TWI719968B - 聚矽氧材料、可固化性聚矽氧組合物,及光學裝置 - Google Patents
聚矽氧材料、可固化性聚矽氧組合物,及光學裝置 Download PDFInfo
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- TWI719968B TWI719968B TW105108131A TW105108131A TWI719968B TW I719968 B TWI719968 B TW I719968B TW 105108131 A TW105108131 A TW 105108131A TW 105108131 A TW105108131 A TW 105108131A TW I719968 B TWI719968 B TW I719968B
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- C08L—COMPOSITIONS OF MACROMOLECULAR 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
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L83/02—Polysilicates
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- C09D183/00—Coating compositions 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; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
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- C08G77/12—Polysiloxanes containing silicon bound to hydrogen
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- C—CHEMISTRY; METALLURGY
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- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- C—CHEMISTRY; METALLURGY
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Abstract
本發明係關於聚矽氧材料,其根據X-射線光電子光譜法(ESCA)滿足以該聚矽氧材料表面之元素組成百分比表示之以下條件中之任一者:(i)碳原子之元素組成百分比係50.0原子%至70.0原子%;(ii)碳原子之元素組成百分比對矽原子之元素組成百分比之比率(C/Si)係2.0至5.0;或(iii)以上條件(i)及(ii)二者。該聚矽氧材料對光及熱穩定,其不易於發生透射率之下降及裂紋之產生。
Description
本發明係關於聚矽氧材料、用於形成該聚矽氧材料之可固化性聚矽氧組合物,及含有該聚矽氧材料之光學裝置。
聚矽氧材料由於其極佳透明度、耐熱性及耐氣候性而用作發光二極體(LED)之透鏡材料或密封材料(參見專利文件1)。
然而,最近隨著LED之亮度增加,已發現,儘管其係聚矽氧材料,亦發生諸如透明度下降及產生裂紋等問題。
專利文件1:日本未審查專利申請公開案第2002-314139號
本發明之目的係提供對光及熱穩定之聚矽氧材料,其不易於發生透射率之下降及裂紋。本發明之其他目的係提供形成此一聚矽氧材料之可固化性聚矽氧組合物,及提供使用此一聚矽氧材料之具有極佳可靠性之光學裝置。
