TWI658090B - 密封用樹脂組成物及密封用薄片 - Google Patents
密封用樹脂組成物及密封用薄片 Download PDFInfo
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- TWI658090B TWI658090B TW103138713A TW103138713A TWI658090B TW I658090 B TWI658090 B TW I658090B TW 103138713 A TW103138713 A TW 103138713A TW 103138713 A TW103138713 A TW 103138713A TW I658090 B TWI658090 B TW I658090B
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- TXMIUMUSEKVUBH-UHFFFAOYSA-M tetrabutylphosphanium;2,2,2-trifluoroacetate Chemical compound [O-]C(=O)C(F)(F)F.CCCC[P+](CCCC)(CCCC)CCCC TXMIUMUSEKVUBH-UHFFFAOYSA-M 0.000 description 1
- GFZMLBWMGBLIDI-UHFFFAOYSA-M tetrabutylphosphanium;acetate Chemical compound CC([O-])=O.CCCC[P+](CCCC)(CCCC)CCCC GFZMLBWMGBLIDI-UHFFFAOYSA-M 0.000 description 1
- WHDWTYUVZOXXKX-UHFFFAOYSA-M tetrabutylphosphanium;formate Chemical compound [O-]C=O.CCCC[P+](CCCC)(CCCC)CCCC WHDWTYUVZOXXKX-UHFFFAOYSA-M 0.000 description 1
- DFQPZDGUFQJANM-UHFFFAOYSA-M tetrabutylphosphanium;hydroxide Chemical compound [OH-].CCCC[P+](CCCC)(CCCC)CCCC DFQPZDGUFQJANM-UHFFFAOYSA-M 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- AYEKOFBPNLCAJY-UHFFFAOYSA-O thiamine pyrophosphate Chemical compound CC1=C(CCOP(O)(=O)OP(O)(O)=O)SC=[N+]1CC1=CN=C(C)N=C1N AYEKOFBPNLCAJY-UHFFFAOYSA-O 0.000 description 1
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 150000004992 toluidines Chemical class 0.000 description 1
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- VTHOKNTVYKTUPI-UHFFFAOYSA-N triethoxy-[3-(3-triethoxysilylpropyltetrasulfanyl)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCSSSSCCC[Si](OCC)(OCC)OCC VTHOKNTVYKTUPI-UHFFFAOYSA-N 0.000 description 1
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Abstract
本發明以提供耐透溼性、接著強度及透過性皆良好的密封用樹脂組成物為目的。該目的藉由相對(A)環氧樹脂80質量份,含有(B)燒成菱水鎂鋁石3~38質量份、(C)滑石1~16質量份、及(D)二氧化矽1~16質量份之樹脂組成物而達成。
Description
本發明係關於密封用樹脂組成物及密封用薄片,尤其關於宜用在有機EL(Electroluminescence)元件等之發光元件及太陽電池等之受光元件等之光電變換元件之密封等的密封用樹脂組成物及密封用薄片。
有機EL(Electroluminescence)元件為發光材料使用有機物質的發光元件,因可在低電壓得到高亮度之發光,在近年受到注目。然而,有機EL元件有對水分極弱,發光材料(發光層)因水分而變質,亮度降低,變得不發光,電極與發光層之界面因水分影響而剝離、金屬氧化而高電阻化的問題。因此,為使元件內部隔絕外界中之水分,進行例如將形成於基板上的發光層全面被覆,形成樹脂組成物構成的密封層,以將有機EL元件密封。
然而,用於如此之有機EL元件之密封的樹脂組成物,不僅高障壁性(耐透溼性),高接著強度亦為必要,又,在從密封面(密封層之表面)取出光的場合,追求高透過性。以往作為此種樹脂組成物,為實現高障壁性
與高接著強度,提案於樹脂組成物含有滑石或氧化鈣、氧化鎂、氧化鍶、氧化鋇等之吸溼性金屬氧化物的粒子(例如專利文獻1:特開2011-84667號公報)。但是,使用該吸溼性金屬氧化物,則因喪失樹脂組成物的透過性,無法得到高透過性。
〔專利文獻1〕特開2011-84667號公報
本發明為有鑑於上述般實情而成者,其欲解決課題為提供耐透溼性、接著強度及透過性皆良好的密封用樹脂組成物。
本發明者,為解決上述課題,努力研究結果,發現使菱水鎂鋁石燒成粉體、滑石及二氧化矽,各自相對環氧樹脂以特定量搭配的組成物,可成為耐透溼性、接著強度及透過性皆良好的樹脂組成物,完成本發明。
