TWI451966B - 電光組件及使用於其中之黏合劑與黏結劑 - Google Patents

電光組件及使用於其中之黏合劑與黏結劑 Download PDF

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TWI451966B
TWI451966B TW097143606A TW97143606A TWI451966B TW I451966 B TWI451966 B TW I451966B TW 097143606 A TW097143606 A TW 097143606A TW 97143606 A TW97143606 A TW 97143606A TW I451966 B TWI451966 B TW I451966B
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electro
optic
display
fluid
adhesive
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TW200932517A (en
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Thomas H Whitesides
Lan Cao
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E Ink Corp
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    • G—PHYSICS
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    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
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Description

電光組件及使用於其中之黏合劑與黏結劑
本發明關於國際申請案公告第WO 2003/104884；WO 2004/023195；WO 2005/041160；WO 2005/073777；與WO 2007/104003號；及國際申請案第PCT/US2006/60049與PCT/US2006/62399號。關於本發明之背景資訊請讀者參考這些國際申請案。
本發明關於可用於製造電光顯示器之電光組件、及用於此組件之黏合劑與黏著劑。更特別地，本發明提供具有經控制體積電阻率之黏合劑與黏著劑組成物、及倂有此黏合劑之電光組件與顯示器。本發明特別地但非絕對地意圖用於包含膠囊化電泳介質(encapsulated electrophoretic media)之顯示器。然而本發明亦可利用各種其他型式之固態電光介質(以其具有固態外表面之方式)，雖然此介質可且經常具有含流體(液體或氣體)之內腔。因此名詞「固態電光顯示器」包括膠囊化電泳顯示器、膠囊化液晶顯示器、及以下討論之其他型式顯示器。在此揭示之黏合劑可用於電光顯示器以外之應用。
關於電光顯示器之背景命名法及技藝狀態詳細地討論於美國專利第7,012,600號，請讀者參考進一步資訊。因而專有名詞及技藝狀態簡單地規歸納如下。
適用於材料或顯示器之名詞「電光」在此以其在影像技藝之習知意義係用於具有至少一種光學性質不同之第一與第二顯示狀態的材料，此材料因對材料施加電場而由其第一變成其第二顯示狀態。一些電光材料為固態(以材料具有固態外表面之方式)，雖然此材料可且經常具有內部充填液體或氣體空間。此使用固態電光材料之顯示器在以下為了方便可稱為「固態電光顯示器」。因此名詞「固態電光顯示器」包括轉動二色構件顯示器、膠囊化電泳顯示器、微胞電泳顯示器、與膠囊化液晶顯示器。
名詞「二安定」及「二安定性」在此以此技藝之習如意義指稱包含具有至少一種光學性質不同之第一及第二顯示狀態的顯示元件之顯示器，使得在已藉有限時間之定址脈衝驅動任何特定元件後，假設其第一或第二顯示狀態在已終止定址脈衝後，此狀態持續改變顯示元件之狀態所需最短定址脈衝時間的至少數倍時間，例如四倍。
已知許多型電光顯示器，例如：
(a)轉動二色構件顯示器(參見例如美國專利第5,808,783、5,777,782、5,760,761、6,054,071、6,055,091、6,097,531、6,128,124、6,137,467、與6,147,791號)；
(b)電致變色顯示器(參見例如O’Regan,B.等人之Nature 1991,353,737、Wood,D.之Information Display,18(3),24(2002年3月)、Bach,U.等人之Adv. Mater.,2002,14(11),845、及美國專利第6,301,038、6,870,657、與6,950,220號)；
(c)電濕潤顯示器(參見Hayes,R.A.等人之”Video-Speed Electronic Paper Based on Electrowetting”,Nature,425,383-385(2003年9月25日)及美國專利公告第2005/0151709號)；
