TWI638011B - 可固化的聚矽氧組合物、其固化產品及光學半導體裝置 - Google Patents
可固化的聚矽氧組合物、其固化產品及光學半導體裝置 Download PDFInfo
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- TWI638011B TWI638011B TW103130019A TW103130019A TWI638011B TW I638011 B TWI638011 B TW I638011B TW 103130019 A TW103130019 A TW 103130019A TW 103130019 A TW103130019 A TW 103130019A TW I638011 B TWI638011 B TW I638011B
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- silicon
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- FDTBETCIPGWBHK-UHFFFAOYSA-N hydroxy-dimethyl-phenylsilane Chemical compound C[Si](C)(O)C1=CC=CC=C1 FDTBETCIPGWBHK-UHFFFAOYSA-N 0.000 description 1
- MPGPMDYRORRRGX-UHFFFAOYSA-N hydroxy-methyl-(2-phenylethenyl)silane Chemical compound C[SiH](O)C=CC1=CC=CC=C1 MPGPMDYRORRRGX-UHFFFAOYSA-N 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 150000007529 inorganic bases Chemical class 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical group OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 1
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- REQXNMOSXYEQLM-UHFFFAOYSA-N methoxy-dimethyl-phenylsilane Chemical compound CO[Si](C)(C)C1=CC=CC=C1 REQXNMOSXYEQLM-UHFFFAOYSA-N 0.000 description 1
- ICXMRHWTMJKRGK-UHFFFAOYSA-N methoxy-methyl-(2-phenylethenyl)silane Chemical compound C[SiH](C=CC1=CC=CC=C1)OC ICXMRHWTMJKRGK-UHFFFAOYSA-N 0.000 description 1
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- 229910052763 palladium Inorganic materials 0.000 description 1
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- 238000004382 potting Methods 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- 239000005053 propyltrichlorosilane Substances 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 230000009257 reactivity 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
- 239000000565 sealant Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- XFTDXEGRBTYXQE-UHFFFAOYSA-N silyl 3-ethenylpent-4-enoate Chemical compound C(=C)C(C=C)CC(=O)O[SiH3] XFTDXEGRBTYXQE-UHFFFAOYSA-N 0.000 description 1
- SJUYHBCRXPVODY-UHFFFAOYSA-N silyl 4-ethylhex-3-enoate Chemical compound C(C)C(=CCC(=O)O[SiH3])CC SJUYHBCRXPVODY-UHFFFAOYSA-N 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- GBXOGFTVYQSOID-UHFFFAOYSA-N trichloro(2-methylpropyl)silane Chemical compound CC(C)C[Si](Cl)(Cl)Cl GBXOGFTVYQSOID-UHFFFAOYSA-N 0.000 description 1
- ZOYFEXPFPVDYIS-UHFFFAOYSA-N trichloro(ethyl)silane Chemical compound CC[Si](Cl)(Cl)Cl ZOYFEXPFPVDYIS-UHFFFAOYSA-N 0.000 description 1
- ORVMIVQULIKXCP-UHFFFAOYSA-N trichloro(phenyl)silane Chemical compound Cl[Si](Cl)(Cl)C1=CC=CC=C1 ORVMIVQULIKXCP-UHFFFAOYSA-N 0.000 description 1
- DOEHJNBEOVLHGL-UHFFFAOYSA-N trichloro(propyl)silane Chemical compound CCC[Si](Cl)(Cl)Cl DOEHJNBEOVLHGL-UHFFFAOYSA-N 0.000 description 1
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 1
- BZBWDJAWLLVYOI-UHFFFAOYSA-N trihydroxy(2-methylpropyl)silane Chemical compound CC(C)C[Si](O)(O)O BZBWDJAWLLVYOI-UHFFFAOYSA-N 0.000 description 1
- FCVNATXRSJMIDT-UHFFFAOYSA-N trihydroxy(phenyl)silane Chemical compound O[Si](O)(O)C1=CC=CC=C1 FCVNATXRSJMIDT-UHFFFAOYSA-N 0.000 description 1
- XYJRNCYWTVGEEG-UHFFFAOYSA-N trimethoxy(2-methylpropyl)silane Chemical compound CO[Si](OC)(OC)CC(C)C XYJRNCYWTVGEEG-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
