFFFAOYSA-N 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- FBCQUCJYYPMKRO-UHFFFAOYSA-N prop-2-enyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC=C FBCQUCJYYPMKRO-UHFFFAOYSA-N 0.000 description 2
- 239000011342 resin composition Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- ISXSCDLOGDJUNJ-UHFFFAOYSA-N tert-butyl prop-2-enoate Chemical compound CC(C)(C)OC(=O)C=C ISXSCDLOGDJUNJ-UHFFFAOYSA-N 0.000 description 2
- SYXTYIFRUXOUQP-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy butaneperoxoate Chemical compound CCCC(=O)OOOC(C)(C)C SYXTYIFRUXOUQP-UHFFFAOYSA-N 0.000 description 1
- JRQJLSWAMYZFGP-UHFFFAOYSA-N 1,1'-biphenyl;phenol Chemical compound OC1=CC=CC=C1.C1=CC=CC=C1C1=CC=CC=C1 JRQJLSWAMYZFGP-UHFFFAOYSA-N 0.000 description 1
- IMYCVFRTNVMHAD-UHFFFAOYSA-N 1,1-bis(2-methylbutan-2-ylperoxy)cyclohexane Chemical compound CCC(C)(C)OOC1(OOC(C)(C)CC)CCCCC1 IMYCVFRTNVMHAD-UHFFFAOYSA-N 0.000 description 1
- MYWOJODOMFBVCB-UHFFFAOYSA-N 1,2,6-trimethylphenanthrene Chemical compound CC1=CC=C2C3=CC(C)=CC=C3C=CC2=C1C MYWOJODOMFBVCB-UHFFFAOYSA-N 0.000 description 1
- VHZJMAJCUAWIHV-UHFFFAOYSA-N 1-(2,4,6-trichlorophenyl)pyrrole-2,5-dione Chemical compound ClC1=CC(Cl)=CC(Cl)=C1N1C(=O)C=CC1=O VHZJMAJCUAWIHV-UHFFFAOYSA-N 0.000 description 1
- ABAMRMYDBGTLHX-UHFFFAOYSA-N 1-(2-phenylphenyl)pyrrole-2,5-dione Chemical group O=C1C=CC(=O)N1C1=CC=CC=C1C1=CC=CC=C1 ABAMRMYDBGTLHX-UHFFFAOYSA-N 0.000 description 1
- IPJGAEWUPXWFPL-UHFFFAOYSA-N 1-[3-(2,5-dioxopyrrol-1-yl)phenyl]pyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C1=CC=CC(N2C(C=CC2=O)=O)=C1 IPJGAEWUPXWFPL-UHFFFAOYSA-N 0.000 description 1
- MKRBAPNEJMFMHU-UHFFFAOYSA-N 1-benzylpyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1CC1=CC=CC=C1 MKRBAPNEJMFMHU-UHFFFAOYSA-N 0.000 description 1
- JNPCNDJVEUEFBO-UHFFFAOYSA-N 1-butylpyrrole-2,5-dione Chemical compound CCCCN1C(=O)C=CC1=O JNPCNDJVEUEFBO-UHFFFAOYSA-N 0.000 description 1
- BQTPKSBXMONSJI-UHFFFAOYSA-N 1-cyclohexylpyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C1CCCCC1 BQTPKSBXMONSJI-UHFFFAOYSA-N 0.000 description 1
- BUXKULRFRATXSI-UHFFFAOYSA-N 1-hydroxypyrrole-2,5-dione Chemical compound ON1C(=O)C=CC1=O BUXKULRFRATXSI-UHFFFAOYSA-N 0.000 description 1
- NQDOCLXQTQYUDH-UHFFFAOYSA-N 1-propan-2-ylpyrrole-2,5-dione Chemical compound CC(C)N1C(=O)C=CC1=O NQDOCLXQTQYUDH-UHFFFAOYSA-N 0.000 description 1
- FTALTLPZDVFJSS-UHFFFAOYSA-N 2-(2-ethoxyethoxy)ethyl prop-2-enoate Chemical compound CCOCCOCCOC(=O)C=C FTALTLPZDVFJSS-UHFFFAOYSA-N 0.000 description 1
- MNYLCGIJDZPKLE-UHFFFAOYSA-N 2-methylbutan-2-yloxy butaneperoxoate Chemical compound CCCC(=O)OOOC(C)(C)CC MNYLCGIJDZPKLE-UHFFFAOYSA-N 0.000 description 1
- CKITYUQKOJMMOI-UHFFFAOYSA-N 3,4-dibromo-1-methylpyrrole-2,5-dione Chemical compound CN1C(=O)C(Br)=C(Br)C1=O CKITYUQKOJMMOI-UHFFFAOYSA-N 0.000 description 1
