CN109415607A - 纳米粒子填充的阻隔性粘合剂组合物 - Google Patents
纳米粒子填充的阻隔性粘合剂组合物 Download PDFInfo
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- CN109415607A CN109415607A CN201780037231.1A CN201780037231A CN109415607A CN 109415607 A CN109415607 A CN 109415607A CN 201780037231 A CN201780037231 A CN 201780037231A CN 109415607 A CN109415607 A CN 109415607A
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- C—CHEMISTRY; METALLURGY
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
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- C—CHEMISTRY; METALLURGY
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Abstract
本发明提供了一种阻隔性粘合剂组合物,其包含聚异丁烯树脂、有机改性纳米粘土(例如蒙脱石或膨润土)和吸附剂纳米粒子(例如用作干燥剂和/或吸气剂的CaO)。在优选的实施方案中,阻隔性粘合剂组合物设置在气体阻挡膜上以形成粘合性阻挡膜。然后,粘合性阻挡膜可用于防止在OLED显示器和固态照明、太阳能电池、电泳和电致变色显示器、薄膜电池、量子点器件、传感器(例如触摸传感器)和其它有机电子器件中遭受氧气和水分。粘合性阻挡膜特别适合于需要氧气和水分保护以及柔韧性和良好的光学透射率的应用。
Description
技术领域
本发明涉及阻隔性粘合剂组合物和粘合性阻挡膜。
背景技术
有机电子器件需要防止遭受水分和氧气,以便为商业应用提供足够长的寿命。因此利用封装材料来保护器件免于接触水分和氧气。玻璃是一种常用的封装材料,但玻璃大大损害了器件的柔韧性。因此,可期望用柔性阻挡膜代替玻璃。柔性阻挡膜可使柔性器件以及更轻、更薄、更坚固的刚性器件成为可能。
柔性阻挡膜已被商业化用于有机电子器件中的一般用途。通常使用粘合剂将柔性阻挡膜层合至其将要保护的器件。因此,重要的是粘合剂也具有良好的阻隔性质以使水分和氧气粘结线边缘侵入最小化。一些阻隔性粘合剂,诸如例如在美国专利申请公布US2014/0377554(Cho等人)中描述的那些包括作为“水分阻断剂”的纳米粘土。其它阻隔性粘合剂如描述于例如美国专利No.6,936,131(McCormick等人)中的那些包括干燥剂和/或吸气材料以吸收和/或吸附氧气和/或水分。
发明内容
鉴于前述内容,我们认识到,对于特定要求的有机电子器件应用,诸如例如长寿命有机发光二极管(OLED)显示器,需要改进的阻隔性粘合剂。
简而言之,在一个方面,本发明提供了包含聚异丁烯树脂、有机改性纳米粘土和吸附剂纳米粒子的阻隔性粘合剂组合物。
如本文所用,术语“吸附剂”是指用于吸收或吸附液体或气体诸如氧气或水分的材料。
在另一方面,本发明提供了阻隔性粘合剂组合物,其包含约50重量%至约75重量%的具有约300,000g/mol至约900,000g/mol的粘均分子量的聚异丁烯树脂、约1重量%至约10重量%的有机改性纳米粘土、约1重量%至约5重量%的钙氧化物纳米粒子和约10重量%至约25重量%的增粘剂,以上含量全部相对于组合物的总重量。
在又一个方面,本发明提供了包括设置在气体阻挡膜上的本发明的阻隔性粘合剂组合物的层的粘合性阻挡膜以及包括设置在防粘层之间的本发明的阻隔性粘合剂组合物的层的阻隔性粘合剂制品。
已发现,与未填充的聚异丁烯粘合剂或填充有纳米粘土或吸附剂纳米粒子中的一种的聚异丁烯粘合剂相比,填充有纳米粘土和吸附剂纳米粒子的本发明的聚异丁烯粘合剂组合物在阻隔性能方面提供显著改善。令人惊讶的是,即使与具有较高载量的纳米粘土或吸附剂纳米粒子中的一种的聚异丁烯粘合剂相比,也观察到这种改善。
附图说明
图1为阻挡膜构造的示意图。
图2是封装的有机器件的示意图。
图3是用于实施例中的阻挡膜构造的示意图。
图4是用于实施例中的钙测试的层合构造的示意图。
图5是用于实施例中的钙测试的层合构造的平面图。
图6是在加速老化条件下随着时间光密度损耗百分比的曲线图。
具体实施方式
本发明的阻隔性粘合剂组合物包含聚异丁烯树脂。聚异丁烯树脂通常具有约40,000g/mol至约2,600,000g/mol的粘均分子量。在一些实施方案中,聚异丁烯树脂具有约300,000g/mol至约900,000g/mol的粘均分子量。在一些实施方案中,树脂体系包括第一聚异丁烯树脂和(b)第二聚异丁烯树脂的共混物,第一聚异丁烯树脂具有约300,000g/mol至约500,000g/mol、约350,000g/mol至约450,000g/mol、或约400,000g/mol的粘均分子量,第二聚异丁烯树脂具有约700,000g/mol至约900,000g/mol、约650,000g/mol至约850,000g/mol、或约800,000g/mol的粘均分子量。
