TW201527437A - 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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- TW201527437A TW201527437A TW103136057A TW103136057A TW201527437A TW 201527437 A TW201527437 A TW 201527437A TW 103136057 A TW103136057 A TW 103136057A TW 103136057 A TW103136057 A TW 103136057A TW 201527437 A TW201527437 A TW 201527437A
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- Prior art keywords
- tetrazole
- group
- component
- optical semiconductor
- compound
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- 239000000203 mixture Substances 0.000 title claims abstract description 94
- 230000003287 optical effect Effects 0.000 title claims abstract description 59
- 239000004065 semiconductor Substances 0.000 title claims abstract description 57
- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 11
- 125000003342 alkenyl group Chemical group 0.000 claims abstract description 31
- 150000001875 compounds Chemical class 0.000 claims abstract description 25
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 23
- 229910052709 silver Inorganic materials 0.000 claims abstract description 13
- 238000007789 sealing Methods 0.000 claims abstract description 5
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 5
- 239000007809 chemical reaction catalyst Substances 0.000 claims abstract description 4
- 150000003536 tetrazoles Chemical class 0.000 claims abstract 2
- -1 polyoxosiloxane Polymers 0.000 claims description 77
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 30
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical group [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 29
- 229910052707 ruthenium Inorganic materials 0.000 claims description 29
- 229910052782 aluminium Inorganic materials 0.000 claims description 19
- KJUGUADJHNHALS-UHFFFAOYSA-N 1H-tetrazole Chemical compound C=1N=NNN=1 KJUGUADJHNHALS-UHFFFAOYSA-N 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 18
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 claims description 17
- 125000000217 alkyl group Chemical group 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 13
- 239000011787 zinc oxide Substances 0.000 claims description 13
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- 229910004298 SiO 2 Inorganic materials 0.000 claims description 9
- 229910004283 SiO 4 Inorganic materials 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 150000002430 hydrocarbons Chemical group 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 238000005984 hydrogenation reaction Methods 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 229920002098 polyfluorene Polymers 0.000 claims description 6
- 229910052726 zirconium Inorganic materials 0.000 claims description 6
- GRWAIJBHBCCLGS-UHFFFAOYSA-N 2-(tetrazol-1-yl)acetic acid Chemical compound OC(=O)CN1C=NN=N1 GRWAIJBHBCCLGS-UHFFFAOYSA-N 0.000 claims description 5
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 5
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
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- 239000011667 zinc carbonate Substances 0.000 claims description 5
- 229910000010 zinc carbonate Inorganic materials 0.000 claims description 5
- 235000004416 zinc carbonate Nutrition 0.000 claims description 5
- IYPXPGSELZFFMI-UHFFFAOYSA-N 1-phenyltetrazole Chemical compound C1=NN=NN1C1=CC=CC=C1 IYPXPGSELZFFMI-UHFFFAOYSA-N 0.000 claims description 4