即,本發明具有以下特徵。
〔1〕一種密封用樹脂組成物,其為含有(A)環氧樹脂、(B)燒成菱水鎂鋁石、(C)滑石及(D)二氧化矽之密封用樹脂組成物,其特徵係
相對(A)環氧樹脂80質量份,(B)為3~38質量份、(C)為1~16質量份及(D)為1~16質量份。
〔2〕如上述〔1〕記載之樹脂組成物,其中,(A)環氧樹脂之透過率為90%以上。
〔3〕如上述〔1〕或〔2〕記載之樹脂組成物,其中,相對(A)環氧樹脂80質量份,再含有(E)熱可塑性樹脂1~40質量份。
〔4〕如上述〔3〕記載之樹脂組成物,其中,(E)熱可塑性樹脂為苯氧樹脂。
〔5〕如上述〔3〕或〔4〕記載之樹脂組成物,其中,(E)熱可塑性樹脂之透過率為90%以上。
〔6〕如上述〔1〕~〔5〕中任1項記載之樹脂組成物,其中,相對(A)環氧樹脂80質量份,再含有(F)表面處理劑0.1~3質量份。
〔7〕如上述〔6〕記載之樹脂組成物,其中,(F)表面處理劑為矽烷耦合劑。
〔8〕如上述〔1〕~〔7〕中任1項記載之樹脂組成物,其中,該樹脂組成物的硬化物之透過率為84%以上。
〔9〕如上述〔1〕~〔8〕中任1項記載之樹脂組成物,其中,相對(A)環氧樹脂80質量份,再含有(G)硬化劑0.1~3質量份。
〔10〕如上述〔9〕記載之樹脂組成物,其中,(G)硬化劑為離子液體。
〔11〕一種密封用薄片,其特徵係由上述〔1〕~
〔10〕中任1項記載之樹脂組成物的層形成於支持體上而成。
根據本發明,可得到障壁性(耐透溼性)、接著強度及透過性皆良好的密封用樹脂組成物。因此,將本發明之密封用樹脂組成物用於例如有機EL元件等之發光元件之密封,則元件內部與外界中之水分可確實且長期阻隔,發光動作長期安定化,並且可實現能由密封面有效率地取出光之發光元件。
又,本發明之密封用樹脂組成物,因障壁性(耐透溼性)、接著強度及透過性皆為良好,亦宜用在例如將在太陽電池面板之玻璃與背部薄片間所挾持的太陽電池單元之矽等之半導體固定於玻璃板、保護遠離溼氣用的密封材等。因此,本發明之密封用樹脂組成物不僅發光元件,且可用作為包含太陽電池等之受光元件的光電變換元件之密封用。
〔圖1〕以耐透溼性試驗評估為耐透溼性良好的浸水域之代表照片。
〔圖2〕以耐透溼性試驗評估為耐透溼性尚可的浸水域之代表照片。圖中之包圍線係為了特定浸水域所附的
線。
〔圖3〕以耐透溼性試驗評估為耐透溼性不良的浸水域之代表照片。圖中之包圍線係為了特定浸水域所附的線。
以下將本發明以其適宜之實施形態詳細說明。
本發明之密封用樹脂組成物為含有(A)環氧樹脂、(B)燒成菱水鎂鋁石、(C)滑石及(D)二氧化矽之組成物,且以
相對(A)環氧樹脂80質量份,(B)為3~38質量份、(C)為1~16質量份及(D)為1~16質量份為主要特徵。
在本發明使用的環氧樹脂為平均每1分子具有2個以上之環氧基,且透過率高者,則無限制皆可使用。例如雙酚A型環氧樹脂、聯苯基型環氧樹脂、聯苯基芳烷基型環氧樹脂、萘酚型環氧樹脂、萘型環氧樹脂、雙酚F型環氧樹脂、含磷環氧樹脂、雙酚S型環氧樹脂、芳香族縮水甘
油基胺型環氧樹脂(例如四縮水甘油基二胺基二苯基甲烷、三縮水甘油基-p-胺基酚、二縮水甘油基甲苯胺、二縮水甘油基苯胺等)、脂環式環氧樹脂、脂肪族鏈狀環氧樹脂、酚酚醛清漆型環氧樹脂、甲酚酚醛清漆型環氧樹脂、雙酚A酚醛清漆型環氧樹脂、具有丁二烯構造的環氧樹脂、雙酚之二縮水甘油基醚化物、萘二醇之二縮水甘油基醚化物、酚類之縮水甘油基醚化物、及醇類之二縮水甘油基醚化物、以及此等之環氧樹脂的烷基取代體、鹵素化物及氫化物等。該環氧樹脂可使用任1種或2種以上混合使用。本發明中之環氧樹脂可使用重量平均分子量未達15000者。
環氧樹脂中以透過率為80%以上者為佳、透過率為85%以上者更佳、透過率為90%以上者特別佳。該適宜之環氧樹脂,可舉例如雙酚A型環氧樹脂、雙酚F型環氧樹脂、酚酚醛清漆型環氧樹脂、聯苯基芳烷基型環氧樹脂、脂環式環氧樹脂、脂肪族鏈狀環氧樹脂等。
又,本發明中所謂透過率係指全光線透過率,為考慮以調查通過材料有何種程度亮度傳遞之目的所測定的反射或散射之光線透過率。入射光以利用可見光線或紫外線,將透過的光以積分球收集之方法測定。具體上可使用纖維式分光光度計(例如MCPD-7700、大塚電子公司製),對試料(絕緣層厚20μm)照射鹵素燈之入射光,將以8°投光之60mm積分球收光的全光線透過率頻譜之450nm值以空氣為對照所測定的值作為本發明中之
透過率。
如後述詳述,本發明之樹脂組成物,以直接塗佈於密封對象物,使該塗膜硬化而形成密封層之態樣外,尚有以本發明之樹脂組成物與溶劑混合作成塗漆,使該塗漆塗佈於支持體上、進行乾燥,製作形成有本發明之樹脂組成物的層之密封用薄片,並使密封用薄片與密封對象物層合後進行密封之態樣使用。
環氧樹脂可為液狀、或固形狀、或使用液狀與固形狀兩者。在此,「液狀」及「固形狀」係指在常溫(25℃)之環氧樹脂的狀態。由塗佈性、加工性、接著性觀點,以使用的環氧樹脂全體之至少10質量%以上為液狀者為佳。
又,環氧樹脂,由反應性觀點,環氧當量以100~1000g/eq之範圍為佳、120~1000g/eq之範圍更佳、150~1000g/eq之範圍再更佳。又,「環氧當量」係指含1公克當量的環氧基之樹脂的公克數(g/eq),且以JIS K 7236規定的方法測定。
本發明之樹脂組成物中之環氧樹脂的含量,每樹脂組成物(不揮發分)全體,以20~80質量%為佳、30~70質量%之範圍者更佳、50~65質量%之範圍者又更佳。
本發明之樹脂組成物含有燒成菱水鎂鋁石。
燒成菱水鎂鋁石為天然菱水鎂鋁石(Mg6Al2(OH)16CO3.4H2O)及/或合成的菱水鎂鋁石(菱水鎂鋁石樣化合物)之燒成者。合成的菱水鎂鋁石(菱水鎂鋁石樣化合物),例如下述一般式(I)所表示之複氫氧化物、下述一般式(II)所表示之複氫氧化物等。
