TW201350543A - 膜狀熱固性聚矽氧密封材料 - Google Patents
膜狀熱固性聚矽氧密封材料 Download PDFInfo
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- TW201350543A TW201350543A TW102115517A TW102115517A TW201350543A TW 201350543 A TW201350543 A TW 201350543A TW 102115517 A TW102115517 A TW 102115517A TW 102115517 A TW102115517 A TW 102115517A TW 201350543 A TW201350543 A TW 201350543A
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- sealing material
- thermosetting
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- 150000003527 tetrahydropyrans Chemical group 0.000 description 1
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- IAQRGUVFOMOMEM-ONEGZZNKSA-N trans-but-2-ene Chemical group C\C=C\C IAQRGUVFOMOMEM-ONEGZZNKSA-N 0.000 description 1
- GRPURDFRFHUDSP-UHFFFAOYSA-N tris(prop-2-enyl) benzene-1,2,4-tricarboxylate Chemical compound C=CCOC(=O)C1=CC=C(C(=O)OCC=C)C(C(=O)OCC=C)=C1 GRPURDFRFHUDSP-UHFFFAOYSA-N 0.000 description 1
- 125000005023 xylyl group Chemical group 0.000 description 1
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Abstract
本發明係關於一種膜狀熱固性聚矽氧密封材料,其用於藉助於壓縮成型密封半導體元件,該密封材料具有如藉由MDR(動模流變儀)在室溫至200℃之成型溫度所量測小於15dN.m之初始扭矩值;一種藉助於使用其壓縮成型生產LED之方法;及一種由此方法所生產之LED。該密封材料具有極佳成型性,不會引起諸如溢出模具之問題,且無諸如空隙之缺陷。
Description
本發明係關於一種用於藉助於壓縮成型密封諸如LED之半導體元件之膜狀熱固性聚矽氧密封材料、一種藉助於使用其壓縮成型用於生產LED之方法及一種由此方法所生產之LED。
本發明主張申請於2012年5月1日之日本專利申請案第2012-104531號之優先權,其內容以引用之方式併入本文中。
慣常地,液體熱固性密封材料被稱為用於密封諸如LED之半導體元件之密封材料。舉例而言,日本未審查專利申請公開案第2008-227119號描述一種用於LED晶片及透鏡之統一結構之生產方法,該統一結構藉由使液體可固化聚矽氧組合物、可固化環氧樹脂組合物或可固化聚矽氧/環氧樹脂組合物熱固性或紫外固化形成。另外,日本未審查專利申請公開案第2006-93354號描述一種用於光學半導體裝置(其中可固化聚矽氧組份係藉助於壓縮成型密封)之生產方法。
然而,當LED係使用此等液體密封材料密封時,存在難以在低溫時成型及節拍時間較長之問題。亦一直存在樹脂洩露至模具外部或由於分配時之起泡浸潤出現缺陷的問題。此等問題由於使液體成型而出現且可藉由使固態或半-固態密封材料成型得以解決。
日本未審查專利申請公開案第2009-235368號描述一種固態或半-固態加成-可固化黏著劑聚矽氧組合物,其包含具有特定結構之有機
聚矽氧烷、有機含氫聚矽氧烷、鉑金屬-型催化劑及螢光物質。另外,日本未審查專利申請公開案第2002-294202號描述一種熱固性聚矽氧橡膠黏著劑組合物,其具有400至800之威廉斯(Williams)塑性值、0.2至0.5MPa之生強度(25℃),及對於具有1mm之厚度之固化薄片至少50%之可見光透射率。雖然描述此等聚矽氧組合物係成型成薄片形狀,但描述於日本未審查專利申請公開案第2009-235368號中之聚矽氧組合物之厚度較薄(1至500μm),且描述於日本未審查專利申請公開案第2002-294202號中之聚矽氧組合物之應用限於建築材料玻璃及建築材料配件之接合。此外,由於未提及密封性能,此等組合物作為密封材料之有用性未知。
相應地,用於密封半導體元件(諸如LED)之習知密封材料已具有由於密封材料之成型性及可操作性及密封材料係易於出現缺陷之液體之事實及其類似者而出現的問題。此外,未知現有片狀聚矽氧組合物作為密封材料之有用性,且亦未知藉助於壓縮成型,此等聚矽氧組合物是否適合於作為LED密封材料之應用。
構想本發明以解決上述問題,且本發明之一個目標為提供一種用於藉助於壓縮成型密封半導體元件(諸如LED)之膜狀熱固性聚矽氧密封材料,該密封材料具有極佳成型性、不引起諸如溢出模具之問題且無諸如空隙之缺陷。
由於旨在達成以上目標之密集研究,本發明人達成本發明。亦即,本發明之目標係藉由一種用於藉助於壓縮成型密封半導體元件之膜狀熱固性聚矽氧密封材料達成,該密封材料具有如藉由動模流變儀(MDR)在室溫至200℃之成型溫度下所量測低於15dN.m之初始扭矩值。