- JUNAPQMUUHSYOV-UHFFFAOYSA-N 2-(2h-tetrazol-5-yl)acetic acid Chemical compound OC(=O)CC=1N=NNN=1 JUNAPQMUUHSYOV-UHFFFAOYSA-N 0.000 claims description 4
- 150000001785 cerium compounds Chemical class 0.000 claims description 4
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- 150000002506 iron compounds Chemical class 0.000 claims description 4
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 4
- HWHNFJYQDMSYAF-UHFFFAOYSA-N 1,5-dimethyltetrazole Chemical compound CC1=NN=NN1C HWHNFJYQDMSYAF-UHFFFAOYSA-N 0.000 claims description 3
- FCERNNLMTCOKHX-UHFFFAOYSA-N 1,5-diphenyltetrazole Chemical compound C1=CC=CC=C1C1=NN=NN1C1=CC=CC=C1 FCERNNLMTCOKHX-UHFFFAOYSA-N 0.000 claims description 3
- KSUSTLKKFLDJNC-UHFFFAOYSA-N 1-butyltetrazole Chemical compound CCCCN1C=NN=N1 KSUSTLKKFLDJNC-UHFFFAOYSA-N 0.000 claims description 3
- HPZIIBYLAYWBSN-UHFFFAOYSA-N 1-ethyl-5-methyltetrazole Chemical compound CCN1N=NN=C1C HPZIIBYLAYWBSN-UHFFFAOYSA-N 0.000 claims description 3
- XBDIFKZMUYFXBN-UHFFFAOYSA-N 1-ethyl-5-phenyltetrazole Chemical compound CCN1N=NN=C1C1=CC=CC=C1 XBDIFKZMUYFXBN-UHFFFAOYSA-N 0.000 claims description 3
- PZDFYVBXRWSAON-UHFFFAOYSA-N 1-ethyltetrazole Chemical compound CCN1C=NN=N1 PZDFYVBXRWSAON-UHFFFAOYSA-N 0.000 claims description 3
- UIEGWLAONRMBOG-UHFFFAOYSA-N 1-methyl-5-phenyltetrazole Chemical compound CN1N=NN=C1C1=CC=CC=C1 UIEGWLAONRMBOG-UHFFFAOYSA-N 0.000 claims description 3
- OMAFFHIGWTVZOH-UHFFFAOYSA-N 1-methyltetrazole Chemical compound CN1C=NN=N1 OMAFFHIGWTVZOH-UHFFFAOYSA-N 0.000 claims description 3
- NMEFJGAOVRFDEQ-UHFFFAOYSA-N 1-pentyltetrazole Chemical compound CCCCCN1C=NN=N1 NMEFJGAOVRFDEQ-UHFFFAOYSA-N 0.000 claims description 3
- AHYVTIGFFGLKHA-UHFFFAOYSA-N 1-propyltetrazole Chemical compound CCCN1C=NN=N1 AHYVTIGFFGLKHA-UHFFFAOYSA-N 0.000 claims description 3
- ZYHXBGMQUWRUBE-UHFFFAOYSA-N 2-(tetrazol-2-yl)acetic acid Chemical compound OC(=O)CN1N=CN=N1 ZYHXBGMQUWRUBE-UHFFFAOYSA-N 0.000 claims description 3
- HHDRWGJJZGJSGZ-UHFFFAOYSA-N 5-benzyl-2h-tetrazole Chemical compound C=1C=CC=CC=1CC=1N=NNN=1 HHDRWGJJZGJSGZ-UHFFFAOYSA-N 0.000 claims description 3
- WYXQDGGJZMWJOX-UHFFFAOYSA-N 5-ethyl-1-methyltetrazole Chemical compound CCC1=NN=NN1C WYXQDGGJZMWJOX-UHFFFAOYSA-N 0.000 claims description 3
- KYRMPMCAOPMOIR-UHFFFAOYSA-N 5-ethyl-2h-tetrazole Chemical compound CCC=1N=NNN=1 KYRMPMCAOPMOIR-UHFFFAOYSA-N 0.000 claims description 3
- QYSASSWEUXOZEQ-UHFFFAOYSA-N 5-methyl-1-phenyltetrazole Chemical compound CC1=NN=NN1C1=CC=CC=C1 QYSASSWEUXOZEQ-UHFFFAOYSA-N 0.000 claims description 3
- XZGLNCKSNVGDNX-UHFFFAOYSA-N 5-methyl-2h-tetrazole Chemical compound CC=1N=NNN=1 XZGLNCKSNVGDNX-UHFFFAOYSA-N 0.000 claims description 3
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- 229910052718 tin Inorganic materials 0.000 claims description 2
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- 150000001335 aliphatic alkanes Chemical class 0.000 claims 1
- 150000001336 alkenes Chemical class 0.000 claims 1
- OJQZSXMWAZUCSH-UHFFFAOYSA-N ethyl acetate;2h-tetrazole Chemical compound C=1N=NNN=1.CCOC(C)=O OJQZSXMWAZUCSH-UHFFFAOYSA-N 0.000 claims 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims 1
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- 239000000758 substrate Substances 0.000 abstract description 12
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- 229910052717 sulfur Inorganic materials 0.000 abstract description 11