- MECNWXGGNCJFQJ-UHFFFAOYSA-N 3-piperidin-1-ylpropane-1,2-diol Chemical compound OCC(O)CN1CCCCC1 MECNWXGGNCJFQJ-UHFFFAOYSA-N 0.000 description 1
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 1
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 1
- 125000004203 4-hydroxyphenyl group Chemical group [H]OC1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- LQZUVUANAHQVJU-UHFFFAOYSA-N 4-nonan-5-yl-1-oxidopyridin-1-ium Chemical compound CCCCC(CCCC)C1=CC=[N+]([O-])C=C1 LQZUVUANAHQVJU-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- HDFGOPSGAURCEO-UHFFFAOYSA-N N-ethylmaleimide Chemical compound CCN1C(=O)C=CC1=O HDFGOPSGAURCEO-UHFFFAOYSA-N 0.000 description 1
- 238000003848 UV Light-Curing Methods 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000004845 glycidylamine epoxy resin Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229940091173 hydantoin Drugs 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- PBOSTUDLECTMNL-UHFFFAOYSA-N lauryl acrylate Chemical compound CCCCCCCCCCCCOC(=O)C=C PBOSTUDLECTMNL-UHFFFAOYSA-N 0.000 description 1
- FEUIEHHLVZUGPB-UHFFFAOYSA-N oxolan-2-yl prop-2-enoate Chemical compound C=CC(=O)OC1CCCO1 FEUIEHHLVZUGPB-UHFFFAOYSA-N 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000010125 resin casting Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- VSJBBIJIXZVVLQ-UHFFFAOYSA-N tert-butyl 3,5,5-trimethylhexaneperoxoate Chemical compound CC(C)(C)CC(C)CC(=O)OOC(C)(C)C VSJBBIJIXZVVLQ-UHFFFAOYSA-N 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Epoxy Resins (AREA)
Abstract
The invention provides an epoxy resin electronic pouring sealant, a preparation method and application thereof, wherein the pouring sealant comprises the following components in parts by weight: 5-30 parts of epoxy resin, 5-30 parts of curing agent, 0.1-2 parts of initiator, 0.1-2 parts of accelerator, 100-200 parts of filler, 0.1-1 part of dispersing agent, 0.1-2 parts of defoamer, 0.1-2 parts of flatting agent, 0.1-2 parts of toughening agent or plasticizer, 0.1-2 parts of coupling agent and 0.1-1 part of colorant. The preparation method comprises the following steps: firstly, heating and melting solid epoxy resin into liquid, then adding filler, curing agent and auxiliary agent, uniformly stirring, and finally adding initiator and accelerator, uniformly mixing. The pouring sealant has high fluidity, low viscosity, high heat resistance, low thermal expansion coefficient and good storage stability, and is suitable for encapsulating and packaging electronic chips.
Description
Technical Field
The invention belongs to the field of application of high polymer materials, relates to pouring sealant for electronic products, and in particular relates to epoxy resin electronic pouring sealant with high fluidity, low viscosity, high heat resistance, low thermal expansion coefficient and good storage stability, and a preparation method and application thereof.