【化1】式(I):[M2+ 1-xM3+ x(OH)2]x+‧[(An-)x/n‧mH2O]x-
(式中,M2+為Mg2+、Zn2+等之2價金屬離子,M3+為Al3+、Fe3+等之3價金屬離子,An-為CO3 2-、Cl-、NO3 -等之n價陰離子,0<x<1,0≦m<1,n為正數。)
【化2】式(II):M2+ xAl2(OH)2x+6-nz(An-)z‧mH2O
(式中,M2+為Mg2+、Zn2+等之2價金屬離子,An-為CO3 2-、Cl-、NO3 -等之n價陰離子,x為2以上之正數,z為2以下之正數,m為正數,n為正數。)
即,「燒成菱水鎂鋁石」為將天然菱水鎂鋁石(Mg6Al2(OH)16CO3.4H2O)及/或合成的菱水鎂鋁石(菱水鎂鋁石樣化合物)燒成,使層間陰離子與水分子氣化而得到的複合氧化物,較佳為以400~900℃、更佳為500~700℃、30分鐘~5小時、更佳為30分鐘~3小時、再較佳為45分鐘~2小時進行燒成而得到的複合氧化物。
較佳的燒成菱水鎂鋁石為使上述式(II)之複氫氧化物等之Mg-Al系菱水鎂鋁石樣化合物燒成而得到的Mg-Al系複合氧化物,該Mg-Al系複合氧化物,以Mg與Al之組成比為Mg:Al=x:2時之x為2≦x≦6的組成比的複合氧化物更佳、該x為3≦x≦6的組成比的複合氧化物再佳、該x為4≦x≦6的組成比的複合氧化物特別佳。
本發明中使用的燒成菱水鎂鋁石,由樹脂組成物的透過性、吸溼性觀點,以使用粒徑小者為佳。一般認為粉體狀態之燒成菱水鎂鋁石,其多成為一次粒子凝集的二次粒子,因一次粒子之平均粒徑測定比較困難,故藉由使BET比表面積為特定值,可以本發明作成適宜之燒成菱水鎂鋁石。適宜之BET比表面積為5~200m2/g,以10~150m2/g更佳。
BET比表面積,係藉由BET法,使用比表面積測定裝置(Macsorb HM Model-1210(股)Mountek製),於試料表面吸附氮氣體,使用BET多點法算出比表面積而得到。燒成菱水鎂鋁石的BET比表面積之調整,可將燒成前的菱水鎂鋁石粉碎、分級,或使菱水鎂鋁石的燒成體(燒成菱水鎂鋁石)粉碎、分級,或者組合此等兩者進行。
燒成菱水鎂鋁石因燒成而多孔化,故入射於樹脂組成物內的光因燒成菱水鎂鋁石的存在而其散射性變高、透過性提升而有利於作用。
本發明之樹脂組成物中,(B)燒成菱水鎂鋁
石的含量,相對(A)環氧樹脂80質量份為3~38質量份,由耐透溼性、透過性觀點,較佳為5~35質量份,更佳為10~35質量份。搭配量過少,則耐透溼性有降低傾向、透過率降低傾向。
又,(B)燒成菱水鎂鋁石的含量,相對樹脂組成物(不揮發分)全體,以2~24質量%為佳、5~23質量%之範圍者更佳。
本發明之樹脂組成物含有滑石。滑石特別賦予樹脂組成物接著強度提升,少量的搭配可使樹脂組成物的接著強度大幅提升。滑石的平均粒徑,由接著強度、透過率觀點,以0.5~2μm為佳、0.8~1.5μm更佳。
滑石的平均粒徑可藉由基於米氏(Mie)散射理論之雷射衍射‧散射法測定。具體上藉由雷射衍射散射式粒度分佈測定裝置,將無機充填材的粒度分佈以體積基準製作,以其中位直徑為平均粒徑來測定。測定樣本,宜使用將無機充填材以超音波分散於水中者。雷射衍射散射式粒度分佈測定裝置,可使用(股)堀場製作所製LA-500。
本發明之樹脂組成物中,(C)滑石的含量,相對(A)環氧樹脂80質量份為1~16質量份,尤其由維持樹脂組成物的接著強度及透過率在高程度觀點,以1~10質量份為佳、更佳為2~8質量份。滑石的搭配量過
少,則有接著強度降低傾向,過多則有透過率降低傾向。
又,(C)滑石的含量,相對樹脂組成物(不揮發分)全體,以0.5~12質量%為佳、1.0~11質量%之範圍者更佳。
本發明之樹脂組成物含有二氧化矽。二氧化矽尤其賦予樹脂組成物耐透溼性及透過率提升,以少量的搭配可不使樹脂組成物的接著強度降低而使耐透溼性及透過率提升。二氧化矽,以一次粒子之粒徑為奈米等級之所謂奈米二氧化矽為佳。一次粒子之粒徑為1~100nm者更佳、1~50nm者更佳、10~20nm者更佳、10~15nm者更佳。因奈米二氧化矽1次粒子徑之測定比較困難,固有使用由比表面積測定值(依據JIS Z8830)之換算值的情形。即使在適合本發明之二氧化矽,藉由使BET比表面積為特定值,而可作成更適合本發明之二氧化矽。適宜之BET比表面積為2720~27m2/g,2720~54m2/g者更佳、272~136m2/g者更佳、272~181m2/g者更佳。
二氧化矽雖可使用溼式二氧化矽、乾式二氧化矽、膠體二氧化矽(水分散型、有機溶劑分散型、氣相二氧化矽等)等之任一,但由不易沈澱、沈降、易與樹脂複合化觀點,以膠體二氧化矽為佳、有機溶劑分散型膠體二氧化矽(有機二氧化矽溶膠)特別佳。具體上作為球狀膠體二氧化矽,有日產化學工業公司製之SNOWTEX-C、
SNOWTEX-O、SNOWTEX-N、SNOWTEX-S、SNOWTEX-OL、SNOWTEX-XS、SNOWTEX-XL、MP1040等,作為分散於有機溶劑的有機二氧化矽溶膠,除IPA-ST、MEK-ST、IPA-ST-ZL等之一般等級外,尚有MEK-EC、MEK-AC、PGM-AC等之表面改質等級。作為鏈狀之膠體二氧化矽,有日產化學工業公司製之SNOWTEX-UP、SNOWTEX-OUP等,作為有機二氧化矽溶膠,有IPA-ST-UP等。作為氣相二氧化矽,有日本AEROSIL公司製之AEROSIL130、AEROSIL200、AEROSIL200CF、AEROSIL300、AEROSIL300CF、AEROSIL380、AEROSILMOX80等。
本發明之樹脂組成物中,(D)二氧化矽之含量,相對(A)環氧樹脂80質量份為1~16質量份,尤其由維持樹脂組成物的接著強度及透過率在高程度觀點,以1~14質量份為佳、更佳為5~12質量份。