該膜狀熱固性聚矽氧密封材料較佳具有如藉由MDR所量測,在
300秒內不超過10dN.m之最小扭矩值。
該膜狀熱固性聚矽氧密封材料較佳具有如在JIS K 6249中所規定,在25℃時200至800之威廉斯塑性值。
該膜狀熱固性聚矽氧密封材料較佳具有在25℃時0.01至0.6MPa之生強度。
該膜狀熱固性聚矽氧密封材料在1mm之厚度時之可見光透射率較佳為至少50%。
本發明之膜狀熱固性聚矽氧密封材料較佳包含膜狀聚矽氧組合物,其包含:(A)100質量份含烯基有機聚矽氧烷生橡膠;(B)30至150質量份濕疏水性增強矽石,其具有至少200m2/g之BET法比表面積,該矽石包含選自由R3SiO1/2單元、R2SiO2/2單元、RSiO3/2單元(其中R各自獨立地為單價烴基)及其混合物組成之群之有機聚矽氧烷單元及SiO4/2單元(有機聚矽氧烷單元與SiO4/2單元之莫耳比為0.08至2.0);(C)0.1至10質量份有機含氫聚矽氧烷;及(D)用於固化該組合物之足量固化劑;或該密封材料藉由固化該聚矽氧組合物至B-階段所產生。
該膜狀熱固性聚矽氧密封材料可在至少一側上具有膜。
膜之透濕性較佳為不超過10g/m2/24hr。
另外,本發明亦關於一種藉助於壓縮成型,使用膜狀熱固性聚矽氧密封材料生產LED之方法,視情況而定,該LED在密封材料之表面上具有膜。
本發明亦關於一種LED,其包含LED晶片、覆蓋該晶片之膜狀熱固性聚矽氧密封材料之固化產品,及覆蓋該固化產品之表面之膜。
藉由本發明,有可能提供一種用於藉助於壓縮成型密封半導體元件(諸如LED)之膜狀熱固性聚矽氧密封材料,該密封材料具有極佳成型性、不引起諸如溢出模具之問題且無諸如空隙之缺陷。
由於經保護不受硫或其類似物之腐蝕,使用本發明之膜狀熱固性聚矽氧密封材料之LED具有極佳耐久性。
本發明中所使用之膜狀熱固性聚矽氧密封材料必須具有如藉由動模流變儀(MDR)在室溫至200℃之成型溫度下所量測低於15dN.m,較佳不超過14dN.m,且更佳不超過13dN.m之初始扭矩值。此係因為當初始扭矩值在上述範圍內時,無成型性之損失,使得有可能減少對於半導體元件(諸如LED)之損害且抑制用於電連接該半導體元件之接線之變形或其類似者的出現。此處,扭矩值係藉由使用MDR(根據JIS K 6300-2「橡膠,未硫化-物理特性-第2部分:藉由振盪硫化測試器判定硫化特性」)量測得到之值,且初始扭矩值係緊接著該硫化之後所得到之扭矩值。
雖然半導體元件之密封通常在較短量之時間(諸如300秒內)內進行,舉例而言,如藉由MDR在上述成型溫度下所量測之在300秒內之最小扭矩值較佳為不超過10dN.m,更佳為不超過8dN.m,且最佳為不超過6dN.m。最小扭矩值之下限較佳為至少1dN.m且更佳為至少2dN.m。此係因為當最小扭矩值低於或等於上述範圍之上限時,填充特性在半導體元件之微小部分得到改良,且當最小扭矩值大於或等於上述範圍之下限時,諸如溢出模具之問題變得不太可能出現。此處,最小扭矩值係如上文所描述之根據JIS使用MDR量測在緊接著硫化之後開始300秒之硫化時間期間之最小扭矩值。
為了達成膜狀熱固性聚矽氧密封材料之極佳可固化性,壓縮成型之成型溫度必須為室溫至200℃且較佳為30℃至150℃。
本發明中所使用之膜狀熱固性聚矽氧密封材料較佳為具有如在JIS K 6249中所規定,在25℃時200至800之威廉斯塑性值。此係因為當威廉斯塑性值至少為200時,膜狀熱固性聚矽氧密封材料變得不大可能溢出模具,且當威廉斯塑性值不超過800時,可操作性得到改良。
本發明中所使用之膜狀熱固性聚矽氧密封材料之生強度(25℃),亦即未固化強度較佳為0.01至0.6MPa。生強度之下限更佳為至少0.1MPa。生強度之上限更佳為不超過0.5MPa。此係因為當生強度大於或等於上述範圍之下限時,在操作期間出現諸如變形或撕碎之問題變得不大可能。當生強度低於或等於上述範圍之上限時,可操作性得到改良,且由於在儲存期間塑化之返回消除塑性之損失,其亦改良密封材料之可加工性。
本發明中所使用之膜狀熱固性聚矽氧密封材料對於厚度為1mm之固化薄片之可見光透射率必須至少為50%,較佳為至少85%,且更佳為至少90%。此係因為當可見光透射率不超過50%時,膜狀熱固性聚矽氧密封材料之透明度減小,且當膜狀熱固性聚矽氧密封材料用於LED時其發光強度減小。
本發明之膜狀熱固性聚矽氧密封材料較佳包含膜狀聚矽氧組合物,其包含:(A)100質量份含烯基有機聚矽氧烷生橡膠;(B)30至150質量份濕法疏水性增強矽石,其具有至少200m2/g之BET法比表面積,該矽石包含選自由R3SiO1/2單元、R2SiO2/2單元、RSiO3/2單元(其中R各自獨立地為單價烴基)及其混合物組成之群之有機聚矽氧烷單元及SiO4/2單元(有機聚矽氧烷單元與SiO4/2單元之莫耳
比為0.08至2.0);(C)0.1至10質量份有機含氫聚矽氧烷;及(D)用於固化該組合物之足量固化劑;或該密封材料係藉由固化該聚矽氧組合物至B-階段所產生。
組分(A)通常稱為有機聚矽氧烷生橡膠,且可使用一種用作可軋聚矽氧橡膠之主試劑的物質。此有機聚矽氧烷生橡膠之一個代表性實例係含烯基有機聚矽氧烷生橡膠,其由平均單元式R'aSiO(4-a)/2(其中R'係單價烴基或鹵化烷基,單價烴基之實例包括諸如甲基、乙基及丙基之烷基;諸如乙烯基及烯丙基之烯基;諸如環己基之環烷基;諸如β-苯乙基之芳烷基;及諸如苯基及甲苯基之芳基;及鹵化烷基之實例包括3,3,3-三氟丙基及3-氯丙基;且「a」為1.9至2.1)表示。
