CN108369985A - Anti-reflection material - Google Patents
Anti-reflection material Download PDFInfo
- Publication number
- CN108369985A CN108369985A CN201780004775.8A CN201780004775A CN108369985A CN 108369985 A CN108369985 A CN 108369985A CN 201780004775 A CN201780004775 A CN 201780004775A CN 108369985 A CN108369985 A CN 108369985A
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- CN
- China
- Prior art keywords
- mentioned
- reflection material
- weight
- resin
- optical semiconductor
- 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
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- 239000000463 material Substances 0.000 title claims abstract description 166
- 239000000945 filler Substances 0.000 claims abstract description 124
- 229920005989 resin Polymers 0.000 claims abstract description 114
- 239000011347 resin Substances 0.000 claims abstract description 114
- 230000003287 optical effect Effects 0.000 claims abstract description 92
- 239000004065 semiconductor Substances 0.000 claims abstract description 75
- 230000002401 inhibitory effect Effects 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims description 126
- 229920000647 polyepoxide Polymers 0.000 claims description 115
- 239000003822 epoxy resin Substances 0.000 claims description 113
- 150000001875 compounds Chemical class 0.000 claims description 71
- 239000011342 resin composition Substances 0.000 claims description 46
- 238000007711 solidification Methods 0.000 claims description 36
- 230000008023 solidification Effects 0.000 claims description 36
- 239000004615 ingredient Substances 0.000 claims description 34
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 19
- 239000007788 liquid Substances 0.000 claims description 18
- 238000007789 sealing Methods 0.000 claims description 16
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- 230000003667 anti-reflective effect Effects 0.000 abstract description 18
- 230000004907 flux Effects 0.000 abstract description 17
- -1 christobalite Substances 0.000 description 148
- 238000001723 curing Methods 0.000 description 93
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- 229910052710 silicon Inorganic materials 0.000 description 69
- 239000010703 silicon Substances 0.000 description 59
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- 125000003700 epoxy group Chemical group 0.000 description 49
- 229920002050 silicone resin Polymers 0.000 description 49
- 239000003795 chemical substances by application Substances 0.000 description 48
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 48
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- 239000003054 catalyst Substances 0.000 description 36
- 125000003342 alkenyl group Chemical group 0.000 description 35
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- 125000000962 organic group Chemical group 0.000 description 27
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 19
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 15
- 125000001118 alkylidene group Chemical group 0.000 description 15
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- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 13
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 13
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 13
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 12
- 238000003756 stirring Methods 0.000 description 12
- 150000008064 anhydrides Chemical class 0.000 description 11
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 10
- 239000001301 oxygen Substances 0.000 description 10
- 229910052760 oxygen Inorganic materials 0.000 description 10
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 10
- 239000003566 sealing material Substances 0.000 description 10
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 9
- 238000010521 absorption reaction Methods 0.000 description 9
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- 125000004450 alkenylene group Chemical group 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 9
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 8
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 8
- 125000001931 aliphatic group Chemical group 0.000 description 8
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 8
- 238000005286 illumination Methods 0.000 description 8
- 150000002460 imidazoles Chemical class 0.000 description 8
- 239000011256 inorganic filler Substances 0.000 description 8
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- 150000001412 amines Chemical class 0.000 description 7
- 125000003710 aryl alkyl group Chemical group 0.000 description 7
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- 239000002184 metal Substances 0.000 description 7
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 7
- 125000001424 substituent group Chemical group 0.000 description 7
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 6
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 6
- 229910002046 SYLYSIA SY430 Inorganic materials 0.000 description 6
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 235000010724 Wisteria floribunda Nutrition 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 6
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 6
- 229920001568 phenolic resin Polymers 0.000 description 6
- 150000002989 phenols Chemical class 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 125000005372 silanol group Chemical group 0.000 description 6
- 238000004381 surface treatment Methods 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- 239000010936 titanium Substances 0.000 description 6
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 6
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 description 5
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 description 5
- 150000001336 alkenes Chemical class 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 5
- WGQKYBSKWIADBV-UHFFFAOYSA-N benzylamine Chemical compound NCC1=CC=CC=C1 WGQKYBSKWIADBV-UHFFFAOYSA-N 0.000 description 5
- 229940106691 bisphenol a Drugs 0.000 description 5
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 5
- 238000010538 cationic polymerization reaction Methods 0.000 description 5
- 229930003836 cresol Natural products 0.000 description 5
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical group [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 5
- 125000000219 ethylidene group Chemical group [H]C(=[*])C([H])([H])[H] 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000005077 polysulfide Substances 0.000 description 5
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- 150000008117 polysulfides Polymers 0.000 description 5
- 230000036299 sexual function Effects 0.000 description 5
- 235000012239 silicon dioxide Nutrition 0.000 description 5
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- ZMANZCXQSJIPKH-UHFFFAOYSA-N N,N-Diethylethanamine Substances CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 4
- 239000004952 Polyamide Substances 0.000 description 4
- 229910020388 SiO1/2 Inorganic materials 0.000 description 4
- 229910020447 SiO2/2 Inorganic materials 0.000 description 4
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- 229910020485 SiO4/2 Inorganic materials 0.000 description 4
- 239000006087 Silane Coupling Agent Substances 0.000 description 4
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 4
- 150000001298 alcohols Chemical class 0.000 description 4
- 125000003545 alkoxy group Chemical group 0.000 description 4
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 4
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 4
- 239000013522 chelant Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
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- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 4
- 125000005843 halogen group Chemical group 0.000 description 4
- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- 125000005842 heteroatom Chemical group 0.000 description 4
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 4
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- 125000000623 heterocyclic group Chemical group 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
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- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 3
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 3
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- URJFKQPLLWGDEI-UHFFFAOYSA-N 1-benzyl-2-methylimidazole Chemical compound CC1=NC=[C]N1CC1=CC=CC=C1 URJFKQPLLWGDEI-UHFFFAOYSA-N 0.000 description 2
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- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 description 2
- NQRYJNQNLNOLGT-UHFFFAOYSA-N Piperidine Chemical class C1CCNCC1 NQRYJNQNLNOLGT-UHFFFAOYSA-N 0.000 description 2
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 229910052771 Terbium Inorganic materials 0.000 description 2
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- 150000004985 diamines Chemical class 0.000 description 1
- 239000012954 diazonium Substances 0.000 description 1
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical class NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 1
- KEIQPMUPONZJJH-UHFFFAOYSA-N dicyclohexylmethanediamine Chemical compound C1CCCCC1C(N)(N)C1CCCCC1 KEIQPMUPONZJJH-UHFFFAOYSA-N 0.000 description 1
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- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 description 1
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- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical group C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000002573 ethenylidene group Chemical group [*]=C=C([H])[H] 0.000 description 1
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- 125000001153 fluoro group Chemical class F* 0.000 description 1
- 150000002240 furans Chemical class 0.000 description 1
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- 235000008434 ginseng Nutrition 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- PYGSKMBEVAICCR-UHFFFAOYSA-N hexa-1,5-diene Chemical group C=CCCC=C PYGSKMBEVAICCR-UHFFFAOYSA-N 0.000 description 1
- 125000006038 hexenyl group Chemical group 0.000 description 1
- 210000004276 hyalin Anatomy 0.000 description 1
- 229940042795 hydrazides for tuberculosis treatment Drugs 0.000 description 1
- 125000003387 indolinyl group Chemical group N1(CCC2=CC=CC=C12)* 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 229910052909 inorganic silicate Inorganic materials 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
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- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical compound CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 238000007561 laser diffraction method Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 235000001510 limonene Nutrition 0.000 description 1
- 229940018564 m-phenylenediamine Drugs 0.000 description 1
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- 238000013507 mapping Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 description 1
- CUXQLKLUPGTTKL-UHFFFAOYSA-M microcosmic salt Chemical compound [NH4+].[Na+].OP([O-])([O-])=O CUXQLKLUPGTTKL-UHFFFAOYSA-M 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- QOHMWDJIBGVPIF-UHFFFAOYSA-N n',n'-diethylpropane-1,3-diamine Chemical compound CCN(CC)CCCN QOHMWDJIBGVPIF-UHFFFAOYSA-N 0.000 description 1
- TVIDDXQYHWJXFK-UHFFFAOYSA-N n-Dodecanedioic acid Natural products OC(=O)CCCCCCCCCCC(O)=O TVIDDXQYHWJXFK-UHFFFAOYSA-N 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
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- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000012766 organic filler Substances 0.000 description 1
- YOURXVGYNVXQKT-UHFFFAOYSA-N oxacycloundecane-2,11-dione Chemical compound O=C1CCCCCCCCC(=O)O1 YOURXVGYNVXQKT-UHFFFAOYSA-N 0.000 description 1
- DIVDFFZHCJEHGG-UHFFFAOYSA-N oxidopamine Chemical compound NCCC1=CC(O)=C(O)C=C1O DIVDFFZHCJEHGG-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- 125000002255 pentenyl group Chemical group C(=CCCC)* 0.000 description 1
- RFPMGSKVEAUNMZ-UHFFFAOYSA-N pentylidene Chemical group [CH2+]CCC[CH-] RFPMGSKVEAUNMZ-UHFFFAOYSA-N 0.000 description 1
- PKELYQZIUROQSI-UHFFFAOYSA-N phosphane;platinum Chemical compound P.[Pt] PKELYQZIUROQSI-UHFFFAOYSA-N 0.000 description 1
- 150000003003 phosphines Chemical class 0.000 description 1
- XYFCBTPGUUZFHI-UHFFFAOYSA-O phosphonium Chemical compound [PH4+] XYFCBTPGUUZFHI-UHFFFAOYSA-O 0.000 description 1
- 125000004193 piperazinyl group Chemical group 0.000 description 1
- 125000003386 piperidinyl group Chemical group 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- OSFBJERFMQCEQY-UHFFFAOYSA-N propylidene Chemical group [CH]CC OSFBJERFMQCEQY-UHFFFAOYSA-N 0.000 description 1
- 125000000168 pyrrolyl group Chemical group 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical group [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 125000000467 secondary amino group Chemical group [H]N([*:1])[*:2] 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 238000002444 silanisation Methods 0.000 description 1
- 150000004819 silanols Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 229940014800 succinic anhydride Drugs 0.000 description 1
- 125000000446 sulfanediyl group Chemical group *S* 0.000 description 1
- 229910019655 synthetic inorganic crystalline material Inorganic materials 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
- 235000007586 terpenes Nutrition 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- RAOIDOHSFRTOEL-UHFFFAOYSA-N tetrahydrothiophene Chemical group C1CCSC1 RAOIDOHSFRTOEL-UHFFFAOYSA-N 0.000 description 1
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
- 238000012719 thermal polymerization Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- WHLUQAYNVOGZST-UHFFFAOYSA-N tifenamil Chemical group C=1C=CC=CC=1C(C(=O)SCCN(CC)CC)C1=CC=CC=C1 WHLUQAYNVOGZST-UHFFFAOYSA-N 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
- 125000003944 tolyl group Chemical group 0.000 description 1
- 229960001124 trientine Drugs 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- AKQNYQDSIDKVJZ-UHFFFAOYSA-N triphenylsilane Chemical compound C1=CC=CC=C1[SiH](C=1C=CC=CC=1)C1=CC=CC=C1 AKQNYQDSIDKVJZ-UHFFFAOYSA-N 0.000 description 1
- 125000002948 undecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- QVTVDJWJGGEOGX-UHFFFAOYSA-N urea;cyanide Chemical group N#[C-].NC(N)=O QVTVDJWJGGEOGX-UHFFFAOYSA-N 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 125000005023 xylyl group Chemical group 0.000 description 1
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 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
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L101/00—Compositions of unspecified macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/52—Encapsulations
- H01L33/56—Materials, e.g. epoxy or silicone resin
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/013—Additives applied to the surface of polymers or polymer particles
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/42—Wire connectors; Manufacturing methods related thereto
- H01L2224/47—Structure, shape, material or disposition of the wire connectors after the connecting process
- H01L2224/48—Structure, shape, material or disposition of the wire connectors after the connecting process of an individual wire connector
- H01L2224/4805—Shape
- H01L2224/4809—Loop shape
- H01L2224/48091—Arched
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- Chemical & Material Sciences (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Led Device Packages (AREA)
- Surface Treatment Of Optical Elements (AREA)
Abstract
The purpose of the present invention is to provide while with sufficient anti-reflective function, the anti-reflection material that can prevent the total light flux of light source from reducing and utilize optical semiconductor device made of the anti-reflection material encapsulating optical semiconductor element.The present invention provides the anti-reflection material for including the resin layer for being dispersed with porous filler, wherein, the porous filler is to form the bumps for inhibiting to reflect on the surface of the resin layer, relative to anti-reflection material total amount (100 weight %), anti-reflection material and utilize optical semiconductor device made of the anti-reflection material encapsulating optical semiconductor element that the content of porous filler is 4~40 weight %.
Description
Technical field
The present invention relates to anti-reflection materials.In addition, the invention further relates to utilize anti-reflection material sealing photosemiconductor member
Optical semiconductor device made of part.The Japanese Patent Application 2016- that the application is filed an application based on January 15th, 2016 in Japan
No. 006638 and the Japanese Patent Application 2016-173980 filed an application in Japan on the 6th of September in 2016 claim priority, and by its
Content is incorporated herein.
Background technology
In recent years, it in various indoor or outdoors display boards, traffic signals, giant display unit etc., is partly led with light
Volume elements part (LED element) is developed as the use of the light-emitting device (optical semiconductor device) of light source.As such light half
Conductor device, it is however generally that, popularized be on substrate (optical semiconductor board for mounting electronic) carry optical semiconductor,
And further optical semiconductor device made of the optical semiconductor is sealed using transparent sealing material.It is partly led in such light
In sealing material in body device, led in order to prevent by total reflection occurs from incident lights such as external illumination light, sunlights
The reduction of the visibility of cause implements antireflection process on its surface.
In the past, the method for assigning anti-reflective function as the surface to resin layer, it is known to by making bead, titanium dioxide
The inorganic fillers such as silicon are dispersed in resin and the method (for example, referenced patent document 1) that makes incident light scatter.
Existing technical literature
Patent document
Patent document 1：Japanese Unexamined Patent Publication 2007-234767
Invention content
Problems to be solved by the invention
However it has been found that：It is difficult in the case where the method for patent document 1 to be applied to the resin of optical semiconductor sealing
To ensure the total light flux of light source while assigning sufficient anti-reflective function.I.e., it has been found that they are in following such
The relationship of compromise：In the case where sufficient anti-reflective function in order to obtain has coordinated necessary an adequate amount of inorganic filler,
The total light flux of light source can be greatly reduced, and on the other hand, it is reduced in the total light flux of light source in order to prevent and reduces inorganic fill out
In the case of the use level of material, it is unable to get sufficient antireflection ability.
Therefore, the purpose of the present invention is to provide while with sufficient anti-reflective function, the total of light source can be prevented
The anti-reflection material that luminous flux reduces.
In addition, other above-mentioned antireflections being designed to provide as optical semiconductor sealing resin combination of the present invention
Material.
Further, other be designed to provide of the invention is formed using above-mentioned anti-reflection material encapsulating optical semiconductor element
Optical semiconductor device.
Solution to the problem
The present inventor finds out：It is unable to get sufficient antireflection energy as in the case where reducing the use level of inorganic filler
One of the reason of power, can not be spread all over because of sedimentation due to inorganic filler to resin layer entirety, as a result, can not be in its whole table
Face forms uniform bumps, thus incident light can not be made effectively to scatter, and on the other hand, in the cooperation for increasing inorganic filler
Amount, so that i.e. bring it about sedimentation also can resin layer whole surface obtain antireflection ability in the case of, inorganic filler
Itself it can absorb light and total light flux is caused to be greatly reduced.
The present inventor has made intensive studies in order to solve the above problems, as a result, it has been found that, make in cooperation porous filler
When filler in the resin layer to constitute anti-reflection material, even a small amount of addition, can also assign sufficient anti-reflective function.By
This, it is possible to provide there is sufficient anti-reflective function, the anti-reflection material without causing the total light flux of light source to be greatly reduced, pole
It is suitable for the material for sealing the optical semiconductor in optical semiconductor device, and then completes the present invention.
That is, the present invention provides a kind of anti-reflection material, it is the antireflection for including the resin layer for being dispersed with porous filler
Material, wherein the porous filler forms the bumps for inhibiting reflection on the surface of the resin layer, relative to anti-reflection material total amount
The content of (100 weight %), porous filler are 4~40 weight %.
In above-mentioned anti-reflection material, porous filler can be inorganic porous property filler.
In above-mentioned anti-reflection material, anti-reflection material before curing can be liquid.
In above-mentioned anti-reflection material, relative to the total amount (100 weight %) of anti-reflection material before curing, in solidification
The amount of the ingredient of volatilization can be 10 weight % or less.
In above-mentioned anti-reflection material, above-mentioned resin layer can be formed by transparent hardening resin composition.