- 239000011593 sulfur Substances 0.000 abstract description 11
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- 238000006459 hydrosilylation reaction Methods 0.000 abstract 1
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- MFGZXPGKKJMZIY-UHFFFAOYSA-N ethyl 5-amino-1-(4-sulfamoylphenyl)pyrazole-4-carboxylate Chemical compound NC1=C(C(=O)OCC)C=NN1C1=CC=C(S(N)(=O)=O)C=C1 MFGZXPGKKJMZIY-UHFFFAOYSA-N 0.000 description 1
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- 239000011737 fluorine Substances 0.000 description 1
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- 125000005417 glycidoxyalkyl group Chemical group 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- NWVVVBRKAWDGAB-UHFFFAOYSA-N hydroquinone methyl ether Natural products COC1=CC=C(O)C=C1 NWVVVBRKAWDGAB-UHFFFAOYSA-N 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
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- 229940011051 isopropyl acetate Drugs 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- CNHDIAIOKMXOLK-UHFFFAOYSA-N monomethylhydroquinone Natural products CC1=CC(O)=CC=C1O CNHDIAIOKMXOLK-UHFFFAOYSA-N 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 125000004365 octenyl group Chemical group C(=CCCCCCC)* 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 125000000466 oxiranyl group Chemical group 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 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
- 229960005152 pentetrazol Drugs 0.000 description 1
- 125000004344 phenylpropyl group Chemical group 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229960005235 piperonyl butoxide Drugs 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000009719 polyimide resin Substances 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- XPGAWFIWCWKDDL-UHFFFAOYSA-N propan-1-olate;zirconium(4+) Chemical compound [Zr+4].CCC[O-].CCC[O-].CCC[O-].CCC[O-] XPGAWFIWCWKDDL-UHFFFAOYSA-N 0.000 description 1
- KVIKMJYUMZPZFU-UHFFFAOYSA-N propan-2-ol;titanium Chemical compound [Ti].CC(C)O.CC(C)O KVIKMJYUMZPZFU-UHFFFAOYSA-N 0.000 description 1
- ZGSOBQAJAUGRBK-UHFFFAOYSA-N propan-2-olate;zirconium(4+) Chemical compound [Zr+4].CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-] ZGSOBQAJAUGRBK-UHFFFAOYSA-N 0.000 description 1
- 125000002572 propoxy group Chemical group [*]OC([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical group [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 229910001427 strontium ion Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- LSZKGNJKKQYFLR-UHFFFAOYSA-J tri(butanoyloxy)stannyl butanoate Chemical compound [Sn+4].CCCC([O-])=O.CCCC([O-])=O.CCCC([O-])=O.CCCC([O-])=O LSZKGNJKKQYFLR-UHFFFAOYSA-J 0.000 description 1
- UAEJRRZPRZCUBE-UHFFFAOYSA-N trimethoxyalumane Chemical compound [Al+3].[O-]C.[O-]C.[O-]C UAEJRRZPRZCUBE-UHFFFAOYSA-N 0.000 description 1
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 description 1
- 125000005065 undecenyl group Chemical group C(=CCCCCCCCCC)* 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 125000005023 xylyl group Chemical group 0.000 description 1
- VNTDZUDTQCZFKN-UHFFFAOYSA-L zinc 2,2-dimethyloctanoate Chemical compound [Zn++].CCCCCCC(C)(C)C([O-])=O.CCCCCCC(C)(C)C([O-])=O VNTDZUDTQCZFKN-UHFFFAOYSA-L 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