本發明之聚矽氧材料具有根據X-射線光電子光譜法(ESCA)滿足
以聚矽氧材料表面之元素組成百分比表示之以下條件之任一者之特性:(i)碳原子之元素組成百分比係50.0原子%至70.0原子%;(ii)碳原子之元素組成百分比對矽原子之元素組成百分比之比率(C/Si)係2.0至5.0;或(iii)以上條件(i)及(ii)二者。
此聚矽氧材料較佳在其結構中含有Si-R1-Si鍵(其中,R1係伸烷基或伸芳基),且此聚矽氧材料較佳係光學材料、具體而言光學元件之密封材料。
本發明之可固化性聚矽氧組合物具有固化以形成此一上述聚矽氧材料之特性,且係包含以下各項之組合物:分子中具有至少兩個矽鍵結之烯基及至少一個矽鍵結之芳基之有機聚矽氧烷;分子中具有至少兩個矽鍵結之氫原子之有機聚矽氧烷;及矽氫化反應觸媒。
本發明之光學裝置之特性在於其係藉由利用上文之聚矽氧材料密封光學元件而形成,且較佳地上文光學元件係LED。
本發明之聚矽氧材料具有對光及熱穩定之特性,且不易於發生透射率之下降及裂紋之產生。此外,本發明之聚矽氧組合物具有形成此一聚矽氧材料之特性。另外,本發明之光學裝置之特徵為具有極佳可靠性。
1‧‧‧基板/COB基板
2‧‧‧LED
3‧‧‧聚矽氧材料
4‧‧‧引線框
4'‧‧‧引線框
5‧‧‧接合線
6‧‧‧光反射材料
圖1係為本發明光學裝置之實例之板上晶片封裝(COB)LED裝置之剖視圖。
圖2係為本發明光學裝置之實例之另一LED裝置之剖視圖。
本發明之聚矽氧材料具有根據X-射線光電子光譜法(ESCA)滿足以聚矽氧材料表面之元素組成百分比表示之以下條件之任一者之特性:(i)碳原子之元素組成百分比係50.0原子%至70.0原子%;(ii)碳原子之元素組成百分比對矽原子之元素組成百分比之比率(C/Si)係2.0至5.0;或(iii)以上條件(i)及(ii)二者。
根據X-射線光電子光譜法(ESCA),在聚矽氧材料表面之原子組成百分比中碳原子之比例係50.0原子%至70.0原子%、且較佳60.0原子%至68.0原子%。此係由於當碳原子之比例不小於上文所給出範圍之最小值時,聚矽氧材料對光及熱穩定且不易於發生聚矽氧材料之透光率之下降,且可製造高度耐久的LED裝置。另一方面,當其不大於上文所給出範圍之最大值時,在聚矽氧材料中不易於發生裂紋之產生,且可製造高度耐久的LED裝置。
此外,根據聚矽氧材料表面之X-射線光電子光譜法(ESCA),在原子組成百分比中碳原子之元素組成百分比對矽原子之元素組成百分比之比率(C/Si)係2.0至5.0、且較佳3.0至4.5。此係由於,若該比率(C/Si)不小於上文所給出範圍之最小值,則可因所賦予之高韌性而阻抑裂紋之產生,且另一方面,若其不大於上文所給出範圍之最大值,則可阻抑因光及熱所致之組合物降解。
此外,聚矽氧材料較佳在其結構中具有Si-R1-Si鍵。此係由於,具有此一鍵之聚矽氧材料可減輕因光及熱所致之降解以及當LED重複接通及切斷時發生因內部壓力所致之損害。
在式中,R1係伸烷基或伸芳基。伸烷基之實例包括具有2至12個碳之伸烷基,例如甲基亞甲基、伸乙基、伸丙基、甲基伸乙基、伸丁基及伸異丁基。伸芳基之實例包括具有6至12個碳之伸芳基,例如伸
苯基、伸甲苯基、伸二甲苯基及伸萘基。
本發明此一聚矽氧材料之形狀並無具體限制,且實例包括片形、膜形、纖維形、板形、球形、半球形、凸透鏡形、凹透鏡形狀菲涅耳(Fresnel)透鏡形狀圓柱形及圓筒形。本發明之聚矽氧材料可單獨存在,但其(例如)亦可用作光學裝置中發光元件之密封材料、黏著材料或覆蓋材料,且亦可用作光學裝置中之透鏡或太陽能電池中之保護材料或聚光透鏡。
形成本發明聚矽氧材料之可固化性聚矽氧組合物之固化機制並無具體限制,且實例包括加成反應、縮合反應及自由基反應。加成反應係較佳的。
