CN104448955A - 电泳颗粒 - Google Patents

电泳颗粒 Download PDF

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CN104448955A
CN104448955A CN201410598350.2A CN201410598350A CN104448955A CN 104448955 A CN104448955 A CN 104448955A CN 201410598350 A CN201410598350 A CN 201410598350A CN 104448955 A CN104448955 A CN 104448955A
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particle
electrophoretic
pigment
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capsule
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J·D·费克
M·D·瓦勒斯
M·D·姆赛克
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E Ink Corp
Shepherd Color Co
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Abstract

一种电泳媒质，包括被分散置于流体中的至少一种带电颗粒。该带电颗粒包括表面积至少为7m2/g的无机黑色颜料。优选的颜料为磁铁矿或含有铁、铬、镍、锰、铜和钴中的两种或更多的混合的金属氧化物，例如铜铁锰氧化物尖晶石或铜铬锰氧化物尖晶石。该无机黑色颜料可带有聚合物涂层。

Description

电泳颗粒
本申请是发明名称为“电泳颗粒”、申请日为2010年2月9日、申请号为2010800125717的中国专利申请的分案申请。
本申请涉及：
(a)美国专利第6,822,782号；
(b)美国专利第7,411,720号；
(c)美国专利第7,002,728号；和
(d)美国专利第7,247,379号。
技术领域
本发明涉及电泳颗粒(即，用在电泳媒质中的颗粒)和用于制造这样的电泳颗粒的方法。本发明还涉及使用这样的颗粒的电泳媒质和显示器。更具体地，本发明涉及新的黑色或深色的电泳颗粒。
背景技术
在美国专利第7,012,600号中详细论述了关于电光显示器的背景术语和技术状况，读者可参照该美国专利获得进一步信息。因此，以下对术语和技术状态作简要概述。
许多年来，基于粒子的电泳显示器一直是人们广泛研究和开发的课题，在这种基于粒子的电泳显示器中多个带电粒子在电场的影响下穿过流体。与液晶显示器相比，这种显示器的优点在于亮度和对比度好、可视角度宽、状态的双稳定性以及功耗低。
此处使用的术语“双稳的”和“双稳定性”取其在本领域中的常规含义，指的是包括具有第一和第二显示状态的显示元件的显示器，所述第一和第二显示状态至少有一种光学性质不同，从而在利用具有有限持续时间的寻址脉冲驱动任何给定元件以呈现其第一或第二显示状态之后，在该寻址脉冲终止后，该状态将持续至少几倍于(例如至少4倍于)改变该显示元件的状态所需的寻址脉冲的最小持续时间的时间。美国专利第7,170,670号示出，某些基于颗粒的能够灰度显示的电泳显示器不仅在处于它们的极端黑色和白色状态时具有稳定的灰度，在处于它们的中间灰度状态时也具有稳定的灰度，且一些其他类型的电光显示器也同样如此。尽管为了方便起见，此处的术语“双稳的”被用于涵盖双稳的或多稳的显示器，但上述类型的显示器更适合被称作“多稳的”，而非双稳。
然而，长期存在的电泳显示器的图像质量问题阻碍了其广泛使用。例如，构成电泳显示器的颗粒易于沉降，这就导致这种显示器的使用寿命不足。
