TWI696664B - 硬化性聚矽氧組合物、及光半導體裝置 - Google Patents
硬化性聚矽氧組合物、及光半導體裝置 Download PDFInfo
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- TWI696664B TWI696664B TW104117672A TW104117672A TWI696664B TW I696664 B TWI696664 B TW I696664B TW 104117672 A TW104117672 A TW 104117672A TW 104117672 A TW104117672 A TW 104117672A TW I696664 B TWI696664 B TW I696664B
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- polysiloxane
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- 239000000203 mixture Substances 0.000 title claims abstract description 79
- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 65
- 230000003287 optical effect Effects 0.000 title claims abstract description 25
- 239000004065 semiconductor Substances 0.000 title claims abstract description 25
- -1 polysiloxane Polymers 0.000 claims abstract description 146
- 125000003342 alkenyl group Chemical group 0.000 claims abstract description 34
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- 238000006459 hydrosilylation reaction Methods 0.000 claims abstract description 7
- 239000002318 adhesion promoter Substances 0.000 claims abstract description 5
- 125000003118 aryl group Chemical group 0.000 claims description 27
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 25
- 125000000217 alkyl group Chemical group 0.000 claims description 25
- 125000003710 aryl alkyl group Chemical group 0.000 claims description 23
- 125000004432 carbon atom Chemical group C* 0.000 claims description 21
- 229910052710 silicon Inorganic materials 0.000 claims description 19
- 229920005989 resin Polymers 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- 239000004593 Epoxy Substances 0.000 claims description 5
- 125000000962 organic group Chemical group 0.000 claims description 5
- 125000005417 glycidoxyalkyl group Chemical group 0.000 claims description 3
- 239000002683 reaction inhibitor Substances 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 239000003112 inhibitor Substances 0.000 claims 1
- 150000002894 organic compounds Chemical class 0.000 claims 1
- 238000007789 sealing Methods 0.000 claims 1
- 239000000758 substrate Substances 0.000 abstract description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 24
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 16
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- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 15
- 125000003545 alkoxy group Chemical group 0.000 description 14
- 238000010992 reflux Methods 0.000 description 14
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 12
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 11
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 11
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 10
- 125000004122 cyclic group Chemical group 0.000 description 10
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 10
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- 238000001816 cooling Methods 0.000 description 9
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- 125000005843 halogen group Chemical group 0.000 description 6
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 6
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- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 description 6
- 239000011787 zinc oxide Substances 0.000 description 6
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 5
