TWI450627B - 水氣反應性組合物及有機電致發光裝置 - Google Patents
水氣反應性組合物及有機電致發光裝置 Download PDFInfo
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- TWI450627B TWI450627B TW096132262A TW96132262A TWI450627B TW I450627 B TWI450627 B TW I450627B TW 096132262 A TW096132262 A TW 096132262A TW 96132262 A TW96132262 A TW 96132262A TW I450627 B TWI450627 B TW I450627B
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Description
本發明係關於一種水氣反應性組合物,其可形成透明且可撓性之水氣吸收層,且係關於一種包括由該組合物形成之乾燥構件之有機電致發光(下文中縮寫為EL)裝置。
利用有機材料之有機EL裝置作為由於低電壓下之直流(DC)驅動而能夠發射高亮度光之發光裝置而已吸引特別關注,該發光裝置包含一陽極、一陰極及一於陽極與陰極之間形成之有機層,該有機層包含相互層疊之一有機電荷輸送層及一有機發光層。又,因為全部材料均可由固體組成,所以期望該有機EL裝置為可撓性顯示器。
另一方面,有機EL裝置遭遇之問題為當有機EL裝置經驅動固定時段時,諸如發光亮度、發光效率及發光均勻度之各種發光特徵與最初階段之情況相比會急劇退化。該等發光特徵退化之原因的實例包括由於氧氣透入有機EL裝置中所引起之電極氧化、由於驅動期間之生熱所引起之有機材料的氧化分解,及有機物之變性。發光特徵退化之原因另外包括結構之機械性損壞,例如結構界面之剝落係藉由氧氣及水氣之影響以及驅動期間之生熱而引起,且由於各自組份熱膨脹係數之差異,高溫環境會觸發於結構界面處產生應力,從而導致界面剝落。
為防止該等問題,已研究了多種密封有機EL裝置之技術以抑制與水氣及氧氣之接觸。舉例而言,如圖1所示,揭示一種防止水氣到達有機EL裝置之方法,其係藉由將於內壁上黏附有吸水劑6之密封帽2放置在包括一基板1及形成於該基板上之包含一透明電極3、一有機功能層4及一金屬陰極電極5之有機EL裝置之像元區上,以氮氣9填充內部,且使用黏著劑7將密封帽固定於基板1上(例如參見,日本未審查專利公開案第9-148066號)。又,揭示一種藉由使用氧氣吸收劑代替吸水劑降低氧氣影響之方法(例如參見,日本未審查專利公開案第7-169567號)。
曾研究各種物質作為吸水劑。在各種物質中,已廣泛研究諸如氧化鋇(BaO)或氧化鈣(CaO)之鹼土金屬氧化物,因為其可藉由化學反應定然捕獲水分子且在高溫下不釋放水分子,與諸如矽膠或沸石之物理性吸附水之吸水劑不同。
然而,該等吸水劑亦具有缺陷,因為其為無機化合物粒子且需要凹形基板以黏附於裝置內,且因此所得裝置較厚。又,鹼土金屬氧化物為不透明的,且因此可應用於所謂底部發射類型(其中顯示光自基板1之側面發出)之顯示裝置。然而,當將鹼土金屬氧化物應用所謂頂部發射類型顯示裝置於其中顯示光欲自與基板1相對之密封帽2之側面發出時,光發射受到吸水劑4之阻礙,且因此吸水劑4必須經安置以免進入圖像區且必須提供一安裝位置。