In above-mentioned anti-reflection material, above-mentioned hardening resin composition can be by comprising selected from epoxy resin, organosilicon
The composition of at least one of resin and acrylic resin curability compound is formed.
Above-mentioned anti-reflection material can be optical semiconductor sealing resin combination.
In addition, the present invention, which provides, utilizes optical semiconductor device made of above-mentioned anti-reflection material encapsulating optical semiconductor element.
More particularly it relates to following aspect.
[1] anti-reflection material, it includes the resin layers for being dispersed with porous filler, wherein the porous filler is in the tree
The surface of lipid layer forms the bumps for inhibiting reflection, relative to anti-reflection material total amount (100 weight %), the content of porous filler
For 4~40 weight %.
[2] anti-reflection material described in above-mentioned [1], wherein porous filler is present uniformly throughout to resin layer entirety.
[3] anti-reflection material described in above-mentioned [1] or [2], wherein porous filler be selected from inorganic porous property filler and
At least one of organic porous filler (preferably inorganic porous property filler).
[4] anti-reflection material described in any one of above-mentioned [1]~[3], wherein inorganic porous property filler is selected from inorganic
Glass [for example, pyrex, sodium borosilicate glass, water soda glass, aluminosilicate glass, quartz etc.], silica, oxidation
Aluminium, zircon, calcium silicates, calcium phosphate, calcium carbonate, magnesium carbonate, silicon carbide, silicon nitride, boron nitride, aluminium hydroxide, iron oxide, oxidation
Zinc, zirconium oxide, magnesia, titanium oxide, aluminium oxide, calcium sulfate, barium sulfate, forsterite (forsterite), steatite, point are brilliant
At least one of stone, clay, kaolin, dolomite, hydroxyapatite, nepheline, christobalite, wollastonite, diatomite and talcum
Powder, and the powder is that powder with cellular structure or their formed body (for example, pearl made of spheroidization etc.) are (excellent
It is selected as porous inorganic glass or porous silica, is more preferably porous silica).
[5] anti-reflection material described in any one of above-mentioned [1]~[4], wherein inorganic porous property filler is to be carried out
Surface treatment is [for example, at based on surfaces such as metal oxide, silane coupling agent, titanium coupling agent, organic acid, polyalcohol, siloxanes
Manage agent surface treatment etc.] filler.
[6] anti-reflection material described in above-mentioned [4] or [5], wherein porous silica is selected from melting titanium dioxide
At least one of silicon, crystalline silica, high-purity synthetic silica and colloidal silicon dioxide porous silica.
[7] anti-reflection material described in any one of above-mentioned [1]~[6], wherein organic porous filler is by being selected from benzene
Vinyl resins, acrylic resin, organic silicon resin, acrylicstyrene resinoid, vinyl chloride resin, inclined chloroethene
Vinyl resin, amide resinoid, polyurethane based resin, phenolic resin, styrene-conjugated diene resinoid, acrylic acid-conjugation two
At least one of polymer such as vinyl resin, olefine kind resin and celluosic resin (crosslinked for also including these polymer)
High-molecular porous property sintered body, foam polymer precursor or the gel porous body that organic matter is constituted.
[8] anti-reflection material described in any one of above-mentioned [1]~[7], wherein the shape of porous filler is selected from powder
At least one of body, spherical, broken shape, threadiness, needle-shaped and flakey (preferably spherical or broken shape).
[9] anti-reflection material described in any one of above-mentioned [1]~[8], wherein the medium particle diameter of porous filler is
0.1~100 μm (preferably 1~50 μm).
[10] anti-reflection material described in any one of above-mentioned [1]~[9], wherein the specific surface area of porous filler is
10~2000m2/ g (preferably 100~1000m2/g)。
[11] anti-reflection material described in any one of above-mentioned [1]~[10], wherein the micropore volume of porous filler is
0.1~10mL/g (preferably 0.2~5mL/g).
[12] anti-reflection material described in any one of above-mentioned [1]~[11], wherein the oil absorption of porous filler is 10
~2000mL/100g (preferably 100~1000mL/100g).
[13] anti-reflection material described in any one of above-mentioned [1]~[12], wherein relative to anti-reflection material total amount
The content (use level) of (100 weight %), porous filler are 4~35 weight % (preferably 4~30 weight %).
[14] anti-reflection material described in any one of above-mentioned [1]~[13], wherein relative to composition anti-reflection material
The content (use level) of resin combination (100 parts by weight), porous filler is 5~80 parts by weight (preferably 5~70 weight
Part, more preferably 5~60 parts by weight).
[15] anti-reflection material described in any one of above-mentioned [1]~[14], wherein constitute the resin in anti-reflection material
The resin of layer is by including the group selected from least one of epoxy resin, organic siliconresin and acrylic resin curability compound
Object is closed to be formed.
[16] anti-reflection material described in any one of above-mentioned [1]~[15], wherein anti-reflection material before curing is liquid
State.
[17] anti-reflection material described in any one of above-mentioned [1]~[16], wherein relative to antireflection material before curing
The total amount (100 weight %) of material, the amount of the ingredient to volatilize in solidification be 10 weight % or less (preferably 8 weight % or less, into
One step is preferably 5 weight % or less).
[18] anti-reflection material described in any one of above-mentioned [1]~[17], wherein above-mentioned resin layer is by transparent solidification
Property resin combination is formed.
[19] anti-reflection material described in above-mentioned [18], wherein above-mentioned hardening resin composition is by comprising selected from epoxy
The composition of at least one of resin, organic siliconresin and acrylic resin curability compound is formed.
[20] anti-reflection material described in any one of above-mentioned [1]~[19], wherein be formed in the bumps of anti-reflection material
The range (preferably 0.2~0.8 μm of range) that the arithmetic mean surface roughness Ra of shape is 0.1~1.0 μm.
[21] anti-reflection material described in any one of above-mentioned [1]~[20] is optical semiconductor sealing resin combination
Object.
[22] optical semiconductor device made of the anti-reflection material encapsulating optical semiconductor element described in above-mentioned [21] is utilized.
The effect of invention
The anti-reflection material of the present invention is due to above-mentioned composition, even if reducing the use level of porous filler
In the case of, it also can be obtained sufficient anti-reflective function, and the total light flux of light source can be prevented to be greatly reduced.Therefore, lead to
It crosses using the anti-reflection material of the present invention as the materials'use for being sealed in the optical semiconductor in optical semiconductor device, it can
Obtain (for example, brightness is also sufficient while gloss is inhibited) optical semiconductor device of high-quality.
Description of the drawings
[Fig. 1] shows the schematic diagram of an embodiment of the optical semiconductor device of the anti-reflection material comprising the present invention.
The figure (a) in left side is stereogram, and the figure (b) on right side is sectional view.
Symbol description
100：Reflector (light reflection resin combination)
101：Metal line (electrode)
102：Optical semiconductor
103：Closing line
104：Sealing material (anti-reflection material)
Specific implementation mode
<Anti-reflection material>
The anti-reflection material of the present invention is characterized as：Porous filler is scattered in resin layer, and the porous filler is in the tree
The surface of lipid layer forms the bumps for inhibiting reflection, relative to anti-reflection material total amount (100 weight %), the content of porous filler
For 4~40 weight %.
Since compared with the filler of imporosity, porous filler makes its table relative to resin layer because of cellular structure
Volume in sight increases, therefore spreads all over to resin layer entirety a small amount of addition, can be formed on its surface uniform
And fine bumps.In addition, by making resin layer immerse to cellular structure, the apparent ratio of porous filler and resin layer
The method of double differences reduces, and thus dispersity can be made to become stable, at the same can inhibit the interaction between the surface of porous filler and
Cohesion is set to become to be not susceptible to, porous filler can spread all over to resin layer entirety, therefore can be formed in resin layer surface
One and fine bumps and effectively make scatter incident light.
It should be noted that in the present specification, the additive amount (usage amount) of porous filler is that a small amount of (few) refers to：With
Weight conversion is few, rather than few with capacity (volume) conversion.
In the case where having used porous filler, compared with the filler of imporosity, reducing usage amount
Effectively inhibit reflection, therefore the substantially drop of the total light flux caused by inhibiting the light absorption by porous filler itself
While low, it is ensured that sufficient anti-reflective function.
Hereinafter, being described in detail for each integral part.
[porous filler]
Porous filler in the anti-reflection material of the present invention spreads all over to resin layer entirety, and dispersity is stablized, as a result,
The porous filler for being present in the surface of resin layer has the function of being formed for making the concave-convex of scatter incident light.
The porous filler of anti-reflection material for use in the present invention refers to that the apparent specific gravity of filler is less than true specific gravity,
Its internal inorganic or organic filler with cellular structure.Hereinafter, also referred to as " inorganic porous property filler ", " organic
Porous filler ".
It as inorganic porous property filler, can use those of known or usual, be not particularly limited, it can be mentioned, for example：
Unorganic glass [for example, pyrex, sodium borosilicate glass, water soda glass, aluminosilicate glass, quartz etc.], silica,
Aluminium oxide, zircon, calcium silicates, calcium phosphate, calcium carbonate, magnesium carbonate, silicon carbide, silicon nitride, boron nitride, aluminium hydroxide, iron oxide,
Zinc oxide, zirconium oxide, magnesia, titanium oxide, aluminium oxide, calcium sulfate, barium sulfate, forsterite, steatite, spinelle, clay,
The powder of kaolin, dolomite, hydroxyapatite, nepheline, christobalite, wollastonite, diatomite, talcum etc., and the powder is tool
There are powder or their formed body (for example, pearl made of spheroidization etc.) etc. of cellular structure.In addition, as inorganic porous
Property filler, can also enumerate and known or usual surface treatment is implemented [for example, being based on metal oxygen to above-mentioned inorganic porous property filler
Those of the surface treatment etc. of the surface conditioning agents such as compound, silane coupling agent, titanium coupling agent, organic acid, polyalcohol, organosilicon]
Deng.By being surface-treated as implementation, can make to improve with the compatibility of the ingredient of resin layer, dispersibility sometimes.Wherein, make
It is whole from spreading all over to resin layer for inorganic porous property filler, it can be from the perspective of its surface be effectively formed bumps, preferably
Porous inorganic glass or porous silica (porous silica filler).
It as porous silica, is not particularly limited, can use for example：Fused silica, crystalline silica
Known in silicon, high-purity synthetic silica, colloidal silicon dioxide etc. or usual porous silica.It needs to illustrate
It is that, as porous silica, can also use and implement known or usual surface treatment [for example, being aoxidized based on metal
Those of the surface treatment etc. of the surface conditioning agents such as object, silane coupling agent, titanium coupling agent, organic acid, polyalcohol, siloxanes].
It as organic porous filler, can use those of known or usual, be not particularly limited, can enumerate by for example
Styrene resin, acrylic resin, organic silicon resin, acrylicstyrene resinoid, vinyl chloride resin, inclined chlorine
Vinyl resins, amide resinoid, polyurethane based resin, phenolic resin, styrene-conjugated diene resinoid, acrylic acid-conjugation
The organic matters institutes such as the polymer such as diene resinoid, olefine kind resin, celluosic resin (crosslinked for also including these polymer)
Organic porous fillers such as the high-molecular porous property sintered body, foam polymer precursor, the gel porous body that constitute etc..
Inorganic-organic porosity alternatively, it is also possible to use the hybrid material by above-mentioned inorganic matter and organic matter to constitute is filled out
Material etc..
Above-mentioned porous filler can be made of homogenous material, can also be made of two kinds or more of material.Wherein, as
Porous filler, from the viewpoint of can spread all over to resin layer it is whole and its surface is effectively formed bumps, preferably without
Machine porous filler, from the viewpoint of availability, ease of manufacturing, more preferably porous silica (porosity dioxy
SiClx filler).
The shape of porous filler is not particularly limited, it can be mentioned, for example：Powder, spherical, broken shape, threadiness, it is needle-shaped,
Flakey etc..Wherein, it is formed on its surface uniform and fine recessed from being easy to make porous filler to spread all over whole to resin layer
From the perspective of convex form, the porous filler of preferably spherical or broken shape.
The medium particle diameter of porous filler is not particularly limited, from be easy to make porous filler spread all over it is whole to resin layer and
It is formed on its surface from the perspective of uniform and fine concaveconvex shape, preferably 0.1~100 μm, more preferably 1~50 μm.
It should be noted that above-mentioned medium particle diameter refer to using laser diffraction/scattering method size distribution in aggregate-value be
50% particle volume diameter (median particle volume diameter).
For the cellular structure of porous filler, each seed ginsengs such as specific surface area, micropore volume, oil absorption can be utilized
Number is limited, and can select the rank of the parameter with the anti-reflection material suitable for the present invention without particular limitation respectively
Porous filler.
The specific surface area of porous filler is not particularly limited, from porous filler be easy to spread all over it is whole to resin layer and
Its surface forms uniform and fine concaveconvex shape, to be effectively prevented reflection from the perspective of, preferably 10~2000m2/
G, it is more preferably 100~1000m2/g.Specific surface area is 10m2When/g or more, there are porous fillers to spread all over to resin layer entirety,
The tendency that the anti-reflective function on its surface improves.On the other hand, by making specific surface area be 2000m2/ g inhibits packet hereinafter, existing
The viscosity raising of resin combination containing porous filler, thixotropy, it is ensured that the tendency of mobility when manufacture anti-reflection material.
It should be noted that above-mentioned specific surface area refers to according to the attached book E of JIS K6430, by the adsorption isotherm of nitrogen, base at -196 DEG C
N2 adsorption specific surface area calculated by BET formulas.
The micropore volume of porous filler is not particularly limited, from be easy to make porous filler spread all over it is whole to resin layer and
Be formed on its surface uniform and fine concaveconvex shape, to be effectively prevented reflection from the perspective of, preferably 0.1~
10mL/g, more preferably 0.2~5mL/g.If micropore volume is 0.1mL/g or more, exists and be easy to make porous filler time
Cloth is whole to resin layer and is formed on its surface the tendency of concaveconvex shape.On the other hand, by make micropore volume be 5mL/g with
Under, there are the tendencies that the mechanical strength of porous filler improves.It should be noted that the micropore volume of porous filler can lead to
Mercury penetration method (porosimeter method) is crossed to measure micropore distribution and find out.
The oil absorption of porous filler is not particularly limited, from be easy to make porous filler spread all over it is whole to resin layer and
Its surface forms uniform and fine concaveconvex shape, to be effectively prevented reflection from the perspective of, preferably 10~2000mL/
100g, more preferably 100~1000mL/100g.If oil absorption is 10mL/100g or more, exists and be easy that porosity is made to fill out
Material spreads all over whole to resin layer and is formed on its surface the tendency of concaveconvex shape.On the other hand, by making oil absorption be 2000mL/
100g is hereinafter, there are the tendencies that the mechanical strength of porous filler improves.It should be noted that the oil absorption of porous filler is
The amount for the oil that 100g fillers are absorbed, can measure according to JIS K5101.
In the anti-reflection material of the present invention, porous filler can be used alone, and two or more can also combine
It uses.In addition, porous filler can be manufactured by known or usual manufacturing method, such as trade name can also be used
“Sylysia 250N”、“Sylysia 256”、“Sylysia 256N”、“Sylysia 310”、“Sylysia 320”、
“Sylysia 350”、“Sylysia 358”、“Sylysia 430”、“Sylysia 431”、“Sylysia 440”、
“Sylysia 450”、“Sylysia 470”、“Sylysia 435”、“Sylysia 445”、“Sylysia 436”、
“Sylysia 446”、“Sylysia 456”、“Sylysia 530”、“Sylysia 540”、“Sylysia 550”、
The Sylysia series such as " Sylysia 730 ", " Sylysia 740 ", " Sylysia 770 ", trade name " Sylosphere C-
1504 ", the Sylosphere such as " Sylosphere C-1510 " series (being manufactured by Fuji's chemistry of silicones (strain)), trade name
“Sunsphere H-31”、“Sunsphere H-32”、“Sunsphere H-33”、“Sunsphere H-51”、
“Sunsphere H-52”、“Sunsphere H-53”、“Sunsphere H-121”、“Sunsphere H-122”、
The commercially available products such as the Sunsphere such as " Sunsphere H-201 " H series (being manufactured by AGC SI-TECH (strain)).
The content (use level) of porous filler in the anti-reflection material of the present invention is relative to anti-reflection material total amount
(100 weight %) is 4~40 weight %, preferably 4~35 weight %, more preferably 4~30 weight %.By making porosity
The content of filler is 4 weight % or more, is easy that porous filler is made to spread all over to the resin layer entirety for constituting anti-reflection material, at it
Whole surface forms uniform concaveconvex shape.On the other hand, by make porous filler content be 40 weight % hereinafter, in the presence of
In the case of the sealing material that the anti-reflection material of the present invention is used as to such as optical semiconductor device, total light can be prevented logical
Amount significantly reduces the tendency so that it is guaranteed that sufficient illumination.