組分(A)之含烯基有機聚矽氧烷生橡膠較佳在一個分子中具有至少兩個矽鍵結烯基。組分(A)之分子結構可為直鏈或分支鏈結構。烯基在組分(A)中之鍵結位置之實例為分子鏈末端及/或分子側鏈。此組分之聚合度通常為3,000至20,000,且質量-平均分子質量為至少20×104。此組分在25℃之黏度為至少106mPa.s,且在25℃之威廉斯塑性值為至少50且較佳為至少100。組分之狀態為生橡膠狀態。
組分(A)可為均聚物、共聚物或此等聚合物之混合物。構成此組分之矽氧烷單元之特定實例包括二甲基矽氧烷單元、甲基乙烯基矽氧烷單元、甲基苯基矽氧烷單元及3,3,3-三氟丙基甲基矽氧烷單元。組分(A)之分子鏈末端較佳為藉由三有機矽氧烷基或羥基封端之鏈,且存在於分子鏈末端之基團之實例包括三甲基矽烷氧基、二甲基乙烯基矽烷氧基、甲基乙烯基羥基矽烷氧基及二甲基羥基矽烷氧基。此有機聚矽氧烷生橡膠之實例包括兩末端均由二甲基乙烯基矽烷氧基-鏈封端之二甲基矽氧烷-甲基乙烯基矽氧烷共聚物生橡膠、兩末端均由二甲基乙烯基矽烷氧基-鏈封端之二甲基聚矽氧烷生橡膠、兩末端均由
二甲基羥基矽烷氧基-鏈封端之二甲基矽氧烷-甲基乙烯基矽氧烷共聚物生橡膠及兩末端均由甲基乙烯基羥基矽烷氧基-鏈封端之二甲基矽氧烷-甲基乙烯基矽氧烷共聚物生橡膠。
組分(B)之濕法疏水性增強矽石具有在未固化狀態及固化後提高機械強度之功能。該濕法疏水性增強矽石亦具有特定言之-向LED晶片提供黏附性-黏著耐久性之功能。此組分(B)係一種濕法疏水性增強矽石,其具有至少200m2/g之BET法比表面積,該矽石包含選自由R3SiO1/2單元、R2SiO2/2單元、RSiO3/2單元(其中R各自獨立地為藉由諸如甲基、乙基、及丙基之烷基或諸如苯基之芳基例示之單價烴基)及其混合物組成之群之有機聚矽氧烷單元及SiO4/2單元(有機聚矽氧烷單元與SiO4/2單元之莫耳比為0.08至2.0)。
組分(B)中有機矽氧烷單元之含量為足以使增強矽石疏水之量,且有機聚矽氧烷單元與SiO4/2單元之莫耳比較佳在0.08至2.0之範圍內。此係因為當莫耳比為至少0.08時,關於LED晶片之黏著性能得到改良,且當莫耳比不超過2.0時,增強性能得到顯著改良。另外,為了提高在未固化及固化狀態之機械強度,BET法比表面積必須為至少200m2/g,較佳為至少300m2/g,且更佳為至少400m2/g。
組分(B)係藉由一種揭示於日本經審查專利申請公開第S61-56255號或美國專利第4,418,165號中之方法製備。組分(B)之量為每100質量份組分(A)30至150質量份且較佳為50至100質量份。
組分(C)之有機含氫聚矽氧烷為組分(A)之交聯劑且為在一個分子中具有至少兩個矽鍵結氫原子之有機聚矽氧烷。組分(C)之分子結構之實例包括直鏈結構、部分支鏈直鏈結構、支鏈結構、環狀結構及網狀結構。矽鍵結氫原子在組分(C)中之鍵結位置之實例為分子鏈末端及/或分子側鏈。在組分(C)中除了氫原子外鍵結至矽原子之基團之實例為經取代或未經取代之單價烴基,其包括諸如甲基、乙基、丙基、
丁基、戊基、己基、庚基之烷基;諸如苯基、甲苯基、二甲苯基及萘基之芳基;諸如苯甲基及苯乙基之芳烷基;及諸如氯甲基、3-氯丙基及3,3,3-三氟丙基之鹵化烷基。此有機含氫聚矽氧烷之實例包括以三甲基矽烷氧基在兩分子末端均封端之甲基含氫聚矽氧烷、以三甲基矽烷氧基在兩分子末端均封端之二甲基矽氧烷-甲基含氫矽氧烷共聚物、以二甲基苯基矽烷氧基在兩末端均封端之甲基苯基矽氧烷-甲基含氫矽氧烷共聚物、環狀甲基含氫聚矽氧烷及包含二甲基含氫矽氧烷單元及SiO4/2單元之共聚物。
組分(C)之量為足以固化該組合物之量。此量較佳為使得組分(A)之含烯基有機聚矽氧烷生橡膠中每1莫耳矽鍵結烯基之矽鍵結氫原子能夠在0.5至10莫耳範圍內且更佳為在1至3莫耳範圍內之量。此係因為當每1莫耳矽鍵結烯基之矽鍵結氫原子之莫耳數大於或等於上述組合物中之此範圍之下限時,組合物之固化充足,且當莫耳數小於或等於此範圍之上限時,組合物之固化產品之耐熱性得到改良。特定言之,該量較佳為每100質量份組分(A)0.1至10質量份且更佳為0.3至5質量份。
組分(D)之固化劑為一種用於固化組合物之催化劑,其實例包括鉑-基催化劑、有機過氧化物及鉑-基催化劑與有機過氧化物之混合物。鉑-基催化劑之實例包括氯鉑酸、酒精-變性氯鉑酸、鉑螯合物、氯鉑酸與烯烴之配位化合物、氯鉑酸與二酮之錯合物及氯鉑酸與二乙烯基四甲基二矽氧烷之錯合物。有機過氧化物之實例包括過氧化苯甲醯、過苯甲酸第三丁酯、過氧化鄰甲基苯甲醯、過氧化對甲基苯甲醯、過氧化間甲基苯甲醯、過氧化二異丙苯及2,5-二甲基-2,5-二(第三丁基過氧基)己烷。
組分(D)之量為足以固化該組合物之量。當使用鉑-基催化劑時,鉑金屬在鉑-基催化劑中之量較佳為每100質量份組分(A)在0.1至500
ppm之範圍內且更佳為在1至100ppm之範圍內。當使用有機過氧化物時,有機過氧化物之量較佳為每100質量份組分(A)0.1至10質量份。
為了提昇黏著力,亦可混合主要包含有機烷氧基矽氧烷或其部分水解縮合物之黏著促進劑作為額外組分,該有機烷氧基矽氧烷具有諸如巰基、胺基、乙烯基、烯丙基、己烯基、甲基丙烯醯氧基、丙烯醯氧基、及縮水甘油氧基之有機官能基。此黏著促進劑之實例包括諸如γ-巰基丙基三甲氧基矽烷、γ-巰基丙基甲基二甲氧基矽烷、γ-(2-胺基乙基)胺基丙基三甲氧基矽烷、γ-甲基丙烯醯氧基丙基三甲氧基矽烷、γ-丙烯醯氧基丙基三甲氧基矽烷、乙烯基三(甲氧基乙氧基)矽烷、烯丙基三甲氧基矽烷及γ-縮水甘油氧基丙基三甲氧基矽烷或其部分水解縮合物之有機烷氧基矽烷;此等有機烷氧基矽烷與苯偏三酸三烯丙酯或均苯四酸四烯丙酯之反應產物;烷氧矽烷與矽氧烷有機物(organomer)之反應物;及此等烷氧矽烷與諸如烯丙基縮水甘油醚、丙烯酸縮水甘油酯、鄰苯二甲酸二烯丙酯、三羥甲基丙烷三丙烯酸酯、含烯基碳酸基化合物及含巰基乙酸基化合物之反應性有機化合物之混合物。在此等黏著促進劑之中,較佳使用γ-甲基丙烯醯氧基丙基三甲氧基矽烷、γ-縮水甘油氧基丙基三甲氧基矽烷、其混合物或其反應混合物。此黏著促進劑之量較佳為每100質量份組分(A)之有機聚矽氧烷0.1至10質量份且更佳為0.3至5質量份。
