TWI685537B - 樹脂組成物、及使用其的銅凸塊用液狀密封劑 - Google Patents
樹脂組成物、及使用其的銅凸塊用液狀密封劑 Download PDFInfo
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- TWI685537B TWI685537B TW104136159A TW104136159A TWI685537B TW I685537 B TWI685537 B TW I685537B TW 104136159 A TW104136159 A TW 104136159A TW 104136159 A TW104136159 A TW 104136159A TW I685537 B TWI685537 B TW I685537B
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- Prior art keywords
- resin composition
- filler
- silane coupling
- liquid
- coupling agent
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- 239000011342 resin composition Substances 0.000 title claims abstract description 57
- 239000007788 liquid Substances 0.000 title claims abstract description 39
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 29
- 239000010949 copper Substances 0.000 title claims abstract description 29
- 239000000565 sealant Substances 0.000 title claims abstract description 27
- 239000000945 filler Substances 0.000 claims abstract description 93
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 37
- 239000004848 polyfunctional curative Substances 0.000 claims abstract description 34
- 239000004850 liquid epoxy resins (LERs) Substances 0.000 claims abstract description 15
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- 230000008878 coupling Effects 0.000 claims description 3
- 238000010168 coupling process Methods 0.000 claims description 3
- 238000005859 coupling reaction Methods 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 3
- 238000000926 separation method Methods 0.000 abstract description 16
- 239000000203 mixture Substances 0.000 abstract description 10
- 238000013007 heat curing Methods 0.000 abstract description 7
- 239000003822 epoxy resin Substances 0.000 description 33
- 229920000647 polyepoxide Polymers 0.000 description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 24
- 239000004065 semiconductor Substances 0.000 description 21
- 239000000758 substrate Substances 0.000 description 21
- 239000000047 product Substances 0.000 description 17
- 239000004593 Epoxy Substances 0.000 description 14
- 150000001412 amines Chemical class 0.000 description 14
- 238000002347 injection Methods 0.000 description 13
- 239000007924 injection Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 12
- 239000002245 particle Substances 0.000 description 12
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- 239000011347 resin Substances 0.000 description 12
- 239000000377 silicon dioxide Substances 0.000 description 12
- -1 p-glycidoxyphenyl Chemical group 0.000 description 10
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 7
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 6
- 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 6
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