如以上所说，电泳媒质需要有流体存在。在大部分现有的电泳媒质中，流体为液体，但电泳媒质可以用气态流体制成；参见例如Kitamura,T.等人的“Electrical toner movement for electronic paper-like display”,IDW Japan,2001,Paper HCSl-1，以及Yamaguchi,Y.等人的“Toner display using insulativeparticles charged triboelectrically”，IDW Japan,2001,Paper AMD4-4。还可以参见美国专利公开号2005/0259068,2006/0087479,2006/0087489,2006/0087718,2006/0209008,2006/0214906,2006/0231401,2006/0238488,2006/0263927和美国专利第7,321,459和7,236,291号。由于当媒质用于在允许沉降的取向上，例如媒质可以在垂直面内下沉时，具有与基于液态的电泳媒质相同的颗粒沉降，因此这种基于气态的电泳媒质遭受了同样的问题。在基于气态的电泳媒质中的颗粒沉降问题比在基于液态的电泳媒质中更严重，因为与液体相比，气态悬浮流体的粘度更低，从而使电泳颗粒的沉降更快。
转让或权属于麻省理工学院(MIT)和伊英克(E Ink)公司的大量专利和申请描述了在封装的电泳和其他电光媒质中使用的各种技术。这种封装的媒质包含大量的小囊(capsule)，每一个小囊本身包含内相以及环绕内相的囊壁，该内相包含流体媒质中的电泳移动粒子。典型地，这些囊本身被保持在聚合物粘合剂内以形成位于两个电极之间的粘附层(coherent layer)。在这些专利和申请中描述的技术包括：
(a)电泳颗粒、流体和流体添加物；参见例如美国专利第5,961,804；6,017,584；6,120,588；6,120,839；6,262,706；6,262,833；6,300,932；6,323,989；6,377,387；6,515,649；6,538,801；6,580,545；6,652,075；6,693,620；6,721,083；6,727,881；6,822,782；6,870,661；7,002,728；7,038,655；7,170,670；7,180,649；7,230,750；7,230,751；7,236,290；7,247,379；7,312,916；7,375,875；7,411,720号；以及美国专利申请公开号2005/0012980；2006/0202949；2007/0146310；2007/0200795；2008/0013155和2008/0013156；
(b)囊、粘合剂和封装方法；参见例如美国专利第6,922,276和7,411,719号；
(c)包含电光材料的膜和子组件；参见例如美国专利第6,982,178号和美国专利申请公开号2007/0109219；
(d)用在显示器中的背板、粘合层和其他辅助层以及方法；参见例如美国专利第7,116,318号；和美国专利申请公开号2007/0035808；
(e)色彩的形成和色彩的调节；参见例如美国专利第7,075,502号；和美国专利申请公开号2007/0109219；
(f)用于驱动显示器的方法；参见例如美国专利第7,012,600号；和美国专利申请公开号2006/0262060；以及
(g)显示器的申请；参见例如美国专利第7,312,784号；和美国专利申请公开号2006/0279527。
可以把已知的封装的和非封装的电泳媒质分为两个主要类型，方便起见，以下分别称为“单颗粒”和“双颗粒”。有关这种单颗粒和双颗粒显示器的描述，参见美国专利第6,870,661号。