- 229910052693 Europium Inorganic materials 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 125000002178 anthracenyl group Chemical group C1(=CC=CC2=CC3=CC=CC=C3C=C12)* 0.000 description 5
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 5
- 239000012964 benzotriazole Substances 0.000 description 5
- 125000004369 butenyl group Chemical group C(=CCC)* 0.000 description 5
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- 125000003493 decenyl group Chemical group [H]C([*])=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])[H] 0.000 description 5
- WHGNXNCOTZPEEK-UHFFFAOYSA-N dimethoxy-methyl-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](C)(OC)CCCOCC1CO1 WHGNXNCOTZPEEK-UHFFFAOYSA-N 0.000 description 5
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 5
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- 229910052697 platinum Inorganic materials 0.000 description 5
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- QWENRTYMTSOGBR-UHFFFAOYSA-N 1H-1,2,3-Triazole Chemical compound C=1C=NNN=1 QWENRTYMTSOGBR-UHFFFAOYSA-N 0.000 description 4
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
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- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Chemical group CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 4
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- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 230000018044 dehydration Effects 0.000 description 4
- 238000006297 dehydration reaction Methods 0.000 description 4
- 125000003438 dodecyl group Chemical group [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])C([H])([H])C([H])([H])* 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 description 4
- 125000005065 undecenyl group Chemical group C(=CCCCCCCCCC)* 0.000 description 4
- 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 4
- 125000004400 (C1-C12) alkyl group Chemical group 0.000 description 3
- NSPMIYGKQJPBQR-UHFFFAOYSA-N 4H-1,2,4-triazole Chemical compound C=1N=CNN=1 NSPMIYGKQJPBQR-UHFFFAOYSA-N 0.000 description 3
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- 238000006482 condensation reaction Methods 0.000 description 3
- 125000002704 decyl group Chemical group [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])* 0.000 description 3
- 125000005066 dodecenyl group Chemical group C(=CCCCCCCCCCC)* 0.000 description 3
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- 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 3
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- 125000001400 nonyl 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])[H] 0.000 description 3
- 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 3
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- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 2
- LRUDIIUSNGCQKF-UHFFFAOYSA-N 5-methyl-1H-benzotriazole Chemical compound C1=C(C)C=CC2=NNN=C21 LRUDIIUSNGCQKF-UHFFFAOYSA-N 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical group [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 2
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- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 2
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- URZLRFGTFVPFDW-UHFFFAOYSA-N ethenyl-diethoxy-phenylsilane Chemical compound CCO[Si](OCC)(C=C)C1=CC=CC=C1 URZLRFGTFVPFDW-UHFFFAOYSA-N 0.000 description 2
- 239000002223 garnet Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 2