又,(D)二氧化矽之含量,每樹脂組成物(不揮發分)全體,以0.5~10質量%為佳、1.0~9質量%之範圍者更佳。
本發明之樹脂組成物,由樹脂組成物的耐透溼性、調製密封薄片時的樹脂組成物塗漆之塗佈性(防止凝起)等之觀點,在不妨礙本發明之效果範圍,可再含有菱水鎂鋁石、滑石及二氧化矽以外之無機充填材。彼般無機充填材,例如氧化鋁、硫酸鋇、黏土、雲母、氫氧化鋁、氫氧化鎂、碳酸鈣、碳酸鎂、氮化硼、硼酸鋁、鈦酸鋇、鈦酸鍶、鈦酸鈣、鈦酸鎂、鈦酸鉍、氧化鈦、鋯酸
鋇、鋯酸鈣等。無機充填材可使用1種或2種以上。
本發明之樹脂組成物含有無機充填材之場合,無機充填材的含量,每樹脂組成物(不揮發分)全體,以30質量%以下者為佳、20質量%以下更佳。
本發明之樹脂組成物,由對樹脂組成物硬化而得到的密封層賦予可撓性、調製密封薄片時的樹脂組成物塗漆之塗佈性(防止凝起)等觀點,可含有熱可塑性樹脂。熱可塑性樹脂,例如苯氧樹脂、聚乙烯縮醛樹脂、聚醯亞胺樹脂、聚醯胺醯亞胺樹脂、聚醚碸樹脂、聚碸樹脂等。此等之熱可塑性樹脂可使用任1種或2種以上混合使用。熱可塑性樹脂,由對樹脂組成物硬化而得到的密封層賦予可撓性、調製密封薄片時的樹脂組成物塗漆之塗佈性(防止凝起)等之點,重量平均分子量以15,000以上者為佳、20,000以上更佳。但是、重量平均分子量過大,則有與環氧樹脂之相溶性降低等之傾向,故重量平均分子量以1,000,000以下者為佳、800,000以下更佳。
又,在此所謂「熱可塑性樹脂的重量平均分子量」為以膠體滲透層析法(GPC)法(聚苯乙烯換算)測定。GPC法之重量平均分子量,具體上可以作為測定裝置使用(股)島津製作所製LC-9A/RID-6A、管柱使用昭和電工(股)製Shodex K-800P/K-804L/K-804L、移動相使用氯仿等,以管柱溫度40℃測定,並使用標準聚苯乙
烯之檢量線算出。
又,熱可塑性樹脂,透過率為80%以上者為佳、透過率為90%以上者更佳。
熱可塑性樹脂在上述例示物中,以苯氧樹脂特別佳。苯氧樹脂與環氧樹脂之相溶性佳,有利於樹脂組成物的透過性、耐透溼性。
苯氧樹脂,可舉例如具有由雙酚A骨架、雙酚F骨架、雙酚S骨架、雙酚苯乙酮骨架、酚醛清漆骨架、聯苯基骨架、茀骨架、二環戊二烯骨架、降冰片烯骨架等所選出之1種以上之骨架者。苯氧樹脂可使用1種或2種以上。
苯氧樹脂的市售品,宜使用例如三菱化學(股)製YL7213B35(含聯苯基骨架苯氧樹脂)、1256(含雙酚A骨架苯氧樹脂)、YX6954BH35(含雙酚苯乙酮骨架苯氧樹脂)等。
本發明之樹脂組成物中,熱可塑性樹脂的含量,每樹脂組成物(不揮發分)全體,以1~40質量%為佳、5~30質量%更佳。
本發明之樹脂組成物中,由樹脂組成物的接著強度提升觀點,可含有表面處理劑。該表面處理劑,例如鈦系耦合劑、鋁系耦合劑、矽烷耦合劑等之耦合劑。耦合劑中以矽烷耦合劑為佳。耦合劑可1種或組合2種以上使用。
矽烷耦合劑,例如3-縮水甘油基氧基丙基三甲氧基矽烷、3-縮水甘油基氧基丙基三乙氧基矽烷、3-縮水甘油基氧基丙基(二甲氧基)甲基矽烷及2-(3,4-環氧基環己基)乙基三甲氧基矽烷等之環氧基系矽烷耦合劑;3-巰基丙基三甲氧基矽烷、3-巰基丙基三乙氧基矽烷、3-巰基丙基甲基二甲氧基矽烷及11-巰基十一基三甲氧基矽烷等之巰基系矽烷耦合劑;3-胺基丙基三甲氧基矽烷、3-胺基丙基三乙氧基矽烷、3-胺基丙基二甲氧基甲基矽烷、N-苯基-3-胺基丙基三甲氧基矽烷、N-甲基胺基丙基三甲氧基矽烷、N-(2-胺基乙基)-3-胺基丙基三甲氧基矽烷及N-(2-胺基乙基)-3-胺基丙基二甲氧基甲基矽烷等之胺基系矽烷耦合劑;3-脲基丙基三乙氧基矽烷等之脲基系矽烷耦合劑;乙烯基三甲氧基矽烷、乙烯基三乙氧基矽烷及乙烯基甲基二乙氧基矽烷等之乙烯基系矽烷耦合劑;p-苯乙烯基三甲氧基矽烷等之苯乙烯基系矽烷耦合劑;3-丙烯醯氧基丙基三甲氧基矽烷及3-甲基丙烯醯氧丙基三甲氧基矽烷等之丙烯酸酯系矽烷耦合劑;3-異氰酸酯丙基三甲氧基矽烷等之異氰酸酯系矽烷耦合劑;雙(三乙氧基矽烷基丙基)二硫化物、雙(三乙氧基矽烷基丙基)四硫化物等之硫化物系矽烷耦合劑;苯基三甲氧基矽烷、甲基丙烯醯氧基丙基三甲氧基矽烷、咪唑矽烷、三嗪矽烷等。此等之中以環氧基系矽烷耦合劑尤佳。
本發明之樹脂組成物中,使用表面處理劑之場合,表面處理劑之含量,每樹脂組成物(不揮發分)全
體,以0.5~10質量%為佳、0.5~5質量%更佳。含有該範圍外的場合,無法得到表面處理劑添加所致之密著性改善效果。
又,本發明中之燒成菱水鎂鋁石、滑石、二氧化矽、其他無機充填材,為了分散性等之提升,可使用以此等表面處理劑進行表面處理者。
本發明之樹脂組成物中,由樹脂組成物硬化而得到的密封層之機械強度之提升或應力緩和等之目的,可含有橡膠粒子。該橡膠粒子以不溶於調製樹脂組成物時的有機溶劑、亦不與環氧樹脂等之樹脂組成物中之成分相溶,在樹脂組成物的塗漆中以分散狀態存在者為佳。如此之橡膠粒子,一般可藉由使橡膠成分的分子量大至不溶於有機溶劑或樹脂程度、且作成粒子狀來調製,具體上可舉例如核殼型橡膠粒子、交聯丙烯腈丁二烯橡膠粒子、交聯苯乙烯丁二烯橡膠粒子、丙烯酸橡膠粒子等。核殼型橡膠粒子為粒子具有核層與殼層之橡膠粒子,例如外層之殼層為玻璃狀聚合物、內層之核層為橡膠狀聚合物所構成的2層構造、或外層之殼層為玻璃狀聚合物、中間層為橡膠狀聚合物、核層為玻璃狀聚合物所構成的3層構造者等。玻璃層為例如以甲基丙烯酸甲基酯之聚合物等所構成,橡膠狀聚合物層為例如以丁基丙烯酸酯聚合物(丁基橡膠)等所構成。核殼型橡膠粒子之具體例,可舉例如StafyroidAC3832、
AC3816N(以上、鋼茲化成(股)製)、Metablen KW-4426(Mitsubishirayon(股)製)、F351(日本zeon(股)製)等。丙烯腈丁二烯橡膠(NBR)粒子之具體例,可舉例如XER-91(JSR(股)製)等。苯乙烯丁二烯橡膠(SBR)粒子之具體例,可舉例如XSK-500(JSR(股)製)等。丙烯酸橡膠粒子之具體例,可舉例如MetablenW300A、W450A(以上、Mitsubishirayon(股)製)。
