CN1673833A - 一种改良的透射式或反射式液晶显示器及其制作方法 - Google Patents
一种改良的透射式或反射式液晶显示器及其制作方法 Download PDFInfo
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Abstract
本发明涉及液晶(LC)显示器,这种显示器包括多个具有明确定义的形状、尺寸、和纵横比的盒,这些盒最好用含有二向色性染料的液晶组分填充。本发明还涉及制造上述液晶显示器的新颖方法。根据本发明的一种液晶显示器,包括多个显示盒,所述显示盒分别由一密封层密封,其中所述显示盒用液晶组分填充,并且所述密封层在原位硬化。根据本发明的一种制造液晶显示器的方法,所述方法包括用液晶组分填充显示盒以及用在原位硬化的密封层密封经过填充的显示盒。
Description
本申请是2001年10月31日提交的名称为“一种改良的透射式或反射式液晶显示器及其新颖的制作方法”的第01134412.1号专利申请的分案申请。
A)本发明所属技术领域
本发明涉及包括具有明确的形状、尺寸、和纵横比的盒的液晶显示器,该盒用液晶填充,优选采用客体染料填充;本发明还涉及液晶显示器的新颖制造方法。
B)背景技术
聚合物分散液晶(聚合物分散型薄膜)(PDLC)显示通常包括两个带有电极的透明平板,彼此相对放置并用隔离物分隔开。聚合物分散液晶薄膜被封装在两板之间。聚合物分散液晶薄膜可以达200微米厚,但通常其厚度是在2微米至50微米之间。盒是密封的,目的是消除氧气和湿气,氧气和湿气会对液晶造成化学侵蚀。聚合物分散液晶技术的详细述评见P.S.Drzaic的《液晶分散型》(1995)一书。
聚合物分散液晶通常由分散于聚合物粘合剂中的低分子量向列液晶的微米尺寸微滴组成。向列微滴强烈散射光,这种材料具有白色不透明或半透明的外观(“关断状态”)。当在两个电极之间施加电压差时(“接通状态”),电场使微粒排列,因而液晶的正常折射率几乎与各向同性聚合物基质的折射率一致,显著地减少了微粒的散射能力,使光线可以通过。在接通状态,盒因而显得明亮或透明;在关断状态,盒则不透明。
在客体-主体(guest-host)聚合物分散液晶显示器中,染料特别是多色性或二向色性的染料作为客体被加入液晶中,从而制成高色对比度的显示器。例如,由于这种染料分子具有与液晶分子平行排列的性能,如果一种具有棒形结构的二向色性染料加到液晶中,如果通过在相对的电极上施加电场改变液晶分子的方向,染料分子的方向也会改变。由于这种染料是用来着色或与排列方向无关,因而有可能通过在两个电极上施加电压来使着色状态(“关断状态”)和无色状态(“接通状态”)进行转换。本领域已知,在客体-主体聚合物分散液晶显示器中使用二向色性或多色性的染料可以改善对比度。
聚合物分散液晶显示器可以是透射式的和/或反射式的。透射式聚合物分散液晶显示器有一个内部照明光源。在两个电极施加电压使光线可以通过盒。透射式聚合物分散液晶显示器的一个典型例子是聚合物分散液晶顶部投影仪。反射式聚合物分散液晶显示器通常包括反射的黑色或着色的滤色片,其在透明状态会变得可见。在个人数字处理器(PDA)装置中可以发现反射式聚合物分散液晶显示器。由于无需用偏光镜,透射式和反射式聚合物分散液晶显示器特别具有吸引力。偏光镜显著地减少光线并降低直视式和投射式显示器的亮度。没有偏光镜还可提供更好的视角。
用在先技术制备的聚合物分散液晶显示器有许多缺点。例如:聚合物分散液晶中的微滴通常具有很宽的尺寸分布,这导致明显滞后、较高操作电压、对比度差、讨厌的红胶斑、和低水平的多路传输。然而,聚合物分散液晶薄膜的滞后必须较低以便显示可重复的灰度,并且对大多数个人数字处理器的应用而言,仪器的低电压操作和高对比度是基本要求。美国专利第5,835,174号(Clikeman等)、第5,976,405号(Clikeman等)、和第6,037,058号(Clikeman等),提示我们使用在微米尺度范围内单分散的液晶颗粒,以减少滞后和操作电压,并改善多路传输的水平。对大多数应用来说,用单分散颗粒制备的聚合物分散液晶装置的对比度仍然较低。为了改善对比度而不牺牲聚合物分散液晶薄膜的厚度和操作电压,需要客体染料,优选多向色性染料或二向色性染料。然而,现有技术的方法在制备过程不能够在液晶相精确封装入高浓度的客体染料,因而,在单分散聚合物颗粒中仅可以包结低浓度的染料。某些客体染料可能会留在颗粒的外边,因而导致Dmin(背景最小光密度)的增加和对比度降低。
人们非常希望产生单分散液晶域,这可以降低对高操作电压的要求、获得高对比度和高水平的多路传输、并减少滞后效应。
发明简述
本发明的第一个方面是关于液晶(LC)显示器,其包括形状、尺寸、和纵横比都基本相同的盒。这种盒优选采用含有客体染料的液晶填充。
本发明的另一个方面涉及制备这种液晶显示器的新颖方法。
本发明还涉及形状、尺寸、和纵横比基本相同的盒的制备。盒中封装优选含有客体染料的液晶,并由根据本发明制作的微型杯制成。简而言之,制备微型杯的方法涉及:用预成型凸模模压涂布于导电膜上的热塑性或热固性前体物层,接着在热塑性或热固性前体物层硬化之前、期间、或之后进行脱模,硬化是通过辐射、冷却、溶剂蒸发、或其他方法。另一方面,微型杯可用下述方法制成:图形曝光涂布有可辐射固化层的导电膜,然后在曝光区域硬化后去除未曝光区域。
