CN105917265B - 具有双相电极层的电光显示器 - Google Patents

具有双相电极层的电光显示器 Download PDF

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CN105917265B
CN105917265B CN201580004604.6A CN201580004604A CN105917265B CN 105917265 B CN105917265 B CN 105917265B CN 201580004604 A CN201580004604 A CN 201580004604A CN 105917265 B CN105917265 B CN 105917265B
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optic displays
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CN105917265A (zh
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R·J·小保利尼
S·特尔佛
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E Ink Corp
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    • G—PHYSICS
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    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
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    • G09G3/34—Control arrangements or circuits, of interest only in connection with visual indicators other than cathode-ray tubes for presentation of an assembly of a number of characters, e.g. a page, by composing the assembly by combination of individual elements arranged in a matrix no fixed position being assigned to or needed to be assigned to the individual characters or partial characters by control of light from an independent source
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Abstract

一种电光显示器，包含双相透光导电层，该导电层包括由高导电基体制成的第一相和由具有受控体积电阻率的聚合物材料成分制成的第二相。第一相的基体可以由碳纳米管、银纳米线、涂布金属的开放泡沫结构、或印刷丝网形成。第二相的聚合物材料成分可以是导电聚合物、或聚合物和诸如盐、聚电解质、聚合物电解质、或固体电解质、或它们的组合的添加物。

Description

具有双相电极层的电光显示器
相关申请的引用
本申请涉及：
(a)于2004年3月26日提交的美国专利No.7,012,735；
(b)于2006年12月20日提交的美国专利No.7,349,148，其是于2004年11月5日提交的美国专利No.7,173,752的分案；
(c)于2011年4月4日提交的美国专利No.8,446,664；以及
(b)共同未决的美国专利公布No.2009/0122389A1。
技术领域
本发明涉及电光显示器，以及更具体地，涉及包含双相透光导电层的电光组件，该双相透光导电层包括由高导电基体制成的第一相和由具有受控体积电阻率的聚合物材料成分制成的第二相。在另一方面，本发明提供双相电极层，其中，第二相的聚合物材料成分由导电聚合物制成。在另一方面，本发明提供双相电极层，其中，第二相的聚合物材料成分由聚合物和添加物制成。此处所公开的聚合物材料成分可以用于除电光显示器以外的应用。
背景技术
电光显示器包括一层电光材料，在这里使用的该术语在本领域中的传统意思是指具有在至少一个光学性质方面不同的第一和第二显示状态的材料，通过将电场施加至该材料，该材料从第一显示状态改变成第二显示状态。光学性质通常是人眼可感知的颜色，但是可以是另一光学性质，诸如光学透射、反射率、发光、或在意于用于机器阅读的情况下，从可见范围外的电磁波长的反射率的改变的意义上来说的伪色。