- AAPLIUHOKVUFCC-UHFFFAOYSA-N trimethylsilanol Chemical compound C[Si](C)(C)O AAPLIUHOKVUFCC-UHFFFAOYSA-N 0.000 description 1
- ZQTYRTSKQFQYPQ-UHFFFAOYSA-N trisiloxane Chemical compound [SiH3]O[SiH2]O[SiH3] ZQTYRTSKQFQYPQ-UHFFFAOYSA-N 0.000 description 1
- 125000005065 undecenyl group Chemical group C(=CCCCCCCCCC)* 0.000 description 1
- 239000004636 vulcanized rubber Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
本發明係關於可固化聚矽氧組合物,其包括:(A)由以下平均單元式表示之有機聚矽氧烷:(R1 3SiO1/2)a(R1 2SiO2/2)b(R2SiO3/2)c(R3SiO3/2)d,其中,R1係相同或不同的具有1至12個碳之烷基、具有2至12個碳之烯基、具有6至20個碳之芳基或具有7至20個碳之芳烷基,限制條件係分子中之至少兩個R1為該等烯基;R2係具有6至20個碳之芳基或具有7至20個碳之芳烷基;R3係具有1至12個碳之烷基;且a、b、c及d分別係滿足以下條件之數值:0.01 a 0.5,0 b 0.7,0.01 c<0.7,0.1 d<0.9,且a+b+c+d=1;(B)分子中具有至少兩個矽鍵結烯基及至少一個矽鍵結芳基之直鏈有機聚矽氧烷;(C)分子中具有至少兩個矽鍵結氫原子之有機聚矽氧烷;(D)矽氫化反應觸媒。該可固化聚矽氧組合物具有極佳處置/可加工性,且在固化時形成具有高折射率及低透氣度之固化產品。
Description
本發明係關於可固化聚矽氧組合物、藉由固化該組合物形成之固化產品及使用該組合物製造之光學半導體裝置。
本發明主張於2013年8月29日提出申請之美國臨時專利申請案第61/871,358號及於2014年2月5日提出申請之美國臨時專利申請案第61/936,008號的優先權,該等申請案之內容以引用方式併入本文中。
可固化聚矽氧組合物用作光學半導體裝置(例如發光二極體(LED)或諸如此類)中之光學半導體元件之密封材料或保護性塗層材料。已提出包括以下各項之可固化聚矽氧組合物作為此一可固化聚矽氧組合物:分子中具有至少兩個矽鍵結烯基及至少一個矽鍵結芳基之直鏈有機聚矽氧烷;分子中具有至少一個矽鍵結烯基、至少一個矽鍵結芳基及由式:C6H5SiO3/2表示之矽氧烷單元的有機聚矽氧烷;分子中具有至少兩個矽鍵結氫原子之有機聚矽氧烷;及矽氫化反應觸媒(參見專利文件1)。
然而,此一可固化聚矽氧組合物之問題在於,儘管可獲得具有高折射率之固化產品,但固化產品之伸長率較低。由於固化產品展現高透氣度,故在將此一固化產品用於展現高光強度且產生大量熱之高亮度LED時,因腐蝕性氣體腐蝕電鍍在LED基板上之銀而出現諸如密
封材料變色及亮度減弱等問題。
專利文件1:日本未審查專利申請公開案第2004-143361號
本發明之目標係提供具有極佳處置/可加工性且在固化時形成具有高折射率、高透明度、低透氣度及極佳伸長率之固化產品的可固化聚矽氧組合物。此外,本發明之另一目標係提供具有高折射率、低透氣度及極佳伸長率之固化產品及提供具有極佳可靠性之光學半導體裝置。
本發明之可固化聚矽氧組合物包括:(A)由以下平均單元式表示之有機聚矽氧烷:(R1 3SiO1/2)a(R1 2SiO2/2)b(R2SiO3/2)c(R3SiO3/2)d
其中,R1係相同或不同的具有1至12個碳之烷基、具有2至12個碳之烯基、具有6至20個碳之芳基或具有7至20個碳之芳烷基,限制條件係分子中之至少兩個R1為烯基;R2係具有6至20個碳之芳基或具有7至20個碳之芳烷基;R3係具有1至12個碳之烷基;且a、b、c及d分別係滿足以下條件之數值:0.01 a 0.5,0 b 0.7,0.01 c<0.7,0.1 d<0.9,且a+b+c+d=1;(B)分子中具有至少兩個矽鍵結烯基及至少一個矽鍵結芳基之直鏈有機聚矽氧烷,其量為0.1至150質量份數/100質量份數組份(A);(C)分子中具有至少兩個矽鍵結氫原子之有機聚矽氧烷,其量係使組份(C)中矽鍵結氫原子之量為組份(A)及(B)中之每1mol總烯基0.1mol至5mol;及
(D)加速本發明組合物固化之量之矽氫化反應觸媒。
本發明之固化產品係藉由固化上述可固化聚矽氧組合物來形成。
本發明之光學半導體裝置係藉由使用上述可固化聚矽氧組合物之固化產品密封光學半導體元件來製造。
本發明之可固化聚矽氧組合物具有極佳處置/可加工性,且在固化時形成具有高折射率、低透氣度及極佳伸長率之固化產品。此外,本發明固化產品之特徵在於具有高折射率及低透氣度,且本發明光學半導體裝置之特徵在於展現極佳可靠性。
1‧‧‧光學半導體元件
2‧‧‧導線框架
3‧‧‧導線框架
4‧‧‧打線
5‧‧‧框架材料
6‧‧‧固化產品
圖1係為本發明光學半導體裝置之實例之LED的剖視圖。
首先,將詳細闡述本發明之可固化聚矽氧組合物。
組份(A)係本發明組合物之主要材料且係由以下平均單元式表示之有機聚矽氧烷:(R1 3SiO1/2)a(R1 2SiO2/2)b(R2SiO3/2)c(R3SiO3/2)d
在該式中,R1可相同或不同,且各自係具有1至12個碳之烷基、具有2至12個碳之烯基、具有6至20個碳之芳基或具有7至20個碳之芳烷基。R1之特定實例包含烷基,例如甲基、乙基、丙基、丁基、戊基、己基、庚基、辛基、壬基、癸基、十一烷基及十二烷基;烯基,例如乙烯基、烯丙基、丁烯基、戊烯基、己烯基、庚烯基、辛烯基、壬烯基、癸烯基、十一烯基及十二烯基;芳基,例如苯基、甲苯基、二甲苯基、萘基、蒽基、菲基及芘基;芳烷基,例如苄基、苯乙基、萘基乙基、萘基丙基、蒽基乙基、菲基乙基、及芘基乙基;及藉由使用烷基(例如甲基或乙基)、烷氧基(例如甲氧基及乙氧基)及鹵素原子
(例如氯原子及溴原子)取代該等芳基及芳烷基中之氫原子獲得之基團。然而,分子中之至少兩個R1係烯基,且較佳係乙烯基。在該式中,R2係具有6至20個碳之芳基或具有7至20個碳之芳烷基。R2之特定實例包含芳基,例如苯基、甲苯基、二甲苯基、萘基、蒽基、菲基及芘基;芳烷基,例如苄基、苯乙基、萘基乙基、萘基丙基、蒽基乙基、菲基乙基及芘基乙基;及藉由使用烷基(例如甲基或乙基)、烷氧基(例如甲氧基及乙氧基)及鹵素原子(例如氯原子及溴原子)取代該等芳基及芳烷基中之氫原子獲得之基團。此外,在該式中,R3係具有1至12個碳之烷基。R3之特定實例包含甲基、乙基、丙基、丁基、戊基、己基、庚基、辛基、壬基、癸基、十一烷基及十二烷基;且甲基較佳。
此外,在該式中,a、b、c及d係各自滿足以下條件之數值:0.01 a 0.5,0 b 0.7,0.01 c<0.7,0.1 d<0.9,且a+b+c+d=1;較佳地,a、b、c及d係各自滿足以下條件之數值:0.05 a 0.45,0 b 0.5,0.01 c<0.6,0.2 d<0.9,且a+b+c+d=1;或a、b、c及d係各自滿足以下條件之數值:0.05 a 0.4,0 b 0.4,0.02 c<0.5,0.3 d<0.9,且a+b+c+d=1。此乃因當a大於或等於上述範圍之下限時,固化產品較難具有黏性,且另一方面,當a小於或等於上述範圍之上限時,固化產品之強度將有利。此亦因當b小於或等於上述範圍之上限時,固化產品之硬度將有利且將增強固化產品之機械特性。此亦因當c大於或等於上述範圍之下限時,固化產品之氣體障壁特性及折射率將有利,且另一方面,當c小於或等於上述範圍之上限時,將增強固化產品之機械特性。此乃因當d大於或等於上述範圍之下限時,將增強固化產品之伸長率,且另一方面,當d小於或等於上述範圍之上限時,將增強氣體障壁特性。