橡膠粒子之平均粒子徑以0.005~1μm之範圍為佳、0.2~0.6μm之範圍更佳。該橡膠粒子之平均粒子徑可使用動態光散射測定。例如於適當的有機溶劑將橡膠粒子以超音波等均勻分散,使用FPRA-1000(大塚電子(股)製),將橡膠粒子之粒度分佈以質量基準製作,以其中位直徑為平均粒子徑來測定。
本發明之樹脂組成物中,使用橡膠粒子之場合,橡膠粒子之含量,每樹脂組成物(不揮發分)全體,以0.1~20質量%為佳、0.1~10質量%更佳。比0.1質量%少,則無法充分得到搭配橡膠粒子之效果,比20質量%多,則有耐熱性、耐透溼性降低之情形。
本發明之樹脂組成物通常含有環氧樹脂的硬化劑。即,密封層為以使樹脂組成物層硬化的硬化物層得到。硬化劑為具有使環氧樹脂硬化機能者則不特別限定,但由抑
制樹脂組成物的硬化處理時中之有機EL元件等之發光元件之熱劣化觀點,以在140℃以下(較佳為120℃以下)之溫度下使環氧樹脂硬化得到者為佳。
例如一級胺、二級胺、三級胺系硬化劑、聚胺基醯胺系硬化劑、二氰二醯胺、有機酸二醯肼等,但其中由速硬化性點,以胺加成系化合物(AjicurePN-23、AjicureMY-24、AjicurePN-D、AjicureMY-D、AjicurePN-H、AjicureMY-H、AjicurePN-31、AjicurePN-40、AjicurePN-40J等(皆Ajinomoto Fine-Techno Co.,Inc.股份公司製))、有機酸二醯肼(AjicureVDH-J、AjicureUDH、AjicureLDH等(皆Ajinomoto Fine-Techno Co.,Inc.股份公司製))等特別佳。
又,在140℃以下(較佳為120℃以下)之溫度下可使環氧樹脂硬化之離子液體,即為在140℃以下(較佳為120℃以下)之溫度區域可熔解之鹽且具有環氧樹脂的硬化作用之鹽尤其適合作為(G)硬化劑使用。本發明之樹脂組成物中,以於環氧樹脂使該離子液體均勻溶解之狀態使用為佳,又,離子液體有利於樹脂硬化物的耐透溼性提升。
構成該離子液體之陽離子,可舉例如咪唑鎓離子、哌啶鎓離子、吡咯烷鎓離子、吡唑鎓離子、胍鎓離子、吡啶鎓離子等之銨系陽離子;四烷基鏻陽離子(例如四丁基鏻離子、三丁基己基鏻離子等)等之鏻系陽離子;三乙基鋶離子等之鋶系陽離子等。
又,構成該離子液體之陰離子,可舉例如氟化物離子、氯化物離子、溴化物離子、碘化物離子等之鹵素化物系陰離子;甲烷磺酸離子等之烷基硫酸系陰離子;三氟甲烷磺酸離子、六氟膦酸離子、三氟參(五氟乙基)膦酸離子、雙(三氟甲烷磺醯基)醯亞胺離子、三氟乙酸離子、四氟硼酸離子等之含氟化合物系陰離子;酚離子、2-甲氧基酚離子、2,6-二-tert-丁基酚離子等之酚系陰離子;天門冬胺酸離子、麩胺酸離子等之酸性胺基酸離子;甘胺酸離子、丙胺酸離子、苯基丙胺酸離子等之中性胺基酸離子;N-苯甲醯基丙胺酸離子、N-乙醯基苯基丙胺酸離子、N-乙醯基甘胺酸離子等之下述一般式(1)所表示之N-醯基胺基酸離子;甲酸離子、乙酸離子、癸烷酸離子、2-吡咯啶酮-5-羧酸離子、α-硫辛酸離子、乳酸離子、酒石酸離子、馬尿酸離子、N-甲基馬尿酸離子、安息香酸離子等之羧酸系陰離子。
(式中,R-CO-為碳數1~5之直鏈或分支鏈之脂肪酸所衍生的醯基、或者取代或無取代苯甲醯基,X為胺基酸之側鏈。)
該式(1)中之胺基酸,可舉例如例如天門冬胺酸、麩胺酸、甘胺酸、丙胺酸、苯基丙胺酸等,其中以甘胺酸為佳。
上述中,陽離子以銨系陽離子、鏻系陽離子為佳、咪唑鎓離子、鏻離子更佳。咪唑鎓離子更詳細為1-乙基-3-甲基咪唑鎓離子、1-丁基-3-甲基咪唑鎓離子、1-丙基-3-甲基咪唑鎓離子等。
又,陰離子以酚系陰離子、一般式(1)所表示之N-醯基胺基酸離子或羧酸系陰離子為佳、N-醯基胺基酸離子或羧酸系陰離子更佳。
酚系陰離子之具體例,可舉例如2,6-二-tert-丁基酚離子。又,羧酸系陰離子之具體例,可舉例如乙酸離子、癸烷酸離子、2-吡咯啶酮-5-羧酸離子、甲酸離子、α-硫辛酸離子、乳酸離子、酒石酸離子、馬尿酸離子、N-甲基馬尿酸離子等,其中,以乙酸離子、2-吡咯啶酮-5-羧酸離子、甲酸離子、乳酸離子、酒石酸離子、馬尿酸離子、N-甲基馬尿酸離子為佳、乙酸離子、N-甲基馬尿酸離子、甲酸離子尤佳。又,一般式(1)所表示之N-醯基胺基酸離子之具體例,可舉例如N-苯甲醯基丙胺酸離子、N-乙醯基苯基丙胺酸離子、天門冬胺酸離子、甘胺酸離子、N-乙醯基甘胺酸離子等,其中,以N-苯甲醯基丙胺酸離子、N-乙醯基苯基丙胺酸離子、N-乙醯基甘胺酸離子為佳、N-乙醯基甘胺酸離子尤佳。
具體的離子液體,例如1-丁基-3-甲基咪唑鎓
乳酸鹽、四丁基鏻-2-吡咯啶酮-5-羧酸鹽、四丁基鏻乙酸鹽、四丁基鏻癸酸鹽、四丁基鏻三氟乙酸鹽、四丁基鏻α-硫辛酸鹽、甲酸四丁基鏻鹽、四丁基鏻乳酸鹽、酒石酸雙(四丁基鏻)鹽、馬尿酸四丁基鏻鹽、N-甲基馬尿酸四丁基鏻鹽、苯甲醯基-DL-丙胺酸四丁基鏻鹽、N-乙醯基苯基丙胺酸四丁基鏻鹽、2,6-二-tert-丁基酚四丁基鏻鹽、L-天門冬胺酸單四丁基鏻鹽、甘胺酸四丁基鏻鹽、N-乙醯基甘胺酸四丁基鏻鹽、1-乙基-3-甲基咪唑鎓乳酸鹽、1-乙基-3-甲基咪唑鎓乙酸鹽、甲酸1-乙基-3-甲基咪唑鎓鹽、馬尿酸1-乙基-3-甲基咪唑鎓鹽、N-甲基馬尿酸1-乙基-3-甲基咪唑鎓鹽、酒石酸雙(1-乙基-3-甲基咪唑鎓)鹽、N-乙醯基甘胺酸1-乙基-3-甲基咪唑鎓鹽為佳、N-乙醯基甘胺酸四丁基鏻鹽、1-乙基-3-甲基咪唑鎓乙酸鹽、甲酸1-乙基-3-甲基咪唑鎓鹽、馬尿酸1-乙基-3-甲基咪唑鎓鹽、N-甲基馬尿酸1-乙基-3-甲基咪唑鎓鹽尤佳。