另外,只要不破壞本發明之目的,已知待添加至普通聚矽氧橡膠組合物或與該等普通聚矽氧橡膠組合物混合之不同添加劑(例如其他無機填充劑、顏料、耐熱劑及鉑-基催化劑之固化阻燃劑)亦可添加至本發明中所使用之膜狀熱固性聚矽氧密封材料中。此等添加劑之實例包括矽藻土、石英粉、碳酸鈣、透明氧化鈦及透明紅色氧化鐵。耐熱劑之實例包括稀土氧化物、矽醇化鈰及鈰脂肪酸鹽。固化阻燃劑之實例包括諸如3-甲基-1-丁基-3-醇、3,5-二甲基-1-己炔-3-醇及苯基丁
醇之乙炔酒精化合物;諸如3-甲基-3-戊烯-1-炔及3,5-二甲基-3-己烯-1-炔之烯炔化合物;及其他肼化合物、磷化氫化合物、硫醇化合物、苯并三唑及甲基參(甲基異丁氧基)矽烷。
本發明之膜狀熱固性聚矽氧密封材料可固化至B-階段。此膜狀熱固性聚矽氧密封材料之固化程度未特定限制。可能狀態之一個實例為在該狀態中膜狀熱固性聚矽氧組合物並非完全固化且以一種溶劑使其膨脹但不完全溶解,因此膜狀熱固性聚矽氧組合物失去流動性;亦即諸如藉由JIS K 6800(熱固性樹脂之固化中間物)所定義之B-階段之狀態。
本發明之膜狀熱固性聚矽氧密封材料係藉由使用雙滾筒機、捏合機、班拍里混合機(Banbury mixer)及其類似物捏合及混合上述組分得到。接下來,用於將所得組合物加工為膜形狀之方法之實例包括經由具有規定蓋子之擠壓機將組合物擠壓成膜形狀、使用砑光輥將組合物夾在有機樹脂膜(諸如聚烯烴膜或聚酯膜)之間以形成均一膜形狀或使用調整至不超過40℃之壓力機將組合物成型為膜形狀之方法。特定言之,藉由使用砑光輥在有機樹脂膜之間層壓組合物來持續使組合物成型從生產效率之角度有效。以此方式所成型之膜狀聚矽氧密封材料在使用切割機或打孔機自長卷形物切割成所需形狀之後可供使用。
本發明之膜狀熱固性聚矽氧密封材料在至少一側上可具有膜。膜之實例包括諸如聚酯、聚四氟乙烯、聚醯亞胺、聚苯硫醚、聚醯胺、聚碳酸酯、聚苯乙烯、聚丙烯、聚乙烯、聚氯乙烯及聚對苯二甲酸伸乙酯之合成樹脂膜。較佳為聚丙烯膜。
為了在LED之壓縮成型中達到極佳成型性,本發明之膜狀熱固性聚矽氧密封材料之厚度較佳為0.1至5mm且更佳為0.5至1.5mm。
本發明之膜狀熱固性聚矽氧密封材料用於LED之壓縮成型。用於生產此LED之方法之一個實例為一種用於LED之生產方法,其中本發
明之膜狀熱固性聚矽氧密封材料係設置於模具中,該模具在與支撐元件相對之位置具有凹穴,LED晶片安裝於支撐元件上,且隨後藉由使該密封材料在將支撐件按壓至模具中之狀態下成型而使聚矽氧密封材料成一體。亦有可能在膜黏附於膜狀熱固性聚矽氧密封材料之單側之狀態下執行壓縮成型,且在此狀況下,可能產生在密封材料之表面上具有膜之LED。
黏附於本發明之膜狀熱固性聚矽氧密封材料之至少一側之膜之透濕性較佳為不超過10g/m2/24hr且更佳為不超過8g/m2/24hr。此係因為若膜狀熱固性聚矽氧密封材料之透濕性較高,LED晶片之耐久性會削弱。另外,黏附於本發明之膜狀熱固性聚矽氧密封材料之至少一側之膜之厚度為至少10μm且較佳為不超過100μm。此係因為當膜之厚度大於或等於上述範圍之下限時,膜在壓縮成型時破裂之風險減少。當厚度小於或等於上述範圍之上限時,膜之模具順應性得到改良,其使得有可能藉由設計模具形狀來完全按規定用模具製作成型產品。
本發明亦關於包含安裝於支撐件上之LED晶片、覆蓋晶片之本發明之膜狀熱固性聚矽氧密封材料及覆蓋密封材料之表面之膜之LED。合適之LED晶片係一種藉由液相磊晶法或MOCVD在基板上形成為發光層之半導體(諸如InN、AlN、GaN、ZnSe、SiC、GaP、GaAs、GaAlAs、GaAlN、AlInGaP、InGaN、或AlInGaN)。支撐件之實例包括有機樹脂基板,諸如陶瓷基板、矽基板、金屬基板、聚醯亞胺樹脂、環氧樹脂及BT樹脂。除提供用於LED晶片之安裝台之外,支撐件還可具有電路、用於電連接電路及LED晶片之接線(諸如金線或鋁線)、用於電路之外部引線及其類似物。當安裝複數個晶片時,藉由分割或破裂支撐件,可將晶片建立為獨立的光學裝置。
當密封LED晶片時,本發明之膜狀熱固性聚矽氧密封材料係整體
地形成,且較佳黏附於支撐件及LED晶片。聚矽氧固化產品之形狀未特定限制,且實例包括凸透鏡形狀、截圓錐形狀、菲涅爾透鏡形狀、凹透鏡形狀及截四角錐。該形狀較佳為凸透鏡形狀。
在下文中,本發明將使用實例詳細描述。在實例中,稱作「份」之組分含量意謂「質量份」。應注意本發明不限於此等實例。
首先,使277g八甲基環四矽氧烷、4.6g 1,3,5,7-四甲基-1,3,5,7-四乙烯基環四矽氧烷、517g甲基三甲氧基矽烷及充當催化劑之0.43g氫氧化鉀在105℃之溫度下反應約2小時以產生疏水劑,其包含開環及重組有機聚矽氧烷。氫氧化鉀與碳酸氣體中和。當分析所得到之有機聚矽氧烷時,觀測到該物質係含有0.7mol%甲基乙烯基矽氧烷基之直鏈有機聚矽氧烷。
隨後,使用包含上文所得到之有機聚矽氧烷之疏水劑如下文所述合成濕法疏水性增強矽石。亦即,將118g甲醇、32g濃氨水及39g上文所得到之疏水劑裝入玻璃反應容器中且使用電磁混合機均一混合。隨後,立即添加96g原矽酸甲酯至混合物中,同時劇烈攪拌該混合物。15秒後反應產物變為凝膠狀,且中斷攪拌。使該產物在此狀態下靜置且老化,同時於室溫下密閉地密封,以獲得濕法疏水性增強矽石之分散液。自此矽石分散液中移除甲醇及氨氣以產生濕法疏水性增強矽石,其包含(CH3)2SiO2/2單元、(CH3)(CH=CH2)SiO2/2單元、CH3SiO3/2單元及SiO4/2單元,(CH3)2SiO2/2單元、(CH3)(CH=CH2)SiO2/2單元、CH3SiO3/2單元之總和與SiO4/2單元之莫耳比為1.0。此濕法疏水性增強矽石之BET法比表面積為540m2/g。