用上述两种方法的任何一种方法都可以制备具有基本上单分散的尺寸和形状的耐溶和热机械稳定的微型杯。对大多数显示器应用而言,微型杯的尺寸范围是从亚微米至10微米,优选0.5微米至5微米。微型杯可以是任意形状,尽管优选使液晶和微型杯之间具有更大界面总面积的形状。然后用最好含有客体染料的液晶填充微型杯并密封。
本发明的另一个方面涉及到对填充有液晶的微型杯进行密封,优选为含有客体染料的液晶。可以用多种方法进行密封,优选的方法是,在填充步骤之前,把含有热塑性或热固性前体物的密封剂组分在液晶相分散。密封剂组分与液晶不互溶并具有比液晶更低的比重。填充后,热塑性或热固性前体物发生相分离,并在液晶的上面形成表面浮层。于是通过硬化前体物层可以方便地完成微型杯的密封,前体物层的硬化可以利用溶剂蒸发、界面反应、湿气、热、或辐射完成。虽然上述两种或更多固化机理的结合可用来增加密封生产量,但是紫外光(UV)辐射是密封微型杯的优选方法。可选地,用含有热塑性或热固性前体物的密封剂组分涂布液晶也可以密封微型杯。在密封剂组分中使用的溶剂很关键。溶剂最好与液晶不互溶并且比重较液晶低。为了保证良好的涂布均匀性,控制表面张力和密封剂组分的粘度也很重要。然后通过硬化密封剂组分来完成密封,硬化则是通过溶剂蒸发、界面反应、湿气、热、辐射、或固化机理的结合来完成。这些密封方法也是本发明的特征。
本发明的另一个方面是液晶显示没有滞后现象。本发明的液晶显示器件由基本上单分散的微型杯组成,该微型杯中填充有液晶并优选地填充有客体染料。对微型杯的组分进行了优化,这样微型杯的各向同性折射率与液晶的一般折射率相匹配。以一种与传统聚合物分散液晶显示器相似的方式,本发明的液晶显示器在没有电场(“关断状态”)时强烈散射光线。当在两个电极之间施加电压差时,电场排列液晶并在相当程度上降低其散射能力,从而允许光线通过“接通状态”透射。然而,与聚合物分散液晶不同的是,本发明的液晶显示在低得多的电压下达到最大光学上清亮状态,当停止施加电压时会回复到起始的“断路”状态而没有不希望的滞后。对于迫切需要的低电耗、可重复灰度和视频率,本发明的低操作电压、快速响应时间、和无滞后的显示器对高质量显示器应用是关键的。
本发明的另一个方面涉及由多层微型杯叠加构成的液晶显示器的制备。该方法步骤包括:用上述任何一种方法在导电基片上制备第一层微型杯,用液晶组分填充微型杯,密封,最后用预涂有粘合剂层的第二导电基片来层叠密封的微型杯。粘合剂可以是热熔粘合剂、加热固化粘合剂、湿气固化粘合剂、或辐射固化粘合剂。特别令人感兴趣的是在本发明中使用了紫外光固化粘合剂。为改善对比度,可使用一层以上的微型杯阵列。该方法步骤包括:制备微型杯,用液晶组分填充,密封,用第二层微型杯形成组分涂布或层叠密封的微型杯阵列,用以前描述的任何一种方法(优选模压法)成形第二个微型杯阵列;重复若干次下述步骤,即微型杯的填充和密封,用另一层微型杯形成组分涂布或层叠密封的微型杯,最后在几层微型杯上层叠预涂有粘合剂层的第二导电基片。制备微型杯用的预成型的凸模是在热塑性或热固性前体物层硬化以前、期间、或之后进行脱模
本发明的另一个方面涉及利用预涂有(红,绿,蓝)滤色片和优选黑色基片的导电基片来制备全色反射式液晶显示器的方法。可选地,全色显示器可用下述步骤制备:用一层正性光致抗蚀剂层叠在预成形的微型杯上,通过图形曝光正性光致抗蚀剂来选择性地打开一定数目的微型杯,然后显影所述抗蚀膜,用含有客体染料(优选第一色的二向色性染料)的液晶组分填充打开的微型杯,用前述密封方法密封已填充的微型杯。这些步骤可以重复进行,以制成填充含有第二或第三色客体染料的液晶组分的密封的微型杯。可用黑色衬底来改善对比度和色彩饱和度。
这些披露的多步骤方法,可以辊对辊连续或半连续地进行。因而它们适合于大批量和低成本生产。与其它大规模生产过程比较而言,这些生产方法也是高效和低成本的。依据本发明制备的液晶显示器对环境不敏感,特别是对湿度和温度不敏感。这种显示器可以很薄、柔性、耐用、易于操作、和款式多样化。因为依据本发明制备的液晶显示器包括多个具有令人满意的纵横比和基本单分散的形状和尺寸的盒,所以依据本发明制成的显示器表现出许多理想的性能,如低电能消耗、快速响应时间、高水平的多路传输、高对比度、以及由于没有不希望的滞后而具有可重复的灰度。
根据本发明的液晶显示器,其中的盒由开口面积约1至约25平方微米的微型杯制成;盒的深度约0.5至约10微米;盒的开口与壁的比例为约0.2到约9;制造过程中所用的热塑性或热固性前体物层的玻璃化温度范围是从约-20℃至约100℃。本发明中的热固性或热塑性前体物材料选自:丙烯酸酯,甲基丙烯酸酯,乙烯基化合物,多价的丙烯酸酯,多价的甲基丙烯酸酯,氰基丙烯酸酯,多价的乙烯基化合物,多价的环氧化物,多价的异氰酸酯,多价的丙烯基化合物,及其衍生的低聚物或聚合物
附图简要描述
图1a、1b分别显示典型的聚合物分散液晶装置的“关断”和“接通”状态。
图1c、1d和1e是本发明的液晶显示器的示意图。
图2a-2d说明一种制备微模压凸模的典型方法。
图3a-3b表示制造液晶显示器的辊对辊方法,特别是通过模压涂有紫外光固化组分的导电膜从而形成微型杯。
图4a-4b显示用微模压制成的微型杯阵列的两张扫描电镜(SEM)显微照片。
图5a1、5a2、5b1、5b2、5c1和5c2是制备微型杯的可选方法步骤,涉及用紫外光辐射对涂有热固性前体物的导电膜进行图形曝光。