上述離子液體之合成法方面,有使由烷基咪唑鎓、烷基吡啶鎓、烷基銨及烷基鋶離子等之陽離子部位與含鹵素之陰離子部位所構成的前驅物,與NaBF4、NaPF6、CF3SO3Na或LiN(SO2CF3)2等反應之陰離子交換法、使胺系物質與酸酯反應邊導入烷基而有機酸殘基成為對陰離子之酸酯法、及使胺類以有機酸中和而得到鹽之中和法等,但不限於此等。在陰離子與陽離子與溶劑之中和法,亦可等量使用陰離子與陽離子,使得到的反應液中之溶劑餾去後直接使用,進而亦可加入有機溶劑(甲醇、甲
苯、乙酸乙基酯、丙酮等)、進行液濃縮。
本發明之樹脂組成物中,硬化劑之含量相對樹脂組成物中所含有之環氧樹脂的總量(不揮發分),以在0.1~50質量%之範圍使用為佳。比該範圍少則有無法得到充分硬化性之虞,比50質量%多,則有損及樹脂組成物的保存安定性之情形。又,使用離子液體的場合,由樹脂組成物的硬化物的耐透溼性等之點,相對環氧樹脂的總量(不揮發分)以0.1~10質量%為佳。
本發明之樹脂組成物中,作為硬化劑使用離子液體的場合,與離子液體同時可含有分子內具有2個以上硫醇基的聚硫醇化合物。藉由含有分子內具有2個以上硫醇基的聚硫醇化合物,可使硬化速度增快。分子內具有2個以上硫醇基的聚硫醇化合物的具體例,例如三羥甲基丙烷參(硫基乙醇酸酯)、季戊四醇肆(硫基乙醇酸酯)、乙二醇二硫基乙醇酸酯、三羥甲基丙烷參(β-硫基丙酸酯)、季戊四醇肆(β-硫基丙酸酯)、二季戊四醇聚(β-硫基丙酸酯)等之多元醇與巰基有機酸之酯化反應而得到的硫醇化合物。該硫醇化合物為製造上不必要使用鹼性物質且分子內具有2個以上硫醇基的硫醇化合物。
又,分子內具有2個以上硫醇基的聚硫醇化合物,可舉例如1,4-丁烷二硫醇、1,6-己烷二硫醇、1,10-癸烷二硫醇等之烷基聚硫醇化合物;含末端硫醇基聚醚;含末端硫醇基聚硫基醚;環氧化合物與硫化氫之反應而得
到的硫醇化合物;聚硫醇化合物與環氧化合物之反應而得到的具有末端硫醇基的硫醇化合物等。又,在環氧化合物與硫化氫之反應而得到的硫醇化合物或聚硫醇化合物與環氧化合物之反應而得到的具有末端硫醇基的硫醇化合物等,作為其製造步驟上之反應觸媒而使用鹼性物質者,以使用進行脫鹼處理,使鹼金屬離子濃度成為50ppm以下者為佳,該脫鹼處理之方法,例如將進行處理之聚硫醇化合物溶於丙酮、甲醇等之有機溶劑,藉由加入稀鹽酸、稀硫酸等之酸進行中和後,以萃取‧洗淨等進行脫鹽之方法或使用離子交換樹脂進行吸附之方法、以蒸餾精製之方法等,但不限於此等。
本發明之樹脂組成物中,使用該聚硫醇化合物的場合,環氧樹脂與聚硫醇化合物的混合比,以SH當量數/環氧當量數計通常以0.2~1.2為佳。比0.2少則有無法得到充分速硬化性之情形,另一方面,比1.2多則有損及耐熱性等之硬化物的物性之情形。由接著性安定觀點以0.5~1.0更佳。
本發明之樹脂組成物,以調整硬化時間等之目的可含有硬化促進劑。硬化促進劑,例如有機膦化合物、咪唑化合物、胺加成化合物(例如於環氧樹脂加成3級胺而使反應在途中停止的環氧基加成化合物等)、3級胺化合物等。有機膦化合物的具體例,可舉例如TPP、TPP-K、
TPP-S、TPTP-S(北興化學工業(股)商品名)等。咪唑化合物的具體例,可舉例如Curezol2MZ、2E4MZ、C11Z、C11Z-CN、C11Z-CNS、C11Z-A、2MZOK、2MA-OK、2PHZ(四國化成工業(股)商品名)等。胺加成化合物的具體例,可舉例如Fujicure(富士化成工業(股)商品名)等。3級胺化合物的具體例,可舉例如DBU(1,8-diazabicyelo[5.4.0]undec-7-ene)、DBU之2-乙基己烷酸鹽、辛基酸鹽等之DBU-有機酸鹽、U-3512T(San-Apro Ltd.製)等之芳香族二甲基脲、U-3503N(San-Apro Ltd.製)等之脂肪族二甲基脲等。其中,由耐溼性點,以脲化合物為佳、芳香族二甲基脲尤宜使用。本發明之樹脂組成物中,硬化促進劑之含量,以樹脂組成物中所含有之環氧樹脂的總量為100質量%(不揮發分)時,通常在0.05~5質量%之範圍使用。未達0.05質量%則有硬化變慢、需要長熱硬化時間之傾向,超過5質量%則有樹脂組成物的保存安定性降低之傾向。
本發明之樹脂組成物,在發揮本發明之效果範圍,可任意含有上述成分以外之各種樹脂添加劑。如此之樹脂添加劑,可舉例如例如矽酮粉末、尼龍粉末、氟粉末等之有機充填劑、Orben、片通等之增黏劑、矽酮系、氟系、高分子系的消泡劑或平坦劑、三唑化合物、噻唑化合物、三嗪化合物、卟啉化合物等之密著性賦予劑等。
本發明之樹脂組成物藉由將搭配成分因應必要進而加入溶劑等,使用混練輪或旋轉混合機等進行混合
來調製。
本發明之樹脂組成物具有高透過率,且形成之密封層(即,樹脂組成物的硬化物)具有較佳為84%以上、更佳為86%以上之透過率。
本發明之樹脂組成物雖可直接塗佈於密封對象物,使該塗膜硬化而形成密封層,亦可製作於支持體上形成有本發明之樹脂組成物的層的密封用薄片,使密封用薄片於密封對象物的必要處層合後,將樹脂組成物層轉印至被覆對象物,進行硬化而形成密封層。
密封用薄片,可藉由該業者習知之方法,例如調製於有機溶劑溶解有樹脂組成物的塗漆,於支持體上塗佈塗漆,進而以加熱、或吹熱風等使有機溶劑乾燥,形成樹脂組成物層來製造。
密封用薄片使用的支持體,可舉例如聚乙烯、聚丙烯、聚氯乙烯等之聚烯烴、聚乙烯對苯二甲酸酯(以下簡稱「PET」。)、聚萘二甲酸乙二醇脂等之聚酯、聚碳酸酯、聚醯亞胺等之塑膠薄膜。塑膠薄膜,尤以PET為佳。支持體除消光處理、電暈處理外,可施以脫模處理。脫模處理,可舉例如以矽酮樹脂系脫模劑、醇酸樹脂系脫模劑、氟樹脂系脫模劑等之脫模劑之脫模處理。
支持體之厚度雖不特別限定,由樹脂組成物薄片之操作性等之觀點,通常為10~150μm,較佳為在20~100μm之範圍使用。
有機溶劑,例如丙酮、甲基乙基酮(以下、