(d)粒子為主電泳顯示器，其中多個帶電粒子在電場影響下移動通過流體(參見美國專利第5,930,026、5,961,804、6,017,584、6,067,185、6,118,426、6,120,588、6,120,839、6,124,851、6,130,773、與6,130,774號、美國專利申請案公開第2002/0060321、2002/0090980、2003/0011560、2003/0102858、200310/5/702、200310222315、2004/0014265、2004/0075634、2004/0094422、2004/0105036、2005/0062714、與2005/0270261號、及國際申請案公告第WO 00/38000、WO 00/36560、WO 00/67110、與WO 01/07961號、及歐洲專利第1,099,207 B1、與1,145,072 B1號、及上述美國專利第7,012,600號討論之其他MIT與E Ink專利及申請案)。
電泳介質有數種不同之變化。電泳介質可使用液態或氣態流體；氣態流體參見例如Kitamura,T.等人之“Electrical toner movement for electronic paper-like display”,IDW Japan,2001,Paper HCSl-1，與Yamaguchi,Y.等人之“Toner display using insulative particles charged triboelectrically”,IDW Japan,2001,Paper AMD4-4)、美國專利公開第2005/0001810號、歐洲專利申請案第1,462,847、1,482,354、1,484,635、1,500,971、1,501,194、1,536,271、1,542,067、1,577,702、1,577,703、與1,598,694、及國際申請案第WO 2004/090626、WO 2004/079442、與WO 2004/001498號。此介質可包含數個小囊而膠囊化，其各本身包含具懸浮在液態懸浮介質中之電泳移地移動粒子的內相、及包圍內相之囊壁。一般而言，此囊本身係保持在聚合物黏結劑內形成位於兩個電極間之內聚層；參見上述MIT與E Ink專利及申請案。或者在膠囊化電泳介質中包圍分離微囊之壁可以連續相代替，以製造聚合分散電泳顯示器，其中電泳介質包含電泳流體之多個分離滴、及聚合材料之連續相；參見例如美國專利第6,866,760號。為了本申請案之目的，其將此聚合物分散電泳介質視為膠囊化電泳介質之次物種。另一種變化為所謂之「微胞電泳顯示器」，其中將帶電粒子與流體保留在多個形成於載體介質(一般為聚合膜)內之腔內；參見例如美國專利第6,672,921與6,788,449號。
雖然電泳介質經常不透明(由於例如在許多種電泳介質中，粒子實質上阻擋可見光穿透通過顯示器)且以反射模式操作，其可使許多種電泳顯示器以所謂之「快門模式」操作，其中一種顯示狀態為實質上不透明且另一為透光性。參見例如上述美國專利第6,130,774與6,172,798號，及美國專利第5,872,552、6,144,361、6,271,823、6,225,971、與6,184,856號。類似電泳顯示器但依賴電場強度變動之介電電泳可以類似模式操作；參見例如美國專利第4,418,346號。其他型式之電光顯示器亦可以快門模式操作。
膠囊化電泳顯示器一般不遭受傳統電泳裝置之群聚及沉降失敗模式，而且提供其他之優點，如在多種撓性與剛性基板上印刷或塗覆之能力。(使用文字「印刷」意圖包括全部形式之印刷及塗覆，其包括但不限於：預先計量塗覆，如貼片模塗覆、槽式或擠壓塗覆、滑片或串接塗覆、簾塗；輥塗，如輥式刮刀塗覆、正向與逆向輥塗；凹版塗覆；浸塗；噴塗；液面彎曲式塗覆；旋塗；刷塗；空氣刀塗覆；絲網印刷法；靜電印刷法；熱印刷法；噴墨印刷法；電泳沉積(參見美國專利第7,339,715號)；及其他類似技術。)因此所得顯示器可為撓性。此外因為顯示介質可被印刷(使用各種方法)，顯示器本身可不昂貴地製造。
其他型式之電光介質(例如聚合物分散液晶)亦可用於本發明之顯示器。
電光顯示器通常包含一層電光材料、及配置於電光材料對立側之至少二其他層，此二層之一為電極層。在大部分之此種顯示器中，兩層均為電極層，而且將電極層之一或兩者均圖案化以界定顯示器之像素。例如可將一電極層圖案化成為長形列電極，及將另一層圖案化成為對列電極以直角伸展之長形行電極，像素係由列與行電極之交叉點界定。或者且更常為一電極層具有單一連續電極之形式，及將另一電極層圖案化成為像素電極之矩陣，其各界定顯示器之一個像素。在另一型欲用於鐵筆(stylus)、印刷頭、或與顯示器分開之類似可移動電極的電光顯示器中，相鄰電光層之層僅一層包含電極，電光層對立側之層為欲防止可移動電極損壞電光層之保護層。
