CN103890088A - Resin composition - Google Patents
Resin composition Download PDFInfo
- Publication number
- CN103890088A CN103890088A CN201280052315.XA CN201280052315A CN103890088A CN 103890088 A CN103890088 A CN 103890088A CN 201280052315 A CN201280052315 A CN 201280052315A CN 103890088 A CN103890088 A CN 103890088A
- Authority
- CN
- China
- Prior art keywords
- resin combination
- strain
- resin
- epoxy resin
- filling material
- 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.)
- Granted
Links
- 239000011342 resin composition Substances 0.000 title abstract description 4
- 239000003822 epoxy resin Substances 0.000 claims abstract description 88
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 88
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 59
- 150000002894 organic compounds Chemical class 0.000 claims abstract description 28
- 229920005989 resin Polymers 0.000 claims description 132
- 239000011347 resin Substances 0.000 claims description 132
- -1 methacryloyl Chemical group 0.000 claims description 73
- 239000000463 material Substances 0.000 claims description 63
- 238000011049 filling Methods 0.000 claims description 49
- 239000004020 conductor Substances 0.000 claims description 35
- 239000004065 semiconductor Substances 0.000 claims description 34
- 238000009413 insulation Methods 0.000 claims description 33
- 229910052799 carbon Inorganic materials 0.000 claims description 32
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 30
- 239000004593 Epoxy Substances 0.000 claims description 21
- 125000003545 alkoxy group Chemical group 0.000 claims description 19
- 238000009835 boiling Methods 0.000 claims description 19
- 150000001875 compounds Chemical class 0.000 claims description 19
- 239000007822 coupling agent Substances 0.000 claims description 18
- 238000004381 surface treatment Methods 0.000 claims description 18
- 238000007747 plating Methods 0.000 claims description 15
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 14
- 125000004432 carbon atom Chemical group C* 0.000 claims description 13
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 12
- 125000003700 epoxy group Chemical group 0.000 claims description 11
- 125000001118 alkylidene group Chemical group 0.000 claims description 10
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 9
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 8
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 8
- 125000000962 organic group Chemical group 0.000 claims description 6
- 125000000843 phenylene group Chemical group C1(=C(C=CC=C1)*)* 0.000 claims description 6
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 6
- 125000000217 alkyl group Chemical group 0.000 claims description 5
- 239000002648 laminated material Substances 0.000 claims description 5
- 150000001398 aluminium Chemical class 0.000 claims description 4
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 claims description 4
- 150000004693 imidazolium salts Chemical class 0.000 claims description 4
- 150000003608 titanium Chemical class 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 4
- 229920002554 vinyl polymer Polymers 0.000 claims description 4
- 150000003754 zirconium Chemical class 0.000 claims description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 3
- 238000007788 roughening Methods 0.000 abstract description 10
- 239000011256 inorganic filler Substances 0.000 abstract 2
- 229910003475 inorganic filler Inorganic materials 0.000 abstract 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 71
- 239000010408 film Substances 0.000 description 70
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 56
- 238000000034 method Methods 0.000 description 54
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 51
- 239000002966 varnish Substances 0.000 description 50
- 238000004519 manufacturing process Methods 0.000 description 47
- 239000000126 substance Substances 0.000 description 37
- 239000000377 silicon dioxide Substances 0.000 description 34
- 239000000758 substrate Substances 0.000 description 34
- 235000012239 silicon dioxide Nutrition 0.000 description 32
- 239000002245 particle Substances 0.000 description 31
- 229960001866 silicon dioxide Drugs 0.000 description 31
- 229920001971 elastomer Polymers 0.000 description 29
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Natural products OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 23
- 238000001723 curing Methods 0.000 description 23
- 238000003756 stirring Methods 0.000 description 23
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 22
- 150000002148 esters Chemical class 0.000 description 21
- 239000000243 solution Substances 0.000 description 20
- 239000003054 catalyst Substances 0.000 description 19
- 238000003475 lamination Methods 0.000 description 18
- 238000005507 spraying Methods 0.000 description 18
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 16
- 238000002360 preparation method Methods 0.000 description 16
- 101000905241 Mus musculus Heart- and neural crest derivatives-expressed protein 1 Proteins 0.000 description 15
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 15
- 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 15
- LRHPLDYGYMQRHN-UHFFFAOYSA-N n-Butanol Substances CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 15
- 229910052726 zirconium Inorganic materials 0.000 description 15
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 14
- 239000000203 mixture Substances 0.000 description 14
- 239000003960 organic solvent Substances 0.000 description 14
- 238000009434 installation Methods 0.000 description 13
- 229920003986 novolac Polymers 0.000 description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 150000002357 guanidines Chemical class 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 12
- 239000002184 metal Substances 0.000 description 12
- 239000011812 mixed powder Substances 0.000 description 12
- 238000012545 processing Methods 0.000 description 11
- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 description 10
- 239000007787 solid Substances 0.000 description 10
- 239000002904 solvent Substances 0.000 description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 9
- 229910052802 copper Inorganic materials 0.000 description 9
- 239000010949 copper Substances 0.000 description 9
- 238000009826 distribution Methods 0.000 description 9
- 239000003063 flame retardant Substances 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- KJCVRFUGPWSIIH-UHFFFAOYSA-N 1-naphthol Chemical compound C1=CC=C2C(O)=CC=CC2=C1 KJCVRFUGPWSIIH-UHFFFAOYSA-N 0.000 description 8
- 239000002253 acid Substances 0.000 description 8
- 239000004305 biphenyl Substances 0.000 description 8
- 235000010290 biphenyl Nutrition 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 230000002787 reinforcement Effects 0.000 description 8
- 229920005992 thermoplastic resin Polymers 0.000 description 8
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 7
- KAKZBPTYRLMSJV-UHFFFAOYSA-N butadiene group Chemical group C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 7
- 238000000576 coating method Methods 0.000 description 7
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical group C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 6
- XNIOWJUQPMKCIJ-UHFFFAOYSA-N 2-(benzylamino)ethanol Chemical compound OCCNCC1=CC=CC=C1 XNIOWJUQPMKCIJ-UHFFFAOYSA-N 0.000 description 6
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical compound CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 239000004411 aluminium Substances 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-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
- 230000008859 change Effects 0.000 description 6
- 239000004643 cyanate ester Substances 0.000 description 6
- 238000007772 electroless plating Methods 0.000 description 6
- 239000012530 fluid Substances 0.000 description 6
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 6
- 235000013824 polyphenols Nutrition 0.000 description 6
- 239000004800 polyvinyl chloride Substances 0.000 description 6
- 229920000915 polyvinyl chloride Polymers 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 230000001681 protective effect Effects 0.000 description 6
- IZSHZLKNFQAAKX-UHFFFAOYSA-N 5-cyclopenta-2,4-dien-1-ylcyclopenta-1,3-diene Chemical group C1=CC=CC1C1C=CC=C1 IZSHZLKNFQAAKX-UHFFFAOYSA-N 0.000 description 5
- 229930185605 Bisphenol Natural products 0.000 description 5
- 229940106691 bisphenol a Drugs 0.000 description 5
- 230000006837 decompression Effects 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 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 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 4
- 150000008065 acid anhydrides Chemical class 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 125000003118 aryl group Chemical group 0.000 description 4
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 4
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 4
- 238000007598 dipping method Methods 0.000 description 4
- 238000005553 drilling Methods 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- 229940079593 drug Drugs 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005530 etching Methods 0.000 description 4
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 description 4
- 150000002460 imidazoles Chemical class 0.000 description 4
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 4
- 239000004922 lacquer Substances 0.000 description 4
- 238000010030 laminating Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 229920006287 phenoxy resin Polymers 0.000 description 4
- 239000013034 phenoxy resin Substances 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical class [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- KMOUUZVZFBCRAM-OLQVQODUSA-N (3as,7ar)-3a,4,7,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1C=CC[C@@H]2C(=O)OC(=O)[C@@H]21 KMOUUZVZFBCRAM-OLQVQODUSA-N 0.000 description 3
- 150000004954 1-(2-hydroxyethyl)-imidazoles Chemical class 0.000 description 3
- AIDLAEPHWROGFI-UHFFFAOYSA-N 2-methylbenzene-1,3-dicarboxylic acid Chemical compound CC1=C(C(O)=O)C=CC=C1C(O)=O AIDLAEPHWROGFI-UHFFFAOYSA-N 0.000 description 3
- BDCLDNALSPBWPQ-UHFFFAOYSA-N 3-oxohexanoic acid Chemical group CCCC(=O)CC(O)=O BDCLDNALSPBWPQ-UHFFFAOYSA-N 0.000 description 3
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 229920002799 BoPET Polymers 0.000 description 3
- KVDCIJNSDWIFOO-UHFFFAOYSA-N CCC(C1=CC=CC=C1)(O)O.N#CO.N#CO Chemical compound CCC(C1=CC=CC=C1)(O)O.N#CO.N#CO KVDCIJNSDWIFOO-UHFFFAOYSA-N 0.000 description 3
- GAWIXWVDTYZWAW-UHFFFAOYSA-N C[CH]O Chemical group C[CH]O GAWIXWVDTYZWAW-UHFFFAOYSA-N 0.000 description 3
- 239000005977 Ethylene Substances 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- CTKINSOISVBQLD-UHFFFAOYSA-N Glycidol Chemical compound OCC1CO1 CTKINSOISVBQLD-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- UMHKOAYRTRADAT-UHFFFAOYSA-N [hydroxy(octoxy)phosphoryl] octyl hydrogen phosphate Chemical compound CCCCCCCCOP(O)(=O)OP(O)(=O)OCCCCCCCC UMHKOAYRTRADAT-UHFFFAOYSA-N 0.000 description 3
- 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 3
- 230000006978 adaptation Effects 0.000 description 3
- 239000002390 adhesive tape Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 239000011889 copper foil Substances 0.000 description 3
- 238000007607 die coating method Methods 0.000 description 3
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 238000005227 gel permeation chromatography Methods 0.000 description 3
- 238000009998 heat setting Methods 0.000 description 3
- 125000005842 heteroatom Chemical group 0.000 description 3
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 3
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 229920002120 photoresistant polymer Polymers 0.000 description 3
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 3
- 229920000139 polyethylene terephthalate Polymers 0.000 description 3
- 239000005020 polyethylene terephthalate Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- CYIDZMCFTVVTJO-UHFFFAOYSA-N pyromellitic acid Chemical compound OC(=O)C1=CC(C(O)=O)=C(C(O)=O)C=C1C(O)=O CYIDZMCFTVVTJO-UHFFFAOYSA-N 0.000 description 3
- 229910000679 solder Inorganic materials 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- HYZQBNDRDQEWAN-LNTINUHCSA-N (z)-4-hydroxypent-3-en-2-one;manganese(3+) Chemical compound [Mn+3].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O HYZQBNDRDQEWAN-LNTINUHCSA-N 0.000 description 2
- GIWQSPITLQVMSG-UHFFFAOYSA-N 1,2-dimethylimidazole Chemical compound CC1=NC=CN1C GIWQSPITLQVMSG-UHFFFAOYSA-N 0.000 description 2
- MNAHQWDCXOHBHK-UHFFFAOYSA-N 1-phenylpropane-1,1-diol Chemical compound CCC(O)(O)C1=CC=CC=C1 MNAHQWDCXOHBHK-UHFFFAOYSA-N 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- JWAZRIHNYRIHIV-UHFFFAOYSA-N 2-naphthol Chemical compound C1=CC=CC2=CC(O)=CC=C21 JWAZRIHNYRIHIV-UHFFFAOYSA-N 0.000 description 2
- ZCUJYXPAKHMBAZ-UHFFFAOYSA-N 2-phenyl-1h-imidazole Chemical compound C1=CNC(C=2C=CC=CC=2)=N1 ZCUJYXPAKHMBAZ-UHFFFAOYSA-N 0.000 description 2
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 101001031591 Mus musculus Heart- and neural crest derivatives-expressed protein 2 Proteins 0.000 description 2
- OPKOKAMJFNKNAS-UHFFFAOYSA-N N-methylethanolamine Chemical compound CNCCO OPKOKAMJFNKNAS-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- MCEBKLYUUDGVMD-UHFFFAOYSA-N [SiH3]S(=O)=O Chemical class [SiH3]S(=O)=O MCEBKLYUUDGVMD-UHFFFAOYSA-N 0.000 description 2
- MHRNQQUEUYMEEH-UHFFFAOYSA-N [[[ethyl(dimethyl)silyl]amino]-dimethylsilyl]ethane Chemical compound CC[Si](C)(C)N[Si](C)(C)CC MHRNQQUEUYMEEH-UHFFFAOYSA-N 0.000 description 2
- YFONAHAKNVIHPT-UHFFFAOYSA-N [methyl-[[methyl(diphenyl)silyl]amino]-phenylsilyl]benzene Chemical compound C=1C=CC=CC=1[Si](C=1C=CC=CC=1)(C)N[Si](C)(C=1C=CC=CC=1)C1=CC=CC=C1 YFONAHAKNVIHPT-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 2
- 229920000800 acrylic rubber Polymers 0.000 description 2
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- 238000000790 scattering method Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- WSFQLUVWDKCYSW-UHFFFAOYSA-M sodium;2-hydroxy-3-morpholin-4-ylpropane-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)CC(O)CN1CCOCC1 WSFQLUVWDKCYSW-UHFFFAOYSA-M 0.000 description 1
- 241000894007 species Species 0.000 description 1
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 235000012222 talc Nutrition 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 125000006158 tetracarboxylic acid group Chemical group 0.000 description 1
- 238000001029 thermal curing Methods 0.000 description 1
- AYEKOFBPNLCAJY-UHFFFAOYSA-O thiamine pyrophosphate Chemical compound CC1=C(CCOP(O)(=O)OP(O)(O)=O)SC=[N+]1CC1=CN=C(C)N=C1N AYEKOFBPNLCAJY-UHFFFAOYSA-O 0.000 description 1
- 150000003557 thiazoles Chemical class 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- XDKMXYYPKSWJNR-UHFFFAOYSA-N thiocyanic acid;triphenylphosphane Chemical compound SC#N.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 XDKMXYYPKSWJNR-UHFFFAOYSA-N 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- QWWIMOOFEDJKFN-UHFFFAOYSA-N titanium;dihydrate Chemical compound O.O.[Ti] QWWIMOOFEDJKFN-UHFFFAOYSA-N 0.000 description 1
- JIVZKJJQOZQXQB-UHFFFAOYSA-N tolazoline Chemical compound C=1C=CC=CC=1CC1=NCCN1 JIVZKJJQOZQXQB-UHFFFAOYSA-N 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 125000005270 trialkylamine group Chemical group 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 1
- BWPNIANVWARHPR-UHFFFAOYSA-N tridecyl dihydrogen phosphite Chemical compound CCCCCCCCCCCCCOP(O)O BWPNIANVWARHPR-UHFFFAOYSA-N 0.000 description 1
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 description 1
- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical compound OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 description 1
- FIQMHBFVRAXMOP-UHFFFAOYSA-N triphenylphosphane oxide Chemical compound C=1C=CC=CC=1P(C=1C=CC=CC=1)(=O)C1=CC=CC=C1 FIQMHBFVRAXMOP-UHFFFAOYSA-N 0.000 description 1
- 229960004418 trolamine Drugs 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 125000002256 xylenyl group Chemical class C1(C(C=CC=C1)C)(C)* 0.000 description 1
- CHJMFFKHPHCQIJ-UHFFFAOYSA-L zinc;octanoate Chemical compound [Zn+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O CHJMFFKHPHCQIJ-UHFFFAOYSA-L 0.000 description 1
- NHXVNEDMKGDNPR-UHFFFAOYSA-N zinc;pentane-2,4-dione Chemical compound [Zn+2].CC(=O)[CH-]C(C)=O.CC(=O)[CH-]C(C)=O NHXVNEDMKGDNPR-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
-
- 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
- H01L21/56—Encapsulations, e.g. encapsulation layers, coatings
- H01L21/568—Temporary substrate used as encapsulation process aid
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/46—Manufacturing multilayer circuits
- H05K3/4644—Manufacturing multilayer circuits by building the multilayer layer by layer, i.e. build-up multilayer circuits
- H05K3/4652—Adding a circuit layer by laminating a metal foil or a preformed metal foil pattern
- H05K3/4655—Adding a circuit layer by laminating a metal foil or a preformed metal foil pattern by using a laminate characterized by the insulating layer
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
- H01L2924/0001—Technical content checked by a classifier
- H01L2924/0002—Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/03—Use of materials for the substrate
- H05K1/0313—Organic insulating material
- H05K1/0353—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement
- H05K1/0373—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement containing additives, e.g. fillers
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
- H05K2201/02—Fillers; Particles; Fibers; Reinforcement materials
- H05K2201/0203—Fillers and particles
- H05K2201/0206—Materials
- H05K2201/0209—Inorganic, non-metallic particles
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
A resin composition, containing an epoxy resin (A), a curing agent (B), and an inorganic filler (C), and characterized by the inorganic filler being surface treated using a specified organic compound. This resin composition: has a low arithmetic average roughness and root-mean-square roughness on an insulating layer surface in a wet roughening step; is capable of forming a plated conductive layer having sufficient peel strength on the insulating layer; and has PCT resistance.