藉由加成反應固化之可固化性聚矽氧組合物包含:在分子中具有至少兩個矽鍵結之烯基及至少一個矽鍵結之芳基之有機聚矽氧烷;在分子中具有至少兩個矽鍵結之氫原子之有機聚矽氧烷;及矽氫化反應觸媒。
作為此一可固化性聚矽氧組合物,包含以下者較佳:(A)藉由平均組成式所表示之有機聚矽氧烷:R2 aSiO[(4-a)/2]
其中,R2各自獨立地係具有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,其中烯基佔所有R2之1mol%至20mol%,芳基佔所有R2之至多40mol%,且「a」係滿足關係式1a<2之數值;(B)在分子中具有至少兩個矽鍵結之氫原子之有機聚矽氧烷,其量使得此組份中矽鍵結之氫原子之量為組份(A)中之每1莫耳總烯基0.1莫耳至5莫耳;及(C)矽氫化反應觸媒,其量使得加速本發明組合物之固化。
組份(A)係本發明組合物之主要組份且係由平均組成式表示之有機聚矽氧烷:R2 aSiO[(4-a)/2]。
在該式中,R2各自獨立地係具有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。特定實例包括烷基,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,例如萘基乙基、萘基丙基、蒽基乙基、菲基乙基及芘基乙基;及其中該等芳基或芳烷基之氫原子經烷基(例如甲基或乙基)、烷氧基(例如甲氧基或乙氧基)或鹵素原子(例如氯原子或溴原子)取代之基團。此外,在上式中,所有R2之1mol%至20mol%、較佳1mol%至15mol%或2mol%至15mol%係以上之烯基。此係由於當烯基之含量不小於上文所給出範圍之最小值時,本發明組合物滿意地固化,且另一方面,當烯基之含量不大於上文所給出範圍之最大值時,藉由固化本發明組合物所獲得之固化產物之物理性質良好。此外,所有R2之至多40mol%、較佳至多35mol%或至多30mol%係上文之芳基,且另一方面,所有R2之至少1mol%、至少5mol%或至少10mol%係上文之芳基。此係由於,當芳基之含量不大於上文所給出範圍之最大值時,藉由固化本發明組合物所獲得之固化產物之耐熱性良好且可改良其中利用本發明組合物密封之光學元件之光學裝置之可靠性。另一方面,當芳基之含量不小於上文所給出範圍之最大值時,可改良其中利用本發明組合物密封之光學元件之光學裝置之發光效率。
式中,「a」係滿足關係式1a<2之數值,較佳地,滿足關
係式1.2a<2之數值、滿足關係式1.3a<2之數值或滿足關係式1.4a<2之數值。此係由於當「a」不小於上文所給出範圍之最小值時,可改良其中利用本發明組合物密封之光學元件之光學裝置之可靠性。另一方面,當「a」不大於上文所給出範圍之最大值時,藉由固化本發明組合物所獲得之固化產物之物理性質良好。
組份(A)之分子結構係例示為直鏈、部分支化之直鏈、具支鏈、環狀及樹枝狀結構,且較佳係直鏈、部分支化之直鏈或樹枝狀結構。組份(A)可係兩種或更多種類型之具有該等分子結構之有機聚矽氧烷之混合物。
組份(B)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之氫原子之有機聚矽氧烷。組份(B)之分子結構係例示為直鏈、部分支化之直鏈、具支鏈、環狀及樹枝狀結構,且較佳係直鏈、部分支化之直鏈或樹枝狀結構。組份(B)中矽鍵結之氫原子之鍵位置無限制,但實例係分子末端及/或側分子鏈。組份(B)中除氫原子外之矽鍵結基團之實例包括: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;及鹵化烷基,例如3-氯丙基及3,3,3-三氟丙基。在該等基團中,甲基及苯基係較佳的。儘管組份(B)之黏度無限制,但黏度在25℃下較佳在1mPa.s至10,000mPa.s範圍內、且尤其較佳在1mPa.s至1,000mPa.s範圍內。