前述的很多专利和申请认识到，在封装的电泳媒质中围绕离散的微囊的壁可以由连续相代替，因而产生所谓的聚合物分散的电泳显示器，其中电泳媒质包含多个离散的电泳流体微滴以及连续相聚合物材料，并且尽管没有与每个单独的微滴关联的离散的囊膜，但可以把这种聚合物分散的电泳显示器中的电泳流体的离散颗粒看作囊或微囊；参见例如前述的美国专利第6,866,760号。因此，为了本申请的目的，将这样的聚合物分散的电泳媒质看作是封装的电泳媒质的子类。
与此相关的电泳显示器类型称为“微单元电泳显示器”。在微单元电泳显示器中，带电颗粒和流体不封装在微囊中，而保持在形成于载体媒质中的多个腔内，该载体媒质一般为聚合物薄膜。参见例如授予给Sipix Imaging公司的美国专利第6,672,921和6,788,449号。以下用术语“微腔电泳显示器”来涵盖封装的和微单元电泳显示器。
尽管电泳媒质通常是不透明的(例如，由于在许多电泳媒质中，粒子基本上阻挡可见光通过显示器的透射)并且工作在反射模式下，但是可以使许多电泳显示器工作在所谓的“快门模式”下，在该模式下一种显示状态是基本上不透明的而一种显示状态是光透射的。参见例如美国专利第5,872,552；6,130,774；6,144,361；6,172,798；6,271,823；6,225,971和6,184,856号。与电泳显示器类似但是依赖于电场强度变化的介电泳显示器可以工作在类似的模式下；参见美国专利第4,418,346号。其他类型的电光显示器也能工作在快门模式下。工作在快门模式下的电光媒质可以用在全彩色显示器的多层膜结构中；在这样的结构中，至少靠近显示器观察面的一层工作在快门模式下以暴露或隐藏离该观察面较远的第二层。
封装的电泳显示器一般不受传统电泳设备的聚集和沉降失效模式的影响并且具有另外的优点，例如可以在各种不同柔性和刚性衬底上印刷或者涂覆该显示器。(使用“印刷”一词旨在包括印刷和涂覆的所有形式，包括但并不局限于：预调式涂覆，例如小块模具型涂覆(patch die coating)，狭缝式或挤压式涂覆，坡流式或阶式涂覆，淋幕式涂覆；压辊涂覆，例如辊式刮刀涂覆、前向和反向辊涂覆；凹版印刷涂覆；浸渍涂覆；喷涂；弯液面涂覆；旋涂；刷涂；气刀涂覆；丝网印刷工艺；静电印刷工艺；热印刷工艺；喷墨印刷工艺；电泳沉积(参见美国专利第7,339,715号)；以及其它类似的技术)。因此，得到的显示器可以为柔性。另外，由于显示器媒质可以是印刷的(使用各种方法)，显示器本身比较低廉。
然而，封装的电泳显示器的电光性能仍可以被改善。电泳显示器一般被设计为具有黑和白的极端光学状态；然后通过提供靠近电泳媒质的滤色片产生颜色。很多现有的双颗粒显示器将二氧化钛用作白色颜料且将碳黑用作黑色颜料。然而，如前述美国专利第7,002,728号中讨论，碳黑给电泳显示器带来很多问题，且该专利教导了用亚铬酸铜替代碳黑，该亚铬酸铜优选具有聚合物壳，并且可选地在亚铬酸铜核和聚合物壳之间有二氧化硅层。
发明内容
把亚铬酸铜用作双颗粒电泳显示器中的黑色颜料解决了与碳黑颜料相关的很多问题。然而，对用在电泳显示器中的颜料的要求在不断提高。特别地，已发现为了确保采用滤色片阵列的彩色电泳显示器具有较好的色彩饱和度，实现显示器的深色状态的较低反射率是非常重要的，即使由亚铬酸铜颜料所提供的深色状态也比为了实现此目的理想反射率还低。因此，需要提供一种能够提供比由亚铬酸铜提供的深色状态更深的黑色颜料，本发明提供了这样的黑色颜料。由本发明提供的一些颜料还具有无铬的优点，从而去除了在含有亚铬酸铜的媒质中充当污染物的六价铬。
因此，在一个方面，本发明提供一种电泳媒质，其包括置于流体内的且能够在施加到该流体上的电场作用下移动通过该流体的至少一种带电颗粒。根据本发明，该至少一种带电颗粒包括表面积至少为7m2/g的无机黑色颜料。