粘均分子量(Mv)通常基于Staudinger指数。Staudinger index Jo(cm3/g)通过Ubbelohde粘度计的毛细管I在20℃下的流动时间计算。
Jo=ηsp/c(1+0.31×ηsp)cm3/g(Schulz-Blaschke等式)
ηsp=t/to–1(比粘度)
t=溶液的流动时间,用Hagenbach Couette校正
to=溶剂的流动时间,用Hagenbach Couette校正
c=溶液浓度(g/cm3)
该粘均分子量是根据式Jo=3.06*10-2*Mv 0.65来计算的。
在一些实施方案中,相对于树脂体系的总重量,树脂体系包含约65重量%至约85重量%的聚异丁烯树脂。在一些实施方案中,相对于树脂体系的总重量,树脂体系包含约15重量%至约35重量%、约20重量%至约30重量%、或约25重量%的第一聚异丁烯树脂。在一些实施方案中,相对于树脂体系的总重量,树脂体系包含约40重量%至约60重量%、约45重量%至约55重量%、或约50重量%的第二聚异丁烯树脂。
聚异丁烯树脂通常为在主链或侧链中具有聚异丁烯树脂骨架的树脂。在一些实施方案中,聚异丁烯树脂基本上为异丁烯的均聚物,例如,可以商品名OPPANOL(BASF AG)和GLISSO-PAL(BASF AG)获得的聚异丁烯树脂。合适的可商购的聚异丁烯树脂的示例包括OPPANOL B15(Mv=85,000)、OPPANOL B50(Mv=400,000)、具有稳定剂的OPPANOL B50SF(Mv=400,000)、OPPANOL N50(Mv=425,000)、具有稳定剂的OPPANOL N50SF(Mv=425,000)、OPPANOL B80(Mv=800,000)和OPPANOL N80(Mv=800,000)。在一些实施方案中,聚异丁烯树脂包含异丁烯的共聚物,诸如例如,其中异丁烯与另一种单体共聚的合成橡胶。合成橡胶包括丁基橡胶,该丁基橡胶是大部分异丁烯与少量异戊二烯的共聚物,诸如例如,可以商品名VISTANEX(埃克森化学公司(Exxon Chemical Co.))和JSR BUTYL(日本丁基聚合物有限公司(Japan Butyl Co.,Ltd.))获得的丁基橡胶。合成橡胶还包括大部分异丁烯与苯乙烯、正丁烯或丁二烯的共聚物。在一些实施方案中,可使用异丁烯均聚物和丁基橡胶的混合物。其它可用的共聚物包括苯乙烯-异丁烯二嵌段共聚物(SIB)和苯乙烯-异丁烯-苯乙烯三嵌段共聚物(SIBS),以商品名SIBSTAR(Kaneka Corporation)购得。
例如,第一聚异丁烯树脂可包含异丁烯均聚物,并且第二聚异丁烯可包含丁基橡胶,或者第一聚异丁烯可包含丁基橡胶,并且第二聚异丁烯可包含异丁烯的均聚物。第一和第二聚异丁烯树脂可各自包含不止一种树脂。
聚异丁烯树脂通常具有与氢化脂环族烃类树脂类似的溶解度参数(SP值,该参数为用于表征化合物极性的指数),并表现出与氢化脂环族烃类树脂(如果使用的话)良好的相容性(即可混溶性),使得可形成透明膜。此外,聚异丁烯树脂具有低表面能,因此可使粘合剂能够铺展到粘附体上,并最大程度减少界面处的空隙生成。另外,聚异丁烯树脂的玻璃化转变温度和水分渗透性均较低,因此其适宜用作粘合剂封装组合物的基体树脂。
聚异丁烯树脂可具有理想的粘弹性,该粘弹性通常可用于赋予粘合剂封装组合物所需程度的流动性。可使用应变流变仪来确定各种温度下的弹性(储能)模量G’和粘性(损耗)模量G”。然后可用G’和G”来确定比率tan(δ)=G”/G’。一般来讲,tan(δ)值越高,材料就越类似粘滞材料,并且tan(δ)值越低,材料就越类似于弹性固体。在一些实施方案中,可选择聚异丁烯树脂,使得当粘合剂封装组合物在约70℃至约110℃的温度下时,该组合物于相对较低频率下具有至少约0.5的tan(δ)值。以此方式,组合物能够在不平的表面上充分流动,并只含有很少量的内部气泡或完全不含内部气泡。
本发明的阻隔性粘合剂组合物可任选地还包含增粘剂。一般来讲,增粘剂可为增强粘合剂封装组合物粘着性的任何化合物或化合物的混合物。理想的是增粘剂不会增强水分渗透性。增粘剂可包括氢化的烃类树脂、部分氢化的烃类树脂、非氢化的烃类树脂或它们的组合。优选地,增粘剂包括氢化石油树脂。在一些实施方案中,相对于组合物的总重量,粘合剂组合物包含约15重量%至约35重量%、约20重量%至约30重量%、或约25重量%的增粘剂。
增粘剂的示例包括但不限于氢化萜烯基树脂(例如,可以商品名CLEARON P、M和K(安原化工(Yasuhara Chemical))商购获得的树脂);氢化树脂或氢化酯基树脂(例如,可以商品名FORAL AX(赫尔克里士公司(Hercules Inc.));FORAL 105(赫尔克里士公司);PENCEL A(荒川化学工业株式会社(Arakawa Chemical Industries.Co.,Ltd.));ESTERGUMH(荒川化学工业株式会社);和SUPER ESTER A(荒川化学工业株式会社)商购获得的树脂);不成比例的树脂或不成比例的酯基树脂(例如,可以商品名PINECRYSTAL(荒川化学工业株式会社)商购获得的树脂);氢化的二环戊二烯基树脂,其为C5型石油树脂的氢化树脂,其中C5型石油树脂通过使石脑油热分解产生的C5级分,诸如戊烯、异戊二烯、胡椒碱和1,3-戊二烯共聚来获得(例如,可以商品名ESCOREZ5300和5400系列(埃克森美孚化学公司(ExxonChemical Co.))