組份(B)之有機聚矽氧烷之實例包括:1,1,3,3-四甲基二矽氧烷;1,3,5,7-四甲基環四矽氧烷;參(二甲基氫矽氧基)甲基矽烷;參(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;兩個分子末端經三甲基矽氧基封端之甲基氫聚矽氧烷;兩個分子末端經三甲基矽氧基封端之二甲基矽氧烷-甲基氫矽氧烷共聚物;兩
個分子末端經二甲基氫矽氧基封端之二甲基聚矽氧烷;兩個分子末端經二甲基氫矽氧基封端之二甲基矽氧烷-甲基氫矽氧烷共聚物;兩個分子末端經三甲基矽氧基封端之甲基氫矽氧烷-二苯基矽氧烷共聚物;兩個分子末端經三甲基矽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;三甲氧基矽烷之水解/縮合反應產物;包含(CH3)2HSiO1/2單元及SiO4/2單元之共聚物;包含(CH3)2HSiO1/2單元、SiO4/2單元及(C6H5)SiO3/2單元之共聚物及其兩種或更多種類型之混合物。
組份(B)之實例亦包括以下有機聚矽氧烷。注意,在式中,Me及Ph分別表示甲基及苯基,「m」係1至100之整數,「n」係1至50之整數且「b」、「c」、「d」及「e」各自係正數,其中分子中「b」、「c」、「d」及「e」之總和為1。
HMe2SiO(Ph2SiO)mSiMe2H
HMePhSiO(Ph2SiO)mSiMePhH
HMePhSiO(Ph2SiO)m(MePhSiO)nSiMePhH
HMePhSiO(Ph2SiO)m(Me2SiO)nSiMePhH
(HMe2SiO1/2)b(PhSiO3/2)c
(HMePhSiO1/2)b(PhSiO3/2)c
(HMePhSiO1/2)b(HMe2SiO1/2)c(PhSiO3/2)d
(HMe2SiO1/2)b(Ph2SiO2/2)c(PhSiO3/2)d
(HMePhSiO1/2)b(Ph2SiO2/2)c(PhSiO3/2)d
(HMePhSiO1/2)b(HMe2SiO1/2)c(Ph2SiO2/2)d(PhSiO3/2)e
組份(A)中每1莫耳總烯基之組份(B)之含量係在使得組份(B)中之矽鍵結氫原子之量在0.1mol至5mol範圍內且較佳0.5mol至2mol範圍內之範圍內。此係由於當組份(B)之含量不小於上文所給出範圍之最小值時,所獲得之組合物滿意地固化,且另一方面,當組份(B)之含
量不大於上文所給出範圍之最大值時,改良聚矽氧材料之耐熱性。
組份(C)係用於加速本發明組合物固化之矽氫化反應觸媒,且實例包括基於鉑之觸媒、基於銠之觸媒及基於鈀之觸媒,其中基於鉑之觸媒係較佳的。此基於鉑之觸媒係由以下各項所例示之基於鉑之化合物: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、鉑之烯基矽氧烷錯合物及諸如此類。
組份(C)之量係加速本發明組合物固化之量,且較佳係使得觸媒中金屬原子之量相對於本發明組合物以質量計在0.01ppm至1,000ppm範圍內之量。此係由於當組份(C)之量小於上文所給出範圍之最小值時,存在所獲得組合物之固化將不充分之風險,且另一方面,當該量超過上文所給出範圍之最大值時,固化不會明顯更快加速,且此外存在將發生諸如固化產物變色之問題的風險。
本發明組合物可包括矽氫化反應抑制劑(D),其作為可選組份用於延長室溫下可用壽命及改良儲存穩定性。組份(D)之實例包括炔烴醇,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(1,1-二甲基-3-丙炔-氧基)矽烷及甲基乙烯基雙(1,1-二甲基-3-丙炔-氧基)矽烷及三烯丙基異氰尿酸酯化合物。