优选的用在本发明的无机黑色颜料的表面积至少为10m2/g，且理想为至少15m2/g。如下面实施例所证明，据经验已发现，平均颜料颗粒尺寸与深色状态的性能之间有很紧密的关系，随着表面积的增大，显示器深色状态的反射率不断降低。因此，期望使用表面积尽可能大的颜料，该颜料不具有使用非常小的颜料颗粒时可能遇到的操作及安全问题。优选的黑色颜料为金属氧化物，例如磁铁矿(magnetite)、(Fe3O4)，以及含有铁、铬、镍、锰、铜、钴和其他可能金属中的两种或更多的混合金属氧化物。合适的颜料参见例如“Industrial Inorganic Pigments”，Gunter Buxbaum and Gerhard Pfaff(eds.),Wiley-VCH,2005。已发现有两种颜料可以提供较好的结果：铜铁锰氧化物尖晶石(从Cincinnati，Ohio的Shepherd Color公司购得的Shepherd Black444)，和铜铬锰氧化物尖晶石(从同一家公司商业购得的Black 20C920)。制造商声称前一种材料的平均颗粒尺寸为约0.5μm，比重为5.3，且表面积为22m2/g，且声称后一种材料的平均颗粒尺寸为约1.0μm，比重为5.1，且表面积为11m2/g。通常，本发明颜料颗粒的平均直径为0.1至2μm；如果颗粒的平均颗粒尺寸超过此范围，可使用研磨或其他常规技术来减小颗粒尺寸。颜料颗粒可以涂布有二氧化硅和/或具有化学键合至颜料颗粒、或在该颜料颗粒周围交联的聚合物。将聚合物化学键合至颜料颗粒一般为优选。该聚合物可包括颜料颗粒的重量的百分之1至15，优选为百分之2至8。聚合物可包括带电或可带电基团，例如氨基基团。聚合物还可包括主链和从主链延伸出的多个侧链，每个侧链包括至少4个碳原子。聚合物还可以由丙烯酸酯或甲基丙烯酸酯制成。关于在颜料颗粒上形成聚合物涂层的方法的进一步细节参见美国专利第6,822,782；7,411,720和7,230,750号。
本发明的电泳媒质可以是任一前述的类型，但优选包括至少一种第二颗粒，该至少一种第二颗粒具有至少一个与本发明的颜料颗粒的光学特性不同的光学特性，该第二颗粒的电泳迁移率与本发明的颜料颗粒的电泳迁移率不同。这两组颗粒可带有极性相反的电荷。第二颗粒可基本为白色，为此优选的白色颜料为二氧化钛。在本发明的电泳媒质中，悬浮的流体可以为液态或气态的，并且该液体可包括碳氢化合物，或烃与氯代烃的混合物。
本发明的电泳媒质可以是封装类型的且包括囊壁，流体和至少一种颗粒保持在该囊壁中。这样的封装媒质可包括多个囊，每个囊包括囊壁和保持在该囊壁中的悬浮流体和至少一种颗粒，该媒质还包括围绕在该囊周围的聚合物粘结剂。
本发明涉及一种电泳显示器，其包括本发明的电泳媒质和被置于靠近所述电泳媒质用于施加电场至该电泳媒质的至少一个电极。在这样的电泳显示器中，电泳媒质可包括多个囊。可替代地，电泳媒质可以是聚合物分散型且包括多个微滴，该微滴包括流体和在该微滴周围的连续相聚合物材料。电泳显示器还可以是微单元类型的且包括基底，该基底具有多个形成在其中的密封的腔，其中流体和颗粒保持在该密封的腔中。
在另一方面，本发明提供了一种无机黑色颜料，其表面积至少为7 m2/g，具有化学键合在颗粒上的或在颗粒周围交联的聚合物。优选地，聚合物被化学键合至该颗粒。聚合物可包括颗粒重量的百分之1至30，优选为百分之4至25。聚合物可包括带电或可带电基团，例如氨基基团。聚合物还可包括主链和从主链延伸出的多个侧链，每个侧链包括至少4个碳原子。聚合物还可以由丙烯酸酯或甲基丙烯酸酯制成。
本发明的显示器可用在现有电光显示器所使用的任何应用中。因此，例如，该显示器可用在电子书阅读器、便携式计算机、平板计算机、手机、智能卡、标牌、表、货架标签或闪存中。
在另一方面，本发明提供一种用于制造涂布聚合物的颜料颗粒的方法，该方法包括：
(a)使表面积至少为约7m2/g的无机黑色颜料颗粒与试剂反应，该试剂具有能够与所述颗粒反应且键合所述颗粒的功能基团，且还具有可聚合的或聚合引发基团，由此使所述功能基团与所述颗粒的表面反应并使可聚合的基团与其相接附；以及
(b)在能有效引起所述颗粒上的可聚合或聚合引发基团与至少一种单体或低聚物之间发生反应的条件下，使步骤(a)的产物与该至少一种单体或低聚物反应，由此形成键合至该颗粒的聚合物。