組份(A)係由上述平均單元式來表示,但在不損害本發明目標之
範圍內亦可具有由式:SiO4/2表示之矽氧烷單元。此外,組份(A)可在不損害本發明目標之範圍內含有矽鍵結烷氧基(例如甲氧基、乙氧基及丙氧基)或矽鍵結羥基。
製備此類型之組份(A)之方法例示為在酸或鹼存在下對以下化合物實施水解及縮合反應之方法:由以下通式表示之矽烷化合物(I):R2SiX3
由以下通式表示之矽烷化合物(II):R3SiX3
由以下通式表示之二矽氧烷(III):R1 3SiOSiR1 3
及/或由以下通式表示之矽烷化合物(IV):R1 3SiX。
矽烷化合物(I)係用於將由式:R2SiO3/2表示之矽氧烷單元引入有機聚矽氧烷中之原材料。在該式中,R2係具有6至20個碳之芳基或具有7至20個碳之芳烷基,其實例與上述基團同義,且較佳係苯基或萘基。此外,在該式中,X各自係烷氧基、醯氧基、鹵素原子或羥基。針對X之烷氧基之實例包含甲氧基、乙氧基及丙氧基。針對X之醯氧基之實例包含乙醯氧基。針對X之鹵素原子之實例包含氯原子及溴原子。
此一矽烷化合物(I)之實例包含烷氧基矽烷,例如苯基三甲氧基矽烷、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、菲基三乙氧基矽烷及芘基三乙氧基矽烷;醯氧基矽烷,例如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及芘基三乙醯氧基矽烷;鹵矽烷,例如苯基三氯矽烷、萘基三氯矽烷、蒽基三氯矽烷、菲基三氯矽烷及芘基三氯
矽烷;及羥基矽烷,例如苯基三羥基矽烷、萘基三羥基矽烷、蒽基三羥基矽烷、菲基三羥基矽烷及芘基三羥基矽烷;及該等中兩種或更多種類型之混合物。
矽烷化合物(II)係用於將由式R3SiO3/2:表示之矽氧烷單元引入有機聚矽氧烷中之原材料。在該式中,R3係具有1至12個碳之烷基,其實例與上述基團同義,且較佳係甲基、乙基或丙基。此外,在該式中,X各自係烷氧基、醯氧基、鹵素原子或羥基;且其實例與上述基團相同。
此一矽烷化合物(II)之實例包含烷氧基矽烷,例如甲基三甲氧基矽烷、乙基三甲氧基矽烷、丙基三甲氧基矽烷、丁基三甲氧基矽烷、異丁基三甲氧基矽烷、甲基三乙氧基矽烷、乙基三乙氧基矽烷、丙基三乙氧基矽烷、丁基三乙氧基矽烷及異丁基三乙氧基矽烷;醯氧基矽烷,例如甲基三乙醯氧基矽烷、乙基三乙醯氧基矽烷、丙基三乙醯氧基矽烷、丁基三乙醯氧基矽烷及異丁基三乙醯氧基矽烷;鹵矽烷,例如甲基三氯矽烷、乙基三氯矽烷、丙基三氯矽烷、丁基三氯矽烷及異丁基三氯矽烷;羥基矽烷,例如甲基三羥基矽烷、乙基三羥基矽烷、丙基三羥基矽烷、丁基三羥基矽烷及異丁基三羥基矽烷;及該等中兩種或更多種類型之混合物。
二矽氧烷(III)係用於將由式R1 3SiO1/2:表示之矽氧烷單元引入有機聚矽氧烷中之原材料。在該式中,R1可相同或不同,且各自係具有1至12個碳之烷基、具有2至12個碳之烯基、具有6至20個碳之芳基或具有7至20個碳之芳烷基,且其實例與上述基團相同。
此一二矽氧烷(III)之實例包含1,1,1,3,3,3-六甲基二矽氧烷、1,3-二苯基-1,1,3,3-四甲基二矽氧烷、1,3-二乙烯基-1,1,3,3-四甲基二矽氧烷、1,3-二乙烯基-1,3-二苯基-1,3-二甲基二矽氧烷、1,3-二乙烯基-1,1,3,3-四乙基二矽氧烷、1,1,3,3-四乙烯基-1,3-二甲基二矽氧烷及
1,1,1,3,3,3-六乙烯基二矽氧烷及該等中兩種或更多種類型之混合物。
矽烷化合物(IV)與二矽氧烷(III)相同,且係用於將由式R1 3SiO1/2:表示之矽氧烷單元引入有機聚矽氧烷中之原材料。在該式中,R1可相同或不同,且各自係具有1至12個碳之烷基、具有2至12個碳之烯基、具有6至20個碳之芳基或具有7至20個碳之芳烷基,且其實例與上述基團相同。此外,在該式中,X係烷氧基、醯氧基、鹵素原子或羥基;且其實例與上述基團相同。
此一矽烷化合物(IV)之實例包含烷氧基矽烷,例如三甲基甲氧基矽烷、二甲基苯基甲氧基矽烷、二甲基乙烯基甲氧基矽烷、甲基苯基乙烯基甲氧基矽烷、二乙基乙烯基甲氧基矽烷、三甲基乙氧基矽烷、二甲基乙烯基乙氧基矽烷、二乙基乙烯基乙氧基矽烷、二乙烯基甲基甲氧基矽烷及三乙烯基甲氧基矽烷;醯氧基矽烷,例如三甲基乙醯氧基矽烷、二甲基苯基乙醯氧基矽烷、二甲基乙烯基乙醯氧基矽烷、甲基苯基乙烯基乙醯氧基矽烷、二乙基乙烯基乙醯氧基矽烷、二乙烯基甲基乙醯氧基矽烷及三乙烯基乙醯氧基矽烷;鹵矽烷,例如三甲基氯矽烷、二甲基苯基氯矽烷、二甲基乙烯基氯矽烷、甲基苯基乙烯基氯矽烷、二乙基乙烯基氯矽烷、二乙烯基甲基氯矽烷及三乙烯基氯矽烷;羥基矽烷,例如三甲基羥基矽烷、二甲基苯基羥基矽烷、二甲基乙烯基羥基矽烷、甲基苯基乙烯基羥基矽烷、二乙基乙烯基羥基矽烷、二乙烯基甲基羥基矽烷及三乙烯基羥基矽烷;及該等中兩種或更多種類型之混合物。
在上述製備方法中,可視需要使用於引入由式R1 2SiO2/2:表示之矽氧烷單元之矽烷化合物(V)或環狀聚矽氧化合物(VI)或用於引入由式SiO4/2:表示之矽氧烷單元之矽烷化合物或矽烷寡聚物與有機聚矽氧烷反應。在該式中,R1可相同或不同,且各自係具有1至12個碳之烷基、具有2至12個碳之烯基、具有6至20個碳之芳基或具有7至20個
碳之芳烷基,且其實例與上述基團相同。
此一矽烷化合物之實例包含烷氧基矽烷,例如二甲基二甲氧基矽烷、甲基乙基二甲氧基矽烷、甲基乙烯基二甲氧基矽烷、甲基苯基二甲氧基矽烷、二苯基二甲氧基矽烷、四甲氧基矽烷、二甲基二乙氧基矽烷、甲基乙基二乙氧基矽烷、甲基乙烯基二乙氧基矽烷、甲基苯基二乙氧基矽烷、二苯基二乙氧基矽烷及四乙氧基矽烷;乙醯氧基矽烷,例如二甲基二乙醯氧基矽烷、甲基乙烯基二乙醯氧基矽烷、甲基苯基二乙醯氧基矽烷、二苯基二乙醯氧基矽烷及四乙醯氧基矽烷;鹵矽烷,例如二甲基二氯矽烷、甲基乙烯基二氯矽烷、甲基苯基二氯矽烷、二苯基二氯矽烷及四氯矽烷;及羥基矽烷,例如二甲基二羥基矽烷、甲基乙烯基二羥基矽烷、甲基苯基二羥基矽烷及二苯基二羥基矽烷。此一環狀聚矽氧化合物之實例包含環狀二甲基矽氧烷寡聚物、環狀甲基乙烯基矽氧烷寡聚物、環狀苯基甲基矽氧烷寡聚物及環狀二苯基矽氧烷寡聚物。此外,矽烷寡聚物之實例包含四甲氧基矽烷之部分水解產物及四乙氧基矽烷之部分水解產物。
上述製備方法之特徵在於,在酸或鹼存在下對矽烷化合物(I)、矽烷化合物(II)及二矽氧烷(III)及/或矽烷化合物(IV)以及上述另一矽烷化合物(V)、環狀聚矽氧化合物(VI)或矽烷寡聚物(若需要)實施水解/縮合反應。應注意,在上述製備方法中,要求二矽氧烷(III)及/或矽烷化合物(IV)或矽烷化合物(V)及/或環狀聚矽氧化合物(VI)係至少含有具有2至12個碳之烯基之化合物。
上述酸之實例包含鹽酸、乙酸、甲酸、硝酸、草酸、硫酸、磷酸、聚磷酸、聚羧酸、三氟甲烷磺酸及離子交換樹脂。此外,上述鹼之實例包含無機鹼,例如氫氧化鉀及氫氧化鈉;及有機鹼化合物,例如三乙胺、二乙胺、單乙醇胺、二乙醇胺、三乙醇胺、氨水、四甲基氫氧化銨、具有胺基之烷氧基矽烷及胺基丙基三甲氧基矽烷。