首先,將100份二甲基矽氧烷-甲基乙烯基矽氧烷共聚物生橡膠
(包含99.63mol%二甲基矽氧烷單元及0.37mol%甲基乙烯基矽氧烷單元且分子鏈之兩末端均以二甲基乙烯基矽烷氧基鏈封端;聚合度:4,000)及75份上文製備之濕法疏水性增強矽石(具有540m2/g之BET法比表面積)裝入捏合混合機中且在180℃下捏合60分鐘。經冷卻之後,將3.0份在25℃時黏度為7mPa.s之甲基含氫聚矽氧烷(分子末端以三甲基矽烷氧基(矽鍵結氫原子含量:1.5%)鏈封端)及氯鉑酸與1,3-二乙烯基四甲基二矽氧烷之錯合物混合至所得到之聚矽氧橡膠基質中使得鉑金屬之量為10ppm,且獲得透明熱固性聚矽氧橡膠黏著劑組合物。藉由使此組合物通過砑光輥製備厚度為1mm之膜狀熱固性聚矽氧密封材料(I)。此膜狀熱固性聚矽氧密封材料(I)之特性展示於表1中。
藉由在120℃將製備於實際實例1中之膜狀熱固性聚矽氧密封材料(I)加熱5分鐘,製備固化至B-階段之膜狀熱固性聚矽氧密封材料(II)。此膜狀熱固性聚矽氧密封材料(II)之特性展示於表1中。
藉由在120℃將製備於實際實例1中之膜狀熱固性聚矽氧密封材料(I)加熱7分鐘,製備固化至B-階段之膜狀熱固性聚矽氧密封材料(III)。此膜狀熱固性聚矽氧密封材料(III)之特性展示於表1中。
以與實際實例1中相同之方式製備膜狀熱固性聚矽氧密封材料(IV),除了將用於實際實例1中之75份濕法疏水性增強矽石替換為40份濕法疏水性增強矽石。此膜狀熱固性聚矽氧密封材料(IV)之特性展示於表1中。
以與實際實例1中相同之方式製備膜狀熱固性聚矽氧密封材料(V),除了在實際實例1中另外添加15份平均顆粒直徑為5μm之石英粉
作為半增強填料外。此膜狀熱固性聚矽氧密封材料(V)之特性展示於表1中。
將附接至壓縮成型設備之上部模具及下部模具加熱至150℃。切出圓頂形狀之模具用作下部模具。將上面安裝有LED晶片之基板設置於上部模具中使得LED晶片面朝下方。剝離附接至膜狀熱固性聚矽氧密封材料(I)之兩側之保護膜及基膜。將由四氟乙烯樹脂(ETFE)製成之脫模膜(AFLEX 50LM)設置於下部模具上,且藉由氣流抽吸來吸附脫模膜。將膜狀熱固性聚矽氧密封材料(I)安置於脫模膜上,且不經真空處理對準上部及下部模具。隨後在將基板夾於上部及下部模具之間之狀態下,在150℃施加3MPa之負荷來進行壓縮成型,持續5分鐘。隨後,自模具中移除樹脂密封之基板且於150℃之烘箱中熱處理一小時。獲得圓頂狀聚矽氧塗層。觀測所獲得之聚矽氧密封LED之外觀以監測存在或不存在溢出、空隙及接線變形。另外,施加電流至所獲得之聚矽氧密封LED,且以肉眼監測存在或不存在發光亮度之減小。
以與實際實例6中相同之方式進行壓縮成型測試,除了進行真空處理持續10秒。其他成型條件展示於表2中。
黏度為2,900mPa.s之液體聚矽氧密封材料係藉由均一混合以下各物來製備:60份由以下平均單元式表示之支鏈有機聚矽氧烷(乙烯基含量=5.6質量%,苯基在所有矽鍵結有機基團中之含量比=50mol%):(PhSiO3/2)0.75(ViMe2SiO1/2)0.25
(其中Ph表示苯基且Vi表示乙烯基),15份兩分子末端均以二甲基乙烯基矽烷氧基(乙烯基含量=1.5質
量%,苯基在所有矽原子鍵結有機基團中之含量比=49mol%)封端之甲基苯基聚矽氧烷、23份由以下式表示之直鏈有機聚矽氧烷(矽鍵結氫原子含量=0.60質量%,苯基在所有矽原子鍵結有機基團中之含量比=33mol%):HMe2SiO(Ph2SiO)SiMe2H
(其中Me表示甲基),2份由以下式表示之直鏈有機聚矽氧烷(矽鍵結氫原子含量=0.65質量%,苯基在所有矽原子-鍵結有機基團中之含量比=25mol%,數量平均分子量=2,260):(PhSiO3/2)0.60(HMe2SiO1/2)0.40
1份鉑之1,3-二乙烯基-1,1,3,3-四甲基二矽氧烷錯合物(在此組合物中,鉑金屬在錯合物中之量就質量單位而言為2.5ppm),及0.05份2-苯基-3-丁炔-2-醇。
在壓縮成型設備之上部模具上安置玻璃環氧基板。隨後,安置於下部模具上由四氟乙烯樹脂製成之脫模膜藉由氣流抽吸密閉附接至下部模具。在施加1.4mL製備之樣品至脫模膜之後,上部及下部模具得到對準。隨後在將基板夾於上部及下部模具之間之狀態下,在120℃不經真空處理,施加3MPa之負荷來進行壓縮成型,持續5分鐘。隨後,自模具中移除樹脂密封之基板且於150℃之烘箱中熱處理一小時。
以與比較實例1中相同之方式進行成型測試,除了進行真空處理持續10秒外。其他成型條件展示於表2中。
將量測裝置(Rheometry,MDR 2000P,根據Alpha技術製造)之溫
度設定至量測溫度。為了防止試片與模具接觸,製成薄膜(由Toray Industries,Inc.製造之Lumirror,25μm)以自上面及下面夾試片。將6g之試片設置於由固定下部模具及升/降上部模具構成之模具之盤狀中空部分。密閉密封上部及下部模具,且在1.66Hz之頻率及1°之振盪角之條件下,記錄緊接著密閉密封之後(0秒之固化時間)的扭矩值作為初始扭矩值。結果展示於表2中。
此外,記錄在高達300秒之成型時間之扭矩最小值作為最小扭矩。結果展示於表2中。
如在表1中所示,使用膜狀聚矽氧密封材料,在實際實例6至14中並不存在溢出或液體排放過程,因此無空隙產生。即使當溫度變化時亦有可能獲得良好圓頂形狀。另一方面,在比較實例1至4中使用液體聚矽氧密封材料,當未進行液體之真空處理時產生空隙。另外,當進行真空處理時出現溢出。此外,當固化時間較短或溫度太低時,液體聚矽氧密封材料未充分固化,因此未獲得良好圓頂形狀。