曾提出某些將吸水劑應用於頂部發射類型顯示裝置之建議。舉例而言,可易於考慮到應用諸如聚乙烯醇及耐綸之透明且具有吸水特性之聚合物作為吸水劑。然而,該等聚合物物理性地吸水且如上所述並不具有足夠之吸水特性。亦曾建議使用經安置以免在頂部發射類型結構中不利影響光透射特性之微粒吸水劑(例如參見,日本未審查專利公開(案)第2001-357973號)。亦建議使用塑料基板,其中具有小於有機EL裝置發射波長之粒度的吸水劑係分散的(例如參見,日本未審查專利公開(案)第2002-56970號)。然而,無機粒子難以安置及以初始粒子形式均勻分散,且因此由光散射所引起之透射退化不可避免。
作為解決該等問題之方式,已有人提議使用吸收較少可見光,但具有足夠透明度之水捕獲薄膜(參見日本未審查專利公開案第2003-142256號)。該水捕獲薄膜可藉由塗佈溶解於溶劑中之特殊金屬化合物來形成。然而,當應用於可撓性基板時,水捕獲薄膜之可撓性不足,因為該水捕獲薄膜係由低分子量化合物製成。吸收水氣之後,該化合物變得更脆且可以粉塵形式黏附於有機EL裝置上。
已進行本發明以解決上述問題。本發明之一目的在於提供一種組合物,此組合物可用作可能受水氣或氧氣影響之裝置諸如有機EL裝置之水氣淨化劑,且為透明的且可安置於光接收表面之側面而不遮光,以及具有可撓性且可應用於可撓性基板。本發明之另一目的在於提供一種長期維持發光特徵之有機EL裝置。
為達成上述目的,提供一種包含以下各物之水氣反應性組合物:包含Al、Mg、Zn、Ti或Zr之水氣反應性有機金屬化合物;及具有500至5,000,000之分子量之聚合物,該聚合物包含羧酸基團且選自由以下各物組成之群:(a)包含一或多種選自由以下各物組成之群之丙烯酸系單體之丙烯酸系聚合物:(甲基)丙烯酸、苯乙烯、α-甲基苯乙烯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸正辛酯、(甲基)丙烯酸月桂酯、(甲基)丙烯酸硬脂醯酯、(甲基)丙烯酸異冰片酯、(甲基)丙烯酸二環戊酯、(甲基)丙烯酸苯氧基乙酯、聚乙二醇(甲基)丙烯酸酯、聚丙二醇(甲基)丙烯酸酯、N-羥甲基(甲基)丙烯醯胺、N-甲氧基甲基(甲基)丙烯醯胺、N-乙氧基甲基(甲基)丙烯醯胺、N-正丁氧基甲基(甲基)丙烯醯胺、N-異丁氧基甲基(甲基)丙烯醯胺、第三丁基(甲基)丙烯醯胺、辛基(甲基)丙烯醯胺、丙烯醯基嗎啉、N-乙烯吡咯啶酮、N,N-二甲基(甲基)丙烯醯胺、N,N-二乙基(甲基)丙烯醯胺、N-(2-羥乙基)(甲基)丙烯醯胺及N,N-二甲胺基丙基(甲基)丙烯醯胺;(b)聚矽氧;(c)聚醚;及(d)氫化聚烯烴。亦提供由該水氣反應性組合物形成之水氣吸收薄膜。
為達成上述目的,亦提供一種包含水氣反應性組合物之有機EL裝置。該有機EL裝置包含一藉由在一對互相面對之電極之間插入由有機材料製成之有機發光材料層而形成之層壓板,且一結構遮蔽該層壓板以使其免受外部空氣影響,且該結構中安置有乾燥構件,其中該乾燥構件由水氣反應性組合物形成。
如上所述,本發明之水氣反應性組合物含有以下各物之反應產物:水氣反應性有機金屬化合物,及在主鏈或側鏈末端具有羧基之聚合物。
水氣反應性有機金屬化合物為可與水反應之化合物,藉此因化學反應而移除水氣。該水氣反應性有機金屬化合物部分地與作為構成組合物之另一組份之具有羧基的聚合物反應,藉此固定在該具有羧基之聚合物上且賦予該聚合物與水及氧氣之反應性。此外,因為該水氣反應性有機金屬化合物在與水反應時不產生腐蝕性化合物,所以諸如腐蝕之問題不會在應用部位出現。
該水氣反應性有機金屬化合物較佳為由下式表示之化合物:MRn