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- 238000011156 evaluation Methods 0.000 description 5
- 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 description 5
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- 229920000768 polyamine Polymers 0.000 description 4
- 229910000679 solder Inorganic materials 0.000 description 4
- 238000004381 surface treatment Methods 0.000 description 4
- PISLZQACAJMAIO-UHFFFAOYSA-N 2,4-diethyl-6-methylbenzene-1,3-diamine Chemical compound CCC1=CC(C)=C(N)C(CC)=C1N PISLZQACAJMAIO-UHFFFAOYSA-N 0.000 description 3
- CBEVWPCAHIAUOD-UHFFFAOYSA-N 4-[(4-amino-3-ethylphenyl)methyl]-2-ethylaniline Chemical compound C1=C(N)C(CC)=CC(CC=2C=C(CC)C(N)=CC=2)=C1 CBEVWPCAHIAUOD-UHFFFAOYSA-N 0.000 description 3
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- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 2
- PLIKAWJENQZMHA-UHFFFAOYSA-N 4-aminophenol Chemical compound NC1=CC=C(O)C=C1 PLIKAWJENQZMHA-UHFFFAOYSA-N 0.000 description 2
- MWSKJDNQKGCKPA-UHFFFAOYSA-N 6-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1CC(C)=CC2C(=O)OC(=O)C12 MWSKJDNQKGCKPA-UHFFFAOYSA-N 0.000 description 2
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- 239000007822 coupling agent Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 2
- 238000001962 electrophoresis Methods 0.000 description 2
- 239000008393 encapsulating agent Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
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- 125000005641 methacryl group Chemical group 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
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- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
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- MUTGBJKUEZFXGO-OLQVQODUSA-N (3as,7ar)-3a,4,5,6,7,7a-hexahydro-2-benzofuran-1,3-dione Chemical compound C1CCC[C@@H]2C(=O)OC(=O)[C@@H]21 MUTGBJKUEZFXGO-OLQVQODUSA-N 0.000 description 1
- LPVHVQFTYXQKAP-YFKPBYRVSA-N (4r)-3-formyl-2,2-dimethyl-1,3-thiazolidine-4-carboxylic acid Chemical compound CC1(C)SC[C@@H](C(O)=O)N1C=O LPVHVQFTYXQKAP-YFKPBYRVSA-N 0.000 description 1
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 description 1
- UWFRVQVNYNPBEF-UHFFFAOYSA-N 1-(2,4-dimethylphenyl)propan-1-one Chemical compound CCC(=O)C1=CC=C(C)C=C1C UWFRVQVNYNPBEF-UHFFFAOYSA-N 0.000 description 1
- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 description 1
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 1
- HGXVKAPCSIXGAK-UHFFFAOYSA-N 2,4-diethyl-6-methylbenzene-1,3-diamine;4,6-diethyl-2-methylbenzene-1,3-diamine Chemical compound CCC1=CC(CC)=C(N)C(C)=C1N.CCC1=CC(C)=C(N)C(CC)=C1N HGXVKAPCSIXGAK-UHFFFAOYSA-N 0.000 description 1
- FALRKNHUBBKYCC-UHFFFAOYSA-N 2-(chloromethyl)pyridine-3-carbonitrile Chemical class ClCC1=NC=CC=C1C#N FALRKNHUBBKYCC-UHFFFAOYSA-N 0.000 description 1