- 150000002430 hydrocarbons Chemical group 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000003384 imaging method Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
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- 125000006850 spacer group Chemical group 0.000 description 2
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- SEUGQQYRPAEMFC-UHFFFAOYSA-N triethoxy(pyren-1-yl)silane Chemical compound C1=C2C([Si](OCC)(OCC)OCC)=CC=C(C=C3)C2=C2C3=CC=CC2=C1 SEUGQQYRPAEMFC-UHFFFAOYSA-N 0.000 description 2
- YFSYFAJGRGDWQT-KTKRTIGZSA-N (z)-1-(benzotriazol-1-yl)octadec-9-en-1-one Chemical compound C1=CC=C2N(C(=O)CCCCCCC\C=C/CCCCCCCC)N=NC2=C1 YFSYFAJGRGDWQT-KTKRTIGZSA-N 0.000 description 1
- 125000003626 1,2,4-triazol-1-yl group Chemical group [*]N1N=C([H])N=C1[H] 0.000 description 1
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- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
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- LQPDFQFGNCXQSL-UHFFFAOYSA-N 1-[(dioctylamino)methyl]benzotriazole-4-carboxylic acid Chemical compound C1=CC=C2N(CN(CCCCCCCC)CCCCCCCC)N=NC2=C1C(O)=O LQPDFQFGNCXQSL-UHFFFAOYSA-N 0.000 description 1
- KGEPBYXGRXRFGU-UHFFFAOYSA-N 1-[[bis(2-ethylhexyl)amino]methyl]benzotriazole-4-carboxylic acid Chemical compound C1=CC=C2N(CN(CC(CC)CCCC)CC(CC)CCCC)N=NC2=C1C(O)=O KGEPBYXGRXRFGU-UHFFFAOYSA-N 0.000 description 1
- OILIWDRDPKUVBC-UHFFFAOYSA-N 1-[[bis(2-hydroxyethyl)amino]methyl]benzotriazole-4-carboxylic acid Chemical compound C1=CC=C2N(CN(CCO)CCO)N=NC2=C1C(O)=O OILIWDRDPKUVBC-UHFFFAOYSA-N 0.000 description 1
- DYNVQVFAPOVHNT-UHFFFAOYSA-N 1-[[bis(2-hydroxypropyl)amino]methyl]benzotriazole-4-carboxylic acid Chemical compound C1=CC=C2N(CN(CC(C)O)CC(O)C)N=NC2=C1C(O)=O DYNVQVFAPOVHNT-UHFFFAOYSA-N 0.000 description 1
- XXJGBENTLXFVFI-UHFFFAOYSA-N 1-amino-methylene Chemical compound N[CH2] XXJGBENTLXFVFI-UHFFFAOYSA-N 0.000 description 1
- RWNUSVWFHDHRCJ-UHFFFAOYSA-N 1-butoxypropan-2-ol Chemical compound CCCCOCC(C)O RWNUSVWFHDHRCJ-UHFFFAOYSA-N 0.000 description 1
- RMSGQZDGSZOJMU-UHFFFAOYSA-N 1-butyl-2-phenylbenzene Chemical group CCCCC1=CC=CC=C1C1=CC=CC=C1 RMSGQZDGSZOJMU-UHFFFAOYSA-N 0.000 description 1
- JOLQKTGDSGKSKJ-UHFFFAOYSA-N 1-ethoxypropan-2-ol Chemical compound CCOCC(C)O JOLQKTGDSGKSKJ-UHFFFAOYSA-N 0.000 description 1
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 description 1
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 description 1
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- FCVNATXRSJMIDT-UHFFFAOYSA-N trihydroxy(phenyl)silane Chemical class O[Si](O)(O)C1=CC=CC=C1 FCVNATXRSJMIDT-UHFFFAOYSA-N 0.000 description 1
- HFHNMMYXHFSSPL-UHFFFAOYSA-N trihydroxy(pyren-1-yl)silane Chemical class C1=C2C([Si](O)(O)O)=CC=C(C=C3)C2=C2C3=CC=CC2=C1 HFHNMMYXHFSSPL-UHFFFAOYSA-N 0.000 description 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 1
- GIULLRLLAPLKNF-UHFFFAOYSA-N trimethoxy(pyren-1-yl)silane Chemical compound C1=C2C([Si](OC)(OC)OC)=CC=C(C=C3)C2=C2C3=CC=CC2=C1 GIULLRLLAPLKNF-UHFFFAOYSA-N 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
- 239000005051 trimethylchlorosilane Substances 0.000 description 1
- ZQTYRTSKQFQYPQ-UHFFFAOYSA-N trisiloxane Chemical compound [SiH3]O[SiH2]O[SiH3] ZQTYRTSKQFQYPQ-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- MQWLIFWNJWLDCI-UHFFFAOYSA-L zinc;carbonate;hydrate Chemical compound O.[Zn+2].[O-]C([O-])=O MQWLIFWNJWLDCI-UHFFFAOYSA-L 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