图6a至6f示意不同形状和图案的微型杯阵列的例子。
图7是制备单色液晶显示器的流程图。
图8a至8h示意用三原色客体染料制备全彩显示器的方法。
图9a是传统的聚合物分散液晶装置的典型滞后曲线。
图9b显示本发明的典型微型杯液晶显示器中没有滞后回线。
发明详述
定义
除非在本专利说明书中另有定义,否则在此所用的技术术语皆根据本专业技术人员通常使用并理解的惯用定义而被使用。
“微型杯(microcup)”一词,是指由微模压或图形曝光所生成的杯状的凹处。
在本专利说明书中,术语“盒”是指由一密封微型杯所形成的独立的单元。这些盒以优选含有客体染料的液晶填充。
当说明该微型杯或盒时,术语“有明确定义的”是指该微型杯或盒具有根据本制造方法的特定参数预定的明确的形状、尺寸、和纵横比。
当说明该微型杯或盒时,术语“单分散的”是指所述微型杯或盒具有窄的尺寸分布,如直径、长度、宽度、和高度。
“纵横比”一词为聚合物分散液晶显示器中一般所知的词汇。在本申请中,它是指微型杯的深度对宽度或深度对长度的比例。
优选实施例
如图1a所示,典型的聚合物分散液晶显示器包括二个电极板(10,11),至少其中一个为透明的电极(10),和一层分散于各向同性聚合物基质中的液晶域。图1a还表明,当在两个电极板(10,11)上未施加电压(13)时,液晶分子随机排列。因液晶分子的无规则排列使入射光(14)形成散射光(15)。
图1b表明,当在两个电极板上施加电压(13)时,液晶分子按一定方向排列。入射光(16)因而可以形成透射光(17),因为液晶通常的折射率与聚合物基质(12)的各向同性的折射率相匹配。
如图1c所示,本发明的单色液晶显示器包括封装在二个电极(10,11)之间的有明确定义的盒(18)。这些盒有基本相同的形状和尺寸,并以液晶组分填充。在观察者一侧的电极是透明的,该二电极至少有一个是图案化的。如使用(图1d)三原色滤色片(19),如红(R)、绿(G)、和蓝(B)则可获得全范围的颜色。
可选地,以分别含有红、绿、和蓝客体染料(优选二向色性染料)的液晶组分填充有明确定义的盒(1,2,和3),则可以获得根据本发明的全色显示器。例如,以含有红色客体染料的液晶填充盒(1),以含有绿色客体染料的液晶填充相邻的盒(2),以含有蓝色客体染料的液晶填充相邻的盒(3)。装有液晶的盒的层数可以多于一层(图1e)。
用于制备这种液晶显示器的方法涉及几个方面。
I.
微型杯的制备
(a)凸模的制备
可以先用光刻法,接着采用蚀刻或电镀的方法制备凸模。制作凸模的代表性实施例见图2a至2d。采用电镀法时(图2a),在一玻璃基片(20)上喷镀一薄层通常为3000的籽金属(21),例如铬镍铁合金(chrome inconel)。接着涂布一层光致抗蚀剂(22),并以紫外光曝光。一掩模(24)被置于紫外光与光致抗蚀剂层(22)之间。该光致抗蚀剂的曝光区域变硬。然后用适当的溶剂清洗,去除未曝光区域。干燥保留的硬化光致抗蚀剂,并再次喷镀一薄层籽金属。然后主模(图2b)准备就绪,可以进行电铸成形。用于电铸成形的典型材料是镍钴合金(23)。此外,该主模可由镍制作,如摄影光学仪器工程师学会会刊卷1663,pp.324(1992)中《薄镀层光学介质的连续制作》(“Continuous manufacturing of thin cover sheetoptical media”,SPIE Proc.)中说明的,采用氨基磺酸镍(nickelsulfamate)电镀或无电镍沉积。该模具的底板(图2d)通常为1至5微米。该主模也可用其他微工程技术制作,包括电子束写入、干式蚀剂、化学蚀剂、激光写入或激光干涉,如摄影光学仪器工程师学会会刊《精密光学复制技术》(“Replicatio techniques formicro-optics”,SPIE Proc.)卷3099,pp.76-82(1997)中说明。此外,该模具可使用塑料、陶瓷、或金属,利用光加工制作。
(b)模压制作微型杯
该方法步骤如图3a和3b所示。凸模(30)可置于支撑网(web)(34)之上(图3a)或支撑网之下(图3b)。在玻璃平板或塑性基片上形成一透明导电膜(31),制成透明导电基片。然后在该导电膜上涂布一层热塑性或热固性前体物(32)。在高于热塑性或热固性前体物层的玻璃化温度条件下,用辊、板、或带凸模对该热塑性或热固性前体物层进行模压。
用于制备微型杯(33)的热塑性或热固性前体物(32),可以是多价的丙烯酸酯、或甲基丙烯酸酯、多价的乙烯基化合物(例如乙烯基苯、乙烯基硅烷、和乙烯醚)、多价的丙烯基化合物,以及包括可交联官能团的低聚物、聚合物、环氧化物以及其低聚物、聚合物、和类似物,该低聚物或聚合物是含有可交联官能团的低聚物或聚合物的衍生物。优选的是多价的丙烯酸酯及其低聚物。多价的环氧化物与多价的丙烯酸酯的组合也非常有利于获得所需要的物理机械性能。通常,也添加赋予挠性的可交联低聚物,例如氨基甲酸乙酯丙烯酸酯或聚酯丙烯酸酯,以改善模压微型杯的抗弯曲性。该组分可以包括聚合物、低聚物、单体和添加剂,或者只有低聚物、单体、和添加剂。这类材料的玻璃化温度(Tg)范围通常为约-70℃至约150℃,优选为约-20℃至50℃。微模压方法通常是在高于玻璃化温度下进行。可以采用加热凸模,或加热模子基板,以控制微模压的温度和压力。