The content (use level) of porous filler in the anti-reflection material of the present invention is relative to composition anti-reflection material
Resin combination (100 parts by weight), usually 5~80 parts by weight, preferably 5~70 parts by weight, more preferably 5~60 weight
Part.Content by making porous filler is 5 parts by weight or more, is easy that porous filler is made to spread all over to composition anti-reflection material
Resin layer is whole, and uniform concaveconvex shape is formed in its whole surface.On the other hand, by making the content of porous filler be 80
Parts by weight work as the case where anti-reflection material of the present invention is used as the sealing material of such as optical semiconductor device hereinafter, existing
Under, can prevent total light flux significantly reduces the tendency so that it is guaranteed that sufficient illumination.
[resin layer]
The resin for constituting the resin layer in the anti-reflection material of the present invention is not particularly limited, and preferable use is suitable for
The sealing material of optical semiconductor in optical semiconductor device, i.e. those of optical semiconductor sealing resin combination, can be excellent
Choosing is solid using can for example be occurred by heat or light, obtains with high transparency, durability (for example, even across heating transparent
Even if property is not easy to the characteristic reduced, the heat that is applied in high temperature, thermal shock are not easy to occur cracking or from the stripping of clung body
Characteristic etc.) also excellent solidfied material curable resin.
As such curable resin, can be not particularly limited using known with thermosetting property or photo-curable
Or usual resin combination, preferably include the composition at least one of being for example selected from the group curability compound：Ring
Oxygen resin (epoxide) (being known as " epoxy resin (A) "), organic siliconresin (organo-silicon compound) (are known as " organosilicon tree
Fat (B) ") and acrylic resin (acyclic compound) (being known as " acrylic resin (C) ").As such composition, can arrange
Citing is such as：Including the composition (curable epoxy resin composition) of epoxy resin (A), including the combination of organic siliconresin (B)
Object (curable silicone resin composition), the composition (curability acrylic acid resin composition) for including acrylic resin (C).
The composition of these embodiments is illustrated below.But hardening resin composition of the invention is not limited to following reality
Apply the composition of mode.
In addition, the anti-reflection material of the present invention is not limited only to the purposes of optical semiconductor sealing resin combination, can also fit
For for example aftermentioned various optical components etc., could be applicable to suitable for respective purposes resin (for example, vistanex,
Polyester resin, polyamide, polyurethane resin etc.).
As the resin of the resin layer in the anti-reflection material for constituting the present invention, preferably heat resistance, the transparency, durability
Etc. excellent curable epoxy resin composition, curable silicone resin composition, curability acrylic acid resin composition, more
Preferably curable epoxy resin composition.
1. curable epoxy resin composition
Above-mentioned curable epoxy resin composition is (also referred to as " curable epoxy resin composition of the invention ") to include
Solidification compound of the epoxy resin (A) as neccessary composition.The curable epoxy resin composition of the present invention further includes
Curing agent (D) and curing accelerator (E) or curing catalysts (F) are used as neccessary composition.That is, the curability asphalt mixtures modified by epoxy resin of the present invention
Oil/fat composition is：Include the composition or work of epoxy resin (A), curing agent (D) and curing accelerator (E) as neccessary composition
Include the composition of epoxy resin (A) and curing catalysts (F) for neccessary composition.The curable epoxy resin composition of the present invention
Can also include other ingredients other than above-mentioned neccessary composition.
1-1. epoxy resin (A)
Epoxy resin (A) in the curable epoxy resin composition of the present invention, which is intramolecular, has 1 or more epoxy group
The compound of (oxirane ring), can the arbitrarily selection use from known or usual epoxide.As epoxy resin
(A), it can be mentioned, for example：Aromatic epoxy compound (aromatic epoxy resin), aliphatic epoxy compound (aliphatic epoxy tree
Fat), cycloaliphatic epoxy (alicyclic epoxy resin), hetero ring type epoxide (hetero ring type epoxy resin), intramolecular
Silicone derivative etc. with 1 or more epoxy group.
As above-mentioned aromatic epoxy compound, it can be mentioned, for example：Aromatic glycidyl ether based epoxy resin [for example,
Bisphenol A type epoxy resin, bisphenol f type epoxy resin, united phenol-type epoxy resin, phenolic resin varnish type epoxy resin are (for example, phenol
Phenolic resin varnish type epoxy resin, cresol novolak type epoxy resin, the cresol novolak type epoxy resin of bisphenol-A) etc., naphthalene
Type epoxy resin, the epoxy resin etc. obtained by tris-phenol] etc..
As above-mentioned aliphatic epoxy compound, it can be mentioned, for example：Aliphatic glycidyl ether class epoxide [example
Such as, aliphatic polyglycidyl ether etc.] etc..
Above-mentioned cycloaliphatic epoxy, which is intramolecular, has 1 or more alicyclic ring (aliphatic hydrocarbon ring) and 1 or more epoxy
The compound of base (wherein, except silicone derivative of the above-mentioned intramolecular with 1 or more epoxy group).As ester ring type epoxy
Compound, it can be mentioned, for example：(i) intramolecular has at least one (preferably 2 or more) alicyclic epoxy group (by constituting alicyclic ring
The epoxy group that adjacent 2 carbon atoms and oxygen atom are constituted) compound；(ii) have directly with singly bound in the epoxy of alicyclic ring
The compound of base；(iii) compound etc. with alicyclic ring and glycidyl.
There is alicyclic epoxy group possessed by the compound of at least one alicyclic epoxy group as above-mentioned (i) intramolecular, do not have
It is particularly limited to, wherein from the viewpoint of curability, preferably epoxycyclohexyl is (by adjacent 2 carbon atoms for constituting cyclohexane ring
The epoxy group constituted with oxygen atom).The compound especially as (i) intramolecular at least one alicyclic epoxy group, from solidification
From the perspective of the transparency of object, heat resistance, preferably intramolecular has the compound of 2 or more epoxycyclohexyls, more preferably
The compound indicated for following formula (1).
[chemical formula 1]
In formula (1), X indicates singly-bound or linking group (bivalent group with 1 or more atom).As above-mentioned linker
Group, it can be mentioned, for example：Part or all of epoxidized alkenylene, carbonyl, ehter bond, ester of bivalent hydrocarbon radical, carbon-to-carbon double bond
Key, carbonate group, amide groups, by multiple groups etc. to link in these groups.
As the compound that X in formula (1) is singly-bound, 3,4,3 ', 4 '-bicyclic oxygens connection hexamethylene can be enumerated.
As the alkyl of above-mentioned divalent, alkylidene, the divalent fat of the straight or branched that carbon atom number is 1~18 can be enumerated
Ring type alkyl etc..As carbon atom number be 1~18 straight or branched alkylidene, it can be mentioned, for example：Methylene, methyl are sub-
Methyl, dimethylated methylene base, ethylidene, propylidene, trimethylene etc..As above-mentioned divalent alicyclic type hydrocarbon, it can be mentioned, for example：
1,2- cyclopentylenes, 1,3- cyclopentylenes, cyclopentylidene, 1,2- cyclohexylidenes, 1,3- cyclohexylidenes, 1,4- cyclohexylidenes, hexamethylene
Divalent cycloalkylidenes such as fork (being pitched comprising cycloalkanes) etc..
Part or all of epoxidized alkenylene (also referred to as " epoxidation alkenylene ") as above-mentioned carbon-to-carbon double bond
In alkenylene, it can be mentioned, for example：Ethenylidene, the third alkenylene, 1- butenylidenes, 2- butenylidenes, Aden's dialkylene, Asia penta
The alkenylene of the straight or brancheds of carbon atom numbers 2~8 such as alkenyl, sub- hexenyl, heptene base, sub- octenyl (also includes Asia
Alkyl polyvinyl) etc..In particular, as above-mentioned epoxidised alkenylene, the preferably epoxidized Asia of whole carbon-to-carbon double bonds
The alkenylene of the epoxidized carbon atom number of alkenyl, more preferably whole carbon-to-carbon double bonds 2~4.
As above-mentioned linking group X, the particularly preferably linking group containing oxygen atom, specific enumerable-CO- ,-O-
CO-O- ,-COO- ,-O- ,-CONH-, epoxidation alkenylene；By multiple groups to link in these groups；1 or 2
The group etc. that the above group and 1 or 2 or more bivalent hydrocarbon radical link.As bivalent hydrocarbon radical, can enumerate above-mentioned
Those of illustrate.
As the typical example for the compound that above-mentioned formula (1) indicates, can enumerate：2,2- bis- (3,4- 7-oxa-bicyclo[4.1.0-1- bases)
Bis- (3,4- 7-oxa-bicyclo[4.1.0-1- bases) ethane of propane, bis- (3,4- epoxycyclohexyl-methyls) ethers, 1,2-, 1,2- epoxies-1,2- are double
The compound etc. that (3,4- 7-oxa-bicyclo[4.1.0-1- bases) ethane, following formula (1-1)~(1-10) are indicated.It should be noted that following
L, m in formula (1-5), (1-7) indicate 1~30 integer respectively.R in following formula (1-5) is the alkylene of carbon atom number 1~8
Base can be enumerated：Methylene, ethylidene, propylidene, isopropylidene, butylidene, isobutylidene, sub- sec-butyl, pentylidene, it is sub- oneself
The alkylidene of the straight or brancheds such as base, heptamethylene, octamethylene.In these, preferably methylene, ethylidene, propylidene, sub- isopropyl
The alkylidene of the straight or branched of the carbon atom numbers such as base 1~3.N1~n6 in following formula (1-9), (1-10) indicates 1 respectively
~30 integer.
[chemical formula 2]
[chemical formula 3]
As the compound with the epoxy group for being bonded directly to above-mentioned (ii) alicyclic ring with singly-bound, it can be mentioned, for example following formula
(2) compound etc. indicated.
[chemical formula 4]
In formula (2), R ' is to remove group (organic group of p valences) made of p hydroxyl (- OH) from p member alcohol on structural formula,
P, q indicates natural number respectively.As p members alcohol [R ' (OH)p], the polyalcohols (carbon such as bis- (the hydroxymethyl)-n-butyl alcohols of 2,2- can be enumerated
The alcohol etc. of atomicity 1~15) etc..P is preferably that 1~6, q is preferably 1~30.In the case where p is 2 or more, in respective ()
Q in the group of (in the bracket in outside) can be the same or different.As the compound that above-mentioned formula (2) indicates, specifically may be used
1,2- epoxies -4- (2- epoxy ethyls) hexamethylene addition product of bis- (the hydroxymethyl)-n-butyl alcohols of 2,2- is enumerated [for example, trade name
" EHPE3150 " ((strain) Daicel systems) etc.] etc..
As the compound with above-mentioned (iii) alicyclic ring and glycidyl, it can be mentioned, for example：Bis- [4- (the 2,3- rings of 2,2-
Oxygen propoxyl group) cyclohexyl] propane, bis- [3,5- dimethyl -4- (2,3- glycidoxies) cyclohexyl] propane of 2,2-, bisphenol A-type
Compound (bisphenol-A epoxy resin) etc. made of epoxy resin is hydrogenated；Bis- [2- (2,3- glycidoxies) hexamethylenes
Base] methane, [2- (2,3- glycidoxies) cyclohexyl] [4- (2,3- glycidoxies) cyclohexyl] methane, bis- [4- (2,3- rings
Oxygen propoxyl group) cyclohexyl] methane, bis- [3,5- dimethyl -4- (2,3- glycidoxies) cyclohexyl] methane, bisphenol F type epoxy
Compound made of resin is hydrogenated (A Hydrogenated Bisphenol A F types epoxy resin) etc.；Hydrogenated biphenyl phenol-type epoxy resin；It is clear to hydrogenate phenolic aldehyde
Paint shaped epoxy resin is (for example, hydrogenation phenol novolak type epoxy resin, hydrogenation cresol novolak type epoxy resin, bisphenol-A
Hydrogenation cresol novolak type epoxy resin etc.)；Hydrogenate naphthalene type epoxy resin；The epoxy resin obtained by tris-phenol
Hydrogenated epoxy resin etc..
As above-mentioned cycloaliphatic epoxy, it can be mentioned, for example 1,2,8,9- bicyclic oxygen limonenes etc. in addition to this.
As above-mentioned hetero ring type epoxide, it can be mentioned, for example：Intramolecular has in addition to epoxy group (oxirane ring)
Heterocycle in addition is [for example, tetrahydrofuran ring, amylene oxide ring, morpholine ring, chroman ring, heterochromatic full ring, thiophane ring, tetrahydrochysene
Bicyclic [3.3.0] octane of thiapyran ring, aziridine ring, pyrrolidine ring, piperidine ring, piperazine ring, indoline ring, 2,6- dioxas
The non-aromatics such as ring, 1,3,5- Trianacyclohexanes ring, tri- azacyclo- hex- 2,4,6- triketones rings (isocyanide urea ring) of 1,3,5- are miscellaneous
Ring；Aromatic series heterocycle such as thiphene ring, pyrrole ring, furan nucleus, pyridine ring etc.] and epoxy group compound.
As above-mentioned hetero ring type epoxide, it is preferable to use for example：Intramolecular has the different of 1 or more epoxy group
Cyanurate (hereinafter also referred to as " isocyanuric acid ester containing epoxy group ").The intramolecular of the above-mentioned isocyanuric acid ester containing epoxy group
The quantity for the epoxy group having is not particularly limited, preferably 1~6, more preferably 1~3.
As the above-mentioned isocyanuric acid ester containing epoxy group, it can be mentioned, for example the compounds indicated with following formula (3).
[chemical formula 5]
In formula (3), RX、RYAnd RZ(RX~RZ) identical or different, indicate hydrogen atom or monovalent organic group.Wherein, RX~RZ
In at least one be the monovalent organic group containing epoxy group.As above-mentioned monovalent organic group, it can be mentioned, for example：Monovalence fat
Fat race alkyl (for example, alkyl, alkenyl etc.)；Monovalence aromatic hydrocarbyl (for example, aryl etc.)；Monovalence heterocycle；Aliphatic alkyl,
2 or more the univalent perssads etc. for being bonded and being formed in alicyclic type hydrocarbon and aromatic hydrocarbyl.It should be noted that monovalence is organic
Group can also have substituent group (for example, the substituent groups such as hydroxyl, carboxyl, halogen atom).It is organic as the monovalence containing epoxy group
Group contains epoxy it can be mentioned, for example epoxy group, glycidyl, 2- methyl epoxypropyl, epoxycyclohexyl etc. are aftermentioned
The univalent perssad etc. of base.
More specifically, as the above-mentioned isocyanuric acid ester containing epoxy group, the chemical combination indicated with following formula (3-1) can be enumerated
Object, the compound indicated with following formula (3-2), the compound etc. indicated with following formula (3-3).
[chemical formula 6]
[chemical formula 7]
[chemical formula 8]
In above-mentioned formula (3-1), formula (3-2) and formula (3-3) (formula (3-1)~(3-3)), R1、R2It is identical or different, it indicates
The alkyl of hydrogen atom or carbon atom number 1~8.As the alkyl of carbon atom number 1~8, it can be mentioned, for example：Methyl, ethyl, propyl,
The alkyl of the straight or brancheds such as isopropyl, butyl, isobutyl group, sec-butyl, amyl, hexyl, heptyl, octyl.Wherein, preferably
The alkyl of the straight or branched of the carbon atom numbers such as methyl, ethyl, propyl, isopropyl 1~3.In above-mentioned formula (3-1)~(3-3)
R1And R2Particularly preferably hydrogen atom.
As the typical example of the compound indicated with above-mentioned formula (3-1), can enumerate：Monoallyl diglycidyl isocyanide
Bis- (the 2- methyl epoxypropyl) isocyanuric acid esters of urea acid esters, 1- allyls -3,5-, 1- (2- methylpropenyls) -3,5- two contractings
Bis- (2- methyl epoxypropyl) isocyanuric acid esters of water glyceryl isocyanuric acid ester, 1- (2- methylpropenyls) -3,5- etc..
As the typical example of the compound indicated with above-mentioned formula (3-2), can enumerate；Diallyl list glycidyl isocyanide
Bis- (2- the methylpropenyls) -5- contractings of urea acid esters, 1,3- diallyls -5- (2- methyl epoxypropyl) isocyanuric acid ester, 1,3-
Bis- (2- methylpropenyls) -5- (2- methyl epoxypropyl) isocyanuric acid esters of water glyceryl isocyanuric acid ester, 1,3- etc..
As the typical example of the compound indicated with above-mentioned formula (3-3), triglycidyl group isocyanuric acid ester, three can be enumerated
(2- methyl epoxypropyl) isocyanuric acid ester etc..
It should be noted that the above-mentioned isocyanuric acid ester containing epoxy group can also add alcohol, acid anhydrides etc. and epoxy reaction
Compound and in advance modified use.