此外,有機溶劑可用於上述製備方法中。所利用有機溶劑之實例包含醚、酮、乙酸酯、芳香族或脂肪族烴及γ-丁內酯;及該等溶劑中兩種或更多種類型之混合物。較佳有機溶劑之實例包含丙二醇單甲基醚、丙二醇單甲基醚乙酸酯、丙二醇單乙基醚、丙二醇單丙基醚、丙二醇單丁基醚、丙二醇單-第三丁基醚、γ-丁內酯、甲苯及二甲苯。
為加速製備方法中每一組份之水解及縮合反應,較佳添加水或水及醇之混合溶液。甲醇及乙醇係醇之較佳實例。若使用有機溶劑且藉由加熱加速此反應,則較佳在有機溶劑之回流溫度下實施反應。
組份(A)可藉由個別摻和所製備之有機聚矽氧烷來獲得。在該等情形下,每一有機聚矽氧烷無需對應於上文所指定之平均單元式,且其混合物可滿足上文所提及之平均單元式。
組份(B)係用來賦予藉由固化本發明組合物所獲得之固化產品撓性之組份,且係分子中具有至少兩個矽鍵結烯基及至少一個矽鍵結芳基之直鏈有機聚矽氧烷。組份(B)中烯基之實例包含乙烯基、烯丙基、丁烯基、戊烯基及己烯基。在該等基團中,乙烯基較佳。此外,組份(B)中芳基之實例包含苯基、甲苯基、二甲苯基及萘基。在該等基團中,苯基較佳。此外,組份(B)中除烯基及芳基外之鍵結至矽原子之基團的實例包含烷基,例如甲基、乙基、丙基、丁基、戊基、己基及庚基;芳烷基,例如苄基及苯乙基;鹵化烷基,例如氯甲基、3-氯丙基及3,3,3-三氟丙基。在該等基團中,甲基較佳。組份(B)之黏度不受特定限制,且在25℃下之黏度較佳介於10mPa.s至10,000,000mPa.s範圍內、介於10mPa.s至1,000,000mPa.s範圍內或介於10mPa.s至100,000mPa.s範圍內。此乃因當組份(B)之黏度小於上述範圍之下限時,所獲得固化產品之機械強度往往減弱,且另一方面,當組份(B)之黏度超過上述範圍之上限時,所獲得組合物之處置/可加工性往
往降低。
組份(B)之分子結構為直鏈,且此一組份(B)之實例包含由以下通式表示之有機聚矽氧烷:
在該式中,R1相同或不同,且各自係具有1至12個碳之烷基、具有2至12個碳之烯基、具有6至20個碳之芳基或具有7至20個碳之芳烷基,且其實例與上述基團相同。然而,分子中之至少兩個R1係烯基。此外,在該式中,R2相同或不同,且各自係具有6至20個碳之芳基或具有7至20個碳之芳烷基,其實例與上述基團同義,且較佳係苯基。此外,在該式中,R3相同或不同,且各自係具有1至12個碳之烷基,其實例與上述基團同義,且較佳係甲基。
此外,在該式中,m係0至800之整數,n係0至300之整數,且o係0至300之整數,限制條件係m、n及o滿足:m n且5 m+n+o 1,000。較佳地,m係0至500之整數,n係0至200之整數,且o係0至200之整數,限制條件係m、n及o滿足:m n且5 m+n+o 500。此乃因當m、n及o小於或等於上述範圍之上限時,組合物之處置/可加工性將增強。此亦因當m+n+o在上述範圍內時可賦予固化產品撓性。
組份(B)係由上述通式來表示,但在不損害本發明目標之範圍內亦可具有矽鍵結烷氧基(例如甲氧基、乙氧基或丙氧基)或矽鍵結羥基。
此類型之組份(B)之實例包含有機聚矽氧烷,例如下文所提及之彼等。應注意,在該等式中,Me表示甲基,Vi表示乙烯基,且Ph表示苯基,且m'係1至100之整數,n'係1至50之整數,且o'係1至50之整
數,限制條件係m' n'且m'+n'+o' 100。
ViMe2SiO(Me2SiO)m' SiMe2Vi
ViPhMeSiO(Me2SiO)m' SiMePhVi
ViPh2SiO(Me2SiO)m' SiPh2Vi
ViMe2SiO(Me2SiO)m'(Ph2SiO)n' SiMe2Vi
ViPhMeSiO(Me2SiO)m'(Ph2SiO)n' SiPhMeVi
ViPh2SiO(Me2SiO)m'(Ph2SiO)n' SiPh2Vi
ViMe2SiO(MePhSiO)O' SiMe2Vi
MePhViSiO(MePhSiO)O' SiMePhVi
Ph2ViSiO(MePhSiO)O' SiPh2Vi
ViMe2SiO(Ph2SiO)n'(PhMeSiO)O' SiMe2Vi
ViPhMeSiO(Ph2SiO)n'(PhMeSiO)O' SiPhMeVi
ViPh2SiO(Ph2SiO)n'(PhMeSiO)O' SiPh2Vi
組份(B)之含量介於0.1至150質量份數/100質量份數組份(A)範圍內,較佳介於1至100質量份數範圍內,且進一步較佳介於1至75質量份數範圍內。此乃因當組份(B)之含量大於或等於上述範圍之下限時,可賦予固化產品撓性,且當含量小於或等於上述範圍之上限時,固化產品之機械特性較為有利。
組份(C)係本發明組合物之交聯劑,且係分子中具有至少兩個矽鍵結氫原子之有機聚矽氧烷。組份(C)之分子結構之實例包含直鏈、部分具支鏈之直鏈、具支鏈、環狀及樹突狀。在該等基團中,直鏈、部分具支鏈之直鏈及樹突狀較佳。組份(C)中矽鍵結氫原子之鍵結位置不受特定限制,且例如可位於分子鏈之末端及/或分子鏈之側鏈上。此外,組份(C)中除氫原子外鍵結至矽原子之基團的實例包含烷基,例如甲基、乙基及丙基;芳基,例如苯基、甲苯基及二甲苯基;芳烷基,例如苄基及苯乙基;鹵化烷基,例如3-氯丙基及3,3,3-三氟
丙基;縮水甘油氧基烷基,例如3-縮水甘油氧基丙基及4-縮水甘油氧基丁基;及烷氧基矽基烷基,例如三甲氧基矽基乙基、三甲氧基矽基丙基、三乙氧基矽基乙基及二甲氧基甲基矽基乙基。在該等基團中,甲基及苯基較佳。組份(C)之黏度不受特定限制,且在25℃下黏度較佳介於1mPa.s至10,000mPa.s範圍內,且尤佳介於1mPa.s至1,000mPa.s範圍內。
組份(C)之此一有機聚矽氧烷之實例包含1,1,3,3-四甲基二矽氧烷、1,3,5,7-四甲基環四矽氧烷、叁(二甲基氫矽氧基)甲基矽烷、叁(二甲基氫矽氧基)苯基矽烷、1-(3-縮水甘油氧基丙基)-1,3,5,7-四甲基環四矽氧烷、1,5-二(3-縮水甘油氧基丙基)-1,3,5,7-四甲基環四矽氧烷、1-(3-縮水甘油氧基丙基)-5-三甲氧基矽基乙基-1,3,5,7-四甲基環四矽氧烷、兩個分子端經三甲基矽氧基封端之甲基氫聚矽氧烷、二甲基矽氧烷與甲基氫矽氧烷之兩個分子端經三甲基矽氧基封端之共聚物、兩個分子端經二甲基氫矽氧基封端之二甲基聚矽氧烷、二甲基矽氧烷與甲基氫矽氧烷之兩個分子端經二甲基氫矽氧基封端之共聚物、甲基氫矽氧烷與二苯基矽氧烷之兩個分子端經三甲基矽氧基封端之共聚物、兩個分子端經三甲基矽氧基封端之甲基氫矽氧烷、二苯基矽氧烷及二甲基矽氧烷之共聚物、三甲氧基矽烷之水解/縮合反應產物、由(CH3)2HSiO1/2單元及SiO4/2單元組成之共聚物、由(CH3)2HSiO1/2單元及SiO4/2單元以及(C6H5)SiO3/2單元組成之共聚物及該等中兩種或更多種類型之混合物。
進一步例示以下有機矽氧烷作為組份(C)。
應注意,在該等式中,Me表示甲基,Ph表示苯基且Naph表示萘基;e、f、g及h係各自滿足以下條件之數值:0.1 e 0.7,0<f 0.5,0<g 0.7,0.1 h<0.9,且e+f+g+h=1;且p係1至100之整數,且q係1或更大之整數,限制條件係p+q係100或更小之整數。
HMe2SiO(Ph2SiO)p SiMe2H
HMePhSiO(Ph2SiO)p SiMePhH
HMeNaphSiO(Ph2SiO)p SiMeNaphH
HMePhSiO(Ph2SiO)p(MePhSiO)q SiMePhH
HMePhSiO(Ph2SiO)p(Me2SiO)q SiMePhH
(HMe2SiO1/2)e(PhSiO3/2)h