製造三層電光層通常涉及至少一種積層操作。例如在許多上述之MIT與E Ink專利及申請案中，其敘述一種用於製造膠囊化電泳顯示器之方法，其中將在黏結劑中包含囊之膠囊化電泳介質塗覆在於塑膠膜上包含氧化銦錫(ITO)或類似導電性塗層(其作為最終顯示器之一個電極)之撓性基板上，囊/黏結劑塗層乾燥形成最終黏附於基板之電泳介質的內聚層。分別地製備含像素電極陣列、與連接像素電極以驅動電路之合適排列導體的底板。為了形成最終顯示器，其使用積層黏合劑將其上具有囊/黏結劑層之基板積層至底板。(其可使用非常類似之方法，藉由以鐵筆或其他可移動電極可在其上滑動之簡單保護層(如塑膠膜)代替底板，而製備可用於鐵筆或類似可移動電極之電泳顯示器。)在此方法之一個較佳形式中，底板本身為撓性，而且係藉由將像素電極與導體印刷在塑膠膜或其他撓性基板上而製備。藉此方法量產顯示器之顯而易知積層技術為使用積層黏合劑之捆式積層。類似之製造技術可用於其他型式之電光顯示器。
如上述美國專利第6,982,178號所討論(參見第3欄，第63行至第5欄，第46行)，許多用於固態電光顯示器之組件、及用於製造此等顯示器之方法係源自用於液晶顯示器(LCD’s)之技術。然而用於組合LCD’s之方法無法用於固態電光顯示器。通常藉由在分別之玻璃基板上形成底板與前電極，然後黏合地將這些組件固定在一起，其間留下小孔，將所得組件置於真空下，及將組件浸於液晶液中，使得液晶流經底板與前電極間之孔來組合成LCD’s。最後液晶在定位而將孔密封提供最終顯示器。
LCD組合方法無法容易地轉移至固態電光顯示器。因為電光材料為固態，其必須在此二個體彼此固定之前存在於底板與前電極之間。此外與液晶材料相反，其係簡單地置於前電極與底板之間而未附著於任一者，固態電光介質通常需要固定於兩者；在大部分之情形，固態電光介質係形成於前電極上，因為其通常較將介質形成於含電路底板上容易，然後將前電極/電光介質組合積層至底板，一般藉由以黏合劑覆蓋電光介質之全部表面且在熱、壓力、可能及真空下積層。因而大部分先行技藝之固態電光顯示器最終積層用方法本質上為分批方法，其中(一般)在最終組合前使電光介質、積層黏合劑與底板緊密地在一起，而且希望提供較佳地適用於量產之方法。
美國專利第6,982,178號敘述一種極適合量產之組合固態電光顯示器(包括膠囊化電泳顯示器)的方法。本質上，此專利敘述所謂之「前面積層板」(front plane laminate,“FPL”)，其依序包含透光性導電層、電接觸導電層之一層固態電光介質、黏合層、及釋放片。一般而言，透光導電層係以基板可人工地捲繞如直徑10吋(254毫米)圓筒而不會永久性變形之方式載於透光基板(其較佳為撓性)上。在此專利所使用名詞「透光性」表示此設計之層傳送足以使透過此層觀看者觀察到電光介質之顯示狀態變化之光，其通常透過導電層與相鄰表面(若有)而觀看；在電光介質顯示非可見光波長之反射率變化的情形，名詞「透光性」當然應解讀成指相關非可見光波長之穿透。
美國專利第6,982,178號亦敘述一種用於在將前面積層板倂入顯示器中之前，測試前面積層板中電光介質之方法。在此測試方法中，釋放片具有導電層，及將足以改變電光介質之光學狀態的電壓施加於此導電層與電光介質對立側導電層之間。然後觀察電光介質顯示介質中之任何缺陷，如此避免將缺陷電光介質積層到顯示器中，造成破壞全部顯示器(不僅是有缺陷的前面積層板)之成本。
美國專利第6,982,178號亦敘述用於測試前面積層板中電光介質之第二方法，其係藉由將靜電荷置於釋放片上，從而在電光介質上形成影像。然後以如前之相同方式觀察此影像以偵測電光介質中之任何缺陷。
使用此前面積層板之電光顯示器的組合可藉由自前面積層板去除釋放片，及在有效地造成黏合層黏附底板之條件下將黏合層接觸底板，因而將黏合層、電光介質層與導電層固定於底板而進行。此方法極適合量產，因為前面積層板可量產，其一般使用輥對輥塗覆技術，然後切成用於指定底板所需之任何大小之片。
美國專利申請案第2004/0155857號敘述所謂之「雙面釋放片」，其本質上為上述美國專利第6,982,178號之前面積層板的簡化版本。雙面釋放片之一種形式包含包夾於二黏合層間之一層固態電光介質，黏合層之一或兩者均被釋放片覆蓋。雙面釋放片之另一種形式包含包夾於二釋放片間之一層固態電光介質。雙面釋放片之兩種形式均欲用於通常類似由已前述之前面積層板組合電光顯示器之方法的方法，但是涉及兩次分別之積層；一般而言，其在第一積層中將雙面釋放片積層至前電極而形成前次組件，然後在第二積層中將前次組件積層至底板形成最終顯示器，然而如果需要則此二積層之次序應可反轉。
上述2007/0109219號專利敘述所謂之「反式前面積層板」，其為上述美國專利第6,982,178號所述之前面積層板的變體。此反式前面積層板依序包含透光性保護層與透光性導電層至少之一、黏合層、一層固態電光介質、及釋放片。此反式前面積層板係用於形成一種在電光層與前電極或前基板之間具有一層積層黏合劑的電光顯示器、在電光層與底板之間可或無第二黏合(一般為薄)層。此電光顯示器可合倂良好之解析度與良好之低溫性能。