- 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 1
- HDPLHDGYGLENEI-UHFFFAOYSA-N 2-[1-(oxiran-2-ylmethoxy)propan-2-yloxymethyl]oxirane Chemical compound C1OC1COC(C)COCC1CO1 HDPLHDGYGLENEI-UHFFFAOYSA-N 0.000 description 1
- CQOZJDNCADWEKH-UHFFFAOYSA-N 2-[3,3-bis(2-hydroxyphenyl)propyl]phenol Chemical compound OC1=CC=CC=C1CCC(C=1C(=CC=CC=1)O)C1=CC=CC=C1O CQOZJDNCADWEKH-UHFFFAOYSA-N 0.000 description 1
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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 1
- CDAWCLOXVUBKRW-UHFFFAOYSA-N 2-aminophenol Chemical compound NC1=CC=CC=C1O CDAWCLOXVUBKRW-UHFFFAOYSA-N 0.000 description 1
- NFPLENSFYDCPOP-UHFFFAOYSA-N 2-methyl-6-(oxiran-2-ylmethoxycarbonyl)cyclohexane-1-carboxylic acid Chemical compound C(C1CO1)OC(C1C(C(=O)O)C(CCC1)C)=O NFPLENSFYDCPOP-UHFFFAOYSA-N 0.000 description 1
- OVEUFHOBGCSKSH-UHFFFAOYSA-N 2-methyl-n,n-bis(oxiran-2-ylmethyl)aniline Chemical compound CC1=CC=CC=C1N(CC1OC1)CC1OC1 OVEUFHOBGCSKSH-UHFFFAOYSA-N 0.000 description 1
- JZUHIOJYCPIVLQ-UHFFFAOYSA-N 2-methylpentane-1,5-diamine Chemical compound NCC(C)CCCN JZUHIOJYCPIVLQ-UHFFFAOYSA-N 0.000 description 1
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 description 1
- ZPQAUEDTKNBRNG-UHFFFAOYSA-N 2-methylprop-2-enoylsilicon Chemical compound CC(=C)C([Si])=O ZPQAUEDTKNBRNG-UHFFFAOYSA-N 0.000 description 1
- DEQUFFZCXSTYJC-UHFFFAOYSA-N 3,4-diphenylbenzene-1,2-diamine Chemical compound C=1C=CC=CC=1C1=C(N)C(N)=CC=C1C1=CC=CC=C1 DEQUFFZCXSTYJC-UHFFFAOYSA-N 0.000 description 1
- RNLHGQLZWXBQNY-UHFFFAOYSA-N 3-(aminomethyl)-3,5,5-trimethylcyclohexan-1-amine Chemical compound CC1(C)CC(N)CC(C)(CN)C1 RNLHGQLZWXBQNY-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
- 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
- GRHBJPZAZOMCTC-UHFFFAOYSA-N 4,6-diethyltriazine Chemical compound CCC1=CC(CC)=NN=N1 GRHBJPZAZOMCTC-UHFFFAOYSA-N 0.000 description 1
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- RPJFWRZEEKJTGN-UHFFFAOYSA-N 4-[2-(4-hydroxyphenyl)propan-2-yl]-2,6-dimethylphenol Chemical compound CC1=C(O)C(C)=CC(C(C)(C)C=2C=CC(O)=CC=2)=C1 RPJFWRZEEKJTGN-UHFFFAOYSA-N 0.000 description 1
- CXXSQMDHHYTRKY-UHFFFAOYSA-N 4-amino-2,3,5-tris(oxiran-2-ylmethyl)phenol Chemical compound C1=C(O)C(CC2OC2)=C(CC2OC2)C(N)=C1CC1CO1 CXXSQMDHHYTRKY-UHFFFAOYSA-N 0.000 description 1
- RMDKEBZUCHXUER-UHFFFAOYSA-N 4-methylbicyclo[2.2.1]hept-2-ene Chemical compound C1CC2C=CC1(C)C2 RMDKEBZUCHXUER-UHFFFAOYSA-N 0.000 description 1
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 description 1
- JNCKCONCDKDQIW-UHFFFAOYSA-N C1(=CC=CC=C1)C1=CC=CC=C1.CC=1C=C(C=C(C1OCC1CO1)C)C1=CC(=C(C(=C1)C)OCC1CO1)C Chemical group C1(=CC=CC=C1)C1=CC=CC=C1.CC=1C=C(C=C(C1OCC1CO1)C)C1=CC(=C(C(=C1)C)OCC1CO1)C JNCKCONCDKDQIW-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- XZAHJRZBUWYCBM-UHFFFAOYSA-N [1-(aminomethyl)cyclohexyl]methanamine Chemical compound NCC1(CN)CCCCC1 XZAHJRZBUWYCBM-UHFFFAOYSA-N 0.000 description 1