如图3a和3b所示,在前体物层硬化期间或硬化后脱模,显露微型杯(33)阵列。用冷却、辐射交联、热、或湿气可使前体物层硬化。如果用紫外光辐射来固化热固性前体物,紫外光则可以从支撑网(34)的底部或顶部辐射到透明导电膜上,如上述两图所示。此外,紫外光灯可置于模子内部。在这种情况下,模子必须是透明的,从而允许紫外光通过预图案化的凸模辐射到热固性前体物层上。
图4a和4b是通过微模压制备的两个微型杯阵列的扫描电镜显微照片。
(c)用图形曝光方法制备微型杯
此外,通过一掩模(50),用紫外光或其他形式的辐射把涂布于导电膜(52)上的辐射固化材料(51)图形曝光(图5a),也可以制备微型杯。导电膜(52)在塑料基片(53)上。
对辊对辊方法来说,光掩模可与支撑网同步,以与后者相同的速度移动。在图5a的光掩模(50)中,深色方块(54)表示不透明区域,深色方块之间的间隔(55)是开口区域。紫外光通过开口区域(55)辐射到辐射固化材料上。曝光区域变硬,然后用适当的溶剂或显影剂除去未曝光区域(由该掩模的不透明区域加以保护),从而形成微型杯(56)。该溶剂或显影剂选自那些通常用来溶解或分散辐射可固化材料的溶剂,如丁酮、甲苯、丙酮、异丙醇、或其类似物。
图5b和5c图示了用图形曝光制作微型杯的两种其他可选方法。此二图特点基本与图5a所示特点一样,并且相应部分采用了同样的编号。在图5b中,使用的导电膜(52)是不透明和预图案化的。在这种情况下,有利于通过导电膜图形对辐射敏感材料进行图形曝光,其中该导电膜图形用作光掩模。在紫外光辐射后除去未曝光区域则可制得微型杯(56)。在图5c中,导电膜(52)也是不透明和区带-图案化的。透过导电膜区带-图案(52),从底部对辐射固化材料进行曝光,其中导电膜区带-图案作为第一个光掩模。通过第二个光掩模(50)从另一边进行二次曝光,第二光掩模具有与导电膜区带垂直的区带图案。然后用溶剂或显影剂除去未曝光区域从而显露出微型杯(56)。
一般来说,微型杯(56)可以是使液晶域光散射效果最大化的任何形状。在一个系统中的微型杯具有基本相同的尺寸和形状。然而,不同形状和尺寸的微型杯可用于不同颜色。例如,用含有红色客体染料的液晶所填充的微型杯可以与绿色微型杯或蓝色微型杯具有不同的形状或尺寸。而且,一个像素可以包括具有不同颜色的不同数目的微型杯。此外,一个像素可以包括一些较小的绿色微型杯、一些较大的红色微型杯、和一些较小的蓝色微型杯。对这三种颜色来说,没有必要具有相同的形状和数目。图6a至6f说明了可用于本发明的6种微型杯图案的实例。
微型杯的开口可以是圆形、正方形、长方形、六边形、或任何其他形状。开口之间的分隔面积最好要保持较小,以便在保持理想的机械性能的同时获得高颜色饱和度和高对比度。
对于本发明的液晶显示器来说,单个微型杯的尺寸范围可以是从大约0.04至大约100平方微米,优选是从大约0.6至大约36平方微米。微型杯的深度范围是大约1至大约10微米,优选是从大约2至大约6微米。开口对壁的比例范围大约为0.05至大约20,优选为大约0.2至10微米。开口边缘到边缘的距离范围通常是大约0.5至6微米,优选为大约1至大约4微米。
II.
液晶、二向色性染料及其混合物
通常采用涂布方法,以液晶填充这样形成的微型杯阵列。液晶中还可以含有二向色性染料以便赋予该显示器单色并增加对比度。
现有技术已知可用于本发明的液晶材料。可用于本发明的液晶材料实施例非限定性地包括来自德国E.Merck公司的E7、TL205、TL213、BL006、BL009、和BL037。其他液晶材料列于美国专利第5,835,174中(Clikeman等)。在某些应用中也可以使用胆甾液晶。
本发明中的液晶优选含有客体染料。本发明的客体染料是二向色性染料,并为本技术领域所熟知。美国专利第5,589,100号(Grasso等)指出偶氮芳基(arylazo)或聚偶氮芳基二向色性染料可与液晶一起使用,并列举了适用于本发明的其他二向色性染料。
加入染料不仅是添加了颜色,而且也相当程度上对一些显示器应用改善了对比度。为了适用,染料必须具有高的序参量和在主体液晶材料中的适当可溶性。具有较大的分子长度对宽度比例、以及类似于液晶主体材料分子形状的长形染料促进了高有序参量。含有客体染料的液晶会提供良好的视觉特性,如高对比度、高消光性,以及化学和光化学稳定性。在本发明中使用的具有高二向色性比率的二向色性染料的实施例包括德国Funktionfluid Gmb公司的蓝AB2、红AR1和黄AG1,以及Mitsui Toatsu公司的SI-486(黄色)、SI426(红色)、M483(蓝色)、S344(黑色)、S428(黑色)和S7(黑色)。
非离子偶氮和蒽醌染料也很用。实施例非限定性地包括:亚利桑那州Pylam Products公司的油溶红EGN(Oil Red EGN)、苏丹红(Sudan Red)、苏丹蓝(Sudan Blue)、油溶蓝(Oil Blue)、Macrolex蓝、溶剂蓝35(Solvent Blue 35)、Pylam Spirit黑、和Fast Spirit黑,Aldrich公司的苏丹黑B(Sudan Black B),BASF公司的Thermoplastic黑X-70,以及Aldrich公司的蒽醌蓝、蒽醌黄114,蒽醌红111、135,蒽醌绿28。任何情况下,在微型杯材料中染料必须是化学稳定的、并应该具有低溶解度。液晶或染料在任何时候都不应侵蚀微型杯。
III.