(HMePhSiO1/2)e(PhSiO3/2)h
(HMePhSiO1/2)e(NaphSiO3/2)h
(HMe2SiO1/2)e(NaphSiO3/2)h
(HMePhSiO1/2)e(HMe2SiO1/2)f(PhSiO3/2)h
(HMe2SiO1/2)e(Ph2SiO2/2)g(PhSiO3/2)h
(HMePhSiO1/2)e(Ph2SiO2/2)g(PhSiO3/2)h
(HMe2SiO1/2)e(Ph2SiO2/2)g(NaphSiO3/2)h
(HMePhSiO1/2)e(Ph2SiO2/2)g(NaphSiO3/2)h
(HMePhSiO1/2)e(HMe2SiO1/2)f(NaphSiO3/2)h
(HMePhSiO1/2)e(HMe2SiO1/2)f(Ph2SiO2/2)g(NaphSiO3/2)h
(HMePhSiO1/2)e(HMe2SiO1/2)f(Ph2SiO2/2)g(PhSiO3/2)h
組份(C)之含量應使組份(C)中之矽鍵結氫原子介於組份(A)及(B)中之每1mol總烯基0.1mol至5mol範圍內,且較佳介於0.5mol至2mol範圍內。此乃因當組份(C)之含量大於或等於上述範圍之下限時,組合物經充分固化,且當含量小於或等於上述範圍之上限時,固化產品之耐熱性得到改良,由此使得可改良使用本發明組合物製造之光學半導體裝置之可靠性。
組份(D)係用於加速本發明組合物固化之矽氫化反應觸媒,且其實例包含基於鉑之觸媒、基於銠之觸媒及基於鈀之觸媒。在該等基團中,基於鉑之觸媒較佳。此基於鉑之觸媒之實例包含基於鉑之化合
物,例如鉑細粉、鉑黑、鉑載二氧化矽細粉、鉑載活性碳、氯鉑酸、氯鉑酸之醇溶液、鉑之烯烴錯合物及鉑之烯基矽氧烷錯合物。
組份(D)之含量係加速本發明組合物固化之量,且組份(D)之含量較佳係使此觸媒中金屬原子之量(以質量計)相對於本發明組合物之量介於0.01ppm至1,000ppm範圍內的量。此乃因當組份(D)之含量小於上述範圍之下限時,所獲得組合物之固化可能不充分。另一方面,甚至當組份(D)之含量超過上述範圍之上限時,將無法顯著加速組合物之固化,且可產生諸如固化產品之著色等問題。
儘管本發明組合物係由至少上述組份(A)至(D)構成,但本發明組合物亦可含有(E)矽氫化反應抑制劑作為可選組份來延長在室溫下之工作壽命並改良儲存穩定性。此一組份(E)之實例包含炔烴醇,例如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;烯炔化合物,例如3-甲基-3-戊烯-1-炔及3,5-二甲基-3-己烯-1-炔;甲基烯基矽氧烷寡聚物,例如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;炔氧基矽烷,例如二甲基雙(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)矽烷及基於三烯丙基異氰尿酸酯之化合物。
組份(E)之含量不受特定限制,且該含量較佳介於0.01至3質量份數/總共100質量份數之組份(A)至(C)範圍內或介於0.01至1質量份數範圍內。此乃因當組份(E)之含量大於或等於上述範圍之下限時,本發明組合物將具有適宜工作壽命,且另一方面,當組份(E)之含量小於或等於上述範圍之上限時,將確保適當可加工性。
此外,本發明組合物亦可含有(F)助黏劑,以進一步改良在固化期間與組合物所接觸之基板之黏著。此一組份(F)較佳係分子中具有至少一個鍵結至矽原子之烷氧基之有機矽化合物。烷氧基之實例包含
甲氧基、乙氧基、丙氧基、丁氧基及甲氧基乙氧基。在該等基團中,甲氧基及乙氧基尤佳。除烷氧基外鍵結至此有機矽化合物之矽原子之基團之實例包含經取代或未經取代之單價烴基團,例如烷基、烯基、芳基、芳烷基及鹵化烷基;縮水甘油氧基烷基,例如3-縮水甘油氧基丙基及4-縮水甘油氧基丁基;環氧基環烷基烷基,例如2-(3,4-環氧基環己基)乙基及3-(3,4-環氧基環己基)丙基;環氧乙烷基烷基,例如4-環氧乙烷基丁基及8-環氧乙烷基辛基;含有丙烯酸基團之單價有機基團,例如3-甲基丙烯醯氧基丙基;異氰酸酯基團;異氰尿酸酯基團;及氫原子。
有機矽化合物較佳具有可與本發明組合物中之矽鍵結烯基或矽鍵結氫原子反應之基團。特定而言,有機矽化合物較佳具有矽鍵結氫原子或矽鍵結烯基。有機矽化合物之分子結構之實例包含直鏈、部分具支鏈之直鏈、具支鏈、環狀及網狀結構。分子結構尤佳係直鏈、具支鏈或網狀結構。此一有機矽化合物之實例包含矽烷化合物,例如3-縮水甘油氧基丙基三甲氧基矽烷、2-(3,4-環氧基環己基)乙基三甲氧基矽烷及3-甲基丙烯醯氧基丙基三甲氧基矽烷;分子中具有矽鍵結烯基或矽鍵結氫原子中之至少一者及至少一個矽鍵結烷氧基之矽氧烷化合物;具有至少一個矽鍵結烷氧基之矽烷化合物或矽氧烷化合物及分子中具有至少一個矽鍵結羥基及至少一個矽鍵結烯基之矽氧烷化合物的混合物;由以下平均單元式表示之矽氧烷化合物:
其中,x、y及z為正數;且由以下平均單元式表示之矽氧烷化合物:[式3]
其中,x、y、z及w為正數。
組份(F)之含量不受特定限制,且該含量較佳介於0.01至10質量份數/總共100質量份數之組份(A)至(C)範圍內,或介於0.1至3質量份數範圍內。此乃因當組份(F)之含量大於或等於上述範圍之下限時黏著較為有利,且當含量小於或等於上述範圍之上限時儲存穩定性較為有利。
本發明組合物可進一步包括(G)螢光材料作為另一可選組份。此一組份(G)之實例包含例如含有氧化物螢光物質、氧氮化物螢光物質、氮化物螢光物質、硫化物螢光物質、氧硫化物螢光物質或諸如此類之發黃光、紅光、綠光及藍光之螢光物質,其廣泛用於發光二極體(LED)中。氧化物螢光物質之實例包含含有鈰離子之釔、鋁及石榴石型YAG發綠光至黃光螢光物質;含有鈰離子之鋱、鋁及石榴石型TAG發黃光螢光物質;及含有鈰或銪離子之矽酸鹽發綠光至黃光螢光物質。氧氮化物螢光物質之實例包含含有銪離子之矽、鋁、氧及氮型SiAlON發紅光至綠光螢光物質。氮化物螢光物質之實例包含含有銪離子之鈣、鍶、鋁、矽及氮型CASN發紅光螢光物質。硫化物螢光物質之實例包含含有銅離子或鋁離子之ZnS發綠光螢光物質。氧硫化物螢光物質之實例包含含有銪離子之Y2O2S發紅光螢光物質。可使用該等螢光材料中之一種類型或兩種或更多種類型之混合物。
組份(G)之平均粒徑不受特定限制,但較佳介於1μm至50μm範圍內或介於5μm至20μm範圍內。此乃因當組份(G)之平均粒徑大於或等於上述範圍之下限時,將阻抑混合時黏度之增加。另一方面,當組份(G)之平均粒徑小於或等於上述範圍之上限時,光透射率將有利。
組份(G)之含量不受特定限制,且該含量較佳係相對於本發明組
合物之量0.1質量%至70質量%之量。此外,自處置/可加工性的角度來看,組份(G)之含量較佳係相對於本發明組合物之量70質量%或更小。另一方面,自至白光之轉化特性的角度來看,組份(G)之含量較佳係相對於本發明組合物之量5質量%或更大。
本發明之此一可固化聚矽氧組合物展現極佳流動性及填充特性。儘管可固化聚矽氧組合物之黏度不受特定限制,但端視應用,在25℃下之黏度通常較佳介於100mPa.s至500,000mPa.s範圍內或介於100mPa.s至100,000mPa.s範圍內。
此外,無機填充劑,例如二氧化矽、玻璃、氧化鋁或氧化鋅;聚甲基丙烯酸酯樹脂之有機樹脂細粉及諸如此類;耐熱劑、染料、顏料、阻燃劑、溶劑及諸如此類可作為可選組份以不損害本發明目標之量納入本發明組合物中。