Background
With the development of electronic circuits, particularly the development of large-scale integrated circuits, electronic products have a trend of miniaturization and high integration, so that the reliability requirements for packaging electronic components in the circuits are higher and higher. In a circuit, due to certain difference of thermal expansion coefficients of the chip and the circuit substrate, the chip has unstable performance and failure in the using process, meanwhile, the chip possibly has problems in performance due to the external collision environment, and the epoxy resin has good physical and mechanical properties after being solidified, has good bonding strength, good electrical property, low shrinkage rate, high hardness and good dimensional stability, so that the thermal expansion coefficient between the chip and the substrate can be effectively reduced by taking the epoxy resin as the electronic pouring sealant, the capability of the electronic component for bearing external impact and vibration is improved, and the cost performance is good. However, the epoxy resin itself has a certain thermal expansion coefficient, and the thermal expansion coefficient is relatively large, so that a large amount of filling material, mainly silicon dioxide, needs to be added into the system in order to reduce the thermal expansion coefficient of the resin, but the addition of a large amount of filling material can increase the viscosity of the epoxy resin and deteriorate the fluidity.
At present, various types of electronic pouring sealants are available, such as a single-component COB epoxy resin electronic pouring sealant reported in a patent CN201310034841, the curing temperature is 120 ℃ for 5 minutes, the curing speed is high, the curing is about 6 months at the temperature of 2-8 ℃ of a refrigerator, but the glue sample is too fast to cure, a large amount of heat can be emitted, the curing performance of the glue sample is affected, meanwhile, the using amount of filler is about 60%, the using amount is relatively less, the viscosity is 36000-4400 mP.s, the fluidity is poor, and the operation is not facilitated. As in patent CN201410402941, a two-component epoxy resin pouring sealant is reported, the pouring sealant has a low thermal expansion coefficient and relatively good thermal conductivity, but the preparation process of the glue sample is complicated, the curing period is long, the A, B glue needs to be mixed again before use, the use is inconvenient, and the hardness of the cured glue sample is also low. As another example, patent CN200310124361 reports an electronic packaging adhesive, where a monofunctional group or a polyfunctional group of vinyl is mixed with a monofunctional group or a polyfunctional group of maleimide, and thermal or UV radiation is used to initiate curing, so that the storage stability before curing is better, but since the packaged electronic component has a certain thickness of the adhesive, when UV curing is used, the early speed is relatively fast, but UV is difficult to radiate into the adhesive to promote the adhesive to cure due to the partial curing of the adhesive in the later period, so that the curing rate and performance of the adhesive are affected.
Disclosure of Invention
The invention aims to provide an epoxy resin electronic pouring sealant which is thermally initiated and cured by thermal catalysis, a preparation method and application thereof, and the pouring sealant has high fluidity, low viscosity, high heat resistance, low thermal expansion coefficient and good storage stability, and can be used for packaging electronic chips.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows.
The epoxy resin electronic pouring sealant comprises the following components in parts by weight:
according to the scheme, the epoxy resin contains two or more epoxy groups and is a plurality of bisphenol A epoxy resin, bisphenol F epoxy resin, phenolic epoxy resin, biphenyl phenol epoxy resin, alicyclic epoxy resin, hydantoin structure epoxy resin, glycidylamine epoxy resin and multifunctional reaction type epoxy resin diluent.
Preferably, the epoxy resin is one of alicyclic epoxy resin, novolac epoxy resin, glycidylamine type epoxy resin, polyfunctional reactive epoxy resin diluent and biphenyl type epoxy resin.
Preferably, the bisphenol A type epoxy resin is NPEL-128, NPEL-128E, NPEL-128R, NPEL-128S, NPEL-144, NPEL-127, NPES-901, NPES-902, NPES-903H, NPES-904, NPES-907, NPES-909, NPES-609 of south Asia of Taiwan.