其中M表示Al、Mg、Zn、Ti或Zr;R獨立地表示經取代或未經取代之烷基、烯基或烷氧基;且n表示M之價數。
在上式中,M更佳為Al或Ti。R更佳為甲基、乙基、丙基、丁基、己基、辛基、甲氧基、乙氧基、丁氧基、己氧基、環己氧基、辛氧基、2-乙基己氧基、異硬脂醯基氧基、異冰片氧基、膽固醇氧基、聚氧化乙烯單甲醚氧基、聚氧化丙烯單丁醚氧基、聚四氫呋喃單甲醚氧基或具有聚二甲基矽氧烷骨架之烷氧基,且更佳為己基、辛基、辛氧基、2-乙基己氧基、異硬脂醯基氧基、聚氧化乙烯單甲醚氧基、聚氧化丙烯單丁醚氧基、聚四氫呋喃單甲醚氧基或具有聚二甲基矽氧烷骨架之烷氧基。具有聚二甲基矽氧烷骨架之烷氧基之特定實例包括由Chisso公司製造之FM2221、FM2241及FM2245。
水氣反應性有機金屬化合物之特定實例包括三甲基鋁、三乙基鋁、三辛基鋁、烷基鋁化合物、其衍生物形式之倍半化合物、參(三乙二醇單丁醚氧基)鋁、三異硬脂醯基氧基鋁及諸如鋁氧烷(alumoxane)之有機鋁化合物。
在主鏈或側鏈末端具有羧基之聚合物可與水氣反應性有機金屬化合物反應,藉此固定該水氣反應性有機金屬化合物且控制反應性、流動性、可撓性及相容性。該具有羧基之聚合物可由下式表示:Y-(A)m
-Y其中A各自獨立地表示CH2
CR'COOY、CH2
CR'CONY2
、Si(R')(Y)O、CH2
CHR'O或CH2
CHR';R'表示氫或烷基;Y表示氫、烷基或羧烷基;且m表示滿足以下關係式之整數:10m10,000。
在該聚合物中,羧基可存在於分子之兩端、一端及側鏈,且平均一個分子中之羧基數目較佳為3個或3個以下。在3個或3個以上之情況下,當與水氣反應性有機金屬化合物反應時發生急劇膠凝作用且變得難以處理。具有羧基之聚合物之重量平均分子量可根據所得組合物之物理特性適當地選擇,但通常在500至5,000,000之範圍內,且較佳為1,000至1,000,000。當平均分子量低於500時,難以賦予組合物足夠之可撓性。另一方面,當平均分子量大於5,000,000時,溶液之黏度增加且可變得難以處理。平均分子量意謂使用凝膠滲透層析法(GCP)所測定之苯乙烯當量分子量。
具有羧基之聚合物之特定實例包括諸如側鏈具有羧基之聚二甲基矽氧烷(X-22-3701E,由Shin-Etsu Chemical Co.,Ltd製造)或末端具有羧基之聚二甲基矽氧烷(X-22-162C,由Shin-Etsu Chemical Co.,Ltd製造)之聚矽氧;諸如末端具有羧基之聚乙二醇雙羧基甲基醚之聚伸烷二醇;及諸如α,ω-聚丁二烯羧酸(C-1000,由Nippon Soda Co.,Ltd製造)或氫化α,ω-聚丁二烯羧酸(CI-1000,由Nippon Soda Co.,Ltd製造)之聚烯烴。
(甲基)丙烯酸及丙烯酸系單體之共聚物為具有羧基之尤其較佳聚合物。如本文所用,“(甲基)丙烯醯基”意謂丙烯醯基或甲基丙烯醯基。該共聚物通常可由相應單體之自由基聚合反應而合成。
可與(甲基)丙烯酸共聚合之較佳單體之實例包括諸如苯乙烯或α-甲基苯乙烯之苯乙烯基單體;(甲基)丙烯酸烷酯,諸如(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸正辛酯、(甲基)丙烯酸月桂酯、(甲基)丙烯酸硬脂醯酯、(甲基)丙烯酸異冰片酯或(甲基)丙烯酸二環戊酯;(甲基)丙烯酸伸烷酯,諸如(甲基)丙烯酸苯氧基乙酯、聚乙二醇(甲基)丙烯酸酯或聚丙二醇(甲基)丙烯酸酯;及丙烯醯胺,諸如N-羥甲基(甲基)丙烯醯胺、N-甲氧基甲基(甲基)丙烯醯胺、N-乙氧基甲基(甲基)丙烯醯胺、N-正丁氧基甲基(甲基)丙烯醯胺、N-異丁氧基甲基(甲基)丙烯醯胺、第三丁基(甲基)丙烯醯胺、辛基(甲基)丙烯醯胺、丙烯醯基嗎啉、N-乙烯吡咯啶酮、N,N-二甲基(甲基)丙烯醯胺、N,N-二乙基(甲基)丙烯醯胺、N-(2-羥乙基)(甲基)丙烯醯胺或N,N-二甲胺基丙基(甲基)丙烯醯胺。