如上述美國專利第7,012,735與7,173,752號所述，用於電光顯示器(或前面積層板、反式前面積層板、雙面釋放膜、或用於製造此雷光顯示器之其他次組件)之積層黏合劑的選擇出現特定之異常問題。由於積層黏合劑通常位於電極之間，其施加所需電場以改變電光介質之電狀態，黏合劑之電性質通常極重要。積層黏合劑亦需要滿足數種機械及流變標準，包括黏合劑強度、可撓性、在積層溫度之承受及流動能力等。可滿足全部相關電與機械標準之市售黏合劑的數量少，而且實際上最適合之積層黏合劑為特定之聚胺基甲酸酯，如美國專利申請案公告第2005/0107564號所述者。這些聚胺基甲酸酯係基於四甲基二甲苯二異氰酸酯(TMXDI-系統名1,3-雙(1-異氰酸基-1-甲基乙基)苯)與聚丙二醇及2,2-雙(羥基甲基)丙酸之聚合，其以伸己二胺延長鏈。在製備聚胺基甲酸酯後，藉由以三乙胺中和且以水稀釋而將其分散成為水性乳膠狀懸浮液。然而實際上無法藉由在其製造中控制所使用材料之比例而改變聚胺基甲酸酯之導電度。
結果聚胺基甲酸酯黏合劑不為足以用於許多電光顯示器及電光組件之導電性，及已知藉由將其摻雜鹽或其他材料而增加其導電度，如上述美國專利第7,012,735與7,173,752號專利所述。用於此目的之較佳摻雜劑為六氟磷酸四丁銨(以下稱為“TBAHFP”)。不幸地，其已發現以此方式調配之黏合劑會損壞包含由特定有機半導體製成之電晶體的主動矩陣底板。本發明提供替代形式之積層黏合劑，其在用於含有機半導體之顯示器時可降低或排除先行技藝黏合劑造成之問題。本發明亦延伸至修改用於電光顯示器之黏結劑以在含有機半導體之顯示器中降低或排除先行技藝黏合劑造成之問題。
本發明具有兩個主要態樣。第一態樣係關於以不使材料擴散出黏合層之方式將離子性材料倂入黏合層中。第二態樣係關於將黏合材料或黏結劑前處理以去除可能損壞有機半導體之特定可擴散物種。
因而本發明之一個態樣提供一種包含黏合層與一層電光材料之電光組件，黏合層包含聚合黏合材料與離子性材料；離子性材料之陽離子與陰離子之一固定於聚合黏合材料，而且其他陽離子與陰離子自由移動通過聚合黏合材料；離子性材料降低聚合黏合材料之體積電阻率，而且在將聚合黏合材料加熱至50℃時不會被去除。
以下為了方便而將固定於聚合黏合材料之離子性材料的陽離子或陰離子稱為「固定離子」，及將自由移動通過聚合黏合材料之陽離子或陰離子稱為「移動離子」。一般而言，固定離子係化學地鍵結至聚合黏合劑，而且用於提供此鍵結聚胺基甲酸酯黏合劑之離子的各種技術討論於下。然而此化學鍵結並非絕對必要，只要使固定離子無法移動通過聚合黏合劑；例如固定離子可形成與聚合黏合劑不同但與之鏈纏結的聚合物之一部分。
在一種形式之電光組件中，離子性材料包含固定於聚合黏合材料之四級銨或鏻陽離子、及羧酸陰離子。聚合黏合材料可包含聚胺基甲酸酯。或者離子性材料可包含固定於聚合黏合材料之四級銨或鏻陽離子，及六氟磷酸、四丁基硼酸、或四苯基硼酸陰離子。在另一種形式之電光組件中，離子性材料包含衍生自鹼性單體、及選自包含磺酸基、硫酸基、六氟磷酸基、四氟硼酸基、雙(甲磺醯基)醯亞胺基、磷酸基、與膦酸基之移動陰離子的重複單元。鹼性單體可包含例如任一或多種乙烯基吡啶、丙烯酸β-二甲胺基乙酯、N-甲基或苄基(乙烯基吡啶)、N-烷基或烷芳基-N’-乙烯基咪唑、與丙烯酸或甲基丙烯酸β-(三甲胺基乙酯)。
在此電光組件中，電光材料可包含轉動二色構件或電致變色材料。或者電光材料可包含一種含多個配置於流體中且在電場影響下可移動通過流體之帶電粒子的電泳材料。帶電粒子與流體可侷限於多個囊或微胞內。或者帶電粒子與流體可如多個被含有聚合材料之連續相所包圍的分離滴而存在。流體可為液態或氣態。
本發明延伸至包含本發明電光組件之電光顯示器、前面積層板、反式前面積層板、或雙面釋放膜。
本發明亦提供一種包含黏合層與一層電光材料之電光組件，黏合層包含聚合黏合材料，其已接受滲析或滲濾以去除分子量小於約3,500之有機物種。
本發明亦提供一種包含黏合層與一層電光材料之電光組件，黏合層包含聚合黏合材料，該聚合黏合材料具有按黏合層與一層電光材料之總重量計為不超過約500ppm之N-甲基吡咯啶酮含量。
在此電光組件中，聚合黏合材料可包含聚胺基甲酸酯。N-甲基吡咯啶酮之含量按黏合層與一層電光材料之總重量計較佳為不超過約200ppm，而且希望為100ppm。
在此電光組件中，電光材料可包含轉動二色構件或電致變色材料。或者電光材料可包含一種含多個配置於流體中且在電場影響下可移動通過流體之帶電粒子的電泳材料。帶電粒子與流體可侷限於多個囊或微胞內。或者帶電粒子與流體可如多個被含聚合材料之連續相包圍的分離滴而存在。流體可為液態或氣態。
本發明延伸至包含本發明電光組件之電光顯示器、前面積層板、反式前面積層板、或雙面釋放膜。
本發明亦提供一種包含連續相與不連續相之電泳介質，不連續相包含多個滴，其各包含懸浮流體、與至少一個配置於懸浮流體內且在電場影響下可移動通過流體至電泳介質之粒子；連續相包圍及膠囊化不連續相且包含已接受滲析或滲濾以去除分子量小於約3,500之有機物種的聚合黏結劑。電泳介質可為膠囊化或聚合分散性，即其在各滴與黏結劑之間可有或無囊壁。
本發明亦提供一種包含連續相與不連續相之電泳介質，不連續相包含多個滴，其各包含懸浮流體、與至少一個配置於懸浮流體內且在電場影響下可移動通過流體至電泳介質之粒子；連續相包圍及膠囊化不連續相且包含具有按電泳介質之重量計為不超過約1000ppm之N-甲基吡咯啶酮含量的黏結劑。
本發明延伸至包含本發明電光組件或電泳介質之電光顯示器、前面積層板、反式前面積層板、或雙面釋放膜。