Preferably, the bisphenol F type epoxy resin is NPEL-170, NPEL-175, NPEL-176, NPEL-185, NPEL-187, NPEL-198, 806H, 807, 4004P, 4005P, 4007P, 4010P of Mitsubishi chemical in Japan, EPALOY 8220E, EPALLOY, EPALOY 8230E of CVC thermosetting specialty materials Co., USA;
preferably, the phenolic epoxy resin is NPPN-631, NPPN-638S, NPCN-701, NPCN-702, NPCN-703, NPCN-704L, EPALOY 8240E, EPALLOY 8250, EPALOY 8280, EPALOY 8330, EPALOY 8350, EPALOY 8370, EPALOY 9000 of CVC thermosetting specialty materials Co, U.S.A.;
preferably, the biphenol type epoxy resin is YX4000, YX4000H, YL6121H, YL6800 of Mitsubishi chemical in Japan, NC-3000-L, NC-3000-H, NC-3100, CER-3000-L of Japanese chemical;
preferably, the cycloaliphatic epoxy resin is CY179, CY184, CY 192, CY 5622, CY 9729, GY 257 of hencky, CELLOXIDE 2021P, CELLOXIDE 2081, CELLOXIDE 8000, EHPE 3150CE of japan;
preferably, the hydantoin epoxy resin is MHR-070 and MHR-154;
preferably, the glycidylamine type epoxy resin is MY 0500, MY 0510, MY 0600, MY 0610, MY 720, MY 721, ELM-100 and ELM-434 of Sumitomo chemistry;
preferably, the multifunctional reactive epoxy resin diluent is ERISYS GE-20, ERISYS GE-21, ERISYS GE-22, ERISYS GE-23, ERISYS GE-24, ERISYS GE-25, ERISYS GE-29, ERISYS GE-30, ERISYS GE-31, ERISYS GE-35H, ERISYS GE-36, ERISYS EGDGE, etc. of CVC thermosetting specialty materials company.
More preferably, the epoxy resin is one or more of alicyclic epoxy resin CY179, phenolic epoxy resin NPPN-638S, glycidyl amine type epoxy resin ELM-434, polyfunctional reactive epoxy resin diluent ERISYS GE-30 and biphenyl type epoxy resin NC-3100.
According to the scheme, the epoxy resin curing agent is a polymerizable monomer containing C=C double bonds and is at least one of maleimide and (methyl) acrylic ester monomers. The C=C double bond resin is selected as the curing agent, can react at medium and high temperature, and has better storage life and heat resistance.
Preferably, the maleimide has a monofunctional group or a multifunctional group, and is at least one of N-methylmaleimide (N-MMI), N-ethylmaleimide (NEM), N-phenylmaleimide (N-PMI), N-isopropylmaleimide, 2, 3-dibromomaleimide, 2, 3-dibromo-N-methylmaleimide, N-cyclohexylmaleimide, N-benzylmaleimide, N-N-butylmaleimide, N-hydroxymaleimide, N- (2, 4, 6-trichlorophenyl) maleimide, N-allylmaleimide, N, N ' -m-Phenylenedimaleimide (PDM), 4' -bis (maleimido) -1,1' -biphenyl, N- (4-hydroxyphenyl) bismaleimide, N, N- (4-methyl-1, 3-phenylene) bismaleimide, diphenylmethane Bismaleimide (BMI), N, N- (1, 4-phenylene) bismaleimide.
Preferably, the (meth) acrylic monomer is at least one of isobutyl acrylate (IBA), t-butyl acrylate (TBA), methoxyethyl acrylate (MEA), ethoxyethoxyethyl acrylate (eoea), dodecyl acrylate (LA), tetrahydrofuranyl acrylate (THFA), neopentyl glycol diacrylate (NPGDA), pentaerythritol triacrylate (PET 3A), pentaerythritol tetraacrylate (PET 4A), t-butyl methacrylate (TBMA), hydroxyethyl methacrylate (2-HEMA), hydroxypropyl methacrylate (2-HPMA), allyl Methacrylate (AMA), cyclohexyl methacrylate (CHMA), glycidyl Methacrylate (GMA), t-butyl methacrylate (TBMA).
More preferably, the curing agent is one or more of N-allylmaleimide, diphenylmethane Bismaleimide (BMI), pentaerythritol triacrylate (PET 3A), glycidyl Methacrylate (GMA).
According to the scheme, the initiator and the accelerator are stable under the medium-low temperature condition, and the rubber-like curing compound is initiated and accelerated under the high temperature condition (more than 120 ℃), so that the stability of the rubber-like can be effectively improved. Meanwhile, through the synergistic use of accelerators with different active temperatures and initiators with different thermal initiation temperatures, the copolymerization reaction of the epoxy resin and the curing agent can be gradually carried out, and a great amount of heat generated by severe reaction is avoided, so that the internal stress generated by curing is reduced, and the thermal expansion and contraction of a curing system are reduced.