微型杯的密封
微型杯的密封可用多种方法完成。一种优选的方法是将紫外光固化密封剂组分分散于液晶组分中。该紫外光固化组分与液晶不互溶,且具有比液晶低的比重。紫外光固化组分与液晶组分在径向混合器中被完全混合,并采用如Myrad棒、凹印板、刮刀片、开槽涂布或开缝涂布等精确的涂布机械装置,立即涂布于该微型杯上。挥发性的溶剂可用于控制粘度、涂层的覆盖厚度,并便于密封剂相从液晶相中分离出来。可用扫杆刮刀或类似的装置将过量的流体刮除。接着烘干填充的微型杯,该紫外光固化组分浮在液晶的顶部。在紫外光固化层浮到表面期间或之后,将其进行固化(原位硬化),密封微型杯。紫外光或其他辐射形式,如可见光、红外线、及电子束等,皆可用于将该微型杯固化和密封。可选地,当使用热或湿气固化密封剂组分时,也可使用热、或湿气、或其组合方式将该微型杯固化并密封。
可用表面活性剂改善密封剂与微型杯壁的粘合性以及改善液晶与密封材料之间界面的润湿性。有用的表面活性剂包括3M公司的FC表面活性剂、DuPont公司的Zonyl氟化表面活性剂、氟化丙烯酸酯、氟化甲基丙烯酸酯、氟代长链醇类、全氟取代的长链羧酸及其衍生物、和Osi公司的Silwet表面活性剂。
可选地,可将液晶和密封剂组分依次涂布于微型杯。这样,可通过涂布一层热塑性或热固性前体物组分薄层(该前体物组分是辐射、热、湿气或界面反应可固化的),并将其固化于经填充的微型杯表面上,以完成此密封过程。界面聚合后进行紫外光固化,对于密封过程极为有利。通过界面聚合形成一个薄的分隔层,使液晶层和外涂布层之间的互相混合明显得到抑制。接着通过后固化步骤完成密封,优选为紫外光辐射。为进一步降低互混程度,最好外涂布层的比重低于液晶的比重。可用挥发性有机溶剂调整涂层的粘度和厚度。当挥发性溶剂用于外涂布层时,优选为与该液晶或该染料不相混溶,并且其比重低于液晶相的比重。这种二步涂布方法,对所用染料至少部分地溶解于密封剂层的情形特别适用。为进一步降低密封剂层和液晶相的互混程度,在涂布密封剂层之前,可以对经填充的微型杯阵列进行急冷降温。
可选地,从一剥离基片转移层叠一粘合剂层到经填充的微型杯上,最好接着用热、辐射、或简单的溶剂蒸发来硬化粘合剂层,最后去掉剥离基片,从而完成微型杯的密封。急冷降温经填充的微型杯也有利于用转移层叠方法进行的密封过程。
IV.
单色液晶显示器的制备
通过图7所示的流程图说明此方法。所有的微型杯都用含有相同颜色客体染料的液晶填充。该方法可为连续的辊对辊方法,包括如下步骤:
1.在一透明导电膜(71)上涂布一层热塑性或热固性前体物(70),非必选地带有溶剂。如有溶剂的话,溶剂应容易蒸发。
2.在温度高于热固性前体物层玻璃化温度的条件下,用预成形的凸模(72)模压热塑性或热固性前体物层。
3.从热塑性或热固性前体物层脱模,优选在热塑性或热固性前体物层以适当方式硬化期间或之后进行。
4.用含有热固性前体物组分的液晶组分(74)填充上述方法制成的微型杯阵列(73),该热固性前体物组分与液晶不相容并且比液晶相的比重低。
5.在该热固性前体物分离并在该液晶相上面形成一表面浮层期间或之后,通过将该热固性前体物硬化密封微型杯,优选采用溶剂蒸发、辐射例如紫外光(75)、或热或湿气,而形成包括有液晶和优选客体染料的密封液晶盒。
6.将预涂布有粘合剂层(77)的第二导电膜(76)层叠在经密封的液晶盒阵列上,其中所述粘合剂层(77)可为压敏粘合剂、热熔粘合剂、热、湿气、或辐射固化粘合剂。
可以用加热或辐射如紫外光(78),通过该顶部导电膜对粘合剂层进行硬化(如果该顶部导电膜对这类辐射是透明的)。层叠后的产品可被切割(79)到适当的尺寸,用于装置的组装。
上述微型杯的制备可以方便地以另一种图形曝光制造的工序取代,即对涂布有热固性前体物的导电膜进行图形曝光,接着用一种适当的溶剂除去未曝光区域。可通过前述的涂布或转移涂层的方法,接着硬化经填充的微型杯表面上的密封剂,从而完成对微型杯的密封。
为改善对比度,可使用一层以上的微型杯阵列(图1c)。因而,在经填充的微型杯上的密封层硬化后(步骤5),把另一层微型杯形成组分涂布在该密封的微型杯阵列上。步骤2至5可重复几次直到获得适合的对比度。然后用第二导电层层叠于该多层微型杯,并切割为适当的尺寸以用于显示器组装。重要的是要注意到两层导电膜中至少有一层是预图案化的。而且至少在观察者一侧的导电膜是透明的。
V.