本發明之顯示器可用於其中已使用先行技藝電光顯示器之任何應用。因此例如本發明顯示器可用於電子書閱讀器、可攜式電腦、平板電腦、行動電話、智慧卡、標誌、手錶、貨架標籤、及隨身碟。
如上所示，本發明具有兩個主要態樣，第一係關於將不可擴散離子性材料倂入黏合層中，及第二係關於在電泳介質與顯示器中使用經滲析或滲濾黏合劑材料及/或黏結劑。以下主要分別地討論本發明之兩個主要態樣，但是顯然本發明之兩個態樣可合倂至單一物理顯示器中。
部分A：不可擴散離子性材料
如上所示，本發明之一個態樣提供一種包含一電光黏合層與一層之電光組件。黏合層含離子性材料，其中一種離子無法移動通過黏合層而其他則可。此型離子性材料防止自黏合層擴散出及可能損壞離子擴散至其中之其他層(例如有機半導體層)。
聚合黏合層中之離子性導電已證明係因「跳躍」機構而發生，其中解離自由離子改寫離子性凝集體(離子對與更高凝集體)，大部分這些凝集體本質上為中性。依照本發明，僅離子性材料之陰離子與陽離子之一可移動。固定離子受限於單一位置，而移動離子仍自由移動。合適離子性材料之一個實例為聚合鹽，例如聚合羧酸之離子性鹽。在此情形，羧酸離子係有效地固定，因為其附著聚合物鏈且僅可隨聚合物整體移動。另一方面，陽離子性抗衡離子可自由地參與跳躍機構，而且其可移動之速率依與陰離子性羧酸基之靜電交互作用、羧酸基抗衡離子凝集體在黏合介質中之濃度、介質之黏度、及抗衡離子被介質溶解之自由能量而定。
如同上述美國專利第7,012,735號所述之摻離子黏合劑，在本發明中大型陽離子為有利的，因為其對離子性凝集狀態可具有相當低之吸引靜電能量，因此易由其解離。至於實例，氫氧化四級銨可用以中和聚胺基甲酸酯之羧酸官能基，導致可支持上述離子性導電之四級銨羧酸鹽聚合物。
其希望選擇離子性材料使得可藉由改變聚胺基甲酸酯之羧酸含量、亦藉使用之陽離子修改及調整乾燥後之最終黏合層之導電度。例如在其中聚胺基甲酸酯上羧酸基經氫氧化四級銨鹽中和之上述系統中，在特定羧酸含量預期導電度依以下之次序增加：
四甲銨<四乙銨<四丁銨等。
亦可使用鏻鹽，而且因為中央原子之大小較大，其應較含氮同系物稍微更有導電性。其他陽離子性物種(例如金屬之錯合物離子)亦可用於此目的。由於離子為介質之固有部分且因此無法相分離成為分離之結晶相，離子性材料在黏合劑中之溶解度不為此方式之議題。
聚合黏合劑之酸性成分亦可藉由以解離常數較高之基(例如硫酸單酯、磺酸、亞磺酸、磷酸、亞磷酸基、或磷酸酯)取代羧酸成分而更為酸性，只要其存在至少一種可解離質子。因其大型大小、及在低極性乾燥黏合介質中之相當高程度離子性解離，四級鹽及其他大型陽離子作為抗衡離子仍預期最有用。如果附著充分拉電子官能基，則亦可使用氮系酸(例如RSO2 -NH-SO2 R)。在此情形可使用幾乎任何移動離子，包括三級銨，因為移動離子係以質子形式存在，即使是在乾燥黏合劑中。然而基於較大胺之移動離子(即烷基尾較長之離子)可能仍較佳，因為其大小有效地較大，因此包含其之離子對較易解離。
或者黏合劑上之羧酸基可用於非強布忍斯特酸之移動離子，即其不具有酸性質子，如以上討論之四級陽離子。
其中陽離子為固定離子之黏合劑組成物可藉由在聚合物主幹中使用四級銨基或作為側鏈，及較佳為使用大型陰離子(例如六氟磷酸基、四丁基硼酸基、四苯基硼酸基等)作為移動離子而構成。四級銨基可被鏻、鋶、或無可解離氫之其他陽離子性基取代，包括由錯合金屬陽離子而形成者。後者之實例包括含多醚/鋰離子錯合物，特別是環形多醚(例如18-冠-6)，或具過渡金屬離子之多胺錯合物。在此情形，陰離子性移動離子可包括上列型式之離子，加上較強烈鹼性材料，如羧酸基或甚至酚。
替代性固定陽離子黏合材料包括含衍生自鹼性單體之重複單元的聚合物，例如聚(乙烯基吡啶)、聚(丙烯酸β-二甲胺基乙酯)等，及含此等基之共聚物，結合非良好布忍斯特受體之移動陰離子(例如磺酸基、硫酸基、六氟磷酸基、四氟硼酸基、雙(甲磺醯基)醯亞胺基、磷酸基、膦酸基等)。亦可使用衍生自此胺基單體之四級鹽，例如聚(N-甲基或苄基(乙烯基吡啶))、聚(N-烷基(或烷芳基)-N’-乙烯基咪唑鹽)、與聚(丙烯酸或甲基丙烯酸(β-三甲胺基乙酯))鹽、及包含這些離子性基之乙烯基共聚物。如前，較大之移動離子較佳。
這些化學修改技術不限於聚胺基甲酸酯，但可應用於任何合適結構之聚合物。例如乙烯基為主聚合物可含陰離子或陽離子固定離子。
部分B：滲析或滲濾黏合材料及/或黏結劑
如所示，本發明之一個態樣降低或排除因離子性摻雜劑自黏合層移動至電光顯示器之其他層中造成之問題，特別是損壞包含由特定有機半導體製成之電晶體的主動矩陣底板。然而現已發現，這些問題之成因不限於離子性摻雜劑，而是包括存在於先行技藝黏合劑與黏結劑組成物中之其他瞬間物種(fugitive species)，其可以類似離子性摻雜劑之方式，自電光顯示器之黏合或黏結層移動至其他層。一種特別顧慮之此種瞬間物種為N-甲基吡咯啶酮(NMP)，其在聚胺基甲酸酯製備中作為溶劑。在某些情形有所顧慮之其他瞬間物種包括用於聚胺基甲酸酯製備之其他溶劑，及來自聚合反應之特徵為滲析不良的低分子量分子。其已發現，藉由小心地乾燥黏合層而去除NMP改良層之儲存安定性。積層黏合劑之滲析去除NMP亦及其他低分子量材料，而且甚至更有效。由於電中性防止固定與移動離子之淨分離，本發明之不可擴散離子性材料黏合劑組成物可接受滲析，而且在滲析後黏合材料含極少或無可擴散材料。本黏合劑因此已發現對於降低積層黏合劑對含有機半導體之底板的性能之有害影響特別有效。亦可使用滲濾代替滲析。