There is the silicone derivative (also referred to as " siloxanes containing epoxy group of 1 or more epoxy group as above-mentioned intramolecular
Derivative "), be intramolecular with the siloxane backbone being made of siloxanes key (Si-O-Si) and with 1 or more epoxy group
Compound.As above-mentioned siloxane backbone, it can be mentioned, for example：Annular siloxane skeleton；The organosilicon of straight or branched is (straight
Chain or branched polysiloxanes), the silicone matrix such as polysilsesquioxane etc. of cage modle, ladder type.The above-mentioned silicon containing epoxy group
The quantity for the epoxy group that the intramolecular of siloxane derivative has is not particularly limited, preferably 2~4, more preferably 3 or 4
It is a.
Epoxy group is not particularly limited possessed by the above-mentioned silicone derivative containing epoxy group, from can make curability ring
Epoxy resin composition effectively cures, the superior solidfied material of intensity can be obtained in terms of set out, preferably at least 1 is alicyclic ring ring
Oxygroup, wherein at least one in particularly preferred epoxy group is epoxycyclohexyl.
As the above-mentioned silicone derivative containing epoxy group, it is (cyclic annular that it can be mentioned, for example the compounds indicated with following formula (4)
Siloxanes).
[chemical formula 9]
In above-mentioned formula (4), R3It is identical or different, indicate alkyl or the monovalent organic group containing epoxy group.Wherein, with
The R for the compound that formula (4) indicates3In, at least one (being preferably at least 2) is that the monovalent organic group containing epoxy group is (special
It is the monovalent organic group containing alicyclic epoxy group).In addition, p in formula (4) indicate 3 or more integer (preferably 3~6 it is whole
Number).It should be noted that multiple R3It can be the same or different.
As the above-mentioned monovalent organic group containing epoxy group, it can be mentioned, for example：Epoxy group, glycidyl, methylglycidyl
Glyceryl, with-A-R4[A indicates alkylidene, R to the group of expression4Indicate alicyclic epoxy group].As above-mentioned A (alkylidene), can arrange
Citing is such as：The carbon atom numbers 1~18 such as methylene, methylmethylene, dimethylated methylene base, ethylidene, propylidene, trimethylene
The alkylidene etc. of straight or branched.As above-mentioned R4, it can be mentioned, for example：Epoxycyclohexyl etc..
More specifically, as the above-mentioned silicone derivative containing epoxy group, it can be mentioned, for example：[2- (3- { the oxygen of 2,4- bis-
Miscellaneous bicyclic [4.1.0] heptyl }) ethyl] -2,4,6,6,8,8- hexamethyls-cyclotetrasiloxane, the [2- (3- { oxabicyclos of 4,8- bis-
[4.1.0] heptyl }) ethyl] -2,2,4,6,6,8- hexamethyls-cyclotetrasiloxane, the [2- (3- { oxabicyclos [4.1.0] of 2,4- bis-
Heptyl }) ethyl] -6,8- dipropyl -2,4,6,8- tetramethyls-cyclotetrasiloxane, the [2- (3- { oxabicyclos [4.1.0] of 4,8- bis-
Heptyl }) ethyl] -2,6- dipropyl -2,4,6,8- tetramethyls-cyclotetrasiloxane, the [2- (3- { oxabicyclos of 2,4,8- tri-
[4.1.0] heptyl }) ethyl] -2,4,6,6,8- pentamethyls-cyclotetrasiloxane, the [2- (3- { oxabicyclos [4.1.0] of 2,4,8- tri-
Heptyl }) ethyl] -6- propyl -2,4,6,8- tetramethyls-cyclotetrasiloxane, the [2- (3- { oxabicyclos [4.1.0] of 2,4,6,8- tetra-
Heptyl }) ethyl] -2,4,6,8- tetramethyls-cyclotetrasiloxane etc..
In addition, as the above-mentioned silicone derivative containing epoxy group, it can be mentioned, for example：The chemical combination indicated with following formula (5)
Object (chain polysiloxanes).
[chemical formula 10]
In above-mentioned formula (5), R5、R6It is identical or different, indicate the monovalent organic group containing epoxy group, alkoxy (for example,
The alkoxy etc. of the carbon atom numbers such as methoxyl group, ethyoxyl 1~4), alkyl is (for example, the alkane of the carbon atom numbers such as methyl, ethyl 1~4
Base etc.) or aryl (for example, aryl etc. of the carbon atom numbers such as phenyl, naphthalene 6~12).Wherein, in the compound indicated with formula (5)
R5And R6In, at least one (being preferably at least 2) is the monovalent organic group containing epoxy group.As one containing epoxy group
Valence organic group can be enumerated and identical group in above-mentioned formula (4).Especially from the viewpoint of curability, preferably R6Appoint
Meaning one or both is the monovalent organic group containing epoxy group.In addition, q in formula (5) indicate 1 or more integer (for example, 1~
500 integer).The structure marked in the bracket of q may be the same or different respectively.In addition, when in the bracket as mark q
Structure there are it is two or more when, addition form is not particularly limited, and can be random, or block type.
As the above-mentioned silicone derivative containing epoxy group, can for example enumerate in addition to this：Organosilicon with epoxy group
Resin (for example, in organic siliconresin etc. containing alicyclic epoxy group described in Japanese Unexamined Patent Publication 2008-248169 bulletins) has
The silsesquioxane of epoxy group in 1 molecule (for example, having at least 2 described in Japanese Unexamined Patent Publication 2008-19422 bulletins
Organic polysilsesquioxane resins etc. of a epoxy functional group) etc..
Wherein, it as epoxy resin (A), is more effectively carried out from the solidification of curable epoxy resin composition can be made
Aspect is set out, and preferably bisphenol A type epoxy resin, intramolecular have isocyanuric acid ester, the phenolic varnish type of 1 or more epoxy group
There is the siloxanes of 1 or more epoxy group to spread out for epoxy resin, cycloaliphatic epoxy, aliphatic epoxy compound, intramolecular
Biology.In particular, from the solidfied material aspect that can obtain the transparency and excellent in te pins of durability with high productivity, it is of the invention
In curable epoxy resin composition, as epoxy resin (A), cycloaliphatic epoxy is preferably comprised as neccessary composition.
As above-mentioned cycloaliphatic epoxy, particularly preferably intramolecular has compound (the especially intramolecular of epoxycyclohexyl
Compound with 2 or more epoxycyclohexyls), more preferably is indicated with formula (1) compound (be especially with formula (1-1) table
The compound shown).
In the curable epoxy resin composition of the present invention, epoxy resin (A) can be used alone, can also two
Kind combination of the above uses.It should be noted that epoxy resin (A) can also be manufactured by known or customary way, also may be used
To use commercially available product.
The content (use level) of epoxy resin (A) in the curable epoxy resin composition of the present invention does not limit especially
It is fixed, relative to the total amount (100 weight %) of curable epoxy resin composition, preferably 25~99.8 weight % (for example, 25~
95 weight %), more preferably 30~90 weight %, further preferably 35~85 weight %, particularly preferably 40~60 weights
Measure %.Content by making epoxy resin (A) is 25 weight % or more, there is the tendency that solidification can be made to be more effectively carried out.
On the other hand, by the way that the content of epoxy resin (A) is set as 99.8 weight % hereinafter, the intensity there are solidfied material further increases
Tendency.
The content (use level) of cycloaliphatic epoxy in the curable epoxy resin composition of the present invention is without spy
It does not limit, it is preferably 20~99.8 weight %, more excellent relative to the total amount (100 weight %) of curable epoxy resin composition
It is selected as 40~95 weight % (for example, 40~60 weight %), further preferably 50~95 weight %, particularly preferably 60~90
Weight %, it is most preferably 70~85 weight %.By the way that the content of cycloaliphatic epoxy is set as 20 weight % or more, exist
Solidification can be made more efficiently to carry out, the tendency that the transparency and durability of solidfied material further increase.On the other hand, pass through
The content of cycloaliphatic epoxy is set as 99.8 weight % hereinafter, there are the tendencies that the intensity of solidfied material further increases.
Total amount (the whole epoxidations for the epoxide for including in curable epoxy resin composition relative to the present invention
Close object；Such as the total amount of epoxy resin (A)) (100 weight %), the ratio of cycloaliphatic epoxy is not particularly limited, excellent
Be selected as 40~100 weight % (for example, 40~90 weight %), more preferably 80~100 weight %, further preferably 90~
100 weight %, particularly preferably 95~100 weight %.By by the ratio of cycloaliphatic epoxy be set as 40 weight % with
On, existing can be such that solidification more efficiently carries out, the tendency that the transparency and durability of solidfied material further increase.
1-2. curing agent (D)
The curing agent (D) of one of the neccessary composition of curable epoxy resin composition as the present invention, passes through to have
The compound of the cured effect of curable epoxy resin composition is reacted and made with epoxide.As curing agent (D),
It is not particularly limited, can be known those of usual used as hardener for epoxy resin, it can be mentioned, for example：Anhydride
(acid anhydride type curing agent), amine (amine curing agent), polyamide, imidazoles (imidazole curing agent), polysulfide alcohols (polysulfide
Alcohols curing agent), phenols (phenols curing agent), multi-carboxylic acid, dicyandiamide class, organic hydrazides etc..
For as the anhydride of curing agent (D) (acid anhydride type curing agent), known or usual anhydride can be used
Curing agent is not particularly limited, it can be mentioned, for example：Methyl tetrahydrophthalic anhydride (4- methyl tetrahydrophthalic anhydrides, 3-
Methyl tetrahydrophthalic anhydride etc.), methylhexahydrophthalic anhydride (4- methylhexahydrophthalic anhydrides, 3- methyl six
Hydrogen phthalic anhydride etc.), dodecenylsuccinic anhydride, methylendomethylenetetrahydrophthalic tetrabydrophthalic anhydride, phthalic anhydride,
Maleic anhydride, tetrabydrophthalic anhydride, hexahydrophthalic anhydride, methylcyclohexene dicarboxylic anhydride, pyromellitic dianhydride, inclined benzene
Three acid anhydrides, benzophenone tetracarboxylic anhydride, carbic anhydride, methylnadic anhydride, hydrogenating methyl carbic anhydride, 4- (4- first
Base -3- amylenes) tetrabydrophthalic anhydride, succinic anhydride, adipic anhydride, sebacic anhydride, dodecanedioic acid acid anhydride, methylcyclohexene
Tetracarboxylic anhydride, vinyl ether-maleic acid copolymer, ring-alkylated styrenes-copolymer-maleic anhydride etc..Wherein, from operability
Viewpoint is set out, preferably at 25 DEG C for liquid acid anhydrides [for example, methyl tetrahydrophthalic anhydride, methyl hexahydro O-phthalic
Acid anhydrides, dodecenylsuccinic anhydride, methylendomethylenetetrahydrophthalic tetrabydrophthalic anhydride etc.].On the other hand, for being at 25 DEG C
There is work for example, the mixture of liquid is made in the acid anhydrides for liquid at 25 DEG C by making it dissolve in the acid anhydrides of solid-like
The tendency improved for the operability of the curing agent (D) in the curable epoxy resin composition of the present invention.Cure as anhydride
Agent, from the viewpoint of the heat resistance of solidfied material, the transparency, the acid anhydrides for being preferably saturated monocyclic hydrocarbon dicarboxylic acids (is also contained on ring
It is bonded with those of substituent groups such as alkyl).
For as the amine of curing agent (D) (amine curing agent), known or usual amine curing agent can be used,
It is not particularly limited, it can be mentioned, for example：Ethylenediamine, diethylenetriamines, trien, tetren, two Asias third
The aliphatic polyamines such as base diamines, diethyl amino propylamine, more propylidene triamines；It is sub-It is alkyl diamine, isophorone diamine, double
(4- amino -3- methyldicyclohexyls) methane, diamino-dicyclohexyl methane, bis- (amino methyl) hexamethylenes, N- amino-ethyls
The ester ring types polyamines such as bis- four oxaspiro [5,5] undecyls of (3- aminopropyls) -3,4,8,10- of piperazine, 3,9-；M-phenylene diamine (MPD),
P-phenylenediamine, Toluene-2,4-diisocyanate, 4- diamines, Toluene-2,4-diisocyanate, 6- diamines, mesitylene -2,4- diamines, 3,5- diethyltoluenes -2,4- two
Monokaryons polyamines, benzidine, 4,4- diaminodiphenyl-methanes, the 2,5- naphthalenes two such as amine, 3,5- diethyltoluene -2,6- diamines
Aromatic polyamines such as amine, 2,6- naphthylenediamines etc..
For as the phenols of curing agent (D) (phenols curing agent), known or usual phenols curing agent can be used,
It is not particularly limited, it can be mentioned, for example：Novolak phenolics, phenolic varnish type cresol novolac resin, terephthaldehyde's base
The aralkyl resins such as phenol-formaldehyde resin modified, terephthaldehyde's base/xyxylene phenol-formaldehyde resin modified, terpene modified phenolic resin,
Dicyclic pentylene modified phenolic resin, three phenolic group propane etc..
For the polyamide as curing agent (D), it can be mentioned, for example：Intramolecular has in primary amino group and secondary amino group
Any one or both polyamide etc..
For as the imidazoles of curing agent (D) (imidazole curing agent), known or usual imidazoles can be used
Curing agent is not particularly limited, it can be mentioned, for example：2-methylimidazole, 2-ethyl-4-methylimidazole, 2- undecyl imidazoles, 2-
Heptadecyl imidazole, 2- phenylimidazoles, 1 benzyl 2 methyl imidazole, 1- 1-cyanoethyl-2-methylimidazoles, 1- cyanoethyl -2- second
Base -4-methylimidazole, 1- cyanoethyl -2- undecyl imidazoles, 1- cyanoethyl -2- undecyl imidazole trimellitic acids salt, 1-
Cyanoethyl -2- phenylimidazole trimellitic acids salt, 2-methylimidazole isocyanurate, 2- phenylimidazoles isocyanurate,
2,4- diamino -6- [2-methylimidazole base-(1)]-ethyl-s-triazine, 2,4- diamino -6- [2-ethyl-4-methylimidazoles
Base-(1)]-ethyl-s-triazine etc..
For as the polysulfide alcohols of curing agent (D) (polysulfide alcohols curing agent), it can be mentioned, for example：The polysulfide of liquid
Alcohol, thio resin etc..
For the multi-carboxylic acid as curing agent (D), it can be mentioned, for example：Adipic acid, decanedioic acid, terephthalic acid (TPA), partially
Benzenetricarboxylic acid, carboxylic polyester etc..
Wherein, preferably sour from the viewpoint of curability, the heat resistance of solidfied material, the transparency as curing agent (D)
Anhydride (acid anhydride type curing agent).It should be noted that in the curable epoxy resin composition of the present invention, curing agent (D) can
One kind is used alone, can also be used in combination.In addition, as curing agent (D), commercially available product can also be used.Example
Such as, as the commercially available product of anhydride, trade name " RIKACID MH-700 ", " RIKACID MH-700F " can be enumerated (by new day
This physics and chemistry (strain) manufactures)；Trade name " HN-5500 " (Hitachi Chemical Industries (Ltd.) manufacture) etc..
The content (use level) of curing agent (D) in the curable epoxy resin composition of the present invention is not particularly limited,
Total amount (whole epoxides relative to the epoxide for including in curable epoxy resin composition；For example, asphalt mixtures modified by epoxy resin
The total amount of fat (A)) 100 parts by weight, preferably 50~200 parts by weight, more preferably 75~150 parts by weight are more preferably
100~120 parts by weight.More specifically, in the case where using anhydride as curing agent (D), preferably with relative to this hair
Every 1 equivalent of epoxy group in the whole epoxides for including in bright curable epoxy resin composition is 0.5~1.5 equivalent
Ratio used.By the way that the content of curing agent (D) is set as 50 parts by weight or more, exist can make solidification more effectively into
It goes, the tendency that the obdurability of solidfied material further increases.On the other hand, by the way that the content of curing agent (D) is set as 200 parts by weight
Hereinafter, there are non-coloring (or coloring less), being easy to get the tendency of the excellent solidfied material of form and aspect.
1-3. curing accelerators (E)
The curing accelerator (E) of one of the neccessary composition of curable epoxy resin composition as the present invention, to have
Promote the change of the function of the reaction speed of the reaction (especially epoxy resin (A) and curing agent (D) react) of epoxide
Close object., can be known those of usual used as epoxy resin curing accelerator as curing accelerator (E), do not have
It is particularly limited to, it can be mentioned, for example：1,8- diazabicyclo [5.4.0] endecatylene -7 (DBU) and its salt are (for example, phenates, pungent
Hydrochlorate, tosilate, formates, tetraphenyl borate salts etc.)；1,5- diazabicyclos [4.3.0] nonene -5 (DBN) and
Its salt (for example, phenates, caprylate, tosilate, formates, tetraphenyl borate salts etc.)；Benzyl dimethylamine, 2,4,6- tri-
(dimethylaminomethyl) phenol, N, the tertiary amines such as N- dimethylcyclohexylam,nes；2-ethyl-4-methylimidazole, 1- cyanoethyl -2- second
The imidazoles such as base -4-methylimidazole；The phosphines such as phosphate, triphenylphosphine；TetraphenylFour (p-methylphenyl) borate Deng Phosphonium chemical combination
Object；The organic metal salts such as tin octoate, zinc octoate；Metallo-chelate etc..