已知几种类型的电光显示器。一种类型的电光显示器是旋转双色构件类型，如例如在美国专利No.5,808,783；5,777,782；5,760,761；6,054,071；6,055,091；6,097,531；6,128,124；6,137,467；和6,147,791中所述(尽管该类型的显示器通常被称为“旋转双色球”显示器，但术语“旋转双色构件”是优选的，其更准确，因为在以上提到的一些专利中，旋转构件不是球形的)。这样的显示器使用大量的小主体(通常是球形或圆柱形的)，其包括具有不同光学特性的两个或更多个分段以及内部偶极子。这些主体悬浮在基体内的填充液体的液泡内，液泡被填充有液体以使得主体自由旋转。通过将电场施加至显示器，由此将主体旋转至各个位置，并且改变通过观察表面看到的主体的哪个分段，来改变显示器的外观。这种类型的电光介质通常是双稳态的。
另一类型的电光显示器使用电致变色介质，例如纳米变色薄膜形式的电致变色介质，其包括至少部分由半导体金属氧化物形成的电极和附着到电极的能够进行可逆性颜色改变的多个染料分子；参见例如O'Regan,B.等,Nature 1991,353,737；以及Wood,D.,Information Display,18(3),24(2002年3月)。也参见Bach,U.等,Adv.Mater.,2002,14(11),845。这种类型的纳米变色薄膜还例如在美国专利No.6,301,038；6,870,657；和6,950,220中描述。这种类型的介质通常也是双稳态的。
另一类型的电光显示器是电润湿显示器，其由Philips开发并在Hayes,R.A.等,"Video-Speed Electronic Paper Based on Electrowetting",Nature,425,383-385(2003)中描述。其在美国专利No.7,420,549中示出这种电润湿显示器可以被制造成双稳态的。
已经在许多年被作为密集研发的主题的一种类型的电光显示器是基于粒子的电泳显示器，其中，多个带电粒子在电场的影响下移动穿过流体。电泳显示器与液晶显示器相比，可以具有以下属性：良好的亮度和对比度、宽的视角、状态双稳定性、以及低功耗。然而，这些显示器的长期图像质量的问题阻止了它们的广泛使用。例如，组成电泳显示器的粒子易于沉降，导致这些显示器的使用寿命不足。
如上所述，电泳介质需要流体的存在。在大多数现有技术的电泳介质中，该流体是液态的，但电泳介质可以使用气态流体来产生；参见例如Kitamura,T.等,"Electricaltoner movement for electronic paper-like display",IDW Japan,2001,Paper HCSl-1,以及Yamaguchi,Y.等,"Toner display using insulative particles chargedtriboelectrically",IDW Japan,2001,Paper AMD4-4。还参见美国专利No.7,321,459和7,236,291。这种基于气体的电泳介质当在允许粒子沉降的方向(例如在其中介质被布置在垂直平面中的招牌中)上使用时，表现为会经历与基于液体的电泳介质相同类型的由于粒子沉降产生的问题。实际上，与在基于液体的电泳介质中相比，粒子沉降在基于气体的电泳介质中表现为更严重的问题，这是由于气态悬浮流体的粘度与液态悬浮流体相比较低，其允许电泳粒子的更快沉降。
授予麻省理工学院(MIT)和伊英克公司或以麻省理工学院(MIT)和伊英克公司的名义的许多专利和申请描述了在封装电泳和其他电光介质中使用的各种技术。这种封装介质包括许多小囊体，每个囊体本身包括含有在流体介质中的可电泳移动的粒子的内部相，以及围绕所述内部相的囊壁。通常，囊体本身保持在聚合粘合剂内以形成位于两个电极之间的连贯层。在这些专利和申请中描述的技术包括：
(a)电泳粒子、流体和流体添加物；参见例如美国专利No.7,002,728和7,679,814；
(b)囊体、粘合剂和封装工艺；参见例如美国专利No.5,930,026；6,067,185；6,130,774；6,172,798；6,249,271；6,327,072；6,392,785；6,392,786；6,459,418；6,839,158；6,866,760；6,922,276；6,958,848；6,987,603；7,061,663；7,071,913；7,079,305；7,109,968；7,110,164；7,202,991；7,242,513；7,304,634；7,339,715；7,391,555；7,411,719；7,477,444；7,561,324；7,848,007；7,910,175；7,952,790；8,035,886；和8,129,655；以及美国专利申请公布No.2005/0156340；2007/0091417；2008/0130092；2009/0122389；2010/0044894；2011/0286080；和2011/0286081；