如已所述，本發明之不可擴散離子性材料黏合材料可藉滲析或滲濾純化。然而藉滲析合成這些黏合材料亦有用。例如多胺或多醚之水溶液可藉聚合物溶液在合適水溶性金屬鹽之溶液中滲析而部分地轉變成陽離子性錯合物。
滲析或滲濾亦可用以在將此黏合劑混合習知離子性摻雜劑之前，自習知聚胺基甲酸酯黏合劑去除NMP及其他短暫物種。因此如已所示，在第二主要態樣中，本發明提供一種包含黏合層與一層電光材料之電光組件，黏合層包含聚合黏合材料，其已接受滲析或滲濾以去除分子量小於約3,500之有機物種。此滲析或滲濾可用以去除NMP、四氫呋喃(THF)、與丙酮等。類似地，本發明之第二態樣亦提供一種包含黏合層與一層電光材料之電光組件，黏合層包含N-甲基吡咯啶酮含量不超過約500ppm，較佳為不超過約200ppm，而且希望為不超過約100ppm之聚合黏合材料，其在全部情形均按黏合層與一層電光材料之總重量計。
本發明之第二態樣亦提供一種包含連續相與不連續相之電泳介質，該不連續相包含多個滴，其各包含懸浮流體、與至少一個配置於懸浮流體內且在施加電場時可移動通過流體至電泳介質之粒子；該連續相包圍及膠囊化不連續相且包含已接受滲析或滲濾以去除分子量小於約3,500之有機物種的聚合黏結劑。電泳介質可為膠囊化或聚合分散性，即其在各滴與黏結劑之間可有或無囊壁。本發明之第二態樣亦提供一種包含連續相與不連續相之電泳介質，該不連續相包含多個滴，其各包含懸浮流體、與至少一個配置於懸浮流體內且在施加電場時可移動通過流體至電泳介質之粒子，該連續相包圍及膠囊化不連續相且包含N-甲基吡咯啶酮、四氫呋喃與丙酮之總含量不超過約1000ppm，較佳為不超過約400ppm，而且希望為不超過約200ppm的聚合黏合材料，其在全部情形均按電泳介質(即連續與不連續相之組合)之重量計。
如已所示，本發明之第二態樣可用於自用於電光顯示器之積層黏合劑及/或黏結劑去除NMP、可能及其他短暫物種。在許多情形，自黏結劑去除短暫物種遠較自積層黏合劑去除重要。積層黏合層之製備一般涉及將可流動形式之黏合劑塗覆在釋放片上，然後將黏合劑之層乾燥使得在釋放片上形成黏合劑之內聚層。乾燥步驟之高溫及低塗覆速度足以驅除高比例之揮發性有機物種；例如其已發現，以50,000ppm之NMP塗覆之積層黏合劑在乾燥後具有僅200ppm之NMP。此外由於在乾燥期間存在之層僅為積層黏合劑與釋放片(黏合劑對電光介質之積層僅在乾燥步驟後發生)，選擇乾燥條件可僅基於積層黏合劑本身之性質，而且不必考量電光介質之性質。相反地，用於電泳介質之黏結劑一般混合介質之不連續相以形成漿液，其然後塗覆及乾燥形成電泳介質。因此在此情形，乾燥條件必須考量不連續相之性質，而且特別地在意同時去除揮發性不連續相溶劑。最後由品管觀點，去除具有損壞任何預期電光介質可能接觸之底板的可能性之全部材料表示良好之確保政策，使得將未知組分之數量(其濃度可因未知或無對照而改變)保持最小，顯然關於良好之製程，其極希望使用已知組成物之純材料。
滲析及滲濾均為純化膠體與聚合物之懸浮液的熟知方式。在兩種技術中，懸浮液被半滲透薄膜侷限，其對立側為洗液，一般為水或緩衝液。可通過薄膜且溶於洗液之分子在設備之兩個區域間平衡，及藉洗液交換而自懸浮液去除。一般而言，薄膜係由可使低分子量材料選擇性通過之材料製造，而且通常使用水作為溶劑；本發明已發現分子量遮斷(MWCO)為約3.5kD之薄膜為有用的。由於NMP為水溶性溶劑，這些技術極適合去除此污染物。同時亦可去除其他之可溶材料，某些具可能有害性質。其未要求去除物種明顯為揮發性，如同乾燥去除之情形。藉由調整薄膜之性質可改變去除分子之種類。例如如果在特定積層黏合劑或黏結劑中存在水溶性寡聚聚合物碎片成問題，則可使用具較高MWCO之薄膜去除此碎片；具各種MWCO之各種半滲透薄膜為市售。
滲析或滲濾可用於本方法，但是滲濾對商業生產較佳。滲析為簡單之平衡方法，而滲濾使用高流動條件及高跨膜壓力加速通過薄膜之質量運輸。滲濾實質上較滲析快，而且可在防止欲純化材料稀釋(其經常為滲析之情形)之條件下使用。滲濾為易縮放方法，而且實驗室規模及生產規模設備均可以合理之價格得到。滲濾為廣泛地用於生化及其他產業之確立產業步驟。
本發明人已證明滲析與滲濾均有效地自市售聚胺基甲酸酯乳膠之懸浮液去除NMP。其已實驗地發現，使用具低MWCO(3.5kD)之薄膜將聚胺基甲酸酯乳膠滲析及滲濾數小時可將NMP含量降低超過10倍。例如其藉滲濾將聚胺基甲酸酯黏結劑之NMP含量自約14%(140,000ppm)降至約500ppm。在使用滲析時，NMP去除效率可能被乳膠之稀釋限制，其使乳膠難以塗覆，特別是在積層黏合劑之情形。乳膠可藉由在低壓下蒸發過量水而濃縮，但是其為不便之方法。檢驗經純化聚胺基甲酸酯乳膠之分子量分布顯示其本質上與起始材料相同，即在滲析期間未失去聚合物。在使用經滲析材料代替未滲析黏結劑與積層黏合劑時，其觀察到一些優點。