Description
Technical field
The present invention relates to resin combination.Further relate to the adhering film, prepreg, multilayer printed circuit board, the semiconductor device that contain this resin combination.
Background technology
In recent years, miniaturization, the high performance of e-machine are developed, and in multilayer printed circuit board, stacking (build up) layer multi-layer, requires miniaturization and the densification of distribution.
This is carried out to various effort.For example, the resin combination that contains organosilicon alcoxyl base oligopolymer is disclosed in patent documentation 1.Wherein record the insulating material being formed by these compositions and can possess cementability.In addition, in patent documentation 2～4, carried out general cooperation research.But its performance is not necessarily met.
Prior art document
Patent documentation
[patent documentation 1] TOHKEMY 2006-117826 communique
No. 4674730th, [patent documentation 2] Japanese Patent
No. 4686750th, [patent documentation 3] Japanese Patent
No. 4782870th, [patent documentation 4] Japanese Patent.
Summary of the invention
The problem that invention will solve
The problem that the present invention will solve is to provide a kind of resin combination, wherein, in wet type roughening operation, arithmetic average roughness, the r.m.s. roughness of surface of insulating layer are little, can form the plated conductor layer with sufficient stripping strength thereon, also there is PCT (Pressure Cooker Test, pressure cooker testing) patience.
Solve the means that problem is used
The inventor etc. conduct in-depth research in order to solve above-mentioned problem, found that a kind of resin combination, it contains (A) epoxy resin, (B) solidifying agent, (C) inorganic filling material, it is characterized in that, above-mentioned inorganic filling material is carried out to surface treatment with specific organic compound, completed thus the present invention.
, the present invention includes following content:
[1] resin combination, it is the resin combination that contains (A) epoxy resin, (B) solidifying agent, (C) inorganic filling material, it is characterized in that, in this resin combination, be that 100 DEG C of above organic compound carry out surface treatment by above-mentioned inorganic filling material with thering is hydroxyl and reactive group and boiling point;
[2] according to the resin combination above-mentioned [1] Suo Shu, it is characterized in that, the reactive group of above-mentioned organic compound is the a kind of above reactive group being selected from amino, epoxy group(ing), sulfydryl, methacryloyl, acryl, vinyl and urea groups;
[3] according to the resin combination above-mentioned [1] Suo Shu, it is characterized in that, above-mentioned organic compound is a kind of above organic compound in compound, imidazolium compounds and the imidazoles-epoxy adduct of compound, following formula (3) of the compound that is selected from following formula (1), following formula (2)
[changing 1]
R1, R2 are the alkyl of phenyl, benzyl, hydrogen atom or carbonatoms 1～5 respectively independently; R3 is alkylidene group or the phenylene of carbonatoms 1～5,
[changing 2]
R4 is alkylidene group or the phenylene of carbonatoms 1～5,
[changing 3]
R5 is the organic group with hydroxyl; R6 is hydrogen atom, methyl, carboxyl or phenyl;
[4] according to the resin combination described in any one in above-mentioned [1]～[3], it is characterized in that, when (C) inorganic filling material is made as to 100 quality %, above-mentioned organic compound is 0.05～2 quality %;
[5] according to the resin combination described in any one in above-mentioned [1]～[4], it is characterized in that, after (C) inorganic filling material is carried out to surface treatment with above-mentioned organic compound, further carry out above surface treatment with a kind that is selected from silane coupling agent, organoalkoxysilane, alkoxyl group oligopolymer, aluminium class coupling agent, titanium class coupling agent and zirconium class coupling agent;
[6] according to the resin combination described in any one in above-mentioned [1]～[5], it is characterized in that, on the surface of (C) inorganic filling material, the carbon amount of the per unit area of combination is 0.05～1.00mg/m
2;
[7] according to the resin combination described in any one in above-mentioned [1]～[6], it is characterized in that, resin combination is solidified to form to insulation layer, this surface of insulating layer is carried out to roughened, carry out plating and obtain conductor layer, the stripping strength of this conductor layer and insulation layer is 0.4kgf/cm～1.5kgf/cm, and resin combination is solidified to form to insulation layer, the arithmetic average roughness that this surface of insulating layer is carried out after roughened is 10nm～300nm, and r.m.s. roughness is 10nm～480nm;
[8] sheet laminated material, is characterized in that, contains the resin combination described in any one in above-mentioned [1]～[7];
[9] multilayer printed circuit board, wherein, has formed insulation layer by the cured article of the resin combination described in any one in above-mentioned [1]～[7];
[10] semiconductor device, is characterized in that, uses above-mentioned [9] described multilayer printed circuit board.
Invention effect
In the resin combination that contains (A) epoxy resin, (B) solidifying agent, (C) inorganic filling material, above-mentioned inorganic filling material is carried out to surface treatment with specific organic compound, there is the resin combination of above-mentioned feature by use, thereby the arithmetic average roughness, the r.m.s. roughness that can be provided in surface of insulating layer in wet type roughening operation are little, can form the plated conductor layer with sufficient stripping strength thereon, also there is the resin combination of PCT patience.
Embodiment
The present invention is a kind of resin combination, it is the resin combination that contains (A) epoxy resin, (B) solidifying agent, (C) inorganic filling material, it is characterized in that, in this resin combination, be that 100 DEG C of above organic compound carry out surface treatment by above-mentioned inorganic filling material with thering is hydroxyl and reactive group and boiling point.
< (A) epoxy resin >
As the epoxy resin using in the present invention, there is no particular limitation, can enumerate: bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol-s epoxy resin, bisphenol AF type epoxy resin, line style phenol aldehyde type epoxy resin, the tertiary butyl-catechu phenol-type epoxy resin, naphthol type epoxy resin, naphthalene type epoxy resin, naphthylidene ether type epoxy, glycidyl amine type epoxy resin, cresoform type epoxy resin, biphenyl type epoxy resin, anthracene type epoxy resin, wire aliphatic epoxy resin, there is the epoxy resin of butadiene structure, alicyclic epoxy resin, hetero ring type epoxy resin, containing whorled epoxy resin, cyclohexanedimethanol type epoxy resin, trishydroxymethyl type epoxy resin, halogenated epoxy resin etc.These epoxy resin can use a kind or two or more is used in combination.
Wherein, from the viewpoint consideration that improves thermotolerance, improves the adaptation of insulating reliability, raising and tinsel, preferably bisphenol A type epoxy resin, naphthol type epoxy resin, naphthalene type epoxy resin, biphenyl type epoxy resin, naphthylidene ether type epoxy, anthracene type epoxy resin, there is the epoxy resin of butadiene structure.Particularly, for example can enumerate: bisphenol A type epoxy resin (Mitsubishi Chemical's (strain) system " エ ピ コ ー ト 828EL ", " YL980 "), bisphenol f type epoxy resin (Mitsubishi Chemical's (strain) system " jER806H ", " YL983U "), (DIC (strain) makes " HP4032 " to naphthalene type 2 officials' energy epoxy resin, " HP4032D ", " HP4032SS ", " EXA4032SS "), (DIC (strain) makes " HP4700 " to naphthalene type 4 officials' energy epoxy resin, " HP4710 "), naphthol type epoxy resin (Dongdu changes into (strain) system " ESN-475V "), there is the epoxy resin (ダ イ セ Le chemical industry (strain) system " PB-3600 ") of butadiene structure, there is epoxy resin (Japanese chemical drug (strain) system " NC3000H " of biphenyl structural, " NC3000L ", " NC3100 ", Mitsubishi Chemical's (strain) system " YX4000 ", " YX4000H ", " YX4000HK ", " YL6121 "), anthracene type epoxy resin (Mitsubishi Chemical's (strain) system " YX8800 "), (DIC (strain) makes " EXA-7310 " to naphthylidene ether type epoxy, " EXA-7311 ", " EXA-7311L ", " EXA7311-G3 ") etc.
Can be used together two or more epoxy resin, but preferably comprise the epoxy resin in 1 molecule with more than 2 epoxy group(ing).Wherein, more preferably comprise in 1 molecule, there is more than 2 epoxy group(ing), at 20 DEG C of temperature for liquid aromatic series based epoxy resin is (hereinafter referred to as " liquid-state epoxy resin ".) and 1 molecule in there is more than 3 epoxy group(ing), at 20 DEG C of temperature for solid-state aromatic series based epoxy resin is (hereinafter referred to as " solid epoxy resin ".) form.Should illustrate, in the present invention, said aromatic series based epoxy resin refers to the epoxy resin in its molecule with aromatic ring structure.As epoxy resin, and in situation with liquid-state epoxy resin and solid epoxy resin, the cured article when resin combination is used with adhering film form with suitable flexible aspect and resin combination has suitable breaking tenacity aspect and considers, its mixing ratio (liquid-state epoxy resin: solid epoxy resin) is preferably the scope of 1: 0.1～1: 2 by quality ratio, the scope of more preferably 1: 0.3～1: 1.8, the scope of more preferably 1: 0.6～1: 1.5.
As liquid-state epoxy resin, preferably bisphenol A type epoxy resin, bisphenol f type epoxy resin, line style phenol aldehyde type epoxy resin or naphthalene type epoxy resin, more preferably naphthalene type epoxy resin.They can use a kind or combine two or more use.
As solid epoxy resin, preferably 4 officials' energy naphthalene type epoxy resin, cresoform type epoxy resin, dicyclopentadiene-type epoxy resin, trisphenol epoxy resin, naphthol novolac epoxy resin (naphthol novolac expoxy resin), biphenyl type epoxy resin or naphthylidene ether type epoxy, more preferably 4 officials' energy naphthalene type epoxy resin, biphenyl type epoxy resin or naphthylidene ether type epoxy.They can use a kind or two or more is used in combination.
In resin combination of the present invention, consider from the mechanical Strong degree of cured article and the viewpoint of water tolerance that improve resin combination, when nonvolatile component in resin combination is made as to 100 quality %, the content of epoxy resin is preferably 3～40 quality %, more preferably 5～35 quality %, more preferably 10～30 quality %.
< (B) solidifying agent >
As the solidifying agent using in the present invention, have no particular limits, can enumerate phenol solidifying agent, aphthols solidifying agent, active ester class solidifying agent, benzo oxazinyl solidifying agent, cyanate solidifying agent, acid anhydride type curing agent etc., wherein preferred phenol solidifying agent, aphthols solidifying agent, active ester class solidifying agent.They can use a kind or two or more is used in combination.
As phenol solidifying agent, aphthols solidifying agent, have no particular limits, can enumerate have phenolic varnish (novolac) structure phenol solidifying agent, there is the aphthols solidifying agent of phenolic varnish structure, preferably lacquer resins, the lacquer resins that contains triazine skeleton, naphthol novolac resin, naphthols aralkyl-type resin, the naphthol resin that contains triazine skeleton, biphenyl aralkyl-type phenol resin.As commercially available product, as biphenyl aralkyl-type phenol resin, can enumerate " MEH-7700 ", " MEH-7810 ", " MEH-7851 ", " MEH7851-4H " (bright and change into (strain) system), " GPH " (Japanese chemical drug (strain) system); As naphthol novolac resin, can enumerate " NHN ", " CBN " (Japanese chemical drug (strain) system); As naphthols aralkyl-type resin, can enumerate " SN170 ", " SN180 ", " SN190 ", " SN475 ", " SN485 ", " SN495 ", " SN395 ", " SN375 " (Dongdu changes into (strain) system); As lacquer resins, can enumerate " TD2090 " (DIC (strain) system); As the lacquer resins that contains triazine skeleton, can enumerate " LA3018 ", " LA7052 ", " LA7054 ", " LA1356 " (DIC (strain) system) etc.They can use a kind or two or more is used in combination.