在作為可選組份添加之組份中,為充分阻抑光學半導體裝置中之銀電極或基板之銀鍍層因空氣中之含硫氣體所致之變色,可添加至少一種類型之平均粒徑為0.1nm至5μm之選自由以下組成之群的細粉:經選自由Al、Ag、Cu、Fe、Sb、Si、Sn、Ti、Zr及稀土元素組成之群之元素的至少一種類型之氧化物表面處理之氧化鋅細粉、經不具烯基之有機矽化合物表面處理之氧化鋅細粉及碳酸鋅之水合物細粉。
在經氧化物表面處理之氧化鋅細粉中,稀土元素之實例包含釔、鈰及銪。氧化鋅細粉之表面上之氧化物的實例包含Al2O3、AgO、Ag2O、Ag2O3、CuO、Cu2O、FeO、Fe2O3、Fe3O4、Sb2O3、SiO2、SnO2、Ti2O3、TiO2、Ti3O5、ZrO2、Y2O3、CeO2、Eu2O3及該等氧化物中兩種或更多種類型之混合物。
在經有機矽化合物表面處理之氧化鋅細粉中,有機矽化合物不具烯基,且實例包含有機矽烷、有機矽氮烷、聚甲基矽氧烷、有機氫
聚矽氧烷及有機矽氧烷寡聚物。特定實例包含有機氯矽烷,例如三甲基氯矽烷、二甲基氯矽烷及甲基三氯矽烷;有機三烷氧基矽烷,例如甲基三甲氧基矽烷、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及γ-甲基丙烯醯氧基丙基三甲氧基矽烷;二有機二烷氧基矽烷,例如二甲基二甲氧基矽烷、二甲基二乙氧基矽烷及二苯基二甲氧基矽烷;三有機烷氧基矽烷,例如三甲基甲氧基矽烷及三甲基乙氧基矽烷;該等有機烷氧基矽烷之部分縮合物;有機矽氮烷,例如六甲基二矽氮烷;及聚甲基矽氧烷、有機氫聚矽氧烷、具有矽醇基團或烷氧基之有機矽氧烷寡聚物、具有矽醇基團或烷氧基且由R4SiO3/2單元(其中,R4係除烯基外之單價烴基團,且單價烴基團之實例包含烷基,例如甲基、乙基或丙基;及芳基,例如苯基)及/或SiO4/2單元構成之樹脂狀有機聚矽氧烷。
碳酸鋅之水合物細粉係其中水鍵結至碳酸鋅之化合物,且較佳化合物係其中在加熱條件下在105℃下保持3小時重量減小率為至少0.1wt.%者。
氧化鋅以質量單位計之含量係介於組合物之1ppm至10%範圍內之量,且較佳係介於1ppm至5%範圍內之量。此乃因當該組份之含量大於或等於上述範圍之下限時,可充分阻抑光學半導體裝置中之銀電極或基板之銀鍍層因含硫氣體所致之變色,且當該含量小於或等於上述範圍之上限時,所得組合物之流動性並不會降低。
此外,本發明組合物亦可含有基於三唑之化合物作為可選組份,以使得能夠進一步阻抑銀電極或基板之銀鍍層因空氣中之含硫氣體所致之變色。該等組份之實例包含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、苯并三唑、甲苯基三唑、羧基苯并三唑、甲酸1H-苯并三唑-5-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、環己醇[1,2-d]三唑、4,5,6,7-四羥基甲苯基三唑、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]甲苯基三唑、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]甲苯基三唑、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'-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-甲酸、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-甲酸、1,2,4-三唑-3-甲醯胺、4-胺基尿唑及1,2,4-三唑-5-酮。此苯并三唑化合物之含量不受特定限制,但以質量單位計係介於組合物之0.01ppm至3%範圍內、且較佳介於0.1ppm至1%範圍內之量。
本發明組合物應使固化發生在在室溫下或加熱下,但較佳加熱組合物以達成快速固化。加熱溫度較佳為50℃至200℃。
現將詳細闡述本發明之固化產品。
本發明之固化產品係藉由固化上述可固化聚矽氧組合物來形成。固化產品之形狀不受特定限制,且實例包含片狀及膜狀。固化產品可處置為簡單物質或亦可處置成其中固化產品覆蓋或密封光學半導體元件或諸如此類之狀態。
現將詳細解釋本發明之光學半導體裝置。
本發明之光學半導體裝置係藉由使用上述可固化聚矽氧組合物
之固化產品密封光學半導體元件來製造。本發明之此一光學半導體裝置之實例包含發光二極體(LED)、光耦合器及CCD。發光二極體(LED)之實例包含SMD(表面安裝裝置)型及COB(板上晶片)型。SMD之實例包含俯視型及側視型。光學半導體元件之實例包含發光二極體(LED)晶片及固態影像感測裝置。發光二極體晶片之實例包含面向上型及倒裝晶片型。此外,發光二極體晶片之實例包含含有Ga-As之紅外LED晶片、含有Ga-Al-As之紅色LED晶片、含有Ga-As-P之橙色或黃色LED晶片、含有氮摻雜Ga-As之黃色LED晶片及含有鎵氮化物化合物之藍色或淺藍色-紫外LED晶片。
圖1圖解說明單一表面安裝型LED之剖視圖,該LED係本發明光學半導體裝置之實例。在圖1所圖解說明之LED中,光學半導體元件1黏晶至導線框架2,且藉由打線4打線接合半導體元件1與導線框架3。在此光學半導體元件1之周邊周圍提供框架材料5,且藉由本發明可固化聚矽氧組合物之固化產品6密封此框架材料5內側上之光學半導體元件1。用於框架材料之材料之實例包含芳香族聚醯胺樹脂、脂肪族環狀聚醯胺樹脂、脂肪族聚醯胺樹脂、液晶聚合物、聚矽氧樹脂、經修飾聚矽氧樹脂、環氧樹脂及經修飾環氧樹脂。
用於製造圖1所圖解說明之表面安裝型LED之方法之實例係包括以下步驟之方法:將光學半導體元件1黏晶至導線框架2,藉由金屬打線4打線接合此光學半導體元件1與導線框架3,對在光學半導體元件1周邊周圍提供之框架材料5內部之本發明可固化聚矽氧組合物充電,且然後藉由加熱至50℃至200℃固化可固化聚矽氧組合物。
下文將使用實例詳細闡述本發明之可固化聚矽氧組合物、其固化產品及光學半導體裝置。在實例中,黏度係在25℃下之值,且Me、Vi、Ph及Ep分別表示甲基、乙烯基、苯基及3-縮水甘油氧基丙
基。如下量測可固化聚矽氧組合物之固化產品之特性。
藉由在循環熱空氣爐中在150℃下將可固化聚矽氧組合物加熱2小時來製造固化產品。使用折射計量測此固化產品在25℃下及633nm波長下之折射率。
藉由使用壓機在150℃下將可固化聚矽氧組合物固化2小時來製備厚度為1mm之膜狀固化產品。在具有40℃之溫度及90%相對濕度之條件下使用由Systech Illinois製造之水蒸氣滲透分析儀(型號:7002)來量測膜狀固化產品之水蒸氣滲透率。作為量測之結果,水蒸氣滲透率為10g/m2.24hr或更大至小於15g/m2.24hr之情形指示為「◎」,水蒸氣滲透率為15g/m2.24hr或更大至小於20g/m2.24hr之情形指示為「○」,且水蒸氣滲透率為20g/m2.24hr或更大之情形指示為「×」。
製備厚度為2mm之片狀固化產品,且如JIS K 6251-1993「硫化橡膠之拉伸測試方法」中所規定以JIS 3號啞鈴形式對此產品進行壓型。使用由Shimadzu公司製得之自動繪圖儀來量測斷裂伸長率(%)。作為量測之結果,伸長率為20%或更大之情形指示為「◎」,伸長率為10%或更大至小於20%之情形指示為「○」,且伸長率小於10%之情形指示為「×」。
使用可固化聚矽氧組合物來製造圖1所圖解說明之光學半導體裝置。應注意,可固化聚矽氧組合物係藉由在150℃下加熱2小時來固化。藉由使用積分球量測總輻射通量之裝置來量測此光學半導體裝置之初始輻射通量。然後,將此光學半導體裝置置於放置有硫化鈉六水