首先其大大地排除有機半導體底板之性能降低。如果僅滲析黏結劑而無積層黏合劑，則可得到相同之結果。然而如果省略黏結劑滲析，則遭遇有機半導體裝置性能之嚴重降低。
第二個優點為使用經滲析材料之胞隙電阻(前面積層板之導電度的一種測度)較高，一般為約50%。較高之胞隙電阻可使對操作電晶體之使用導電度的要求較少(即可為較低之開關比)。其為有機半導體電晶體之特別重要特徵，其一般不如無機電晶體之開關比高。
第三個優點為小幅改良由經滲析乳膠製造之電泳介質的電光性質。如以下實例5所描述，使用經滲析聚胺基甲酸酯乳膠相對使用未滲析材料在動態範圍(介質之全白與黑色電光狀態間之差異)產生約2L*(使用L*之一般CIE定義)之改良。
以下藉實例顯示用於本發明之較佳試劑、條件及技術的細節，雖然其僅為描述性。
實例1：以氫氧化四丁銨中和而合成TMXDI-PPO聚胺基甲酸酯
此實例製備之聚胺基甲酸酯類似以下實例2製備之先行技藝聚胺基甲酸酯，除了其具有較高之酸含量。
在裝有磁性攪拌器、冷凝器與氮入口之三頸圓底燒瓶中製備預聚物。反應係在氮下進行。將四甲基二甲苯二異氰酸酯(TMXDI，由Aldrich Chemical Compgny供應，16.34克，0.067莫耳)、聚(丙二醇)二醇(由Aldrich Chemical Company供應，平均Mn 為約2000，33.5克，0.0168莫耳)、與二月桂酸二丁錫(由Aldrich Chemical Company供應，0.04克)裝入燒瓶中且將混合物在90℃油浴中加熱2小時。然後將於1-甲基-2-吡咯啶酮(得自Aldrich，8.5克)之2,2-雙(羥基甲基)丙酸(得自Aldrich，3.35克，0.025莫耳)溶液加入燒瓶，及使反應在90℃進行又2小時而得到NCO封端預聚物。然後將反應混合物之溫度降至70℃。分別地將氫氧化四丁銨(NBu4 OH)(得自Aldrich，6.15克，0.0237莫耳)與去離子水(100克)裝入具機械攪拌器、溫度計與氮入口之外套500毫升玻璃反應器中，及將所得混合物在氮下加熱至35℃。然後將預聚物混合物緩慢地加入NBu4 OH水溶液，以在機械攪拌及氮大氣下將預聚物轉化成水系分散液(water-borne dispersion)。在伸己二胺(得自Aldrich)溶於少量35℃水之分散步驟後進行鏈延長反應。鏈延長反應之終點係由pH測量決定。最後將所得分散液加熱至50℃經1小時，以確定任何殘餘異氰酸基被水消耗。
實例2：以三乙胺中和而合成TMXDI-PPO聚胺基甲酸酯
重複實例1至得到NCO封端預聚物且將反應混合物之溫度降至70℃之處。然後將三乙胺(得自Aldrich，2.4克，0.0237莫耳)經30分鐘時間緩慢地加入以中和羧酸。然後在外套500毫升玻璃反應器中，在機械攪拌及氮大氣下將反應混合物緩慢地加入35℃去離子水(100克)，以將預聚物轉化成水系分散液。以如實例1之相同方式進行鏈延長反應及最終將分散液加熱至50℃。
實例3：由實例1及2製備之材料製備實驗單像素顯示器
將以上實例1及2製備之聚胺基甲酸酯分別地以約20微米之(乾燥)厚度塗覆在金屬化釋放膜上。在60℃及運輸速率為1呎/分鐘(約5.1毫米/秒)之帶式運輸乾燥烤箱中進行經塗覆聚合膜之乾燥；已知這些條件將NMP含量降至非常低之程度。分別地實質上如美國專利第7,002,728號之實例4所述而製備電泳介質，及塗覆在5mil(127微米)聚(對酞酸伸乙酯)(PET)膜(其一個表面塗有ITO)之塗氧化銦錫(ITO)表面上。將兩個次組件以電泳層接觸積層黏合劑而彼此積層，形成上述美國專利第6,982,178號所述之前面積層板。將釋放片自前面積層板剝除且將其餘層積層至實驗單像素2吋(51毫米)平方底板，其在PET膜上包含一層碳黑，而形成實驗單像素顯示器。無額外摻雜劑倂入任一黏合劑塗層。使實驗顯示器在50%相對濕度條件下1日(如一些上述E Ink專利及申請案所討論，電泳顯示器之電光性質隨電泳層之水分含量而改變，因此希望在測試前使測試樣本在標準條件下)。
然後藉由在各種電壓使用250毫秒脈衝將其驅動至其黑及白色光學狀態，測量黑及白色光學狀態之反射率，及將這些反射率換算成習知L*值，而測試實驗顯示器之電光性質，其中L*具有一般之CIE定義：
L*=116(R/R0 )1/3 -16，
其中R為反射率，及R0 為標準反射率值。以下表1顯示在各種電壓得到之動態範圍(介質之黑與白色光學狀態L*值間之差異)：
由表1可知，本發明之積層黏合劑在全部驅動電壓均顯示實質上比對照黏著劑有較大之動態範圍。此改良與由不同導電度之預期一致，而且類似使用低酸含量之先行技藝摻雜黏合劑。以三乙胺中和之對照黏著劑顯示對很有阻抗性的積層黏合劑有預期之電光回應。在操作期間，顯示器顯示的目視檢查具對照黏合劑之顯示器僅在顯示器邊緣顯示少量之光暈，而使用本發明黏合劑之顯示器顯示大量光暈。高程度光暈亦與高導電度之黏合劑一致。
實驗顯示器亦接受低溫測試。如許多上述E Ink專利及申請案所討論，電泳顯示器之電光性能在低溫驅於快速地下降，其至少部分地因為積層黏合劑之導電度隨溫度下降。為了測定本發明實驗顯示器之低溫行為，其在+25至-25℃之溫度使用250或500毫秒時間之15伏脈衝驅動顯示器，而且使用在驅動脈衝結束後2分鐘取得之反射率值測定動態範圍。(取得反射率值前之此2分鐘暫停可得影響反射率值散逸之短期效果。)以如前之相同方式將所得反射率值換算成動態範圍值，及結果示於以下表2。
