TW201402656A - 可硬化性聚矽氧組合物、其硬化產品及光半導體裝置 - Google Patents
可硬化性聚矽氧組合物、其硬化產品及光半導體裝置 Download PDFInfo
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
- H01L23/293—Organic, e.g. plastic
- H01L23/296—Organo-silicon compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/52—Encapsulations
- H01L33/56—Materials, e.g. epoxy or silicone resin
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Abstract
本發明係關於一種可硬化性聚矽氧組合物,其包含:(A)(A1)一分子中具有至少兩個烯基且不含矽鍵接型羥基及矽鍵接型氫原子之有機聚矽氧烷,或該組分(A1)及(A2)由平均單元化學式表示之分支鏈有機聚矽氧烷之混合物;(B)一分子中具有至少兩個矽鍵接型氫原子之有機聚矽氧烷;(C)由通式表示之二有機二烷氧基矽烷;(D)一分子中具有至少一個矽鍵接型羥基且不含矽鍵接型氫原子之直鏈有機矽氧烷寡聚物;及(E)矽氫化觸媒,該組合物可形成顯示極佳初始黏著性及透明度且於高溫及高濕度條件下顯示極佳黏著耐久性及透明度保持性之硬化產品。
Description
本發明主張2012年3月30日申請之日本專利申請案第2012-079251號之優先權,該案之內容以引用之方式併入本文中。
本發明係關於一種可硬化性聚矽氧組合物、其硬化產品及使用該硬化產品之光半導體裝置。
矽氫化反應可硬化性組合物形成具有極佳性質(例如耐候性及耐熱性)之硬化產品,且因此係用於各種應用。然而,該等組合物顯示不良黏著性。因此,已提出包含黏著性賦予劑之可硬化性聚矽氧組合物。例如,日本未審查專利申請公開案第2008-528788號提出一種可硬化性聚矽氧組合物,其包含丙烯醯氧基官能性烷氧基矽烷或甲基丙烯醯氧基官能性烷氧基矽烷、烯基官能性矽烷醇封端型有機聚矽氧烷及環氧官能性烷氧基矽烷;且日本未審查專利申請公開案第2010-248384號提出一種可硬化性聚矽氧組合物,其包含一分子中具有兩個直接鍵接至矽原子之烷氧基之矽烷偶合劑及至少一種選自硼偶合劑、鈦偶合劑、鋁偶合劑及鋯偶合劑之偶合劑。
日本未審查專利申請公開案第2008-528788號中所提出之可硬化性聚矽氧組合物係關於一種合成纖維材料用塗覆組合物且其未指示或指出可藉由使特定烷氧基矽烷與烯基官能性矽烷醇封端型有機聚矽氧
烷組合來解決自該組合物獲得之硬化產品於高溫及高濕度條件下顯示隨時間降低之黏著性及透明度之問題。
另外,日本未審查專利申請公開案第2010-248384號中所提出之可硬化性聚矽氧組合物具有自該組合物獲得之硬化產品於高溫及高濕度條件下顯示隨時間降低之黏著性及透明度之問題。因此,使用該組合物作為光半導體元件之密封劑或黏著劑會導致光半導體裝置之可靠性於高溫及高濕度條件下顯著降低之問題。