、EASTOTAC H(伊士曼化学公司(Eastman Chemical Co.))商购获得的树脂);部分氢化的芳族改性二环戊二烯基树脂(例如,可以商品名ESCOREZ 5600(埃克森美孚化学公司)商购获得的树脂);由C9-型石油树脂的氢化产生的树脂,其中C9-型石油树脂通过使石脑油热分解产生的C9级分,诸如茚、乙烯基甲苯和α-或β-甲基苯乙烯共聚来获得(例如,可以商品名ARCON P或ARCON M(荒川化学工业株式会社)商购获得的树脂);由上述C5级分和C9级分的共聚石油树脂的氢化产生的树脂(例如,可以商品名IMARV(出光兴产石油化学公司(Idemitsu Petrochemical Co.))商购获得的树脂)。
非氢化的烃类树脂包括C5、C9、C5/C9烃类树脂、聚萜烯树脂、芳族改性的聚萜烯树脂或松香衍生物。如果使用非氢化的烃类树脂,则通常将其与另一种氢化的或部分氢化的增粘剂组合使用。
在一些实施方案中,增粘剂包含氢化的烃类树脂,特别是氢化的脂环族烃类树脂。氢化的脂环族烃类树脂的具体示例包括ESCOREZ 5340(埃克森美孚化学公司)。在一些实施方案中,氢化的脂环族烃类树脂为氢化的二环戊二烯基树脂,这是因为该树脂具有较低的水分渗透性和透明度。可用于粘合剂封装组合物中的氢化脂环族烃类树脂的重均分子量通常为约200g/mol至5,000g/mol。在另一个实施方案中,氢化脂环族烃类树脂的重均分子量为约500g/mol至3,000g/mol。如果重均分子量超过5,000g/mol,则会导致增粘作用变差,或者与聚异丁烯树脂的相容性会降低。
增粘剂可具有软化温度或软化点(环球法软化温度),该软化温度可至少部分地根据组合物的粘合力、使用的温度、生产的容易性等而变化。环球法软化温度一般来讲可在约50℃至200℃。在一些实施方案中,环球法软化温度为约80℃至150℃。如果环球法软化温度小于80℃,则增粘剂会因在电子器件发光时产生的热而经历分离并液化。当有机电致发光器件直接用粘合剂封装组合物进行封装时,这会导致有机层(诸如发光层)劣化。另一方面,如果环球法软化点超过150℃,则添加的增粘剂的量是如此之低,以至于不会获得令人满意的相关特性的改善。
在一些实施方案中,增粘剂包含氢化的烃类树脂,特别是氢化的脂环族烃类树脂。氢化的脂环族烃类树脂的具体示例包括ESCOREZ 5300和ESCOREZ 5340(Exxon Chemical)。在一些实施方案中,氢化的脂环族烃类树脂为氢化的二环戊二烯基树脂,这是因为该树脂具有较低的水分渗透性和透明度。可用于粘合剂封装组合物中的氢化脂环族烃类树脂的重均分子量通常为约200g/mol至5,000g/mol。在另一个实施方案中,氢化的脂环族烃类树脂的重均分子量为约500g/mol至3,000g/mol。如果重均分子量超过5,000g/mol,则会导致增粘作用变差,或者与聚异丁烯树脂的相容性会降低。
本发明的阻隔性粘合剂组合物包含有机改性纳米粘土。纳米粘土通常是已经用有机改性剂处理过以便与树脂体系相容的可阳离子取代的矿物。在一些实施方案中,纳米粘土在其最长尺寸方面为约100nm至约1000nm。
合适的纳米粘土材料包括例如绿土、高岭土、伊利石、绿泥石、蛇纹石、绿坡缕石、坡缕石、蛭石、海绿石、海泡石和混合层粘土的地质类别中的那些。绿土例如可包括蒙脱石、膨润土、叶蜡石、锂蒙脱石、皂石、锌蒙脱石、绿脱石、滑石、贝得石和铬高岭石。高岭土例如可包括高岭石、地开石、珍珠陶土、叶蛇纹石、蠕陶土、多水高岭土、indellite和温石绒。伊利石,例如,包括漂云母、白云母、钠云母、金云母和黑云母。绿泥石例如可包括绿泥间蛭石、叶绿泥石(penninite)、片硅铝石、须藤石、叶绿泥石(pennine)和斜绿泥石。混合层粘土例如可包括钠板石和黑云母蛭石。这些层状粘土矿物的变体和同晶型取代物提供独特的应用。优选地,使用蒙脱石、膨润土或它们的组合。
用于粘土的合适的有机改性剂包括例如具有二甲基苄基氢化牛脂季铵离子、双(氢化牛脂)二甲基季铵离子、甲基牛脂双-2-羟乙基季铵离子、二甲基氢化牛脂2-乙基己基季铵离子或二甲基脱氢牛脂季铵离子的那些。
相对于组合物的总重量,阻隔性粘合剂组合物通常包含约1重量%至约10重量%、或约2重量%至约5重量%的有机改性纳米粘土。
本发明的阻隔性粘合剂组合物还包含吸附剂纳米粒子,诸如纳米级干燥剂和/或吸气剂,以吸附和/或吸收氧气和/或水分。
合适的干燥剂的示例包括脱水金属卤化物、盐、硅酸盐、氧化物、氢氧化物、卤化物、硫酸盐、高氯酸盐、碳酸盐和活性炭。具体的示例包括氯化钴、氯化钙、溴化钙、氯化锂、氯化锌、溴化锌、二氧化硅(硅胶)、氧化铝(活性氧化铝)、硫酸钙、硫酸铜、碳酸钾、碳酸镁、二氧化钛、膨润土、酸性粘土、蒙脱土、硅藻土(粘土矿物)二氧化硅氧化铝、沸石、二氧化硅、氧化锆、活性炭、五氧化二磷、硫酸镁和碱土金属氧化物如氧化钡、氧化钙、氧化铁和氧化镁。
合适的吸气剂的示例包括细分的金属,例如Al、Fe、Mg和Mn。
在一些实施方案中,氧化钙是优选的吸附剂材料。在一些实施方案中,吸附剂材料具有不大于约200nm、例如约1nm至约200nm的平均粒度。