It should be noted that in the curable epoxy resin composition of the present invention, curing accelerator (E) can individually make
With one kind, can also be used in combination.
As the curing accelerator (E) in the curable epoxy resin composition of the present invention, can use for example：Trade name
" U-CAT SA 506 ", " U-CAT SA 102 ", " U-CAT 5003 ", " U-CAT 18X ", " 12XD " (exploitation product) (above by
San Apro (strain) are manufactured)；Trade name " TPP-K ", " TPP-MK " (being manufactured above by the emerging chemical industry (strain) in north)；Trade name
Commercially available products such as " PX-4ET " (Japan Chemical Industry (strain) manufactures).
The content (use level) of curing accelerator (E) in the curable epoxy resin composition of the present invention does not limit especially
It is fixed, total amount (whole epoxides relative to the epoxide for including in curable epoxy resin composition；For example, ring
The total amount of oxygen resin (A)) 100 parts by weight, preferably 0.05~5 parts by weight, more preferably 0.1~3 parts by weight, further preferably
For 0.2~3 parts by weight, particularly preferably 0.25~2.5 parts by weight.By the way that the content of curing accelerator (E) is set as 0.05 weight
Part or more is measured, there is the tendency that can obtain more fully curing facilitation effect.On the other hand, by by curing accelerator (E)
Content be set as 5 parts by weight hereinafter, in the presence of the tendency for being easy to get non-coloring (or coloring less), the excellent solidfied material of form and aspect.
1-4. curing catalysts (F)
The curing catalysts (F) of one of the neccessary composition of curable epoxy resin composition as the present invention, to have
Make curability by causing and/or promoting curing reaction (polymerisation) of the cationically polymerizables compound such as epoxide
The compound of the effect of epoxy resin composition.As curing catalysts (F), it is not particularly limited, it can be mentioned, for example：It is logical
It overheats and generates cation kind to cause cationic polymerization initiators (hot cationic polymerization), the Louis of polymerization
Acid-amine complex, Bronsted Barbiturates, imidazoles etc..
Specifically, as curing catalysts (F), it can be mentioned, for example：Aryl diazonium salts, aryl iodideSalt, aryl sulfonium salt,
It is preferable to use trade name " PP-33 ", " CP-66 ", " CP-77 " (above by (strain) ADEKA for allene-ionic complex etc.
Manufacture)；Trade name " FC-509 " (3M systems)；Trade name " UVE1014 " (G.E. systems)；Trade name " San-Aid SI-60L ",
" San-Aid SI-80L ", " San-Aid SI-100L ", " San-Aid SI-110L ", " San-Aid SI-150L " (above by
Three new chemical industry (strain) manufactures)；The commercially available products such as trade name " CG-24-61 " (BASF AG's system).Further, it is urged as solidification
Agent (F), also it can be mentioned, for example：The metals such as aluminium, titanium and acetoacetate or the chelate compound and tri-phenyl-silane alcohol of diones
The phenols such as metals and the chelate compound and bisphenol S of acetoacetate or diones such as the compound of equal silanols formation or aluminium, titanium
The compound etc. of formation.
For lewis acid-amine complex as curing catalysts (F), known or usual Louis can be used
Acid-amine complex class curing catalysts, is not particularly limited, it can be mentioned, for example：BF3N- hexylamines, BF3Mono aminoethane, BF3·
Benzylamine, BF3Diethylamine, BF3Piperidines, BF3Triethylamine, BF3Aniline, BF4N-hexylamine, BF4Mono aminoethane, BF4·
Benzylamine, BF4Diethylamine, BF4Piperidines, BF4Triethylamine, BF4Aniline, PF5Ethamine, PF5Isopropylamine, PF5Fourth
Amine, PF5Lauryl amine, PF5Benzylamine, AsF5Lauryl amine etc..
For the Bronsted Barbiturates as curing catalysts (F), known or usual Bu Langsi can be used
Platform moral Barbiturates, is not particularly limited, it can be mentioned, for example：Aliphatic sulfonium salt, aromatic series sulfonium salt, salt compounded of iodine, microcosmic salt etc..
For the imidazoles as curing catalysts (F), known or usual imidazoles can be used, are not limited especially
It is fixed, it can be mentioned, for example：2-methylimidazole, 2-ethyl-4-methylimidazole, 2- undecyl imidazoles, 2- heptadecyl imidazoles, 2- benzene
Base imidazoles, 1 benzyl 2 methyl imidazole, 1- 1-cyanoethyl-2-methylimidazoles, 1- cyanoethyls -2-ethyl-4-methylimidazole, 1- cyanogen
Ethyl -2- undecyl imidazoles, 1- cyanoethyl -2- undecyl imidazole trimellitic acids salt, 1-cyanoethyl-2-phenylimidazole
Trimellitic acid salt, 2-methylimidazole isocyanuric acid ester, 2- phenylimidazoles isocyanuric acid ester, 2,4- diamino -6- [2- methyl
Imidazole radicals-(1)]-ethyl-s-triazine, 2,4- diamino -6- [2-ethyl-4-methylimidazole base-(1)]-ethyl-s-triazine etc..
It should be noted that in the curable epoxy resin composition of the present invention, curing catalysts (F) can individually make
With one kind, can also be used in combination.It should be noted that as described above, as curing catalysts (F), such as can
To use commercially available product.
The content (use level) of curing catalysts (F) in the curable epoxy resin composition of the present invention does not limit especially
It is fixed, total amount (whole epoxides relative to the epoxide for including in curable epoxy resin composition；For example, ring
The total amount of oxygen resin (A)) 100 parts by weight, preferably 0.01~15 parts by weight, more preferably 0.01~12 parts by weight, further
Preferably 0.05~10 parts by weight, particularly preferably 0.05~8 parts by weight.By the way that the content of curing catalysts (F) is set as
More than 0.01 parts by weight, there is the tendency that curing reaction can be made more fully to carry out.On the other hand, by by curing catalysts
(F) content be set as 15 parts by weight hereinafter, in the presence of be easy to get non-coloring (or coloring less), the excellent solidfied material of form and aspect inclines
To.That is, by controlling the content of curing catalysts (F) to above range, there are the solidifications of curable epoxy resin composition
Speed improves and is easy to get the tendency of the excellent solidfied material in terms of the transparency and the balance of durability.
It should be noted that the curable epoxy resin composition of the present invention can also substantially include the irradiation by light
And generate the light cationic polymerization initiator of the initiation kind (acid etc.) of cationic polymerization.In the curable epoxy resin group of the present invention
In the case that conjunction object includes light cationic polymerization initiator, such as relative to the epoxy for including in curable epoxy resin composition
Total amount (whole epoxides of compound；For example, the total amount of epoxy resin (A)) 100 parts by weight, content is such as 0.01
~20 parts by weight or so, preferably 0.1~10 parts by weight.
1-5. polyalcohol
The curable epoxy resin composition of the present invention can include polyalcohol.In particular, from the curability in the present invention
Composition epoxy resin includes that can make the side that solidification is more effectively carried out in the case of curing agent (D) and curing accelerator (E)
Face is set out, and includes preferably further polyalcohol.As polyalcohol, known or usual polyalcohol can be used, is not limited especially
It is fixed, it can be mentioned, for example：Ethylene glycol, propylene glycol, butanediol, 1,3 butylene glycol, 1,4- butanediols, 1,6-HD, diethylene glycol,
Triethylene glycol, neopentyl glycol, polyethylene glycol, polypropylene glycol, polytetramethylene glycol, trimethylolpropane, glycerine, pentaerythrite, two seasons
Penta tetrol etc..
Wherein, as above-mentioned polyalcohol, it is less susceptible to occur cracking, stripping from solidification can be well controllled, be easy to get
Solidfied material in terms of set out, preferably the aklylene glycol of carbon atom number 1~6, more preferably carbon atom number 2~4 alkylene
Base glycol.
The present invention curable epoxy resin composition in, polyalcohol can be used alone, can also two kinds with
On be applied in combination.
The content (use level) of polyalcohol in the curable epoxy resin composition of the present invention is not particularly limited, relatively
Total amount (the whole epoxides for the epoxide for including in curable epoxy resin composition；For example, epoxy resin
(A) total amount) 100 parts by weight, preferably 0.05~5 parts by weight, more preferably 0.1~3 parts by weight, further preferably 0.2
~3 parts by weight, particularly preferably 0.25~2.5 parts by weight.By the way that the content of polyalcohol is set as 0.05 parts by weight or more, exist
The tendency that solidification can be made to be more effectively carried out.On the other hand, by the content of polyalcohol is set as 5 parts by weight hereinafter, in the presence of
It is easy to control the tendency of above-mentioned cured reaction speed.
1-6. fluorophor
The curable epoxy resin composition of the present invention can include fluorophor.In the curable epoxy resin group of the present invention
It, can be particularly preferable as the seal applications of the optical semiconductor in optical semiconductor device in the case that conjunction object includes fluorophor
(sealant use), i.e. optical semiconductor sealing are used with resin combination.As above-mentioned fluorophor, can use known or used
Fluorophor (fluorophor especially used in the seal applications of optical semiconductor), is not particularly limited, can arrange
Citing is such as：With general formula A3B5O12:[in formula, A is indicated selected from one or more of Y, Gd, Tb, La, Lu, Se and Sm element, B tables M
Show that, selected from one or more of Al, Ga and In element, M is indicated selected from one or more of Ce, Pr, Eu, Cr, Nd and Er element]
The phosphor particles of the YAG classes of expression are (for example, Y3Al5O12:Ce phosphor particles, (Y, Gd, Tb)3(Al,Ga)5O12:Ce fluorescence
Body particle etc.), silicate-based phosphors particle is (for example, (Sr, Ca, Ba)2SiO4:Eu etc.) etc..It should be noted that being, for example,
Dispersibility is improved, fluorophor can also be that surface is repaiied using organic group (for example, chain alkyl, phosphate etc.) etc.
Those of decorations.The present invention curable epoxy resin composition in, fluorophor can be used alone, can also two kinds with
On be applied in combination.In addition, as fluorophor, commercially available product can be used.
The content (use level) of fluorophor in the curable epoxy resin composition of the present invention is not particularly limited, can be with
It is suitably selected in the range of the total amount (100 weight %) relative to curable epoxy resin composition is 0.5~20 weight %.
The other ingredients of 1-7.
In the range of will not cause notable harmful effect to curability, transparency etc., curability asphalt mixtures modified by epoxy resin of the invention
Oil/fat composition can also include other ingredients other than the above.As above-mentioned other ingredients, it can be mentioned, for example：With straight chain or branch
The organic silicon resin of chain, the organic silicon resin with alicyclic ring, the organic silicon resin with aromatic ring, cage modle/ladder type/random
The defoaming of the silane coupling agents, organic silicon, fluorine class such as silsesquioxane, the γ-glycidoxypropyltrime,hoxysilane of type
Agent etc..The content (use level) of above-mentioned other ingredients is not particularly limited, the total amount relative to curable epoxy resin composition
(100 weight %), preferably 5 weight % or less (for example, 0~3 weight %).
The present invention curable epoxy resin composition be not particularly limited, such as can by by above-mentioned each ingredient according to
It needs to be stirred in the state of heated, mix and prepare.It should be noted that the curable epoxy resin group of the present invention
The composition that object can be the direct one-pack type using mixture made of being all pre-mixed each ingredient is closed, can also be
Such as the multigroup parting for using the ingredient for being divided into 2 parts or more to be mixed to certainty ratio immediately before use is (for example, double groups
Parting) composition.Stirring, the method mixed are not particularly limited, and can use the various mixing such as disperser, homogenizer
Known in device, kneader, roller, ball mill, rotation-revolution formula agitating device etc. or usual stirring, mixed organization.Alternatively, it is also possible to
Deaeration is carried out under reduced pressure or under vacuum after stirring, mixing.
2. curable silicone resin composition
Above-mentioned curable silicone resin composition (also referred to as " curable silicone resin composition of the invention ") is
Include solidification compound of the organic siliconresin (B) as curability compound as neccessary composition.The curability of the present invention
Organosilicon resin composition can also include the ingredient other than organic siliconresin (B).
As organic siliconresin (B), it can be mentioned, for example：Not only contain-Si-O-Si- (siloxanes key) as main chain, also contains
There is-Si-RA- Si- (silicon alkylene bonds：RAIndicate alkylidene) poly-organosilicon oxygroup silicon alkylidene；As main chain without containing above-mentioned
The curability polysiloxanes such as polysiloxane of silicon alkylene bond.
In addition, as organic siliconresin (B), curability that can be known or usual used as curability compound has
Machine silicones (curability polysiloxanes), is not particularly limited, it can be mentioned, for example：Add-on type (addition reaction curing type) it is organic
The organic siliconresin etc. of silicones, condensed type (condensation reaction curing type).In the curable silicone resin composition of the present invention
Including in the case of the former, it can be used as addition reaction curable silicone resin composition, comprising the latter the case where
Under, it can be used as condensation reaction curable silicone resin composition.Hereinafter, to these addition reaction curable silicones
Resin combination and condensation reaction curable silicone resin composition illustrate, but the curable silicone resin of the present invention
Composition is not limited to these, can also be for example the organic siliconresin of the organic siliconresin comprising add-on type and condensed type this
The two, the organosilicon resin composition that is cured by addition reaction and condensation reaction.That is, in above-mentioned curing process
The solidification of curable silicone resin composition can be by being selected from least one of addition reaction and condensation reaction reaction
And carry out.
2-1. addition reaction curable silicone resin compositions
As above-mentioned addition reaction curable silicone resin composition, it can be mentioned, for example：Containing as organic siliconresin
(B) in the molecule with 2 or more alkenyls polysiloxanes (B1) and further as needed and include to have in the molecule
The curable silicone tree of the polysiloxanes, metallic curing catalyst of 1 or more (preferably 2 or more) hydrosilyl etc.
Oil/fat composition.
Above-mentioned polysiloxanes (B1) can be divided into polysiloxane (B1-1) and poly-organosilicon oxygroup silicon alkylidene (B1-2).
In the present specification, poly-organosilicon oxygroup silicon alkylidene (B1-2) refers to：Intramolecular has 2 or more alkenyls, is removed as main chain
Also contain-Si-R other than-Si-O-Si- (siloxanes key)A- Si- (silicon alkylene bonds：RAIndicate alkylidene) polysiloxanes.
Also, the polysiloxane (B1-1) in this specification, which is intramolecular, has 2 or more alkenyls and as main chain without containing upper
State the polysiloxanes of silicon alkylene bond.
As polysiloxane (B1-1), can enumerate with straight-chain, branched (a part of straight chain with branch
Shape, branched, netted etc.) those of molecular structure.It should be noted that polysiloxane (B1-1) can be used alone
One kind can also be used in combination.Furthermore it is also possible to which different poly- organic of two or more molecular structures is applied in combination
Siloxanes (B1-1), such as the poly organo of polysiloxane (B1-1) and branched of straight-chain can also be applied in combination
Alkane (B1-1).
Alkenyl possessed by intramolecular as polysiloxane (B1-1) can enumerate vinyl, allyl, butylene
The substituted or unsubstituted alkenyl such as base, pentenyl, hexenyl.As substituent group, halogen atom, hydroxyl, carboxyl etc. can be enumerated.Wherein,
As alkenyl, preferably vinyl.In addition, polysiloxane (B1-1) can have only a kind of poly organo of alkenyl
Alkane can also be the polysiloxane with two or more alkenyls.Though being not particularly limited, preferred polysiloxane
(B1-1) alkenyl possessed by is and silicon atom bonding.
The possessed group in addition to alkenyl with silicon atom bonding of polysiloxane (B1-1) is not limited especially
It is fixed, it can be mentioned, for example：Hydrogen atom, monovalent organic group etc..As monovalent organic group, it can be mentioned, for example：Alkyl is [for example, first
Base, ethyl, propyl, butyl, amyl, hexyl etc.], naphthenic base is [for example, cyclopropyl, cyclobutyl, cyclopenta, cyclohexyl, ring 12
Alkyl etc.], aryl [for example, phenyl, tolyl, xylyl, naphthalene etc.], naphthenic base-alkyl is [for example, cyclohexyl methyl, first
Butylcyclohexyl etc.], aralkyl [for example, benzyl, phenethyl etc.], 1 or more hydrogen atom in alkyl is replaced by halogen atom
The monovalencies such as halohydrocarbyl [for example, halogenated alkyls such as chloromethyl, 3- chloropropyls, 3,3,3- trifluoro propyls etc.] substitution or without taking
For alkyl etc..It should be noted that " group with silicon atom bonding " is often referred to the group without containing silicon atom in this specification.