本發明之一目標係欲提供一種可硬化性聚矽氧組合物,其形成顯示極佳初始黏著性及透明度且於高溫及高濕度條件下顯示極佳黏著耐久性及透明度保持性之硬化產品。本發明之另一目標係欲提供此種硬化產品。本發明之另一目標係欲提供使用此種硬化產品之具有極佳可靠性之光半導體裝置。
本發明之可硬化性聚矽氧組合物包含:(A)100質量份(A1)一分子中具有至少兩個烯基且不含矽鍵接型羥基及矽鍵接型氫原子之有機聚矽氧烷,或該組分(A1)及(A2)由以下平均單元化學式表示之分支鏈有機聚矽氧烷之混合物:(R1 2R2SiO1/2)a(R1 3SiO1/2)b(SiO4/2)c(HO1/2)d
其中R1係相同或不同之具有1至10個碳之烷基;R2係烯基;且「a」、「b」、「c」及「d」均係滿足以下條件之正數:a+b+c=1;a/(a+b)=0.15至0.35;c/(a+b+c)=0.53至0.62;及d/(a+b+c)=0.005至0.03;(B)一分子中具有至少兩個矽鍵接型氫原子之有機聚矽氧烷,其含量為相對於組分(A)中之每1莫耳烯基,在此組分中提供0.1至10莫耳矽鍵接型氫原子;(C)0.01至10質量份由以下通式表示之二有機二烷氧基矽烷;
R3R4Si(OR5)2
其中R3係縮水甘油氧基烷基、環氧環己基烷基、環氧烷基、丙烯醯氧基烷基或甲基丙烯醯氧基烷基;R4係具有1至6個碳之烷基;且R5係具有1至4個碳之烷基;(D)0.01至10質量份一分子中具有至少一個矽鍵接型羥基且不含矽鍵接型氫原子之直鏈有機矽氧烷寡聚物;及(E)催化量的矽氫化觸媒。
此外,藉由使上述組合物硬化來獲得本發明之硬化產品。
另外,本發明之光半導體裝置包含:光半導體元件;及藉由使上述可硬化性聚矽氧組合物硬化而獲得且密封或黏結該元件之硬化產品。
本發明之可硬化性聚矽氧組合物形成顯示極佳初始黏著性及透明度且於高溫及高濕度條件下顯示極佳黏著耐久性及透明度保持性之硬化產品。另外,本發明之硬化產品顯示極佳初始黏著性及透明度且於高溫及高濕度條件下顯示極佳黏著耐久性及透明度保持性。此外,本發明之光半導體裝置顯示極佳可靠性。
1‧‧‧聚鄰苯二甲醯胺(PPA)樹脂外殼
2‧‧‧內引線
3‧‧‧晶粒座
4‧‧‧黏著材料
5‧‧‧發光二極體(LED)晶片
6‧‧‧接線
7‧‧‧密封材料
圖1係本發明光半導體裝置之一實例LED之橫截面視圖。
首先,將詳細闡釋本發明之可硬化性聚矽氧組合物。
組分(A)係本發明組合物中之主要組分且係(A1)一分子中具有至少兩個烯基且不含矽鍵接型羥基及矽鍵接型氫原子之有機聚矽氧烷,或該組分(A1)及(A2)由以下平均單元化學式表示之分支鏈有機聚矽氧烷之混合物:(R1 2R2SiO1/2)a(R1 3SiO1/2)b(SiO4/2)c(HO1/2)d
組分(A1)中之烯基之實例包括乙烯基、烯丙基、異丙烯基、丁烯基、己烯基及環己烯基,其中以乙烯基較佳。組分(A1)中除烯基以外之矽鍵接型有機基團之實例包括:烷基,例如甲基、乙基、丙基、丁基、戊基、己基、環戊基或環己基;芳基,例如苯基、甲苯基或二甲苯基;芳烷基,例如苄基或苯乙基;或鹵代烷基,例如3-氯丙基或3,3,3-三氟丙基,其中以甲基或苯基較佳。組分(A1)於25℃下之黏度係不受限制,但較佳係10至10,000,000mPa.s,且更佳係50至1,000,000mPa.s。組分(A1)之分子結構係不受限制,且可係直鏈、部分分支型直鏈或分支鏈,其中以直鏈較佳。