簡稱「MEK」)、環己酮等之酮類、乙酸乙基酯、乙酸丁基酯、溶纖劑乙酸酯、丙二醇單甲基醚乙酸酯、卡必醇乙酸酯等之乙酸酯類、溶纖劑、丁基卡必醇等之卡必醇類、甲苯、二甲苯等之芳香族烴類、二甲基甲醯胺、二甲基乙醯胺、N-甲基吡咯啶酮等。該有機溶劑可任1種單獨使用或2種以上組合使用。
乾燥條件雖不特別限制,通常以50~100℃程度、3~15分鐘程度為宜。
乾燥後所形成的樹脂組成物層之厚度,通常為3μm~200μm、較佳為5μm~100μm、更佳為5μm~50μm之範圍。
樹脂組成物層可以保護薄膜保護,藉由以保護薄膜保護,可防止樹脂組成物層表面之塵埃等之附著或損傷。保護薄膜以使用與支持體同樣之塑膠薄膜為佳。又,保護薄膜除消光處理、電暈處理外,亦可施以脫模處理。保護薄膜的厚度雖不特別限制,通常為1~150μm、較佳為在10~100μm之範圍使用。
密封用薄片,支持體若使用具有防溼性且透過率高的支持體,使密封用薄片層合於密封對象物的必要處,直接使樹脂組成物層硬化形成密封層,可形成具有高耐防溼性與高透過性的密封構造。如此之具有防溼性且透過率高的支持體,可舉例如表面蒸鍍有氧化矽(二氧化矽)、氮化矽、SiCN、非晶質矽等之無機物的塑膠薄膜等。塑膠薄膜,可使用例如聚乙烯、聚丙烯、聚氯乙烯等
之聚烯烴、聚乙烯對苯二甲酸酯、聚萘二甲酸乙二醇脂等之聚酯、聚碳酸酯、聚醯亞胺等之塑膠薄膜。塑膠薄膜,尤以PET為佳。市售的具有防溼性之塑膠薄膜的例,可舉例如Techbarrier HX、AX、LX、L系列(三菱樹脂公司製)或防溼效果更高的X-BARRIER(三菱樹脂公司製)等。密封基材可使用具有2層以上之複層構造者。
密封用薄片,在樹脂組成物層被保護薄膜保護的場合,將其剝離後,使密封用薄片以該樹脂組成物層與密封對象物(例如有機EL元件等)直接相接之方式層合。層合之方法可為批次式或以輥之連續式。層合後將支持體剝離,進行後述樹脂組成物層之熱硬化作業。密封用薄片之支持體為具有防溼性之支持體,將密封用薄片層合後,不剝離支持體而直接進行後述樹脂組成物層之熱硬化作業。
樹脂組成物層之硬化以通常熱硬化進行。例如熱風循環式烤箱、紅外線加熱機、熱風機、高頻誘導加熱裝置、以加熱工具之壓著的加熱等。硬化溫度及硬化時間各自下限值,由可使硬化後樹脂組成物層(密封層)以充分滿足對密封對象物之接著強度接著觀點,硬化溫度中以50℃以上為佳、55℃以上更佳、硬化時間中以20分鐘以上為佳、30分鐘以上更佳。
以下以實施例及比較例將本發明更具體說
明,但本發明不限於以下實施例。
實施例及比較例使用的材料(原料)如下。
(A)環氧樹脂
‧jER828EL(三菱化學公司製):液狀雙酚A型環氧樹脂、環氧當量(185g/eq)、透過率(91.8%)
‧jER1001B80(三菱化學公司製):固形狀雙酚A型環氧樹脂、環氧當量(475g/eq)、透過率(91.6%)
(B)燒成菱水鎂鋁石
KW2200(協和化學工業公司製):平均粒徑(0.4μm)、BET比表面積(146m2/g)
(C)滑石
‧FG-15(日本滑石公司製):滑石、平均粒徑(1.4μm)
(D)二氧化矽
MEK-EC-2130Y(日產化學工業公司製):有機溶劑分散膠體二氧化矽(二氧化矽粒徑:10~15nm、固形分30質量%、MEK溶劑)
(E)苯氧樹脂
‧YL7213B35(三菱化學公司製):透過率(91.4%
)、重量平均分子量(約38,000)
(F)耦合劑
‧KBM403(信越化學公司製):矽烷耦合劑(3-縮水甘油基氧基丙基三甲氧基矽烷)
(G)硬化劑(離子液體)
TBP‧N-Ac-Gly(合成品):N-乙醯基甘胺酸四丁基鏻鹽
該離子液體用以下手段合成。
對四丁基鏻氫氧化物41.4質量%水溶液(北興化學工業公司製)20.0g,在0℃加入N-乙醯基甘胺酸(東京化成工業公司製)3.54g,並進行10分鐘攪拌。使用蒸發器,減壓至40-50mmHg,在60-80℃進行2小時、在90℃進行5小時濃縮。在室溫,再度溶解於乙酸乙基酯(純正化學公司製)14.2ml,使用蒸發器,減壓至40-50mmHg,在70-90℃進行3小時濃縮。得到四丁基鏻N-乙醯基甘胺酸酯11.7g(純度:96.9%)油狀化合物。
[NMR頻譜]
1HNMR(CDCl3)d:0.89-0.99(m,12H),1.42-1.55(m,16H),1.92(s,3H),2.24-2.35(m,8H),3.66(d,J=3.8Hz,2H),6.70(br s,1H)
(H)硬化促進劑
‧U-3512T(San-Apro Ltd.製):芳香族二甲基脲
將如下述表1上段所示之搭配比的樹脂組成物的塗漆用以下手段調製。於液狀雙酚A型環氧樹脂(三菱化學公司製「jER828EL」)中,搭配將矽烷耦合劑(信越化學工業公司製「KBM-403」)、滑石粉末(日本滑石公司製「FG15」)、及燒成菱水鎂鋁石(協和化學工業公司製「KW2200」)以3支輥分散的混合物(混合物A)、使硬化促進劑(San-Apro Ltd.製「U-3512T」)溶於苯氧樹脂(三菱化學公司製「YL7213」之35質量%MEK溶液)的混合物(混合物B)、固形雙酚A型環氧樹脂(三菱化學公司製「jER1001」)之80質量%MEK溶液、有機溶劑分散型膠體二氧化矽(非晶質二氧化矽粒徑10~15nm(BET比表面積272~181m2/g)、固形分30質量%、MEK溶劑、日產化學工業公司製「MEK-EC-2130Y」)、離子液體硬化劑(N-乙醯基甘胺酸四丁基鏻鹽),並以高速旋轉混合機均勻分散而得到塗漆狀之樹脂組。
接著,使該樹脂組成物的塗漆於以醇酸系脫模劑處理的PET薄膜(厚度38μm)之脫模處理面上,以乾燥後樹脂組成物層之厚度成為30μm之方式,以模具塗佈機均勻塗佈,並藉由以60~80℃進行6分鐘乾燥,得到密封用薄片。且使得到的密封用薄片用於下述評估試驗。
又,表1上段各欄數值為各材料之使用量(質量
份),括弧內數值為固形分量(質量份)。
1. 透過率(透過性之評估)