Preferably, the initiator is at least two of peroxyesters, dialkyl peroxides, alkyl hydroperoxides; more preferred are at least two of 1, 1-bis (t-amyl peroxy) cyclohexane, 1-bis (t-amyl peroxy) -3, 5-trimethylcyclohexane, ethyl 3, 3-bis (t-amyl peroxy) butyrate, ethyl 3, 3-bis (t-butyl peroxy) butyrate, t-amyl peroxy-2-ethylhexanoate (TAPO), t-butyl peroxy-2-ethylhexanoate (TBPO), t-butyl peroxybenzoate (TBPB), di-t-amyl peroxide (DTAP), di-t-butyl peroxide (DTBP), dicumyl peroxide (DCP), di-t-amyl peroxide (DTAP), t-butyl peroxy3, 5-trimethylhexanoate (TBPMH/6402S), t-amyl peroxyacetate (TAPA), t-amyl peroxybenzoate (TAPB).
Preferably, the accelerator is at least two of a latent tertiary amine compound derivative, a latent organophosphorus compound derivative, a quaternary ammonium salt compound, a quaternary phosphonium salt compound, a boron trichloride amine complex, an imidazole compound and its derivative, and a transition metal compound. More preferably at least two of di-t-amyl peroxide (DTAP), di-t-butyl peroxide (DTBP), modified imidazole, boron trichloride amine complex.
According to the scheme, the filler is fused silica or spherical silica.
Preferably, the median particle size of the silica filler is from 32 to 40 μm, the volume average particle size is from 38 to 45 μm, and the maximum particle size of the filler is not more than 125 μm.
Preferably, the silica has a particle size distribution of: 9-12% of less than 125 μm and greater than or equal to 75 μm, 15-20% of less than 75 μm and greater than or equal to 45 μm, 40-60% of less than 45 μm and greater than or equal to 25 μm, 10-15% of less than 25 μm and greater than or equal to 10 μm, and 5-10% of less than 10 μm and greater than or equal to 5 μm; the percentages are percentages by volume of the total silica filler. The filler is prepared by mixing different particle sizes, so that the filler has particle grading, namely, the filler with small particle size is filled into gaps with large particle size, so that the use amount of the filler can be increased, and meanwhile, the filler is spherical and relatively good in fluidity, so that the addition of a large amount of filler can reduce the internal stress generated by solidification.
Preferably, the silica filler has a median particle diameter of 38 to 40 μm, preferably a silica filler having a mohs hardness of less than 6.
According to the scheme, the dispersing agent is a high-molecular dispersing agent, so that the grinding and dispersing performances of resin, curing agent, filler, pigment and the like in the system can be improved, different raw materials can be uniformly mixed to a certain extent, the viscosity is reduced, and the system sedimentation is prevented. Such as Efka FA 4672, efka FA 4663 of Basff, BYK-103, BYK-106, BYK-107, BYK-110, BYK-111, BYK-115, BYK-161, BYK-163, BYK-164, BYK-168, BYK-171, BYK-180, BYK-181, BYK-182, BYK-184, BYK-190, BYK-333, BYK-9076, BYK-9077, BYK-2155, BYK-220S, preferably BYK-111.
According to the scheme, the defoamer eliminates bubbles generated in the curing process of the glue sample, and particularly comprises an organosilicon defoamer, a polyether modified silicone defoamer, a polysiloxane defoamer, such as BYK-A500, BYK-A501, BYK-A515, BYK-A525, BYK-A530, BYK-A550, BYK-A555, BYK-A560, BYK-065, BYK-6N, BYK-067A, BYK-077, BYK-085, BYK-088 and BYK-1790, wherein the foam suppressor eliminates bubbles generated in the curing process of the glue sample, and the foam suppressor is an anti-foaming agent such as an Efka SI 2008, an Efka PB 2720, an Efka SL 3239, an Efka FL 3785,Efka PB 2001, a Foamaster SI 2292, an EnvirGem AD01, a Surfynol 104S, surfynol S, a Surfynol AD01, a Surfynol MD 20, BYK-022, a BYK-057, a BYK-430, a BYK-A500, a BYK-A530, a BYK-A550, a BYK-A B-A550, a BYK-A, a YK-A550, a BYK-A, an A550, a BYK-A, and BYK-A B-A550, and a YK-A550, BYK is preferably BYK is obtained.