As active ester class solidifying agent, have no particular limits, conventionally preferably use phenol ester class, thiophenol ester class, N-oxyamine ester class, heterocycle hydroxyl compound ester class etc., in 1 molecule, there is the compound of the ester group that more than 2 reactive behavior is high.This active ester class solidifying agent preferably obtains by the condensation reaction of carboxylic acid cpd and/or thiocarboxylic acid compound and oxy-compound and/or mercaptan compound.Especially consider the active ester class solidifying agent preferably being obtained by carboxylic acid cpd and oxy-compound, the active ester class solidifying agent more preferably being obtained by carboxylic acid cpd and oxybenzene compound and/or naphthol compound from improving stable on heating viewpoint.As carboxylic acid cpd, for example, can enumerate: phenylformic acid, acetic acid, succsinic acid, toxilic acid, methylene-succinic acid, phthalic acid, m-phthalic acid, terephthalic acid, pyromellitic acid etc.As oxybenzene compound or naphthol compound, for example can enumerate: quinhydrones, Resorcinol, dihydroxyphenyl propane, Bisphenol F, bisphenol S, phenolphthalin, the dihydroxyphenyl propane that methylates, the Bisphenol F that methylates, the bisphenol S that methylates, phenol, ortho-cresol, meta-cresol, p-cresol, catechol, naphthyl alcohol, 2-Naphthol, 1,5-dihydroxy naphthlene, 1,6-dihydroxy naphthlene, 2,6-dihydroxy naphthlene, dihydroxy benaophenonel, trihydroxybenzophenone, tetrahydroxybenzophenone, Phloroglucinol, benzenetriol, dicyclopentadienyl xenol, novolak (phenol novolac) etc.Active ester class solidifying agent can use one kind or two or more.As active ester class solidifying agent, can use disclosed active ester class solidifying agent in TOHKEMY 2004-277460 communique, also can use commercially available active ester class solidifying agent.As commercially available active ester class solidifying agent; preferably contain the active ester class solidifying agent of dicyclopentadienyl xenol structure, acetylate, the benzoylate of novolak etc. of novolak, wherein more preferably contain the active ester class solidifying agent of dicyclopentadienyl xenol structure.Particularly, as the active ester class solidifying agent that contains dicyclopentadienyl xenol structure, can enumerate EXB9451, EXB9460, EXB9460S-65T, HPC-8000-65T (DIC (strain) system, active group equivalent approximately 223), as the acetylate of novolak, can enumerate DC808 (Mitsubishi Chemical's (strain) system, active group equivalent approximately 149), as the benzoylate of novolak, can enumerate YLH1026 (Mitsubishi Chemical's (strain) system, active group equivalent approximately 200), YLH1030 (Mitsubishi Chemical's (strain) system, active group equivalent approximately 201), YLH1048 (Mitsubishi Chemical's (strain) system, active group equivalent approximately 245) etc., wherein from the storage stability of varnish, the viewpoint of the thermal expansivity of cured article is considered, preferably HPC-8000-65T.
As the active ester class solidifying agent that contains dicyclopentadienyl xenol structure, more specifically can enumerate the compound of following formula (4).
[chemical formula 4]
(in formula, R is phenyl, naphthyl, k represent 0 or 1, n on average count 0.05～2.5 with repeating unit.)
Consider from the viewpoint that makes dielectric loss tangent reduce, make thermotolerance to improve, R is preferably naphthyl, and on the other hand, k is preferably 0, and n is preferably 0.25～1.5.
As benzo oxazinyl solidifying agent, have no particular limits, can enumerate F-a, P-d (four countries change into (strain) system), HFB2006M (clear and polymer (strain) system) etc. as concrete example.
As cyanate solidifying agent, have no particular limits, can enumerate phenolic varnish type (ノ ボ ラ ッ Network type) (novolac-type, alkyl novolac-type etc.) cyanate solidifying agent, dicyclopentadiene-type cyanate solidifying agent, bisphenol type (bisphenol A-type, Bisphenol F type, bisphenol S type etc.) cyanate solidifying agent and their part and carry out prepolymer of triazine etc.The weight-average molecular weight of cyanate solidifying agent, has no particular limits, and is preferably 500～4500, and more preferably 600～3000.As the concrete example of cyanate solidifying agent, for example can enumerate: dihydroxyphenyl propane dicyanate, polyphenol cyanate (few (3-methylene radical-1, 5-phenylene cyanate), 4, 4'-methylene-bis (2, 6-3,5-dimethylphenyl cyanate), 4, 4'-ethylene phenyl dicyanate, hexafluoro bisphenol-a dicyanate, 2, two (4-cyanate) phenyl-propanes of 2-, 1, 1-two (4-cyanate phenylmethane), two (4-cyanate-3, 5-3,5-dimethylphenyl) methane, 1, two (4-cyanate phenyl-1-(methyl the ethylidene)) benzene of 3-, two (4-cyanate phenyl) thioether, 2 officials' energy cyanate ester resins such as two (4-cyanate phenyl) ether, by novolak, cresoform varnish (cresol novolac), the derivative multifunctional cyanate ester resins such as the resol that contains Dicyclopentadiene (DCPD) structure, a part for these cyanate ester resins has been carried out the prepolymer of triazine etc.They can use one kind or two or more being used in combination.As commercially available cyanate ester resin, can enumerate: novolac-type multifunctional cyanate ester resin (ロ Application ザ ジ ャ パ Application (strain) system that following formula (5) represents, PT30, cyanate equivalent 124), part or all of the dihydroxyphenyl propane dicyanate that following formula (6) represents carried out triazine and changed into as trimerical prepolymer (ロ Application ザ ジ ャ パ Application (strain) system, BA230, cyanate equivalent 232), the cyanate ester resin that contains Dicyclopentadiene (DCPD) structure (ロ Application ザ ジ ャ パ Application (strain) system that following formula (7) represents, DT-4000, DT-7000) etc.
[chemical formula 5]
[in formula, n represents to count arbitrarily (preferably 0～20) as mean value.]。
[chemical formula 6]
。
[chemical formula 7]
(in formula, n represents 0～5 number as mean value.)。
As acid anhydride type curing agent, have no particular limits, can enumerate: Tetra hydro Phthalic anhydride, Tetra Hydro Phthalic Anhydride, hexahydrophthalic anhydride, methyl tetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, methyl Na Dike (nadic) acid anhydrides, hydrogenation methyl carbic anhydride, trialkyl Tetra Hydro Phthalic Anhydride, dodecenyl succinic anhydride, 5-(2,5-dioxo tetrahydrochysene-3-furyl (Off ラ ニ Le))-3-methyl-3-tetrahydrobenzene-1,2-dicarboxylic anhydride, trimellitic acid 1,2-anhydride, pyromellitic acid acid anhydride, benzophenone tetracarboxylic dianhydride, biphenyl tetracarboxylic dianhydride, naphthalene tetracarboxylic acid dianhydride, hydroxyl two O-phthalic acid dianhydrides, 3,3'-4,4'-sulfobenzide tetracarboxylic dianhydride, 1,3,3a, 4,5,9b-, six hydrogen-5-(tetrahydrochysene-2,5-dioxo-3-furyl)-naphtho-[1,2-C] furans-1,3-diketone, ethylene glycol bis (trimellitate acid anhydride) (エ チ レ Application グ リ コ ー Le PVC ス (ア Application ヒ De ロ ト リ メ リ テ ー ト)), vinylbenzene and maleic acid copolymerized acid anhydrides that closes the polymer-types such as the styrene-maleic acid resin that forms etc.
In resin combination of the present invention, consider from the mechanical Strong degree of cured article and the viewpoint of water tolerance that improve resin combination, (A) sum of the epoxy group(ing) of epoxy resin be preferably 1: 0.2 with (B) ratio of the sum of the reactive group of solidifying agent～1: 2, more preferably 1: 0.3～1: 1.5, more preferably 1: 0.4～1: 1.Should illustrate, the sum of the epoxy group(ing) of the epoxy resin existing in resin combination refers to, for whole epoxy resin, by the solids component quality with each epoxy resin divided by the value of epoxy equivalent (weight) gained amounts to value; The sum of the reactive group of solidifying agent refers to, for whole solidifying agent, by the solids component quality with each solidifying agent divided by the value of reactive group equivalent gained amounts to value.
In resin combination of the present invention, consider from the mechanical Strong degree of cured article and the viewpoint of water tolerance that improve resin combination, when nonvolatile component in resin combination is made as to 100 quality %, the content of solidifying agent is preferably 3～30 quality %, more preferably 5～25 quality %, more preferably 7～20 quality %.
< (C) inorganic filling material >
As (C) inorganic filling material using in the present invention, have no particular limits, for example, can enumerate: silicon-dioxide, aluminum oxide, barium sulfate, talcum, clay, mica powder, aluminium hydroxide, magnesium hydroxide, calcium carbonate, magnesiumcarbonate, magnesium oxide, boron nitride, aluminum borate, barium titanate, strontium titanate, calcium titanate, magnesium titanate, bismuth titanates, titanium oxide, barium zirconate, calcium zirconate etc.Wherein, preferred silicon-dioxide.The silicon-dioxide such as preferred soft silica, pulverizing silicon-dioxide, fused silica, crystalline silica, synthetic silica, hollow silica, more preferably fused silica.As silicon-dioxide, preferably spherical silicon-dioxide.They can use a kind or two or more to be used in combination.As commercially available spheroidal fused silicon-dioxide, can enumerate: (strain) ア De マ テ ッ Network ス system " SOC2 ", " SOC1 ".
The median size of inorganic filling material has no particular limits, but from carrying out at insulation layer the angle consideration of the formation of fine distribution, be preferably below 5 μ m, more preferably below 3 μ m, more preferably, below 1 μ m, be further preferably below 0.7 μ m, be especially preferably below 0.5 μ m, be particularly preferably below 0.4 μ m, be more particularly preferably below 0.3 μ m.On the other hand, from in the time that composition epoxy resin is formed as to resinous varnish, the angle that viscosity raises, operability reduces that prevents varnish is considered, more than the median size of inorganic filling material is preferably 0.01 μ m, more preferably more than 0.03 μ m, more preferably more than 0.05 μ m, more than being especially preferably 0.07 μ m, more than being particularly preferably 0.1 μ m.The median size of above-mentioned inorganic filling material can be measured by the laser diffraction-scattering method based on Michaelis (Mie) scattering theory.Particularly, can use laser diffraction and scattering formula particle size distribution device to make the size-grade distribution of inorganic filling material with volume reference, its median particle diameter is measured as median size.Working sample can preferably use the sample that utilizes ultrasonic wave that inorganic filling material is dispersed in water to form.As laser diffraction formula particle size distribution device, can use (strain) hole field to make made LA-500,750,950 etc.
When nonvolatile component in resin combination is made as to 100 quality %, consider from the viewpoint that the thermal expansivity of cured article is reduced, more than content while coordinating inorganic filling material is preferably 20 quality %, more preferably more than 30 quality %, more preferably more than 40 quality %, more than being further preferably 50 quality %.From improve cured article mechanical characteristics viewpoint consider, be preferably below 85 quality %, more preferably, below 80 quality %, more preferably, below 75 quality %, be further preferably below 70 quality %.
From the dispersiveness of resinous varnish improve, the viewpoint of the reduction of the reduction of arithmetic average roughness, r.m.s. roughness considers, (C) inorganic filling material can use in advance and carry out surface-treated inorganic filling material with silicon nitrogen silane compound.After having carried out surface treatment with silicon nitrogen silane compound, be that 100 DEG C of above organic compound carry out surface treatment with thering is hydroxyl and reactive group and boiling point, improve in dispersiveness thus, and the affinity raising of conductor layer aspect become favourable.As silicon nitrogen silane compound, for example can enumerate: hexamethyldisilazane, 1, 3-divinyl-1, 1, 3, 3-tetramethyl-disilazane, prestox three silazane, six (tertiary butyl) disilazane, six butyl disilazanes, six octyl group disilazanes, 1, 3-diethyl tetramethyl-disilazane, 1, 3-di-n-octyl tetramethyl-disilazane, 1, 3-phenylbenzene tetramethyl-disilazane, 1, 3-dimethyl tetraphenyl disilazane, 1, 3-diethyl tetramethyl-disilazane, 1, 1, 3, 3-tetraphenyl-1, 3-dimethyl disilazane, 1, 3-dipropyl tetramethyl-disilazane, pregnancy basic ring three silazane, hexaphenyl disilazane, dimethylamino trimethyl silicane azane, three silazane, encircle three silazane, 1, 1, 3, 3, 5, 5-pregnancy basic ring three silazane etc., particularly preferably hexamethyldisilazane.They can use a kind or two or more to be used in combination.As carried out surface-treated spheroidal fused silicon-dioxide with hexamethyldisilazane, can enumerate (strain) ア De マ テ ッ Network ス system " SC2050-SQ ".
In the present invention, use, to have hydroxyl and reactive group and boiling point be 100 DEG C of above organic compound, thereby hydroxyl and the coating fully of inorganic filling material covalent attachment make the dispersiveness raising of reactive group in resin combination.Because boiling point is more than 100 DEG C, thereby can make the water being produced by dehydrating condensation evaporate on one side, stably carry out the surface treatment of this organic compound on one side.The preferred upper limit value of boiling point is 500 DEG C, more preferably 400 DEG C, and further preferably 300 DEG C.Should illustrate, in the present invention, " boiling point " of organic compound refers to the boiling point under standard pressure (0.101325MPa).As this organic compound, have no particular limits, the reactive group of this organic compound be preferably be selected from amino, epoxy group(ing), sulfydryl, methacryloyl, acryl, vinyl, urea groups more than a kind, more preferably amino, epoxy group(ing).This organic compound is not preferably in fact containing the element being selected from silicon, aluminium, titanium, zirconium.Here, " not containing in fact " refers to, except the situation comprising as inevitable impurity, containing the element being selected from silicon, aluminium, titanium, zirconium.So, as this organic compound, be more preferably selected from compound, imidazolium compounds and the imidazoles-epoxy adduct of compound, following formula (3) of compound, the following formula (2) of following formula (1) more than a kind.
[chemical formula 8]
(R1, R2 are the alkyl of phenyl, benzyl, hydrogen atom or carbonatoms 1～5 respectively independently.R3 is alkylidene group or the phenylene of carbonatoms 1～5.)。
R1, R2 are preferably phenyl, benzyl or hydrogen atom.R3 is preferably the alkylidene group of carbonatoms 1～5, more preferably the alkylidene group of carbonatoms 1～3.
[chemical formula 9]
(R4 is alkylidene group or the phenylene of carbonatoms 1～5.)。
R4 is preferably the alkylidene group of carbonatoms 1～5, more preferably the alkylidene group of carbonatoms 1～3.