(c)含有电光材料的薄膜和子组件；参见例如美国专利No.6,825,829；6,982,178；7,236,292；7,443,571；7,513,813；7,561,324；7,636,191；7,649,666；7,728,811；7,729,039；7,791,782；7,839,564；7,843,621；7,843,624；8,034,209；8,068,272；8,077,381和8,177,942；以及美国专利申请公布No.2008/0309350；2009/0034057；2009/0109519；2009/0168067；2011/0032595；2011/0032396；2011/0075248；2011/0164301和2012/0176664；
(d)在显示器中使用的背板、粘合剂层和其他辅助层以及方法；参见例如美国专利No.7,116,318和7,535,624；
(e)颜色形成和颜色调整；参见例如美国专利No.7,075,502和美国专利申请公开No.2007/0109219；
(f)用于驱动显示器的方法；参见例如美国专利No.7,012,600和7,453,445；
(g)显示器的应用；参见例如美国专利No.7,312,784和8,009,348；以及
(h)非电泳显示器，如在美国专利No.6,241,921；6,950,220；7,420,549和8,319,759；以及美国专利申请公布No.2012/0293858中描述。
授予麻省理工学院(MIT)和伊英克公司或以麻省理工学院(MIT)和伊英克公司的名义的许多专利和申请近来被公布，其描述了封装的电泳介质。这种封装介质包括许多小囊体，每个囊体本身包括含有悬浮在液体悬浮介质中的可电泳移动的粒子的内部相，以及围绕所述内部相的囊壁。通常，囊体本身保持在聚合粘合剂内以形成位于两个电极之间的连贯层。这种类型的封装介质例如在以下描述：美国专利Nos.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；6,130,774；6,172,798；6,177,921；6,232,950；6,249,271；6,252,564；6,262,706；6,262,833；6,300,932；6,312,304；6,312,971；6,323,989；6,327,072；6,376,828；6,377,387；6,392,785；6,392,786；6,413,790；6,422,687；6,445,374；6,445,489；6,459,418；6,473,072；6,480,182；6,498,114；6,504,524；6,506,438；6,512,354；6,515,649；6,518,949；6,521,489；6,531,997；6,535,197；6,538,801；6,545,291；6,580,545；6,639,578；6,652,075；6,657,772；6,664,944；6,680,725；6,683,333；6,693,620；6,704,133；6,710,540；6,721,083；6,724,519；6,727,881；6,738,050；6,750,473；6,753,999；6,816,147；6,819,471；6,822,782；6,825,068；6,825,829；6,825,970；6,831,769；6,839,158；6,842,167；6,842,279；6,842,657；6,864,875；6,865,010；6,866,760；6,870,661；6,900,851；6,922,276；6,950,220；6,958,848；6,967,640；6,980,196；6,982,178；6,987,603；6,995,550；7,002,728；7,012,600；7,012,735；7,023,420；7,030,412；7,030,854；7,034,783；7,038,655；7,061,663；7,071,913；7,075,502；7,075,703；7,079,305；7,106,296；7,109,968；7,110,163；7,110,164；7,116,318；7,116,466；7,119,759；7,119,772；7,148,128；7,167,155；7,170,670；7,173,752；7,176,880；7,180,649；7,190,008；7,193,625；7,202,847；7,202,991；7,206,119；7,223,672；7,230,750；7,230,751；7,236,290；7,236,292；7,242,513；7,247,379；7,256,766；7,259,744；7,280,094；7,304,634；7,304,787；7,312,784；7,312,794；7,312,916；7,327,511；7,339,715；7,349,148；7,352,353；7,365,394；和7,365,733；以及美国专利申请公布Nos.2002/0060321；2002/0090980；2003/0102858；2003/0151702；2003/0222315；2004/0105036；2004/0112750；2004/0119681