水氣反應性有機金屬化合物與具有羧基之聚合物之間之反應係由混合而達成。調整兩種物質之混合比率以使與水氣反應性有機金屬化合物之水氣反應之全部位點不由具有羧基之聚合物之羧基消耗。特定言之,水氣反應性有機金屬化合物之量基於1 mol羧基計較佳為0.05 mol至10 mol。
水氣反應性組合物亦可描述為包含以下各物:包含Al、Mg、Zn、Ti或Zr之水氣反應性有機金屬化合物;及具有500至5,000,000之分子量之聚合物,該聚合物包含羧酸基團且選自由以下各物組成之群:(a)包含一或多種選自由以下各物組成之群之丙烯酸系單體之丙烯酸系聚合物:(甲基)丙烯酸、苯乙烯、α-甲基苯乙烯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸正辛酯、(甲基)丙烯酸月桂酯、(甲基)丙烯酸硬脂醯酯、(甲基)丙烯酸異冰片酯、(甲基)丙烯酸二環戊酯、(甲基)丙烯酸苯氧基乙酯、聚乙二醇(甲基)丙烯酸酯、聚丙二醇(甲基)丙烯酸酯、N-羥甲基(甲基)丙烯醯胺、N-甲氧基甲基(甲基)丙烯醯胺、N-乙氧基甲基(甲基)丙烯醯胺、N-正丁氧基甲基(甲基)丙烯醯胺、N-異丁氧基甲基(甲基)丙烯醯胺、第三丁基(甲基)丙烯醯胺、辛基(甲基)丙烯醯胺、丙烯醯基嗎啉、N-乙烯吡咯啶酮、N,N-二甲基(甲基)丙烯醯胺、N,N-二乙基(甲基)丙烯醯胺、N-(2-羥乙基)(甲基)丙烯醯胺及N,N-二甲胺基丙基(甲基)丙烯醯胺;(b)聚矽氧;(c)聚醚;及(d)氫化聚烯烴。
舉例而言,包含羧酸基團之聚合物可基本上由丙烯酸2-乙基己酯及丙烯酸組成。包含羧酸基團之聚合物亦可包含:具有末端羧基之聚氧化乙烯或具有末端羧基之氫化聚丁二烯。
水氣反應性有機金屬化合物包含三甲基鋁、三乙基鋁、三辛基鋁、參(三乙二醇單丁醚氧基)鋁或三異硬脂醯基氧基鋁。水氣反應性組合物可另外包含矽石、氧化鈦、氧化鋅、氧化鋁、氧化鋯或黏土。水氣反應性組合物可為透明的。由水氣反應性組合物形成之水氣吸收薄膜可如先前所述而形成。
本發明之組合物除水氣反應性有機金屬化合物及具有羧基之聚合物之外,亦可含有不具有羧基之化合物及/或填充劑以調整黏度。作為不具有羧基之化合物,可使用具有與具有羧基之聚合物相容之結構的化合物,且該聚合物因其在處理後具有黏性而可用作黏著劑。不具有羧基之化合物之實例包括聚二甲基矽氧烷或基本上由丙烯酸2-乙基己酯組成之聚合物。填充劑較佳為具有羥基之能夠與水氣反應性有機金屬化合物反應之無機填充劑,且其實例包括矽石、氧化鈦、氧化鋅、氧化鋁、氧化鋯及黏土。填充劑之粒度可視情況經選擇,只要其不不利影響組合物之透明度即可,且較佳為1至1,000 nm。
本發明之組合物可在諸如有機EL裝置之可能受水氣影響之裝置中用作水氣淨化劑。該組合物為透明的且因此可安置於該裝置之發光表面側面及右側接收表面上而不遮光,以及可有效地利用發光部分之區域,而未對顯示器或太陽能電池板提供安裝位置。
由本發明之組合物形成之薄膜為透明的且因此可用於各種光學裝置。亦即,本發明之第二態樣係關於由該組合物所形成之水氣吸收性薄膜。該薄膜例如可藉由在基板上塗佈該組合物,繼而乾燥來形成。