相对于组合物的总重量,阻隔性粘合剂组合物通常包含约0.5重量%至约10重量%、或约1重量%至约5重量%的吸附剂纳米粒子。
在一些实施方案中,本发明的阻隔性粘合剂组合物为溶剂基粘合剂。可使用溶解树脂的任何可用溶剂。合适的溶剂的示例包括庚烷、甲苯、二甲苯、苯、乙苯和己烷(优选庚烷、甲苯或它们的组合)。在一些实施方案中,可优选溶剂具有低于约200℃的沸点。
在一些实施方案中,溶剂包含约40重量%至约95重量%、约65重量%至约95重量%、约70重量%至约90重量%、约75重量%至约85重量%、或约80重量%的总阻隔性粘合剂组合物。
本发明的阻隔性粘合剂组合物可通过对本领域的技术人员已知的各种方法来制备。例如,阻隔性粘合剂组合物可通过完全混合上述组分来制备。为了混合该组合物,可使用任意的搅拌器,诸如捏合机或挤出机。在一些实施方案中,该组合物可例如通过制备树脂体系与溶剂的混合物,将有机改性纳米粘土和吸附剂纳米粒子分散到溶剂中,然后将树脂混合物与纳米粒子分散体混合来制备。
本发明的阻隔性粘合剂组合物表现出良好的可见光透射率和低雾度。在一些实施方案中,该阻隔性粘合剂组合物具有约90%或更大的可见光透射率。在一些实施方案中,该阻隔性粘合剂组合物具有约3%或更小的雾度。
本发明的阻隔性粘合剂组合物通常为不可固化组合物或非反应性组合物。不可固化组合物是有利的因为它们不需要使用迁徙物质如抑制剂。它们还消除了对高温固化的需要,高温固化这会损坏下面的设备。该组合物可为例如,溶剂基干燥粘合剂、压敏粘合剂、接触粘合剂或热熔粘合剂。优选地,该组合物为在干燥时硬化的溶剂基干燥粘合剂。随着溶剂蒸发,粘度增加并且粘合剂组合物变硬。
本发明的阻隔性粘合剂组合物可通过任何可用的涂覆方法施加至衬底、器件或任何器件部件。溶剂基干燥粘合剂通常通过刷子、辊、小珠或带或喷雾施加。可将阻隔性粘合剂组合物涂覆到适当的衬底上以形成阻隔性粘合剂制品。
阻隔性粘合剂组合物可例如被涂覆到气体阻挡膜上并使其干燥以形成粘合性阻挡膜。气体阻挡膜具有对氧气的低渗透性,并且可用于帮助防止诸如食品、电子产品和药品的物品通过接触氧气而劣化。通常,食品级气体阻挡膜在20℃和65%相对湿度下具有小于约1cm3/m2/天的氧气透过率。优选地,气体阻挡膜还具有对水分的阻隔性质。
聚合物气体阻挡膜的示例包括乙烯乙烯醇共聚物(EVOH)膜,诸如聚乙烯EVOH膜和聚丙烯EVOH膜;聚酰胺膜,诸如共挤出的聚酰胺/聚乙烯膜、共挤出的聚丙烯/聚酰胺/聚丙烯膜;和聚乙烯膜,诸如低密度、中密度或高密度的聚乙烯膜和共挤出的聚乙烯/乙烯乙酸乙烯酯膜。聚合物气体阻挡膜还可被金属化,例如在聚合物膜上涂布诸如铝的金属薄层。
无机气体阻挡膜的示例包括包含氧化硅、氮化硅、氮氧化硅、氧化铝的膜、钻石样膜、钻石样玻璃和诸如铝箔的箔的膜。
优选地,气体阻挡膜是柔性的。对于一些应用,还优选的是,气体阻挡膜是透可见光的。如本文所用,术语“透可见光的”是指在光谱的可见部分(例如,在400nm至700nm之间)的平均透射率为至少约80%,优选至少约88%或90%。
对于一些应用,需要防止遭受水分和氧气。对于尤其敏感的应用,可能需要“超阻挡膜”。超阻挡膜在23℃和90%RH下通常具有小于约0.005cc/m2/天的氧气透过率并且在23℃和90%RH下具有小于约0.005g/m2/天的水蒸气透过率。
一些超阻挡膜为包括设置在聚合物层之间的无机透可见光层的多层膜。合适的超阻挡膜的一个示例包括设置在具有玻璃化转变温度(Tg)的聚合物之间的透可见光无机阻挡层,该玻璃化转变温度(Tg)大于或等于热稳定的聚对苯二甲酸乙二醇酯(HSPET)的玻璃化转变温度。
可采用具有的Tg大于或等于HSPET的Tg的多种聚合物。尤其优选形成适当高的Tg聚合物的易挥发性单体。优选第一聚合物层具有的Tg大于PMMA的Tg,更优选至少约110℃,还更优选至少约150℃,并且最优选至少约200℃的Tg。可用于形成第一层的特别优选的单体包括聚氨酯丙烯酸酯(例如,CN-968,Tg=约84℃,以及CN-983,Tg=约90℃,两者均可从沙多玛公司(Sartomer Co.)商购获得)、丙烯酸异冰片酯(例如,SR-506,可从沙多玛公司商购获得,Tg=约88℃)、二季戊四醇五丙烯酸酯(例如,SR-399,可从沙多玛公司商购获得,Tg=约90℃)、与苯乙烯共混的环氧丙烯酸酯(例如,CN-120S80,可从沙多玛公司商购获得,Tg=约95℃)、二-三羟甲基丙烷四丙烯酸酯(例如,SR-355,可从沙多玛公司商购获得,Tg=约98℃)、二乙二醇二丙烯酸酯(例如,SR-230,可从沙多玛公司商购获得,Tg=约100℃)、1,3-丁二醇二丙烯酸酯(例如,SR-212,可从沙多玛公司商购获得,Tg=约101℃)、五丙烯酸酯(例如,SR-9041,可从沙多玛公司商购获得,Tg=约102℃)、季戊四醇四丙烯酸酯(例如,SR-295,可从沙多玛公司商购获得,Tg=约103℃)、季戊四醇三丙烯酸酯(例如,SR-444,可从沙多玛公司商购获得,Tg=约103℃)、乙氧基化(3)三羟甲基丙烷三丙烯酸酯(例如,SR-454,可从沙多玛公司商购获得,Tg=约103℃)、乙氧基化(3)三羟甲基丙烷三丙烯酸酯(例如,SR-454HP,可从沙多玛公司商购获得,Tg=约103℃)、烷氧基