[Chemical formula 1 0]
(R5 is the organic group with hydroxyl.R6 is hydrogen atom, methyl, carboxyl or phenyl.)。
R5 is preferably the organic group of 1 valency with hydroxyl and amino, the organic group of 1 valency that more preferably following formula (8) represents.R6 is preferably hydrogen atom or methyl, more preferably methyl.
[Chemical formula 1 1]
(R7, R8 are hydroxyl, phenolic group, hydroxymethyl, hydroxyethyl respectively independently.N is 0～5 integer arbitrarily.In formula, * portion represents the atomic linkage with N.)。
R7, R8 are preferably respectively hydroxymethyl or hydroxyethyl, more preferably hydroxyethyl independently.N is preferably 1～3.
Also can use the compound of following formula (9).
[Chemical formula 1 2]
More specifically, further preferably, be selected from N-benzylamino ethanol, N-β-anilino-ethanol, Racemic glycidol, imidazoles-epoxy adduct, benzotriazole derivatives, 3-benzylamino-1-propyl alcohol, 4-benzylamino-n-butyl alcohol, 5-benzylamino-1-amylalcohol, 2-methylamino ethanol, 2-ethyl amido alcohol, 2-propyl group monoethanolamine, 2-isopropylaminoethanol, 2-butyl monoethanolamine, 2-((1-methyl-propyl) amino) ethanol, 2-(tertiary butyl amino) ethanol, 2-amyl group monoethanolamine, 3-anilino propyl alcohol, 4-phenyl amino-n-butyl alcohol, in 5-phenyl amino-1-amylalcohol and 1-(2-hydroxyethyl) imidazoles more than a kind.Wherein, from safety in utilization, give and viewpoint that the high adhesion of conductor layer, storage stability improve is considered, particularly preferably be, be selected from N-benzylamino ethanol, N-β-anilino-ethanol, Racemic glycidol, 2,2-[{ (methyl isophthalic acid H-benzotriazole-1-yl) methyl } imino-] in di-methylcarbinol, 1-(2-hydroxyethyl) imidazoles and imidazoles-epoxy adduct more than a kind.
As with this organic compound, (C) inorganic filling material being carried out to surface-treated method, can enumerate: (C) inorganic filling material is dropped into impeller, this organic compound of spraying on one side, stirs (C) inorganic filling material method of 5～30 minutes on one side.
Consider from preventing the viewpoint that melt viscosity rises, when (C) inorganic filling material is made as to 100 quality %, the content of this organic compound is preferably below 2 quality %, more preferably below 1.8 quality %, more preferably, below 1.6 quality %, be further preferably below 1.4 quality %.Consider from the viewpoint that the dispersiveness of resinous varnish improves, the coating rate of inorganic filling material improves, more than being preferably 0.05 quality %, more preferably more than 0.1 quality %, more preferably more than 0.15 quality %, more than being further preferably 0.2 quality %.
After (C) inorganic filling material having been carried out to surface treatment with this organic compound, improve, make the dispersed viewpoint consideration further improving by react with unreacted silanol group from hydrophobicity, can further carry out above surface treatment with a kind that is selected from silane coupling agent, organoalkoxysilane, alkoxyl group oligopolymer, aluminium class coupling agent, titanium class coupling agent, zirconium class coupling agent.
As silane coupling agent, can use epoxy silane class coupling agent, aminosilane class coupling agent, hydrosulphonyl silane class coupling agent etc.They can use a kind or two or more to be used in combination.Particularly, for example can enumerate: glycidoxypropyltrimewasxysilane, glycidoxypropyl triethoxyl silane, glycidoxypropyl methyldiethoxysilane, glycidyl butyl trimethoxy silane, (3, 4-epoxycyclohexyl) the epoxy silane class coupling agent such as ethyl trimethoxy silane, aminopropyl methoxy silane, aminopropyltriethoxywerene werene, N-phenyl-3-TSL 8330, the aminosilane class coupling agents such as N-2 (amino-ethyl) TSL 8330, sulfydryl propyl trimethoxy silicane, the hydrosulphonyl silane class coupling agents such as sulfydryl propyl-triethoxysilicane.
As organoalkoxysilane, can use methyltrimethoxy silane, octadecyl Trimethoxy silane, phenyltrimethoxysila,e, methacryloxy (メ タ Network ロ キ シ) propyl trimethoxy silicane, imidazoles silane, triazine silane etc.They can use a kind or two or more to be used in combination.
Alkoxyl group oligopolymer refers to the low-molecular-weight resin in the lump with organic group and alkoxysilyl, for example, can enumerate: methylic alkoxyl group oligopolymer, containing the alkoxyl group oligopolymer of phenyl, containing the alkoxyl group oligopolymer of methyl/phenyl, containing the alkoxyl group oligopolymer of epoxy group(ing), containing the alkoxyl group oligopolymer of sulfydryl, containing amino alkoxyl group oligopolymer, containing the alkoxyl group oligopolymer of acryl, containing the alkoxyl group oligopolymer of methacryloyl, containing the alkoxyl group oligopolymer of urea groups, containing the alkoxyl group oligopolymer of isocyanate group, containing the alkoxyl group oligopolymer of vinyl etc.They can use a kind or two or more to be used in combination.
As aluminium class coupling agent, for example, can enumerate: aluminum isopropylate, single aluminium-sec-butylate diiso propoxide, aluminium secondary butylate, aluminum ethylate, ethyl acetoacetic acid aluminium diiso propoxide, three (ethyl acetoacetic acid) aluminium, alkyl acetoacetate aluminium diiso propoxide, two (ethyl acetoacetic acid) aluminium of monoacylphosphine acetone, three (Acetyl Acetone) aluminium, ring-type aluminum oxide isopropoxide, ring-type aluminum oxide isopropoxide, ring-type aluminum oxide stearate, ring-type aluminum oxide octanol salt (オ Network チ レ ー ト), ring-type aluminum oxide stearate etc.They can use a kind or two or more to be used in combination.
As titanium class coupling agent, for example, can enumerate: butyl (tetra) titanate dimer, ethohexadiol titanium, two (trolamine) diisopropoxy titanium (ジ イ ソ プ ロ Port キ シ チ タ Application PVC ス (ト リ エ タ ノ ー Le ア ミ ネ ー ト)), dilactic acid titanium dihydroxide, two (DL-Lactic acid ammonium salt) titaniums of dihydroxyl, two (dioctyl pyrophosphate) ethylene titanate, two (dioctyl pyrophosphate) oxyacetate titanate, tri-n-butoxytitanium monostearate, tetra-n-butyl titanate, metatitanic acid four (2-ethylhexyl) ester, two (dioctyl phosphite) titanium isopropylate, two (phosphorous acid two (tridecyl) ester) metatitanic acid four monooctyl esters, two (phosphorous acid two (tridecyl) ester) metatitanic acid four (2,2-, bis-allyloxy methyl isophthalic acid-butyl) ester, three capryloyl isopropyl titanates, isopropyl tricumylphenyltitanate, isopropyl triisostearoyl titanate, isostearoyl base two acryloyl isopropyl titanates, dimethyl propylene enoyl-isostearoyl isopropyl titanate, isopropyl tri (dioctyl phosphate)titanate, three (dodecyl benzenesulfonyl) isopropyl titanate, isopropyl tris (dioctyl pyrophosphate)titanate, three (N-acid amides ethyl-aminoethyl) isopropyl titanate etc.They can use a kind or two or more to be used in combination.
As zirconium class coupling agent, for example can enumerate: zirconium IV (2, two (the 2-propylene alkoxide methyl) butanolate of 2-, three new decyl alcohol salt) (ジ Le コ ニ ウ system IV(2, 2-PVC ス (2-プ ロ ペ ノ ラ ー ト メ チ Le) Block タ ノ ラ ー ト, ト リ ス ネ オ デ カ ノ ラ ー ト)), zirconium IV (2, two (the 2-propylene alkoxide methyl) butanolate of 2-, three (dodecylbenzyl sulfonic acid salt)), zirconium IV (2, two (the 2-propylene alkoxide methyl) butanolate of 2-, three (dioctyl) phosphoric acid salt), zirconium IV (2, two (the 2-propylene alkoxide methyl) butanolate of 2-, three 2-methyl 2-propylene alkoxide), zirconium IV-two (2, two (the 2-propylene alkoxide methyl) butanolate of 2-, biconjugate aminobenzoate), zirconium IV (2, two (the 2-propylene alkoxide methyl) butanolate of 2-, three (diisooctyl) pyrophosphate salt), zirconium IV (2, two (the 2-propylene alkoxide methyl) butanolate of 2-, three 2-acrylate), zirconium IV (2, two (the 2-propylene alkoxide methyl) butanolate of 2-, three (2-ethylene amino) ethylate), zirconium IV, two (2, two (the 2-propylene alkoxide methyl) butanolate of 2-, two (3-mercapto propionates)), zirconium IV (2, two (the 2-propylene alkoxide methyl) butanolate of 2-, three (2-amino) phenyl compound) (ジ Le コ ニ ウ system IV(2, 2-PVC ス (2-プ ロ ペ ノ ラ ー ト メ チ Le) Block タ ノ ラ ー ト, ト リ ス (2-ア ミ ノ) Off ェ ニ レ ー ト)), zirconium IV (2, two (the 2-propylene alkoxide methyl) butanolate of 2-, three (diisooctyl) pyrophosphate salt), N-substituent methyl acryl acid amides affixture, zirconium IV (2-ethyl, 2-propylene alkoxide methyl)-1, 3-propylene ジ オ ク レ ー ト, encircle 22, 2-(two-2-propylene alkoxide methyl) butanolate, pyrophosphate salt), zirconium IV (four-2, 2-(two-2-propylene alkoxide methyl) butanolate, two (tridecyl) hydrogen phosphite, 2 monoadducts etc.They can use a kind or two or more to be used in combination.
(C), after the surface treatment of inorganic filling material, on the surface of inorganic filling material, the carbon amount of the per unit area of combination is preferably 1.00mg/m
2below, 0.75mg/m more preferably
2below, 0.70mg/m more preferably
2below, be further preferably 0.65mg/m
2below, be especially preferably 0.60mg/m
2below, be particularly preferably 0.55mg/m
2below, be more particularly preferably 0.50mg/m
2below.On the other hand, the carbon amount of the per unit area of its upper combination in surface is preferably 0.05mg/m
2above, 0.08mg/m more preferably
2above, 0.11mg/m more preferably
2above, be further preferably 0.14mg/m
2above, be especially preferably 0.17mg/m
2above, be particularly preferably 0.20mg/m
2above, be more particularly preferably 0.23mg/m
2above, be further particularly preferably 0.26mg/m
2above.The conductor layer of high-peeling strength is stablized and can stably be formed to arithmetic average roughness after wet type roughening operation, r.m.s. roughness by this.
The surface-treated degree of inorganic filling material can adopt to be come the carbon amount of the per unit surface-area of the cleaned inorganic filling material of the solvent for inorganic filling material after surface treatment (for example methyl ethyl ketone (MEK)) (, the carbon amount of the per unit area of combination on the surface of inorganic filling material) quantitatively.For example, on the surface of inorganic filling material, the carbon amount of the per unit area of combination can calculate by following step.In inorganic filling material after surface treatment, add the MEK of q.s as solvent, carry out ultrasonic cleaning.Remove supernatant liquor, after making solids component dry, measure the carbon amount of combination on the surface of inorganic filling material with carbon analysis meter.Specific surface area by the carbon amount of gained divided by inorganic filling material, calculates the carbon amount of the per unit area of combination on inorganic filling material thus,
Should illustrate, as carbon analysis meter, can use hole field making made " EMIA-320V " etc.
Resin combination of the present invention is solidified to form to insulation layer, its surface of insulating layer is carried out to roughened, carry out plating and obtain conductor layer, the stripping strength of gained conductor layer and insulation layer can adopt the measuring method of recording in the mensuration > of pull strength (stripping strength) of < plated conductor layer described later to grasp.
Stripping strength is preferably below 0.8kgf/cm, more preferably, below 0.9kgf/cm, more preferably, below 1.0kgf/cm, is further preferably below 1.5kgf/cm.More than stripping strength is preferably 0.4kgf/cm, more preferably more than 0.5kgf/cm.
Resin combination of the present invention is solidified to form to insulation layer, its surface of insulating layer is carried out to arithmetic average roughness (Ra value), r.m.s. roughness (Rq value) after roughened and can adopt the measuring method of recording in the mensuration > of arithmetic average roughness (Ra value) after < roughening described later, r.m.s. roughness (Rq value) to grasp.
In order to reduce the transmission loss of electrical signal, arithmetic average roughness (Ra value) is preferably below 300nm, more preferably below 260nm, more preferably below 240nm, further be preferably below 220nm, be especially preferably below 200nm, be particularly preferably below 170nm, more be particularly preferably below 160nm, further elect as especially below 150nm.On the other hand, from the viewpoint that stripping strength improves is considered, more than arithmetic average roughness (Ra value) is preferably 10nm, more preferably more than 20nm, more preferably more than 30nm, more than being further preferably 40nm, more than being especially preferably 50nm.
In order to reduce the transmission loss of electrical signal, r.m.s. roughness (Rq value) is preferably below 480nm, more preferably below 440nm, more preferably below 420nm, further be preferably below 380nm, be especially preferably below 340nm, be particularly preferably below 300nm, more be particularly preferably below 260nm, be further particularly preferably below 220nm.On the other hand, from the viewpoint that stripping strength improves is considered, more than r.m.s. roughness (Rq value) is preferably 10nm, more preferably more than 30nm, more preferably more than 50nm, more than being further preferably 70nm, more than being especially preferably 90nm.
< (D) curing catalyst >
Resin combination of the present invention, by further containing curing catalyst, can make epoxy resin and solidifying agent solidify efficiently.As curing catalyst, have no particular limits, can enumerate: amine curing catalyst, guanidine class curing catalyst, imidazoles curing catalyst, Phosphonium class curing catalyst, metal species curing catalyst etc.They can use one kind or two or more being used in combination.
As amine curing catalyst, have no particular limits, can enumerate: the trialkylamines such as triethylamine, tributylamine, 4-dimethylaminopyridine, benzyl dimethyl amine, 2,4,6-tri-(dimethylaminomethyl) phenol, 1,8-diazabicyclo (5,4,0)-hendecene (being abbreviated as below DBU) etc.They can use a kind or two or more to be used in combination.