According to the scheme, the leveling agent can improve the wettability of the glue sample, so that the glue sample can be quickly leveled in the curing process, and particularly comprises polydimethylsiloxane, polyether polyester modified organosiloxane, polyether modified polyorganosiloxane, modified hydrogenated castor oil, alkyl modified organosiloxane, such as a leveling agent Efka RM 1900,Efka RM 1920 of Basff, germany, such as leveling agents BYK-300, BYK306, BYK-307, BYK-310, BYK-320, BYK-322, BYK-323, BYK-325, BYK-331, BYK-333, BYK-344, BYK-345, BYK-346, BYK-347, BYK-348, BYK-349, BYK-354, BYK-370, BYK-371 and BYK-378, and preferably Efka RM.
According to the above scheme, the toughening agent or plasticizer is used for improving the internal stress generated in the glue-like curing process, and specifically is epoxy-terminated reactive liquid nitrile rubber, acrylonitrile modified epoxy resin, polypropylene glycol diglycidyl ether, linoleic acid dimer diglycidyl ether, epoxy modified silicone oil, and liquid silicone rubber, such as HyPox RA 95, hyPox RA 1340, hyPox RA 16213, hyPox RA 840, hyPox RA 20, hyPox RA 928, hyPox RF 1320, hyPox RF 1341, hyPox RF 928, hyPox RF 933, hyPox RM 20, hyPox RM 22, VTBN 1300X33LC, VTBN 1300X43LC,VTB 2000X168,Hypro 2000X174 ETB, hypro 1300X68 ETB, hypro 1300X63 ETB of CVC thermosetting special materials company in the United states, and preferably HyPox RA 20.
According to the scheme, the coupling agent is used for improving the compatibility between the filler, the resin and the curing agent, improving the dispersibility of the glue sample, reducing the viscosity of the glue sample, improving the adhesive strength of the glue sample, and has the general formula YSiX 3 Wherein X is generally a hydrolyzable group such as methoxy, ethoxy, methoxyethoxy, acetoxy, etc., Y is an organic functional group such as amino, vinyl, epoxy, methacryloxy, aminoethyl, ureido, etc., such as the Japanese Kogyo chemical silane coupling agents KBM-1003, KBE-903, KBM403, KBM503, KBM602, KBM603, KBM303, preferably coupling agent KBM403.
According to the above scheme, the colorant is used to adjust the color of the glue sample, and different colors such as yellow, red, blue, black, green, etc. can be selected according to different requirements, and carbon black is generally selected as the colorant to prepare a black pouring sealant, such as black MA7, MA11, MA100 of Mitsubishi chemical, NEROX 305, NEROX 500, NEROX 505, NEROX 600, NEROX 605, HIBLACK 900L, HIBLACK LB, HIBLACK 890B, HIBLACK 600L, HIBLACK LB, HIBLACK 50L, HIBLACK LB, HIBLACK 41Y, preferably HIBLACK 7.
The preparation method of the epoxy resin electronic pouring sealant comprises the following steps:
adding epoxy resin to melt at 60-80 ℃, sequentially adding filler, curing agent, dispersing agent, defoaming agent, leveling agent, toughening agent or plasticizer, coupling agent and coloring agent according to the metering, mixing and stirring for 2-3h at 25-35 ℃, then adding a certain amount of initiator and accelerator, and stirring for 20-30min at 25-30 ℃ to obtain the epoxy resin electronic pouring sealant. And finally, vacuumizing the prepared single-component epoxy resin pouring sealant, and sealing and preserving.
The resin composition can be used as an IC memory card, a chip carrier, a hybrid circuit, a chip substrate, a multi-chip module, a ball grid array, a pin grid array package, or the like.
The application of the pouring sealant in the electronic chip packaging is provided.