化三官能丙烯酸酯(例如,SR-9008,可从沙多玛公司商购获得,Tg=约103℃)、二丙二醇二丙烯酸酯(例如,SR-508,可从沙多玛公司商购获得,Tg=约104℃)、新戊二醇二丙烯酸酯(例如,SR-247,可从沙多玛公司商购获得,Tg=约107℃)、乙氧基化(4)双酚a二甲基丙烯酸酯(例如,CD-450,可从沙多玛公司商购获得,Tg=约108℃)、环己烷二甲醇二丙烯酸酯(例如,CD-406,可从沙多玛公司商购获得,Tg=约110℃)、甲基丙烯酸异冰片酯(例如,SR-423,可从沙多玛公司商购获得,Tg=约110℃)、环状二丙烯酸酯(例如,SR-833,可从沙多玛公司商购获得,Tg=约186℃)和三(2-羟基乙基)异氰尿酸酯三丙烯酸酯(例如,SR-368,可从沙多玛公司商购获得,Tg=约272℃),前述甲基丙烯酸酯的丙烯酸酯以及前述丙烯酸酯的甲基丙烯酸酯。
第一聚合物层可通过如下形成:将一层单体或低聚物施加至衬底并且使该层交联以原位形成聚合物,例如,通过可辐射交联的单体的闪蒸和气相沉积,然后使用例如电子束装置、UV光源、放电装置或其它合适的装置来交联。可通过冷却载体来改善涂布效率。也可以使用常规的涂布方法诸如辊涂(例如,凹版辊涂布)或喷涂(例如,静电喷雾涂布)将单体或低聚物施加至衬底,然后如上文所述进行交联。第一聚合物层也可通过施加包含溶剂中的低聚物或聚合物的层以及干燥由此施加的层以移除溶剂来形成。如果提供在高温下具有玻璃态的聚合物层,其玻璃化转变温度大于或等于HSPET的玻璃化转变温度,也可采用等离子体聚合。最优选地,通过闪蒸和气相沉积随后通过原位交联来形成第一聚合物层,例如如以下文献中所述:美国专利No.4,696,719(Bischoff)、4,722,515(Ham)、4,842,893(Yializis等人)、4,954,371(Yializis)、5,018,048(Shaw等人)、5,032,461(Shaw等人)、5,097,800(Shaw等人)、5,125,138(Shaw等人)、5,440,446(Shaw等人)、5,547,908(Furuzawa等人)、6,045,864(Lyons等人)、6,231,939(Shaw等人)和6,214,422(Yializis);在公布的PCT专利申请No.WO 00/26973(Delta V技术公司);D.G.Shaw和M.G.Langlois,“一种用于涂布纸和聚合物幅材的新型气相沉积工艺”,第六次国际真空涂布会议(A New VaporDeposition Process for Coating Paper and Polymer Webs,6th InternationalVacuum Coating Conference)(1992年)中;D.G.Shaw和M.G.Langlois,“一种用于气相沉积丙烯酸酯薄膜的新型高速工艺:更新”,真空镀膜协会第36届年度技术会议录(1993年)(“ANew High Speed Process for Vapor Depositing Acrylate Thin Films:An Update”,Society of Vacuum Coaters 36th Annual Technical Conference Proceedings(1993))中;D.G.Shaw和M.G.Langlois,“气相沉积丙烯酸酯涂层用于改善金属化膜的阻隔性质的用途”,真空镀膜协会第37届年度技术会议录(1994年)(“Use of Vapor Deposited AcrylateCoatings to Improve the Barrier Properties of Metallized Film”,Society ofVacuum Coaters 37th Annual Technical Conference Proceedings(1994));D.G.Shaw、M.Roehrig、M.G.Langlois和C.Sheehan,“使用蒸发丙烯酸酯涂层来平整聚酯和聚丙烯膜衬底的表面”,RadTech(1996年)(“Use of Evaporated Acrylate Coatings to Smooth theSurface of Polyester and Polypropylene Film Substrates”,RadTech(1996))中所述;J.Affinito、P.Martin、M.Gross、C.Coronado和E.Greenwell,“光学应用中的真空沉积聚合物/金属多层膜”,《固体薄膜》,第270卷第43至48页(1995年)(“Vacuum depositedpolymer/metal multilayer films for optical application”,Thin Solid Films 270,4348(1995));以及J.D.Affinito、M.E.Gross、C.A.Coronado、G.L.Graff、E.N.Greenwell和P.M.Martin,“聚合物-氧化物透明阻挡层”,真空镀膜协会第39届年度技术会议录(1996年)(“Polymer-Oxide Transparent Barrier Layers”,Society of Vacuum Coaters 39thAnnual Technical Conference Proceedings(1996))。