本發明之第三態樣係關於一種有機EL裝置,其中該組合物經安置於內部作為乾燥構件。該EL裝置可具有與圖1所示之習知有機EL裝置之構造相同之構造。亦即,本文所揭示之有機EL裝置包含一藉由在一對互相面對之電極3及電極5之間插入一由有機材料製成之有機發光材料層4而形成之層壓板、一遮蔽該層壓板以使其免受外部空氣影響之結構2及安置於該結構中之乾燥構件6(吸水劑),且該乾燥構件係由上述水氣反應性組合物形成。因為該組合物為透明的,所以對於安置乾燥構件6之位置不存在限制。如圖2所示,其可直接用作薄膜6以覆蓋電極5。或者,如圖3所示,該薄膜6可經安置以覆蓋基板1上之電極3及5及有機功能層4,以及可覆蓋其上之密封黏著劑7。層8可為一薄膜封裝層、鈍化層或保護層以分離薄膜6以免接觸4及5。
其他例示性裝置包括圖4及圖5中所示之彼等裝置。在圖4中,該裝置與圖1所示之裝置類似,除密封黏著劑7與層壓板兩側均相鄰以外。在圖5中,該裝置與圖4所示之裝置類似,除在薄膜6與電極5之間不存在氣隙9以外。
材料
如表1所示,丙烯酸系樹脂係藉由習知方法使用丙烯酸2-乙基己酯(2-EHA;由Nippon Shokubai Co.,Ltd.製造)及丙烯酸(AA;由Wako Pure Chemical Industries,Ltd.製造)來合成。
以下材料為市售之產品且經購買且原樣使用:聚合物4:Shin-Etsu Silicones Co.,Ltd.,X-22-162C,以COOH基團封端之嵌段聚矽氧;聚合物5:Shin-Etsu Silicones Co.,Ltd.,X-22-3701E,含有COOH基團側鏈之嵌段聚矽氧;聚合物6:Sigma Aldrich Co.,Ltd.Co.,聚氧化乙烯,以COOH基團封端之嵌段,Mw:600;聚合物7:Nippon Soda Co.,Ltd.Co.,以COOH基團封端之氫化聚丁二烯,Mw:1,000;聚合物8:GE Toshiba Silicones Co.,Ltd.Co.,TSE200,聚二甲基矽氧烷,Mw:2,000,000;化合物1:三辛基鋁,Sigma Aldrich Co.,Ltd.;化合物2:參(三乙二醇單丁醚氧基)鋁;化合物3:三異硬脂醯基氧基鋁;及化合物4:液體Oliepe AOO,辛酸氧化鋁,Hope Chemical Co.,Ltd.。
全部試劑及溶劑均為市售產品且經購買且原樣使用。於20 mL經氮氣取代之螺紋管中饋入4.0 g三辛基鋁(由Sigma Aldrich Co.製造)之己烷溶液(固體含量:25重量%),且添加10.0 g聚合物1之甲苯溶液(固體含量:40重量%),繼而劇烈攪拌以獲得溶液組合物。
以實例1中相同之方式,使用表2中所示之材料獲得溶液組合物。
以實例1中相同之方式,使用表2中所示之材料獲得溶液組合物。
水氣吸收特性之量測
將上述溶液組合物之每一者在氮氣氛下使用一刀塗佈器塗佈於市售之聚對苯二甲酸乙二酯(PET)薄膜(LUMIRROR T-60,厚度:50 μm,由Toray Industries,Inc.製造)上。乾燥後,所得薄膜各自具有50 μm之厚度。將由此獲得之薄膜切成量測值為30 mm×40 mm之片,置於具有420 mL容積之玻璃瓶中,且隨後用具有一溫度計及一濕度計之金屬帽(testo Co.,605-H1)密封。量測直至玻璃杯中之相對濕度減少至10%之時間及12小時後之相對濕度。測量結果顯示於表3中。