；2004/0155857；2004/0180476；2004/0190114；2004/0257635；2004/0263947；2005/0000813；2005/0007336；2005/0012980；2005/0018273；2005/0024353；2005/0062714；2005/0099672；2005/0122284；2005/0122306；2005/0122563；2005/0134554；2005/0151709；2005/0152018；2005/0156340；2005/0179642；2005/0190137；2005/0212747；2005/0253777；2005/0280626；2006/0007527；2006/0038772；2006/0139308；2006/0139310；2006/0139311；2006/0176267；2006/0181492；2006/0181504；2006/0194619；2006/0197737；2006/0197738；2006/0202949；2006/0223282；2006/0232531；2006/0245038；2006/0262060；2006/0279527；2006/0291034；2007/0035532；2007/0035808；2007/0052757；2007/0057908；2007/0069247；2007/0085818；2007/0091417；2007/0091418；2007/0109219；2007/0128352；2007/0146310；2007/0152956；2007/0153361；2007/0200795；2007/0200874；2007/0201124；2007/0207560；2007/0211002；2007/0211331；2007/0223079；2007/0247697；2007/0285385；2007/0286975；2007/0286975；2008/0013155；2008/0013156；2008/0023332；2008/0024429；2008/0024482；2008/0030832；2008/0043318；2008/0048969；2008/0048970；2008/0054879；2008/0057252；和2008/0074730；以及国际申请公布Nos.WO 00/38000；WO 00/36560；WO 00/67110；和WO 01/07961；以及欧洲专利Nos.1,099,207B1；和1,145,072B1。
上述专利和申请中的许多认识到在封装的电泳介质中包围离散的微囊体的壁可以被连续相替代，因此产生所谓的聚合物分散型电泳显示器，其中电泳介质包括电泳流体的多个离散微滴和聚合物材料的连续相，并且在这种聚合物分散型电泳显示器内的电泳流体的离散微滴可以被认为是囊体或者微囊体，即使没有与每个单独微滴相关联的离散囊体薄膜；参见例如上述美国专利No.6,866,760。因此，为了本申请的目的，这样的聚合物分散型电泳介质被认定为是封装的电泳介质的子类。
一种相关类型的电泳显示器是所谓的“微单元电泳显示器”。在微单元电泳显示器中，带电粒子和流体未封装在微囊体内，而是保持在形成于载体介质(通常是聚合物薄膜)内的多个空腔内。参见例如都授予Sipix Imaging公司的美国专利No.6,672,921和6,788,449。在下文中，术语“微腔电泳显示器”可以用于覆盖封装电泳显示器和微单元电泳显示器。
于2003年5月22日提交的美国专利No.6,982,178描述了用于电光显示器中的“前平面层压板”(FPL)，其依次包括透光导电层或电极层、与导电层电接触的固态电光介质层、粘合剂层、以及释放片。
大多数电光显示器需要透光导电层来用作显示器的一个电极，观察者可以通过该透光导电层来观察电光介质的光学状态的改变。在一些情况中，例如可变的透射窗口，两个电极都必须是透光的。传统地，透光导电层在诸如聚合物薄膜或玻璃板的某种类型的机械支撑件上由铟锡氧化物(ITO)形成。最近，由诸如碳纳米管和银线的薄金属网状材料制成的薄膜替代ITO薄膜作为透光导电层。这种薄膜包括由明显较小的导电率的区域围绕的高导电率的区域，其可能累积电荷并干扰电光显示器的性能。因此，需要不遭受这些缺点的基于金属网的电极层。
发明内容
本发明提供一种电光显示器，其包括双相电极层，其中，第一相由高导电基体制成，以及第二相由具有受控体积电阻率的聚合物材料成分制成。在本发明的一种形式中，第二相的聚合物材料可以是固有地导电的或者可以是与添加物混合的聚合物，以使得聚合物材料具有不大于1x1012Ohm-cm的电阻率。聚合物可以从例如聚氨酯、醋酸乙烯、乙烯-醋酸乙烯、环氧树脂、或聚丙烯酸、或它们的组合中选择。
在另一形式中，本发明提供双相电极层，其中第二相是离子导电聚合物，其中，一个离子可以迁移通过聚合物材料，而另一离子不能，例如聚合物羧酸盐的离子盐。
在本发明的另一形式中，第二相的聚合物材料可以包含从PEDOT-PSS、聚乙炔、聚苯硫醚、聚苯撑乙烯、和它们的组合中选择的一种或多种导电聚合物。