As guanidine class curing catalyst, have no particular limits, can enumerate: Dyhard RU 100, 1-methylguanidine, 1-ethyl guanidine, 1-cyclohexyl guanidine, 1-guanidines, 1-(o-tolyl) guanidine, dimethylguanidine, diphenylguanidine, trimethylammonium guanidine, tetramethyl guanidine, pentamethyl-guanidine, 1, 5, 7-tri-azabicyclos [4.4.0] 12 carbon-5-alkene, 7-methyl isophthalic acid, 5, 7-tri-azabicyclos [4.4.0] 12 carbon-5-alkene, 1-methyl two guanidines, 1-ethyl two guanidines, 1-normal-butyl two guanidines, 1-Octadecane base two guanidines, 1, 1-dimethyl two guanidines, 1, 1-diethyl two guanidines, 1-cyclohexyl two guanidines, 1-allyl group two guanidines, 1-phenyl two guanidines, 1-(o-tolyl) two guanidines etc.They can use a kind or two or more to be used in combination.
As imidazoles curing catalyst, have no particular limits, can enumerate: glyoxal ethyline, 2-undecyl imidazole, 2-heptadecyl imidazoles, 1,2 dimethylimidazole, 2-ethyl-4-methylimidazole, 1,2 dimethylimidazole, 2-ethyl-4-methylimidazole, 2-phenylimidazole, 2-phenyl-4-methylimidazole, 1 benzyl 2 methyl imidazole, 1-benzyl-2-phenylimidazole, 1-cyano ethyl-glyoxal ethyline, 1-cyano ethyl-2-undecyl imidazole, 1-cyano ethyl-2-ethyl-4-methylimidazole, 1-cyano ethyl-2-phenylimidazole, 1-cyano ethyl-2-undecyl imidazole trimellitate, 1-cyano ethyl-2-phenylimidazole trimellitate, 2,4-diamino-6-[2'-methylimidazolyl-(1')]-ethyl-s-triazine, 2,4-diamino-6-[2'-undecyl imidazole base-(1')]-ethyl-s-triazine, 2,4-diamino-6-[2'-ethyl-4'-methylimidazolyl-(1')]-ethyl-s-triazine, 2,4-diamino-6-[2'-methylimidazolyl-(1')]-ethyl-s-triazine tricarbimide affixture, 2-phenylimidazole tricarbimide affixture, 2-phenyl-4,5-dihydroxyl Methylimidazole, 2-phenyl-4-methyl-5-hydroxymethyl imidazoles, 2,3-dihydro-1H-pyrrolo-[1,2-a] benzoglyoxaline, 1-dodecyl-2-methyl-3-benzyl imidazole muriate, glyoxal ethyline quinoline, the adducts of the imidazolium compoundss such as 2-benzylimidazoline and imidazolium compounds and epoxy resin.They can use a kind or two or more to be used in combination.
Zuo Wei Phosphonium class curing catalyst, have no particular limits, can enumerate: triphenylphosphine, Phosphonium borate compound, tetraphenylphosphoniphenolate tetraphenyl borate salts, Zheng Ding Ji Phosphonium tetraphenyl borate salts, 4-butyl-phosphonium caprate, (4-aminomethyl phenyl) triphenyl phosphonium thiocyanate, tetraphenylphosphoniphenolate thiocyanate, Ding base triphenyl phosphonium thiocyanate etc.They can use a kind or two or more to be used in combination.
In resin combination of the present invention, when nonvolatile component in resin combination is made as to 100 quality %, the content of curing catalyst (except metal species curing catalyst) is preferably the scope of 0.005～1 quality %, the more preferably scope of 0.01～0.5 quality %.If less than 0.005 quality %, exist need to solidify slack-off, the tendency that thermal curing time is long, if exceed 1 quality %, the tendency that exists the storage stability of resin combination to reduce.
As metal species curing catalyst, have no particular limits, can enumerate: organometallic complex or the organic metal salt of the metals such as cobalt, copper, zinc, iron, nickel, manganese, tin.As the object lesson of organometallic complex, can enumerate the Organic Manganese complex compounds such as the organic nickel complex compound such as Organic Iron complex compound, acetylacetonate nickel (II), manganese acetylacetonate (II) such as the organic zinc complex compound such as organic copper complex, zinc acetylacetonate (II), the ferric acetyl acetonades (III) such as organic cobalt complex such as acetylacetone cobalt (II), acetylacetone cobalt (III), acetylacetone copper (II) etc.As the concrete example of organic metal salt, can enumerate zinc octoate, stannous octoate, zinc naphthenate, cobalt naphthenate, stearic acid tin, Zinic stearas etc.They can use one kind or two or more being used in combination.
In resin combination of the present invention, for the addition of metal species curing catalyst, when nonvolatile component in resin combination is made as to 100 quality %, the content of the metal based on metal species curing catalysts is preferably the scope of 25～500ppm, more preferably the scope of 40～200ppm.If not enough 25ppm, exists and be difficult to form the tendency of the conductor layer of adaptation excellence on the surface of insulating layer of low arithmetic average roughness, if exceed 500ppm, there is the storage stability of resin combination, the tendency that insulativity reduces.
< (E) thermoplastic resin >
In resin combination of the present invention, by further containing (E) thermoplastic resin, can make the mechanical Strong degree of cured article improve, can also improve the film forming ability while use with the form of adhering film.As this thermoplastic resin, for example, can enumerate: phenoxy resin, polyimide resin, polyamide-imide resin, polyetherimide resin, polysulfone resin, polyethersulfone resin, poly (phenylene ether) resin, polycarbonate resin, polyether-ether-ketone resin, vibrin.These thermoplastic resins can use a kind or two or more to be used in combination.Consider from the viewpoint that film forming ability, mechanical Strong degree improve, the consistency of resinous varnish improves, the weight-average molecular weight of thermoplastic resin is preferably 5000～200000 scope.Should illustrate, the weight-average molecular weight in the present invention adopts gel permeation chromatography (GPC) method (polystyrene conversion) to measure.Adopt the weight-average molecular weight of GPC method particularly can calculate as follows: as determinator, use the LC-9A/RID-6A processed of (strain) Shimadzu Seisakusho Ltd., as post, use the clear and Shodex K-800P/K-804L/K-804L processed of electrician's (strain) society, as moving phase, use chloroform etc., at 40 DEG C of column temperatures, measure, use the typical curve of polystyrene standard.
While coordinating (E) thermoplastic resin in resin combination of the present invention, the content of the thermoplastic resin in resin combination has no particular limits, with respect to the nonvolatile component 100 quality % in resin combination, be preferably 0.1～10 quality %, more preferably 1～5 quality %.When the content of thermoplastic resin is very few, existence can not be brought into play the tendency of the effect of film forming ability and the raising of mechanical Strong degree, if too much, melt viscosity rises, the tendency that exists the arithmetic average roughness that makes the surface of insulating layer after wet type roughening operation to increase.
< (F) rubber particles >
Resin combination of the present invention is by further containing (F) rubber particles, can improve coating stripping strength, (the De リ Le) raising of processibility that can also obtain Drilling, the reduction of dielectric loss tangent, stress alleviation effects.Spendable rubber particles in the present invention, for example, the organic solvent that uses while being not dissolved in the varnish of this resin combination of preparation, also not compatible with solidifying agent and epoxy resin etc. as essential component rubber particles.Therefore, this rubber particles exists with dispersion state in the varnish of resin combination of the present invention.Such rubber particles is prepared as follows conventionally: make the molecular weight of rubber constituent large to the level that is not dissolved in organic solvent or resin, make particle shape.
As the preference of spendable rubber particles in the present invention, can enumerate: core-sheath-type rubber particles, crosslink propylene nitrile divinyl rubber particle, cross-linked styrene divinyl rubber particle, acrylic rubber particle etc.Core-sheath-type rubber particles is the rubber particles with sandwich layer and sheath layer, and for example, outer field sheath layer is by glassy polymers forms, the sandwich layer of internal layer is made up of rubbery polymer 2 layers of structure; Or, outer field sheath layer by glassy polymers form, middle layer is by rubber particles of the 3-tier architecture that rubbery polymer forms, sandwich layer is made up of glassy polymers etc.Glassy polymers layer is for example made up of polymkeric substance of methyl methacrylate etc., and rubbery polymer layer is for example by formations such as butyl acrylate things (isoprene-isobutylene rubber).Rubber particles can be used in combination two or more.As the concrete example of core-sheath-type rubber particles, can enumerate: ス タ Off ィ ロ イ De AC3832, AC3816N, IM-401 change 1, IM-401 changes 7-17 (trade(brand)name, ガ Application Star change into (strain) system), メ タ Block レ Application KW-4426 (trade(brand)name, Mitsubishi's レ イ ヨ Application (strain) system).As the concrete example of crosslink propylene nitrile divinyl rubber (NBR) particle, can enumerate XER-91 (median size 0.5 μ m, JSR (strain) system) etc.As the concrete example of cross-linked styrene divinyl rubber (SBR) particle, can enumerate XSK-500 (median size 0.5 μ m, JSR (strain) system) etc.As the concrete example of acrylic rubber particle, can enumerate: (median size 0.1 μ m), (median size 0.2 μ is (Mitsubishi's レ イ ヨ Application (strain) system) m) for W450A for メ タ Block レ Application W300A.
The median size of rubber particles is preferably the scope of 0.005～1 μ m.The more preferably scope of 0.2～0.6 μ m.The median size of the rubber particles using in the present invention can adopt dynamic light scattering method to measure.For example can measure as follows: by ultrasonic wave etc., rubber particles is scattered in suitable organic solvent equably, using dense is particle size analysis device (FPAR-1000; Large mound electronics (strain) system), the size-grade distribution of making rubber particles with quality criteria, using its median particle diameter as median size.
With respect to the nonvolatile component 100 quality % in resin combination, the content of rubber particles is preferably 1～10 quality %, more preferably 2～5 quality %.
< (G) fire retardant >
Resin combination of the present invention, by further containing (G) fire retardant, can be given flame retardant resistance.As fire retardant, for example, can enumerate: the nitrogenous phosphorus compound of organic phosphates fire retardant, organic, nitrogen compound, silicone based flame retardant, metal hydroxides etc.As the concrete example of organic phosphates fire retardant, can enumerate: the HCA of three light (strain) system, HCA-HQ, the luxuriant and rich with fragrance type phosphorus compound such as HCA-NQ, the phosphorous benzoxazine compounds such as the HFB-2006M of clear and polymer (strain) system, the レ オ Off ォ ス 30 of aginomoto Off ァ イ Application テ Network ノ (strain) system, 50, 65, 90, 110, TPP, RPD, BAPP, CPD, TCP, TXP, TBP, TOP, KP140, TIBP, the TPPO of the emerging chemical industry in north (strain) system, PPQ, the OP930 of Network ラ リ ア Application ト (strain) system, the phosphate compounds such as the PX200 of large eight chemistry (strain) system, Dongdu changes into the FX289 of (strain) system, FX305, the epoxy resin that TX0712 etc. are phosphorous, Dongdu changes into the phosphorous phenoxy resins such as the ERF001 of (strain) system, the epoxy resin that the YL7613 of japan epoxy resin (strain) system etc. are phosphorous etc.As the concrete example of the nitrogenous phosphorus compound of organic, can enumerate: four countries change into SPB100, SPE100, (strain) volt of phosphoric ester amides compound, great mound chemistry (strain) the society system of SP670, the SP703 etc. of industry (strain) system and see the phosphazene compounds such as the made FP-series of pharmacy etc.As the concrete example of metal hydroxides, can enumerate: the aluminium hydroxides such as the magnesium hydroxide such as UD65, UD650, UD653 of the マ テ リ ア Le ズ of space portion (strain) system, B-30, the B-325 of bar industry (strain) society system, B-315, B-308, B-303, UFH-20 etc.
Other composition of < >
Not hindering in the scope of effect of the present invention, also can in resin combination of the present invention, coordinate as required other composition.As other composition, can enumerate: the heat-curing resin of vinyl benzyl based compound, acrylic compound, maleimide compound, block isocyanate compound and so on, the organic fillers such as Si powder, nylon powder, fluorine powder, the thickening materials such as オ Le ベ Application, ベ Application ト Application, defoamer or the levelling agent of silicone based, fluorine class, high score subclass, the adaptation imparting agents such as imidazoles, thiazoles, triazole species, silane coupling agent, tinting material such as phthalocyanine blue, phthalocyanine green, iodine are green, two diazonium Huangs, carbon black etc.
There is no particular limitation for the preparation method of resin combination of the present invention, for example, can enumerate: for gradation composition, add as required solvent etc., the method that use impeller etc. mixes etc.
The purposes of resin combination of the present invention has no particular limits, can be for the following scope of purposes widely that needs resin combination: the sheet laminated materials such as adhering film, prepreg, circuit substrate (laminated plate, multilayer printed circuit board etc.), solder resist, bottom filling material (ア Application ダ ー Off ィ Le material), chips welding material, encapsulating semiconductor material, filling perforation resin (め Trees fat is buried in cave), component packages resin etc. (component is buried め Write body Trees fat).Wherein, in the manufacture of multilayer printed circuit board, can be preferably used as and form the resin combination that insulation layer is used, can be more preferably as forming by plating the resin combination that conductor layer is used.Resin combination of the present invention can also be applied on circuit substrate and form insulation layer with varnish state, but conventionally preferably uses with the form of the sheet such as adhering film, prepreg laminated material industrial.Consider from the viewpoint of the plyability of sheet laminated material, the softening temperature of resin combination is preferably 40～150 DEG C.
< adhering film >
Adhering film of the present invention can adopt the method for well known to a person skilled in the art manufacture, for example, the preparation resinous varnish that dissolving resin composition forms in organic solvent, use die coating machine etc., this resinous varnish is coated on supporter, and then make organic solvent dry by heating or blowing hot-air etc., form resin combination layer.
As organic solvent, for example can enumerate: the ketones such as acetone, methyl ethyl ketone, pimelinketone, the acetate esters such as ethyl acetate, butylacetate, cellosolve acetate, propylene glycol methyl ether acetate, Trivalin SF acetic ester, the Trivalin SF such as cellosolve, diethylene glycol monobutyl ether class, toluene, dimethylbenzene etc. are aromatic hydrocarbon based, the amide solvents such as dimethyl formamide, N,N-DIMETHYLACETAMIDE, N-Methyl pyrrolidone etc.Organic solvent can be used in combination two or more.
Drying conditions is not particularly limited, as long as be dried, so that the content of organic solvent in resin combination layer is below 10 quality %, is preferably below 5 quality %.According to the boiling point of the organic solvent amount in varnish, organic solvent and difference, but for example by the varnish of the organic solvent that contains 30～60 quality % being dried to about 3～10 minutes at 50～150 DEG C, can forming resin combination the adhering film that has formed layer on supporter.