合物之高壓釜中,加熱至50℃且靜置100小時。此後,藉由使用積分球量測總輻射通量之裝置來量測輻射通量。變化率為20%或更小之情形指示為「◎」,且變化率大於20%至30%或更小之情形指示為「○」。
使用可固化聚矽氧組合物來製造圖1之光學半導體裝置。應注意,可固化聚矽氧組合物係藉由在150℃下加熱2小時來固化。使所獲得光學半導體裝置老化,同時在85℃之溫度、85%之濕度條件下發光,並施加420mA之電荷。500小時後,使用電子顯微鏡觀察光學半導體裝置之外觀。未觀察到裂紋之情形指示為「◎」,且出現裂紋之情形指示為「×」。
使用可固化聚矽氧組合物來製造圖1所圖解說明之光學半導體裝置。應注意,可固化聚矽氧組合物係藉由在150℃下加熱2小時來固化。藉由使用積分球量測總輻射通量之裝置來量測此光學半導體裝置之初始輻射通量。然後,使此光學半導體裝置老化,同時在85℃之溫度、85%之濕度條件下發光,並施加400mA之電荷。1000小時後,藉由使用積分球量測總輻射通量之裝置來量測光學半導體裝置之輻射通量。變化率為5%或更小之情形指示為「◎」,變化率大於5%至10%或更小之情形指示為「○」,且變化率大於10%之情形指示為「△」。
在反應容器中放置14.0g(0.08mol)1,3-二乙烯基-1,1,3,3-四甲基二矽氧烷、137.3g甲苯、50.2g異丙醇及78.9g濃鹽酸,且在60℃或更低下逐滴添加59.5g(0.30mol)苯基三甲氧基矽烷、74.9g(0.55mol)甲基三甲氧基矽烷及65g甲苯之混合溶液。完成逐滴添加後,在
70℃下將所獲得混合物攪拌3小時。此後,蒸餾出所產生甲醇,並洗滌所獲得混合物以使系統呈中性。然後,在減壓下移除溶劑,以獲得57g(產率:40%)由以下平均單元式表示之有機聚矽氧烷樹脂:(Me2ViSiO1/2)0.15(PhSiO3/2)0.30(MeSiO3/2)0.55
其為無色且透明並具有1,400之數量平均分子量及1.49之折射率。
在反應容器中放置14.0g(0.08mol)1,3-二乙烯基-1,1,3,3-四甲基二矽氧烷、137.3g甲苯、50.2g異丙醇及78.9g濃鹽酸,且在60℃或更低下逐滴添加39.7g(0.20mol)苯基三甲氧基矽烷、88.5g(0.65mol)甲基三甲氧基矽烷及65g甲苯之混合溶液。完成逐滴添加後,在70℃下將所獲得混合物攪拌3小時。此後,蒸餾出所產生甲醇,並洗滌所獲得混合物以使系統呈中性。然後,在減壓下移除溶劑,以獲得57g(產率:40%)由以下平均單元式表示之有機聚矽氧烷樹脂:(Me2ViSiO1/2)0.15(PhSiO3/2)0.20(MeSiO3/2)0.65
其為無色且透明並具有1,450之數量平均分子量及1.48之折射率。
在反應容器中放置14.0g(0.08mol)1,3-二乙烯基-1,1,3,3-四甲基二矽氧烷、137.3g甲苯、50.2g異丙醇及78.9g濃鹽酸,且在60℃或更低下逐滴添加23.8g(0.12mol)苯基三甲氧基矽烷、99.4g(0.73mol)甲基三甲氧基矽烷及65g甲苯之混合溶液。完成逐滴添加後,在70℃下將所獲得混合物攪拌3小時。此後,蒸餾出所產生甲醇,並洗滌所獲得混合物以使系統呈中性。然後,在減壓下移除溶劑,以獲得57g(產率:40%)由以下平均單元式表示之有機聚矽氧烷樹脂:(Me2ViSiO1/2)0.15(PhSiO3/2)0.12(MeSiO3/2)0.73
其為無色且透明並具有1,385之數量平均分子量及1.46之折射率。
在反應容器中放置14.0g(0.08mol)1,3-二乙烯基-1,1,3,3-四甲基二矽氧烷、137.3g甲苯、50.2g異丙醇及78.9g濃鹽酸,且在60℃或更低下逐滴添加9.92g(0.05mol)苯基三甲氧基矽烷、109.0g(0.80mol)甲基三甲氧基矽烷及65g甲苯之混合溶液。完成逐滴添加後,在70℃下將所獲得混合物攪拌3小時。此後,蒸餾出所產生甲醇,並洗滌所獲得混合物以使系統呈中性。然後,在減壓下移除溶劑,以獲得57g(產率:40%)由以下平均單元式表示之有機聚矽氧烷樹脂:(Me2ViSiO1/2)0.15(PhSiO3/2)0.05(MeSiO3/2)0.80
其為無色且透明並具有1,724之數量平均分子量及1.44之折射率。
在反應容器中放置37.7g(0.23mol)六甲基二矽氧烷、65.0g(0.35mol)1,3-二乙烯基-1,1,3,3-四甲基二矽氧烷及0.42g三氟甲烷磺酸,且逐滴添加187.4g(10.4mol)離子交換水、202.7g(1.02mol)苯基三甲氧基矽烷及335.4g(2.45mol)甲基三甲氧基矽烷。完成逐滴添加後,將所獲得混合物回流1小時以移除低沸點組份。然後,將267g甲苯及0.8g氫氧化鉀添加至所獲得混合物中,且形成共沸物以移除水。此後,在120℃下將所獲得混合物攪拌6小時。此後,藉由乙酸中和所獲得混合物,並過濾出所得鹽。然後,在減壓下移除溶劑,以獲得由以下平均單元式表示之有機聚矽氧烷樹脂:(Me2ViSiO1/2)0.15(Me3SiO1/2)0.10(PhSiO3/2)0.22(MeSiO3/2)0.53
其為無色且透明並具有2,350之數量平均分子量及1.47之折射率。
在反應容器中放置280.0g(1.41mol)苯基三甲氧基矽烷、192.3g(1.41mol)甲基三甲氧基矽烷、131.0g(0.422mol)1,3-二乙烯基-1,3-二苯基-1,3-二甲基二矽氧烷及4.87g(32.5mmol)三氟甲烷磺酸,且逐滴添加154.0g(8.5mol)離子交換水。完成逐滴添加後,將所獲得混合物回流2小時以移除低沸點組份。然後,將272g甲苯及2.67g(47.6mmol)氫氧化鉀添加至所獲得混合物中,且形成共沸物以移除水。此後,在120℃下將所獲得混合物攪拌6小時。此後,藉由1.1g(18mmol)乙酸中和所獲得混合物,並過濾出所得鹽。然後,在減壓下移除溶劑,以獲得396g(產率:96%)由以下平均單元式表示之有機聚矽氧烷樹脂:(MePhViSiO1/2)0.228(PhSiO3/2)0.388(MeSiO3/2)0.384
其為無色且透明並具有2,200之數量平均分子量及1.533之折射率。
在反應容器中放置200.0g(1.01mol)苯基三甲氧基矽烷、58.5g(0.43mol)甲基三甲氧基矽烷、66.7g(0.215mol)1,3-二乙烯基-1,3-二苯基-1,3-二甲基二矽氧烷及1.24g(8.3mmol)三氟甲烷磺酸,且逐滴添加55.0g(3mol)離子交換水。完成逐滴添加後,將所獲得混合物回流2小時以移除低沸點組份。然後,將56.5g甲苯及0.97g(17.3mmol)氫氧化鉀添加至所獲得混合物中,且形成共沸物以移除水。此後,在120℃下將所獲得混合物攪拌6小時。此後,藉由0.89g(15mmol)乙酸中和所獲得混合物,並過濾出所得鹽。然後,在減壓下移除溶劑,以獲得218g(產率:97%)由以下平均單元式表示之有機聚矽氧烷樹脂:(MePhViSiO1/2)0.235(PhSiO3/2)0.539(MeSiO3/2)0.226
其為無色且透明並具有1,700之數量平均分子量及1.545之折射率。
在反應容器中放置40.0g(0.045mol)由下式表示之二甲基聚矽氧烷:HO(Me2SiO)12H
62.0g甲苯及10.9g(0.107mol)三乙胺,且在攪拌的同時添加22.0g(0.090mol)乙烯基二苯基氯矽烷。在室溫下將所獲得混合物攪拌1小時後,將混合物加熱至50℃且攪拌3小時。然後添加水。用水洗滌後,藉由在減壓下加熱自有機相移除低沸點物質,以獲得由下式表示之有機聚矽氧烷:Ph2ViSiO(Me2SiO)12SiPh2Vi