在该方法中，颜料颗粒可以在步骤(a)前涂布二氧化硅。用在步骤(a)中的试剂包括硅烷偶联基团，例如三烷氧基硅烷偶联基团。试剂还可包括氨基基团。例如试剂包括N-[3-(三甲氧基硅基)丙基]-N'-(4-乙烯苄基)-乙二胺。单体或低聚物可以包括至少一种丙烯酸酯或甲基丙烯酸酯，例如，月桂醇甲基丙烯酸酯。
附图说明
附图1和附图2分别示出了本发明的一些实验性显示器和在下面示例3所描述的实验中得到的对照显示器的深色和浅色状态的反射率值。
图3为在下面示例4所描述的实验中得到的本发明的一些实验性显示器的深色颜料的深色状态对每单位重量的表面积的图。
具体实施方式
如以上所述，本发明提供一种采用带电颗粒的电泳媒质，所述带电颗粒包括表面积至少为7m2/g的黑色无机颜料。期望该颗粒涂布有聚合物。已发现，采用这样的黑色无机颜料的电泳媒质可显示出强烈的深黑状态，其L*值为约13至约22(其中L*的一般CIE定义为：
L*＝116(R/Ro)1/3-16,
其中R为反射率，R0为标准反射率值)，该L*值显著低于基于亚铬酸铜的电泳媒质的L*值。本发明的电泳媒质的白色状态仅比基于亚铬酸铜的电泳媒质稍暗，使得本发明媒质的动态范围更大(极端深色和白色状态之间的差异，用单位L*表示)。另外，通过模拟获知，为了优化基于滤色片阵列的显示器中的色彩饱和度，改善深色状态比改善白色状态更重要，本发明的媒质在这样的显示器中具有更优异的色彩饱和度，且还具有更令人愉悦的色彩特性。
仅仅为了示意提供下面的示例，用以示出用在本发明的电泳媒质和方法中使用的优选的试剂、条件和技术。
示例1：制备涂布有聚合物的无机颜料颗粒
将原始颜料(Shepherd Black 444和Shepherd Black 20C920)在水中研磨以将前一颜料的平均颗粒尺寸降低至约0.3μm，将后一颜料降低至约0.5μm。然后采用基本相似于前述美国专利第6,822,782号中示例26的方法利用N-[3-(三甲氧基硅基)丙基]-N'-4-乙烯苯基)乙二胺双盐酸盐(N-[3-(trimethoxysilyl)propyl]-N'-(4-vinylbenzyl)ethylenediaminebishydrochloride)(从United Chemical Technologies获得)将研磨后的颜料的表面功能化。通过热重分析评价所实现的表面功能化的量，结果表明Black444中的易挥发(有机)材料为4-10％，Black 20C920中的易挥发(无机)材料为1.1-1.3％。
示例2：制备包含涂布有聚合物的无机颜料颗粒的电泳媒质
制备示例1中形成两个黑色颜料的标准溶液以及电泳媒质内部相的各种其他组分的标准溶液，并在250mL的塑料瓶中混合以形成下面的内部相：
在配备有搅拌器和滴液漏斗的500mL夹套反应器中制备温度为42.5℃的明胶(10克)的去离子水(240克)溶液。在强烈搅拌下，采用具有流出口的额外漏斗将所制备的以上描述的内部相在1分钟内加入到明胶溶液的表面下。在完成以上加入后，马上把搅拌速率升高至750rpm以使形成的内部相液滴的尺寸在期望的范围内，且在该搅拌速率下保持1小时。在这段时间结束时，将温度为40℃的阿拉伯胶(10克)的水溶液(251.6克)加入至内部相分散剂，且通过加入重量百分比为10％的醋酸将所得混合物的pH调节至4.9。然后，将反应混合物的温度逐步降低至8℃；当其温度达到10℃时，加入戊二醛(2.5克的50％水溶液)。然后将反应混合物加热至25℃，且使其在该温度下保持一晚以在水性媒质中形成分散的微囊的。微囊通过沉淀分离、利用去离子水清洗，然后用目数为45μm和20μm的筛子过筛。通过分析可知，所得到的囊的平均大小为约40μm，其中囊中超过97％的囊的直径在20μm到60μm之间。
示例3：从囊到实验性显示器的转变
如下将示例2所制备的囊转变为聚合物粘合剂中的囊浆。将囊沉降至少一个小时，并倒掉一部分而非全部的过量水。摇动包含囊的瓶子以重新分散水中的囊且用氢氧化铵把分散体的pH调节至9.0-9.5。再次摇动瓶子以重新分散囊，然后用热重分析测量固态囊。通过离心并倒掉上层液体对囊进行浓缩。加入充足的用于制造的聚合物粘合剂、8：1w/w的囊对粘合剂的比例、羟丙基甲基纤维素(hydroxypropylmethylcellulose)(浆质量的0.2％)、TritonXl00表面活性剂(浆质量的0.03％)和水以制备含有按重量计33％的囊固态的浆，猛烈摇动所得的浆以分散浓缩在容器底部的囊。然后把包含该浆的瓶子置于辊式制粉机上且至少滚动10小时。