對組份(D)之含量無限制,但其相對於100質量份組份(A)至(C)之總和較佳在0.01質量份至3質量份之範圍內、或0.01質量份至1質量份之範圍內。此係由於當組份(D)之含量不小於上文所給出範圍之最小值時,本發明組合物具有足夠可用壽命,且另一方面,當組份(D)之含量不大於上文所給出範圍之最大值時,其足夠容易的處置。
本發明組合物亦可含有用於改良組合物之黏著之黏著賦予劑(E)。較佳組份(E)係分子中具有至少一個矽鍵結之烷氧基之有機矽化合物。此烷氧基係例示為甲氧基、乙氧基、丙氧基、丁氧基及甲氧基乙氧基,其中甲氧基係尤佳的。此外,組份(E)中除烷氧基外之矽鍵結之基團係例示為經鹵素取代或未經取代之單價烴基團,例如烷基、烯基、芳基、芳烷基、鹵化烷基及諸如此類;縮水甘油氧基烷基,例如3-縮水甘油氧基丙基、4-縮水甘油氧基丁基及諸如此類;環氧基環己基烷基,例如2-(3,4-環氧基環己基)乙基、3-(3,4-環氧基環己基)丙基及諸如此類;環氧基烷基,例如3,4-環氧基丁基、7,8-環氧基辛基及諸如此類;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及諸如此類;及氫原子。組份(E)較佳含有可與本發明組合物中之烯基或矽鍵結之氫原子反應之基團。特定而言,組份(E)較佳含有矽鍵結之氫原子或烯基。此外,由於賦予不同類型之基板良好黏著之能力,組份(E)較佳在分子中具有至少一個含有環氧基之單價有機基團。此類型之組份(E)係例示為有機矽烷化合物、有機矽氧烷寡聚物及矽酸烷基酯。有機矽氧烷寡聚物或矽酸烷基酯之分子結構係例示為直鏈、部分支化之直鏈、具支鏈、環狀及網狀結構。直鏈、具支鏈及網狀結構尤佳。組份(E)係例示為矽烷化合物,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及諸如此類;在分子中具有矽鍵結之烯基或矽鍵結之氫原子中之至少一者及至少一個矽鍵結之烷氧基之矽氧烷化合物;分子中具有至少一個矽鍵結之烷氧基之矽烷化合物或矽氧烷化合物及具有至少一個矽鍵結之羥基及至少一個矽鍵結之烯基之矽氧烷化合物的混合物;及聚矽酸甲酯、聚矽酸乙酯及含有環氧基之聚矽酸乙酯。組份(E)較佳係低黏度液體,且其黏度並無具體限制但在25℃下較佳係1mPa.s至500mPa.s。在本發明組合物中,組份(E)之
含量並無具體限制,但較佳在每100質量份組合物之總和0.01質量份至10質量份之範圍內。
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;螢光物質、耐熱劑、染料、顏料、阻燃劑、溶劑及諸如此類可作為可選組份納入本發明組合物中,只要其不損害本發明之目的即可。
本發明組合物應使固化在室溫下或加熱下發生,但較佳加熱組合物以達成快速固化。加熱溫度較佳在50℃至200℃範圍內。
本發明之光學裝置之特徵為其係藉由利用上文之聚矽氧材料密封光學元件而形成。本發明之光學裝置中之光學元件可係光耦合器、發光二極體、固態影像感測器或諸如此類。光學元件較佳係發光二極體。將使用圖1及2詳細地闡述本發明之此一光學裝置。
圖1圖解說明為本發明之光學裝置之實例之晶片封裝(COB)LED之剖視圖。在圖1之COB LED裝置中,LED 2係藉由晶粒接合安裝於COB基板1上,且LED 2係用聚矽氧材料3密封。此外,光反射材料(未圖解說明)可於基板1上圍繞LED 2形成,使得有效反射自LED 2發出之光。
圖2圖解說明為本發明之光學裝置之實例之另一LED之剖視圖。在圖2之LED裝置中,LED 2係藉由晶粒接合安裝於引線框4’上,且藉由接合線5電連接至引線框4。LED 2係用聚矽氧材料3密封。此外,光反射材料6係於引線框4、4’上圍繞LED 2形成,使得有效反射自LED 2發出之光。