其為無色且透明並具有36mPa.s之黏度及1.466之折射率。
首先,將82.2g(0.44mol)1,3-二乙烯基-1,1,3,3-四甲基二矽氧烷、143g水、0.38g三氟甲烷磺酸及500g甲苯裝載至具有攪拌器、回流冷卻器及溫度計之4頸燒瓶中,且在攪拌的同時經1小時之時程將524.7g(2.65mol)苯基三甲氧基矽烷逐滴添加至混合物中。完成逐滴添加後,將混合物熱回流1小時。然後將混合物冷卻,且分離底部相後,用水將甲苯溶液相洗滌三次。在所洗滌甲苯溶液相中,添加314g(1.42mol)3-縮水甘油氧基丙基甲基二甲氧基矽烷、130g水及0.50g氫氧化鉀,且熱回流1小時。然後蒸餾掉甲醇,,且藉由共沸脫水移除過量水。熱回流4小時後,將甲苯溶液冷卻,用0.55g乙酸中和,且用水洗滌三次。移除水後,在減壓下蒸餾掉甲苯以製備黏度為8,500mPa.s之由以下平均單元式表示之黏著賦予劑:(Me2ViSiO1/2)0.18(PhSiO3/2)0.53(EpMeSiO2/2)0.29
使用下文所列示之組份根據表1中所顯示之組成(質量份數)製備可固化聚矽氧組合物。應注意,在表1中,組份(D)之含量係根據鉑金屬相對於可固化聚矽氧組合物之含量(ppm,以質量單位計)來表示。表1中之H/Vi表示組份(C)中之矽原子鍵結氫原子相對於組份(A)及組份(B)中之總共1mol乙烯基的莫耳數。
使用以下組份作為組份(A)。
組份(A-1):在參考實例1中製備且由以下平均單元式表示之有機聚矽氧烷樹脂:(Me2ViSiO1/2)0.15(PhSiO3/2)0.30(MeSiO3/2)0.55
組份(A-2):在參考實例2中製備且由以下平均單元式表示之有機聚矽氧烷樹脂:
(Me2ViSiO1/2)0.15(PhSiO3/2)0.20(MeSiO3/2)0.65
組份(A-3):在參考實例3中製備且由以下平均單元式表示之有機聚矽氧烷樹脂:(Me2ViSiO1/2)0.15(PhSiO3/2)0.12(MeSiO3/2)0.73
組份(A-4):在參考實例4中製備且由以下平均單元式表示之有機聚矽氧烷樹脂:(Me2ViSiO1/2)0.15(PhSiO3/2)0.05(MeSiO3/2)0.80
組份(A-5):在參考實例5中製備且由以下平均單元式表示之有機聚矽氧烷樹脂:(Me2ViSiO1/2)0.15(Me3SiO1/2)0.10(PhSiO3/2)0.22(MeSiO3/2)0.53
組份(A-6):具有1,300之數量平均分子量及1.54之折射率且由以下平均單元式表示之有機聚矽氧烷樹脂:(Me2ViSiO1/2)0.2(PhSiO3/2)0.8
組份(A-7):具有1,100之數量平均分子量及1.54之折射率且由以
下平均單元式表示之有機聚矽氧烷樹脂:(Me2ViSiO1/2)0.25(PhSiO3/2)0.75
組份(A-8):在參考實例6中製備且由以下平均單元式表示之有機聚矽氧烷樹脂:(MePhViSiO1/2)0.228(PhSiO3/2)0.388(MeSiO3/2)0.384
組份(A-9):在參考實例7中製備且由以下平均單元式表示之有機聚矽氧烷樹脂:(MePhViSiO1/2)0.235(PhSiO3/2)0.539(MeSiO3/2)0.226
使用以下組份作為組份(B)。
組份(B-1):在參考實例8中製備且由下式表示之有機聚矽氧烷:Ph2ViSiO(Me2SiO)12Siph2Vi
組份(B-2):具有3,000mPa.s之黏度且由下式表示之兩個分子端經二甲基乙烯基矽氧基封端之甲基苯基聚矽氧烷:Me2ViSiO(MePhSiO)25SiMe2Vi
使用以下組份作為組份(C)。
組份(C-1):具有4mPa.s之黏度且由下式表示之有機三矽氧烷:HMe2SiOPh2SiOSiMe2H
組份(C-2):具有30mPa.s之黏度且由以下平均單元式表示之聚矽氧樹脂:(Me2HSiO1/2)0.6(PhSiO3/2)0.4
使用以下組份作為組份(D)。
組份(D-1):鉑-1,3-二乙烯基-1,1,3,3-四甲基二矽氧烷錯合物於1,3,5,7-四甲基-1,3,5,7-四乙烯基環四矽氧烷中之溶液(該溶液含有0.1質量%之鉑)
使用以下組份作為組份(E)。
組份(E-1):1-乙炔基環己醇
使用以下組份作為組份(F)。
組份(F-1):在參考實例9製備之黏著賦予劑
組份(F-2):黏著賦予劑,其具有在25℃下30mPa.s之黏度且含有3-縮水甘油氧基丙基三甲氧基矽烷及兩個分子端經矽醇基團封端之甲基乙烯基矽氧烷寡聚物之縮合反應產物
使用以下組份作為組份(G)。
組份(G-1):平均粒徑為13μm之鋁酸鹽型發綠光螢光物質
組份(G-2):平均粒徑為15μm之氮化物型發紅光螢光物質
根據表1中顯示之結果,確認在實踐實例1至6中製備之可固化聚矽氧組合物可阻抑裂紋,且與在比較實例1中製備之可固化聚矽氧組合物相比具有優異伸長率。
使用上文所列示之組份根據表2中所顯示之組成(質量份數)製備可固化聚矽氧組合物。應注意,在表2中,組份(D)之含量係根據鉑金屬相對於可固化聚矽氧組合物之含量(ppm,以質量單位計)來表示。表2中之H/Vi表示組份(C)中之矽原子鍵結氫原子相對於組份(A)及組份(B)中之總共1mol乙烯基的莫耳數。
本發明之可固化聚矽氧組合物可用作黏著劑、灌封劑、保護劑、塗覆劑或底部填充劑以供電/電子應用。具體而言,可固化聚矽氧組合物具有高反應性且可形成具有低透氣度之固化產品,因此該組合物適於作為光學半導體裝置(例如發光二極體(LED)或諸如此類)中之光學半導體元件之保護性塗層材料或密封劑。
Claims (8)
- 一種可固化聚矽氧組合物,其包括:(A)由以下平均單元式表示之有機聚矽氧烷:(R1 3SiO1/2)a(R2SiO3/2)c(R3SiO3/2)d其中,R1係相同或不同的具有1至12個碳之烷基、具有2至12個碳之烯基、具有6至20個碳之芳基或具有7至20個碳之芳烷基,限制條件係分子中之至少兩個R1為該等烯基;R2係具有6至20個碳之芳基或具有7至20個碳之芳烷基;R3係具有1至12個碳之烷基;且a、c及d分別係滿足以下條件之數值:0.01 a 0.5,0.01 c<0.7,0.1 d<0.9,且a+c+d=1;(B)分子中具有至少兩個矽鍵結烯基及至少一個矽鍵結芳基之直鏈有機聚矽氧烷,其量為0.1至150質量份數/100質量份數組份(A);(C)分子中具有至少兩個矽鍵結氫原子之有機聚矽氧烷,其量係使組份(C)中矽鍵結氫原子之量為組份(A)及(B)中之每1mol總烯基0.1mol至5mol;及(D)加速本發明組合物固化之量之矽氫化反應觸媒。
- 如請求項1之可固化聚矽氧組合物,其中組份(A)中之R2係苯基。
- 如請求項1或2之可固化聚矽氧組合物,其中組份(A)中之R3係甲基。
- 如請求項1之可固化聚矽氧組合物,其進一步包括(E)矽氫化反應抑制劑,其量為0.01至3質量份數/總共100質量份數之組份(A)至(C)。
- 如請求項1或5之可固化聚矽氧組合物,其進一步包括(F)助黏劑,其量為0.1至3質量份數/總共100質量份數之組份(A)至(C)。
- 一種固化產品,其係藉由固化如請求項1至6中任一項之可固化聚矽氧組合物來製造。
- 一種光學半導體裝置,其包括經如請求項1至6中任一項之可固化聚矽氧組合物之固化產品密封的光學半導體元件。
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