在本发明的另一形式中，第二相中的添加物可以从例如盐、聚电解质、聚合物电解质、固体电解质、或它们的组合中选择。
在一种形式中，聚合物材料中的添加物是盐；例如，无机盐、有机盐或它们的组合。在一个特定实施例中，盐包括乙酸钾。在可替换形式中，盐可以包括季铵盐，例如四烷基铵盐，诸如四丁基氯化铵或六氟磷酸盐。在另一形式中，添加物可以是具有包含至少三个氟原子的阴离子的盐；例如，添加物可以具有六氟磷酸盐阴离子，诸如1-丁基-3-甲基咪唑六氟磷酸盐。
在本发明的另一形式中，第二相中的添加物是聚电解质，并且可以包括多酸的盐，诸如但不限于聚丙烯酸的碱金属盐。
在本发明的另一形式中，第二相的聚合物材料中的添加物可以从非反应性溶剂、导电有机化合物和它们的组合中选择。
在本发明的另一形式中，第二相中的添加物可以是低数值平均分子量的包含羟基的聚合物，诸如聚(乙二醇)(PEG)，其中，质子而非电子移动。
包含添加物的聚合物材料可以提供有不同颜色的区域并用作颜色滤光器。可替换地，聚合物材料可以包括光学偏置元素。
在一个方面中，提供一种电光组件，包括第一和第二基板，以及粘合剂层和设置在第一和第二基板之间的电光材料层。在电光组件中，第一和第二基板中的至少一个可以包括双相电极层，其中，第一相是高导电基体，以及第二相是具有受控电阻率的聚合物材料，第二基板可以包括释放片，以及电光介质可以是固体电光介质；由此，整个电光组件具有前述美国专利No.6,982,178中描述的前平面层压板的形式。
在本发明的另一方面中，提供一种电光组件，包括第一和第二基板，粘合剂层以及设置在第一和第二基板之间的电光材料层、以及双相电极层，其中，第一相是高导电基体，以及第二相是具有受控电阻率的聚合物材料。
具体实施方式
因此，本发明提供一种电光显示器，其包括双相透光导电层，该双相透光导电层包含由高导电基体制成的第一相和由具有受控体积电阻率的聚合物材料成分制成的第二相。电光显示器通常包括电光材料层和设置在电光材料的相对侧上的至少两个其他层，这些中的至少一个是透光导电层。术语“透光”在这里使用来意味着由此指定的层透射足够的光以使得观察者在看向该层时观察到电光介质的显示状态的变化，其通常通过导电层和相邻的基板(如果存在)来观察。
第一相可以是导电基体。术语“导电基体”在此使用来描述电极层的高导电区域的第一相阵列。基体可以由碳纳米管、银纳米线、涂布金属的开放泡沫结构、印刷丝网、或不完全覆盖观察表面的任何这种材料来构造。第一相可以是透光的或光吸收的，直径尺寸的范围从几纳米至几毫米。基体可以规则地(即，网格状、六角形地、网状地等)或不规则地(即，随机地)布置。基体可以被布置得非常薄或者稀疏地填充，以使得电极层是透光的。
第二相可以由本质上导电的聚合物或混合有导电添加物的聚合物制成。第二相尽管与第一相相比导电性显著较小，但具有导电性质(即，不多于1×1012Ohm-cm的电阻率)。优选地，第二相具有大约1x107至1x1012Ohm-cm的电阻率。第二相可以是离子地或电子地导电的。通常，第二相围绕或涂布第一相以创建围绕导电基体的不太导电的区域。这为第一相提供了机械完整性和保护，该第一相由于其结构可能是易碎的。如果第一相是光吸收的，并且第二相是透光的，则不太导电区域与高导电区域的高比率是期望的。更优选地，第一相构成小于10％的观察区域，而第二相构成剩余的观察区域。
聚合物材料可以是满足最终使用应用的特殊需要的任何聚合物材料。合适的聚合物材料的例子包括聚氨酯、醋酸乙烯、乙烯-醋酸乙烯、环氧树脂、基于聚丙烯酸的粘合剂、或它们的组合。这些粘合剂材料可以是基于溶剂的或基于水的。可以使用的特定聚氨酯的例子在美国专利No.7,342,068中进行了描述。
附图是本发明的具有导电层的电光显示器的基础前平面层压板(10)的示意横截面。通常，透光导电层(14)将被承载在透光基板(12)上，透光基板(12)优选地是柔性的，在这个意义上，基板可以围绕直径为10英寸(254mm)的桶(例如)人工地缠绕而没有永久变形。基板典型地是聚合物薄膜，并通常具有在约1至约25密耳(25至634μm)、优选地约2至约10密耳(51至254μm)的范围的厚度。基板(12)形成最终的显示器的观察表面，并且可以具有一个或多个另外的层，例如，吸收紫外辐射的保护层、防止水分的进入的阻挡层、或者防反射涂层。
导电层(14)包括双相电极层。电光介质层(16)与导电层(14)电接触。图中所示的电光介质是具有多个微囊体的相反电荷双粒子封装电泳介质，微囊体中的每一个包括包含基于碳氢化合物的液体的囊体壁(18)，负带电白色粒子(22)和正带电黑色粒子(24)悬浮在液体中。微囊体被保持在粘合剂(25)内。在电光层(16)上施加电场时，白色粒子(22)移动至正电极，并且黑色粒子(24)移动至负电极，以使得对于经由基板(12)观察显示器的观察者来说，根据层(14)在最终显示器内的任意点处相对于背板是正的还是负的，层(16)看起来是白色或黑色。
图中所示的前平面层压板(10)还包括邻近电光介质层(16)的一层层压粘合剂(26)以及覆盖粘合剂层(26)的释放片(28)。释放层(28)从粘合剂层(26)剥离，并且粘合剂层被层压至背板以形成最终的电光显示器。