- QLBRROYTTDFLDX-UHFFFAOYSA-N [3-(aminomethyl)cyclohexyl]methanamine Chemical compound NCC1CCCC(CN)C1 QLBRROYTTDFLDX-UHFFFAOYSA-N 0.000 description 1
- FDLQZKYLHJJBHD-UHFFFAOYSA-N [3-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=CC(CN)=C1 FDLQZKYLHJJBHD-UHFFFAOYSA-N 0.000 description 1
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 description 1
- 125000002723 alicyclic group Chemical group 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 125000003342 alkenyl group Chemical group 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- IMUDHTPIFIBORV-UHFFFAOYSA-N aminoethylpiperazine Chemical compound NCCN1CCNCC1 IMUDHTPIFIBORV-UHFFFAOYSA-N 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 125000002529 biphenylenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3C12)* 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
- HGXHJQLDZPXEOG-UHFFFAOYSA-N bis(oxiran-2-ylmethyl) cyclohexane-1,4-dicarboxylate Chemical compound C1CC(C(=O)OCC2OC2)CCC1C(=O)OCC1CO1 HGXHJQLDZPXEOG-UHFFFAOYSA-N 0.000 description 1
- LMMDJMWIHPEQSJ-UHFFFAOYSA-N bis[(3-methyl-7-oxabicyclo[4.1.0]heptan-4-yl)methyl] hexanedioate Chemical compound C1C2OC2CC(C)C1COC(=O)CCCCC(=O)OCC1CC2OC2CC1C LMMDJMWIHPEQSJ-UHFFFAOYSA-N 0.000 description 1
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- 230000008602 contraction Effects 0.000 description 1
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- IFDVQVHZEKPUSC-UHFFFAOYSA-N cyclohex-3-ene-1,2-dicarboxylic acid Chemical class OC(=O)C1CCC=CC1C(O)=O IFDVQVHZEKPUSC-UHFFFAOYSA-N 0.000 description 1
- YMHQVDAATAEZLO-UHFFFAOYSA-N cyclohexane-1,1-diamine Chemical compound NC1(N)CCCCC1 YMHQVDAATAEZLO-UHFFFAOYSA-N 0.000 description 1
- VEIOBOXBGYWJIT-UHFFFAOYSA-N cyclohexane;methanol Chemical compound OC.OC.C1CCCCC1 VEIOBOXBGYWJIT-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- OTARVPUIYXHRRB-UHFFFAOYSA-N diethoxy-methyl-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](C)(OCC)CCCOCC1CO1 OTARVPUIYXHRRB-UHFFFAOYSA-N 0.000 description 1
- ZZTCPWRAHWXWCH-UHFFFAOYSA-N diphenylmethanediamine Chemical compound C=1C=CC=CC=1C(N)(N)C1=CC=CC=C1 ZZTCPWRAHWXWCH-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
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- 239000003063 flame retardant Substances 0.000 description 1
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- VANNPISTIUFMLH-UHFFFAOYSA-N glutaric anhydride Chemical class O=C1CCCC(=O)O1 VANNPISTIUFMLH-UHFFFAOYSA-N 0.000 description 1
- 239000004845 glycidylamine epoxy resin Substances 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
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