多色液晶显示器的制备
本发明的多色液晶显示器可以利用(红,绿,蓝)滤色片和一种黑色基质制作而成,该黑色质体置于在前节制作的单色显示器的下面(图1d)。可选地,本发明的全彩显示器可通过用含有不同颜色客体染料的液晶填充微型杯制成(图1e)。除了在制作单色显示器时所描述的方法外,需要额外的步骤来制备这样的彩色显示器。这些额外的步骤包括:(1)将一种正性作用干膜光致抗蚀剂层叠在制成的微型杯上,该光致抗蚀剂由以下成分组成:至少一种可去除支撑膜(如马萨诸塞州Worcester的Saint-Gobain公司所生产的PET-4851),酚醛树脂正性光致抗蚀剂(如Shipley公司的MicropositS1818),以及一种碱性显影粘合剂层(如National Starch公司的Nacor72-8685与BF Goodrich公司的Carboset 515的混合物);(2)通过将光致抗蚀剂进行图形曝光,除去可去除支撑膜,并用一种显影剂,如Shipley公司的经稀释的Microposit 351显影剂,将该正性光致抗蚀剂显影,从而选择性地打开一定数目的微型杯;(3)用包括第一原色客体染料的液晶填充打开的微型杯;以及(4)按照单色显示器制备中说明的方法,将经填充的微型杯密封。这些额外的步骤可以重复,以形成用第二和第三原色的液晶填充的微型杯。
更特别地,可根据图8所示步骤制备一种多色液晶显示器。
1.在导电膜(81)上涂布一层热固性前体物(80)。
2.在温度高于其玻璃化温度的条件下,用预成形凸模(图中未示出)模压该热塑性或热固性前体物层。
3.优选在热塑性或热固性前体物层通过溶剂蒸发、冷却、辐射、热、或湿气交联硬化期间或之后,将该凸模从该热塑性或热固性前体物层脱模。
4.在这样制成的微型杯阵列(82)上层叠一正性干膜光致抗蚀剂,其中至少包括一种正性光致抗蚀剂(84),以及一种可去除的塑料保护片(图中未示出)。该正性干膜光致抗蚀剂可包括一粘合剂层(83),以改善微型杯和该光致抗蚀剂之间的粘合性。
5.用紫外光、可见光或其他辐射将该正性光致抗蚀剂进行图形曝光(图8c),除去保护片,在曝光区域显影并打开微型杯。步骤4和5的目的是在一预定区域选择性地打开一些微型杯(图8d)。
6.用液晶组分填充打开的微型杯,该液晶组分包括第一原色的客体染料(85)以及与该液晶相不相容的密封剂组分(86),并且该密封剂组分比该液晶相比重低。
7.在密封剂分离并在液晶相上面形成一表面浮层的期间或之后,采用溶剂蒸发,或优选紫外光辐射、较好为热或湿气固化方法硬化密封剂层,密封微型杯,以形成包括第一原色客体染料的液晶的封闭液晶盒(图8e)。
8.可以重复上述步骤5至7,以便在不同区域产生包括不同颜色客体染料的液晶的有明确定义的盒(图8e,8f和8g)。
9.将预涂布有粘合剂层(88)的一第二透明导电膜(87),层叠在密封的液晶盒阵列上,其中所述粘合剂层可为压敏粘合剂、热熔粘合剂、或一种热、湿气、或辐射固化粘合剂。
10.硬化粘合剂。
上述方法中的微型杯的制备,可以方便地以另一种工序取代:图形曝光涂布有热固性前体物的导电膜,接着用一种适当的溶剂去除未曝光区域。另外,可通过在液晶相表面直接涂布并固化热固性前体物组分层,完成对微型杯的密封。
用本方法制造的显示器可以达到仅一张纸的厚度。该显示器的宽度为涂布支撑网的宽度(通常为3至90英寸)。该显示器的长度可为任意长,可以从几英寸至几千英尺,取决于卷的大小。
实施例
以下所描述的实施例,是为便于本领域技术人员能够更清楚地了解并实践本发明。这些实施例不应理解为是对本发明范围的限制,而仅仅是对本发明的说明和示范。
实施例1
用微模压方法制备微型杯
将表1所示组分用Myrad棒#6涂布到预涂有Sheldahl公司(Northfield,MN)的ITO导电膜层的2密尔(千分之一英寸)PET膜上。一预成形(4×4×4微米)镍钴合金凸模和来自Henkel公司的脱模Frekote700-NC用于微模压。涂布厚度控制在约5微米。然后在90℃下,借助于一个压力辊,用模版模压涂布膜。采用有金属氟灯的固化区带曝光装置(自ADAC Technologies公司),在365纳米光强度为80毫瓦/平方厘米,通过聚酯树脂薄膜,对涂层进行紫外光固化约1分钟。模压后的薄膜从膜具上脱模,显露出有明确定义(4×4×4微米)的微型杯。微模压成形是在90℃下用GBC层压机完成的。
表1:用于制造微型杯的紫外光固化丙烯酸酯配方
编号 | 说明 | 成分 | 供货商 | 份数 |
1 | 环氧丙烯酸酯 | Ebecryl 600 | UCBChemicals | 55 |
2 | 聚酯丙烯酸酯 | Ebecryl 830 | UCBChemicals | 15 |
3 | 氨基甲酸乙酯丙烯酸酯 | Ebecryl 6700 | UCBChemicals | 10 |
4 | 硅丙烯酸酯 | Ebecryl 350 | UCBChemicals | 5 |
5 | 单体 | SartomerSR238 | Sartomer | 10 |
6 | 单体 | SartomerSR306 | Sartomer | 5 |
7 | 单体 | SartomerSR351 | Sartomer | 5 |
8 | 光引发剂 | Irgacure 500 | Ciba | 1 |
9 | 增强剂 | 甲基二乙醇胺 | Aldrich | 0.5 |
10 | 溶剂 | 丁酮 | Aldrich | 100 |
实施例2
用微模压方法制备微型杯
与实施例1相同,不同之处是采用表2配方进行涂布,用4×4×4微米的凸模进行模压。
表2:用于制造微型杯的紫外光固化丙烯酸酯配方
编号 | 说明 | 成分 | 供货商 | 份数 |
1 | 环氧丙烯酸酯 | Ebecryl 600 | UCB Chemicals | 50 |
2 | 聚酯丙烯酸酯 | Ebecryl 830 | UCB Chemicals | 15 |
3 | 氨基甲酸乙酯丙烯酸酯 | Ebecryl 6700 | UCB Chemicals | 10 |
