CN113372783A - 光学透明的剪切增稠流体以及包含其的光学显示装置 - Google Patents
光学透明的剪切增稠流体以及包含其的光学显示装置 Download PDFInfo
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- CN113372783A CN113372783A CN202110167191.0A CN202110167191A CN113372783A CN 113372783 A CN113372783 A CN 113372783A CN 202110167191 A CN202110167191 A CN 202110167191A CN 113372783 A CN113372783 A CN 113372783A
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Abstract
本发明公开了一种光学透明的剪切增稠流体以及包含所述光学透明的剪切增稠流体的保护组件。本发明进一步涉及所述光学透明的剪切增稠流体在电子装置中、特别是在光学显示装置中的用途。所述光学透明的剪切增稠流体包含:(a)具有等于或小于100nm的平均粒度的固体纳米颗粒;(b)至少一种聚合物;以及(c)液体介质。所述至少一种聚合物基本上可溶于所述液体介质。
Description
技术领域
本公开涉及一种光学透明的剪切增稠流体以及包括所述光学透明的剪切增稠流体的保护组件。其进一步涉及所述光学透明的剪切增稠流体在电子装置中、特别是在光学显示装置中的用途。
背景技术
许多电子装置包括用于显示图像的光学显示面板。此类装置的实例包括移动装置,如智能手机、数码相机、平板电脑、膝上型电脑、导航系统和电视。光学显示面板通常具有用于保护免于划痕、指纹、外力的冲击造成的损坏等的盖窗。例如,损坏可能是由电子装置(包括光学显示面板)掉落而引起的。此类盖窗含有光学透明的膜,并使用光学透明的粘合剂粘附到显示基底。
最近,已经开发并广泛使用了柔性显示装置。柔性显示装置采用柔性显示面板。此类面板可以是可弯曲的、可折叠的或可卷起的。与传统的刚性显示器相比,柔性显示器需要显著减小盖窗的厚度和刚度,以使能够实现可弯曲/柔性的特征。聚合物膜通常用于柔性显示装置的盖窗。结果是,显示面板中的在盖窗下方的敏感部件(例如,有机发射层、TFT阵列和阻挡层)易受到由于外部震动或冲击造成的损坏。损坏包括盖窗上的凹坑或裂缝、单个层之间的分层以及对于显示模块的像素损坏,其都对电子部件有害。显示器制造商一直在寻找一种有效的抗冲击材料,所述有效的抗冲击材料可用于在外力的冲击下保护显示装置下方的敏感电子部件。
剪切增稠流体(STF)是其粘度随剪切速率增加的流体。在一些情况下,在高剪切速率下,STF转化为具有类固体的特性的材料。此类材料在不存在剪切的情况下或在低剪切速率下是流体并且是柔性的,但在高剪切速率下变硬。
此类剪切增稠流体主要用于通过浸渍所述剪切增稠流体增强由基于织物的柔性防弹衣提供的弹道防护。还将剪切增稠流体掺入到护肘垫和护膝垫中用于防止由于钝性创伤对皮肤和关节的损伤。此外,它们可以用于工程泡沫、塑料和纳米复合材料中,这些是用于包括自行车、摩托车头盔、高尔夫球杆和球、以及运动鞋的运动设备,汽车以及航空器的粗糙且能量吸收性材料。
最近,此类STF材料具有作为用于柔性电子装置,如显示器的保护层的用途。STF层在正常运行期间是柔性的,但当装置暴露于外力时变硬且具有保护性。然而,STF材料是不透明的或半透明的,并且不适合用于显示装置的观看区域。
持续需要光学透明的STF材料,其可以用于显示装置、尤其是柔性显示装置并在外部震动或冲击下保护显示装置。
附图说明
附图中示出了实施例,以提高对如本文提出的概念的理解。