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- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 description 1
- KEZAKPHSMMMPQD-UHFFFAOYSA-N methylsulfanyl-(2-methylsulfanylphenyl)methanediamine Chemical compound CSC1=CC=CC=C1C(N)(N)SC KEZAKPHSMMMPQD-UHFFFAOYSA-N 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- ZETYUTMSJWMKNQ-UHFFFAOYSA-N n,n',n'-trimethylhexane-1,6-diamine Chemical compound CNCCCCCCN(C)C ZETYUTMSJWMKNQ-UHFFFAOYSA-N 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
- 125000001624 naphthyl group Chemical group 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000003071 parasitic effect Effects 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 125000000843 phenylene group Chemical group C1(=C(C=CC=C1)*)* 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012552 review Methods 0.000 description 1
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- 239000010703 silicon Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229940014800 succinic anhydride Drugs 0.000 description 1
- PXQLVRUNWNTZOS-UHFFFAOYSA-N sulfanyl Chemical class [SH] PXQLVRUNWNTZOS-UHFFFAOYSA-N 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- 238000005382 thermal cycling Methods 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
Classifications
-
- 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
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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Abstract
提供可抑制加熱硬化時的填充料之分離的液狀組成物、及包含該液狀組成物的可抑制在凸塊之龜裂產生的銅凸塊用液狀密封劑。
本發明的樹脂組成物,其係包含(A)液狀環氧樹脂、(B)硬化劑、及(C)以下述式(1)的矽烷偶合劑所表面處理的氧化鋁填充料。
Description
本發明為關於樹脂組成物、及使用其的銅凸塊用液狀密封劑。
隨著電子機器的小型化、輕量化、及高性能化,半導體之安裝形態亦由打線接合型變化至倒裝晶片型。
倒裝晶片型的半導體裝置,係於基板上以隔著凸塊電極來連接電極部與半導體元件。具有如此般構造的半導體裝置,在外加溫度循環等的熱負荷之際,由於環氧樹脂等的有機材料製基板與半導體元件之熱膨脹係數差,對凸塊電極會產生應力。因而在凸塊電極有產生龜裂等的不良之問題。為了抑制此不良之產生,係以使用被稱為底部填充劑(underfill)的液狀密封劑,來將半導體元件與基板之間的間隙予以密封。亦即,廣泛地進行藉由以底部填充劑來將半導體元件與基板相互固定,而使耐熱循環性得以提升。
對於作為底部填充劑所使用的液狀密封劑而
言,係要求注入性、接著性、硬化性、及保存穩定性等為優異,且不會產生空孔(void)。又,藉由液狀密封劑所密封的部位,亦要求著耐濕性、耐熱循環性、耐回流、耐龜裂性、及耐翹曲等為優異。
為了滿足上述要求,作為底部填充劑所使用的液狀密封劑方面,以環氧樹脂作為基底樹脂的底部填充劑廣為使用。
為了提升藉由液狀密封劑所密封的部位的耐濕性及耐熱循環性(特以提升耐熱循環性),係將如矽石填充料般的由無機物質所構成的填充劑(以下稱為「填充料」)添加於液狀密封劑。因此,已知可有效地控制環氧樹脂等的有機材料製基板與半導體元件之熱膨脹係數差,及補強凸塊電極,而使耐熱循環性得以提升(日本特開2007-56070號公報)。
近年,特別是在高密度的倒裝晶片安裝中,已變得使用銅柱凸塊(以下稱為「銅凸塊」)。相較於以往的焊錫凸塊,銅凸塊的優點方面,可舉例:可縮小凸塊之間距、可降低鉛之使用量(因而對環境所造成之影響為小)、高導熱性(因而放熱特性為優異)、及高導電度(因而可降低寄生電阻)等。
日本再公表特許2010-103934號公報中揭示著使用銅凸塊與底部填充劑的以往的倒裝晶片安裝程序之一例。依專利文獻2之揭示,以該程序使用銅柱來進行倒裝晶片安裝時,底部填充劑中的填充料於加熱硬化中會有自樹脂分
離之情形。該情形時,底部填充劑樹脂中會形成填充料為不存在之區域。其結果,由於無法吸收矽晶片與基板之線膨脹率之差,而造成在凸塊會產生龜裂等之問題之情形。
〔專利文獻1〕日本特開2007-56070號公報
〔專利文獻2〕日本再公表特許2010-103934號公報
為了解決上述以往技術中的問題點,本發明之目的之一為提供可抑制加熱硬化時的填充料之分離的樹脂組成物。又,本發明之其他目的為提供使用該組成物而成的可抑制在凸塊之龜裂產生的銅凸塊用液狀密封劑。
本案發明人們對於使用於銅凸塊用液狀密封劑的樹脂組成物深入研究檢討有關在加熱硬化時的填充料之分離。其結果得到下述般的見解。