本發明之目的在於提供一種對基材之接著性較高且形成透明之硬化物的硬化性聚矽氧組合物、及使用該組合物而成之可靠性優異之光半導體裝置。
本發明提供一種硬化性聚矽氧組合物,其至少包含:(A)一分子中具有至少2個烯基之有機聚矽氧烷、(B)一分子中具有至少2個鍵結矽原子之氫原子之有機氫化聚矽氧烷、(C)平均單元式所表示之接著促進劑、及(D)矽氫化反應用觸媒。
Description
本發明係關於一種硬化性聚矽氧組合物、及使用該組合物而成之光半導體裝置。
藉由矽氫化反應而硬化之硬化性聚矽氧組合物係用作光電耦合器、發光二極體、固體攝像元件等光半導體裝置中之光半導體元件之保護劑或塗佈劑。由於上述元件係發光或受光,故而對於此種組合物之硬化物,要求吸收光或不散射,又,亦要求接著於上述元件、引線框架、基板、及殼材等。
例如,專利文獻1中記載有含有平均單元式:[(CH2=CH)(CH3)2SiO1/2]25(C6H5SiO3/2)75[Ep(CH3)SiO2/2]40所表示之有機矽化物之硬化性聚矽氧組合物,專利文獻2中記載有含有平均單元式:[(CH3)(C6H5)SiO2/2]0.15[(CH3)(CH2=CH)SiO2/2]0.24(EpSiO3/2)0.19(CH3O1/2)0.42所表示之有機矽化物之硬化性聚矽氧組合物,專利文獻3中記載有含有平均單元式:(C6H5SiO3/2)0.50(EpSiO3/2)0.25[(CH2=CH)(CH3)2SiO1/2]0.25所表示之有機矽化物之硬化性聚矽氧組合物,專利文獻4中記載有含有平均單元式:
(EpSiO3/2)0.3[(CH2=CH)(CH3)SiO2/2]0.3[(CH3)2SiO2/2]0.3(CH3O1/2)0.2所表示之有機矽化物之硬化性聚矽氧組合物,專利文獻5中記載有含有平均單元式:[(CH2=CH)(CH3)SiO2/2]0.2[(C6H5)2SiO2/2]0.5(EpSiO3/2)0.3所表示之有機矽化物之硬化性聚矽氧組合物。再者,上式中,Ep表示3-縮水甘油氧基丙基。
但是,該等硬化性聚矽氧組合物存在發生硬化而獲得之硬化物之透光率較低,或缺乏硬化物對基材之接著性之問題。
[專利文獻1]日本專利特開2007-008996號公報
[專利文獻2]日本專利特開2007-327019號公報
[專利文獻3]日本專利特開2010-001335號公報
[專利文獻4]日本專利特開2010-001336號公報
[專利文獻5]日本專利特開2012-052045號公報
本發明之目的在於提供一種對基材之接著性較高且形成透明之硬化物之硬化性聚矽氧組合物、及使用該組合物而成之可靠性優異之光半導體裝置。
本發明之硬化性聚矽氧組合物之特徵在於至少包含:(A)一分子中具有至少2個烯基之有機聚矽氧烷100質量份、(B)一分子中具有至少2個鍵結矽原子之氫原子之有機氫化聚矽氧烷{相對於(A)成分與(C)成分所含之烯基之合計1莫耳,提供0.1~10.0莫耳之鍵結矽原子之氫原子之量}、
(C)平均單元式:(R1R2SiO2/2)a(R2R3SiO2/2)b(R4SiO3/2)c
(式中,R1為碳數2~12之烯基,R2為相同或不同之碳數1~12之烷基、碳數6~20之芳基、或碳數7~20之芳烷基,R3為含環氧基之有機基,R4為碳數6~20之芳基或碳數7~20之芳烷基,a、b、及c分別為滿足0.1≦a≦0.6、0.1≦b≦0.5、0.3≦c<0.8、0.15≦a/c≦1.5、0.15≦b/c≦1.8、且a+b+c=1之數)
所表示之接著促進劑0.1~50質量份、及(D)矽氫化反應用觸媒(促進本組合物之硬化之量)。
本發明之光半導體裝置之特徵在於:其係利用上述硬化性聚矽氧組合物之硬化物密封光半導體元件而成。
本發明之硬化性聚矽氧組合物具有對基材之接著性較高且形成透明之硬化物之特徵,又,本發明之光半導體裝置具有由於光半導體元件係利用上述組合物之硬化物進行密封,故而可靠性優異之特徵。
1‧‧‧發光元件
2‧‧‧引線框架
3‧‧‧引線框架
4‧‧‧接合線
5‧‧‧殼材
6‧‧‧硬化性聚矽氧組合物之硬化物
圖1係作為本發明之光半導體裝置之一例之LED(Light Emitting Diode,發光二極體)之剖視圖。
首先,對本發明之硬化性聚矽氧組合物進行詳細說明。
(A)成分係作為本組合物之主劑的一分子中具有至少2個烯基之有機聚矽氧烷。作為(A)成分中之烯基,可例示乙烯基、烯丙基、丁烯基、戊烯基、己烯基、庚烯基、辛烯基、壬烯基、癸烯基、十一碳烯基、十二碳烯基等碳數為2~12個之烯基,較佳為乙烯基。又,作為(A)成分中之烯基以外之鍵結矽原子之基,可例示:甲基、乙基、丙基、異丙基、丁基、異丁基、第三丁基、戊基、新戊基、己基、環己
基、庚基、辛基、壬基、癸基、十一烷基、十二烷基等碳數為1~12個之烷基;苯基、甲苯基、二甲苯基、萘基等碳數為6~20個之芳基;苄基、苯乙基、苯丙基等碳數為7~20個之芳烷基;將該等基之氫原子之一部分或全部取代為氟原子、氯原子、溴原子等鹵素原子之基。再者,於(A)成分中之矽原子上,亦可於無損本發明之目的之範圍內具有少量之羥基或甲氧基、乙氧基等烷氧基。
(A)成分之分子結構並無特別限定,可例示直鏈狀、一部分具有支鏈之直鏈狀、支鏈狀、環狀及立體網狀結構。(A)成分可為1種具有該等分子結構之有機聚矽氧烷、或2種以上具有該等分子結構之有機聚矽氧烷之混合物。
(A)成分於25℃下之性狀並無特別限定,例如為液狀或固體狀。(A)成分於25℃下為液狀之情形時,較佳為其於25℃下之黏度為1~1,000,000mPa‧s之範圍內,尤佳為10~1,000,000mPa‧s之範圍內。再者,該黏度例如可藉由使用依據JIS K 7117-1之B型黏度計之測定而求出。
較佳為此種(A)成分包含以平均單元式:(R1R5 2SiO1/2)d(R5 2SiO2/2)e(R4SiO3/2)f
表示,且一分子中具有至少2個烯基之有機聚矽氧烷樹脂。
式中,R1為碳數2~12之烯基。具體而言,可例示:乙烯基、烯丙基、丁烯基、戊烯基、己烯基、庚烯基、辛烯基、壬烯基、癸烯基、十一碳烯基、十二碳烯基。
式中,R4為碳數6~20之芳基或碳數7~20之芳烷基。具體而言,可例示:苯基、甲苯基、二甲苯基、萘基、蒽基、菲基、芘基等芳基;萘乙基、萘丙基、蒽乙基、菲乙基、芘乙基等芳烷基;及將該等芳基或芳烷基之氫原子之一部分或全部取代為甲基、乙基等烷基,甲氧基、乙氧基等烷氧基,氯原子、溴原子等鹵素原子之基。
式中,R5為相同或不同之碳數1~12之烷基、碳數2~12之烯基、碳數6~20之芳基、或碳數7~20之芳烷基。具體而言,可例示:甲基、乙基、丙基、丁基、戊基、己基、庚基、辛基、壬基、癸基、十一烷基、十二烷基等烷基;乙烯基、烯丙基、丁烯基、戊烯基、己烯基、庚烯基、辛烯基、壬烯基、癸烯基、十一碳烯基、十二碳烯基等烯基;苯基、甲苯基、二甲苯基、萘基、蒽基、菲基、芘基等芳基;萘乙基、萘丙基、蒽乙基、菲乙基、芘乙基等芳烷基;及將該等芳基或芳烷基之氫原子之一部分或全部取代為甲基、乙基等烷基,甲氧基、乙氧基等烷氧基,氯原子、溴原子等鹵素原子之基。
式中,d、e、及f分別為滿足0.01≦d≦0.5、0≦e≦0.7、0.1≦f<0.9、且d+e+f=1之數,較佳為滿足0.1≦d≦0.4、0≦e≦0.5、0.4≦f<0.9、且d+e+f=1之數。其原因在於:若d為上述範圍之下限以上,則所獲得之組合物之硬化性良好,另一方面,若為上述範圍之上限以下,則所獲得之硬化物之強度提高。又,若e為上述範圍之上限以下,則所獲得之硬化物之可撓性提高。又,若f為上述範圍之下限以上,則所獲得之硬化物之透明性提高,另一方面,若為上述範圍之上限以下,則本成分之操作作業性提高。
進而,較佳為(A)成分包含一分子中具有至少2個鍵結矽原子之烯基與至少1個鍵結矽原子之芳基的直鏈狀之有機聚矽氧烷。
作為此種(A)成分,可例示如下之有機聚矽氧烷。再者,式中,Me、Vi、Ph分別表示甲基、乙烯基、苯基,x、x'分別為1~100之整數。
ViPhMeSiO(Me2SiO)xSiMePhVi
ViPh2SiO(Me2SiO)xSiPh2Vi