此種組分(A1)之實例包括分子末端均經二甲基乙烯基矽氧基封端之二甲基聚矽氧烷、分子末端均經二甲基乙烯基矽氧基封端之二甲基矽氧烷與甲基乙烯基矽氧烷之共聚物、分子末端均經二甲基乙烯基矽氧基封端之二甲基矽氧烷與甲基苯基矽氧烷之共聚物、分子末端均經三甲基矽氧基封端之甲基乙烯基聚矽氧烷、分子末端均經三甲基矽氧基封端之二甲基矽氧烷與甲基乙烯基矽氧烷之共聚物或此等中之兩者或更多者之混合物。
組分(A2)係用於賦予本發明組合物之硬化產品適當硬度及機械強度之可選組分,且係由以下平均單元化學式表示:(R1 2R2SiO1/2)a(R1 3SiO1/2)b(SiO4/2)c(HO1/2)d
在該式中,R1係相同或不同之具有1至10個碳原子之烷基,其特定實例包括甲基、乙基、丙基、丁基、戊基、己基、環戊基及環己基,其中以甲基較佳。在該式中,R2係烯基,其實例包括乙烯基、烯丙基、異丙烯基、丁烯基、己烯基及環己烯基,其中以乙烯基較佳。在該式中,「a」、「b」、「c」及「d」均係滿足以下條件之正數:a+b+c=1;a/(a+b)=0.15至0.35;c/(a+b+c)=0.53至0.62;及d/(a+b+c)=0.005至0.03。為賦予本發明組合物令人滿意之可硬化性,
a/(a+b)的值較佳係0.2至0.3。為賦予本發明組合物之硬化產品令人滿意之硬度及機械強度,c/(a+b+c)的值較佳係0.55至0.60。為賦予本發明組合物之硬化產品令人滿意之黏著性及機械強度,d/(a+b+c)的值較佳係0.01至0.025。
組分(A2)係可選組分,但為使組分(A2)賦予本發明組合物之硬化產品令人滿意之硬度及機械強度,組分(A)較佳係組分(A1)及組分(A2)之混合物。為使本發明組合物顯示良好的可處理性,組分(A2)於組分(A)中之含量較佳係60質量%或更少,且更佳係15至60質量%。
組分(B)係用於使本發明組合物硬化,且係一分子中具有至少兩個矽鍵接型氫原子之有機聚矽氧烷。組分(B)中之矽鍵接型有機基團之實例包括:烷基,例如甲基、乙基、丙基、丁基、戊基、己基、環戊基或環己基;芳基,例如苯基、甲苯基或二甲苯基;芳烷基,例如苄基或苯乙基;或鹵代烷基,例如3-氯丙基或3,3,3-三氟丙基,其中以甲基或苯基較佳。組分(B)於25℃下之黏度係不受限制,但較佳係1至10,000mPa.s,且更佳係5至1,000mPa.s。組分(B)之分子結構係不受限制,且可係直鏈、部分分支型直鏈、環狀或分支鏈,其中以直鏈較佳。
此種組分(B)之實例包括分子末端均經二甲基氫矽氧基封端之二甲基聚矽氧烷;分子末端均經二甲基氫矽氧基封端之二甲基矽氧烷與甲基氫矽氧烷之共聚物;分子末端均經三甲基矽氧基封端之甲基氫聚矽氧烷;分子末端均經三甲基矽氧基封端之二甲基矽氧烷與甲基氫矽氧烷之共聚物;包含SiO4/2單元及(CH3)2HSiO1/2單元之有機聚矽氧烷;包含SiO4/2單元、(CH3)2HSiO1/2單元及(CH3)3SiO1/2單元之有機聚矽氧烷;及此等中之兩者或更多者之混合物。
組分(B)之含量係相對於組分(A)中之每1莫耳烯基在此組分中提供0.1至10莫耳及較佳0.5至5莫耳矽鍵接型氫原子之量。此係因為:若
組分(B)之含量不低於上述範圍之下限,則本發明組合物之可硬化性係經改良,且若組分(B)之含量不高於上述範圍之上限,則藉由使本發明組合物硬化所獲得之硬化產品之機械性質及耐熱性係經改良。