图1是具有本公开的光学透明的剪切增稠流体的显示装置的示意图。
熟练的技术人员应理解,图中的物体是为了简化和清楚而示出的,并且不一定按比例绘制。例如,图中的一些物体的尺寸相对于其他物体可能有所放大,以帮助提高对实施例的理解。
具体实施方式
如本说明书通篇所使用的,除非上下文另有明确指示,否则以下缩写应具有以下含义:℃=摄氏度;g=克;nm=纳米;μm=微米(micron/micrometer);mm=毫米;sec.=秒;并且min.=分钟。除非另外指出,否则所有量是重量百分比(“wt.%”)并且所有比率是摩尔比。所有数值范围都是包含端值的,并且可以按任何顺序组合,除了显然此数值范围被限制为加起来最高达100%的情况之外。除非另外指出,否则所有聚合物和低聚物的分子量均为以g/mol或道尔顿为单位的重均分子量(“Mw”),并且是使用凝胶渗透色谱法与聚苯乙烯标准品进行比较而确定的。
如本文所使用的,术语“可交联基团”是指在一个化合物或聚合物链上的可经由热处理或暴露于辐射连接至另一个化合物或聚合物链的基团。
术语“交联”“交联的”“固化”和“经固化的”是指连接化合物或聚合物中的键或链并在整个本说明书中可互换使用。
术语“液体介质”是指在室温(20℃-25℃)下是液体的并且可以是纯液体或液体的组合的材料。无论是否存在一种或多种液体都使用术语液体介质。
术语“光学透明的”是指视觉上透明且不模糊的材料或层。
术语“透射率”是指照射在膜或层上的穿过膜或层以便在另一侧上可检测到的给定波长的光的百分比。光透射率测量可以在可见光区(380nm至800nm)内进行。
术语“基本上可溶的”意指至少95%、或至少96%、或至少97%、或至少98%、或至少99%的聚合物可溶于液体介质,即5%或更少、或4%或更少、或3%或更少、或2%或更少、或1%或更少的聚合物以固体形式存在。
在整个本说明书中,术语“膜”和“层”可互换使用。
在本说明书中,除非由使用上下文另外明确指明或相反指示,否则其中在本发明主题的实施例被陈述或描述为包含(comprising)、包括(including)、含有(containing)、具有某些特征或要素、由某些特征或要素组成或由某些特征或要素构成时,除了明确陈述或描述的那些之外的一个或多个特征或要素也可存在于所述实施例中。所公开的本发明主题的替代实施例被描述为基本上由某些特征或要素组成,其中将实质性改变操作原理或实施例的区别特征的实施例特征或要素在此不存在。所描述的本发明主题的另一个替代实施例被描述为由某些特征或要素组成,在所述实施例中或在其非本质变型中,仅存在所具体陈述或描述的特征或要素。
而且,使用“一个/种(“a/an”)”来描述本文所述的要素和组分。这样做只是为了方便并给出本发明范围的一般意义。此描述应当被解读为包括一个/种或至少一个/种,并且单数形式也包括复数形式,除非很明显其另有所指。
除非另有定义,否则本文所使用的所有技术和科学术语均具有与本发明所属领域普通技术人员所通常理解的相同含义。尽管与本文描述的那些方法和材料的类似者或等同者均可用于本公开实施例的实践或检验,但以下描述了合适的方法和材料。此外,材料、方法和实例仅为说明性的并且不旨在是限制性的。
至于本文未描述的范围,有关特定材料、加工行为和电路的许多细节均是常规的并且可以在有机发光二极管显示器、光电检测器、光伏电池、和半导体构件领域的教科书和其他来源中找到。
本公开提供了一种光学透明的剪切增稠流体(“STF”),其包含具有等于或小于100nm的平均粒度的固体纳米颗粒;至少一种聚合物;以及液体介质,其中所述至少一种聚合物基本上可溶于所述液体介质中。
至少一种聚合物是光学透明的且无色的。聚合物可以是均聚物或衍生自两种或更多种单体的共聚物。在一些实施例中,至少一种聚合物可以包含可交联基团。可交联基团的实例可以包括但不限于乙烯基、羟基、羧基、全氟乙烯基醚、苯并环丁烷(如1-苯并-3,4-环丁烷)、邻醌二甲烷、硅氧烷、氰酸酯基团、环醚(如环氧)、环烯、炔属基团及其组合。