ViMe2SiO(Me2SiO)x(Ph2SiO)x'SiMe2Vi
ViPhMeSiO(Me2SiO)x(Ph2SiO)x'SiPhMeVi
ViPh2SiO(Me2SiO)x(Ph2SiO)x'SiPh2Vi
ViMe2SiO(MePhSiO)xSiMe2Vi
MePhViSiO(MePhSiO)xSiMePhVi
Ph2ViSiO(MePhSiO)xSiPh2Vi
ViMe2SiO(Ph2SiO)x(PhMeSiO)x'SiMe2Vi
ViPhMeSiO(Ph2SiO)x(PhMeSiO)x'SiPhMeVi
ViPh2SiO(Ph2SiO)x(PhMeSiO)x'SiPh2Vi
(B)成分係本組合物之交聯劑,且係一分子中具有至少2個鍵結矽原子之氫原子的有機聚矽氧烷。作為(B)成分之分子結構,例如可列舉直鏈狀、一部分具有支鏈之直鏈狀、支鏈狀、環狀、樹枝狀,較佳為直鏈狀、一部分具有支鏈之直鏈狀、樹枝狀。(B)成分中之鍵結矽原子之氫原子之鍵結位置並無限定,例如可列舉分子鏈之末端及/或側鏈。又,作為(B)成分中之氫原子以外之鍵結矽原子之基,可例示:甲基、乙基、丙基等烷基,苯基、甲苯基、二甲苯基等芳基,苄基、苯乙基等芳烷基,3-氯丙基、3,3,3-三氯丙基等鹵化烷基,較佳為甲基、苯基。又,(B)成分之黏度並無限定,較佳為於25℃下之黏度為1~10,000mPa‧s之範圍內,尤佳為1~1,000mPa‧s之範圍內。
作為此種(B)成分,可例示:1,1,3,3-四甲基二矽氧烷、1,3,5,7-四甲基環四矽氧烷、三(二甲基氫矽烷氧基)甲基矽烷、三(二甲基氫矽烷氧基)苯基矽烷、1-縮水甘油氧基丙基-1,3,5,7-四甲基環四矽氧烷、1,5-縮水甘油氧基丙基-1,3,5,7-四甲基環四矽氧烷、1-縮水甘油氧基丙基-5-三甲氧基矽烷基乙基-1,3,5,7-四甲基環四矽氧烷、三甲基矽氧基封阻分子鏈兩末端之甲基氫聚矽氧烷、三甲基矽氧基封阻分子鏈兩末端之二甲基矽氧烷-甲基氫矽氧烷共聚物、二甲基氫矽氧基封阻分子鏈兩末端之二甲基聚矽氧烷、二甲基氫矽氧基封阻分子鏈兩末端之二甲基矽氧烷-甲基氫矽氧烷共聚物、三甲基矽氧基封阻分子鏈兩末端
之甲基氫矽氧烷-二苯基矽氧烷共聚物、三甲基矽氧基封阻分子鏈兩末端之甲基氫矽氧烷-二苯基矽氧烷-二甲基矽氧烷共聚物、三甲氧基矽烷之水解縮合物、包含(CH3)2HSiO1/2單元與SiO4/2單元之共聚物、及包含(CH3)2HSiO1/2單元與SiO4/2單元與(C6H5)SiO3/2單元之共聚物,此外可例示如下之有機矽氧烷。再者,式中,Me、Vi、Ph、Naph分別表示甲基、乙烯基、苯基、萘基,y、y'分別為1~100之整數,g、h、i、j分別為正數,其中,g、h、i、j之合計為1。
HMe2SiO(Ph2SiO)ySiMe2H
HMePhSiO(Ph2SiO)ySiMePhH
HMeNaphSiO(Ph2SiO)ySiMeNaphH
HMePhSiO(Ph2SiO)y(MePhSiO)y'SiMePhH
HMePhSiO(Ph2SiO)y(Me2SiO)y'SiMePhH
(HMe2SiO1/2)g(PhSiO3/2)h
(HMePhSiO1/2)g(PhSiO3/2)h
(HMePhSiO1/2)g(NaphSiO3/2)h
(HMe2SiO1/2)g(NaphSiO3/2)h
(HMePhSiO1/2)g(HMe2SiO1/2)h(PhSiO3/2)i
(HMe2SiO1/2)g(Ph2SiO2/2)h(PhSiO3/2)i
(HMePhSiO1/2)g(Ph2SiO2/2)h(PhSiO3/2)i
(HMe2SiO1/2)g(Ph2SiO2/2)h(NaphSiO3/2)i
(HMePhSiO1/2)g(Ph2SiO2/2)h(NaphSiO3/2)i
(HMePhSiO1/2)g(HMe2SiO1/2)h(NaphSiO3/2)i
(HMePhSiO1/2)g(HMe2SiO1/2)h(Ph2SiO2/2)i(NaphSiO3/2)j
(HMePhSiO1/2)g(HMe2SiO1/2)h(Ph2SiO2/2)i(PhSiO3/2)j
關於(B)成分之含量,相對於(A)成分及(C)成分所含之烯基之合計1莫耳,為本成分中之鍵結矽原子之氫原子成為0.1~10.0莫耳之範
圍內之量,較佳為成為0.1~5莫耳之範圍內之量,進而較佳為成為0.5~2莫耳之範圍內之量。其原因在於:若(B)成分之含量為上述範圍之下限以上,則所獲得之組合物充分硬化,另一方面,若為上述範圍之上限以下,則所獲得之硬化物之耐熱性提高,進而,使用本組合物所製作之光半導體裝置之可靠性提高。
(C)成分係用以對本組合物賦予接著性之接著促進劑,其以平均單元式:(R1R2SiO2/2)a(R2R3SiO2/2)b(R4SiO3/2)c表示。
式中,R1為碳數2~12之烯基。具體而言,可例示:乙烯基、烯丙基、丁烯基、戊烯基、己烯基、庚烯基、辛烯基、壬烯基、癸烯基、十一碳烯基、十二碳烯基,較佳為乙烯基。
式中,R2為相同或不同之碳數1~12之烷基、碳數6~20之芳基、或碳數7~20之芳烷基。具體而言,可例示:甲基、乙基、丙基、丁基、戊基、己基、庚基、辛基、壬基、癸基、十一烷基、十二烷基等烷基;乙烯基、烯丙基、丁烯基、戊烯基、己烯基、庚烯基、辛烯基、壬烯基、癸烯基、十一碳烯基、十二碳烯基等烯基;苯基、甲苯基、二甲苯基、萘基、蒽基、菲基、芘基等芳基;萘乙基、萘丙基、蒽乙基、菲乙基、芘乙基等芳烷基;及將該等芳基或芳烷基之氫原子之一部分或全部取代為甲基、乙基等烷基,甲氧基、乙氧基等烷氧基,及氯原子、溴原子等鹵素原子之基,較佳為甲基、乙烯基、苯基。
式中,R3為含環氧基之有機基。具體而言,可例示:2-縮水甘油氧基乙基、3-縮水甘油氧基丙基、4-縮水甘油氧基丁基等縮水甘油氧基烷基;2-(3,4-環氧環己基)乙基、3-(3,4-環氧環己基)丙基等環氧環烷基烷基;3,4-環氧丁基、7,8-環氧辛基等環氧烷基,較佳為縮水甘油氧基烷基,尤佳為3-縮水甘油氧基丙基。
式中,R4為碳數6~20之芳基或碳數7~20之芳烷基,可例示與上
述R2相同之基。
式中,a、b、及c分別為滿足0.1≦a≦0.6、0.1≦b≦0.5、0.3≦c<0.8、0.15≦a/c≦1.5、0.15≦b/c≦1.8、且a+b+c=1之數,較佳為滿足0.2≦a≦0.6、0.1≦b≦0.45、0.3≦c<0.7、0.15≦a/c≦1.5、0.15≦b/c≦1.8、且a+b+c=1之數,更佳為滿足0.2≦a≦0.5、0.1≦b≦0.4、0.3≦c<0.65、0.15≦a/c≦1.5、0.15≦b/c≦1.8、且a+b+c=1之數。其原因在於:若a為上述範圍之下限以上,則所獲得之硬化物變得難以黏膩,另一方面,若為上述範圍之上限以下,則所獲得之硬化物之接著性良好。又,若b為上述範圍之下限以上,則所獲得之硬化物之接著性良好,另一方面,若為上述範圍之上限以下,則所獲得之硬化物之耐熱性提高。又,若c為上述範圍之下限以上,則所獲得之硬化物之折射率良好。進而,若a/c之值為上述範圍之下限以上,則所獲得之硬化物之接著性良好,另一方面,若為上述範圍之上限以下,則所獲得之組合物之硬化性良好。又,若b/c之值為上述範圍之下限以上,則所獲得之硬化物之接著性良好,另一方面,若為上述範圍之上限以下,則所獲得之硬化物之耐熱性良好。
(C)成分係以上述平均單元式表示,但於無損本發明之目的之範圍內亦可具有式:R5 3SiO1/2所表示之矽氧烷單元、式:R6SiO3/2所表示之矽氧烷單元、或式:SiO4/2所表示之矽氧烷單元。式中,R5為相同或不同之碳數1~12之烷基、碳數6~20之芳基、或碳數7~20之芳烷基。作為R5之烷基、芳基、及芳烷基,可例示與上述R2相同之烷基、芳基、及芳烷基。式中,R6為碳數1~12之烷基或碳數2~12之烯基。作為R6之烷基,可例示與上述R2相同之烷基。作為R6之烯基,可例示與上述R1相同之烯基。進而,於(C)成分中,於無損本發明之目的之範圍內亦可具有甲氧基、乙氧基、丙氧基等鍵結矽原子之烷氧基、或鍵結矽原子之羥基。