組分(C)係用於改善本發明組合物之黏著性,且係由以下通式表示之二有機二烷氧基矽烷:R3R4Si(OR5)2
在此式中,R3係縮水甘油氧基烷基,例如3-縮水甘油氧基丙基或4-縮水甘油氧基丁基;環氧環己基烷基,例如2-(3,4-環氧環己基)乙基或3-(3,4-環氧環己基)丙基;環氧烷基,例如5,6-環氧己基或9,10-環氧癸基;丙烯醯氧基烷基,例如3-丙烯醯氧基丙基或4-丙烯醯氧基丁基;或甲基丙烯醯氧基烷基,例如3-甲基丙烯醯氧基丙基或4-甲基丙烯醯氧基丁基。在此式中,R4係具有1至6個碳原子之烷基,其實例包括甲基、乙基、丙基、丁基、戊基及己基,其中以甲基較佳。在此式中,R5係具有1至4個碳原子之烷基,其實例包括甲基、乙基、丙基及丁基,其中以甲基或乙基較佳。
此種組分(C)之實例包括3-縮水甘油氧基丙基甲基二甲氧基矽烷、3-縮水甘油氧基丙基甲基二乙氧基矽烷、2-(3,4-環氧環己基)乙基甲基二甲氧基矽烷、2-(3,4-環氧環己基)乙基甲基二乙氧基矽烷、5,6-環氧己基甲基二甲氧基矽烷、5,6-環氧己基甲基二乙氧基矽烷、3-丙烯醯氧基丙基甲基二甲氧基矽烷、3-丙烯醯氧基丙基甲基二乙氧基矽烷、3-甲基丙烯醯氧基丙基甲基二甲氧基矽烷及3-甲基丙烯醯氧基丙基甲基二乙氧基矽烷。
每100質量份組分(A)中組分(C)之含量係0.01至10質量份(且較佳0.1至10質量份)。此係因為:若組分(C)之含量不低於上述範圍之下限,則藉由使本發明組合物硬化所獲得之硬化產品之黏著性係提高,且若組分(C)之含量不高於上述範圍之上限,則本發明組合物之儲存
安定性係提高。
組分(D)係有助於維持藉由使本發明組合物硬化所獲得之硬化產品之透明度及黏著性之組分,且係一分子中具有至少一個矽鍵接型羥基(即矽烷醇基)且不含矽鍵接型氫原子之直鏈有機矽氧烷寡聚物。組分(D)中之矽鍵接型有機基團之實例包括:烷基,例如甲基、乙基、丙基、丁基、戊基、己基、環戊基或環己基;烯基,例如乙烯基、烯丙基、異丙烯基、丁烯基、己烯基或環己烯基;芳基,例如苯基、甲苯基或二甲苯基;芳烷基,例如苄基或苯乙基;或鹵代烷基,例如3-氯丙基或3,3,3-三氟丙基;其中以甲基或乙烯基較佳。此外,一分子中組分(D)較佳具有至少一個烯基。組分(D)於25℃下之黏度係不受限制,但較佳係1至100mPa.s且更佳係1至50mPa.s。
此種組分(D)之實例包括分子末端均經矽烷醇基封端之二甲基矽氧烷與甲基乙烯基矽氧烷之共聚物寡聚物、分子末端均經矽烷醇基封端之甲基乙烯基矽氧烷寡聚物及分子末端均經矽烷醇基封端之二甲基矽氧烷寡聚物。
每100質量份組分(A)中組分(D)之含量係0.01至10質量份(且較佳0.1至10質量份)。此係因為:若組分(D)之含量不低於上述範圍之下限,則可維持藉由使本發明組合物硬化所獲得之硬化產品之良好透明度,且若組分(D)之含量不高於上述範圍之上限,則可維持藉由使本發明組合物硬化所獲得之硬化產品之良好黏著性。
組分(E)係用於加速本發明組合物硬化之矽氫化觸媒。此種組分(E)之實例包括鉑基觸媒、銠基觸媒及鈀基觸媒,其中以鉑基觸媒較佳,因為其可顯著加速本發明組合物之硬化。鉑基觸媒之實例包括鉑細粉、氯鉑酸、氯鉑酸之醇溶液、鉑-烯基矽氧烷錯合物、鉑-烯烴錯合物及鉑-羰基錯合物,其中以鉑-烯基矽氧烷錯合物特別佳。該烯基矽氧烷之實例包括1,3-二乙烯基-1,1,3,3-四甲基二矽氧烷及1,3,5,7-四