In addition, as the group with silicon atom bonding, it is possible to have hydroxyl, alkoxy.
The character of polysiloxane (B1-1) is not particularly limited, and can be liquid, or solid-like.
As polysiloxane (B1-1), the polysiloxane preferably indicated with following averaged unit formulas.
(R7SiO3/2)a1(R7 2SiO2/2)a2(R7 3SiO1/2)a3(SiO4/2)a4(ZO1/2)a5
In above-mentioned averaged unit formula, R7It is identical or different, it is the substituted or unsubstituted alkyl of monovalence, above-mentioned tool can be enumerated
Body example (for example, alkyl, alkenyl, aryl, aralkyl, halohydrocarbyl etc.).Wherein, R7A part be alkenyl (especially ethylene
Base), ratio is controlled in the range for 2 or more in the molecule.For example, relative to R7Total amount (100 moles of %) alkene
The ratio of base is preferably 0.1~40 mole of %.By the way that the ratio of alkenyl is controlled in above range, there are curable silicone trees
The tendency that the curability of oil/fat composition further increases.In addition, as the R in addition to alkenyl7, preferably alkyl (especially first
Base), aryl (especially phenyl).
In above-mentioned averaged unit formula, Z is hydrogen atom or alkyl.As alkyl, methyl, ethyl, propyl, fourth can be enumerated
Base, amyl, hexyl etc., particularly preferably methyl.
In above-mentioned averaged unit formula, a1 is 0 or positive number, a2 are 0 or positive number, a3 are 0 or positive number, a4 are 0 or positive number, a5
For 0 or positive number, and (a1+a2+a3) is positive number.
Poly-organosilicon oxygroup silicon alkylidene (B1-2) is as described above, be to have 2 or more alkenyls in the molecule, as main chain
The not only polysiloxane containing siloxanes key also containing silicon alkylene bond.It should be noted that as above-mentioned silicon alkylidene
Alkylidene in key, preferably C2-4Alkylidene (especially ethylidene).Compared with polysiloxane (B1-1), above-mentioned poly- have
Machine siloxy silicon alkylidene (B1-2) is not likely to produce the ring of low molecular weight in manufacturing process, and is not easy to decompose simultaneously because of heating
Silanol group (- SiOH) is generated, therefore, using poly-organosilicon oxygroup silicon alkylidene (B1-2), there are curability
The surface adhesiveness (viscosity) of the solidfied material of organosilicon resin composition is lower, is more not easy the tendency of xanthochromia.
As poly-organosilicon oxygroup silicon alkylidene (B1-2), can enumerate (a part of that there is branch with straight-chain, branched
Straight-chain, branched, netted etc.) those of molecular structure.It should be noted that poly-organosilicon oxygroup silicon alkylidene (B1-
2) it can be used alone, can also be used in combination.Such as two or more molecular structures can be applied in combination
Different poly-organosilicon oxygroup silicon alkylidenes (B1-2), such as the poly-organosilicon oxygroup silicon alkylene of straight-chain can also be applied in combination
The poly-organosilicon oxygroup silicon alkylidene (B1-2) of base (B1-2) and branched.
Alkenyl possessed by intramolecular as poly-organosilicon oxygroup silicon alkylidene (B1-2), can enumerate above-mentioned concrete example,
But wherein preferred vinyl.In addition, poly-organosilicon oxygroup silicon alkylidene (B1-2) can have only a kind of alkenyl, it is possible to have
Two or more alkenyls.Though be not particularly limited, alkenyl possessed by preferred poly-organosilicon oxygroup silicon alkylidene (B1-2) be with
Silicon atom bonding.
The possessed group in addition to alkenyl with silicon atom bonding of poly-organosilicon oxygroup silicon alkylidene (B1-2) does not have
It is particularly limited to, it can be mentioned, for example：Hydrogen atom, monovalent organic group etc..As monovalent organic group, it can be mentioned, for example：Above-mentioned one
Substituted or unsubstituted alkyl of valence etc..Wherein, preferably alkyl (especially methyl), aryl (especially phenyl).
In addition, as the group with silicon atom bonding, it is possible to have hydroxyl, alkoxy.
The character of poly-organosilicon oxygroup silicon alkylidene (B1-2) is not particularly limited, can be liquid, or Gu
Body shape.
As poly-organosilicon oxygroup silicon alkylidene (B1-2), the poly organo preferably indicated with following averaged unit formulas
Base silicon alkylidene.
(R8 2SiO2/2)b1(R8 3SiO1/2)b2(R8SiO3/2)b3(SiO4/2)b4(RA)b5(ZO1/2)b6
In above-mentioned averaged unit formula, R8It is identical or different, it is the substituted or unsubstituted alkyl of monovalence, above-mentioned tool can be enumerated
Body example (for example, alkyl, alkenyl, aryl, aralkyl, halogenated alkyl etc.).Wherein, R8A part be alkenyl (especially ethylene
Base), ratio is controlled in the range for 2 or more in the molecule.For example, relative to R8Total amount (100 moles of %) alkene
The ratio of base is preferably 0.1~40 mole of %.By the way that the ratio of alkenyl is controlled in above range, there are curable silicone trees
The tendency that the curability of oil/fat composition further increases.In addition, as the R in addition to alkenyl8, optimizing alkyl (especially first
Base), aryl (especially phenyl).
In above-mentioned averaged unit formula, RAAs described above, being alkylidene.Particularly preferably ethylidene.
In above-mentioned averaged unit formula, Z is same as described above, is hydrogen atom or alkyl.As alkyl, methyl, second can be enumerated
Base, propyl, butyl, amyl, hexyl etc., particularly preferably methyl.
In above-mentioned averaged unit formula, b1 is positive number, b2 is positive number, b3 is 0 or positive number, b4 are 0 or positive number, b5 are just
Number, b6 are 0 or positive number.Wherein, b1 be preferably 1~200, b2 be preferably 1~200, b3 be preferably 0~10, b4 be preferably 0~5,
B5 is preferably 1~100.Especially in the case where (b3+b4) is positive number, further increased there are the mechanical strength of solidfied material
Tendency.
Above-mentioned addition reaction curable silicone resin composition has 1 as set forth above, it is possible to further include intramolecular
Polysiloxanes (also referred to as " the poly- silicon of containing hydrogenated silicyl of a above (preferably 2 or more) hydrosilyl (Si-H)
Oxygen alkane ").The polysiloxanes of above-mentioned containing hydrogenated silicyl is divided into the polysiloxane and containing hydrogenated first of containing hydrogenated silicyl
The poly-organosilicon oxygroup silicon alkylidene of silylation.In the present specification, the poly-organosilicon oxygroup silicon alkylene of containing hydrogenated silicyl
Base refers to that intramolecular has 1 or more hydrosilyl and not only contains-Si-O-Si- (siloxanes key) also as main chain
Contain-Si-RA- Si- (silicon alkylene bonds：RAIndicate alkylidene) polysiloxanes.In addition, the containing hydrogenated first silicon in this specification
The polysiloxane of alkyl has 1 or more hydrosilyl for intramolecular and does not contain above-mentioned silicon alkylene as main chain
The polysiloxanes of base key.It should be noted that as RA(alkylidene), same as described above, it can be mentioned, for example straight or brancheds
C1-12The C of alkylidene, preferably straight or branched2-4Alkylidene (especially ethylidene).
As the polysiloxane of above-mentioned containing hydrogenated silicyl, can enumerate with straight-chain, branched (part tool
Have the straight-chain of branch, branched, netted etc.) those of molecular structure.It should be noted that above-mentioned containing hydrogenated silicyl
Polysiloxane can be used alone, can also be used in combination.Two or more points can be applied in combination
The polysiloxane of the different containing hydrogenated silicyl of minor structure, for example, it is also possible to which the containing hydrogenated first of straight-chain is applied in combination
The polysiloxane of the polysiloxane of silylation and the containing hydrogenated silicyl of branched.
In group possessed by the polysiloxane of above-mentioned containing hydrogenated silicyl with silicon atom bonding, dehydrogenation is former
Group other than son is not particularly limited, and it can be mentioned, for example the substituted or unsubstituted alkyl of above-mentioned monovalence, more specifically, can arrange
Lift alkyl, aryl, aralkyl, halohydrocarbyl etc..Wherein, preferably alkyl (especially methyl), aryl (especially phenyl).Separately
Outside, in the polysiloxane of above-mentioned containing hydrogenated silicyl, as the group with silicon atom bonding in addition to hydrogen atom,
There can be alkenyl (such as vinyl).
The character of the polysiloxane of above-mentioned containing hydrogenated silicyl is not particularly limited, and can be liquid, can also
For solid-like.Wherein preferred liquid, the more preferably viscosity at 25 DEG C are the liquid of 0.1~1000000000mPas.
As the polysiloxane of above-mentioned containing hydrogenated silicyl, preferably indicate poly- organic with following averaged unit formulas
Siloxanes.
(R9SiO3/2)c1(R9 2SiO2/2)c2(R9 3SiO1/2)c3(SiO4/2)c4(ZO1/2)c5
In above-mentioned averaged unit formula, R9It is identical or different, it, can for hydrogen atom or substitution or the unsubstituted alkyl of monovalence
Enumerate hydrogen atom, above-mentioned concrete example (for example, alkyl, alkenyl, aryl, aralkyl, halogenated alkyl etc.).Wherein, R9A part
For hydrogen atom the hydrogen atom of hydrosilyl (constitute), ratio is controlled in that make hydrosilyl in the molecule be 1
The range of (preferably 2 or more) above.For example, relative to R9The ratio of hydrogen atom of total amount (100 moles of %) be preferably
0.1~40 mole of %.By the way that the ratio of hydrogen atom is controlled in above range, there are consolidating for curable silicone resin composition
The tendency that the property changed further increases.In addition, as the R in addition to hydrogen atom9, preferably alkyl (especially methyl), aryl be (special
It is not phenyl).
In above-mentioned averaged unit formula, Z is same as described above, is hydrogen atom or alkyl.As alkyl, methyl, second can be enumerated
Base, propyl, butyl, amyl, hexyl etc., particularly preferably methyl.
In above-mentioned averaged unit formula, c1 is 0 or positive number, c2 are 0 or positive number, c3 are 0 or positive number, c4 are 0 or positive number, c5
For 0 or positive number, and (c1+c2+c3) is positive number.
The poly-organosilicon oxygroup silicon alkylidene of above-mentioned containing hydrogenated silicyl as described above, be have in the molecule 1 with
Upper hydrosilyl and as the main chain not only polysiloxane containing siloxanes key also containing silicon alkylene bond.It needs
Illustrate, as the alkylidene in above-mentioned silicon alkylene bond, preferably such as C2-4Alkylidene (especially ethylidene).Due to
Compared with the polysiloxane of above-mentioned containing hydrogenated silicyl, the poly-organosilicon oxygroup silicon alkylene of above-mentioned containing hydrogenated silicyl
Base is not likely to produce the ring of low molecular weight in manufacturing process, and be not easy because heating etc. due tos decompose and generate silanol group (-
SiOH), therefore, in the case of the poly-organosilicon oxygroup silicon alkylidene for stating containing hydrogenated silicyl in use, there are curability
The surface adhesiveness of the solidfied material of organosilicon resin composition is lower, is less susceptible to that the tendency of xanthochromia occurs.
As the poly-organosilicon oxygroup silicon alkylidene of above-mentioned containing hydrogenated silicyl, can enumerate with straight-chain, branched
Those of the molecular structure of (a part of branch has straight-chain, branched, netted etc.).It should be noted that above-mentioned containing hydrogenated
The poly-organosilicon oxygroup silicon alkylidene of silicyl can be used alone, and can also be used in combination.It can group
The poly-organosilicon oxygroup silicon alkylidene using the different containing hydrogenated silicyl of two or more molecular structures is closed, for example, it is also possible to
The poly-organosilicon oxygroup silicon alkylidene of the containing hydrogenated silicyl of straight-chain and the containing hydrogenated silicyl of branched is applied in combination
Poly-organosilicon oxygroup silicon alkylidene.
It is former with silicon in addition to hydrogen atom possessed by the poly-organosilicon oxygroup silicon alkylidene of above-mentioned containing hydrogenated silicyl
The group that sub-key is closed is not particularly limited, and it can be mentioned, for example monovalent organic groups etc..As monovalent organic group, example can be enumerated
Such as：Substituted or unsubstituted alkyl of above-mentioned monovalence etc..Wherein, preferably alkyl (especially methyl), aryl (especially phenyl).
The character of the poly-organosilicon oxygroup silicon alkylidene of above-mentioned containing hydrogenated silicyl is not particularly limited, and can be liquid
State, or solid-like.
As the poly-organosilicon oxygroup silicon alkylidene of above-mentioned containing hydrogenated silicyl, preferably indicated with following averaged unit formulas
Poly-organosilicon oxygroup silicon alkylidene.
(R10 2SiO2/2)d1(R10 3SiO1/2)d2(R10SiO3/2)d3(SiO4/2)d4(RA)d5(ZO1/2)d6
In above-mentioned averaged unit formula, R10It is identical or different, it is hydrogen atom or the substituted or unsubstituted alkyl of monovalence, can arranges
Lift hydrogen atom and above-mentioned concrete example (for example, alkyl, alkenyl, aryl, aralkyl, halogenated alkyl etc.).Wherein, R10A part be
Hydrogen atom, ratio are controlled in the molecule as the range of 1 or more (preferably 2 or more).For example, relative to R10It is total
The ratio for measuring the hydrogen atom of (100 moles of %) is preferably 0.1~50 mole of %, more preferably 5~35 moles of %.By the way that hydrogen is former
The ratio of son is controlled in above range, and there are the tendencies that the curability of curable silicone resin composition further increases.Separately
Outside, as the R in addition to hydrogen atom10, preferably alkyl (especially methyl), aryl (especially phenyl).In particular, relative to
R10Total amount (100 moles of %), the ratio of aryl (especially phenyl) be preferably 5 moles of % or more (such as 5~80 moles of %),
More preferably 10 moles of % or more.
In above-mentioned averaged unit formula, RAAs described above, being alkylidene.Particularly preferably ethylidene.
In above-mentioned averaged unit formula, Z is same as described above, is hydrogen atom or alkyl.As alkyl, methyl, second can be enumerated
Base, propyl, butyl, amyl, hexyl etc., particularly preferably methyl.
In above-mentioned averaged unit formula, d1 is positive number, d2 is positive number, d3 is 0 or positive number, d4 are 0 or positive number, d5 are just
Number, d6 are 0 or positive number.Wherein, it be preferably 1~50, d3 be preferably 0~10, d4 is preferably 0~5, d5 that d1, which is preferably 1~50, d2,
Preferably 1~30.
It, can as the polysiloxanes of the containing hydrogenated silicyl in above-mentioned addition reaction curable silicone resin composition
Using only the polysiloxane of containing hydrogenated silicyl, the poly-organosilicon oxygroup of containing hydrogenated silicyl can also be used only
Silicon alkylidene, furthermore it is also possible to which the polysiloxane of containing hydrogenated silicyl and gathering for containing hydrogenated silicyl is applied in combination
Organosiloxy silicon alkylidene.In the poly- of the polysiloxane and containing hydrogenated silicyl that containing hydrogenated silicyl is applied in combination
In the case of organosiloxy silicon alkylidene, their ratio is not particularly limited, and can suitably set.
Above-mentioned addition reaction curable silicone resin composition is not particularly limited, preferably relative to curable resin
1 mole of hydrosilyl present in composition, alkenyl are to form (with being combined into) as 0.2~4 mole, more preferably
0.5~1.5 mole, further preferably 0.8~1.2 mole.By the way that the ratio of hydrosilyl and alkenyl is controlled in
State range, there are the heat resistance of solidfied material, the transparency, thermal shock resistance and it is resistance to reflow and for corrosive gas (such as
SOx gases etc.) the tendency that further increases of barrier property.
Above-mentioned addition reaction curable silicone resin composition is as described above, can also include metallic curing catalyst.
As metallic curing catalyst, can example go out：The well-known hydrogenations such as platinum-type catalyst, rhodium class catalyst, palladium class catalyst
Silanization reaction catalyst, it is specific enumerable：Platinum micro mist, platinum black, load have the work that the fine silica powder of platinum, load have platinum
The complex compound of property charcoal, chloroplatinic acid, chloroplatinic acid and alcohol, aldehyde, ketone etc., alkene complex, the platinum-carbonyl ethenyl methyl complex of platinum
Carbonyl complex, platinum-divinyl tetramethyl disiloxane complex compound, the platinum-cyclovinylmethylsiloxane complex compound of equal platinum
Platinum-type catalysts and the replacements such as equal platinum vinyl methyl siloxane complex compound, platinum-phosphine complex compound, platinum-phosphite ester complex compound
Pt atom in above-mentioned platinum-type catalyst and the palladium class catalyst containing palladium atom or rhodium atom or rhodium class catalyst.Wherein, make
For hydrosilylation catalysts, platinum vinyl methyl siloxane complex compound, platinum-carbonyl ethenyl methyl complex, chloroplatinic acid with
Alcohol, aldehyde complex compound due to reaction speed it is good, therefore it is preferred that.