然后利用4密尔(101μm)的涂布间隙，通过棒式涂布把所得的浆涂布到聚(对苯二甲酸乙二醇)(PET)/ITO膜的涂布有铟锡氧化物(ITO)的表面上，将被涂布的膜在传送式炉子中在60℃下干燥约2分钟以制备厚度为约18μm的囊(电光)层。单独地，将美国专利第7,012,735号中描述的定制聚氨酯层压粘合剂掺杂以180ppm四丁基六氟磷酸胺(tetrabutylammoniumhexafluorophosphate)，并涂布释放板上，厚度约为25μm，采用热辊层压机把得到的释放板/层压粘合剂子组件层压至PET/ITO/囊层子组件，其中层压粘合剂与囊层相接触。然后把得到的前平面层压(参见前述的美国专利6,982,178)切成2英寸(51mm)方形，去除释放板，且将层压粘合剂热辊层压至2英寸(51mm)方形的背板，该背板包括位于柔性聚合物板上的石墨电极。把适合的导电体连接至石墨和ITO电极以制造实验性单像素显示器。
采用15V、240毫秒的驱动脉冲测试如此制造的实验性显示器的电光性能。首先在深色和白色状态之间重复开关每个显示器，然后采用15V、240毫秒的驱动脉冲将其最终驱动至其深色和白色状态之一的状态。不施加驱动脉冲使该显示器保持在同一状态中2分钟(这2分钟的静止时间用以除掉出现在一些电泳显示器中的某些短时变化)，然后测量其反射率并将其转化成单位L*。附图中的图1示出了深色状态的结果，图2示出了白色状态的结果。在两个图中均提供了利用亚铬酸铜以相同方式制备的黑色颜料的比照显示器的结果以进行对比。
从图1和图2可以看出，本发明制造的两个颜料明显比现有的亚铬酸铜颜料的深色状态更深，同时白色状态的反射率仅稍有降低。因此，与基于亚铬酸铜的颜料的对比度(8:1)相比，本发明的显示器的对比度显著提高(基于Black 20C920的颜料的对比度为14:1，基于Black 444的颜料的对比度为20:1)。基于Black 444的颜料还具有提供无铬颜料的优点。
示例4：实验性显示器的深色状态与颜料颗粒尺寸的关系
从Shepherd Color公司获得每单位重量的表面积在一定范围内的一系列黑色颜料，且利用常规BET(氮气吸附)技术测量它们每单位重量的表面积。然后以与示例1至3中相同的方式把黑色颜料制作成实验性单像素显示器，且以与示例3中相同的方式测试显示器的深色状态。图3是深色状态对每单位重量的表面积的图(图3中的横坐标为平方米每克)。图3最左边的实验点为亚铬酸铜颗粒，接下来的两组是具有不同表面积的Black 20C920颗粒，剩下的组都是具有不同表面积的Black444颗粒。从图3中所示的线性回归线可以看出，增大的表面积与改善的深色状态(即，L*值较低)之间有很大关系，该关系看起来与颜料的化学性质基本无关，至少对于在这些实验中使用的金属氧化物颜料基本无关。

Claims (3)

1.一种用于制造涂布聚合物的颜料颗粒的方法，该方法包括：
(a)使表面积至少为约7m2/g的无机黑色颜料颗粒与试剂反应，该试剂具有能够与所述颗粒反应且键合所述颗粒的功能基团，且还具有可聚合的或聚合引发基团，由此使所述功能基团与所述颗粒的表面反应并使可聚合的基团与其相接附；以及
(b)在能有效引起所述颗粒上的可聚合的或聚合引发基团与至少一种单体或低聚物之间发生反应的条件下，使步骤(a)的产物与该至少一种单体或低聚物反应，由此形成键合至该颗粒的聚合物。
2.根据权利要求1的方法，其中用在步骤(a)中的试剂包括硅烷偶联基团。
3.根据权利要求2的方法，其中所述溶剂还包括氨基基团。
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