甲基-1,3,5,7-四乙烯基環四矽氧烷。為使該鉑-烯基矽氧烷錯合物顯示良好安定性,以使用1,3-二乙烯基-1,1,3,3-四甲基二矽氧烷特別佳。另外,為了能夠提高該鉑-烯基矽氧烷錯合物之安定性,較佳地,將烯基矽氧烷(例如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或1,3,5,7-四甲基-1,3,5,7-四乙烯基環四矽氧烷)或有機矽氧烷寡聚物(例如二甲基矽氧烷寡聚物)且尤其係烯基矽氧烷添加至該錯合物中。
組分(E)之含量係催化量且係不受特定限制,只要所用量可加速本發明組合物之硬化即可,但其含量較佳係使得此組分中之金屬原子含量相對於本發明組合物為0.01至500ppm及更佳0.01至50ppm(以質量單位計)。此係因為:若組分(E)之含量不低於上述範圍之下限,則可使本發明組合物令人滿意地硬化,且若組分(E)之含量不高於上述範圍之上限,則藉由使本發明組合物硬化所獲得之硬化產品之透明度係提高。
可將反應抑制劑(例如:炔醇,例如2-甲基-3-丁炔-2-醇、3,5-二甲基-1-己炔-3-醇或2-苯基-3-丁炔-2-醇;烯炔化合物,例如3-甲基-3-戊烯-1-炔或3,5-二甲基-3-己烯-1-炔;或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或苯并三唑)作為可選組分併入本發明組合物中。該反應抑制劑之含量係不受限制,但較佳每100質量份組分(A)中係0.0001至5質量份。
另外,可將有機鈦化合物(例如,異丙醇鈦、異丁醇鈦、二異丙氧基雙(2,4-戊二酸)鈦、二異丙氧基雙(四甲基庚二酸)鈦或二異丙氧基雙(乙基乙醯乙酸)鈦)、有機鋁化合物(例如,乙醯丙酮酸鋁、二第二丁氧基乙基乙醯乙酸鋁或二異丙氧基乙基乙醯乙酸鋁)、有機鋯化合物(例如,正丁醇鋯、二正丁氧基雙(2,4-戊二酸)鋯或2,4-戊二酸鋯)或有機金屬化合物(例如2,4-戊二酸鐵、四甲基庚二酸鐵或其他有機鐵
化合物)併入本發明組合物中以改善其黏著性。每100質量份組分(A)中該有機金屬化合物之含量較佳係0.0001至1質量份。
可將無機填充劑(例如矽石、玻璃、氧化鋁或氧化鋅)、聚甲基丙烯酸酯樹脂及類似物之有機樹脂細粉、耐熱劑、染料、顏料、阻燃劑、溶劑及類似物作為可選組分以不損害本發明目標之濃度併入本發明組合物中。
本發明組合物係於室溫或加熱下發生硬化,但較佳地,加熱該組合物以實現快速硬化。該加熱溫度較佳係50至200℃。
本發明之硬化產品係藉由使上述組合物硬化而獲得,且其硬度不受限制,但於JIS K 6253中指定之A型硬度計硬度較佳係20至99且更佳係30至95。此係因為:若該硬化產品之硬度不低於上述範圍之下限,則該硬化產品之表面黏性係較低且可抑制硬化產品之間的黏著及污垢之附著,且若該硬化產品之硬度不高於上述範圍之上限,則該硬化產品中幾乎不發生破裂。