It should be noted that in above-mentioned addition reaction curable silicone resin composition, metallic curing catalyst (hydrogen
SiClx Alkanizing catalyst) it can be used alone, it can also be used in combination.
Metallic curing catalyst (hydrosilylation catalyst in above-mentioned addition reaction curable silicone resin composition
Agent) content (use level) be not particularly limited, relative to the alkene for including in addition reaction curable silicone resin composition
1 mole of the total amount of base, preferably 1 × 10-8~1 × 10-2Mole, more preferably 1.0 × 10-6~1.0 × 10-3Mole.Passing through will
Content is set as 1 × 10-8Mole or more, there is the tendency that solidfied material can be made more effectively to be formed.On the other hand, by by content
It is set as 1 × 10-2Mole hereinafter, tendency in the presence of the solidfied material that can obtain form and aspect better (coloring few).
Above-mentioned addition reaction curable silicone resin composition can include ingredient than that described above.
2-2. condensation reaction curable silicone resin compositions
As above-mentioned condensation reaction curable silicone resin composition, it can be mentioned, for example：Containing as organic siliconresin
(B) the polysiloxanes (B2) with 2 or more silanol groups (Si-OH) or siloxy (Si-OR) in the molecule, goes forward side by side one
Step includes the curable silicone resin composition of metallic curing catalyst etc. as needed.It should be noted that poly- silica
Alkane (B2) can only have any one of silanol group and siloxy, it is possible to have silanol group and siloxy this two
Person.With silanol group and in the case of siloxy the two, their total sum number is intramolecular 2 or more.
As polysiloxanes (B2), it can be mentioned, for example：The polysiloxane indicated with following average composition formulas.
R11 eSi(OR12)f(OH)gO(4-e-f-g)/2
[in above-mentioned average composition formula, R11It is identical or different, indicate the monovalent organic group of carbon atom number 1~20.R12
It is identical or different, indicate the monovalent organic group of carbon atom number 1~4.E indicates that 0.8~1.5 number, f indicate 0~0.3 number, g
Indicate 0~0.5 number.F+g be 0.001 less than 1.2 number.In addition, e+f+g be 0.801 less than 2 number.]
With regard to as the R in above-mentioned average composition formula11Monovalent organic group for, it can be mentioned, for example：Univalent aliphatic series hydrocarbon
Base (for example, alkyl, alkenyl etc.)；Monovalence aromatic hydrocarbyl (for example, aryl etc.)；Monovalence heterocycle；Aliphatic alkyl, ester ring type
2 or more the univalent perssads etc. for being bonded and being formed in alkyl and aromatic hydrocarbyl.It should be noted that these any monovalent organic radicals
Group can also have substituent group (for example, the substituent groups such as hydroxyl, carboxyl, halogen atom).Wherein, as R11, preferably carbon atom number 1
The aryl of~20 alkyl, the alkenyl of carbon atom number 1~20, carbon atom number 6~20.In addition, being just used as above-mentioned average composition formula
In R12Monovalent organic group for, it can be mentioned, for example：Optionally with substituent group univalent aliphatic series alkyl (for example, alkyl,
Alkenyl etc.) etc..Wherein, as R12, preferably the alkyl of carbon atom number 1~4, carbon atom number 2~4 alkenyl.
In above-mentioned condensation reaction curable silicone resin composition, polysiloxanes (B2) can be used alone,
It can also be used in combination.
Above-mentioned condensation reaction curable silicone resin composition is as described above, can also include metallic curing catalyst.
As such metallic curing catalyst, known or usual condensation catalyst can be enumerated, it can be mentioned, for example：Organic metatitanic acid
Ester, organic titanium chelate compound, organo-aluminum compound, organic zirconate, organo-tin compound, organic carboxyl acid metal salt,
Amine compounds or its salt, quaternary ammonium salt, the lower aliphatic hydrochlorate of alkali metal, dialkylhydroxyamines, the organo-silicon compound etc. containing guanidine radicals.
Wherein, from the viewpoint of reactivity, preferred organic zirconate.These compounds both can be used alone, can also group
It closes and uses two or more.Metallic curing catalyst in above-mentioned condensation reaction curable silicone resin composition (urge by condensation reaction
Agent) content (use level) be not particularly limited, for example, can be in 100 parts by weight of total amount relative to polysiloxanes (B2)
Suitably to be selected in the range of 0.01~20 parts by weight.
Above-mentioned condensation reaction curable silicone resin composition can also include ingredient than that described above.
The curable silicone resin composition of the present invention is (for example, above-mentioned addition reaction curable silicone resin combination
Object, condensation reaction curable silicone resin composition etc.) in can also include other ingredients.As other ingredients, can enumerate
Such as：Those of exemplified by the ingredient that can include in curable epoxy resin composition as the present invention etc..Its content
It is not particularly limited, can suitably select.For example, the curable silicone resin composition in the present invention is optical semiconductor sealing
In the case of with resin combination, above-mentioned fluorophor is preferably comprised.It is glimmering in the curable silicone resin composition of the present invention
The content (use level) of body of light is not particularly limited, can be in total amount (100 weights relative to curable silicone resin composition
Amount %) be 0.5~20 weight % in the range of suitably select.
The curable silicone resin composition of the present invention is not particularly limited, such as can be by by above-mentioned each ingredient root
It is stirred, mixes to prepare in the state of heated according to needs.It should be noted that the curable silicone tree of the present invention
Oil/fat composition can be the composition of the direct one-pack type using mixture made of being all pre-mixed each ingredient, also may be used
Be for example by the multigroup parting for being divided into 2 parts or more of ingredient and being used immediately before use with being mixed to certainty ratio (for example,
Two-component-type) composition.Stirring, the method mixed are not particularly limited, and can use various such as disperser, homogenizer
Known in mixer, kneader, roller, ball mill, rotation-revolution formula agitating device etc. or usual stirring, mixed organization.In addition,
Deaeration can be carried out under reduced pressure or under vacuum after stirring, mixing.In addition, the curable silicone resin group as the present invention
Object or its constituent are closed, commercially available product can also be directly used.
3. curability acrylic acid resin composition
Above-mentioned curability acrylic acid resin composition (also referred to as " curability acrylic acid resin composition of the invention ") is
Include solidification compound of the acrylic resin (C) as curability compound as neccessary composition.The curability of the present invention
Acrylic acid resin composition can also include the ingredient in addition to acrylic resin (C).
As acrylic resin (C), it can be mentioned, for example：There is intramolecular 1 or more (methyl) acryloyl group (to be selected from propylene
At least one of acyl group and methylacryloyl group) compound.As acrylic resin (C), intramolecular can be enumerated only
(methyl) acryl compound with 1 (methyl) acryloyl group；Intramolecular has 2 or more (methyl) acryloyl groups
Multifunctional (methyl) acryl compound etc..It should be noted that above-mentioned intramolecular is only with 1 (methyl) acryloyl group
(methyl) acryl compound includes：Simple function (first without the polymerizable functional group in addition to (methyl) acryloyl group
Base) acryl compound and 1 or more epoxy group, oxygen is further had other than there is (methyl) acryloyl group
Multifunctional (methyl) acryl compound of other polymerizable functional groups such as heterocycle butyl, vinyl, ethyleneoxy.Acrylic acid
Resin (C) can be used alone, and can also be used in combination.It should be noted that the curability third of the present invention
The content of acrylic resin (C) in olefin(e) acid resin combination is not particularly limited, and can suitably select.
The curability acrylic acid resin composition of the present invention can include for example for keeping the polymerization of acrylic resin (C) anti-
The initiator that should be carried out.As initiator, polymerization initiator known in thermal polymerization etc. or usual can be enumerated.These chemical combination
Object both can be used singly or in combination of two or more.It, can be in addition, the content of initiator is not particularly limited
Appropriate selection.
The curability acrylic acid resin composition of the present invention can also include other ingredients.As other ingredients, can enumerate
Such as：Those of example etc. as the ingredient that can include in curable epoxy resin composition of the invention.Its content
It is not particularly limited, can suitably select.For example, the curability acrylic acid resin composition in the present invention is optical semiconductor sealing
In the case of with resin combination, above-mentioned fluorophor is preferably comprised.It is glimmering in the curability acrylic acid resin composition of the present invention
The content (use level) of body of light is not particularly limited, can be in total amount (100 weights relative to curability acrylic acid resin composition
Amount %) be 0.5~20 weight % in the range of suitably select.
The curability acrylic acid resin composition of the present invention is not particularly limited, such as can be by by above-mentioned each ingredient root
It is stirred, mixes to prepare in the state of heated according to needs.It should be noted that the curability acrylic acid tree of the present invention
Oil/fat composition can be the composition of the direct one-pack type using mixture made of being all pre-mixed each ingredient, also may be used
Be for example by the multigroup parting for being divided into 2 parts or more of ingredient and being used immediately before use with being mixed to certainty ratio (for example,
Two-component-type) composition.Stirring, the method mixed are not particularly limited, and can use various such as disperser, homogenizer
Known in mixer, kneader, roller, ball mill, rotation-revolution formula agitating device etc. or usual stirring, mixed organization.In addition,
Deaeration can be carried out under reduced pressure or under vacuum after stirring, mixing.In addition, the curable silicone resin group as the present invention
Object or its constituent are closed, commercially available product can also be directly used.
[concaveconvex shape]
For the anti-reflection material of the present invention, above-mentioned porous filler spreads all over to above-mentioned resin layer entirety, dispersity
Stablize, as a result, the porous filler for being present in the surface of resin layer forms concaveconvex shape and makes scatter incident light, thus plays
Go out anti-reflective function.In addition, the cellular structure on porous filler surface can also make scatter incident light, counnter attack is further increased
Penetrate function.
Make above-mentioned porous filler spread all over to the method for above-mentioned resin layer entirety to be not particularly limited, it can be mentioned, for example：Make
Porous filler is homogeneously dispersed in the method etc. for the resin combination for constituting resin layer.In order to effectively manufacture the anti-of the present invention
Reflecting material, the method for preferably making porous filler evenly dispersed.
Hereinafter, illustrated for a kind of embodiment of the manufacturing method of the anti-reflection material of the present invention, but the present invention
It is not intended to be limited thereto.
It can be kept evenly dispersed by adding porous filler to resin layer and carrying out mixed/stirred.To mixing/stirring
The method mixed is not particularly limited, can use the various mixers such as disperser, homogenizer, kneader, roller, ball mill,
Known in rotation-revolution formula agitating device etc. or usual stirring, mixed organization.Alternatively, it is also possible to depressurized after stirring, mixing
Deaeration is carried out under lower or vacuum.
The character of the anti-reflection material before curing of the present invention is not particularly limited, preferably liquid.Due to forming this hair
The resin combination before curing of bright anti-reflection material can show to prevent due to using porous filler in a small amount of addition
Reflection function, therefore liquid is easily become without using toluene equal solvent, therefore it is preferred that.
[curing process]
By making the evenly dispersed resin layer solidification by for having porous filler that solidfied material be made (hereinafter also referred to as " present invention
Solidfied material "), can obtain the present invention anti-reflection material.
The amount of the ingredient to volatilize in solidification for the total amount (100 weight %) of anti-reflection material before curing
It is not particularly limited, preferably 10 weight % or less, more preferably 8 weight % or less, further preferably 5 weight % or less.
By making the amount of the ingredient to volatilize in solidification be 10 weight % hereinafter, the dimensional stability of solidfied material is got higher, therefore it is preferred that.Due to this
The anti-reflection material before curing of invention can show anti-reflective function due to using porous filler in a small amount of addition, because
This easily becomes liquid without using solvent (toluene etc.) volatile ingredient, it is possible to reduce the ingredient to volatilize in solidification
Amount.
As cured method, can utilize known in heat treatment, photo-irradiation treatment etc. or usual method.For by adding
Heat makes the temperature (solidification temperature) when its solidification be not particularly limited, preferably 45~200 DEG C, more preferably 50~190 DEG C, into
One step is preferably 55~180 DEG C.In addition, the time (hardening time) heated when solidification is not particularly limited, preferably
It is 30~600 minutes, more preferably 45~540 minutes, further preferably 60~480 minutes.In solidification temperature and solidification
Between it is lower than the lower limiting value of above range in the case of, solidification becomes inadequate, on the contrary, in the feelings of the upper limit value higher than above range
Under condition, it may occur that the decomposition of resin component, not preferably.Condition of cure depend on various conditions, for example, can by
Shorten hardening time in the case of improving solidification temperature, extend hardening time etc. in the case where reducing solidification temperature and fitted
Work as adjustment.In addition, solidification can be carried out with a stage, can also be carried out with two multiple stages more than stage.
In addition, when making its solidification by illumination, such as can be by with 10~1200mW/cm of illumination2, irradiate light quantity 20~
2500mJ/cm2Irradiation includes the light (radioactive ray) of i- lines (365nm), h- lines (405nm), g- lines (436nm) etc. and obtains this hair
Bright anti-reflection material.From the viewpoint of inhibiting the viewpoint and productivity of deterioration of the resin layer based on radioactive ray, preferably put
The irradiate light quantity of ray is 20~600mJ/cm2, more preferably it is expected irradiate light quantity be 20~300mJ/cm2.It, can in irradiation
To use high-pressure mercury-vapor lamp, xenon lamp, carbon arc lamp, metal halide lamp, laser etc. as irradiation source.
[anti-reflection material]
The anti-reflection material of the present invention is as described above, have both high transparency and excellent anti-reflective function, therefore can fit
Share the resin for being used as optical material (purposes for being used to form optical material).Optical material refers to showing light diffusing, light
The material of the various optics sexual functions such as permeability, light reflective.By using the anti-reflection material of the present invention, at least wrapped
The optical component of solidfied material (optical material) containing the present invention.It should be noted that the optical component can be only by the present invention's
Anti-reflection material is constituted, can also only a part use anti-reflection material of the invention.As optical component, can enumerate：Display
Go out the component of the various optics sexual functions such as light diffusing, photopermeability, light reflective, above-mentioned optics sexual function is utilized in composition
The component etc. of device or equipment, is not particularly limited, can exemplify for example optical semiconductor device, organic el device, bonding agent,
Electrical insulating material, laminated plate, coating, black liquid, coating, sealer, resist, composite material, transparent base, slide, thoroughly
It is bright film, optical element, optical lens, light chisel, Electronic Paper, touch panel, solar cell substrate, optical waveguide, light guide plate, complete
The known or usual optical component used in the various uses such as breath memory, optical pickup sensor.
For the anti-reflection material of the present invention, porous filler spreads all over whole to resin layer and disperses, as a result, at it
Surface has the fine and uniform concaveconvex shape that is formed by porous filler, by the concaveconvex shape make scatter incident light without
It is totally reflected, therefore gloss can be inhibited and visibility is made to improve.It is formed in the concaveconvex shape of the anti-reflection material of the present invention
Arithmetic mean surface roughness Ra be preferably 0.1~1.0 μm of range, more preferable 0.2~0.8 μm of range.If concave-convex
The arithmetic mean surface roughness Ra of shape is the range, then total light flux will not significantly be damaged, can play adequately by existing
The tendency of anti-reflective function.
It should be noted that in the present invention, arithmetic mean surface roughness Ra is defined according to JIS B0601-2001
Numerical value, expression is the roughness for being measured, being calculated using the method described in aftermentioned embodiment.
The anti-reflection material of the present invention can be used preferably as such as optical semiconductor sealing with resin combination.That is, this
The anti-reflection material of invention can be preferably as the composition (light for being sealed in the optical semiconductor in optical semiconductor device
The sealing material of optical semiconductor in semiconductor device) it uses.Use the anti-reflection material (optical semiconductor sealing of the present invention
With resin combination), it can obtain using the anti-reflection material and optical semiconductor device (example made of encapsulating optical semiconductor element
Such as, 104 in Fig. 1 are the optical semiconductor device being made of the anti-reflection material of the present invention).The sealing of optical semiconductor is for example
It can carry out as follows：The evenly dispersed resin combination for having porous filler is injected in given molding die, what is given
Under the conditions of be heating and curing or photocuring.Condition of solidification temperature, hardening time or photocuring etc. can with prepare it is above-mentioned
It is suitably set in identical range when anti-reflection material.The optical semiconductor device of aforementioned present invention can not especially make total light logical
Amount reduces and plays excellent anti-reflective function.It should be noted that in the present specification, " photosemiconductor dress of the invention
Set " refer to that at least part of member of formation (for example, sealing material, mold grafting material etc.) of optical semiconductor device uses
The optical semiconductor device of the anti-reflection material of the present invention.
Embodiment
Hereinafter, the present invention is described in more detail in conjunction with the embodiments, but the present invention is not limited to these implementations
Example.It should be noted that the unit of the ingredient for constituting resin combination shown in table 1~4 is parts by weight.