优选地通过适当的预处理来提高每个聚合物层的光滑度和连续性以及其对下面层的粘附力。优选的预处理方式采用在存在合适的反应性或非反应性气氛(例如,等离子体、辉光放电、电晕放电、介质阻挡放电或大气压放电)的情况下放电;化学预处理或火焰预处理。这些预处理有助于使下面层的表面更加易于接受随后所施加的聚合物层的形成。等离子体预处理是特别优选的。也可在下面层顶上使用可具有与高Tg聚合物层不同组成的单独的粘附促进层以改善层间粘附力。粘附促进层可为例如单独的聚合物层或含金属层,诸如金属层、金属氧化物层、金属氮化物层、或金属氮氧化物层。粘附促进层可具有数纳米(例如1nm或2nm)至约50nm的厚度,并且如果需要可以更厚。
第一聚合物层所需的化学组成和厚度部分地取决于载体的性质和表面形貌。厚度优选地足以提供光滑、无缺陷的表面,随后可施加第一无机阻挡层至该表面。例如,第一聚合物层可具有数纳米(例如2nm或3nm)至约5μm的厚度,并且如果需要可更厚。
由具有的Tg大于或等于HSPET的Tg的聚合物层隔开的一个或多个透可见光无机阻挡层位于第一聚合物层的顶上。这些层可分别称为“第一无机阻挡层”、“第二无机阻挡层”和“第二聚合物层”。如果需要,附加的无机阻挡层和聚合物层也可以存在,包括不具有大于或等于HSPET的Tg的Tg的聚合物层。。然而,每个相邻的一对无机阻挡层优选只被具有的Tg大于或等于HSPET的Tg的一个或多个聚合物层隔开,并且更优选只被具有的Tg大于PMMA的Tg的一个或多个聚合物层隔开。
这些无机阻挡层无需相同。可采用多种无机阻隔性材料。优选的无机阻隔性材料包括金属氧化物、金属氮化物、金属碳化物、金属氮氧化物、金属硼氧化物以及它们的组合,例如,氧化硅诸如二氧化硅、氧化铝诸如矾土、氧化钛诸如二氧化钛、氧化铟、氧化锡、氧化铟锡(“ITO”)、氧化钽、氧化锆、氧化铌、碳化硼,碳化钨、碳化硅、氮化铝、氮化硅、氮化硼、氮氧化铝、氮氧化硅、氮氧化硼、硼氧化锆、硼氧化钛以及它们的组合。氧化铟锡、氧化硅、氧化铝以及它们的组合是特别优选的无机阻隔性材料。ITO为正确选择各元素成分的相对比例可变得导电的特定类别陶瓷材料的示例。无机阻挡层优选地使用膜金属化领域中所采用的诸如溅射(例如阴极或平面磁控溅射)、蒸镀(例如电阻式或电子束蒸镀)、化学气相沉积、原子层沉积、电镀等技术形成。最优选使用溅射,例如,反应性溅射来形成无机阻挡层。当无机层通过相比于较低能量技术诸如常规化学气相沉积工艺而言的高能量沉积技术诸如溅射而形成时,已经观察到增强的阻隔性质。可以通过预处理(例如,等离子体预处理)诸如以上参照第一聚合物层所描述的方法来提高各无机阻挡层的光滑度和连续性以及其对下面层的粘附力。
这些无机阻挡层无需具有相同的厚度。各无机阻挡层所需的化学组成和厚度将部分地取决于下面层的性质和表面形貌以及阻挡组件所需的光学性质。无机阻挡层优选地足够厚以便是连续的,并且足够薄以便保证阻挡组件和包含组件的制品将具有所需程度的可见光透射性和柔韧性。各无机阻挡层优选的物理厚度(相对于光学厚度)为约3nm至约150nm,更优选地为约4nm至约75nm。
隔开第一、第二以及任何附加无机阻挡层的第二聚合物层无需相同,也无需具有相同的厚度。可以采用多种第二聚合物层材料。优选的第二聚合物层材料包括上面提到的关于第一聚合物层的材料。优选的一个或多个第二聚合物层通过上面关于第一聚合物层描述的闪蒸和气相沉积随后通过原位交联来施加。诸如上述那些的预处理(例如,等离子预处理)也优选地在第二聚合物层形成之前采用。一个或多个第二聚合物层所需的化学组成和厚度部分地取决于一个或多个下面层的性质和表面形貌。第二聚合物层的厚度优选地足以提供光滑、无缺陷的表面并且随后无机阻挡层可施加至该表面。通常一个或多个第二聚合物层可具有比第一聚合物层更小的厚度。例如,每个第二聚合物层可具有约5nm至约10μm的厚度,如果需要可更厚。
柔性透可见光超阻挡膜及其制造描述于例如美国专利No.7,940,004(Padiyath等人)中,该专利以引用方式并入本文。
可商购获得的超阻挡膜包括例如购自3M公司的FTB 3-50和FTB 3-125。
涂覆有本发明的粘合剂阻隔性组合物的层的气体阻挡膜可设置在衬底上。衬底优选为柔性的和透可见光的。合适的衬底材料包括有机聚合物材料,诸如聚对苯二甲酸乙二醇酯(PET)、聚丙烯酸酯、聚碳酸酯、有机硅、环氧树脂、有机硅官能化的环氧树脂、聚酯(诸如由杜邦公司(E.I.du Pont de Nemours&Co.)制备的Mylar)、聚酰亚胺(诸如由杜邦公司(du Pont)制备的Kapton H或Kapton E、由钟渊化学工业公司(Kanegafugi ChemicalIndustry Company)制备的Apical AV、由UBE工业公司(UBE Industries,Ltd.)制备的Upilex)、聚醚砜(PES,由住友公司(Sumitomo)制备)、聚醚酰亚胺、聚萘二甲酸乙二醇酯(PEN)、聚甲基丙烯酸甲酯、苯乙烯/丙烯腈、苯乙烯/马来酸酐、聚甲醛、聚乙烯基萘、聚醚醚酮、聚芳醚酮、高Tg含氟聚合物(例如,六氟丙烯、四氟乙烯和乙烯的DYNEONTMHTE三元共聚物)、聚α-甲基苯乙烯、聚芳酯、聚砜、聚苯醚、聚酰胺酰亚胺、聚酰亚胺、聚邻苯二甲酰胺、聚乙烯和聚丙烯。也可利用无色的聚酰亚胺、环烯烃共聚物和环烯烃共聚物。优选地该衬底包含PET。