當使用膜狀聚矽氧密封材料(III)進行成型時,產生具有較弱發光強度之LED晶片。此可能係由於在LED之線接合中之變形。在使用具有較低可見光透射率之聚矽氧密封材料(V)之實際實例14中,LED之發光強度較弱。
將附接至壓縮成型設備之上部模具及下部模具加熱至100℃。切出圓頂形狀之模具用作下部模具。將上面安裝有LED晶片之基板設置於上部模具中使得LED晶片面朝下方。剝離附接至膜狀熱固性聚矽氧密封材料(I)之單側之保護性塑膠膜(由Toray Industries,Inc.製造之2500H Torayfan,60μm厚)。使得剝離膜之表面面朝裝置側,且將具有殘餘塑膠膜(由Toray Industries,Inc.製造之2500H Torayfan,60μm厚)之側安置於模具上。對準上部及下部模具,且在將基板夾於上部及下部模具之間之狀態下,在100℃施加3MPa之負荷來進行壓縮成型,持續5分鐘。隨後,自模具中移除樹脂密封之基板且於150℃之烘箱中熱處理一小時。獲得在聚矽氧密封材料之頂部附接有塑膠膜之LED。當觀測所獲得之LED之外觀以監測存在或不存在溢出、空隙、接線變形及發光亮度之減小時,LED在所有方面均令人滿意。將此LED在80℃在硫氛圍中靜置4小時,且當監測LED之銀電極由於硫腐蝕之變色時,並未觀測到變色。
與此對比,將除了塑膠膜附接至膜狀熱固性聚矽氧密封材料(I)
之兩側外以與上述相同之方式所得到之LED剝離。當觀測所獲得之LED之外觀以監測存在或不存在溢出、空隙、接線變形及發光亮度之減小時,LED在所有方面均令人滿意。將LED在80℃在硫氛圍中靜置4小時,且當監測LED之銀電極由於硫腐蝕之變色時,銀電極變為暗紅-棕色。
當分別量測在150℃下固化1小時之後厚度為1mm之膜狀聚矽氧密封材料及塑膠膜層之透濕性時,獲得以下值。可以確定,藉由將透濕性不超過10g/m2/24hr之塑膠膜附接至密封材料之頂部可獲得具有良好抗硫腐蝕特性之LED裝置。
實際實例之塑膠膜層(60μm厚):7g/m2/24hr。
膜狀聚矽氧密封材料(膜狀聚矽氧密封材料(I)):93g/m2/24hr。
實際實例之塑膠膜層及密封材料:4g/m2/24hr。
Claims (13)
- 一種膜狀熱固性聚矽氧密封材料,其用於藉助於壓縮成型密封半導體元件,該密封材料具有如藉由動模流變儀(MDR)在室溫至200℃之成型溫度所量測,小於15dN.m之初始扭矩值。
- 如請求項1之膜狀熱固性聚矽氧密封材料,其中如藉由MDR所量測,在300秒內之最小扭矩值不超過10dN.m。
- 如請求項1之膜狀熱固性聚矽氧密封材料,其中如JIS K 6249中所規定,在25℃之威廉斯(Williams)塑性值為200至800。
- 如請求項1之膜狀熱固性聚矽氧密封材料,其中在25℃之生強度為0.01至0.6MPa。
- 如請求項1之膜狀熱固性聚矽氧密封材料,其中在1mm之厚度之可見光透射率為至少50%。
- 如請求項1之膜狀熱固性聚矽氧密封材料,該密封材料包含膜狀聚矽氧組合物,其包含:(A)100質量份含烯基有機聚矽氧烷生橡膠;(B)30至150質量份濕法疏水性增強矽石,其具有至少200m2/g之BET法比表面積,該矽石包含選自由R3SiO1/2單元、R2SiO2/2單元、RSiO3/2單元(其中R各自獨立地為單價烴基)及其混合物組成之群之有機聚矽氧烷單元及SiO4/2單元(該等有機聚矽氧烷單元與該等SiO4/2單元之莫耳比為0.08至2.0);(C)0.1至10質量份有機含氫聚矽氧烷;及(D)用於固化該組合物之足量固化劑;或該密封材料係藉由固化該聚矽氧組合物至B-階段所產生。
- 如請求項1至6中任一項之膜狀熱固性聚矽氧密封材料,其在至少一側上具有膜。
- 如請求項7之膜狀熱固性聚矽氧密封材料,其中該膜之透濕性不超過10g/m2/24hr。
- 一種生產LED之方法,其藉助於使用如請求項1至6中任一項之膜狀熱固性聚矽氧密封材料壓縮成型來實現。
- 一種藉助於壓縮成型生產LED之方法,其中在密封材料之表面上具有膜,該LED包含如請求項7之在一側上具有膜之膜狀熱固性聚矽氧密封材料。
- 如請求項10之方法,其中該膜之透濕性不超過10g/m2/24hr。
- 一種LED,其包含LED晶片、覆蓋該晶片之膜狀熱固性聚矽氧密封材料之固化產品及覆蓋該固化產品之表面之膜。
- 如請求項12之LED,其中該膜之透濕性不超過10g/m2/24hr。
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EP (1) | EP2844700A1 (zh) |
JP (1) | JP2013232580A (zh) |
KR (1) | KR20150005662A (zh) |
CN (1) | CN104271675A (zh) |
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WO (1) | WO2013165010A1 (zh) |
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JP2015126124A (ja) * | 2013-12-26 | 2015-07-06 | 日東電工株式会社 | 半導体パッケージの製造方法 |
JP2017536448A (ja) * | 2014-10-29 | 2017-12-07 | テーザ・ソシエタス・ヨーロピア | 多官能性シロキサン水捕捉剤を含む接着剤 |
CN107251665B (zh) * | 2015-03-05 | 2018-06-15 | 住友电木株式会社 | 密封用树脂组合物、车载用电子控制单元的制造方法和车载用电子控制单元 |