- IFNXAMCERSVZCV-UHFFFAOYSA-L zinc;2-ethylhexanoate Chemical compound [Zn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O IFNXAMCERSVZCV-UHFFFAOYSA-L 0.000 description 1
- DVSILEVINNCNTQ-UHFFFAOYSA-L zinc;3-oxobutanoate Chemical compound [Zn+2].CC(=O)CC([O-])=O.CC(=O)CC([O-])=O DVSILEVINNCNTQ-UHFFFAOYSA-L 0.000 description 1
- 150000003755 zirconium compounds Chemical class 0.000 description 1
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Abstract
本發明係關於一種用於密封、被覆、或接著光半導體元件之矽氫化反應硬化性聚矽氧組合物,其係供形成可抑制因空氣中之含硫氣體所引起之光半導體裝置中之銀電極或鍍銀之基板之變色之硬化物,並且至少包含:(A)一分子中具有至少2個與矽原子鍵結之烯基的有機聚矽氧烷、(B)一分子中具有至少2個與矽原子鍵結之氫原子的有機氫化聚矽氧烷、(C)四唑系化合物、及(D)矽氫化反應用觸媒。又,本發明係關於一種光半導體元件經上述組合物之硬化物進行密封、被覆、或接著,且可抑制因空氣中之含硫氣體所引起之銀電極或鍍銀之基板之變色的光半導體裝置。
Description
本發明係關於一種硬化性聚矽氧組合物、及使用該組合物之光半導體裝置。
為了密封、被覆、或接著光半導體裝置中之光半導體元件,而使用會於矽氫化反應中發生硬化之硬化性聚矽氧組合物。作為此種硬化性聚矽氧組合物,日本專利特開2000-198930號公報中提出有包含如下成分之硬化性聚矽氧組合物:一分子中具有至少2個與矽原子鍵結之烯基之二有機聚矽氧烷、具有乙烯基之樹脂結構之有機聚矽氧烷、一分子中具有至少2個與矽原子鍵結之氫原子的有機氫化聚矽氧烷、及鉑族金屬系觸媒。
但是,此種硬化性聚矽氧組合物存在無法充分地抑制因空氣中之硫化氫等含硫氣體所引起之光半導體裝置中之銀電極或鍍銀之基板之變色的問題。
另一方面,日本專利特開平11-29709號公報中提出有為了對聚矽氧硬化物賦予阻燃性,而含有具有選自胺基、醯胺基、羰基、羧基、及硫醇基中之至少1種官能基之四唑化合物的硬化性聚矽氧組合物,作為其硬化機制,亦例示有矽氫化反應。
但是,日本專利特開平11-29709號公報中雖然記載有可將此種硬
化性聚矽氧組合物用於電氣、電子零件,但對光半導體元件之密封、被覆、或接著之用途並無提示。
專利文獻1:日本專利特開2000-198930號公報
專利文獻2:日本專利特開平11-29709號公報
本發明之目的在於提供一種硬化性聚矽氧組合物,其形成抑制因空氣中之含硫氣體所引起之光半導體裝置中之銀電極或鍍銀之基板之變色之硬化物。又,本發明之另一目的在於提供一種光半導體裝置,其抑制因空氣中之含硫氣體所引起之銀電極或鍍銀之基板之變色。
本發明之硬化性聚矽氧組合物之特徵在於:其係用於密封、被覆、或接著光半導體元件之矽氫化反應硬化性聚矽氧組合物,並且至少包含:(A)一分子中具有至少2個與矽原子鍵結之烯基的有機聚矽氧烷、(B)一分子中具有至少2個與矽原子鍵結之氫原子的有機氫化聚矽氧烷{相對於(A)成分中之與矽原子鍵結之烯基1莫耳,本成分中之與矽原子鍵結之氫原子成為0.1~10莫耳之量}、(C)四唑系化合物(相對於本組合物,以質量單位計成為1ppm~0.5%之量)、及(D)矽氫化反應用觸媒(促進本組合物之硬化之量)。
較佳為上述(A)成分為(A-1)通式:R1 3SiO(R1 2SiO)mSiR1 3
(式中,R1為相同或不同之一價烴基,其中,於一分子中,至少2個R1為烯基,m為5~1,000之整數)
所表示之直鏈狀之有機聚矽氧烷及/或(A-2)平均單元式:(R1SiO3/2)a(R1 2SiO2/2)b(R1 3SiO1/2)c(SiO4/2)d(XO1/2)e
(式中,R1與上述相同,其中,R1之合計之0.01~50莫耳%為烯基,X為氫原子或烷基,a、b、c、d、及e為滿足0≦a≦1.0、0≦b≦1.0、0≦c<0.9、0≦d<0.5、0≦e<0.4、且a+b+c+d=1.0之數)
所表示之支鏈狀之有機聚矽氧烷。
上述(C)成分較佳為選自由1H-四唑、1H-四唑-1-乙酸、1H-四唑-5-乙酸、1H-四唑-1-乙酸乙酯、1H-四唑-5-乙酸乙酯、1-甲基-1H-四唑、1-乙基-1H-四唑、1-丙基-1H-四唑、1-丁基-1H-四唑、1-戊基-1H-四唑、1-苯基-1H-四唑、1,5-二甲基-1H-四唑、1-乙基-5-甲基-1H-四唑、1-苯基-5-甲基-1H-四唑、1-甲基-5-乙基-1H-四唑、1-甲基-5-苯基-1H-四唑、1-乙基-5-苯基四唑、1,5-二苯基-1H-四唑、1,5-三亞甲基-1H-四唑、1,5-四亞甲基-1H-四唑、1,5-五亞甲基-1H-四唑、5-甲基-1H-四唑、5-乙基-1H-四唑、5-苯基-1H-四唑、5-苄基-1H-四唑、5-甲氧基-1H-四唑、及2H-四唑-2-乙酸所組成之群中之至少1種四唑系化合物。
本發明之光半導體裝置係以光半導體元件經上述硬化性聚矽氧組合物之硬化物進行密封、被覆、或接著為特徵,較佳為上述光半導體元件為發光二極體。
本發明之硬化性聚矽氧組合物具有如下特徵:形成抑制因空氣中之含硫氣體所引起之光半導體裝置中之銀電極或鍍銀之基板之變色之硬化物。又,本發明之光半導體裝置具有如下特徵:抑制因空氣中之含硫氣體所引起之銀電極或鍍銀之基板之變色。
1‧‧‧光半導體元件
2‧‧‧引線框架
3‧‧‧引線框架
4‧‧‧接合線
5‧‧‧反射材
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)的剖面圖。
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個與矽原子鍵結之烯基的有機聚矽氧烷。作為該烯基,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、十一烯基、十二烯基等碳數為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於矽原子上之基,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;該等基之氫原子之一部分或全部被取代為氟原子、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,於無損本發明之目的之範圍內,可具有少量之羥基或甲氧基、乙氧基等烷氧基。
作為(A)成分之分子結構,可例示:直鏈狀、一部分具有支鏈之直鏈狀、支鏈狀、環狀、及三維網狀結構。(A)成分亦可為具有該等分子結構之1種有機聚矽氧烷、或具有該等分子結構之2種以上有機聚矽氧烷之混合物。
此種(A)成分較佳為(A-1)通式:R1 3SiO(R1 2SiO)mSiR1 3
所表示之直鏈狀之有機聚矽氧烷及/或(A-2)平均單元式:(R1SiO3/2)a(R1 2SiO2/2)b(R1 3SiO1/2)c(SiO4/2)d(XO1/2)e
所表示之支鏈狀之有機聚矽氧烷。
於(A-1)成分中,式中,R1為相同或不同之一價烴基,可例示:與上述相同之烷基、烯基、芳基、芳烷基、及該等基之氫原子之一部分或全部被取代為氟原子、氯原子、溴原子等鹵素原子之基。其中,於一分子中,至少2個R1為烯基。又,式中,m為5~1,000之整數,較佳為50~1,000之整數或100~1,000之整數。