在圖1之LED裝置中,基板1可係由鋁、銅或諸如此類製得之金屬基板,且在金屬基板之表面上,形成電路及插入之絕緣層(未示出)。此外,當使用非金屬基板作為基板1時,不需要形成絕緣層。此等非
金屬基板之實例包括玻璃環氧基板、聚對苯二甲酸丁二酯(PBT)基板、聚醯亞胺基板、聚酯基板、氮化鋁基板、氮化硼基板、氮化矽基板、氧化鋁陶瓷基板、玻璃基板及撓性玻璃基板。另外,自鋁基板或銅基板製得之具有絕緣樹脂層之混合基板、印刷矽基板、碳化矽基板及藍寶石基板亦可用作基板1。
在圖2之LED裝置中,對於引線框4、4’,使用至少一種類型之選自由具有高電導率之銀、銅及鋁組成之群之金屬,或含有至少一種類型之選自由銀、銅及鋁組成之群之金屬之合金。另外,光反射材料6較佳於引線框4、4’上形成以便暴露安裝LED 2之部分。
圖1僅繪示於基板1上之一個LED 2,但基板1上可安裝複數個LED 2。
現將使用實踐實例詳細闡述本發明之聚矽氧材料、可固化性聚矽氧組合物及光學裝置。
矽材料表面之原子組成百分比係藉由X-射線光電子光譜學量測。使用由Kratos Analytical有限公司製造之AXIS Nova實施量測。使用Al-Kα射線作為X-射線激發源,使用150W單色器及0.4mm×0.9mm之分析區。藉由全掃描量測測定C1、O1、N1及F1之峰面積,且針對每一元素藉由XPS相對靈敏度校正之後確定原子組成百分比。自所獲得之原子組成百分比值確定C原子之比例及C原子相對Si原子之比率。
表1中所示之可固化性聚矽氧組合物(質量份數)係使用下文所提及之組份製備。此外,表1中,組份(C)之含量係以鉑金屬相對於可固化性聚矽氧組合物之含量表示(ppm,就質量單位而言)。此外,表1
中,「SiH/Vi」表示在可固化性聚矽氧組合物中組份(A)中每1莫耳乙烯基組份(B)中矽鍵結之氫原子之莫耳數值。應注意在該等式中,Me、Ph、Vi及Ep分別表示甲基、苯基、乙烯基及3-縮水甘油氧基丙基。
使用以下組份作為組份(A)。
組份(a-1):由以下平均組成式表示之有機聚矽氧烷:Me1.62Vi0.06Ph0.26SiO1.03
(乙烯基含量=3.1mol%,苯基含量=13.4mol%)
組份(a-2):由以下平均組成式表示之有機聚矽氧烷:Me1.14Vi0.14Ph0.26SiO1.22
(乙烯基含量=9.1mol%,苯基含量=16.9mol%)
組份(a-3):由以下平均組成式表示之有機聚矽氧烷:Me1.17Vi0.13Ph0.23SiO1.23
(乙烯基含量=8.5mol%,苯基含量=15.0mol%)
組份(a-4):由以下平均組成式表示之有機聚矽氧烷:Me0.94Vi0.18Ph0.44SiO1.22
(乙烯基含量=11.5mol%,苯基含量=28.2mol%)
組份(a-5):由以下平均組成式表示之有機聚矽氧烷:Me0.68Vi0.34Ph0.73SiO1.11
(乙烯基含量=19.4mol%,苯基含量=41.7mol%)
組份(a-6):由以下平均組成式表示之有機聚矽氧烷:Me1.78Vi0.04SiO1.09
(乙烯基含量=2.2mol%)
使用以下組份作為組份(B)。
組份(b-1):由以下平均單元式表示之有機聚矽氧烷樹脂:(Me2HSiO1/2)0.65(SiO4/2)0.35
組份(b-2):由下式表示之有機三矽氧烷:HMe2SiOPh2SiOSiMe2H
組份(b-3):由以下平均單元式表示之有機聚矽氧烷樹脂:(Me2HSiO1/2)0.6(PhSiO3/2)0.4
組份(b-4):由下式表示之有機聚矽氧烷:Me3SiO(MeHSiO)50SiMe3
使用以下組份作為組份(C)。
組份(c-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(D)。
組份(d-1):1,3,5,7-四甲基-1,3,5,7-四乙烯基環四矽氧烷