即,有關底部填充劑的填充料,若使用在作為底部填充劑的填充料為廣為使用的矽石填充料時,容易引起加熱硬化時的填充料之分離。相較於矽石填充料,氧化鋁填充料則不易引起加熱硬化時的填充料之分離。
關於上述見解,本案發明人之推測如下。
在銅柱與焊錫接合之際,由於兩者的電位差之影響,使得底部填充劑在加熱硬化中填充料會受到電泳作用而被吸引至銅柱。其結果推測因而引起填充料之分離。
如上述般,就所謂抑制加熱硬化時的填充料之分離之點而言,相較於矽石填充料,氧化鋁填充料為佳。然而,相較於含有矽石填充料的底部填充劑,含有氧化鋁填充料的底部填充劑在對於半導體元件與基板之間之間隙之注入性為差。該理由係由於氧化鋁填充料容易受到吸濕之影響,因吸濕而引起氧化鋁填充料之凝聚之故。
本發明為有鑑於上述見解所完成之發明。藉由本發明,可提供一種樹脂組成物,其係包含(A)液狀環氧樹脂、(B)硬化劑、及(C)以下述式(1)的矽烷偶合劑所表面處理的氧化鋁填充料。
本發明的樹脂組成物亦可進而含有(D)矽烷偶合劑。
本發明的樹脂組成物,前述(C)以矽烷偶合所表面處理的氧化鋁填充料的含有量,相對於樹脂組成物的全成分的合計質量100質量份,較佳為45~77質量份。
又,本發明為提供使用本發明的樹脂組成物而成的液狀密封劑。
又,本發明為提供使用本發明的樹脂組成物而成的銅凸塊用液狀密封劑。
將本發明的樹脂組成物使用作為銅凸塊用液狀密封劑時,對於該半導體元件與基板之間之間隙之注入性為良好。又,可抑制上述密封材的加熱硬化時的填充料之分離、及抑制因而在凸塊之龜裂之產生。
以下對於本發明實施形態的樹脂組成物進行詳細說明。
本發明實施形態的樹脂組成物,係至少含有下述所示的(A)~(C)成分。
(A)液狀環氧樹脂
(A)成分的液狀環氧樹脂,係相當於本發明實施形態的樹脂組成物的基底樹脂的成分。
在本發明實施形態中,所謂的液狀環氧樹脂,係意味著常溫下為液狀的環氧樹脂。
作為本發明實施形態的液狀環氧樹脂之例,舉例如:具有約400以下的平均分子量的雙酚A型環氧樹脂;如對-縮水甘油氧基苯基二甲基參雙酚A二縮水甘油醚之分支
狀多官能基雙酚A型環氧樹脂;雙酚F型環氧樹脂;具有約570以下的平均分子量的酚酚醛清漆型環氧樹脂;如乙烯基(3,4-環己烯)二氧化物、3,4-環氧基環己基羧酸(3,4-環氧基環己基)甲酯、己二酸雙(3,4-環氧基-6-甲基環己基甲基)酯、及2-(3,4-環氧基環己基)5,1-螺(3,4-環氧基環己基)-間-二噁烷之脂環式環氧樹脂;如3,3’,5,5’-四甲基-4,4’-二縮水甘油氧基聯苯之聯苯型環氧樹脂;如六氫苯二甲酸二縮水甘油酯、3-甲基六氫苯二甲酸二縮水甘油酯、及六氫對苯二甲酸二縮水甘油酯之縮水甘油酯型環氧樹脂;如二縮水甘油基苯胺、二縮水甘油基甲苯胺、三縮水甘油基-對-胺基苯酚、四縮水甘油基-間-二甲苯二胺、及四縮水甘油基雙(胺基甲基)環己烷之縮水甘油基胺型環氧樹脂;1,3-二縮水甘油基-5-甲基-5-乙基乙內醯脲之乙內醯脲型環氧樹脂;以及含有萘環之環氧樹脂。又亦可使用如1,3-雙(3-縮水甘油氧基丙基)-1,1,3,3-四甲基二矽氧烷之具有聚矽氧骨架之環氧樹脂。再者,亦可使用如(聚)乙二醇二縮水甘油醚、(聚)丙二醇二縮水甘油醚、丁二醇二縮水甘油醚、新戊二醇二縮水甘油醚、及環己烷二甲醇二縮水甘油醚之二環氧化合物;如三羥甲基丙烷三縮水甘油醚、甘油三縮水甘油醚之三環氧化合物等。
該等液狀環氧樹脂之中,較佳可使用液狀雙酚型環氧樹脂、液狀胺基苯酚型環氧樹脂、聚矽氧變性環氧樹脂、及萘型環氧樹脂。更佳可使用液狀雙酚A型環氧樹脂、液
狀雙酚F型環氧樹脂、對-胺基苯酚型液狀環氧樹脂、及1,3-雙(3-縮水甘油氧基丙基)四甲基二矽氧烷。
作為(A)成分,可使用該等液狀環氧樹脂之中的單獨1種,或亦可併用2種以上。
又,即使是常溫下為固體的環氧樹脂,藉由與液狀的環氧樹脂之併用以作為混合物而展現出液狀時,亦可使用此環氧樹脂。
(B)硬化劑
(B)成分的硬化劑未特別限定。亦可使用包含環氧樹脂的任何習知的硬化劑。可使用例如胺系硬化劑、酸酐系硬化劑、及酚系硬化劑之中之任一者。
作為胺系硬化劑之具體例,舉例如三伸乙四胺、四伸乙五胺、間-苯二甲胺、三甲基六亞甲基二胺、及2-甲基五亞甲基二胺等的脂肪族聚胺、異佛爾酮二胺、1,3-雙胺基甲基環己烷、雙(4-胺基環己基)甲烷、降冰片烯二胺、及1,2-二胺基環己烷等的脂環式聚胺、N-胺基乙基哌嗪、及1,4-雙(2-胺基-2-甲基丙基)哌嗪等的哌嗪型聚胺、二乙基甲苯二胺、二甲基硫代甲苯二胺、4,4’-二胺基-3,3’-二乙基二苯基甲烷、雙(甲硫基)甲苯二胺、二胺基二苯基甲烷、間-苯二胺、二胺基二苯基碸、二乙基甲苯二胺、三亞甲基雙(4-胺基苯甲酸酯)、及聚氧化四亞甲基-二-對-胺基苯甲酸酯等的芳香族聚胺類。
又,作為被市售的胺系硬化劑之例,舉例如T-12
(商品名、三洋化成工業製)(胺當量116)。
作為酸酐系硬化劑之具體例,舉例如甲基四氫鄰苯二甲酸酐、甲基六氫鄰苯二甲酸酐、及甲基四氫鄰苯二甲酸酐等的烷基化四氫鄰苯二甲酸酐、六氫鄰苯二甲酸酐、甲基降冰片烯二酸酐、烯基取代的琥珀酸酐、甲基納迪克酸酐、戊二酸酐等。
酚系硬化劑之具體例,係包含具有酚羥基的單體、低聚物、聚合物的全部。作為更具體之例,舉例如酚酚醛清漆樹脂及其烷基化物或烯丙基化物、甲酚酚醛清漆樹脂、苯酚芳烷基(包含伸苯基、伸聯苯基骨架)樹脂、萘酚芳烷基樹脂、三酚基甲烷樹脂、及雙環戊二烯型苯酚樹脂。
該等中,就耐濕性及耐熱循環性為優異之點而言,較佳為使用胺系硬化劑。其中,就耐熱性、機械性特性、密著性、電氣特性、及耐濕性之觀點而言,較佳為使用二乙基甲苯二胺、二甲基硫代甲苯二胺、及4,4’-二胺基-3,3’-二乙基二苯基甲烷。又,就常溫下為呈現液狀之點而言,作為本發明實施形態的樹脂組成物中的環氧樹脂的硬化劑,亦以使用胺系硬化劑為較佳。
作為(B)成分的硬化劑,可使用該等硬化劑之中的單獨1種,或亦可併用2種以上。
本發明實施形態的樹脂組成物中,(B)成分的硬化劑的調配比例未特別限定。例如,相對於(A)成分的液狀環氧樹脂的環氧基1當量,(B)成分的調配比
例較佳為0.5~1.6當量,特佳為0.6~1.3當量。
(C)以下述式(1)的矽烷偶合劑所表面處理的氧化鋁填充料
(C)成分的氧化鋁填充料,係以提升密封部位的耐濕性及耐熱循環性(特以耐熱循環性)為目的而添加者。之所以藉由添加氧化鋁填充料而可提升耐熱循環性,係藉由降低線膨脹係數,而可抑制因熱循環所造成的密封劑組成物的硬化物之膨脹及收縮之故。
作為(C)成分為使用氧化鋁填充料,係由於如下述之理由。即,如上述般,相較於矽石填充料,氧化鋁填充料具有高的等電位點。因而,將氧化鋁填充料使用於銅凸塊用液狀密封劑時,填充料為維持正電位。因此,氧化鋁填充料在加熱硬化中不會受到電泳之作用,故不易引起填充料之分離。該結果可抑制在凸塊之龜裂之產生。