4 | 硅丙烯酸酯 | Ebecryl 350 | UCB Chemicals | 5 |
5 | 单体 | 聚(乙二醇)甲基丙烯酸酯 | Aldrich | 5 |
6 | 单体 | Sartomer SR238 | Sartomer | 5 |
7 | 单体 | Sartomer SR306 | Sartomer | 5 |
8 | 单体 | Sartomer SR351 | Sartomer | 5 |
9 | 光引发剂 | Irgacure 907 | Ciba | 0.5 |
10 | 溶剂 | 丁酮 | Aldrich | 300 |
使用Myrad棒#12。控制厚度为5微米。用加热到90℃的压力辊(GBC层压机)进行微模压。
实施例3
用微模压方法制备微型杯
将表3所示的组分用压力辊层叠在一个预涂有ITO导电层的2密尔PET膜和预成形(4×4×4微米)镍钴合金模具之间。用电晕放电装置(Electro-Technic Products公司,型号BD-10A,Chicago,IL)处理PET/ITO膜5秒钟。用Frekote 750-NC脱模剂对镍钴合金模具进行预处理。透过PET/ITO膜,用紫外光固化涂层1分钟。然后将该模压膜从模具上脱模,显露出有明确定义的(4×4×4微米),厚度为5.5微米的微型杯,其中厚度的测量是采用Mituyoto厚度规。
表3:用于制造微型杯的紫外光固化丙烯酸酯配方
编号 | 说明 | 成分 | 供货商 | 份数 |
1 | 环氧丙烯酸酯 | Ebecryl 600 | UCB Chemicals | 40 |
2 | 聚酯丙烯酸酯 | Ebecryl 830 | UCB Chemicals | 15 |
3 | 氨基甲酸乙酯丙烯酸酯 | Ebecryl 6700 | UCB Chemicals | 10 |
4 | 硅丙烯酸酯 | Ebecryl 350 | UCB Chemicals | 5 |
5 | 单体 | 聚(乙二醇)甲基丙烯酸酯 | Aldrich | 15 |
6 | 单体 | Sartomer SR238 | Sartomer | 5 |
7 | 单体 | Sartomer SR306 | Sartomer | 5 |
8 | 单体 | Sartomer SR351 | Sartomer | 5 |
9 | 光引发剂 | Irgacure 907 | Ciba | 0.5 |
实施例4
用液晶溶液填充的微型杯的制备
先用己烷、然后用丁酮冲洗在实施例3中制成的微型杯,接着在烘箱(66℃)中干燥10分钟。含有1%(重量百分比)Silwet L7608(自Osi Specialties公司)的液晶BL006(自德国E.Merck公司)与9倍体积的戊酮进行混合,用Myrad棒#16把所形成的溶液涂布于微型杯上。在烘箱(66℃)中蒸发10分钟微型杯中多余的溶剂。
实施例5
用含有蓝色二向色性染料的液晶溶液填充的微型杯的制备
先用己烷、然后用丁酮冲洗在实施例3中制成的微型杯,接着在烘箱(66℃)中干燥10分钟。含有3%(重量百分比)二向色性染料蓝AB2(自德国Funktionfluid Gmb公司)和1%(重量百分比)Silwet L7608(自Osi Specialties公司)的液晶BL006(自德国E.Merck公司)与9倍体积的戊酮(MPK)进行混合,用#16号Myrad棒把形成的溶液涂布在微型杯上。在烘箱(66℃)中蒸发10分钟微型杯中多余的溶剂。
实施例6
用含有黑色二向色性染料混合物的液晶溶液填充的微型杯的制备
先用己烷、然后用丁酮(MEK)冲洗在实施例3中制成的微型杯,接着在烘箱(66℃)中干燥10分钟。把三种二向色性染料蓝AB2、红AR1和黄AG1(来自德国Funktionfluid Gmb公司)混合在一起,制成一种黑色二向色性染料混合物。把含有2%(重量百分比)黑色二向色性染料混合物和1%(重量百分比)Silwet L7608(自Osi Specialties公司)的液晶BL006(自德国E.Merck公司)溶液与9倍体积的戊酮进行混合,用Myrad棒#16把形成的溶液涂布于微型杯上。在烘箱(66℃)中蒸发微型杯中多余的溶剂10分钟。
实施例7
用二步(涂布)方法密封微型杯
用10%的Vistalon 0106(来自Exxon Mobil Chemicals公司)Isopar E(来自Exxon Chemicals公司)溶液涂布在实施例4、5和6制备的BL006填充的微型杯上。该涂层是均匀和透明的。使用一#3Myrad棒,获得密封聚合物层重量为0.39毫克/平方英寸,厚度估计为0.7微米。使用#8号Myrad棒,获得密封聚合物层重量为0.75毫克/平方英寸,厚度估计为1.3微米。Vistalon 0106的密度约为0.9克/立方厘米。
实施例8
用二步(涂布)方法密封微型杯
按照实施例7相同的步骤,用Amphomer28-4910(来自NationalStarch公司的一种羰酸酯(或盐)丙烯酸共聚物,在2-丙醇中的10%溶液涂布于依据实施例5制备的BL006填充的微型杯上,从而密封该微型杯。该涂层是均匀和透明的。使用一种#3 Myrad棒,获得密封聚合物层,重量为0.44毫克/平方英寸,厚度估计为0.6微米。使用#8号Myrad棒,获得密封聚合物层重量为1.0毫克/平方英寸,该密封聚合物层的厚度估计为1.3微米。Amphomer 28-4910的密度约为1.2克/立方厘米。
实施例9
传统聚合作用引起的相分离聚合物分散液晶显示器
为比较目的,制备了传统聚合作用引起的相分离聚合物分散液晶显示器。用不同比例的液晶E7(来自德国E.Merck公司)与Norland65(来自Norland公司)进行混合,并把混合物夹在两层ITO涂层玻璃板之间,间隔物分别为4.5微米、25微米、或50微米。采用步进式光楔优化使用固化区带曝光装置(自ADAC Technologies公司)的紫外光固化时间。图9a是按上述程序制备的聚合作用引起的相分离聚合物分散液晶显示器的典型滞后曲线。