The thickness of the resin combination layer forming in adhering film is preferably the thickness more than thickness of conductor layer.The thickness with the conductor layer of circuit substrate is generally the scope of 5～70 μ m, and therefore resin combination layer preferably has the thickness of 10～100 μ m, more preferably has the thickness of 20～80 μ m.
As supporter, can enumerate: the polyolefinic films such as polyethylene, polypropylene, polyvinyl chloride, polyethylene terephthalate is (below sometimes referred to as " PET ".), the film of the polyester such as Polyethylene Naphthalate, the various plastics films such as polycarbonate film, Kapton.Also can use the tinsel such as release paper or Copper Foil, aluminium foil etc.For supporter and protective film described later, can implement the surface treatments such as delustring processing, corona treatment.Can also use the releasing agents such as silicone resin class releasing agent, Synolac class releasing agent, fluorine type resin releasing agent to implement demoulding processing.
The thickness of supporter has no particular limits, and is preferably 10～150 μ m, more preferably 25～50 μ m.
The further protective film of lamination taking supporter as benchmark on the face of the not closely sealed supporter of resin combination layer.The thickness of protective film has no particular limits, for example, be 1～40 μ m.By lamination protective film, can prevent adhering to or scar of lip-deep dust of resin combination layer etc.Adhering film is preserved after can being rolled into web-like.
< uses the multilayer printed circuit board > of adhering film
Then describe for an example of manufacturing the method for multilayer printed circuit board with the adhering film of as above manufacturing.
First, use vacuum laminator adhering film to be laminated to the one or both sides of circuit substrate.As the substrate using, can enumerate glass epoxy substrate, metal substrate, polyester substrate, polyimide substrate, BT resin substrate, thermohardening type polyphenylene oxide substrate etc. in circuit substrate.Should illustrate, circuit substrate refers to the circuit substrate that is formed with the conductor layer (circuit) that has carried out pattern processing at the one or both sides of above-mentioned such substrate here.In addition in the multilayer printed circuit board that conductor layer and insulation layer alternative stacked are formed, the circuit substrate that the outermost one or both sides of this multilayer printed circuit board are formed with the conductor layer (circuit) that has carried out pattern processing is also contained in here in said circuit substrate.Should illustrate, can utilize Darkening process, copper etching etc. to implement in advance roughened on conductor layer surface.
In above-mentioned lamination, when adhering film has protective film, after this protective film is removed, as required by adhering film and circuit substrate preheating, adhering film is pressurizeed and heat while be laminated to circuit substrate.For adhering film of the present invention, applicable use utilizes vacuum layer platen press to be under reduced pressure laminated to the method on circuit substrate.The condition of lamination is not particularly limited, and preference is preferably 1～11kgf/cm as, crimping temperature (laminating temperature) is preferably 70～140 DEG C, crimping pressure
2(9.8 × 10
4～107.9 × 10
4n/m
2), under the decompression below air pressure 20mmHg (26.7hPa), carry out lamination.In addition, the method for lamination can be batch-type, can be also the continous way that has used roller.Vacuum lamination can use commercially available vacuum laminator to carry out.As commercially available vacuum laminator, such as ニ チ ゴ ー モ ー ト Application (strain) vacuum pack system device processed, (strain) name mechanism can enumerated is made made vacuum pressure type laminating machine, (strain) イ of Hitachi Application ダ ス ト リ イ ズ roll-type dry type processed coating machine, the エ ー ア イ ー シ ー of Hitachi (strain) vacuum laminator processed etc.
The lamination procedure heating under decompression and pressurize also can be carried out with general vacuum hotpressing machine.For example can be by the metal sheets such as the SUS plate through heating being pressurizeed to carry out from support body layer side.Pressurized conditions is to make vacuum tightness be generally 1 × 10
-2mPa is following, be preferably 1 × 10
-3under decompression below MPa.Heating and pressurization also can within a stage, carry out, but from control resin the angle of oozing out consider, preferably condition is divided into two stages with on carry out.For example, the pressurization of first stage is preferably that 70～150 DEG C, pressure are 1～15kgf/cm in temperature
2the condition of scope under carry out, the pressurization of subordinate phase is preferably that 150～200 DEG C, pressure are 1～40kgf/cm in temperature
2the condition of scope under carry out.The time in each stage preferably carries out 30～120 minutes.As commercially available vacuum hotpressing machine, can exemplify such as MNPC-V-750-5-200 ((strain) name mechanism is done made), VH1-1603 (Beichuan essence machine (strain) system) etc.
After adhering film is laminated to circuit substrate, be cooled to after near room temperature, in the time that supporter is peeled off, peel off, carry out thermofixation, thereby can on circuit substrate, form insulation layer.The condition of thermofixation can suitably be selected according to kind, the content etc. of the resinous principle in resin combination, preferably at 150 DEG C～220 DEG C, in the scope of 20 minutes～180 minutes, select, more preferably at 160 DEG C～210 DEG C, in the scope of 30～120 minutes, select.
After having formed insulation layer, before solidifying, unstripped supporter in the situation that, now peel off.Then as required the insulation layer being formed on circuit substrate is carried out to perforate processing, form through hole (via hole), open-work (through hole).Perforate processing for example can or be carried out these Combination of Methods as required by known methods such as Drilling, laser apparatus, plasma bodys, and adopting the perforate processing of the laser apparatus such as carbon dioxide gas laser, YAG laser apparatus is the most conventional method.
Then, utilize dry type plating or wet type plating can on insulation layer, form conductor layer.As dry type plating, can use the known methods such as evaporation, sputter, ion plating.In the situation of wet type plating, for surface of insulating layer, adopt successively the neutralizing treatment of the expansion process of inflation fluid, the roughened that adopts oxygenant and employing neutralizer, form thus the anchor (ア ン カ ー) of convex-concave.Adopt the expansion process of inflation fluid to carry out as follows: during insulation layer be impregnated in to inflation fluid at 50～80 DEG C 5～20 minutes.Can enumerate alkaline solution, surfactant soln etc. as inflation fluid, preferred bases solution, as this alkaline solution, for example, can enumerate: sodium hydroxide solution, potassium hydroxide solution etc.As commercially available inflation fluid, for example, can enumerate: ス ウ ェ リ Application グ デ ィ ッ プ セ キ ュ リ ガ Application ス P (Swelling Dip Securiganth P), the ス ウ ェ リ Application グ デ ィ ッ プ セ キ ュ リ ガ Application ス SBU (Swelling Dip Securiganth SBU) etc. of ア ト テ ッ Network ジ ャ パ Application (strain) system.Adopt the roughened of oxygenant to carry out as follows: during insulation layer be impregnated in to oxidizing agent solution at 60 DEG C～80 DEG C 10 minutes～30 minutes.As oxygenant, for example, can enumerate: in the aqueous solution of sodium hydroxide, dissolved alkaline permanganic acid solution, dichromate, ozone, hydrogen peroxide/sulfuric acid, nitric acid of potassium permanganate, sodium permanganate etc.In addition, the concentration of the permanganate in alkaline permanganic acid solution is preferably 5～10 quality %.As commercially available oxygenant, for example, can enumerate: the alkaline permanganic acid solutions such as the コ Application セ Application ト レ ー ト コ Application パ Network ト CP, ド ー ジ Application グ ソ リ ュ ー シ ョ Application セ キ ュ リ ガ Application ス P of ア ト テ ッ Network ジ ャ パ Application (strain) system.Adopt the neutralizing treatment of neutralizer within 3～10 minutes, to carry out by impregnated in neutralizer at 30～50 DEG C in.As neutralizer, be preferably the acid aqueous solution, as commercially available product, can enumerate the リ ダ Network シ ョ Application ソ リ ュ ー シ Application セ キ ュ リ ガ Application ト P of ア ト テ ッ Network ジ ャ パ Application (strain) system.
Then, combination electroless plating applies with electrolysis plating and forms conductor layer.Also the resist pattern that can to form with conductor layer be opposite pattern, only utilizes electroless plating to apply and forms conductor layer.The method forming as pattern afterwards, can example subtract each other (subtractive) method, semi-additive process etc. as known to the skilled person.
< prepreg >
Prepreg of the present invention can be manufactured as follows, utilizes hot melt process or solvent method that resin combination of the present invention is soaked in flake reinforcement base material, and heating makes its semicure., can make resin combination of the present invention and soak into the prepreg forming in flake reinforcement base material.As flake reinforcement base material, for example, can use and comprise the flake reinforcement base material as the conventional fiber of prepreg fiber such as woven fiber glass or aromatic arginyl amine fiber.
Hot melt process is, not by resin dissolves in organic solvent, first by resin-coated with the good White Board of the separability of this resin on, be laminated to again on flake reinforcement base material, or not by resin dissolves in organic solvent, by die coating machine, resin is directly coated on to flake reinforcement base material first-class, manufactures the method for prepreg.Solvent method is that resinous varnish is prepared resin dissolves in operation same with adhering film in organic solvent, and flake reinforcement base material is immersed in this varnish, makes resinous varnish soak into flake reinforcement base material, then dry method.
< uses the multilayer printed circuit board > of prepreg
Then, for describing by an example of manufacturing the method for multilayer printed circuit board as the prepreg of above-mentioned manufacture.On circuit substrate 1 of overlapping prepreg of the present invention or as required overlapping several pieces, be situated between and clamped with metal sheet by mould release film, in pressurization, carry out vacuum pressed lamination under heating condition.Preferably, pressure is 5～40kgf/cm for pressurization, heating condition
2(49 × 10
4～392 × 10
4n/m
2), temperature is at 120～200 DEG C 20～100 minutes.Same with adhering film, after prepreg being laminated on circuit substrate by vacuum layer platen press, can be heating and curing.Then,, with same operation of method of above-mentioned record, after can carrying out roughening to curing prepreg surface, utilize plating to form conductor layer and manufacture multilayer printed circuit board.
< semiconductor device >
The multilayer printed circuit board of the application of the invention can be manufactured semiconductor device.By the conducting position at multilayer printed circuit board of the present invention, mounting semiconductor chip, can manufacture semiconductor device." conducting position " refers to " position of the electrical signal of conduction in multilayer printed circuit board ", and its position can be any one of position of surface or landfill.In addition, " semi-conductor chip ", as long as the circuit element taking semi-conductor as material, is not particularly limited.
As long as the installation method of the semi-conductor chip while manufacturing semiconductor device of the present invention makes semi-conductor chip effectively bring into play function, be not particularly limited, particularly, can enumerate wire-bonded installation method, flip-chip installation method, adopt the stack layer (BBUL) that there is no convex protrusion installation method, adopt anisotropic conductive film (ACF) installation method, adopt the installation method etc. of non-conductive film (NCF).
" employing does not have the installation method of the stack layer (BBUL) of convex protrusion " is " recess by direct semi-conductor chip landfill to multilayer printed circuit board; the installation method that semi-conductor chip is connected with the distribution on printed-wiring board (PWB) ", and then roughly divide into following BBUL method 1), BBUL method 2) installation method
BBUL method 1) use the bottom weighting agent installation method at the recess mounting semiconductor chip of multilayer printed circuit board
BBUL method 2) use adhering film or the prepreg installation method at the recess mounting semiconductor chip of multilayer printed circuit board.
BBUL method 1) comprise particularly following operation:
Operation 1) material of having removed conductor layer from the two sides of multilayer printed circuit board is set, utilize laser apparatus, mechanical Drilling to form communicating pores;
Operation 2) in the one side of multilayer printed circuit board, attach adhesive tape, in communicating pores, be configured in the mode that the bottom surface of semi-conductor chip is fixed on adhesive tape.Semi-conductor chip is now preferably lower than the height of communicating pores;
Operation 3) inject bottom weighting agent in the gap of communicating pores and semi-conductor chip, by filling, semi-conductor chip is fixed on to communicating pores;
Operation 4) then peel off adhesive tape, the bottom surface of semi-conductor chip is exposed;
Operation 5) at bottom surface side lamination adhering film of the present invention or the prepreg of semi-conductor chip, coating semi-conductor chip;
Operation 6) adhering film or prepreg are solidified after, utilize laser apparatus to carry out perforate processing, the bond pad (ボ Application デ ィ Application グ パ ッ ト) of the bottom surface that is present in semi-conductor chip is exposed, carry out that roughened as noted above, electroless plating are applied, electrolysis plating, thereby be connected with distribution.Further lamination adhering film or prepreg as required.
BBUL method 2) comprise particularly following operation:
Operation 1) on the conductor layer on the two sides of multilayer printed circuit board, form photoresist film (Off ォ ト レ ジ ス ト film), only form peristome at the one side of photoresist film by photolithography;
Operation 2) remove the conductor layer exposing at peristome with etching solution, insulation layer is exposed, then remove the photoresist film (レ ジ ス ト film) on two sides;
Operation 3) use laser apparatus or Drilling, the insulation layer exposing is all removed, carry out perforate processing, form recess; For the energy of laser apparatus, preferably can adjust the laser apparatus of energy, the laser absorption rate reduction of copper, the laser absorption rate of insulation layer are improved, more preferably carbon dioxide gas laser.By using this laser apparatus, can make laser apparatus can not connect the conductor layer on the opposite of the peristome of conductor layer, only remove insulation layer;
Operation 4) bottom surface of semi-conductor chip is disposed to recess towards peristome side, from peristome one side lamination adhering film of the present invention or prepreg, coating semi-conductor chip, the gap of landfill semi-conductor chip and recess.Semi-conductor chip is now preferably lower than the height of recess;
Operation 5) adhering film or prepreg are solidified after, utilize laser apparatus to carry out perforate processing, the bond pad of the bottom surface that is present in semi-conductor chip is exposed;
Operation 6) carry out that roughened as noted above, electroless plating are applied, electrolysis plating, thus connect distribution, further lamination adhering film or prepreg as required.
In the installation method of semi-conductor chip, consider from the miniaturization of semiconductor device, the viewpoint reducing of transmission loss, and never use solder thus for semi-conductor chip without undergoing its thermal history so the viewpoint that can not produce in the future the distortion of solder and resin consider, preferably adopt the installation method of the stack layer (BBUL) that there is no convex protrusion, more preferably BBUL method 1), BBUL method 2), further preferably BBUL method 2).
Embodiment
Below utilize embodiment to be described more specifically the present invention, but the present invention is not subject to the restriction of these embodiment.
< measuring method, evaluation method >
First describe for various measuring methods, evaluation method.