本发明的双相导电层可以是电光显示器的前电极，其是位于离观察表面最近的一侧上的电极。在完全透光或具有两个观察表面的电光显示器中，本发明的双相导电层可以是前电极和背电极。
对于电光显示器，关键的是控制聚合物材料的电性质；否则，显示器可能经历减弱的光学性能。当聚合物材料的体电阻不大于1x 1012Ohm-cm时，光学性能可以增强。
导电聚合物
以另一形式，本发明提供一种双相电极层，其中，第二相是离子导电聚合物，其中，一个离子可以迁移通过聚合物材料，而另一个不能。该类型的离子材料防止离子从聚合物材料扩散出并潜在地损坏离子扩散至的其他层(例如，有机半导体层)。
离子导电被示出为通过“跳跃”机制发生，其中，离解的自由离子在离子聚集体(离子对和更高的聚集体)之间转移，这些聚集体中的大多数实质上是中性的。根据本发明，离子材料的阴离子和阳离子中的仅一个能够运动。固定的离子被约束至单个位置，而移动离子仍然自由迁移。合适的离子材料的示例是聚合物盐，例如，聚合羧酸盐的离子盐。在该情况下，羧酸盐离子是被有效地固定的，因为其附接至聚合物链，并且仅可以整体随着聚合物移动。另一方面，阳离子的平衡离子可以自由地参与跳跃运动，并且其可以移动的速率取决于与阴离子羧酸盐的静电相互作用的强度、粘合剂介质中羧酸盐-平衡离子聚集体的浓度、介质的粘度、以及通过介质的平衡离子的溶解的自由能。
如在美国专利公布No.2009/0122389中所述，大的阳离子是有利的，因为它们具有对离子聚集状态的吸引的相对低的静电能，并且因此容易从离子聚集状态离解。作为示例，季铵碱可以用于中和聚氨酯上的羧基功能，导致能够支持如上所述的离子导电的季铵羧酸盐聚合物。
期望的是，离子材料被选择以使得最终的聚合物材料在干燥之后的导电性可以通过改变聚氨酯的羧酸含量并且还通过所使用的阳离子来修改和调节。例如，在聚氨酯上的羧基被季铵碱中和的前述系统中，以给定的羧酸含量，导电性可以期望以以下顺序增大：
四甲基铵<四乙铵<四丁基铵，等。
磷盐也可以被使用，并且由于较大尺寸的中心原子，应当比包含类似物的氮更导电。其他阳离子活性种(例如，金属的配离子)也可以用于该目的。聚合物材料中离子材料的溶解度在该方法中不是问题，因为离子是介质的内在部分，并且因此不能相分离(phaseseparate)为单独的结晶相。
聚合物材料的酸性成分也可以通过将羧酸成分替代为具有较高离解常数的基(例如，硫酸酯、磺酸、亚磺酸、膦酸、次膦酸基或磷酸酯)来被制作得更酸，只要存在至少一个可离解质子即可。季盐和其他大的阳离子由于它们的大尺寸和在低极性的干燥粘合介质中相对高的离子离解度，仍将期望用作平衡离子。氮基酸也可以在依附至足够地吸电子功能的情况下使用(例如，RSO2-NH-SO2R)。在该情况下，可以使用几乎任何可移动离子，包括叔胺，因为可移动离子甚至以质子化形式存在于干燥的粘合剂中。然而，基于较大的胺(即，具有较长的烷基尾的胺)的可移动离子可能仍是优选的，因为它们实际上尺寸更大，并且因此包括它们的离子对将更可离解。可替换地，聚合物上的羧酸基可以与不是强布朗斯台德酸的可移动离子(即，不具有酸质子，诸如上述季阳离子)一起使用。
可以通过在聚合物主链中使用季铵基或作为侧链，以及优选地使用大的阴离子(例如，六氟磷酸盐、四丁基铵、四苯硼酸等)作为可移动离子来构造其中阳离子是固定离子的聚合物材料。季铵基可以由磷、硫或没有可离解氢的其他阳离子基来代替，包括通过与金属阳离子的络合作用形成的阳离子基。后者的示例包括聚醚/包含锂离子的复合物，特别是大环聚醚(例如，18-冠醚-6)或具有过渡金属离子的聚胺复合物。在该情况下，阴离子的可移动离子可以包括以上列出的那些类型的离子，加上诸如羧酸盐或甚至酚盐的更强基础的材料。
可替代的固定阳离子聚合物材料包括含有从基础单体获得的重复单元的聚合物，例如，聚(乙烯基吡啶)、聚(β-二甲氨基丙烯酸乙酯)等，以及包含这种基的共聚物，连同不是良好的布朗斯台德受体的可移动阴离子(例如，磺酸盐、硫酸盐、六氟磷酸盐、四氟硼酸盐、双(甲基磺酰)亚胺酯、磷酸盐、膦酸盐等)。从这种氨基单体获得的季盐也可以使用，例如，聚(N-甲基或苯基(乙烯基吡啶))、聚(N-烷基(或芳基)-N'-乙烯基咪唑)、以及聚(β-三甲胺基乙基)丙烯酸或甲基丙烯酸盐，以及包括这些离子基的乙烯基共聚物。如之前那样，较大的可移动离子是优选的。
这些化学改性技术不限于聚氨酯，而是可以应用至合适结构的任何聚合物。例如，乙烯基聚合物可以包含阴离子或阳离子的固定离子。
在本发明的另一形式中，聚合物材料可以包含从PEDOT-PSS、聚乙炔、聚苯硫醚、聚苯撑乙烯和它们的组合中选择的一个或多个导电聚合物。聚合物材料的厚度的范围可以从大约0.1μm至20μm。聚合物材料可以是(a)水溶性或水分散性并由水涂布，(b)可溶解或可分散于有机溶剂中并由有机溶剂涂布，或(c)以单体形式或低聚物形式涂布并且之后通过UV、辐照、加热或本领域中已知的其他方法聚合。合并至聚合物材料的添加物可以原位形成；换句话说，一个或多个前体材料可以合并至聚合物材料中，其中前体材料可以相互反应或与聚合物材料反应，或通过将聚合物材料暴露于导致前体材料的变化的条件(例如，暴露于热、光、或磁场或电场)而改变以形成最终的添加物。