图1示出了包括衬底110、气体阻挡膜120(优选超阻挡膜)和阻隔性粘合剂层130的示例性阻挡膜构造100的横截面结构。在一些实施方案中,阻隔性粘合剂层具有约5μm至约50μm的厚度。在一些实施方案中,阻挡膜构造具有约20μm至约250μm的厚度。
在一些实施方案中,阻隔性粘合剂层的外表面可用诸如防粘衬垫(140)的装置来保护。可使用任何可用的防粘衬垫,诸如例如用剥离剂(例如有机硅树脂)处理的膜材或片材。最终使用者可移除防粘衬垫,以将阻挡构造粘附到它将保护的器件。
另选地,本发明的阻隔性粘合剂可设置在两个防粘衬垫之间而提供给最终使用者。
本发明的阻挡膜构造可用于防止OLED显示器和固态照明、太阳能电池、电泳和电致变色显示器、薄膜电池、量子点器件、传感器(例如,触摸传感器)和其它有机电子器件遭受氧气和水分。它们特别适合于需要氧气和水分保护以及柔韧性和良好的光学透射率的应用。
图2示出了用于封装有机电子器件(诸如OLED)的本发明的阻挡膜构造。有机电子器件250设置在器件衬底260上。有机电子器件250用阻挡膜构造200和器件衬底260封装,阻挡膜构造200包括超阻挡膜220、阻隔性粘合剂层230和衬底210。
实施例
下面的实施例对本发明的目的和有益效果作出更进一步的解释,但这些实施例中列举的具体材料和用量以及其它条件和细节不应解释为是对本发明不当的限制。除非另外指明,否则下述实例中提及的所有份数、百分比和比率均按重量计。除非另外指明,试剂购自密苏里州圣路易斯的西格玛奥德里奇化工公司(Sigma Aldrich Company,St.Louis,MO)。
表1:材料和来源。
光学性质特征
利用BYK Gardner Haze-Gard Plus(马里兰州哥伦比亚市的毕克-加特纳(美国)公司(BYK-Gardner USA,Inc.,Columbia,MD))获得透射率、清晰度和雾度数据。
水分阻隔性测试
通过将阻挡组件层合到沉积有元素钙的玻璃以产生试样,测试了阻挡组件防止水分或水蒸气运输的能力。然后将这些试样暴露于升高的温度和湿度,并且测量由于元素钙与水的反应而造成的光密度损耗。首先在80℃下真空烘烤每个阻挡组件以确保去除任何残余水分。将钙(反射金属)作为正方形的阵列热沉积在玻璃板的指定区域上。将每个阻挡组件设置在玻璃板上的四个钙正方形(称为像素)上,并且将该组件层合以提供试样。使用Epson v750专业人员来扫描试样且使用Aphelion图像分析软件来分析扫描,测量每个刚制成的试样的每个钙像素的光密度。然后将每个试样放置在60℃和90%相对湿度的环境室中,使其加速老化。在前三天里,每天测量光密度两次。然后每天测量光密度一次,直到光密度变为初始密度的50%为止。水蒸气透过率(WVTR)与钙像素的光密度达到其初始值50%所需的时间成反比。该关系通过以下等式描述:
其中dCa是钙层的厚度;
ρCa是钙的密度;
ti是时间;
是水的摩尔数;
nCa是钙的摩尔数;
是水的分子量;以及,
MWCa是钙的分子量。
制备例1:聚异丁烯基粘合剂混合物
将大块Oppanol B80和Oppanol B50SF聚异丁烯聚合物树脂切成大约1英寸(2.5cm)的立方体。然后将所称量的这些树脂立方体在加盖的玻璃广口瓶中与Escorez5300增粘剂混合在甲苯中。粘合剂混合物的重量比为足量甲苯中的两份Oppanol B80、一份Oppanol B50SF和一份Escorez 5300以提供25重量%的溶液。使用辊式搅拌器将所得制剂混合2周,直至溶液均匀。
制备例2-4:纳米粒子分散体
纳米粒子为氧化钙纳米粉末(CaO)和Claytone APA(“粘土”),其以表2中提供的重量比加入甲苯中。将纳米粒子以5重量%固体直接加入甲苯中,然后使用Sonics VibraCell VCX750超声仪(康涅狄格州纽敦的超音速及材料有限公司(Sonics&Materials Inc.,Newtown,CT))在18%-20%振幅下分散20分钟。
表2:用于该工作的分散体中纳米粒子的比率。
制备例5-9:纳米粒子填充的粘合剂制剂
将制备例2-4的纳米粒子分散体与制备例1的聚异丁烯基聚合物溶液以表3中提供的重量比混合。使用辊式搅拌器将所得制剂混合一周。用甲苯稀释所得溶液以达到最终固体含量为20重量%固体。
表3:纳米粒子填充的聚异丁烯基粘合剂制剂的组成。
为制备粘合剂膜,使用台式凹口棒涂布机将制备例5-9的纳米粒子填充的粘合剂制剂施加至SKC-12N防粘衬垫。将涂覆的防粘衬垫放置于80℃下烘箱中20分钟以去除溶剂,从而提供具有12微米的厚度的粘合剂膜。之后,将M74F或SKC-02N防粘衬垫层合到粘合剂,使得粘合剂被夹在两个防粘衬垫之间。随后通过去除M74F或SKC-02N防粘衬垫并将粘合剂层合到超阻挡膜的阻挡层侧以提供阻挡组件,将粘合剂转移至3M FTB3-50超阻挡膜。在表4中提供了用于制备被测试的阻挡组件中的粘合剂的组合物。包含聚异丁烯但不包含纳米粒子的粘合剂在表中被称为PIB。
表4:粘合剂组合物。