該硬化產品於高溫及高濕度條件下顯示極佳的透明度保持性,但在使用上述組合物作為光半導體元件之密封劑或黏著劑之情況下亦提高該光半導體裝置之可靠性,且該硬化產品較佳具有90%或更高且更佳95%或更高的透光率變化率[(T2/T1)×100],其中T1(%)係該硬化產品於25℃及450nm波長下之初始透光率(光程長度:1.0mm)且T2(%)係前述硬化產品於85℃溫度及85%相對濕度下曝露1,000小時後之透光率。
另外,該硬化產品於高溫及高濕度條件下顯示極佳的黏著耐久性,但在使用上述組合物作為光半導體元件之密封劑或黏著劑之情況下亦提高該光半導體裝置之可靠性,且該硬化產品較佳具有80%或更高且更佳90%或更高的黏著強度變化率[(S2/S1)×100],其中S1(%)係該硬化產品於25℃下對聚鄰苯二甲醯胺(PPA)薄片之初始黏著強度且
S2(%)係該硬化產品於85℃溫度及85%相對濕度下曝露1,000小時後之黏著強度。
現將詳細闡釋本發明之光半導體裝置。
本發明之光半導體裝置包含光半導體元件及藉由使上述可硬化性聚矽氧組合物硬化獲得且密封或黏結該元件之硬化產品。該光半導體元件之實例包括發光二極體(LED)、半導體雷射器、光二極體、光電晶體、固態成像裝置及用於光耦合器之光發射體及光受體,其中以發光二極體(LED)較佳。
在發光二極體(LED)裝置中,因為發光二極體(LED)以垂直及水平方式發光,因此不希望該光半導體裝置之構成組件吸收光,且選擇具有高透光率或高反射率之材料。此係亦適用於其上安裝有光半導體元件上之基板。該基板之實例包括:導電金屬,例如銀、金或銅;非導電金屬,例如鋁或鎳;含白色顏料之熱塑性樹脂,例如PPA或LCP;含白色顏料之熱固性樹脂,例如環氧樹脂、BT樹脂、聚醯亞胺樹脂或聚矽氧樹脂;或陶瓷,例如氧化鋁或氮氧化鋁。本發明之光半導體裝置使用上述組合物,且因此在光半導體元件與基板之間顯示極佳黏著性且可提高該光半導體裝置之可靠性。
現將藉由圖1來闡釋本發明之光半導體裝置。圖1係獨立表面安裝型發光二極體(LED)裝置(其係光半導體裝置之一典型實例)之橫截面視圖。圖1中所示之發光二極體(LED)裝置係其中發光二極體(LED)晶片(5)係經由黏著材料(4)晶粒接合至聚鄰苯二甲醯胺(PPA)樹脂外殼(1)內部之晶粒座(3)上之裝置。發光二極體(LED)晶片(5)及內引線(2)係藉由接線(6)打線接合並藉由密封材料(7)密封至該外殼之內壁。在該光半導體裝置中,形成該密封材料(7)之組合物係上述組合物。
實例
現將使用實例闡釋本發明之可硬化性聚矽氧組合物、其硬化產
品及光半導體裝置。此外,該等物理性質值係於25℃下測得的值且如下測量該硬化產品之性質。
[硬化產品之硬度]
藉由於150℃下加熱該可硬化性聚矽氧組合物1小時來製備硬化產品。使用JIS K 6253中指定之A型硬度計測量該硬化產品之硬度。
隨後,使該硬化產品於85℃的溫度及85%相對濕度下曝露1,000小時。以如上所述之相同方式測量該硬化產品在於高溫及高濕度條件下經處理後之硬度。
[硬化產品之透光率]
藉由於150℃下加熱該可硬化性聚矽氧組合物1小時來製備具有1.0mm光程長度之硬化產品。測量該硬化產品於450nm波長下之透光率。
隨後,使該硬化產品於85℃的溫度及85%相對濕度下曝露1,000小時。以如上所述之相同方式測量該硬化產品在於高溫及高濕度條件下經處理後之透光率。
[硬化產品之黏著強度]