然而,如上述般,相較於含有矽石填充料的液狀密封劑,含有氧化鋁填充料的液狀密封劑在對於半導體元件與基板之間之間隙之注入性為差。本發明實施形態中作為(C)成分,係藉由使用以上述式(1)的矽烷偶合劑所表面處理的氧化鋁填充料,可改善氧化鋁填充料之對於半導體元件與基板之間之間隙之注入性。之所以藉由使用以上述式(1)的矽烷偶合劑所表面處理的氧化鋁填充
料而可改善氧化鋁填充料之對於半導體元件與基板之間之間隙之注入性,係由於如下述之理由。即,藉由以上述式(1)的矽烷偶合劑予以表面處理,會提升氧化鋁填充料的耐吸濕性。因而可防止氧化鋁填充料之凝聚。
相對於此,若以上述式(1)以外的矽烷偶合劑來表面處理時,會引起起因為矽烷偶合劑的氧化鋁填充料之凝聚。因此,以上述(1)的矽烷偶合劑的表面處理,對用來防止氧化鋁填充料之凝聚為有效之方法。即,使用以上述(1)的矽烷偶合劑所表面處理的氧化鋁填充料而成的樹脂組成物,藉由使用該樹脂組成物時可改善對於半導體元件與基板之間之間隙之注入性。
本發明實施形態的樹脂組成物中,相對於樹脂組成物的全成分的合計質量100質量份,(C)成分的以矽烷偶合所表面處理的氧化鋁填充料的含有量較佳為45~77質量份。
當(C)成分的氧化鋁填充料的含有量未滿45質量份時,樹脂組成物的線膨脹係數會變大。因此,使用於銅凸塊用液狀密封劑時,密封部位的耐熱循環性會降低。
另一方面,當(C)成分的氧化鋁填充料的含有量超過77質量份時,樹脂組成物的黏度會增加。因此,使用於銅凸塊用液狀密封劑時,對於半導體元件與基板之間之間隙之注入性會降低。
(C)成分的氧化鋁填充料的含有量,又較佳為50~75質量份,更佳為50~70質量份。
本發明實施形態的樹脂組成物中,(C)成分的氧化鋁填充料的平均粒徑,就樹脂組成物的良好流動性之觀點而言,較佳為0.1~10μm。
(C)成分的氧化鋁填充料的平均粒徑,又較佳為0.5~5μm,更佳為0.7~1.7μm。
(C)成分的氧化鋁填充料的形狀未特別限定。該形狀可為粒狀、粉末狀、及鱗片等的任意形態。尚,氧化鋁填充料的形狀為粒狀以外時,所謂氧化鋁的平均粒徑,係意味著氧化鋁填充料的最大徑之平均。
本發明實施形態的樹脂組成物,除了上述(A)~(C)成分以外,可因應所需含有下述成分。
(D):矽烷偶合劑
本發明實施形態的樹脂組成物,為了提升在作為銅凸塊用液狀密封劑使用之際的密著性,亦可含有作為(D)成分的矽烷偶合劑。
(D)成分的矽烷偶合劑,不限定於使用於氧化鋁填充料的表面處理的上述式(1)的矽烷偶合劑((C)成分)。作為如此般的矽烷偶合劑之例,可使用環氧系、胺基系、乙烯基系、甲基丙烯醯基系、丙烯醯基系、及巰基系等的各種矽烷偶合劑。該等中,就作為銅凸塊用液狀密封劑使用之際的提升密著性及機械性強度之效果為優異之點而言,較佳為使用環氧系矽烷偶合劑。
作為環氧系矽烷偶合劑的具體例,舉例如3-
環氧丙氧基丙基三甲氧基矽烷、2-(3,4-環氧環己基)乙基三甲氧基矽烷(商品名:KBM-303、信越化學(股)公司製)、3-環氧丙氧基丙基甲基二甲氧基矽烷(商品名:KBM-402、信越化學(股)公司製)、3-環氧丙氧基丙基三甲氧基矽烷(商品名:KBM-403、信越化學(股)公司製)、3-環氧丙氧基丙基甲基二乙氧基矽烷(商品名:KBE-402、信越化學(股)公司製)、及3-環氧丙氧基丙基三乙氧基矽烷(商品名:KBE-403、信越化學(股)公司製)等。
作為(D)成分的矽烷偶合劑的含有量,相對於樹脂組成物的全成分的合計質量100質量份,較佳為0.01~5質量份,又較佳為0.05~3質量份,更佳為0.1~1質量份。
(其他的調配劑)
本發明實施形態的樹脂組成物,可因應所需進而含有上述(A)~(D)成分以外的成分。作為如此般的可調配成分的具體例,可舉例如彈性體、硬化促進劑、金屬錯合體、平整劑、著色劑、離子補集劑、消泡劑、及難燃劑。各調配劑的種類及調配量可參照常法來決定。
(樹脂組成物之調製)
本發明實施形態的樹脂組成物係將上述(A)~(C)成分、及進而含有時的(D)成分,以及因應所需進而調
配的其他的調配劑混合、攪拌而製成的。
混合攪拌可使用輥磨機來進行。當然,混合攪拌之方法並不限定於此。當(A)成分的環氧樹脂為固形時,較佳為混合藉由加熱等而成的液狀化或流動化的環氧樹脂。
同時混合各成分時,適當改變該混合方法亦無妨。例如,可事先混合一部份的成分,剩餘的成分之後再混合即可。難以使(C)成分的氧化鋁填充料對於(A)成分的液狀環氧樹脂均勻分散時,可事先將(A)成分的液狀環氧樹脂與(C)成分的氧化鋁填充料混合後,再混合剩餘的成分。
接著,對於本發明實施形態的樹脂組成物的特性加以說明。
本發明實施形態的樹脂組成物,可使用旋轉黏度計並以50rpm、25℃之條件來進行測定。該黏度較佳為200Pa.s以下。當黏度為此範圍時,在作為銅凸塊用液狀密封劑使用之際,樹脂組成物可展現出良好的流動性。
本發明實施形態的樹脂組成物在50rpm、25℃的黏度較佳為100Pa.s以下。
又,本發明實施形態的樹脂組成物,在作為銅凸塊用液狀密封劑使用時,展現出良好的對於半導體元件與基板之間之間隙之注入性。具體而言,以後述實施例中所記載的程序來評估對於間隙之注入性時,注入時間為1200秒以下。
又,將本發明實施形態的樹脂組成物使用作
為銅凸塊用液狀密封劑時,可抑制加熱硬化時的氧化鋁填充料之分離。具體而言,以後述實施例中所記載的程序來評估填充料分離指數時,可得到50以上(特以55以上)的填充料分離指數。
接著,將本發明實施形態的樹脂組成物的使用方法,以舉例作為銅凸塊用液狀密封劑之使用來進行說明。
將本發明實施形態的樹脂組成物作為銅凸塊用液狀密封劑使用時,本發明實施形態的樹脂組成物為依下述程序而填充至基板與半導體元件之間之間隙。
一邊將基板加熱至例如70~130℃,一邊將本發明實施形態的樹脂組成物塗布至半導體元件的一端,藉由毛細管現象來使本發明實施形態的樹脂組成物填充至基板與半導體元件之間之間隙。此時,為了縮短填充本發明實施形態的樹脂組成物所需之時間,亦可使基板傾斜,或使該間隙內外產生壓力差。
將本發明實施形態的樹脂組成物填充至該間隙後,以指定溫度、指定時間加熱該基板,具體而言為以80~200℃加熱0.2~6小時,藉此來使樹脂組成物加熱硬化。因而藉此可使該間隙被密封。
以下藉由實施例詳細說明本發明的實施形態。但本發明實施形態的實施形態並不受限於下述該等實
施例。
(實施例1~16、比較例1~5)