製備此種(C)成分之方法並無特別限定,例如可列舉:使通式(I-1):R1R2SiX2所表示之矽烷化合物或通式(I-2):(R1R2SiO)m所表示之環狀聚矽氧化合物、通式(II):R2R3SiX2所表示之矽烷化合物及通式(III):R4SiX3所表示之矽烷化合物於酸或鹼之存在下進行水解、縮合反應之方法。
通式(I-1)所表示之矽烷化合物係用以對(C)成分導入式:R1R2SiO2/2所表示之矽氧烷單元之原料。式中,R1為碳數2~12之烯基,可例示與上述相同之基,較佳為乙烯基。R2為相同或不同之碳數1~12之烷基、碳數6~20之芳基、或碳數7~20之芳烷基,可例示與上述相同之基,較佳為甲基。式中,X為相同或不同之烷氧基、醯氧基、鹵素原子、或羥基。作為X之烷氧基,可例示甲氧基、乙氧基、丙氧基。又,作為X之醯氧基,可例示乙醯氧基。又,作為X之鹵素原子,可例示氯原子、溴原子。
作為此種矽烷化合物,可例示:乙烯基甲基二甲氧基矽烷、苯基乙烯基二甲氧基矽烷、乙烯基甲基二乙氧基矽烷、苯基乙烯基二乙氧基矽烷等烷氧基矽烷;乙烯基甲基二乙醯氧基矽烷、苯基乙烯基二乙醯氧基矽烷等醯氧基矽烷;乙烯基甲基二氯矽烷、苯基乙烯基二氯矽烷等鹵矽烷及乙烯基甲基二羥基矽烷等羥基矽烷。
通式(I-2)所表示之環狀聚矽氧化合物係用以對(C)成分導入式:R1R2SiO2/2所表示之矽氧烷單元之原料。式中,R1為碳數2~12之烯基,可例示與上述相同之基,較佳為乙烯基。式中,R2為碳數1~12之烷基、碳數6~20之芳基、或碳數7~20之芳烷基,可例示與上述相同之基,較佳為甲基。
作為此種環狀聚矽氧化合物,可例示乙烯基甲基環矽氧烷、苯基乙烯基環矽氧烷。
通式(II)所表示之矽烷化合物係用以對(C)成分導入式:
R2R3SiO2/2所表示之矽氧烷單元之原料。式中,R2為碳數1~12之烷基、碳數6~20之芳基、或碳數7~20之芳烷基,可例示與上述相同之基,較佳為乙烯基。又,式中,R3為含環氧基之有機基,可例示與上述相同之基。
作為此種矽烷化合物,可例示:3-縮水甘油氧基丙基甲基二甲氧基矽烷、4-縮水甘油氧基丁基甲基二甲氧基矽烷、2-(3,4-環氧環己基)乙基二甲氧基矽烷、3-(3,4-環氧環己基)丙基二甲氧基矽烷、3-縮水甘油氧基丙基甲基二乙氧基矽烷、4-縮水甘油氧基丁基甲基二乙氧基矽烷、2-(3,4-環氧環己基)乙基二乙氧基矽烷、3-(3,4-環氧環己基)丙基二乙氧基矽烷。
通式(III)所表示之矽烷化合物係用以對(C)成分導入式:R4SiO3/2所表示之矽氧烷單元之原料。式中,R4為碳數6~20之芳基、或碳數7~20之芳烷基,可例示與上述相同之基,較佳為苯基。
作為此種矽烷化合物,可例示:苯基三甲氧基矽烷、萘基三甲氧基矽烷、蒽基三甲氧基矽烷、菲基三甲氧基矽烷、芘基三甲氧基矽烷、苯基三乙氧基矽烷、萘基三乙氧基矽烷、蒽基三乙氧基矽烷、菲基三乙氧基矽烷、芘基三乙氧基矽烷等烷氧基矽烷;苯基三乙醯氧基矽烷、萘基三乙醯氧基矽烷、蒽基三乙醯氧基矽烷、菲基三乙醯氧基矽烷、芘基三乙醯氧基矽烷等醯氧基矽烷;苯基三氯矽烷、萘基三氯矽烷、蒽基三氯矽烷、菲基三氯矽烷、芘基三氯矽烷等鹵矽烷;苯基三羥基矽烷、萘基三羥基矽烷、蒽基三羥基矽烷、菲基三羥基矽烷、芘基三羥基矽烷等羥基矽烷。
上述製備方法之特徵在於:使矽烷化合物(I-1)或環狀聚矽氧化合物(I-2)、矽烷化合物(II)、及矽烷化合物(III)於酸或鹼之存在下進行水解、縮合反應。
作為上述酸,可例示:鹽酸、乙酸、甲酸、硝酸、草酸、硫
酸、磷酸、多磷酸、多元羧酸、三氟甲磺酸、離子交換樹脂。又,作為上述鹼,可例示:氫氧化鉀、氫氧化鈉等無機鹼;三乙胺、二乙胺、單乙醇胺、二乙醇胺、三乙醇胺、氨水、氫氧化四甲基銨、具有胺基之烷氧基矽烷、胺基丙基三甲氧基矽烷等有機鹼化合物。
又,於上述製備方法中,可使用有機溶劑。作為可使用之有機溶劑,可例示:醚類、酮類、乙酸酯類、芳香族或脂肪族烴、γ-丁內酯、及2種以上該等之混合物。作為較佳之有機溶劑,可例示:丙二醇單甲醚、丙二醇單甲醚乙酸酯、丙二醇單乙醚、丙二醇單丙醚、丙二醇單丁醚、丙二醇單第三丁醚、γ-丁內酯、甲苯、二甲苯。
於上述製備方法中,為了促進上述各成分之水解、縮合反應,較佳為添加水、或水與醇之混合液。作為該醇,較佳為甲醇、乙醇。該反應藉由加熱得以促進,於使用有機溶劑之情形時,較佳為於其回流溫度下進行反應。
(C)成分之含量相對於(A)成分100質量份為0.1~50質量份之範圍內,較佳為0.1~20質量份之範圍內。其原因在於:若(C)成分之含量為上述範圍之下限以上,則可對所獲得之組合物賦予充分之接著性,另一方面,若為上述範圍之下限以下,則難以阻礙所獲得之組合物之硬化性,又,可抑制所獲得之硬化物之著色等。
(D)成分係用以促進本組合物之硬化之矽氫化反應用觸媒,可例示:鉑系觸媒、銠系觸媒、鈀系觸媒。尤其是由於可顯著地促進本組合物之硬化,故而較佳為(D)成分為鉑系觸媒。作為該鉑系觸媒,可例示:鉑細粉末、氯鉑酸、氯鉑酸之醇溶液、鉑-烯基矽氧烷錯合物、鉑-烯烴錯合物、鉑-羰基錯合物,較佳為鉑-烯基矽氧烷錯合物。
(D)成分之含量係用以促進本組合物之硬化之有效量。具體而言,(D)成分之含量由於可充分地促進本組合物之硬化反應,故而相對於本組合物,以質量單位計較佳為(D)成分中之觸媒金屬成為0.01
~500ppm之範圍內之量,進而較佳為成為0.01~100ppm之範圍內之量,尤佳為成為0.01~50ppm之範圍內之量。
又,於本組合物中,作為其他任意之成分,亦可含有:2-甲基-3-丁炔-2-醇、3,5-二甲基-1-己炔-3-醇、2-苯基-3-丁炔-2-醇等炔醇;3-甲基-3-戊烯-1-炔、3,5-二甲基-3-己烯-1-炔等烯炔化合物;1,3,5,7-四甲基-1,3,5,7-四乙烯基環四矽氧烷、1,3,5,7-四甲基-1,3,5,7-四己烯基環四矽氧烷、苯并三唑等反應抑制劑。於本組合物中,該反應抑制劑之含量並無限定,相對於上述(A)成分~(C)成分之合計100質量份,較佳為0.0001~5質量份之範圍內。
進而,於本組合物中,為了提高硬化過程中硬化物對於所接觸之基材之接著性,亦可含有(C)成分以外之接著促進劑。作為該接著促進劑,較佳為一分子中具有至少1個鍵結矽原子之烷氧基之有機矽化物。作為該烷氧基,可例示:甲氧基、乙氧基、丙氧基、丁氧基、甲氧基乙氧基,尤佳為甲氧基。又,作為該有機矽化物之鍵結矽原子之烷氧基以外之基,可例示:烷基、烯基、芳基、芳烷基、鹵化烷基等經取代或未經取代之一價烴基;3-縮水甘油氧基丙基、4-縮水甘油氧基丁基等縮水甘油氧基烷基;2-(3,4-環氧環己基)乙基、3-(3,4-環氧環己基)丙基等環氧環己基烷基;3,4-環氧丁基、7,8-環氧辛基等環氧烷基;3-甲基丙烯醯氧基丙基等含丙烯醯基之一價有機基;氫原子。較佳為該有機矽化物具有鍵結矽原子之烯基或鍵結矽原子之氫原子。又,由於可對各種基材賦予良好之接著性,故而較佳為該有機矽化物係一分子中具有至少1個含環氧基之一價有機基者。作為此種有機矽化物,可例示:有機矽烷化合物、有機矽氧烷低聚物、矽酸烷基酯。作為該有機矽氧烷低聚物或矽酸烷基酯之分子結構,可例示直鏈狀、一部分具有支鏈之直鏈狀、支鏈狀、環狀、網狀,尤佳為直鏈狀、支鏈狀、網狀。作為此種有機矽化物,可例示:3-縮水甘油氧基丙基三
甲氧基矽烷、2-(3,4-環氧環己基)乙基三甲氧基矽烷、3-甲基丙烯醯氧基丙基三甲氧基矽烷等矽烷化合物;一分子中分別具有至少1個鍵結矽原子之烯基或鍵結矽原子之氫原子、及鍵結矽原子之烷氧基的矽氧烷化合物、具有至少1個鍵結矽原子之烷氧基之矽烷化合物或矽氧烷化合物與一分子中分別具有至少1個鍵結矽原子之羥基及鍵結矽原子之烯基之矽氧烷化合物的混合物、聚矽酸甲酯、聚矽酸乙酯、含環氧基之聚矽酸乙酯。