由表2之資料可知，本發明之黏合劑在低至約-10℃提供合適之性能，其條件為使用脈衝時間補償，即其條件為在低溫延長驅動脈衝。此低溫性能與高摻雜先行技藝積層黏合劑相似。
實例4：藉滲析純化本發明之積層黏合劑
將以上實例1製備之積層黏合劑樣品(49.3克，35重量%固體)置於滲析薄膜(Fisher(註冊商標)再生纖維素薄膜，MWCO 3500)之管中。在以夾子封閉管子兩端後，將管子浸於連續添補攪拌水槽中經約4小時。在此時間結束時回收61.6克之材料，其具29.5%之固體含量(回收率95%)。起初NMP含量為4.4%；在滲析後此含量為1.4%。NMP含量可作為去除其他水溶性低分子量材料之代用品。
使用以上實例4製備之經滲析積層黏合劑與先行技藝積層黏合劑(經滲析與未滲析)、及有專利的有機半導體底板，顯示器之預備長期儲存測試顯示本發明之經滲析積層黏合劑具有實質上優於先行技藝黏合劑之長期儲存特徵。
實例5：在電泳顯示器中使用經滲析黏結劑及積層黏合劑
實質上如美國專利申請案公告第2008/0074730號之實例2所述合成聚胺基甲酸酯乳膠，而且在下述實驗中作為黏結劑。實質上如美國專利申請案公告第2005/0107564號之實例2所述合成第二聚胺基甲酸酯乳膠，而且在這些實驗中作為積層黏合劑。
實質上如美國專利第7,002,728號之實例7所述製備實驗單像素顯示器，但是使用上述黏結劑與積層黏合劑；將積層黏合劑摻雜180ppm之六氟磷酸四丁銨。其產生4組實驗顯示器如下：
(A)黏結劑或積層黏合劑均未滲析；
(B)黏結劑實質上如以上實例4所述而滲析，但是積層黏合劑未滲析；
(C)黏結劑未滲析，但是積層黏合劑實質上如以上實例4所述而滲析；及
(D)黏結劑或積層黏合劑均實質上如以上實例4所述而滲析。
然後實質上如美國專利第7,002,728號之實例7所述測試4組實驗顯示器之電光性質，但是使用300毫秒脈衝±15伏，及測量全白與黑色狀態反射率且換算成CIE L*單位。結果示於附圖之單一圖式中。在各組讀數中，左邊條表示顯示器之全白狀態，中間條表示全黑狀態，及右邊條表示動態範圍(即全白與黑色狀態間之差異，按L*單位測量)。
由圖式可知，黏結劑與積層黏合劑之滲析對顯示器之電光性質無影響。事實上，其中將黏結劑滲析之兩種顯示器(B與D)顯示改良之白色狀態，顯示器C與D顯示改良之黑色狀態(黑色狀態之改良當然由較低之L*表示)。其中黏結劑與積層黏合劑均滲析之顯示器D顯示4組顯示器中最大之動態範圍。
使用100與500毫秒時間之±15伏脈衝、及±10伏、100、300與500毫秒脈衝重複電光測試。在全部之情形，所得結果均與圖式所示一致。
在將含以上(A)-(D)所述黏結劑與積層黏合劑組合之前面積層板積層至使用有機電晶體之底板時，其觀察到含未滲析黏結劑之前面積層板造成有機電晶體之快速降解，而含經滲析黏結劑之前面積層板則否。使用經滲析積層黏合劑注意到類似但較小之影響。
由以上可知，本發明可提供積層黏合劑，其提供與先行技藝黏合劑相似之電光特徵與低溫性能，同時避免使用可損壞特定底板且可能導致其他問題之短暫離子性物種。
附圖之唯一圖式為顯示在以上實例5中得到之光學狀態讀數的圖表。

Claims (9)

  1. 一種包含黏合層與一層電光材料之電光組件，其中該黏合層包含聚胺基甲酸酯，其已接受滲析或滲濾以去除分子量小於約3,500之有機物種。
  2. 一種包含黏合層與一層電光材料之電光組件，其中該黏合層包含聚胺基甲酸酯，其具有按黏合層與一層電光材料之總重量計為不超過約500ppm之N-甲基吡咯啶酮含量。
  3. 如申請專利範圍第2項之電光組件，其中N-甲基吡咯啶酮之含量不超過200ppm。
  4. 如申請專利範圍第2項之電光組件，其中電光材料包含一種含多個配置於流體中且在電場影響下可移動通過流體之帶電粒子的電泳材料。
  5. 如申請專利範圍第4項之電光組件，其中流體為氣態。
  6. 如申請專利範圍第2項之電光組件，其係用於電光顯示器、前面積層板、反式前面積層板、或雙面釋放膜。
  7. 如申請專利範圍第6項之電光組件，其中該電光顯示器係用於電子書閱讀器、可攜式電腦、平板電腦、行動電話、智慧卡、標誌、手錶、貨架標籤、或隨身碟。
  8. 一種包含連續相與不連續相之電泳介質，其中該不連續相包含多個滴，每一滴各包含懸浮流體、與至 少一個配置於該懸浮流體內且在電場影響下可移動通過流體至電泳介質之粒子；該連續相包圍及膠囊化該不連續相且包含已接受滲析或滲濾以去除分子量小於3,500之有機物種的聚合黏結劑。
  9. 一種包含連續相與不連續相之電泳介質，其中該不連續相包含多個滴，每一滴各包含懸浮流體、與至少一個配置於該懸浮流體內且在電場影響下可移動通過流體至電泳介質之粒子；該連續相包圍及膠囊化該不連續相且包含具有按電泳介質之重量計為不超過1000ppm之N-甲基吡咯啶酮含量的聚合黏結劑。
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