试样的加速老化制备用于加速老化测试的试样并且如图3-5中所示的和在水分阻隔性测试中先前描述进行测试(其中470、570是玻璃衬底并且480、580是钙)。试样的加速老化测试结果汇总于表5和图6中。如表5中所示,与未填充的粘合剂(比较例1)相比,对于包含两种纳米粒子类型中任一种的试样(比较例2-5)达到50%光密度损耗的时间更长。与包含单独10重量%粘土或单独1重量%CaO的比较例相比,包含组合的5重量%的粘土和1重量%CaO的实施例显示达到50%光密度损耗的时间增加。在300小时加速老化之后分化变得明显。
表5比较例1-5和实施例的达到50%光密度损耗的时间。
本文所引述的专利公开的全部公开内容以引用方式全文并入本文,如同每种专利公开单独并入本文。在不脱离本发明范围和实质的前提下,对本发明的各种变型和更改对本领域的技术人员而言将显而易见。应当理解,本发明并非意图不当地限制于本文所示出的示例性实施方案和实施例,并且上述实施例和实施方案仅以举例的方式提出,而且本发明的范围旨在仅受下面本文所示出的权利要求书的限制。
Claims (29)
1.一种阻隔性粘合剂组合物,其包含:
(a)聚异丁烯树脂;
(b)有机改性纳米粘土;和
(c)吸附剂纳米粒子。
2.根据权利要求1所述的阻隔性粘合剂组合物,其中所述纳米粘土为膨润土纳米粘土或蒙脱石纳米粘土。
3.根据权利要求1或2所述的阻隔性粘合剂组合物,其中所述纳米粘土的最长尺寸为约100nm至约1000nm。
4.根据上述权利要求中任一项所述的阻隔性粘合剂组合物,其中所述纳米粘土是经过季铵离子的改性的。
5.根据上述权利要求中任一项所述的阻隔性粘合剂组合物,其中所述吸附剂纳米粒子包含金属氧化物。
6.根据权利要求5所述的阻隔性粘合剂组合物,其中所述吸附剂纳米粒子包含氧化钙。
7.根据权利要求6所述的阻隔性粘合剂组合物,其中所述氧化钙具有不大于约200nm的平均粒度。
8.根据上述权利要求中任一项所述的阻隔性粘合剂组合物,其中所述树脂体系包含具有约40,000g/mol至约2,600,000g/mol的粘均分子量的第一聚异丁烯树脂。
9.根据权利要求8所述的阻隔性粘合剂组合物,其中所述树脂体系包含具有约300,000g/mol至约900,000g/mol的粘均分子量的第一聚异丁烯树脂。
10.根据上述权利要求中任一项所述的阻隔性粘合剂组合物,相对于所述组合物的总重量,所述阻隔性粘合剂组合物包含约1重量%至约10重量%的所述有机改性纳米粘土。
11.根据权利要求10所述的阻隔性粘合剂组合物,相对于所述组合物的总重量,所述阻隔性粘合剂组合物包含约2重量%至约5重量%的所述有机改性纳米粘土。
12.根据上述权利要求中任一项所述的阻隔性粘合剂组合物,相对于所述组合物的总重量,所述阻隔性粘合剂组合物包含约0.5重量%至约10重量%的所述吸附剂纳米粒子。
13.根据权利要求12所述的阻隔性粘合剂组合物,相对于所述组合物的总重量,所述阻隔性粘合剂组合物包含约1重量%至约5重量%的所述吸附剂纳米粒子。
14.根据上述权利要求中任一项所述的阻隔性粘合剂组合物,所述阻隔性粘合剂组合物还包含溶剂。
15.根据上述权利要求中任一项所述的阻隔性粘合剂组合物,所述阻隔性粘合剂组合物还包含紫外阻断剂。
16.根据上述权利要求中任一项所述的阻隔性粘合剂组合物,所述阻隔性粘合剂组合物还包含增粘剂。
17.根据上述权利要求中任一项所述的阻隔性粘合剂组合物,其中所述聚异丁烯树脂包含异丁烯共聚物。
18.根据权利要求17所述的阻隔性粘合剂组合物,其中所述聚异丁烯树脂包含丁基橡胶。
19.一种阻隔性粘合剂组合物,其包含:
(a)约50重量%至约75重量%的聚异丁烯树脂,所述聚异丁烯树脂具有约300,000g/mol至约900,000g/mol的粘均分子量,
(b)约1重量%至约10重量%的有机改性纳米粘土,
(c)约1重量%至约5重量%的氧化钙纳米粒子,以及
(d)约10重量%至约25重量%的增粘剂,
以上含量全部相对于所述组合物的总重量。
20.一种粘合性阻挡膜,其包括设置在气体阻挡膜上的根据上述权利要求中任一项所述的阻隔性粘合剂组合物的层。
21.根据权利要求20所述的粘合性阻挡膜,其中所述气体阻挡膜为在23℃和90%RH下具有小于约0.005cc/m2/天的氧气透过率并且在23℃和90%RH下具有小于约0.005g/m2/天的水蒸气透过率的超阻挡膜。
22.根据权利要求21所述的粘合性阻挡膜,其中所述超阻挡膜为包括设置在聚合物层之间的无机透可见光层的多层膜。
23.根据权利要求20至22中任一项所述的粘合性阻挡膜,其还包括设置在所述气体阻挡膜上且与所述阻隔性粘合剂组合物的层相背对的衬底。
24.根据权利要求23所述的粘合性阻挡膜,其中所述衬底包含聚对苯二甲酸乙二醇酯。
25.根据权利要求20至24中任一项所述的粘合性阻挡膜,其还包括设置在所述阻隔性粘合剂组合物的层上且与所述气体阻挡膜相背对的防粘层。
26.一种封装的有机电子器件,其包含封装薄膜器件的根据权利要求1至19中任一项所述的阻隔性粘合剂组合物。
27.根据权利要求26所述的封装的有机电子器件,其中所述器件为OLED。
28.一种封装的触摸传感器,其包含封装触摸传感器的根据权利要求1至19中任一项所述的阻隔性粘合剂组合物。
29.一种阻隔性粘合剂制品,其包括设置在防粘层之间的根据权利要求1至19中任一项所述的阻隔性粘合剂组合物的层。
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