進而,於本組合物中,亦可含有用以轉換自利用本組成之硬化物密封或被覆而成之發光元件所放出之光之波長而獲得所需波長之光的螢光體。作為此種螢光體,可例示:廣泛地用於發光二極體(LED)之包含氧化物系螢光體、氮氧化物系螢光體、氮化物系螢光體、硫化物系螢光體、氧硫化物系螢光體等之黃色、紅色、綠色、藍色發光螢光體。作為氧化物系螢光體,可例示:包含鈰離子之釔、鋁、石榴石系之YAG系綠色~黃色發光螢光體、包含鈰離子之鋱、鋁、石榴石系之TAG系黃色發光螢光體、及包含鈰或銪離子之矽酸鹽系綠色~黃色發光螢光體。作為氮氧化物系螢光體,可例示:包含銪離子之矽、鋁、氧、氮系之賽隆系紅色~綠色發光螢光體。作為氮化物系螢光體,可例示:包含銪離子之鈣、鍶、鋁、矽、氮系之CASN系紅色發光螢光體。作為硫化物系螢光體,可例示:包含銅離子或鋁離子之ZnS系綠色顯色螢光體。作為氧硫化物系螢光體,可例示:包含銪離子之Y2O2S系紅色發光螢光體。該等螢光體可使用1種或2種以上之混合物。於本組合物中,螢光體之含量相對於(A)成分與(B)成分之合計量為0.1~70質量%之範圍內,較佳為1~20質量%之範圍內。
又,於本組合物中,只要無損本發明之目的,則作為其他任意之成分,亦可含有:二氧化矽、玻璃、氧化鋁、氧化鋅等無機填充劑;聚甲基丙烯酸酯樹脂等有機樹脂細粉末;耐熱劑、染料、顏料、
阻燃性賦予劑、溶劑等。
作為任意成分而添加之成分中,為了充分地抑制因空氣中之含硫氣體引起之光半導體裝置中之銀電極或基板之鍍銀層之變色,可添加選自由表面被覆有選自由Al、Ag、Cu、Fe、Sb、Si、Sn、Ti、Zr、及稀土元素所組成之群中之至少1種元素之氧化物的氧化鋅細粉末、利用不具有烯基之有機矽化物進行過表面處理之氧化鋅細粉末、及碳酸鋅之水合物細粉末所組成之群中之平均粒徑為0.1nm~5μm之至少一種細粉末。
於表面被覆有氧化物之氧化鋅細粉末中,作為稀土元素,可例示釔、鈰、銪。作為氧化鋅細粉末之表面之氧化物,可例示:Al2O3、AgO、Ag2O、Ag2O3、CuO、Cu2O、FeO、Fe2O3、Fe3O4、Sb2O3、SiO2、SnO2、Ti2O3、TiO2、Ti3O5、ZrO2、Y2O3、CeO2、Eu2O3及2種以上該等氧化物之混合物。
於利用有機矽化物進行過表面處理之氧化鋅細粉末中,該有機矽化物係不具有烯基者,可例示:有機矽烷、有機矽氮烷、聚甲基矽氧烷、有機氫聚矽氧烷、及有機矽氧烷低聚物,具體而言,可例示:三甲基氯矽烷、二甲基氯矽烷、甲基三氯矽烷等有機氯矽烷;甲基三甲氧基矽烷、甲基三乙氧基矽烷、苯基三甲氧基矽烷、乙基三甲氧基矽烷、正丙基三甲氧基矽烷、γ-甲基丙烯醯氧基丙基三甲氧基矽烷等有機三烷氧基矽烷;二甲基二甲氧基矽烷、二甲基二乙氧基矽烷、二苯基二甲氧基矽烷等二有機二烷氧基矽烷;三甲基甲氧基矽烷、三甲基乙氧基矽烷等三有機烷氧基矽烷;該等有機烷氧基矽烷之部分縮合物;六甲基二矽氮烷等有機矽氮烷;聚甲基矽氧烷、有機氫聚矽氧烷、具有矽烷醇基或烷氧基之有機矽氧烷低聚物、包含R6SiO3/2單元(式中,R6為甲基、乙基、丙基等烷基,苯基等芳基所例示之除烯基以外之一價烴基)或SiO4/2單元且具有矽烷醇基或烷氧基之樹脂狀有機
聚矽氧烷。
又,於本組合物中,由於可進而抑制因空氣中之含硫氣體引起之銀電極及基板之鍍銀層之變色,故而作為任意之成分,亦可含有三唑系化合物。作為此種成分,可例示:1H-1,2,3-三唑、2H-1,2,3-三唑、1H-1,2,4-三唑、4H-1,2,4-三唑、2-(2'-羥基-5'-甲基苯基)苯并三唑、1H-1,2,3-三唑、2H-1,2,3-三唑、1H-1,2,4-三唑、4H-1,2,4-三唑、苯并三唑、甲苯并三唑、羧基苯并三唑、1H-苯并三唑-5-羧酸甲酯、3-胺基-1,2,4-三唑、4-胺基-1,2,4-三唑、5-胺基-1,2,4-三唑、3-巰基-1,2,4-三唑、氯苯并三唑、硝基苯并三唑、胺基苯并三唑、環己并[1,2-d]三唑、4,5,6,7-四羥基甲苯并三唑、1-羥基苯并三唑、乙基苯并三唑、萘并三唑、1-N,N-雙(2-乙基己基)-[(1,2,4-三唑-1-基)甲基]胺、1-[N,N-雙(2-乙基己基)胺基甲基]苯并三唑、1-[N,N-雙(2-乙基己基)胺基甲基]甲苯并三唑、1-[N,N-雙(2-乙基己基)胺基甲基]羧基苯并三唑、1-[N,N-雙(2-羥基乙基)胺基甲基]苯并三唑、1-[N,N-雙(2-羥基乙基)胺基甲基]甲苯并三唑、1-[N,N-雙(2-羥基乙基)胺基甲基]羧基苯并三唑、1-[N,N-雙(2-羥基丙基)胺基甲基]羧基苯并三唑、1-[N,N-雙(1-丁基)胺基甲基]羧基苯并三唑、1-[N,N-雙(1-辛基)胺基甲基]羧基苯并三唑、1-(2',3'-二羥基丙基)苯并三唑、1-(2',3'-二羧基乙基)苯并三唑、2-(2'-羥基-3',5'-二第三丁基苯基)苯并三唑、2-(2'-羥基-3',5'-二戊基苯基)苯并三唑、2-(2'-羥基-4'-辛氧基苯基)苯并三唑、2-(2'-羥基-5'-第三丁基苯基)苯并三唑、1-羥基苯并三唑-6-羧酸、1-油醯基苯并三唑、1,2,4-三唑-3-醇、5-胺基-3-巰基-1,2,4-三唑、5-胺基-1,2,4-三唑-3-羧酸、1,2,4-三唑-3-羧醯胺、4-胺基脲唑、及1,2,4-三唑-5-酮。該苯并三唑化合物之含量並無特別限定,於本組合物中以質量單位計為成為0.01ppm~3%之範圍內之量,較佳為成為0.1ppm~1%之範圍內之量。
本組合物係於室溫下進行硬化或藉由加熱進行硬化,但為了使之迅速硬化,較佳為進行加熱。作為該加熱溫度,較佳為50~200℃之範圍內。
其次,對本發明之光半導體裝置進行詳細說明。
本發明之光半導體裝置之特徵在於:其係利用上述硬化性聚矽氧組合物之硬化物對光半導體元件進行密封而成。作為此種本發明之光半導體裝置,可例示發光二極體(LED)、光電耦合器、CCD(Charge Coupled Device,電荷耦合元件)。又,作為光半導體元件,可例示發光二極體(LED)晶片、固體攝像元件。
將作為本發明之光半導體裝置之一例的單獨體之表面安裝型LED之剖視圖表示於圖1。於圖1所表示之LED中,發光元件(LED晶片)1係黏晶於引線框架2上,該發光元件(LED晶片)1係利用接合線4而與引線框架3進行打線接合。該發光元件(LED晶片)1之周圍設置有殼材5,該殼材5之內側之發光元件(LED晶片)1係利用本發明之硬化性聚矽氧組合物之硬化物6而被密封。
作為製造圖1所示之表面安裝型LED的方法,可例示:將發光元件(LED晶片)1黏晶於引線框架2上,將該發光元件(LED晶片)1與引線框架3利用金製之接合線4進行打線接合,繼而於發光元件(LED晶片)1之周圍所設置之殼材5之內側填充本發明之硬化性聚矽氧組合物後,藉由在50~200℃下進行加熱而使之硬化的方法。
藉由實施例,對本發明之硬化性聚矽氧組合物、及光半導體裝置進行詳細說明。再者,於實施例中,黏度係於25℃下之值,Me、Vi、Ph、Ep分別表示甲基、乙烯基、苯基、3-縮水甘油氧基丙基。又,藉由如下方式測定硬化性聚矽氧組合物之硬化物之特性。
[透過率]
將表1所表示之硬化性聚矽氧組合物澆注至長100mm×寬10mm×厚4mm之模具內,於150℃下加熱120分鐘而使之硬化。將所製作之硬化物試驗體放入石英池中並利用自動分光光度計測定透射光譜而求出450nm之透過率。
[接著力]
[硬化性聚矽氧組合物之硬化物之接著力]
於2塊鋁板、銀板、聚鄰苯二甲醯胺板(寬25mm,長75mm,厚1mm)之間挾入聚四氟乙烯樹脂製之間隔片(寬10mm,長20mm,厚1mm),於其間隙中填充硬化性聚矽氧組合物並利用夾具加以固定,於150℃之循環式熱風烘箱中保持1小時使之硬化,藉此製作試驗體。冷卻至室溫後,拆去夾具與間隔片並利用拉力試驗機測定硬化物之剪切接著力。
[表面安裝型之發光二極體(LED)之製作]
朝向底部經堵塞之圓筒狀聚鄰苯二甲醯胺(PPA)樹脂製殼材5(內徑2.0mm,深1.0mm)之內底部之中心部,引線框架2、3自側壁外延,引線框架2之中央部載置有LED晶片1,LED晶片1與引線框架3係利用接合線4進行電性連接之未密封之光半導體裝置內,將硬化性聚矽氧組合物消泡並使用分注器注入其中。其後,於加熱烘箱中,藉由在100℃下加熱30分鐘,繼而在150℃下加熱1小時,使硬化性聚矽氧組合物硬化,而製作圖1所示之表面安裝型之發光二極體(LED)。
[熱衝擊試驗]