US20160257819A1 (en) * | 2015-03-06 | 2016-09-08 | Prc-Desoto International Incorporated | Partially reacted silane primer compositions |
CN107134521A (zh) * | 2016-02-26 | 2017-09-05 | 光宝光电(常州)有限公司 | 光电半导体装置 |
JP6884979B2 (ja) * | 2016-03-09 | 2021-06-09 | 株式会社スリーボンド | 硬化性樹脂組成物、燃料電池およびシール方法 |
EP3486288B1 (en) * | 2016-07-14 | 2021-10-20 | ThreeBond Co., Ltd. | Curable resin composition, cured product, fuel cell, sealing agent and sealing method |
EP3517577A4 (en) | 2016-09-26 | 2020-05-06 | Dow Toray Co., Ltd. | CURABLE REACTIVE SILICONE GEL AND USE THEREOF |
WO2018056298A1 (ja) * | 2016-09-26 | 2018-03-29 | 東レ・ダウコーニング株式会社 | 積層体、その製造方法および電子部品の製造方法 |
JP6622171B2 (ja) * | 2016-11-08 | 2019-12-18 | 信越化学工業株式会社 | 加熱硬化型シリコーン組成物、ダイボンド材及び光半導体装置 |
WO2018186165A1 (ja) | 2017-04-06 | 2018-10-11 | 東レ・ダウコーニング株式会社 | 液状硬化性シリコーン接着剤組成物、その硬化物およびその用途 |
WO2020138411A1 (ja) | 2018-12-27 | 2020-07-02 | ダウ・東レ株式会社 | トランスファー成型用硬化性シリコーン組成物、その硬化物、およびその製造方法 |
EP3979309A4 (en) * | 2019-05-31 | 2023-06-07 | Dow Toray Co., Ltd. | CURABLE ORGANOPOLYSILOXA COMPOSITION AND OPTICAL ELEMENT MADE THEREOF |
JP2021021058A (ja) * | 2019-07-30 | 2021-02-18 | デュポン・東レ・スペシャルティ・マテリアル株式会社 | ホットメルト性硬化性シリコーン組成物、封止剤、フィルム、光半導体素子 |
US11173692B2 (en) | 2019-12-19 | 2021-11-16 | Prc-Desoto International, Inc. | Free radical polymerizable adhesion-promoting interlayer compositions and methods of use |
US11608458B2 (en) | 2019-12-19 | 2023-03-21 | Prc-Desoto International, Inc. | Adhesion-promoting interlayer compositions containing organic titanates/zirconates and methods of use |
US11624007B2 (en) | 2020-01-29 | 2023-04-11 | Prc-Desoto International, Inc. | Photocurable adhesion-promoting compositions and methods of use |
EP4181183A4 (en) * | 2020-07-13 | 2024-08-21 | Dow Toray Co Ltd | SILICONE GEL COMPOSITION, CURED ARTICLE THEREOF, AND APPLICATIONS THEREOF |
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US4418165A (en) | 1980-06-03 | 1983-11-29 | Dow Corning Corporation | Optically clear silicone compositions curable to elastomers |
US4344800A (en) | 1980-06-03 | 1982-08-17 | Dow Corning Corporation | Method for producing hydrophobic reinforcing silica fillers and fillers obtained thereby |
JPH07226414A (ja) * | 1994-02-10 | 1995-08-22 | Toshiba Corp | 半導体素子の樹脂封止方法および樹脂封止型半導体装置 |
JPH08120177A (ja) * | 1994-10-20 | 1996-05-14 | Toray Dow Corning Silicone Co Ltd | シリコーンゴム組成物 |
JP3420473B2 (ja) * | 1997-04-30 | 2003-06-23 | 東レ・ダウコーニング・シリコーン株式会社 | シリコーン系接着性シート、その製造方法、および半導体装置 |