將以下述表中表示之比例所調配的原料,以藉由使用輥磨機來將原料進行混練,而調製成使用於實施例1~16、及比較例1~5的液狀密封劑。但是係以事先混合(A)成分的液狀環氧樹脂與(C)成分的氧化鋁填充料後,再混合剩餘的成分。尚,表中各組成相關之數值,係以質量份來表示。
(A)環氧樹脂
環氧樹脂A1:雙酚F型環氧樹脂、製品名YDF8170、新日鐵化學(股)製、環氧當量158g/eq
環氧樹脂A2:雙酚A型環氧樹脂、製品名850CRP、DIC(股)製、環氧當量170~175g/eq
環氧樹脂A3:萘型環氧樹脂、製品名4032D、DIC(股)製、環氧當量136~148g/eq
環氧樹脂A4:多官能型環氧樹脂、製品名630、三菱化學(股)製、環氧當量90~105g/eq
(B)硬化劑
硬化劑B1:胺系硬化劑、4,4’-二胺基-3,3’-二乙基二苯基甲烷、製品名Kayahard A-A、日本化藥(股)製
硬化劑B2:胺系硬化劑、二甲基硫代甲苯二胺(包
含變性芳香族胺)、製品名EH105L、(股)ADEKA製
硬化劑B3:胺系硬化劑、二乙基三烯二胺、製品名ETHACURE 100、ALBEMARLE JAPAN(股)製
硬化劑B4:酸酐系硬化劑、製品名YH307、三菱化學(股)製
硬化劑B5:酚系硬化劑、製品名MEH-8005、明和化成(股)製
(C)填充料
填充料C1:以下述式(1)的矽烷偶合劑(製品名KBM573(信越化學工業(股)製)所表面處理的氧化鋁填充料(平均粒徑0.7μm)
填充料C2:以式(1)的矽烷偶合劑(製品名KBM573(信越化學工業(股)製)所表面處理的氧化鋁填充料(平均粒徑1.7μm)
填充料C3:表面未處理的矽石填充料(平均粒徑0.7μm)
填充料C4:表面未處理的氧化鋁填充料(平均粒徑0.7μm)
填充料C5:以環氧系矽烷偶合劑(3-環氧丙氧基丙基三甲氧基矽烷)、製品名KBM403(信越化學工業
(股)製))所表面處理的氧化鋁填充料(平均粒徑0.7μm)
填充料C6:以甲基丙烯醯基系矽烷偶合劑(3-甲基丙烯醯氧基丙基三乙氧基矽烷)、製品名KBM503(信越化學工業(股)製))所表面處理的氧化鋁填充料(平均粒徑0.7μm)
填充料C7:以胺基系矽烷偶合劑(3-胺基丙基三甲氧基矽烷)、製品名KBM903(信越化學工業(股)製))所表面處理的氧化鋁填充料(平均粒徑0.7μm)
(D)矽烷偶合劑
矽石偶合劑D1:環氧系矽烷偶合劑(3-環氧丙氧基丙基三甲氧基矽烷)、製品名KBM403(信越化學工業(股)製)
矽石偶合劑D2:式(1)的矽烷偶合劑(製品名KBM573(信越化學工業(股)製)
(E)硬化促進劑
硬化促進劑E1:2-乙基-4-甲基咪唑、製品名2P4MZ、四國化成工業(股)製
使用已調製的樹脂組成物來作為評估用試樣,以實施下述的評估。
(填充料分離指數)
將以上述程序調製而成的樹脂組成物注入於具有銅凸
塊的配線基板、與半導體元件之間之間隙(50μm)。之後,將已注入的樹脂組成物以150℃、2小時來加熱硬化。使用掃瞄型電子顯微鏡(SEM)攝影樹脂硬化物的剖面照片。將該攝影畫像藉由畫像處理軟體,並以下述般藉由電腦來進行分析。即,指定該攝影畫像中的樹脂組成物之區域。接著,將經指定的區域的輝度分布之中央值作為基準,將畫像予以二值化處理。在此,經二值化的畫像之中,白色部分表示為填充料,黑色部分表示為填充料以外的樹脂成分。其次,將經指定的區域以沿著銅柱與焊錫之邊界線L,區畫成為銅柱側區域Ra、及焊錫側區域Rb的二區域。然後,依據銅柱側區域Ra、及焊錫側區域Rb的各畫像分別算出矽石填充料的佔有率。分離指數為藉由下述式所算出。
分離指數=100×(區域Ra之佔有率)/(區域Rb之佔有率)
(黏度)
使用布氏黏度計以液溫25℃、50rpm來測定調製後不久的評估用試樣之黏度。
(搖變性指數(T.I.))
使用布氏公司製旋轉黏度計HBDV-1(使用spindle SC4-14)來測定以5rpm、25℃時的黏度(Pa.s)、及以50rpm、25℃時的黏度(Pa.s)。然後,將以5rpm所測定
的黏度的測定值除以以50rpm所測定的黏度的測定值,將所得的值(以5rpm之黏度對以50rpm之黏度之比)以作為搖變性指數算出。
(注入性)
於有機基板(FR-4基板)上設置50μm的間隙,以玻璃板取代半導體元件來進行固定,藉此以製作試片。將該試片放置於設定為110℃的加熱板上。然後,將樹脂組成物塗布至該玻璃板之一端側,之後測定該組成物在間隙內的注入距離為達到20mm為止之時間。實施該程序2次,將測定值之平均值以注入時間之測定值予以算出。
實施例1~16的樹脂組成物,填充料分離指數、以液溫25℃、50rpm測定的黏度、搖變性指數(T.I.)、20mm注入性的評估結果皆為良好。實施例1與實施例2~16之差異處如同下述。
實施例2:使用平均粒徑為相異的氧化鋁填充料(平均粒徑1.7μm)。
實施例3~5:氧化鋁填充料的含有量與實施例1為相異(相對於全成分的合計質量100質量份,為45質量份(實施例3)、70質量份(實施例4)、75質量份(實施例5))。
實施例6、7:使用含有成分(D)(矽烷偶合劑)的(環氧系矽烷偶合劑(3-環氧丙氧基丙基三甲氧基矽烷)(實施例6);使用與用於氧化鋁填充料的表面處理的矽烷偶合劑為相同的矽烷偶合劑(實施例7)。
實施例8、9:硬化劑當量比與實施例1為相異(硬化劑當量比:0.5(實施例8)、1.8(實施例9))。
實施例10~12:成分(A)的環氧樹脂之種類與實施例1為相異(雙酚F型環氧樹脂(環氧當量170~175g/eq)(實施例10)、萘型環氧樹脂(環氧當量136~148g/eq)(實施例11)、多官能型環氧樹脂(環氧當量90~105g/eq)(實施例12)。
實施例13、14:成分(B)的胺系硬化劑之種類與實施例1為相異(二甲基硫代甲苯二胺(包含變性芳香族胺)(實施例13)、二乙基三烯二胺(實施例14)。
實施例15:使用酸酐系硬化劑作為成分(B)。
實施例16:使用酚系硬化劑作為成分(B)。
另一方面,作為(C)成分,使用表面未處理的矽石填充料而成的比較例1,填充料分離指數之數值為低,確認到加熱硬化時的填充料之分離。
又,作為(C)成分,使用表面未處理的氧化鋁填充料而成的比較例2、使用以環氧系矽烷偶合劑(3-環氧丙氧基丙基三甲氧基矽烷)所表面處理的氧化鋁填充料而成的比較例3、使用以甲基丙烯醯基系矽烷偶合劑(3-甲基丙烯醯氧基丙基三乙氧基矽烷)所表面處理的氧化鋁填充料而成的比較例4、使用以胺基系矽烷偶合劑(3-胺基丙基三甲氧基矽烷)所表面處理的氧化鋁填充料而成的比較例5,在注入性評估之際,樹脂組成物無法注入至蓋內(無法注入)。
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