Production Example 1
Using rotation-revolution formula agitating device (trade name " practice Taro agitator (あ わ と り Practice Taros) AR-250 ",
(strain) Thinky systems, similarly hereinafter) by curing agent (trade name " RIKACID MH-700 ", new Japan Chemical (strain) manufacture) 100 weight
Part, curing accelerator (trade name " U-CAT 18X ", San Apro (strain) manufacture) 0.5 parts by weight and ethylene glycol (and the pure medicine of light
Industrial (strain) manufacture) 1 parts by weight are mixed, manufacture epoxy hardener (K agent).
Embodiment 1
By cycloaliphatic epoxy (trade name " Celloxide 2021P ", (strain) Daicel systems) 100 parts by weight, system
Make 101.5 parts by weight of epoxy hardener obtained in example 1 mixed using rotation-revolution formula agitating device, deaeration, manufacture
Curable epoxy resin composition.
Using rotation-revolution formula agitating device by 100 parts by weight of curable epoxy resin composition obtained above and porous
Property filler (trade name " Sylysia 430 ", Fuji's chemistry of silicones (strain) manufacture) 20 parts by weight mixed, deaeration, will obtained by
Curable epoxy resin composition cast to the lead frame (InGaN elements, 3.5mm × 2.8mm) of photosemiconductor shown in FIG. 1
Afterwards, it is heated 5 hours using 150 DEG C of resin solidification baking oven, has thus manufactured the anti-reflection material sealing light half using the present invention
Optical semiconductor device made of conductor element.It should be noted that in Fig. 1,100 indicate that reflector, 101 indicate hardware cloth
Line, 102 indicate that optical semiconductor, 103 indicate that closing line, 104 indicate sealing material (anti-reflection material), spread all over to 104
Whole, porous filler is uniformly dispersed, to be formd using porous filler existing for upper face wherein
One and fine concaveconvex shape (diagram omits concaveconvex shape).
Embodiment 2~20, comparative example 1~6
The composition of curable epoxy resin composition, porous filler is changed to shown in table 1~3 like that, in addition to this
It carries out similarly to Example 1, has manufactured optical semiconductor device.
Embodiment 21
Using rotation-revolution formula agitating device by curable silicone resin composition (trade name " OE-6630A/B " (Gu
The property changed organic siliconresin, Dow Corning Toray Toray (strain) manufactures) 100 parts by weight and porous filler (trade name
" Sylysia 430 ", Fuji's chemistry of silicones (strain) manufacture) 20 parts by weight are mixed, deaeration, by obtained curable silicone
Resin combination is cast to the lead frame (InGaN elements, 3.5mm × 2.8mm) of photosemiconductor shown in FIG. 1, utilizes 150 DEG C
Resin solidification baking oven heat 1 hour, thus manufactured using the present invention anti-reflection material encapsulating optical semiconductor element form
Optical semiconductor device.
Embodiment 22~27
The composition of curable silicone resin composition is changed to shown in table 4 like that, it is same with embodiment 21 in addition to this
It carries out to sample, has manufactured optical semiconductor device.
Embodiment 28
Using rotation-revolution formula agitating device by curability acrylic acid resin composition (trade name " TB3030 ", curability
Acrylic resin, (strain) ThreeBond systems) 100 parts by weight and porous filler (trade name " Sylysia 430 ", Fuji's silication
Learn (strain) manufacture) 20 parts by weight are mixed, deaeration, obtained curability acrylic acid resin composition is cast to Fig. 1 institutes
After the lead frame (InGaN elements, 3.5mm × 2.8mm) of the photosemiconductor shown, in being stored at room temperature 24 hours, height is further utilized
Medium pressure mercury lamp (UVC-02516S1AA02：Oxtail Motor Corporation system, illumination 120mW/cm2, irradiate light quantity 199mJ/cm2) carry out light
Irradiation, manufactured using the present invention anti-reflection material and optical semiconductor device made of encapsulating optical semiconductor element (light is partly led
The optical semiconductor device that volume elements part is sealed to form by anti-reflection material).
[evaluation]
Following evaluations have been carried out to above-mentioned manufactured optical semiconductor device.Result is shown in table 1~4.
(1) fluorescent lamp is mirrored
Will the fluorescent lamp that lighted be aligned embodiment, the optical semiconductor device obtained in comparative example upper table surface (Fig. 1's
The upper surface of sealing material 104) and observe reflection when, carried out in the clarity of the fluorescent lamp of anti-reflection material with estimating mapping
The evaluation of 3 grades.
Will be unable to identification fluorescent lamp profile the case where be set as zero, by profile it is unintelligible and but identifiable situation be set as
△, will be set as the case where being clearly identified profile ×.
(2) arithmetic mean surface roughness Ra
Using laser microscope, (" measuring shape laser microscope (Xing Zhuan Measuring Ding レ ー ザ マ イ Network ロ ス コ ー to trade name
プ) VK-8710 ", Keyence corporation) to the upper surface of the optical semiconductor device obtained in embodiment, comparative example, (Fig. 1's is close
The upper surface of closure material 104) it is determined.
(3) total light flux
For each optical semiconductor device obtained in embodiment, comparative example, using total light flux measuring instrument, (trade name is " more
Spectroradiometric measurement system (マ Le チ light splitting Fang She Measuring determine シ ス テ system) OL771 ", Optronic Laboratories companies
System) determine under conditions of 5V, 20mA be powered when total light flux.
(4) comprehensive judgement
For each optical semiconductor device obtained in embodiment, comparative example, whole feelings of following (a)~(c) will be met
Condition is determined as zero (good), is unsatisfactory in following (a)~(c) being determined as × (bad) the case where any one.
(a) mirroring for zero or △ in above-mentioned (1) the middle fluorescent lamp measured.
(b) the arithmetic mean surface roughness Ra measured in above-mentioned (2) is 0.10~1.0 μm.
(c) total light flux measured in above-mentioned (3) is 0.60lm or more.
It is illustrated below for each ingredient for constituting anti-reflection material shown in table 1~4.
(porous filler)
Sylysia 430：Trade name " Sylysia 430 ", Fuji's chemistry of silicones (strain) system, volume average particle size：4.1μm；
Specific surface area：350m2/g；Average micro-pore diameter：17nm；Micropore volume：1.25mL/g；Oil absorption：230mL/100g
Sylosphere C-1504：Trade name " Sylosphere C-1504 ", Fuji's chemistry of silicones (strain) system, volume are average
Grain size：4.5μm；Specific surface area：520m2/g；Average micro-pore diameter：12nm；Micropore volume：1.5mL/g；Oil absorption：290mL/
100g
Sunsphere H-52：Trade name " Sunsphere H-52 ", AGC SI-TECH (strain) systems, volume average particle size：
5μm；Specific surface area：700m2/g；Average micro-pore diameter：10nm；Micropore volume：2mL/g；Oil absorption：300mL/100g
(inorganic filler)
Melting is crushed shape silica：The gloomy system of (strain) dragon, volume average particle size：6~7 μm
Melt spherical silicon dioxide：The gloomy system of (strain) dragon, volume average particle size：5μm
Crystallinity is crushed shape silica：The gloomy system of (strain) dragon, volume average particle size：5μm
(epoxy resin)
Celloxide 2021P：Trade name " Celloxide 2021P " [3,4- epoxycyclohexyl-methyls (3,4- epoxies)
Cyclohexane-carboxylic acid salt], (strain) Daicel systems
YD-128：Aurification (strain) system is lived by trade name " YD-128 " [bisphenol A type epoxy resin], Nippon Steel
TEPIC-VL：Trade name " TEPIC-VL " [triglycidyl group isocyanuric acid ester], Nissan Chemical Industries (strain) system
152：Trade name " 152 " [phenol novolak type epoxy resin], Mitsubishi Chemical's (strain) system
YL7410：Trade name " YL7410 " [aliphatic epoxy compound], Mitsubishi Chemical's (strain) system
X-22-169AS：[(two ends have the poly dimethyl of epoxycyclohexyl to modified silicon oil to trade name " X-22-169AS "
Siloxanes)], SHIN-ETSU HANTOTAI's chemical industry (strain) system
X-40-2670：Trade name " X-40-2670 " [annular siloxane with epoxycyclohexyl], SHIN-ETSU HANTOTAI's chemical industry
(strain) makes
(epoxy hardener)
MH-700：Trade name " RIKACID MH-700 " [4- methylhexahydrophthalic anhydrides/hexahydrophthalic anhydride
=70/30], new Japan Chemical (strain) system
U-CAT 18X：Trade name " U-CAT 18X " [curing accelerator], San Apro (strain) systems
Ethylene glycol：It is made with Wako Pure Chemical Industries (strain)
SI-100L：Trade name " San-Aid SI-100L ", San Apro (strain) systems
(organic siliconresin)
OE-6630A/B：Trade name " OE-6630A/B " [addition reaction curable silicone resin], Dow Corning
Toray (strain) makes
KER-2500A/B：Trade name " KER-2500A/B " [addition reaction curable silicone resin (methyl rubber)],
SHIN-ETSU HANTOTAI's chemical industry (strain) is made
SCR-1012A/B：Trade name " SCR-1012A/B " [addition reaction curable silicone resin (modified silicon oil)],
SHIN-ETSU HANTOTAI's chemical industry (strain) is made
ETERLED GD1012A/B：Trade name " ETERLED GD1012A/B " [addition reaction curable silicone resin
(including poly-organosilicon oxygroup silicon alkylidene)], Changxing chemical industry system
ETERLED GD1130A/B：Trade name " ETERLED GD1130A/B " [addition reaction curable silicone resin
(including poly-organosilicon oxygroup silicon alkylidene)], Changxing chemical industry system
X-21-5841：Trade name " X-21-5841 " [condensation reaction curable silicone resin (organosilicon two-component-type
RTV rubber)], SHIN-ETSU HANTOTAI's chemical industry (strain) system
KF-9701：Trade name " KF-9701 " [condensation reaction curable silicone resin (modified silicon oil)], SHIN-ETSU HANTOTAI's chemistry
Industrial (strain) system
(acrylic resin)
TB3030：Trade name " TB3030 " [curability acrylic resin], (strain) ThreeBond systems)
As shown in table 1,3,4, it is added to involved by the embodiment of porous filler with the specified rate of the present invention using having
Anti-reflection material optical semiconductor device when, fluorescent lamp mirror be zero or △ evaluation, can confirm have it is excellent anti-
Reflection function.
In addition, the arithmetic of the optical semiconductor device of the embodiment of the present invention for mirroring the evaluation for zero or △ of fluorescent lamp is flat
Equal surface roughness Ra is in 0.10~1.0 μm of range, can confirm and form appropriate concaveconvex shape.
Further, the total light flux of the optical semiconductor device of the embodiment of the present invention is 0.60lm or more, it is shown that good
Good illumination.
On the other hand, as shown in table 2, the ratio of porous filler has been coordinated with the use level of the given range less than the present invention
Compared with example 2 and the optical semiconductor device of the comparative example 4~6 for the silica filler for being added to imporosity, fluorescent lamp mirror by
It is evaluated as × (bad), the value of arithmetic mean surface roughness Ra is also low (being less than 0.1 μm), only shows and does not add filler
The anti-reflective function of 1 degree of comparative example.It is believed that in comparative example 2, the use level of porous filler is insufficient, in addition, than
Compared in example 4~6, silica filler settles, as a result, not forming uniform and fine concaveconvex shape on surface.It is another
Aspect, in having coordinated the comparative example 3 of porous filler with the use level of the given range more than the present invention, it is shown that good
Anti-reflective function, on the other hand, total light flux are 0.46lm or more, and illumination significantly reduces.It is believed that due to porous filler
Use level is more and light is caused to be absorbed.
Industrial applicibility
The anti-reflection material of the present invention can be suitable for use as light due to having both high transparency and excellent anti-reflective function
Learn resin of the material with (purposes for being used to form optical material).As optical component, can enumerate：Show light diffusing, light
The component of the various optics sexual functions such as permeability, light reflective constitutes the device or equipment that above-mentioned optics sexual function is utilized
Component etc., is not particularly limited, and can exemplify for example in optical semiconductor device, organic el device, bonding agent, electric insulation material
Material, laminated plate, coating, black liquid, coating, sealer, resist, composite material, transparent base, slide, hyaline membrane, optics member
Part, optical lens, light chisel, Electronic Paper, touch panel, solar cell substrate, optical waveguide, light guide plate, holographic memory, light
Learn the known or usual optical component used in the various uses such as sound pickup sensor.
Claims (8)
1. a kind of anti-reflection material, it includes the resin layers for being dispersed with porous filler, wherein
The porous filler forms the bumps for inhibiting reflection on the surface of the resin layer,
Relative to anti-reflection material total amount (100 weight %), the content of porous filler is 4~40 weight %.
2. anti-reflection material according to claim 1, wherein porous filler is inorganic porous property filler.
3. anti-reflection material according to claim 1 or 2, wherein anti-reflection material before curing is liquid.
4. anti-reflection material described in any one of claim 1 to 3, wherein relative to anti-reflection material before curing
Total amount (100 weight %), the amount of the ingredient to volatilize in solidification is 10 weight % or less.
5. anti-reflection material according to any one of claims 1 to 4, wherein the resin layer is by transparent curability
Resin combination is formed.
6. anti-reflection material according to any one of claims 1 to 5, wherein the hardening resin composition is by wrapping
Composition containing curability compound is formed, and the curability compound is selected from epoxy resin, organic siliconresin and acrylic acid
At least one of resin.
7. it is optical semiconductor sealing resin combination according to anti-reflection material according to any one of claims 1 to 6.
8. a kind of optical semiconductor device is formed using the anti-reflection material encapsulating optical semiconductor element described in claim 7
's.
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2016006638 | 2016-01-15 | ||
| JP2016-006638 | 2016-01-15 | ||
| JP2016173980 | 2016-09-06 | ||
| JP2016-173980 | 2016-09-06 | ||
| PCT/JP2017/000666 WO2017122691A1 (en) | 2016-01-15 | 2017-01-11 | Anti-reflection material |
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| Publication Number | Publication Date |
|---|---|
| CN108369985A true CN108369985A (en) | 2018-08-03 |
| CN108369985B CN108369985B (en) | 2022-04-29 |
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| CN201780004775.8A Active CN108369985B (en) | 2016-01-15 | 2017-01-11 | Antireflection material |
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| Country | Link |
|---|---|
| JP (1) | JP7127989B2 (en) |
| KR (1) | KR20180103862A (en) |
| CN (1) | CN108369985B (en) |
| TW (1) | TWI739790B (en) |
| WO (1) | WO2017122691A1 (en) |
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| CN114262530A (en) * | 2022-01-06 | 2022-04-01 | 山西日盛达太阳能科技股份有限公司 | Antireflection coating solution, preparation method, photovoltaic glass and preparation method thereof |
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| KR20190059969A (en) * | 2016-10-11 | 2019-05-31 | 주식회사 다이셀 | Antireflective material |
| CN111936568B (en) * | 2018-01-23 | 2023-09-15 | 沃利化学有限公司 | Adhesive composition and application thereof |
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- 2017-01-11 JP JP2017561141A patent/JP7127989B2/en active Active
- 2017-01-11 WO PCT/JP2017/000666 patent/WO2017122691A1/en active Application Filing
- 2017-01-11 CN CN201780004775.8A patent/CN108369985B/en active Active
- 2017-01-11 KR KR1020187018574A patent/KR20180103862A/en not_active Application Discontinuation
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20050287816A1 (en) * | 2004-06-28 | 2005-12-29 | Blalock Guy T | Methods of forming patterned photoresist layers over semiconductor substrates |
| CN1869736A (en) * | 2005-05-26 | 2006-11-29 | 财团法人工业技术研究院 | Three-D nano-porous film and its manufacturing method |
| CN102544331A (en) * | 2010-12-28 | 2012-07-04 | 日亚化学工业株式会社 | Light emitting device |
| CN102796413A (en) * | 2011-05-20 | 2012-11-28 | 东友精细化工有限公司 | Composition for anti-dazzling and anti-reflection coating, anti-dazzling and anti-reflection film, polarizer, and display device using the composition |
| US20150221837A1 (en) * | 2011-12-26 | 2015-08-06 | Konica Minolta, Inc. | Sealant for led device, led device, and method for producing led device |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114262530A (en) * | 2022-01-06 | 2022-04-01 | 山西日盛达太阳能科技股份有限公司 | Antireflection coating solution, preparation method, photovoltaic glass and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JPWO2017122691A1 (en) | 2018-11-01 |
| WO2017122691A1 (en) | 2017-07-20 |
| JP7127989B2 (en) | 2022-08-30 |
| KR20180103862A (en) | 2018-09-19 |
| TW201731986A (en) | 2017-09-16 |
| CN108369985B (en) | 2022-04-29 |
| TWI739790B (en) | 2021-09-21 |
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