The preparation > of < stripping strength, arithmetic average roughness (Ra value), r.m.s. roughness (Rq value) test sample
(1) substrate treatment of internal layer circuit substrate
Copper foil laminate is covered in the woven fiber glass base material epoxy resin two sides that has formed internal layer circuit, and (thickness of Copper Foil is 18 μ m, substrate thickness is 0.3mm, SUNX (strain) R5715ES processed) two sides utilize メ ッ Network (strain) CZ8100 etching 1 μ m processed, carry out the roughened on copper surface.
(2) lamination of adhering film
Batch-type vacuum pressed laminating machine MVLP-500 for the adhering film of making in embodiment and comparative example (name machine (strain) trade(brand)name processed) is laminated to the two sides of internal layer circuit substrate.Lamination is as described below to carry out: carry out the decompression in 30 seconds, air pressure is reached below 13hPa, then with 30 seconds, 100 DEG C, the pressurization of the condition of pressure 0.74MPa.
(3) solidifying of resin combination
By PET film from lamination adhering film peel off, with 100 DEG C, 30 minutes, and then with the condition of cure of 180 DEG C, 30 minutes, resin combination is solidified.For embodiment 10, after thermofixation, peel off PET film under the same conditions, form insulation layer.
(4) roughened
Using the internal layer circuit substrate that has formed insulation layer as the ア ト テ ッ Network ジ ャ パ Application (strain) of inflation fluid containing in the ス エ リ Application グ デ ィ ッ プ セ キ ュ リ ガ Application ト P (aqueous solution of gylcol ether, sodium hydroxide) of diglycol monotertiary butyl ether in 60 DEG C of dippings 5 minutes, for embodiment 7, flood 10 minutes at 60 DEG C, then at the コ Application セ of the ア ト テ ッ Network ジ ャ パ Application (strain) as roughening liquid Application ト レ ー ト コ Application パ Network ト P (KMnO
4: the aqueous solution of 60g/L, NaOH:40g/L) in 80 DEG C dipping 15 minutes, for embodiment 10, flood 20 minutes at 80 DEG C, finally in the リ ダ Network シ of the ア ト テ ッ Network ジ ャ パ Application (strain) as neutralizer ョ Application シ ョ リ ュ ー シ Application セ キ ュ リ ガ Application ト P (グ リ オ キ ザ ー Le, sulphur aqueous acid), flood 5 minutes in 40 DEG C.After dry 30 minutes, for the surface of insulating layer after this roughened, carry out the mensuration of arithmetic average roughness (Ra value), r.m.s. roughness (Rq value) at 80 DEG C.
(5) plating of employing half adding technology
In order to form circuit at surface of insulating layer, internal layer circuit substrate is being contained to PdCl
2electroless plating application solution in 40 DEG C dipping 5 minutes, then in electroless plating copper liquid in 25 DEG C dipping 20 minutes.After carrying out anneal, form erosion shield 150 DEG C of heating 30 minutes, form after pattern by etching, carry out copper sulfate plating, form conductor layer with the thickness of 35 ± 5 μ m.Then carry out the anneal of 60 minutes at 200 DEG C.For this circuit substrate, carry out the mensuration of the pull strength (stripping strength) of plated conductor layer.
The mensuration > of the pull strength (stripping strength) of < plated conductor layer
On the conductor layer of circuit substrate, cut the otch of the part of wide 10mm, long 100mm, by its one end strip off, clamp with fixture (TSE of Co., Ltd.; オ ー ト コ system type trier AC-50C-SL), measure at room temperature, load (kgf/cm) while vertically peeling off 35mm with the speed of 50mm/ minute.
Arithmetic average roughness (Ra value) after < roughening, the mensuration > of r.m.s. roughness (Rq value)
Use non-contact type surfaceness meter (the PVC ー コ イ Application ス ツルメン Star WYKO NT3300 processed of society), utilize VSI contact mode, 50 times of lens, obtain numerical value in the measurement range of 121 μ m × 92 μ m, try to achieve Ra value, Rq value by this numerical value.Measure by the mean value of trying to achieve at random respectively at 10.
The evaluation > of < PCT patience
Use batch-type vacuum pressed laminating machine MVLP-500 (name machine (strain) trade(brand)name processed) to be laminated to the two sides of internal layer circuit substrate the adhering film of making in embodiment and comparative example.Lamination is as described below to carry out: carry out the decompression in 30 seconds, air pressure is reached below 13hPa, then with 30 seconds, 100 DEG C, the pressurization of the condition of pressure 0.74MPa.By PET film from lamination adhering film peel off after, with the condition of cure of 190 DEG C, 1 hour, resin combination is solidified to form to insulation layer.And then using height accelerated life test device (ETAC PM422 processed), the PCT that implements to place 100 hours under 121.5 DEG C, the environment of 100%RH tests (Pressure Cooker Test).Then be back to room temperature, confirm whether produce expansion at the interface of insulation layer and ground copper.Carry out crosscut (the cancellate otch of wide 1mm) at surface of insulating layer, whether jaggedly confirm on insulation layer.To on insulation layer and ground copper interface, be designated as "○" without the situation that does not produce breach after expansion, crosscut, by be designated as " △ " without the situation that produces breach after expansion, crosscut on insulation layer and ground copper interface, the situation that produces breach have expansion, crosscut on insulation layer and ground copper interface after is designated as to "×".
The mensuration > of the carbon amount of < per unit area
Use surface treated inorganic filling material 3g as test portion.The MEK of test portion and 30g (methyl ethyl ketone) is added in the centrifuge tube of separating centrifuge, stir solids component is suspended, the ultrasonic wave of irradiation 500W 5 minutes.Then, carry out solid-liquid separation by centrifugation, remove supernatant liquor.And then, supply the MEK of 30g, stir solids component is suspended, irradiate the ultrasonic wave 5 minutes of 500W.Then, carry out solid-liquid separation by centrifugation, remove supernatant liquor.Solids component is dried to 30 minutes at 150 DEG C.Correct this dry test portion 0.3g of weighing is placed in and measures with crucible, further to measuring with adding ignition dope (tungsten 3.0g, tin 0.3g) in crucible.Mensuration is placed in to carbon analysis meter with crucible, measures carbon amount.Carbon analysis meter uses hole field to make made EMIA-320V.Specific surface area by the carbon amount of measuring divided by inorganic filling material, the carbon amount using the value of gained as per unit area.
< Production Example 1 >
By spherical silicon dioxide, ((strain) ア De マ テ ッ Network ス system " SOC2 ", median size 0.5 μ m) 100 mass parts drop into the mixed powder machine of Henschel type, the N-benzylamino ethanol of spraying on one side (Tokyo changes into 280 DEG C of industry (strain) system, boiling points) 0.3 mass parts, stir spherical silicon dioxide 10 minutes on one side, thing 1 (the carbon amount 0.13mg/m of per unit area is manufactured in preparation
2).
< Production Example 2 >
By spherical silicon dioxide, ((strain) ア De マ テ ッ Network ス system " SC2050-SQ ", median size 0.5 μ m) 100 mass parts drop into the mixed powder machine of Henschel type, N-β-anilino-ethanol (Tokyo changes into 268 DEG C of industry (strain) system, boiling points) 0.3 mass parts of spraying on one side, stir spherical silicon dioxide after 10 minutes on one side, alkoxyl group oligopolymer (SHIN-ETSU HANTOTAI's chemical industry (strain) system " X-40-9227 ") 0.3 mass parts that spraying contains methyl/phenyl on one side, stir 10 minutes on one side, thing 2 (the carbon amount 0.25mg/m of per unit area is manufactured in preparation
2).
< Production Example 3 >
By spherical silicon dioxide, ((strain) ア De マ テ ッ Network ス system " SC2050-SQ ", median size 0.5 μ m) 100 mass parts drop into the mixed powder machine of Henschel type, spray on one side 167 DEG C of Racemic glycidol (Japanese grease (strain) system " エ ピ オ ー Le OH "), boiling points) 0.3 mass parts, stir spherical silicon dioxide after 10 minutes on one side, the phenyltrimethoxysila,e of spraying on one side (SHIN-ETSU HANTOTAI's chemical industry (strain) system " KBM-103 ") 0.3 mass parts, stir 10 minutes on one side, thing 3 (the carbon amount 0.18mg/m of per unit area is manufactured in preparation
2).
< Production Example 4 >
By spherical silicon dioxide, ((strain) ア De マ テ ッ Network ス system " SC2050-SQ ", median size 0.5 μ m) 100 mass parts drop into the mixed powder machine of Henschel type, the N-benzylamino ethanol of spraying on one side (Tokyo changes into 280 DEG C of industry (strain) system, boiling points) 0.3 mass parts, stir spherical silicon dioxide after 10 minutes on one side, the phenyltrimethoxysila,e of spraying on one side (SHIN-ETSU HANTOTAI's chemical industry (strain) system " KBM-103 ") 0.3 mass parts, stir 10 minutes on one side, thing 4 (the carbon amount 0.27mg/m of per unit area is manufactured in preparation
2).
< Production Example 5 >
By spherical silicon dioxide, ((strain) ア De マ テ ッ Network ス system " SC2050-SQ ", median size 0.5 μ m) 100 mass parts drop into the mixed powder machine of Henschel type, the N-benzylamino ethanol of spraying on one side (Tokyo changes into 280 DEG C of industry (strain) system, boiling points) 0.3 mass parts, stir spherical silicon dioxide after 10 minutes on one side, alkoxyl group oligopolymer (chemistry that rubs (strain) system " MTMS-A ") 0.3 mass parts that spraying contains methyl on one side more, stir 5 minutes on one side, thing 5 (the carbon amount 0.18mg/m of per unit area is manufactured in preparation
2).
< Production Example 6 >
By spherical silicon dioxide ((strain) ア De マ テ ッ Network ス system " SC2050-SQ ", median size 0.5 μ m) 100 mass parts drops into the mixed powder machine of Henschel type, spraying on one side, (Mitsubishi Chemical's (strain) makes " P200 " to imidazoles-epoxy adduct, the pimelinketone solution of nonvolatile component 30%) 0.9 mass parts, stir spherical silicon dioxide after 10 minutes on one side, alkoxyl group oligopolymer (chemistry that rubs (strain) system " MTMS-A ") 0.3 mass parts that spraying contains methyl on one side more, stir 5 minutes on one side, thing 6 (the carbon amount 0.29mg/m of per unit area is manufactured in preparation
2).
< Production Example 7 >
By spherical silicon dioxide ((strain) ア De マ テ ッ Network ス system " SC2050-SQ ", median size 0.5 μ m) 100 mass parts drops into the mixed powder machine of Henschel type, spray 2 on one side, 2-[{ (methyl isophthalic acid H-benzotriazole-1-yl) methyl } imino-] di-methylcarbinol (north of the city chemistry (strain) system " TT-LYK ", the MEK solution of nonvolatile component 60%) 0.5 mass parts, stir spherical silicon dioxide after 10 minutes on one side, alkoxyl group oligopolymer (chemistry that rubs (strain) system " MTMS-A ") 0.3 mass parts that spraying contains methyl on one side more, stir 5 minutes on one side, thing 7 (the carbon amount 0.16mg/m of per unit area is manufactured in preparation
2).
< Production Example 8 >
By spherical silicon dioxide ((strain) ア De マ テ ッ Network ス system " SC2050-SQ ", median size 0.5 μ m) 100 mass parts drops into the mixed powder machine of Henschel type, spray 2 on one side, 2-[{ (methyl isophthalic acid H-benzotriazole-1-yl) methyl } imino-] di-methylcarbinol (north of the city chemistry (strain) system " TT-LYK ", the MEK solution of nonvolatile component 60%) 0.5 mass parts, stir spherical silicon dioxide after 10 minutes on one side, spraying on one side contains amino silane coupling agent (SHIN-ETSU HANTOTAI's chemical industry (strain) system " KBM-573 ") 0.3 mass parts, stir 5 minutes on one side, thing 8 (the carbon amount 0.32mg/m of per unit area is manufactured in preparation
2).
< Production Example 9 >
By spherical silicon dioxide ((strain) ア De マ テ ッ Network ス system " SC2050-SQ ", median size 0.5 μ m) 100 mass parts drops into the mixed powder machine of Henschel type, spraying on one side, 1-(2-hydroxyethyl) imidazoles (make by Japanese compound probability chemistry (strain), 120 DEG C of boiling points (4.4Pa), the MEK solution of nonvolatile component 60%) 0.5 mass parts, stir spherical silicon dioxide after 10 minutes on one side, dimethyldiethoxysilane (SHIN-ETSU HANTOTAI's chemical industry (strain) system " KBE-22 ") 0.3 mass parts of spraying on one side, stir 10 minutes on one side, thing 9 (the carbon amount 0.12g/m of per unit area is manufactured in preparation
2).
< Production Example 10 >
By spherical silicon dioxide, ((strain) ア De マ テ ッ Network ス system " SC2050-SQ ", median size 0.5 μ m) 100 mass parts drop into the mixed powder machine of Henschel type, the phenyltrimethoxysila,e of spraying on one side (218 DEG C of SHIN-ETSU HANTOTAI's chemical industry (strain) system " KBM-103 ", boiling points) 0.6 mass parts, stir 10 minutes on one side, thing 10 (the carbon amount 0.09mg/m of per unit area is manufactured in preparation
2).
< Production Example 11 >
By spherical silicon dioxide, ((strain) ア De マ テ ッ Network ス system " SC2050-SQ ", median size 0.5 μ m) 100 mass parts drop into the mixed powder machine of Henschel type, silane coupling agent (290 DEG C of SHIN-ETSU HANTOTAI's chemical industry (strain) system " KBM403 ", boiling points) 0.6 mass parts that spraying contains epoxy group(ing) on one side, stir 5 minutes on one side, thing 11 (the carbon amount 0.24mg/m of per unit area is manufactured in preparation
2).
< Production Example 12 >
By spherical silicon dioxide, ((strain) ア De マ テ ッ Network ス system " SC2050-SQ ", median size 0.5 μ m) 100 mass parts drop into the mixed powder machine of Henschel type, spraying on one side contains amino silane coupling agent (215 DEG C of SHIN-ETSU HANTOTAI's chemical industry (strain) system " KBM903 ", boiling points) 0.6 mass parts, stir 5 minutes on one side, thing 12 (the carbon amount 0.14mg/m of per unit area is manufactured in preparation
2).