將聚四氟乙烯樹脂間隔物(寬度:10mm,長度:20mm,厚度:1mm)插入兩個聚鄰苯二甲醯胺(PPA)樹脂片(寬度:25mm,長度:50mm,厚度:1mm)之間,用該可硬化性聚矽氧組合物填充此間隙,使用夾具夾緊該等薄片,且隨後藉由於150℃的內部空氣循環型烘箱中加熱1小時使上述組合物硬化。在冷卻至室溫後,藉由使用拉伸測試儀以水平相反方向牽拉樣品(藉由移除該夾具及間隔物所獲得)來測量該硬化產品之黏著強度。
另外,隨後使上述樣品於85℃溫度及85%相對濕度下曝露1,000小時。以如上所述之相同方式,在於高溫及高濕度條件下進行處理後測量該樣品中該硬化產品之黏著強度。
[實例1至4及比較例1至5]
藉由以表1中所示之組成均勻混合以下組分來製備可硬化性聚矽氧組合物。其中,Vi表示乙烯基且Me表示甲基。在該表中,SiH/Vi表示:在該可硬化性聚矽氧組合物中,相對於組分(A-1)至(A-4)中之總計每1莫耳乙烯基,組分(B-1)至(B-2)中之矽鍵接型氫原子之總莫耳數;透光率變化率意指硬化產品於高溫及高濕度條件下經處理後之透光率相對於初始透光率之變化;且黏著強度變化率意指硬化產品於高溫及高濕度條件下經處理後之黏著強度相對於初始黏著強度之變化。
組分(A-1):分子末端均經二甲基乙烯基矽氧基封端之二甲基聚矽氧烷,其具有360mPa.s的黏度(乙烯基含量=0.44質量%);組分(A-2):分子末端均經二甲基乙烯基矽氧基封端之二甲基聚矽氧烷,其具有11.000mPa.s的黏度(乙烯基含量=0.14質量%);組分(A-3):有機聚矽氧烷樹脂,其於25℃下係白色固體,可溶於甲苯且係由以下平均單元化學式表示:(ViMe2SiO1/2)0.13(Me3SiO1/2)0.45(SiO4/2)0.42(HO1/2)0.01
(乙烯基含量=3.4質量%);組分(A-4):有機聚矽氧烷,其於25℃下係白色固體,可溶於甲苯且係由以下平均單元化學式表示:(ViMe2SiO1/2)0.15(Me3SiO1/2)0.38(SiO4/2)0.47(HO1/2)0.01
(乙烯基含量=4.2質量%);組分(B-1):分子末端均經三甲基矽氧基封端之二甲基矽氧烷與甲基氫矽氧烷之共聚物,其具有5mPa.s的黏度(矽鍵接型氫原子含量=1.4質量%);組分(B-2):分子末端均經三甲基矽氧基封端之聚甲基氫矽氧烷,其具有20mPa.s的黏度(矽鍵接型氫原子含量=1.57質量%);組分(C-1):3-縮水甘油氧基丙基三甲氧基矽烷;
組分(C-2):3-縮水甘油氧基丙基甲基二甲氧基矽烷;組分(C-3):3-縮水甘油氧基丙基甲基二乙氧基矽烷;組分(C-4):3-丙烯醯氧基丙基甲基二甲氧基矽烷;組分(D-1):分子末端均經矽鍵接型羥基封端之二甲基矽氧烷與甲基乙烯基矽氧烷之共聚物寡聚物,其具有40mPa.s的黏度;組分(E-1):1,3-二乙烯基四甲基二矽氧烷鉑錯合物之1,3-二乙烯基四甲基二矽氧烷溶液(鉑金屬含量=4.000ppm);組分(F-1):3,5-二甲基-1-辛炔-3-醇。
本發明之可硬化性聚矽氧組合物對金屬(例如鋼、不鏽鋼、鋁、銅、銀、鈦或鈦合金)、半導體元件(例如矽半導體、鎵磷基半導體、鎵砷基半導體或氮化鎵基半導體)、陶瓷材料、玻璃、熱固性樹脂、具有極性基團之熱塑性樹脂及類似物顯示極佳的初始黏著性及黏著耐久性,且其在經歷加熱及冷卻循環時顯示特別佳的黏著耐久性,且因此適用作光半導體元件(例如發光二極體(LED)、半導體雷射器、光二極體、光電晶體、固態成像裝置或用於光耦合器之光發射體及光受體)之密封劑或黏著劑。另外,本發明之光半導體裝置係適用作諸如光學裝置、光學設備、照明設備或照明裝置之光半導體裝置。