透射特性之量測
使用由Hitachi,Ltd.製造之分光光度計U-4000量測透射率。由上述方法形成之50 μm厚之薄膜藉由於50%之相對濕度及25℃之空氣中靜置3天而充分固化,且隨後用作量測之樣品。在分析中,採用PET薄膜作為基線。將400 nm至800 nm範圍內之波長處之最小透射率顯示於表3中。
可撓性之量測
將用於上述測試之薄膜繞一鐵棒(R=10 mm)彎曲且經目測觀察。將此操作重複10次。如表3中所示,在實例1至7之薄膜表面上未觀察到裂縫。
如由表3所示之結果顯而易見,實例1至7之組合物具有足夠之水氣可固化性且可用作水氣淨化劑。由該等組合物形成之薄膜亦具有足夠之可撓性。此外,該等薄膜在可見光範圍內具有足夠之透明度。另一方面,比較實例1之組合物在水氣吸收後極脆且其難以彎曲。比較實例2之組合物在塗佈後立即為透明的且在靜置12小時後發生變白。
1...基板
2...密封帽/遮蔽結構
3...透明電極
4...有機功能層/吸水劑/有機發光材料層
5...金屬陰極電極
6...吸水劑/乾燥構件/薄膜
7...黏著劑/密封黏著劑
8...薄膜封裝層/鈍化層/保護層
9...氮氣/氣隙
圖1為示意性地展示本發明及先前技術之一有機EL裝置之一結構的剖視圖。
圖2-5為各自示意性地展示本發明之一有機EL裝置之一結構的剖視圖。
1...基板
2...密封帽/遮蔽結構
3...透明電極
4...有機功能層/吸水劑/有機發光材料層
5...金屬陰極電極
6...吸水劑/乾燥構件/薄膜
7...黏著劑/密封黏著劑
9...氮氣/氣隙
Claims (11)
- 一種水氣反應性組合物,其包含:包含Al、Mg、Zn、Ti或Zr之水氣反應性有機金屬化合物;及具有末端羧基之聚氧化乙烯聚合物,其具有500至5,000,000之分子量。
- 如請求項1之水氣反應性組合物,其中該水氣反應性有機金屬化合物包含三甲基鋁、三乙基鋁、三辛基鋁、參(三乙二醇單丁醚氧基)鋁或三異硬脂醯氧基鋁。
- 如請求項1之水氣反應性組合物,其中該組合物另外包含矽石、氧化鈦、氧化鋅、氧化鋁、氧化鋯或黏土。
- 如請求項1之水氣反應性組合物,其中該組合物另外包含不具有羥基之化合物。
- 如請求項4之水氣反應性組合物,其中該不具有羥基之化合物包含聚二甲基矽氧烷或基本上由丙烯酸2-乙基己酯組成之聚合物。
- 如請求項1之水氣反應性組合物,其中該組合物係透明的。
- 一種水氣吸收薄膜,其係由如請求項1至6中任一項之水氣反應性組合物形成。
- 一種由如請求項1之水氣反應性組合物形成之水氣吸收薄膜,其中該水氣吸收薄膜具有一大於10之彎曲頻率。
- 一種有機電致發光裝置,其包含:一層壓板,其包含一插入一對互相面對之電極之間之 由一有機材料製成之有機發光材料層;一結構,遮蔽該層壓板以使其免受外部空氣影響;及一安置於該結構內之水氣反應性組合物,該水氣反應性組合物係如請求項1至6中任一項之水氣反應性組合物。
- 如請求項9之有機電致發光裝置,其中該水氣反應性組合物覆蓋該等電極中之一者。
- 如請求項9之有機電致發光裝置,其另外包含一黏著劑,其中該水氣反應性組合物及該黏著劑覆蓋該層壓板。
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CN101511924B (zh) | 2012-07-04 |
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