The beneficial effects of the invention are as follows:
1. the invention provides an epoxy resin electronic pouring sealant, which is prepared by compounding epoxy resin with high heat resistance and a curing agent containing C=C double bond, and combining accelerators with different active temperatures and initiators with different thermal initiation temperatures, and matching fillers and related auxiliary agents; the obtained pouring sealant has high fluidity, low viscosity and high T value g (150 ℃) and low thermal expansion (30-40 ppm); when the pouring sealant is used for packaging chips, the thermal expansion coefficient of the packaged chips is basically matched with that of the substrate, so that the internal stress generated by the change of external environments such as heat and the like and the internal stress generated by the heating of the chips are relieved, the chips are prevented from being damaged and invalid, and the pouring sealant has wide application prospect.
2. The filling material ratio in the electronic pouring sealant is high, and the cost can be reduced while the thermal expansion coefficient is reduced.
3. The invention provides a preparation method of epoxy resin electronic pouring sealant, which is simple to operate, mild in condition and has industrial application prospect.
Detailed Description
The invention is further illustrated by, but is not limited to, the following examples.
Example 1
The preparation method of the epoxy resin electronic pouring sealant is provided, the raw material proportion of the epoxy resin electronic pouring sealant is shown in table 1, and the preparation method comprises the following steps:
5g of phenolic epoxy resin (NPPN-638S), 6g of cycloaliphatic epoxy resin (CY 179), 7.2g of glycidylamine type epoxy resin (ELM-434), 4g of trimethylolpropane triglycidyl ether (ERISYS GE-30) were weighed into a 1L vessel, then the solid epoxy resin was melted in the liquid resin at 70℃and 144g of filler, 9.2g of diphenylmethane Bismaleimide (BMI), 7.2g N-allylmaleimide, 8g of Glycidyl Methacrylate (GMA), 5g of pentaerythritol triacrylate (PET 3A) were added, 1g of a silane coupling agent (KBM 403), 0.6g of a toughening agent (HyPox RA 20), 0.4g of a dispersing agent (BYK-111), 0.6g of a defoaming agent (Efka SL 3239), 0.4g of a leveling agent (Efka RM 1920), 0.2g of a colorant (MA 7), mixing and stirring at 30 ℃ for 3 hours by a high-speed stirrer, finally adding 0.2g of an initiator (DTAP), 0.4g of an initiator (DTBP), 0.4g of an accelerator (boron trichloride amine complex) and 0.2g of an accelerator (modified imidazole), stirring at 30 ℃ for 30min, and finally vacuumizing the prepared epoxy resin pouring sealant, and sealing and preserving.
Wherein: the particle size distribution of the filler is as follows: 9-12% of less than 125 μm and greater than or equal to 75 μm, 15-20% of less than 75 μm and greater than or equal to 45 μm, 40-60% of less than 45 μm and greater than or equal to 25 μm, 10-15% of less than 25 μm and greater than or equal to 10 μm, and 5-10% of less than 10 μm and greater than or equal to 5 μm; the percentages are percentages by volume of the total silica filler.
Examples 2 to 8
The preparation method of examples 2-8 was basically the same as that of example 1, except that the kinds and amounts of the raw materials were different, and the raw materials of examples 2-8 are shown in Table 1.
Table 1 list of starting materials for examples 1-8
The epoxy potting adhesive prepared according to examples 1 to 8 was cured at 150℃for 3 hours, and the cured samples and the samples before curing were subjected to detailed performance tests such as glass transition temperature, thermal expansion coefficient, viscosity, etc., and the test results are shown in Table 2.
TABLE 2 Performance test Table of epoxy resin casting sealants obtained in examples 1 to 8
Table 2 can be seen: the resin composition has lower viscosity, certain operability, higher glass transition temperature and low thermal expansion coefficient, and can meet the requirements of chips on packaging.
The above test data are only typical formulations or test data of the present invention and are not intended to limit the present invention, the scope of which is defined by the claims. Any person skilled in the art, within the scope of the present disclosure, may substitute or change the formulation and idea according to the present disclosure, and all fall within the scope of the present disclosure.