< embodiment 1 >
Naphthalene type epoxy resin (epoxy equivalent (weight) 144, DIC (strain) make " HP4700 ") 5 mass parts, liquid bisphenol A type epoxy resin (epoxy equivalent (weight) 180, Mitsubishi Chemical's (strain) system " jER828EL ") 14 mass parts, biphenyl type epoxy resin (epoxy equivalent (weight) 269, Japanese chemical drug (strain) system " NC3000H ") 14 mass parts are stirred while heating for dissolving in solvent oil 30 mass parts, then be cooled to room temperature, prepare mixture 1.Then, at 20 DEG C, rubber particles (ガ Application Star changes into (strain) system, ス タ Off ィ ロ イ De AC3816N) 1.5 mass parts are left standstill and expanded in solvent oil 6 mass parts 12 hours, prepare mixture 2.In mixture 1, add mixture 2 and manufacture thing 1, further add fire retardant (three light (strain) system " HCA-HQ ", 10-(2,5-dihydroxy phenyl)-10-hydrogen-9-oxa--10-phospho hetero phenanthrene-10-oxide compound, m) 5 mass parts of median size 1 μ, mixing with three rollers, dispersed.(DIC (strain) makes " LA-7054 " to mix wherein novolak class solidifying agent, the MEK solution of the nonvolatile component 60 quality % of phenolic hydroxyl group equivalent 124) 10 mass parts, naphthalene class resol (phenolic hydroxyl group equivalent 215, Nippon Steel's chemistry (strain) system " SN485 ", the MEK solution of nonvolatile component 60 quality %) 10 mass parts, phenoxy resin (weight-average molecular weight 35000, Mitsubishi Chemical's (strain) system " YL7553 ", the MEK of nonvolatile component 30 quality % and 1: 1 solution of pimelinketone) 7 mass parts, as MEK solution 2 mass parts of 5 quality % of the 4-dimethylaminopyridine of curing catalyst, MEK4 mass parts, dispersed with rotary blender, prepare resinous varnish.Then, this resinous varnish is coated on to polyethylene terephthalate thin film with alcohol acids demoulding processing (on thickness 38 μ stripping surface m) equably with die coating machine, make the thickness of dried resin combination layer reach 40 μ m, in 80～110 DEG C (average 95 DEG C) lower dry 5 minutes (the residual solvent amount in resin combination layer: approximately 2 quality %).Then, the polypropylene film of coating thickness 15 μ m on the surface of resin combination layer on one side, coils into web-like on one side.The adhering film of web-like is divided into wide 507mm, obtains the sheet adhering film of 507 × 336mm size.
< embodiment 2 >
Manufacture thing 2 except the manufacture thing 1 of embodiment 1 is changed to, all similarly prepare resinous varnish.Then use this resinous varnish, completely similarly operate with embodiment 1 and obtain adhering film.
< embodiment 3 >
Manufacture thing 3 except the manufacture thing 1 of embodiment 1 is changed to, all similarly prepare resinous varnish.Then use this resinous varnish, completely similarly operate with embodiment 1 and obtain adhering film.
< embodiment 4 >
Manufacture thing 4 except the manufacture thing 1 of embodiment 1 is changed to, all similarly prepare resinous varnish.Then use this resinous varnish, completely similarly operate with embodiment 1 and obtain adhering film.
< embodiment 5 >
Manufacture thing 5 except the manufacture thing 1 of embodiment 1 is changed to, all similarly prepare resinous varnish.Then use this resinous varnish, completely similarly operate with embodiment 1 and obtain adhering film.
< embodiment 6 >
Manufacture thing 6 except the manufacture thing 1 of embodiment 1 is changed to, all similarly prepare resinous varnish.Then use this resinous varnish, completely similarly operate with embodiment 1 and obtain adhering film.
< embodiment 7 >
Manufacture thing 7 except the manufacture thing 1 of embodiment 1 is changed to, all similarly prepare resinous varnish.Then use this resinous varnish, completely similarly operate with embodiment 1 and obtain adhering film.
< embodiment 8 >
Manufacture thing 8 except the manufacture thing 1 of embodiment 1 is changed to, all similarly prepare resinous varnish.Then use this resinous varnish, completely similarly operate with embodiment 1 and obtain adhering film.
< embodiment 9 >
Manufacture thing 9 except the manufacture thing 1 of embodiment 1 is changed to, all similarly prepare resinous varnish.Then use this resinous varnish, completely similarly operate with embodiment 1 and obtain adhering film.
< embodiment 10 >
Naphthalene type epoxy resin (epoxy equivalent (weight) 144, DIC (strain) make " EXA4032SS ") 10 mass parts, two xylenol type (PVC キ シ レ ノ ー Le type) epoxy resin (epoxy equivalent (weight) 190, Mitsubishi Chemical's (strain) system " YX4000HK ") 1 mass parts, modification naphthalene type epoxy resin (epoxy equivalent (weight) approximately 330, Nippon Steel's chemistry (strain) system " ESN475V ") 12 mass parts are stirred while heating for dissolving in solvent oil 20 mass parts, then be cooled to room temperature, prepare mixture 3.Then, at 20 DEG C, rubber particles (ガ Application Star changes into (strain) system, ス タ Off ィ ロ イ De AC3816N) 1.5 mass parts are left standstill and expanded in solvent oil 6 mass parts 12 hours, prepare mixture 4.In mixture 3, add mixture 4 and manufacture thing 4, and then (three light (strain) are made " HCA-HQ ", 10-(2 to add fire retardant, 5-dihydroxy phenyl)-10-hydrogen-9-oxa--10-phospho hetero phenanthrene-10-oxide compound, m) 2.5 mass parts of median size 1 μ, mixing with 3 rollers, dispersed.Add wherein active ester class solidifying agent (active group equivalent approximately 223, DIC (strain) makes " HPC-8000-65T ", the toluene solution of nonvolatile component 65 quality %) 10 mass parts, phenoxy resin (weight-average molecular weight 35000, Mitsubishi Chemical's (strain) system " YL7553 ", the MEK of nonvolatile component 30 quality % and 1: 1 solution of pimelinketone) 10 mass parts, dihydroxyphenyl propane dicyanate (ロ Application ザ ジ ャ パ Application (strain) Primaset BADCy processed) 11 mass parts, and then mixing is as MEK solution 0.6 mass parts of 5 quality % of the 4-dimethylaminopyridine of curing catalyst, (Tokyo changes into (strain) system to acetylacetone cobalt (III), Co (III) AcAc) MEK solution 3 mass parts of 1 quality %, dispersed with rotary blender, prepare resinous varnish.Then use this resinous varnish, completely similarly operate with embodiment 1 and obtain adhering film.
< comparative example 1 >
Except the manufacture thing 1 of embodiment 1 being changed to spherical silicon dioxide, ((strain) ア De マ テ ッ Network ス system " SOC2 ", median size 0.5 μ m) 100 mass parts, all similarly prepare resinous varnish.Then use this resinous varnish, completely similarly operate with embodiment 1 and obtain adhering film.
< comparative example 2 >
Except the manufacture thing 1 of embodiment 1 is changed to spherical silicon dioxide ((strain) ア De マ テ ッ Network ス system " SOC2 ", median size 0.5 μ m) 100 mass parts, add N-benzylamino ethanol (Tokyo change into industry (strain) system) 0.3 mass parts in addition, all similarly prepare resinous varnish.Then use this resinous varnish, completely similarly operate with embodiment 1 and obtain adhering film.
< comparative example 3 >
Manufacture thing 10 except the manufacture thing 1 of embodiment 1 is changed to, all similarly prepare resinous varnish.Then use this resinous varnish, completely similarly operate with embodiment 1 and obtain adhering film.
< comparative example 4 >
Manufacture thing 11 except the manufacture thing 1 of embodiment 1 is changed to, all similarly prepare resinous varnish.Then use this resinous varnish, completely similarly operate with embodiment 1 and obtain adhering film.
< comparative example 5 >
Manufacture thing 12 except the manufacture thing 1 of embodiment 1 is changed to, all similarly prepare resinous varnish.Then use this resinous varnish, completely similarly operate with embodiment 1 and obtain adhering film.
The results are shown in table 1,
As can be known from the results of Table 1, the resin combination of embodiment 1～10 has PCT patience, can obtain stripping strength with low arithmetic average roughness, low r.m.s. roughness and be worth fully.On the other hand, in comparative example 1～5, PCT patience is poor, and arithmetic average roughness, r.m.s. roughness become large, and plating expands, and stripping strength is remarkable little value.
Industrial usability
A kind of resin combination can be provided, and wherein, in wet type roughening operation, arithmetic average roughness, the r.m.s. roughness of surface of insulating layer are little, can form the plated conductor layer with sufficient stripping strength thereon, also have PCT patience.And then, the adhering film, prepreg, multilayer printed circuit board, the semiconductor device that use this resin combination can be provided.Further also can provide carried these, the electrical article such as computer, mobile phone, digital camera, TV, and the vehicles such as motorcycle (from Move bis-Wheels Trucks), automobile, electric car, boats and ships, aircraft.
Claims (10)
1. resin combination, it is the resin combination that contains (A) epoxy resin, (B) solidifying agent, (C) inorganic filling material, it is characterized in that, in this resin combination, be that 100 DEG C of above organic compound carry out surface treatment by above-mentioned inorganic filling material with thering is hydroxyl and reactive group and boiling point.
2. resin combination according to claim 1, is characterized in that, the reactive group of above-mentioned organic compound is the a kind of above reactive group being selected from amino, epoxy group(ing), sulfydryl, methacryloyl, acryl, vinyl and urea groups.
3. resin combination according to claim 1, it is characterized in that, above-mentioned organic compound is a kind of above organic compound in compound, imidazolium compounds and the imidazoles-epoxy adduct of compound, following formula (3) of the compound that is selected from following formula (1), following formula (2)
[changing 1]
R1, R2 are the alkyl of phenyl, benzyl, hydrogen atom or carbonatoms 1～5 respectively independently; R3 is alkylidene group or the phenylene of carbonatoms 1～5,
[changing 2]
R4 is alkylidene group or the phenylene of carbonatoms 1～5,
[changing 3]
R5 is the organic group with hydroxyl; R6 is hydrogen atom, methyl, carboxyl or phenyl.
4. according to the resin combination described in any one in claim 1～3, it is characterized in that, when (C) inorganic filling material is made as to 100 quality %, above-mentioned organic compound is 0.05～2 quality %.
5. according to the resin combination described in any one in claim 1～4, it is characterized in that, after (C) inorganic filling material is carried out to surface treatment with above-mentioned organic compound, further carry out above surface treatment with a kind that is selected from silane coupling agent, organoalkoxysilane, alkoxyl group oligopolymer, aluminium class coupling agent, titanium class coupling agent and zirconium class coupling agent.
6. according to the resin combination described in any one in claim 1～5, it is characterized in that, on the surface of (C) inorganic filling material, the carbon amount of the per unit area of combination is 0.05～1.00mg/m
2.
7. according to the resin combination described in any one in claim 1～6, it is characterized in that, resin combination is solidified to form to insulation layer, this surface of insulating layer is carried out to roughened, carry out plating and obtain conductor layer, the stripping strength of this conductor layer and insulation layer is 0.4kgf/cm～1.5kgf/cm, and resin combination is solidified to form to insulation layer, the arithmetic average roughness that this surface of insulating layer is carried out after roughened is 10nm～300nm, and r.m.s. roughness is 10nm～480nm.
8. sheet laminated material, is characterized in that, contains the resin combination described in any one in claim 1～7.
9. multilayer printed circuit board, wherein, has formed insulation layer by the cured article of the resin combination described in any one in claim 1～7.
10. semiconductor device, is characterized in that, right to use requires the multilayer printed circuit board described in 9.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/JP2011/075242 WO2013061478A1 (en) | 2011-10-26 | 2011-10-26 | Resin composition |
| JPPCT/JP2011/075242 | 2011-10-26 | ||
| PCT/JP2012/072075 WO2013061688A1 (en) | 2011-10-26 | 2012-08-30 | Resin composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103890088A true CN103890088A (en) | 2014-06-25 |
| CN103890088B CN103890088B (en) | 2016-05-18 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201280052315.XA Active CN103890088B (en) | 2011-10-26 | 2012-08-30 | Resin combination |
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| Country | Link |
|---|---|
| KR (1) | KR101489175B1 (en) |
| CN (1) | CN103890088B (en) |
| WO (2) | WO2013061478A1 (en) |
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| CN106085169A (en) * | 2015-05-01 | 2016-11-09 | 味之素株式会社 | Solidification compound |
| CN108148349A (en) * | 2016-12-02 | 2018-06-12 | 味之素株式会社 | Resin combination |
| CN109071957A (en) * | 2016-04-05 | 2018-12-21 | 日立化成株式会社 | Resin combination, hydrogen barrier material, solidfied material, composite material and works |
| CN111164151A (en) * | 2017-10-10 | 2020-05-15 | 味之素株式会社 | Cured product, method for producing same, resin sheet, and resin composition |
| JP2021185251A (en) * | 2020-06-25 | 2021-12-09 | 味の素株式会社 | Resin composition |
| TWI761408B (en) * | 2016-12-28 | 2022-04-21 | 日商納美仕有限公司 | Surface-treated silica filler, and resin composition including the surface-treated silica filler |
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| JP6413444B2 (en) * | 2014-07-31 | 2018-10-31 | 味の素株式会社 | Resin sheet, laminated sheet, laminated board, and semiconductor device |
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| KR102461516B1 (en) | 2017-01-10 | 2022-11-02 | 스미토모 세이카 가부시키가이샤 | epoxy resin composition |
| JP7148946B2 (en) | 2017-12-21 | 2022-10-06 | ナミックス株式会社 | resin composition |
| KR102661683B1 (en) * | 2018-08-03 | 2024-04-29 | 가부시끼가이샤 레조낙 | Adhesive composition, film adhesive, adhesive sheet, and method for producing semiconductor devices |
| JP6690692B2 (en) * | 2018-11-21 | 2020-04-28 | 味の素株式会社 | Method for producing roughened cured body |
| WO2020136902A1 (en) * | 2018-12-28 | 2020-07-02 | 日立化成株式会社 | Die bonding film, adhesive sheet, and semiconductor package and method for manufacturing same |
| JP7463736B2 (en) * | 2020-01-24 | 2024-04-09 | 味の素株式会社 | Resin composition |
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| TWI713500B (en) * | 2015-05-01 | 2020-12-21 | 日商味之素股份有限公司 | Hardening composition |
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Also Published As
| Publication number | Publication date |
|---|---|
| KR20140062172A (en) | 2014-05-22 |
| KR101489175B1 (en) | 2015-02-03 |
| WO2013061688A1 (en) | 2013-05-02 |
| WO2013061478A1 (en) | 2013-05-02 |
| CN103890088B (en) | 2016-05-18 |
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