JPH11209735A (ja) * | 1998-01-28 | 1999-08-03 | Dow Corning Toray Silicone Co Ltd | フイルム状シリコーンゴム接着剤及び接着方法 |
JP4875245B2 (ja) * | 2001-03-29 | 2012-02-15 | 東レ・ダウコーニング株式会社 | 建材用ガラスと建材用金具の接合方法 |
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JP5101788B2 (ja) * | 2003-12-22 | 2012-12-19 | 東レ・ダウコーニング株式会社 | 半導体装置の製造方法および半導体装置 |
JP4676735B2 (ja) * | 2004-09-22 | 2011-04-27 | 東レ・ダウコーニング株式会社 | 光半導体装置の製造方法および光半導体装置 |
JP4741230B2 (ja) * | 2004-12-28 | 2011-08-03 | 東レ・ダウコーニング株式会社 | フィルム状シリコーンゴム接着剤 |
JP2008163060A (ja) * | 2006-12-26 | 2008-07-17 | Shindo Seni Kogyo Kk | 繊維質基材の被覆・含浸処理用シリコーンゴム形成性エマルション組成物およびシリコーンゴムで被覆・含浸処理された繊維質基材の製造方法 |
JP2008227119A (ja) | 2007-03-13 | 2008-09-25 | Shin Etsu Chem Co Ltd | 発光ダイオードチップとレンズとの一体化構造物及びその製造方法 |
JP4927019B2 (ja) | 2007-04-10 | 2012-05-09 | 信越化学工業株式会社 | 蛍光体含有接着性シリコーン組成物、該組成物からなる組成物シート、及び該シートを使用する発光装置の製造方法 |
JP5555989B2 (ja) * | 2008-08-08 | 2014-07-23 | 横浜ゴム株式会社 | シリコーン樹脂組成物、これを用いるシリコーン樹脂および光半導体素子封止体 |
JP4877381B2 (ja) * | 2008-12-16 | 2012-02-15 | 横浜ゴム株式会社 | シラノール縮合触媒、加熱硬化性光半導体封止用シリコーン樹脂組成物およびこれを用いる光半導体封止体 |
JP2010192624A (ja) * | 2009-02-17 | 2010-09-02 | Showa Denko Kk | 発光装置及び発光モジュール |
JP2011219597A (ja) * | 2010-04-08 | 2011-11-04 | Nitto Denko Corp | シリコーン樹脂シート |
JP5455065B2 (ja) * | 2010-06-22 | 2014-03-26 | 信越化学工業株式会社 | シクロアルキル基含有シリコーン樹脂組成物及び該組成物の使用方法。 |
JP2012082320A (ja) * | 2010-10-12 | 2012-04-26 | Nitto Denko Corp | 半硬化状シリコーン樹脂シート |
-
2012
- 2012-05-01 JP JP2012104531A patent/JP2013232580A/ja active Pending
-
2013
- 2013-04-23 EP EP13722865.6A patent/EP2844700A1/en not_active Withdrawn
- 2013-04-23 KR KR1020147033054A patent/KR20150005662A/ko not_active Application Discontinuation
- 2013-04-23 CN CN201380022964.XA patent/CN104271675A/zh active Pending
- 2013-04-23 WO PCT/JP2013/062688 patent/WO2013165010A1/en active Application Filing
- 2013-04-23 US US14/397,688 patent/US20150115311A1/en not_active Abandoned
- 2013-04-30 TW TW102115517A patent/TW201350543A/zh unknown
-
2016
- 2016-04-22 US US15/136,156 patent/US20160240753A1/en not_active Abandoned
Also Published As
Publication number | Publication date |
---|---|
KR20150005662A (ko) | 2015-01-14 |
JP2013232580A (ja) | 2013-11-14 |
US20150115311A1 (en) | 2015-04-30 |
WO2013165010A1 (en) | 2013-11-07 |
EP2844700A1 (en) | 2015-03-11 |
CN104271675A (zh) | 2015-01-07 |
US20160240753A1 (en) | 2016-08-18 |
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