实施例10
SIPix无滞后液晶显示器
用实施例1、2或3制备的微型杯来组装单层液晶显示器。依据在实施例4、5和6的步骤,用含有或不含有二向色性染料的液晶填充微型杯。然后依据实施例7或8的步骤,密封这些液晶填充的微型杯。依据本发明制备的液晶显示器看不到滞后(见图9b)。
实施例11
多层显示器的组装及其性能
组装多层液晶显示器以改进显示器的性能。依实施例10所述方法制备单层液晶显示器。以相同的步骤,在第一层液晶显示器的顶部模压第二层微型杯,用含有或不含有染料的液晶进行填充,并密封第二层液晶显示器。在第一层微型杯上对正第二层微型杯时,第二层微型杯偏离第一层微型杯约0至10度,以使光散射能力最大。层叠两个双层阵列从而叠合成四层液晶显示器。得到一高对比度显示器,该显示器分别具有~1msec和~10msec(在40伏时)的增强和衰减响应时间。未观察到任何滞后回线。
Claims (21)
1.一种液晶显示器,包括多个显示盒,所述显示盒分别由一密封层密封,其中所述显示盒用液晶组分填充,并且所述密封层在原位硬化。
2.根据权利要求1所述的液晶显示器,其中所述密封层由一密封组分形成,所述密封组分的比重低于所述液晶组分的比重。
3.根据权利要求1所述的液晶显示器,其中所述显示盒具有基本相同的尺寸和形状。
4.根据权利要求1所述的液晶显示器,其中所述盒是非球形的。
5.根据权利要求1所述的液晶显示器,其中所述显示盒由开口为圆形,多边形,六边形,矩形的或者正方形的微型杯制成。
6.根据权利要求1所述的液晶显示器,其中在预定区域中的所述显示盒用含有预定颜色的客体染料的液晶组分填充。
7.根据权利要求6所述的液晶显示器,其中所述的用含有预定颜色的客体染料的液晶组分填充的盒彼此相邻。
8.根据权利要求6所述的液晶显示器,其中所述的用含有预定颜色客体染料的液晶组分填充的显示盒在彼此的顶部层叠。
9.根据权利要求1所述的液晶显示器,其中所述的液晶组分用一种客体染料着色。
10.根据权利要求9所述的液晶显示器,其中所述客体染料是一种减色或加色体系。
11.根据权利要求1所述的液晶显示器,其中所述显示器包括一层以上的填充有液晶组分的微型杯阵列。
12.根据权利要求1所述的液晶显示器,其中所述显示器是多彩的并且滤色片层叠或涂布于所述显示器上。
13.根据权利要求12所述的液晶显示器,其中所述滤色片是红色,绿色,和蓝色滤色片。
14.根据权利要求1所述的液晶显示器,其中所述液晶组分被部分地填充在所述显示盒的每一个中。
15.根据权利要求14所述的液晶显示器,其中所述部分填充的液晶组分与所述密封层接触。
16.一种制造液晶显示器的方法,所述方法包括用液晶组分填充显示盒以及用在原位硬化的密封层密封经过填充的显示盒。
17.根据权利要求16所述的方法,其中所述密封层由UV,热或湿气固化的组分形成。
18.根据权利要求16所述的方法,其中所述密封层由包含热塑性或热固性前体物的组分形成。
19.根据权利要求16所述的方法,其中所述的硬化是通过溶剂蒸发,界面反应,湿气,热,辐射或其组合来完成的。
20.根据权利要求19所述的方法,其中所述的硬化是通过辐射来完成的。
21.根据权利要求2所述的液晶显示器,其中所述密封层在所述密封组分位于填充于所述显示盒中的液晶组分的顶部时进行原位硬化。
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113262735A (zh) * | 2021-04-21 | 2021-08-17 | 华南师范大学 | 液晶聚合物表面微纳结构的制备方法 |
CN113262735B (zh) * | 2021-04-21 | 2023-09-26 | 华南师范大学 | 液晶聚合物表面微纳结构的制备方法 |
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HK1047476B (zh) | 2005-12-09 |
WO2002056097A3 (en) | 2003-01-09 |
WO2002056097A2 (en) | 2002-07-18 |
CN100543543C (zh) | 2009-09-23 |
JP2004521377A (ja) | 2004-07-15 |
US20040169813A1 (en) | 2004-09-02 |
US7095477B2 (en) | 2006-08-22 |
MXPA03006176A (es) | 2004-03-10 |
JP4278978B2 (ja) | 2009-06-17 |
CN1206564C (zh) | 2005-06-15 |
HK1047476A1 (en) | 2003-03-14 |
TWI304140B (en) | 2008-12-11 |
KR100844305B1 (ko) | 2008-07-07 |
AU2002241837A1 (en) | 2002-07-24 |
EP1352289A2 (en) | 2003-10-15 |
JP2007233419A (ja) | 2007-09-13 |
KR20030075159A (ko) | 2003-09-22 |
US20030169387A1 (en) | 2003-09-11 |
US6784953B2 (en) | 2004-08-31 |
CN1363849A (zh) | 2002-08-14 |
US6795138B2 (en) | 2004-09-21 |
TWI293701B (en) | 2008-02-21 |
TW200813528A (en) | 2008-03-16 |
CA2434222A1 (en) | 2002-07-18 |
US20020126249A1 (en) | 2002-09-12 |
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