重複進行熱衝擊試驗750次,該熱衝擊試驗係將藉由上述方法所製作之16個發光二極體於-40℃下保持30分鐘後,於120℃下保持30分鐘作為1個循環(-40℃120℃),其後,恢復至室溫(25℃)進行點亮試驗並確認通電。將導線切斷之比率(切斷之個數/16個)表示於表1。
[參考例1]
向附帶攪拌機、回流冷卻管、溫度計之反應容器中投入苯基三甲氧基矽烷148.5g(0.75mol)、環狀乙烯基甲基環矽氧烷43.0g(0.5mol)、及三氟甲磺酸0.11g,添加水21g。其後,回流2小時而去除低沸點成分。繼而,將反應體系冷卻後,添加甲苯、氫氧化鉀水溶液。其後,添加3-縮水甘油氧基丙基甲基二甲氧基矽烷88.1g(0.4mol)、水14.4g。回流1小時後,蒸餾去除甲醇,藉由共沸脫水去除過剩之水。加熱回流5小時後,將甲苯溶液冷卻,利用1.1g乙酸進行中和後,水洗3次。去除水後,於減壓下蒸餾去除甲苯,而製備黏度為25.3Pa‧s之平均單元式:(PhSiO3/2)0.45(MeViSiO2/2)0.30(MeEpSiO2/2)0.25
所表示之接著促進劑。
[參考例2]
向附帶攪拌機、回流冷卻管、溫度計之反應容器內投入苯基三甲氧基矽烷148.5g(0.75mol)、環狀乙烯基甲基環矽氧烷64.5g(0.75mol)、及三氟甲磺酸0.11g,添加水21.2g。其後,回流2小時,去除低沸點成分。繼而,將反應體系冷卻後,添加甲苯、氫氧化鉀水溶液。其後,添加3-縮水甘油氧基丙基甲基二甲氧基矽烷88.1g(0.4mol)、水14.4g。回流1小時後,蒸餾去除甲醇,藉由共沸脫水去除過剩之水。加熱回流5小時後,將甲苯溶液冷卻,利用1.1g乙酸進行中和後,水洗3次。去除水後,於減壓下蒸餾去除甲苯,而製備黏度為21.1Pa‧s之平均單元式:(PhSiO3/2)0.39(MeViSiO2/2)0.40(MeEpSiO2/2)0.21
所表示之接著促進劑。
[參考例3]
向附帶攪拌機、回流冷卻管、溫度計之反應容器內投入苯基三甲氧基矽烷148.5g(0.75mol)、環狀乙烯基甲基環矽氧烷21.5g(0.25
mol)、及三氟甲磺酸0.11g,添加水21.2g。其後,回流2小時,去除低沸點成分。繼而,將反應系冷卻後,添加甲苯、氫氧化鉀水溶液。其後,添加3-縮水甘油氧基丙基甲基二甲氧基矽烷88.1g(0.4mol)、水14.4g。回流1小時後,蒸餾去除甲醇,藉由共沸脫水去除過量之水。加熱回流5小時後,將甲苯溶液冷卻,利用1.1g乙酸進行中和後,水洗3次。去除水後,於減壓下蒸餾去除甲苯,而製備黏度為29.1Pa‧s之平均單元式:(PhSiO3/2)0.54(MeViSiO2/2)0.18(MeEpSiO2/2)0.28
所表示之接著促進劑。
[參考例4]
向附帶攪拌機、回流冷卻管、溫度計之四口燒瓶中投入1,3-二乙烯基-1,1,3,3-四甲基二矽氧烷82.2g(0.44mol)、水143g、三氟甲磺酸0.38g、及甲苯500g,於攪拌下以1小時滴加苯基三甲氧基矽烷524.7g(2.65mol)。滴加完畢後,加熱回流1小時。其後,進行冷卻並分離下層,將甲苯溶液層水洗3次。向經水洗之甲苯溶液層投入3-縮水甘油氧基丙基甲基二甲氧基矽烷314g(1.42mol)、水130g、及氫氧化鉀0.50g,加熱回流1小時。繼而,蒸餾去除甲醇,藉由共沸脫水去除過量之水。加熱回流4小時後,冷卻甲苯溶液,利用0.55g乙酸進行中和後,水洗3次。去除水後,於減壓下蒸餾去除甲苯,而製備黏度為8,500mPa‧s之平均單元式:(PhSiO3/2)0.53(Me2ViSiO1/2)0.18(EpMeSiO2/2)0.29
所表示之接著促進劑。
[實施例1~4、比較例1]
使用下述成分而製備表1所表示之組成之硬化性聚矽氧組合物。再者,表1中,(D)成分之含量係以質量單位計之鉑金屬相對於硬化性聚矽氧組合物之含量(ppm)表示。又,表1中之H/Vi係表示(B)成分所
含之鍵結矽原子之氫原子相對於(A)成分與(C)成分所含之烯基之合計1莫耳的莫耳數。
作為(A)成分,使用如下成分:
(A-1)成分:平均單元式:(Me2ViSiO1/2)0.20(PhSiO3/2)0.80
所表示之有機聚矽氧烷
(A-2)成分:平均單元式:(MePhViSiO1/2)0.23(PhSiO3/2)0.77
所表示之有機聚矽氧烷
(A-3)成分:於25℃下之黏度為3,000mPa‧s之二甲基乙烯基矽氧基封阻分子鏈兩末端之甲苯基聚矽氧烷
作為(B)成分,使用如下成分:
(B-1)成分:於25℃下之黏度為4mPa‧s之式:HMe2SiOPh2SiOSiMe2H
所表示之有機三矽氧烷
作為(C)成分,使用如下成分:
(C-1)成分:參考例1中所製備之接著促進劑
(C-2)成分:參考例2中所製備之接著促進劑
(C-3)成分:參考例3中所製備之接著促進劑
(C-4)成分:參考例4中所製備之接著促進劑
作為(D)成分,使用如下成分:
(D-1)成分:鉑-1,3-二乙烯基-1,1,3,3-四甲基二矽氧烷錯合物之1,3,5,7-四甲基-1,3,5,7-四乙烯基環四矽氧烷之溶液(以鉑計含有0.1質量%之溶液)。
作為(E)成分,使用如下成分:
(E-1)成分:1-乙炔基環己醇
本發明之硬化性聚矽氧組合物可用作電氣、電子用之接著劑、灌封劑、保護劑、塗佈劑、底部填充劑,尤其是由於可形成具有高反應性、低透氣性之硬化物,故而適合作為發光二極體(LED)等光半導體裝置中之光半導體元件之密封材料或保護塗佈材料。
1‧‧‧發光元件
2‧‧‧引線框架
3‧‧‧引線框架
4‧‧‧接合線
5‧‧‧殼材
6‧‧‧硬化性聚矽氧組合物之硬化物
Claims (8)
- 一種硬化性聚矽氧組合物,其至少包含:(A)一分子中具有至少2個烯基之有機聚矽氧烷100質量份、(B)一分子中具有至少2個鍵結矽原子之氫原子之有機氫化聚矽氧烷{相對於(A)成分與(C)成分所含之烯基之合計1莫耳,提供0.1~10.0莫耳之鍵結矽原子之氫原子之量}、(C)平均單元式:(R1R2SiO2/2)a(R2R3SiO2/2)b(R4SiO3/2)c(式中,R1為碳數2~12之烯基,R2為相同或不同之碳數1~12之烷基、碳數6~20之芳基、或碳數7~20之芳烷基,R3為含環氧基之有機基,R4為碳數6~20之芳基或碳數7~20之芳烷基,a、b、及c分別為滿足0.1≦a≦0.6、0.1≦b≦0.5、0.3≦c<0.8、0.15≦a/c≦1.5、0.15≦b/c≦1.8、且a+b+c=1之數)所表示之接著促進劑0.1~50質量份、及(D)矽氫化反應用觸媒(促進本組合物之硬化之量)。
- 如請求項1之硬化性聚矽氧組合物,其中(A)成分包含以平均單元式:(R1R5 2SiO1/2)d(R5 2SiO2/2)e(R4SiO3/2)f(式中,R1及R4為與上述相同之基,R5為相同或不同之碳數1~12之烷基、碳數2~12之烯基、碳數6~20之芳基、或碳數7~20之芳烷基,d、e、及f分別為滿足0.01≦d≦0.5、0≦e≦0.7、0.1≦f<0.9、且d+e+f=1之數)表示,且一分子中具有至少2個烯基之有機聚矽氧烷樹脂。
- 如請求項1之硬化性聚矽氧組合物,其中(A)成分包含一分子中具有至少2個鍵結矽原子之烯基與至少1個鍵結矽原子之芳基的直 鏈狀之有機聚矽氧烷。
- 如請求項2之硬化性聚矽氧組合物,其中(A)成分包含一分子中具有至少2個鍵結矽原子之烯基與至少1個鍵結矽原子之芳基的直鏈狀之有機聚矽氧烷。
- 如請求項1至4中任一項之硬化性聚矽氧組合物,其中(C)成分中之R3為縮水甘油氧基烷基、環氧環己基烷基、或環氧烷基。
- 如請求項1至4中任一項之硬化性聚矽氧組合物,其進而含有(E)矽氫化反應抑制劑{相對於(A)成分~(D)成分之合計100質量份為0.01~3質量份}。
- 如請求項5之硬化性聚矽氧組合物,其進而含有(E)矽氫化反應抑制劑{相對於(A)成分~(D)成分之合計100質量份為0.01~3質量份}。
- 一種光半導體裝置,其係利用如請求項1至7中任一項之硬化性聚矽氧組合物之硬化物密封光半導體元件而成。
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