可扩散的离子添加物
第二相可以包含一种或多种离子添加物，例如，(a)盐、聚电解质、聚合物电解质、固体电解质和它们的组合；或(b)非反应性溶剂、导电有机化合物和它们的组合。
在一个形式中，添加物可以是盐，诸如无机盐、有机盐或它们的组合，如在美国专利No.7,012,735中所述。示例性盐包括乙酸钾和四烷基铵盐，特别是四丁基铵盐，诸如氯化物。盐的另外的示例包括诸如RCF3SOF3,RClO4,LiPF6,RBF4,RAsF6,RB(Ar)4和RN(CF3SO2)3的盐，其中R可以是任何阳离子，诸如Li+、Na+、H+或K+。可替换地，R可以包括形式N+R1R2R3R4的铵基。优选的盐是四丁基六氟磷酸铵。
在另一形式中，添加物可以是具有包含至少三个氟原子的阴离子的盐，如在美国专利No.8,446,664中所述。盐可以例如具有六氟磷酸盐阴离子。盐还可以具有咪唑阳离子。示例性盐包括1-丁基-3-甲基咪唑六氟磷酸盐(以下为“BMIHFP”)、1-丁基-3-甲基哌啶六氟磷酸盐、1-丁基-3-甲基吡啶六氟磷酸盐、1-乙基-3-甲基吡啶六氟磷酸盐、六氟磷酸钠、1-丁基-3-甲基咪唑三氟甲磺酸盐、和1-丁基-3-甲基咪唑四氟化硼。优选的盐是BMIHFP。该优选的盐在25℃是液体并且可以直接分散在水性聚合物分散体或乳液中，而不使用任何溶剂。可替换地，由于优选的盐在25℃以约百分之一的量可溶解于水，因而该盐可以以稀水溶液的形式添加。作为水溶液的该盐的添加避免将任何不期望的有机溶剂引入至粘合剂中。
可替换地，含氟的盐可以具有四氟硼酸盐阴离子、四苯硼酸盐阴离子、双(三氟甲烷)磺酰胺阴离子(“triflimide”)、四(五氟苯基)硼酸盐阴离子、四(3,5-双(三氟甲基)苯基)硼酸盐阴离子、或三氟甲烷磺酸盐(“triflate”)，例如，1-丁基-3-甲基咪唑四氟化硼、或1-丁基-3-甲基咪唑三氟甲磺酸盐。含氟的盐可以基于聚合物材料的固体含量以从约50至约10000ppm的量存在，并且通常为约100至约1000ppm。
在其他实施例中，聚合物电解质是聚电解质。聚电解质通常是其中约10％或更多的分子由能够离子化以形成带电粒种的官能团组成的聚合物。聚电解质内的特定官能团的示例包括但不限于羧酸、磺酸、磷酸和季铵化合物。这些聚合物可以与有机或无机盐组合或可替换地单独使用。聚电解质的示例包括但不限于聚丙烯酸、聚磺苯乙烯、聚(2-乙烯基吡啶)、聚(4-乙烯基吡啶)、聚(二甲基氯化铵)、聚(甲基丙烯酸二甲胺乙酯)、聚(甲基丙烯酸二乙胺乙酯)，并且可以包括多酸的盐，诸如但不限于聚丙烯酸的碱金属盐。优选的聚电解质是聚丙烯酸的钠盐。
在本发明的另一形式中，添加物是聚合物电解质。这里使用的术语“聚合物电解质”描述了能够溶解盐的聚合物。这些聚合物中的盐的溶解度可以通过聚合物中形成醚、羰基、羧酸、伯、仲、叔、季胺基、磺酸基、酸的氧和/或氮原子的存在来增强。聚合物电解质的示例包括聚醚类化合物，诸如聚环氧乙烷、聚环氧丙烷、聚四氢呋喃；聚胺，如聚乙烯亚胺、聚乙烯吡咯烷酮；含有季铵基的聚合物，诸如N+R1R2R3R4，其中，R1、R2、R3和R4各自独立地是具有1-25个碳原子的H或笔直、分支、或环烷基，其中，平衡离子可以从任何有机或无机阴离子中选择。
其他添加物仍然可以包括非反应性溶剂，其可以改善或可替换地阻碍离子在溶液中的移动性。合适的非反应性溶剂的示例包括水、乙醚、丙醚、二甘醇、乙二醇二甲醚、二乙二醇二甲醚、N-甲基吡咯烷酮等。在另一实施例中，导电有机化合物可以用作添加物。这些化合物的一些非限制性示例包括聚苯胺、聚噻吩、聚吡咯、聚-3,4-二氧亚乙基噻吩、以及这些材料在它们的n型或p型掺杂状态的衍生物。
如在美国专利No.7,256,766中公开的，还已知“光学偏置元素”可以设置在封装的电泳显示器的一个层中以调节显示器的外观。这种光学偏置元素可以被添加至聚合物材料。包含这种光学偏置元素的聚合物材料的电性质可以通过使用本文描述的添加物来优化。
添加物的最佳量当然随着所使用的确切聚合物材料和确切添加物、以及最终混合物的期望体积电阻率而宽泛地变化。然而，作为一般的指导，可以指出的是，每克聚合物材料的约10-5至约10-4摩尔的添加物的浓度被发现给出有用的结果。当添加物是盐时，该范围用于1:1盐，诸如四丁基氯化铵,四丁基六氟磷酸铵和醋酸钾；如果使用诸如碳酸钠或氯化钙的1:2盐，每克聚合物材料的10-6摩尔的级别的盐的较低浓度可能足够。聚合物材料的体积电阻率通常随着添加物的浓度以可预测的方式变化，因此多少添加物应当被添加以实现期望的体积电阻率的最终选择可以容易地凭经验确定。
尽管在现有技术的电光显示器中少量的盐已经被添加至用作粘结剂和层压粘合剂的聚合物，例如作为杀菌剂，以保护聚合物以免在延长的存储期间生物降解，但是这种盐通常在存储期间(它们执行它们的杀菌或类似功能)用完。相反，在本发明中使用的添加物意图作为聚合物材料的永久成分，因为它们意图实现其导电率的永久调节。而且，所使用的添加物的最佳量通常显著大于用作杀菌剂等的盐的量。
包含羟基的低分子量聚合物/乙二醇添加物