組份(d-2):1-乙快基環己醇
使用以下組份作為組份(E)。
組份(e-1):在25℃黏度為30mPa.s且包含在兩個分子末端處經矽醇基團封端之3-縮水甘油氧基丙基三甲氧基矽烷與甲基乙烯基矽氧烷寡聚物之縮合反應產物之黏著賦予劑
組份(e-2):由藉由以下平均單元式表示之有機聚矽氧烷樹脂組成之黏著賦予劑
(Me2ViSiO1/2)0.18(MeEpSiO2/2)0.28(PhSiO3/2)0.54
所獲得之可固化性聚矽氧組合物1至6各自藉由以120℃熱壓機加熱5分鐘並然後在150℃烘箱中進一步加熱1小時固化,以產生聚矽氧材料1至6。該等聚矽氧材料表面之元素組成比率係藉由X-射線光電子光譜學量測。此外,藉由13C核磁光譜學確定聚矽氧材料之結構中存在或不存在Si-C2H4-Si鍵。該等結果顯示於表1中。
將其中LED晶片安裝於其上之陶瓷基板放置於壓製模具中。將可
固化性聚矽氧組合物1傾倒於模空腔中,且藉由在120℃下熱壓模製5分鐘在LED晶片上形成拱頂形密封材料。在150℃下額外實施固化1小時,並製得LED裝置。在85℃及85% RH之恒溫-恒濕烘箱中,使700mA之電流流經所獲得之LED裝置,並進行加電(power-on)測試。在規定時期內(50hr),未觀察到因密封材料之透明度減小所致之LED亮度降低(在加電測試中降至初始亮度的90%或更少)及聚矽氧材料中之裂紋。
使用可固化性聚矽氧組合物2,以與工作實例1相同之方式製造LED裝置並進行加電測試。在規定時期內(50hr),未觀察到因密封材料之透明度減小所致之LED亮度降低及聚矽氧材料中之裂紋。
使用可固化性聚矽氧組合物3,以與工作實例1相同之方式製造LED裝置並進行加電測試。在規定時期內(50hr),未觀察到因密封材料之透明度減小所致之LED亮度降低及聚矽氧材料中之裂紋。
使用可固化性聚矽氧組合物4,以與工作實例1相同之方式製造LED裝置並進行加電測試。在規定時期內(50hr),未觀察到因密封材料之透明度減小所致之LED亮度降低及聚矽氧材料中之裂紋。
使用可固化性聚矽氧組合物5,以與工作實例1相同之方式製造LED裝置並進行加電測試。在規定時期內(50hr),LED裝置之亮度因密封材料之透明度減小而降低。
使用可固化性聚矽氧組合物6,以與工作實例1相同之方式製造LED裝置並進行加電測試。然而,在規定時期內(50hr),聚矽氧材料
中發生裂紋。
由於本發明之聚矽氧材料對光及熱穩定且不易於發生透射率之下降及裂紋之產生,因此其有利的作為其中需要在高亮度下高耐久性之LED密封材料。
1‧‧‧COB基板/基板
2‧‧‧LED
3‧‧‧聚矽氧材料
Claims (7)
- 一種聚矽氧材料,其根據X-射線光電子光譜法(ESCA)滿足以聚矽氧材料表面之元素組成百分比表示之以下條件:(i)碳原子之元素組成百分比係50.0原子%至70.0原子%;及(ii)碳原子之元素組成百分比對矽原子之元素組成百分比之比率(C/Si)係2.0至5.0。
- 如請求項1之聚矽氧材料,其中該聚矽氧材料在結構中含有Si-R1-Si鍵,其中R1係伸烷基或伸芳基。
- 如請求項1或2之聚矽氧材料,其中該聚矽氧材料係光學材料。
- 如請求項1或2之聚矽氧材料,其中該聚矽氧材料係光學元件之密封材料。
- 一種可固化性聚矽氧組合物,其固化以形成如請求項1至4中任一項之聚矽氧材料,該組合物包含:在分子中具有至少兩個矽鍵結之烯基及至少一個矽鍵結之芳基之有機聚矽氧烷;在分子中具有至少兩個矽鍵結之氫原子之有機聚矽氧烷;及矽氫化反應觸媒。
- 一種光學裝置,其藉由用如請求項1或2之聚矽氧材料密封光學元件而形成。
- 如請求項6之光學裝置,其中該光學元件係LED。
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