作為此種(A-1)成分,可例示:分子鏈兩末端經二甲基乙烯基矽烷氧基封端之二甲基聚矽氧烷、分子鏈兩末端經二甲基乙烯基矽烷氧基封端之二甲基矽氧烷-甲基乙烯基矽氧烷共聚物、分子鏈兩末端經二甲基乙烯基矽烷氧基封端之二甲基矽氧烷-甲基苯基矽氧烷共聚物、分子鏈兩末端經二甲基乙烯基矽烷氧基封端之甲基苯基聚矽氧烷、分子鏈兩末端經三甲基矽烷氧基封端之二甲基矽氧烷-甲基乙烯基矽氧烷共聚物、分子鏈兩末端經三甲基矽烷氧基封端之二甲基矽氧烷-甲基乙烯基矽氧烷-甲基苯基矽氧烷共聚物、及該等之2種以上之混合物。
又,於(A-2)成分中,式中,R1為相同或不同之一價烴基,可例示與上述相同之烷基、烯基、芳基、芳烷基、及該等基之氫原子之一部分或全部被取代為氟原子、氯原子、溴原子等鹵素原子之基。其中,較佳為R1之合計之0.01~50莫耳%、0.05~40莫耳%、或0.09~32莫耳%為烯基。其原因在於:若烯基之比例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,若烯基之比例為上述範圍之上限以下,則所獲得之硬化物之機械特性良好。再者,烯基之含量例如可藉由傅立葉變換紅外分光光度計(FT-IR,Fourier Transform-Infrared Radiation)、核磁共振(NMR,Nuclear Magnetic Resonance)、凝膠滲透層析法(GPC,Gel Permeation Chromatography)等分析而求出。
又,式中,X為氫原子或烷基。作為該烷基,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,較佳為碳數1~3之烷基。
又,式中,a係表示式:R1SiO3/2所表示之矽氧烷單元之比例、且滿足0≦a≦1.0之數,b係表示式:R1 2SiO2/2所表示之矽氧烷單元之比例、且滿足0≦b≦1.0之數,c係表示式:R1 3SiO1/2所表示之矽氧烷單元之比例、且滿足0≦c<0.9之數,d係表示式:SiO4/2所表示之矽氧烷單元之比例、且滿足0≦d<0.5之數。其中,式中,a+b+c+d=1.0。又,e係表示鍵結於矽原子上之羥基或烷氧基之比例、且滿足0≦e<0.4之數。
作為(A)成分,可使用(A-1)成分單獨、(A-2)成分單獨、或(A-1)成分與(A-2)成分之混合物。於使用(A-1)成分與(A-2)成分之混合物之情形時,由於所獲得之組合物之操作性良好,因此(A-2)成分之含量較佳為(A-1)成分與(A-2)成分之合計量之90質量%以下或60質量%以下。又,由於所獲得之硬化物之機械特性良好,因此(A-2)成分之含量較佳為(A-1)成分與(A-2)成分之合計量之至少10質量%。
(A)成分於25℃下為液狀或固體狀。於(A)成分於25℃下為液狀之情形時,其25℃之黏度較佳為1~1,000,000mPa‧s之範圍內或10~1,000,000mPa‧s之範圍內。再者,該黏度例如可藉由使用依據JIS K7117-1之B型黏度計之測定而求出。
(B)成分係作為本組合物之交聯劑之一分子中具有至少2個與矽原子鍵結的氫原子之有機氫化聚矽氧烷。作為(B)成分中之氫原子以外之鍵結於矽原子上之基,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;該等基之氫原子之一部分或全部被取代為氟原子、氯原子、溴原子等鹵素原子之基。再者,於(B)成分中之矽原子上,於無損本發明之目的之範圍內,可具有少量之羥基或甲氧基、乙氧基等烷氧基。
作為(B)成分之分子結構,可例示:直鏈狀、一部分具有支鏈之直鏈狀、支鏈狀、環狀、及三維網狀結構,較佳為一部分具有支鏈之直鏈狀、支鏈狀、或三維網狀結構。
(B)成分於25℃下為固體狀或液狀。於(B)成分於25℃下為液狀之情形時,其25℃之黏度較佳為10,000mPa‧s以下、0.1~5,000mPa‧s之範圍內、或0.5~1,000mPa‧s之範圍內。再者,該黏度例如可藉由使用依據JIS K7117-1之B型黏度計之測定而求出。
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、分子鏈兩末端經三甲基矽烷氧基封端之甲基氫化聚矽氧烷、分子鏈兩末端經三甲基矽烷氧基封端之二甲基矽氧烷-甲基氫矽氧烷共聚物、分子鏈兩末端經二甲基氫矽烷氧基封端之二甲基聚矽氧烷、分子鏈兩末端經二甲基氫矽烷氧基封端之二甲基矽氧烷-甲基氫矽氧烷共聚物、分子鏈兩末端經三甲基矽烷氧基封端之甲基氫矽氧烷-二苯基矽氧烷共聚物、分子鏈兩末端經三甲基矽烷氧基封端之甲基氫矽氧烷-二苯基矽氧烷-二甲基矽氧烷共聚物、包含(CH3)2HSiO1/2單元與SiO4/2單元之共聚物、包含(CH3)2HSiO1/2單元、SiO4/2單元及(C6H5)SiO3/2單元之共聚物、及該等之2種以上之混合物。
關於(B)成分之含量,相對於(A)成分中之與矽原子鍵結之烯基1
莫耳,為本成分中之與矽原子鍵結之氫原子成為0.1~10莫耳之量,較佳為成為0.5~5莫耳之量。其原因在於:若(B)成分之含量為上述範圍之上限以下,則所獲得之硬化物之機械特性良好,另一方面,若為上述範圍之下限以上,則所獲得之組合物之硬化性良好。再者,(B)成分中之與矽原子鍵結之氫原子之含量例如可藉由傅立葉變換紅外分光光度計(FT-IR)、核磁共振(NMR)、凝膠滲透層析法(GPC)等分析而求出。
(C)成分係用於對本組合物之硬化物賦予耐硫化性之四唑系化合物。作為(C)成分,由於更不易引起本組合物之硬化阻礙,因此較佳為不具有胺基或硫醇基等官能基之四唑系化合物,具體而言,可例示:1H-四唑、1H-四唑-1-乙酸、1H-四唑-5-乙酸、1H-四唑-1-乙酸乙酯、1H-四唑-5-乙酸乙酯、1-甲基-1H-四唑、1-乙基-1H-四唑、1-丙基-1H-四唑、1-丁基-1H-四唑、1-戊基-1H-四唑、1-苯基-1H-四唑、1,5-二甲基-1H-四唑、1-乙基-5-甲基-1H-四唑、1-苯基-5-甲基-1H-四唑、1-甲基-5-乙基-1H-四唑、1-甲基-5-苯基-1H-四唑、1-乙基-5-苯基四唑、1,5-二苯基-1H-四唑、1,5-三亞甲基-1H-四唑、1,5-四亞甲基-1H-四唑、1,5-五亞甲基-1H-四唑、5-甲基-1H-四唑、5-乙基-1H-四唑、5-苯基-1H-四唑、5-苄基-1H-四唑、5-甲氧基-1H-四唑、及2H-四唑-2-乙酸。作為(C)成分,亦可使用此種四唑系化合物之一種或者組合使用2種以上。
關於(C)成分之含量,係於本組合物中以質量單位計成為1ppm~0.5%之範圍內之量,較佳為成為5ppm~0.3%之範圍內或10ppm~0.1%之範圍內之量。其原因在於:若(C)之含量為上述範圍之下限以上,則可充分地賦予耐硫化性,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不會降低,又,所獲得之硬化物之物性不會降低。
(D)成分係用於促進本組合物之硬化之矽氫化反應用觸媒。作為(D)成分,可例示:鉑族元素觸媒、鉑族元素化合物觸媒,具體而言,可例示:鉑系觸媒、銠系觸媒、鈀系觸媒、及該等之至少2種之組合,尤其是由於可明顯促進本組合物之硬化,因此較佳為鉑系觸媒。作為該鉑系觸媒,可例示:鉑細粉末、鉑黑、氯鉑酸、氯鉑酸之醇改性物、氯鉑酸與二烯烴之錯合物、鉑-烯烴錯合物、二(乙醯乙酸)鉑、二(乙醯丙酮)鉑等鉑-羰基錯合物、氯鉑酸-二乙烯基四甲基二矽氧烷錯合物、氯鉑酸-四乙烯基四甲基環四矽氧烷錯合物等氯鉑酸-烯基矽氧烷錯合物、鉑-二乙烯基四甲基二矽氧烷錯合物、鉑-四乙烯基四甲基環四矽氧烷錯合物等鉑-烯基矽氧烷錯合物、氯鉑酸與乙炔醇類之錯合物、及該等之2種以上之混合物,尤其是由於可促進本組合物之硬化,因此較佳為鉑-烯基矽氧烷錯合物。
作為鉑-烯基矽氧烷錯合物中所使用之烯基矽氧烷,可例示:1,3-二乙烯基-1,1,3,3-四甲基二矽氧烷、1,3,5,7-四甲基-1,3,5,7-四乙烯基環四矽氧烷、該等烯基矽氧烷之甲基之一部分被取代為乙基、苯基等而成之烯基矽氧烷低聚物、及該等烯基矽氧烷之乙烯基被取代為烯丙基、己烯基等而成之烯基矽氧烷低聚物,尤其是由於所生成之鉑-烯基矽氧烷錯合物之穩定性良好,因此較佳為1,3-二乙烯基-1,1,3,3-四甲基二矽氧烷。