Claims (6)
1. The epoxy resin electronic pouring sealant is characterized by comprising the following components in parts by weight:
5-30 parts of epoxy resin
5-30 parts of curing agent
Initiator 0.1-2 parts
0.1-2 parts of promoter
100-200 parts of filler
0.1 to 1 part of macromolecular dispersing agent
0.1-2 parts of defoaming agent
0.1-2 parts of leveling agent
0.1-2 parts of toughening agent or plasticizer
0.1-2 parts of coupling agent
0.1-1 parts of a colorant; wherein:
the initiator is at least two of alkyl peroxides;
the accelerator is at least two of a latent tertiary amine compound derivative, a latent organophosphorus compound derivative, a quaternary ammonium salt compound, a quaternary phosphonium salt compound, a boron trichloride amine complex, an imidazole compound, a derivative thereof and a transition metal compound;
the epoxy resin contains two or more epoxy groups and is a plurality of bisphenol A epoxy resin, bisphenol F epoxy resin, phenolic epoxy resin, biphenol epoxy resin, alicyclic epoxy resin, hydantoin structure epoxy resin, glycidol amine epoxy resin and multifunctional group reaction type epoxy resin diluent;
the epoxy resin curing agent is at least one of maleimide and (methyl) acrylic ester monomers;
the filler is at least one of spherical silica and fused silica; the particle size distribution of the silica is: 9-12% of less than 125 [ mu ] m and greater than or equal to 75 [ mu ] m, 15-20% of less than 75 [ mu ] m and greater than or equal to 45 [ mu ] m, 40-60% of less than 45 [ mu ] m and greater than or equal to 25 [ mu ] m, 10-15% of less than 25 [ mu ] m and greater than or equal to 10 [ mu ] m, and 5-10% of less than 10 [ mu ] m and greater than or equal to 5 [ mu ] m; the percentages are percentages by volume of the total silica filler.
2. The epoxy resin electronic potting adhesive according to claim 1, wherein the epoxy resin is a plurality of alicyclic epoxy resins, novolac epoxy resins, glycidylamine type epoxy resins, polyfunctional reactive epoxy resin diluents, biphenol type epoxy resins.
3. The epoxy resin electronic potting adhesive of claim 1, wherein the epoxy resin curing agent is one or more of N-allyl maleimide, diphenylmethane bismaleimide, pentaerythritol triacrylate, and glycidyl methacrylate.
4. The epoxy resin electronic pouring sealant according to claim 1, wherein,
the defoaming agent is an organosilicon defoaming agent, a polyether modified silicon defoaming agent or high-carbon alcohol;
the leveling agent is polydimethylsiloxane, polyether polyester modified organosiloxane, polyether modified polyorganosiloxane, modified hydrogenated castor oil or alkyl modified organosiloxane;
the toughening agent or the plasticizer is epoxy-terminated reactive liquid nitrile rubber, acrylonitrile-modified epoxy resin, polypropylene glycol diglycidyl ether, linoleic acid dimer diglycidyl ether, epoxy-modified silicone oil or liquid silicone rubber;
the coupling agent is of the general formula YSiX 3 Wherein X is typically a hydrolyzable group, methoxy, ethoxy, methoxyethoxy or acetoxy, Y is an organofunctional group, and is amino, vinyl, epoxy, methacryloxy, aminoethyl or ureido.
5. A method for preparing the epoxy resin electronic pouring sealant according to any one of claims 1 to 4, which is characterized by comprising the following steps:
adding epoxy resin to melt at 60-80 ℃, sequentially adding filler, curing agent, dispersing agent, defoaming agent, leveling agent, toughening agent or plasticizer, coupling agent and coloring agent according to the metering, mixing and stirring for 2-3h at 25-35 ℃, then adding initiator and accelerator, and stirring for 20-30min at 25-30 ℃ to obtain the epoxy resin electronic pouring sealant.
6. Use of the potting adhesive of any one of claims 1-4 in electronic chip packaging.
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| CN113480958A (en) * | 2021-06-30 | 2021-10-08 | 顺德职业技术学院 | Special dual-curing epoxy adhesive for automobile camera AA (acrylic acid) manufacturing process and preparation method and application thereof |
| CN114231233A (en) * | 2021-11-22 | 2022-03-25 | 深圳先进电子材料国际创新研究院 | Low-viscosity-distribution cavity conductive adhesive and preparation method and application thereof |
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