1‧‧‧聚鄰苯二甲醯胺(PPA)樹脂外殼
2‧‧‧內引線
3‧‧‧晶粒座
4‧‧‧黏著材料
5‧‧‧發光二極體(LED)晶片
6‧‧‧接線
7‧‧‧密封材料
Claims (6)
- 一種可硬化性聚矽氧組合物,其包含:(A)100質量份(A1)一分子中具有至少兩個烯基且不含矽鍵接型羥基及矽鍵接型氫原子之有機聚矽氧烷,或該組分(A1)及(A2)由以下平均單元化學式表示之分支鏈有機聚矽氧烷之混合物:(R1 2R2SiO1/2)a(R1 3SiO1/2)b(SiO4/2)c(HO1/2)d其中R1係相同或不同之具有1至10個碳原子之烷基;R2係烯基;且「a」、「b」、「c」及「d」均係滿足以下條件之正數:a+b+c=1;a/(a+b)=0.15至0.35;c/(a+b+c)=0.53至0.62;及d/(a+b+c)=0.005至0.03;(B)一分子中具有至少兩個矽鍵接型氫原子之有機聚矽氧烷,其含量為相對於組分(A)中之每1莫耳烯基,在此組分中提供0.1至10莫耳矽鍵接型氫原子;(C)0.01至10質量份由以下通式表示之二有機二烷氧基矽烷;R3R4Si(OR5)2其中R3係縮水甘油氧基烷基、環氧環己基烷基、環氧烷基、丙烯醯氧基烷基或甲基丙烯醯氧基烷基;R4係具有1至6個碳原子之烷基;且R5係具有1至4個碳原子之烷基;(D)0.01至10質量份一分子中具有至少一個矽鍵接型羥基且不含矽鍵接型氫原子之直鏈有機矽氧烷寡聚物;及(E)催化量的矽氫化觸媒。
- 如請求項1之可硬化性聚矽氧組合物,其中組分(A)係組分(A1)及組分(A2)之混合物,且組分(A2)於組分(A)中之含量係60質量%或更少。
- 如請求項1或2之可硬化性聚矽氧組合物,其係用於光半導體元 件之密封劑或黏著劑。
- 一種硬化產品,其係藉由使如請求項1或2中所述之可硬化性聚矽氧組合物固化所獲得。
- 一種光半導體裝置,其包含:光半導體元件;及如請求項1或2中所述之可硬化性聚矽氧組合物之硬化產品,其密封或黏結該元件。
- 如請求項5之光半導體裝置,其中該光半導體裝置係發光二極體。
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EP3087151B1 (en) | 2013-12-23 | 2017-11-22 | Dow Corning Corporation | Uv-curable silicone compositions and anti-dust coating compositions containing same |
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TWI688629B (zh) * | 2015-03-05 | 2020-03-21 | 日商陶氏東麗股份有限公司 | 聚矽氧系感壓接著劑及具有聚矽氧系感壓接著層之積層體 |
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