本发明的另一形式涉及具有电极层的电光显示器，电极层包括由导电基体制成的第一相和由混合有添加物的聚合物制成的第二相，其中，添加物是低数值平均分子量(Mn不大于约5000)的包含羟基的聚合物。如在美国专利No.7,349,148中所述，用于该目的的优选的聚合物是聚(乙二醇)(PEG)，其期望地具有不大于约2000的Mn。在该添加物中，质子移动，而不是电子。用于任何特定系统的包含羟基的聚合物添加物的最佳浓度最好地由经验确定，但是作为一般的指导，可以说是通常每克聚合物材料大约10-6到10-5摩尔的最佳浓度。
通常情况下，如果通过将第二相的溶液的薄膜涂布在包含第一相的基板上并干燥以形成电极层来形成电极层，则添加物通常简单地在涂布之前溶解或分散在聚合物材料的溶液中。添加物可以添加至不掺水的溶液，或者可以溶解在水溶液、非水溶液或它们的组合中。当然需要确保添加物在聚合物材料中均匀地分布，以防止最终的导电层内的导电率的变化，但涂布技术的技术人员将熟悉常规的技术，诸如在辊式磨碎机上的超长搅拌，用于确保这种均匀分布。双相电极层可以适当地与基板一起使用。可替换地，一旦设置，第二相可以添加足够的结构至第一相以使得基板可以被移除。
要使用的具体添加物的选择很大程度上通过考虑与电极的兼容性和在要添加添加物的聚合物材料中的溶解度来确定。通常情况下，如果添加物要被添加至含水的聚合物材料，则添加物应当被选择为具有良好的水溶性，从而在盐中，碱性金属和替代的铵盐通常是优选的。应当注意确保添加物不会导致聚合物粒子的聚集。而且，添加物应当期望地不导致聚合物材料的pH的重大改变，并且应当不与其最终接触的最终显示器的电极或聚合物材料或其他部件(例如背板)化学反应。
一个或多个添加物的添加极大地扩展了可以用于电光显示器的聚合物材料的范围。特别地，一个或多个添加物的添加使得能够使用以下聚合物材料，该聚合物材料具有在电光显示器中高度期望的机械性质但是具有在它们的纯态下太高而无法使用的体积电阻率。而且，由于一些电光显示器，特别是封装的电泳显示器和电致变色显示器对湿气敏感，因而一个或多个添加物的添加可以用于将在这种显示器中到目前为止使用的基于水的聚氨酯分散物替换为不吸湿的和/或疏水的聚合物材料。
聚合物材料可以包含除所使用的添加物以外的成分以调节其体积电阻率；例如，聚合物材料还可以包含染料或其他着色剂。
应该理解，本文所公开的改良的聚合物材料可以用于除电光显示器以外的应用中。

Claims (16)

1.一种电光显示器，包括电光材料层和配置为将电场施加至所述电光材料层的电极层，所述电极层包括：
第一相，由高导电基体制成，以及
第二相，由具有受控体积电阻率的透光聚合物材料成分制成。
2.根据权利要求1所述的电光显示器，其中，所述第一相的基体是碳纳米管、银纳米线、涂布金属的开放泡沫结构、或印刷丝网，或它们的组合。
3.根据权利要求1所述的电光显示器，其中，所述第一相的基体规则地布置。
4.根据权利要求1所述的电光显示器，其中，所述第一相的基体不规则地布置。
5.根据权利要求1所述的电光显示器，其中，所述第一相组成观察区域的少于10％。
6.根据权利要求1所述的电光显示器，其中，所述第二相的受控体积电阻率不大于1x1012Ohm-cm。
7.根据权利要求1所述的电光显示器，其中，所述第二相的透光聚合物材料成分由导电聚合物制成。
8.根据权利要求7所述的电光显示器，其中，所述导电聚合物是PEDOT-PSS、聚乙炔、聚苯硫醚、或聚苯撑乙烯、或它们的组合。
9.根据权利要求7所述的电光显示器，其中，所述导电聚合物是离子导电聚合物。
10.根据权利要求9所述的电光显示器，其中，所述离子导电聚合物是聚合物盐。
11.根据权利要求1所述的电光显示器，其中，所述第二相的透光聚合物材料成分由聚合物和添加物制成。
12.根据权利要求11所述的电光显示器，其中，所述添加物是一种或多种离子添加物。
13.根据权利要求12所述的电光显示器，其中，所述离子添加物是盐、聚电解质、聚合物电解质、或固体电解质、或它们的组合。
14.根据权利要求13所述的电光显示器，其中，所述离子添加物是盐，以及所述盐是含氟的盐。
15.根据权利要求11所述的电光显示器，其中，所述添加物是低数值平均分子量的包含羟基的聚合物。
16.根据权利要求15所述的电光显示器，其中，所述添加物是聚乙二醇。
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US20150205178A1 (en) 2015-07-23
US20170068125A1 (en) 2017-03-09
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KR20160100358A (ko) 2016-08-23
US9529240B2 (en) 2016-12-27
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CN109491173A (zh) 2019-03-19
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