又,為了提高鉑-烯基矽氧烷錯合物之穩定性,較佳為將該等鉑-烯基矽氧烷錯合物溶解於1,3-二乙烯基-1,1,3,3-四甲基二矽氧烷、1,3-二烯丙基-1,1,3,3-四甲基二矽氧烷、1,3-二乙烯基-1,3-二甲基-1,3-二苯基二矽氧烷、1,3-二乙烯基-1,1,3,3-四苯基二矽氧烷、及1,3,5,7-四甲基-1,3,5,7-四乙烯基環四矽氧烷等烯基矽氧烷低聚物或二甲基矽氧烷低聚物等有機矽氧烷低聚物中,尤佳為溶解於烯基矽氧烷低聚物中。
(D)成分之含量係促進本組合物之硬化之量,具體而言,較佳為相對於本組合物,(D)成分中之觸媒金屬原子以質量單位計成為0.01~500ppm之範圍內之量、成為0.01~100ppm之範圍內之量、或成為0.1~50ppm之範圍內之量。其原因在於:若(D)成分之含量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,則可抑制所獲得之硬化物之著色。
於本組合物中,為了延長常溫下之使用壽命,提高保存穩定性,亦可含有(E)矽氫化反應抑制劑。作為(E)成分,可例示:1-乙炔基環己-1-醇、2-甲基-3-丁炔-2-醇、3,5-二甲基-1-己炔-3-醇、及2-苯基-3-丁炔-2-醇等炔醇;3-甲基-3-戊烯-1-炔、及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、及1,3,5,7-四甲基-1,3,5,7-四己烯基環四矽氧烷等甲基烯基矽氧烷低聚物;二甲基雙(3-甲基-1-丁炔-3-氧基)矽烷、及甲基乙烯基雙(3-甲基-1-丁炔-3-氧基)矽烷等炔氧基矽烷;及異氰尿酸三烯丙酯系化合物。
(E)成分之含量並無特別限定,相對於本組合物100質量份,較佳為0.0001~5質量份之範圍內或0.01~3質量份之範圍內。
於本組合物中,為了對所獲得之硬化物賦予進一步之耐硫化性,亦可含有(F)氧化鋅或碳酸鋅。作為(F)成分,較佳為選自由如下成分所組成之群中之質量平均粒徑為0.1nm~5μm之至少一種細粉末:利用選自由Al、Ag、Cu、Fe、Sb、Si、Sn、Ti、Zr、及稀土元素所組成之群中之至少1種元素之氧化物及/或氫氧化物進行表面被覆之氧化鋅細粉末、利用不具有烯基之有機矽化合物進行表面處理之氧化鋅細粉末、及碳酸鋅之水合物細粉末。再者,該質量平均粒徑可藉由雷射繞射、散射法等進行測定。本發明之「質量平均粒徑」係指測定粒度分佈而獲得之累積質量為50%時之粒徑(D50)。
於利用氧化物進行表面被覆之氧化鋅細粉末中,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、及該等氧化物之2種以上之混合物、進而,Al2O3‧nH2O、Fe2O3‧nH2O、Fe3O4‧nH2O、Sb2O3‧nH2O、SiO2‧nH2O、TiO2‧nH2O、ZrO2‧nH2O、CeO2‧nH2O等氧化物之水合物,較佳為Al2O3、SiO2。再者,n通常為正整數,但根據脫水之程度,n未必取整數。
於利用氫氧化物進行表面被覆之氧化鋅細粉末中,作為稀土元素,可例示:釔、鈰、銪。作為氧化鋅細粉末之表面之氫氧化物,可例示:Al(OH)3、Cu(OH)2、Fe(OH)3、Ti(OH)4、Zr(OH)3、Y(OH)3、Ce(OH)3、Ce(OH)4、及該等氧化物之2種以上之混合物、進而,Ce(OH)3‧nH2O等氧化物之水合物,較佳為Al(OH)3。再者,n通常為正整數,但根據脫水之程度,n未必取整數。
再者,利用上述氧化物進行表面被覆之氧化鋅可進而利用上述氫氧化物進行表面被覆,又,亦可進而利用上述其他氧化物進行表面被覆。又,利用上述氫氧化物進行表面被覆之氧化鋅可進而利用上述氧化物進行表面被覆,又,亦可進而利用上述其他氫氧化物進行表面被覆。又,(F)成分亦可為利用上述氧化物與上述氫氧化物進行表面被覆之氧化鋅。例如,作為氧化物與氫氧化物之組合,可例示:Al2O3與Al(OH)3之組合、SiO2與Al(OH)3之組合。
於利用有機矽化合物進行表面處理之氧化鋅細粉末中,該有機矽化合物係不具有烯基者,可例示:有機矽烷、有機矽氮烷、聚甲基矽氧烷、有機氫化聚矽氧烷、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、之有機三烷氧基矽烷;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、有機氫化聚矽氧烷、具有矽烷醇基或者烷氧基之有機矽氧烷低聚物、包含R8SiO3/2單元(式中,R8為甲基、乙基、丙基等烷基;苯基等芳基中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,亦可對上述氧化鋅細粉末進行進一步之表面處理。例如可列舉:硬脂酸等高級脂肪酸或其金屬皂、棕櫚酸辛酯等高級脂肪酸酯、三羥甲基乙烷、三羥甲基丙烷、季戊四醇等多元醇類、二乙醇胺、三乙醇胺等胺化合物。進而,亦可使用鈦酸烷基酯、鋁酸烷基酯、鋯酸烷基酯等偶合劑、或全氟烷基矽烷、全氟烷基磷酸酯等氟系有機化合物。
碳酸鋅之水合物細粉末係於碳酸鋅上結合有水之化合物,較佳為於105℃、3小時之加熱條件下之質量減少率為0.1質量%以上者。
關於(F)成分之含量,相對於本組合物,以質量單位計較佳為0.0001~10%之範圍內之量或0.0001~5%之範圍內之量。其原因在於:若(F)成分之含量為上述範圍之下限以上,則充分地抑制因含硫氣體引起之光半導體裝置中之銀電極或鍍銀之基板之變色,另一方面,若為上述範圍之上限以下,則無損所獲得之組合物之流動性。
於本組合物中,為了對所獲得之硬化物賦予耐剝離性,亦可含有(G)金屬系縮合反應觸媒。作為(G)成分,可例示:有機鋁化合物、有機鈦化合物、有機鋯化合物、有機鎂化合物、有機鋅化合物、有機銅化合物、有機鎳化合物、有機鉻化合物、有機鈷化合物、有機鐵化合物、有機銦化合物、有機鑭化合物、有機錫化合物、有機鉿化合
物、及該等之2種以上之混合物。
作為有機鋁化合物,可例示:三甲氧基鋁、三乙氧基鋁、異丙氧基鋁、異丙氧基二乙氧基鋁、三丁氧基鋁等烷氧基化合物;三乙醯氧基鋁、三硬脂酸鋁、三丁酸鋁等醯氧基化合物;異丙醇鋁、第二丁醇鋁、第三丁醇鋁、三(乙醯乙酸乙酯)鋁、三(六氟乙醯丙酮)鋁、三(乙醯乙酸乙酯)鋁、三(乙醯乙酸正丙酯)鋁、三(乙醯乙酸異丙酯)鋁、三(乙醯乙酸正丁酯)鋁、三水楊醛鋁、三(2-乙氧基羰基酚基)鋁、三(乙醯丙酮)鋁等螯合化合物。
作為有機鈦化合物,可例示:四乙氧基鈦、四異丙氧基鈦、四丁氧基鈦等四烷氧基鈦;四乙二醇鈦酸酯、二正丁基雙(三乙醇胺)鈦酸酯、二(乙醯丙酮)酸二異丙氧基鈦、辛酸異丙氧基鈦、三甲基丙烯酸異丙基鈦、三丙烯酸異丙基鈦、異丙基三異硬脂醯基鈦酸酯、異丙基三(癸基苯磺醯基)鈦酸酯、異丙基三(丁基/甲基焦磷醯基)鈦酸酯、四異丙基二(二月桂基亞磷醯基)鈦酸酯、二甲基丙烯醯基羥乙酸鈦酸酯、二丙烯醯基羥乙酸鈦酸酯、二(二辛基磷醯基)伸乙基鈦酸酯、三(二辛基磷醯氧基)異丙氧基鈦、異丙基三(二辛基焦磷醯基)鈦酸酯、四異丙基雙(二辛基亞磷醯基)鈦酸酯、四辛基雙(二-十三烷基亞磷醯基)鈦酸酯、四(2,2-二烯丙基氧基甲基-1-丁基)雙(二-十三烷基)亞磷醯基鈦酸酯、雙(二辛基焦磷醯基)羥乙酸鈦酸酯、三(二辛基焦磷醯基)伸乙基鈦酸酯、異丙基三(正十二烷基苯磺醯基)鈦酸酯、異丙基三辛醯基鈦酸酯、異丙基二甲基丙烯醯基異硬脂醯基鈦酸酯、異丙基異硬脂醯基二丙烯醯基鈦酸酯、異丙基三(二辛基磷醯基)鈦酸酯、異丙基三(異丙苯基苯基)鈦酸酯、異丙基三(N-胺基乙基-胺基乙基)鈦酸酯。
作為有機鋯化合物,可例示:正丙醇鋯、正丁醇鋯、第三丁醇鋯、異丙醇鋯、乙醇鋯、乙酸氧鋯、乙醯丙酮鋯、丁氧基乙醯丙酮鋯、雙乙醯丙酮鋯、乙醯乙酸乙酯鋯、乙醯丙酮雙乙醯乙酸乙酯鋯、
六氟乙醯丙酮鋯、三氟乙醯丙酮鋯。
作為有機鎂化合物,可例示:乙醯乙酸乙酯鎂單異丙酯、二(乙醯乙酸乙酯)鎂、乙醯乙酸烷基酯鎂單異丙酯、二(乙醯丙酮)鎂。