將以PET薄膜為支持體作成的密封用薄片(PET薄膜厚度38μm、樹脂組成物層厚度20μm)切為長度50mm、寬20mm後,層合於玻璃板(長度76mm、寬26mm、厚度1.2mm之載玻片玻璃、松浪玻璃工業(股)白載玻片S1112緣磨No.2)。之後將PET薄膜剝離,於露出的密封用薄片上進而與上述相同地層合玻璃板。將得到的層合體在加熱板上、110℃進行30分鐘加熱硬化後(絕緣層厚度20μm),使用裝設有8°投光之60mm積分球(型名SRS-99-010、反射率99%)的纖維式分光光度計(MCPD-7700、形式311C、大塚電子公司製、外部光源單元:鹵素燈MC-2564(24V、150W仕樣),測定樣本之光透過率頻譜。光透過率,以積分球與樣本之距離為0mm,作為平行線透過率亦包含反射成分與擴散成分的全光線透過率。對照為空氣,採用450nm中之值為透過率。
2. 剝離強度(接著強度之評估)
將以PET薄膜為支持體作成的密封用薄片切為長度50mm、寬20mm,層合於長度100mm、寬25mm之鋁箔(厚度50μm、東海東洋鋁販賣公司製)。之後將PET薄膜剝離,於露出的密封用薄片上進而層合玻璃板(長度76mm、寬26mm、厚度1.2mm之載玻片玻璃)。使得到
的層合體在加熱板上以110℃進行30分鐘加熱硬化後,測定沿著鋁箔長度方向在90度方向剝離時的接著強度(拉伸速度50mm/分鐘)。以樣本數(n)=2測定,採用平均值。
3. 耐透溼性之評估
將與上述同樣地作成的剝離強度評估用層合體在121℃、100%RH之條件下維持24小時後,將自密封薄片端面之浸水域以顯微鏡比較,作為耐透溼性之指標。
浸水域自薄片端面0~0.5mm之範圍者為良好(○)、
浸水域超過0.5mm、1.0mm以下之範圍、或產生具有未達0.5mm之直徑的小水泡者為尚可(△)、
浸水度超過1.0mm超、或產生具有0.5mm以上之直徑的大水泡者為不良(×)。
圖1為耐透溼性評估為良好(○)的浸水域之代表照片、圖2為耐透溼性評估為尚可(△)的浸水域之代表照片、圖3為耐透溼性評估為不良(×)的浸水域之代表照片。
4. 操作性
調製液狀雙酚A型環氧樹脂(三菱化學公司製「jER828EL」)、與矽烷耦合劑(信越化學工業公司製「KBM-403」)、滑石粉末(日本滑石公司製「FG-15」)
、及燒成菱水鎂鋁石(協和化學工業公司製「KW2200」)以3支輥分散的混合物(混合物A)時,黏度太過高而無法以3支輥適當分散者評估為不良(×)。
又,比較例1未使用滑石及燒成菱水鎂鋁石,比較例2未使用燒成菱水鎂鋁石。
將下述表2上段所示之搭配比的樹脂組成物的塗漆以與前述實驗例1同樣手段調製,進而由得到的樹脂組成物的塗漆以與前述實驗例1同樣手段製作密封用薄片。進而將得到的密封用薄片用於前述之評估試驗。
又,表2上段各欄數值為各材料之使用量(質量份),括弧內之數值為固形分量(質量份)。
將下述表3上段所示之搭配比的樹脂組成物的塗漆以與前述實驗例1同樣手段調製,進而由得到的樹脂組成物
的塗漆以與前述實驗例1同樣手段製作密封用薄片。進而將得到的密封用薄片用於前述之評估試驗。
又,表3上段各欄數值為各材料之使用量(質量份),括弧內之數值為固形分量(質量份)。
本申請以日本申請的特願2013-232532為基礎,彼等之內容全部包含於本說明書。
Claims (11)
- 一種密封用樹脂組成物,其為含有(A)環氧樹脂、(B)燒成菱水鎂鋁石、(C)滑石及(D)二氧化矽之密封用樹脂組成物,其特徵係相對(A)環氧樹脂80質量份,(B)為3~38質量份、(C)為1~16質量份及(D)為1~16質量份。
- 如請求項1記載之樹脂組成物,其中,(A)環氧樹脂之透過率為90%以上。
- 如請求項1或2記載之樹脂組成物,其中,相對(A)環氧樹脂80質量份,再含有(E)熱可塑性樹脂1~40質量份。
- 如請求項3記載之樹脂組成物,其中,(E)熱可塑性樹脂為苯氧樹脂。
- 如請求項1或2記載之樹脂組成物,其中,(E)熱可塑性樹脂之透過率為90%以上。
- 如請求項1或2記載之樹脂組成物,其中,相對(A)環氧樹脂80質量份,再含有(F)表面處理劑0.1~3質量份。
- 如請求項6記載之樹脂組成物,其中,(F)表面處理劑為矽烷耦合劑。
- 如請求項1或2記載之樹脂組成物,其中,該樹脂組成物的硬化物之透過率為84%以上。
- 如請求項1或2記載之樹脂組成物,其中,相對(A)環氧樹脂80質量份,再含有(G)硬化劑0.1~3質量份。
- 如請求項9記載之樹脂組成物,其中,(G)硬化劑為離子液體。
- 一種密封用薄片,其特徵係由請求項1~10中任1項記載之樹脂組成物的層形成於支持體上而成。
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KR102244167B1 (ko) | 2021-04-26 |
US10385185B2 (en) | 2019-08-20 |
EP3067392B1 (en) | 2018-03-07 |
EP3067392A1 (en) | 2016-09-14 |
CN105683284B (zh) | 2017-04-19 |
EP3067392A4 (en) | 2017-07-05 |
CN105683284A (zh) | 2016-06-15 |
US20160244590A1 (en) | 2016-08-25 |
WO2015068786A1 (ja) | 2015-05-14 |
TW201522490A (zh) | 2015-06-16 |
JP6369475B2 (ja) | 2018-08-08 |
JPWO2015068786A1 (ja) | 2017-03-09 |
KR20160083097A (ko) | 2016-07-11 |
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