作為有機鋅化合物,可例示:二(乙醯乙酸乙酯)鋅、乙醯丙酮鋅、二(2-乙基己酸)鋅、(甲基)丙烯酸鋅、新癸酸鋅、乙酸鋅、辛酸鋅、水楊酸鋅。
作為有機銅化合物,可例示:二(乙醯乙酸乙酯)銅、二(乙醯丙酮)銅。
作為有機鎳化合物,可例示:二(乙醯乙酸乙酯)鎳、二(乙醯丙酮)鎳。
作為有機鉻化合物,可例示:三(乙醯乙酸乙酯)鉻、三(乙醯丙酮)鉻。
作為有機鈷化合物,可例示:三(乙醯乙酸乙酯)鈷、三(乙醯丙酮)鈷。
作為有機鐵化合物,可例示:三(乙醯乙酸乙酯)鐵、三(乙醯丙酮)鐵。
作為有機銦化合物,可例示:三(乙醯乙酸乙酯)銦、三(乙醯丙酮)銦。
作為有機鑭化合物,可例示:三(乙醯乙酸乙酯)鑭、三(乙醯丙酮)鑭。
作為有機錫化合物,可例示:四(乙醯乙酸乙酯)錫、四(乙醯丙酮)錫。
作為有機鉿化合物,可例示:正丁醇鉿、第三丁醇鉿、乙醇鉿、異丙醇給、異丙醇鉿單異丙酯、乙醯丙酮鉿、四(二甲基胺基)鉿。
(G)成分尤佳為選自由有機鋁化合物、有機鈦化合物、有機鋯化
合物、有機鋅化合物、及有機鐵化合物所組成之群中之至少1種之金屬系縮合反應觸媒。
關於(G)成分之含量,較佳為相對於本組合物,以質量單位計成為20ppm~0.1%之範圍內之量、成為30ppm~0.05%之範圍內之量、或成為50ppm~0.03%之範圍內之量。其原因在於:若(G)成分之含量為上述範圍之下限以上,則可充分地抑制對吸濕回焊之剝離,另一方面,若為上述範圍之上限以下,則所獲得之組合物之保存穩定性提高。
又,於本組合物中,為了進一步提高對在硬化中所接觸之基材之接著性,亦可含有接著促進劑。作為該接著促進劑,較佳為一分子中具有1個以上鍵結於矽原子上之烷氧基之有機矽化合物。作為該烷氧基,可例示:甲氧基、乙氧基、丙氧基、丁氧基、及甲氧基乙氧基等,尤佳為甲氧基或乙氧基。又,作為該有機矽化合物之鍵結於矽原子上之烷氧基以外之基,可例示:烷基、烯基、芳基、芳烷基、及鹵化烷基等與上述相同之經鹵素取代或者未經取代之一價烴基;3-縮水甘油氧基丙基、及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、及3-(3,4-環氧環己基)丙基等環氧環己基烷基;4-環氧乙烷基丁基、及8-環氧乙烷基辛基等環氧乙烷基烷基;3-甲基丙烯醯氧基丙基等含丙烯醯基之一價有機基;異氰酸酯基;異氰尿酸酯基;以及氫原子。該有機矽化合物較佳為具有可與本組合物中之脂肪族不飽和烴基或與矽原子鍵結之氫原子進行反應之基,具體而言,較佳為具有與矽原子鍵結之脂肪族不飽和烴基或與矽原子鍵結之氫原子。
接著促進劑之含量並無特別限定,相對於本組合物100質量份較佳為0.01~10質量份之範圍內或0.1~3質量份之範圍內。
又,於本組合物中,亦可含有螢光體作為其他任意成分。作為
該螢光體,可例示:發光二極體(LED)中所廣泛利用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、酸硫化物系螢光體等之黃色、紅色、綠色、藍色發光螢光體、及該等之至少2種之混合物。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系綠色發色螢光體。作為酸硫化物系螢光體,可例示包含銪離子之Y2O2S系紅色發光螢光體。
該螢光體之含量並無特別限定,於本組合物中,較佳為0.1~70質量%之範圍內或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,則亦可含有自二氧化矽、玻璃、及氧化鋁等中選擇之1種以上無機質填充劑;聚矽氧橡膠粉末;聚矽氧樹脂、及聚甲基丙烯酸酯樹脂等樹脂粉末;自耐熱劑、染料、顏料、阻燃性賦予劑、界面活性劑、溶劑等中選擇之1種以上之成分作為其他任意成分。
本組合物藉由室溫放置、或加熱而進行硬化,但為了使之迅速地硬化,較佳為進行加熱。加熱溫度較佳為50~200℃之範圍內。
本組合物較佳為進行硬化而形成JIS K 6253中所規定之A型硬度計硬度為15~99或30~95之硬化物。其原因在於:若硬化性聚矽氧組合物之硬化物之硬度為上述範圍之下限以上,則具有強度,於將其用作光半導體元件之密封材或被覆材之情形時之保護性優異,另一方面,若為上述範圍之上限以下,則硬化物變得柔軟、耐久性優異。
繼而,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:光半導體元件經上述組合物之硬化物進行密封、被覆、或接著。作為該光半導體元件,可例示:發光二極體(LED)、半導體雷射、光電二極體、光電晶體、固體攝像、光電耦合器用發光體與光接收體,尤佳為發光二極體(LED)。
發光二極體(LED)由於係自光半導體元件之上下左右產生發光,因此構成發光二極體(LED)之零件中,吸收光者欠佳,較佳為光透過率較高、或反射率較高之材料。因此,搭載有光半導體元件之基板亦較佳為光透過率較高、或反射率較高之材料。作為此種搭載有光半導體元件之基板,例如可例示:銀、金、及銅等導電性金屬;鋁、及鎳等非導電性之金屬;PPA(Polyphthalamide,聚鄰苯二甲醯胺)、及LCP(Liquid Crystal Polymer,液晶聚合物)等混合有白色顏料之熱塑性樹脂;環氧樹脂、BT(Bismaleimide Triazine,雙馬來醯亞胺三)樹脂、聚醯亞胺樹脂、及聚矽氧樹脂等含有白色顏料之熱硬化性樹脂;氧化鋁、及氮化氧化鋁等陶瓷。由於硬化性聚矽氧組合物對光半導體元件及基板耐熱衝擊性良好,因此所獲得之光半導體裝置可顯示良好之可靠性。
將作為本發明之光半導體裝置之一例的表面安裝型LED之剖面圖示於圖1。圖1所示之LED中,光半導體元件1係晶片接合於引線框架2上,該光半導體元件1與引線框架3藉由接合線4而進行線結合。於該光半導體元件1之周圍,形成光反射材5,該光反射材5之內側之光半導體元件1係經上述硬化性聚矽氧組合物之硬化物6密封。
作為製造圖1所示之表面安裝型LED之方法,可例示如下方法:將光半導體元件1晶片接合於光反射材5之內側之引線框架2上,藉由金製之接合線4而將該光半導體元件1與引線框架3線接合,繼而,利用上述硬化性聚矽氧組合物樹脂密封光半導體元件1。
藉由實施例及比較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,硬化性聚矽氧組合物之硬化物之硬度係以如下方式進行測定。
將硬化性聚矽氧組合物於150℃下以5MPa之壓力加壓成形5分鐘,藉此製作片狀之硬化物。藉由JIS K 6253中所規定之A型硬度計測定該片狀之硬化物之硬度。
又,使用硬化性聚矽氧組合物,於150℃下加熱5分鐘,藉此製作圖1所示之光半導體裝置。藉由該光半導體裝置之輻射束之測定,以如下方式進行測定耐硫化性、及硬化性聚矽氧組合物對該光半導體裝置之耐剝離性。
對光半導體裝置,使用利用積分球之總輻射束測定裝置而進行初始輻射束測定,並算出初始之光提取效率(%)。繼而,對該光半導體裝置,將硫化鈉六水合物放入至高壓釜中,加熱至50℃,放置2小時。其後,使用利用積分球之總輻射束測定裝置而進行輻射束測定,算出2小時後之光提取效率(%)。
對20個光半導體裝置,利用光學顯微鏡觀察引線框架或線結合與該組合物之加熱硬化物間之剝離狀態,將剝離之比例(剝離之個數/20個)設為剝離率。
將20個上述光半導體裝置於85℃/85%RH烘箱中保管168小時,於280℃之烘箱內放置30秒鐘後,恢復至室溫(25℃)下,利用光學顯微鏡觀察引線框架或線結合與該組合物之加熱硬化物間之剝離狀態,
將剝離之比例(剝離之個數/20個)設為剝離率。
以表1所示之組成(質量份)均勻地混合以下之成分,而製備實施例1~8及比較例1~6之硬化性聚矽氧組合物。再者,式中,Vi表示乙烯基,Me表示甲基。又,於表1及表2中,SiH/Vi表示於硬化性聚矽氧組合物中,(B)成分中之與矽原子鍵結之氫原子相對於(A)成分中之乙烯基的合計1莫耳之合計莫耳數。
使用以下之成分作為(A)成分。再者,黏度係於25℃下之值,且依據JIS K 7117-1使用B型黏度計而進行測定。
(a-1-1)成分:黏度為300mPa‧s,平均式:Me2ViSiO(Me2SiO)150SiMe2Vi
所表示之分子鏈兩末端經二甲基乙烯基矽烷氧基封端之二甲基聚矽氧烷(乙烯基之含量=0.48質量%)
(a-1-2)成分:黏度為10,000mPa‧s,平均式:Me2ViSiO(Me2SiO)500SiMe2Vi
所表示之分子鏈兩末端經二甲基乙烯基矽烷氧基封端之二甲基聚矽氧烷(乙烯基之含量=0.15質量%)
(a-2-1)成分:於25℃下為白色固體狀,且為甲苯可溶性之平均單元式:(Me2ViSiO1/2)0.15(Me3SiO1/2)0.38(SiO4/2)0.47(HO1/2)0.01
所表示之一分子中具有2個以上乙烯基之有機聚矽氧烷(乙烯基之含量=5.5質量%;9.4莫耳%)
(a-2-2)成分:於25℃下為白色固體狀,且為甲苯可溶性之平均單元式:(Me2ViSiO1/2)0.13(Me3SiO1/2)0.45(SiO4/2)0.42(HO1/2)0.01
所表示之一分子中具有2個以上乙烯基之有機聚矽氧烷(乙烯基之
含量=4.7質量%;7.5莫耳%)
使用以下之成分作為(B)成分。再者,黏度係於25℃下之值,且依據JIS K7117-1使用B型黏度計而進行測定。
(b-1)成分:平均式:Me3SiO(MeHSiO)55SiMe3
所表示之黏度20mPa‧s之分子鏈兩末端經三甲基矽烷氧基封端之聚甲基氫矽氧烷(與矽原子鍵結之氫原子含量=1.6質量%)
(b-2)成分:平均式:Me3SiO(MeHSiO)15SiMe3
所表示之黏度5mPa‧s之分子鏈兩末端經三甲基矽烷氧基封端之二甲基矽氧烷-甲基氫矽氧烷共聚物(與矽原子鍵結之氫原子之含量=1.42質量%)
使用以下之成分作為(C)成分。
(c-1)成分:1H-四唑-1-乙酸
(c-2)成分:1H-四唑-5-乙酸
(c-3)成分:1,5-五亞甲基四唑
(c-4)成分:1H-四唑
(c-5)成分:苯并咪唑
(c-6)成分:2-巰基苯并噻唑
使用鉑之1,3-二乙烯基四甲基二矽氧烷錯合物之1,3-二乙烯基四甲基二矽氧烷溶液(鉑金屬之含量=約6000ppm)作為(D)成分。
使用1-乙炔基環己-1-醇作為(E)成分。
使用質量平均粒徑為0.5μm,且對利用SiO2進行表面被覆之氧化鋅粉末,進而藉由黏度20mPa‧s之分子鏈兩末端經三甲基矽烷氧基封端之二甲基矽氧烷-甲基氫矽氧烷共聚物進行表面處理之氧化鋅細粉末作為(F)成分。
使用乙醯烷氧基二異丙醇鋁作為(G)成分。
由表1顯示,實施例1~8之硬化性聚矽氧組合物之硬化物具有較高之耐硫化性。
本發明之硬化性聚矽氧組合物作為發光二極體(LED)、半導體雷射、光電二極體、光電晶體、固體攝像、光電耦合器用發光體與光接收體等光半導體元件之密封劑或接著劑有用。又,本發明之光半導體裝置作為光學裝置、光學設備、照明設備、照明裝置等光半導體裝置有用。
Claims (12)
- 一種硬化性聚矽氧組合物,其係用於密封、被覆、或接著光半導體元件之矽氫化反應硬化性聚矽氧組合物,並且至少包含:(A)一分子中具有至少2個與矽原子鍵結之烯基的有機聚矽氧烷、(B)一分子中具有至少2個與矽原子鍵結之氫原子的有機氫化聚矽氧烷{相對於(A)成分中之與矽原子鍵結之烯基1莫耳,本成分中之與矽原子鍵結之氫原子成為0.1~10莫耳之量}、(C)四唑系化合物(相對於本組合物,以質量單位計成為1ppm~0.5%之量)、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)成分為(A-1)通式:R1 3SiO(R1 2SiO)mSiR1 3(式中,R1為相同或不同之一價烴基,其中,於一分子中,至少2個R1為烯基,m為5~1,000之整數)所表示之直鏈狀之有機聚矽氧烷及/或(A-2)平均單元式:(R1SiO3/2)a(R1 2SiO2/2)b(R1 3SiO1/2)c(SiO4/2)d(XO1/2)e(式中,R1與上述相同,其中,R1之合計之0.01~50莫耳%為烯基,X為氫原子或烷基,a、b、c、d、及e為滿足0≦a≦1.0、0≦b≦1.0、0≦c<0.9、0≦d<0.5、0≦e<0.4、且a+b+c+d=1.0之數)所表示之支鏈狀之有機聚矽氧烷。
- 如請求項1或2之硬化性聚矽氧組合物,其中(C)成分係選自由1H-四唑、1H-四唑-1-乙酸、1H-四唑-5-乙酸、1H-四唑-1-乙酸乙酯、1H-四唑-5-乙酸乙酯、1-甲基-1H-四唑、1-乙基-1H-四唑、 1-丙基-1H-四唑、1-丁基-1H-四唑、1-戊基-1H-四唑、1-苯基-1H-四唑、1,5-二甲基-1H-四唑、1-乙基-5-甲基-1H-四唑、1-苯基-5-甲基-1H-四唑、1-甲基-5-乙基-1H-四唑、1-甲基-5-苯基-1H-四唑、1-乙基-5-苯基四唑、1,5-二苯基-1H-四唑、1,5-三亞甲基-1H-四唑、1,5-四亞甲基-1H-四唑、1,5-五亞甲基-1H-四唑、5-甲基-1H-四唑、5-乙基-1H-四唑、5-苯基-1H-四唑、5-苄基-1H-四唑、5-甲氧基-1H-四唑、及2H-四唑-2-乙酸所組成之群中之至少1種四唑系化合物。
- 如請求項1至3中任一項之硬化性聚矽氧組合物,其相對於(A)成分~(D)成分之合計100質量份,進而含有(E)矽氫化反應抑制劑0.0001~5質量份。
- 如請求項1至4中任一項之硬化性聚矽氧組合物,其相對於(A)成分~(D)成分之合計100質量份,進而含有(F)氧化鋅或碳酸鋅0.0001~10質量份。
- 如請求項5之硬化性聚矽氧組合物,其中(F)成分係選自由如下成分所組成之群中之質量平均粒徑為0.1nm~5μm之至少一種細粉末:利用選自由Al、Ag、Cu、Fe、Sb、Si、Sn、Ti、Zr、及稀土元素所組成之群中之至少1種元素之氧化物及/或氫氧化物作表面被覆之氧化鋅細粉末、利用不具有烯基之有機矽化合物作表面處理之氧化鋅細粉末、及碳酸鋅之水合物細粉末。
- 如請求項6之硬化性聚矽氧組合物,其中(F)成分係利用選自由有機矽烷、有機矽氮烷、有機矽氧烷低聚物、聚甲基矽氧烷、有機氫化聚矽氧烷所組成之群中之至少1種不具有烯基之有機矽化合物作表面處理之氧化鋅細粉末。
- 如請求項5或6之硬化性聚矽氧組合物,其中(F)成分係於105℃、3小時之加熱下之質量減少率為0.1質量%以上的碳酸鋅之水合物 細粉末。
- 如請求項1至8中任一項之硬化性聚矽氧組合物,其相對於(A)成分~(D)成分之合計100質量份,進而含有(G)金屬系縮合反應觸媒0.002~0.1質量份。
- 如請求項9之硬化性聚矽氧組合物,其中(G)成分係選自由有機鋁化合物、有機鈦化合物、有機鋯化合物、有機鋅化合物、及有機鐵化合物所組成之群中之至少1種有機金屬化合物。
- 一種光半導體裝置,其光半導體元件係經如請求項1至10中任一項之硬化性聚矽氧組合物之硬化物密封、被覆、或接著。
- 如請求項11之光半導體裝置,其中光半導體元件為發光二極體。
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CN106317894B (zh) * | 2015-06-30 | 2019-03-29 | 比亚迪股份有限公司 | 有机硅组合物、反光涂层及其制备方法与包括其的光伏组件 |
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US11495776B2 (en) * | 2018-04-16 | 2022-11-08 | Shin-Etsu Chemical Co., Ltd. | Transparent desiccant for organic EL, and method for using same |
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