至少一种具有可交联基团的聚合物可以选自由以下组成的组:聚(丙烯酸2-羟乙酯-共-甲基丙烯酸缩水甘油酯-共-甲基丙烯酸)、聚(丙烯酸2-羟乙酯-共-甲基丙烯酸缩水甘油酯-共-丙烯酸2-羧乙酯)、部分地用丙烯酸酯官能团封端的聚(丙烯酸2-羟乙酯)、聚乙二醇二丙烯酸酯、聚乙二醇二甲基丙烯酸酯、聚乙二醇单丙烯酸酯、聚乙二醇单甲基丙烯酸酯、丙烯酸2-羟乙酯的共聚物、及其组合。
在一个实施例中,丙烯酸2-羟乙酯的共聚物具有小于-20℃的玻璃化转变温度(Tg)。用于形成丙烯酸2-羟乙酯的共聚物的单体的实例可以包括但不限于2-(2-乙氧基乙氧基)乙基(甲基)丙烯酸酯、(甲基)丙烯酸苯氧基乙酯、丙烯酸丁酯、丙烯酸异丁酯、丙烯酸异丙酯、丙烯酸2-甲氧基乙酯、丙烯酸2-乙氧基乙酯、甲基丙烯酸2-乙基己酯、丙烯酸异癸酯、甲基丙烯酸异癸酯、乙基二乙二醇丙烯酸酯、丙烯酸十七烷基酯、丙烯酸4-羟丁酯、丙烯酸2-羟乙酯、羟乙基己内酯丙烯酸酯、丙烯酸2-丙基庚酯、甲基丙烯酸月桂酯、甲基丙烯酸异十三烷基酯、丙烯酸正丙酯、及其组合。
在一些实施例中,至少一种聚合物包含两种或更多种聚合物。在一个实施例中,至少一种聚合物包含具有第一可交联基团的第一聚合物以及具有第二可交联基团的第二聚合物。将第一聚合物与第二聚合物交联。第一可交联基团可以与第二可交联基团相同或不同。
在一些实施例中,光学透明的剪切增稠流体可以进一步包含可以交联至少一种聚合物的交联剂。交联剂可以包括但不限于四(甲氧基甲基)甘脲;六甲氧基甲基三聚氰胺;聚乙二醇二缩水甘油醚;丁烷二缩水甘油醚;琥珀酸;丙烷三甲酸;异氰酸酯,如异佛尔酮二异氰酸酯和六亚甲基二异氰酸酯;以及封端的异氰酸酯,如BL 3475 BA/SN、PL 340 BA/SN和BL 350 MPA/SN(从科思创德国公司(Covestro Deutscheland AG)可商购的);及其组合。
通过交联剂交联的至少一种聚合物可以包括但不限于聚(丙烯酸2-羟乙酯)、聚(丙烯酸2-羟乙酯-共-(甲基)丙烯酸丙烯酸酯)、聚(丙烯酸2-羟乙酯-共-丙烯酸2-羟乙酯)、聚(丙烯酸2-羟乙酯-共-甲基丙烯酸缩水甘油酯)、及其组合。交联剂可以基于聚合物的重量5至25wt.%或10至20wt.%存在。
至少一种聚合物可以热交联或在辐射下交联。在一些实施例中,至少一种聚合物可以在低于250℃、或低于240℃、或低于230℃、或低于220℃、或低于210℃、或低于200℃的温度下热交联。可以存在交联催化剂以促进热交联。交联催化剂可以是酸或碱。交联催化剂的实例可以包括但不限N,N-二甲基苄胺、2-乙基咪唑、2-乙基己酸、四甲基胍、苄基三甲基溴化铵、苄基三甲基氢氧化铵、四丁基氢氧化铵、2-乙基己酸铬(III)、辛酸钴、三乙醇胺钛螯合物、辛酸锆、及其组合。
商业的交联催化剂的实例可以包括但不限于K-PURE TAG-2678、K-PURE TAG-2713和K-PURE TAG-2678(从金氏工业有限公司(King Industries,Inc)可商购的),
TA-103
(从贺利氏电子化工公司(Heraeus Epurio LLC)可商购的)。
在一些实施例中,至少一种聚合物可以在具有在100至600nm、或150nm至600nm、或190nm至600nm(紫外线至可见光范围)处的峰最大值的光化辐射下在自由基引发剂的存在下交联。
自由基引发剂可以包括但不限于二苯甲酮、苯偶酰(1,2-二酮)、噻吨酮、2-苄基-2-二甲基氨基-1-[4-(4-吗啉基)苯基]-1-丁酮、2,4,6-三甲基-苯甲酰基-二苯基氧化膦、1-羟基-环己基-苯基-酮、2-羟基-2-甲基-1-苯基-1-丙酮、低聚的2-羟基-2-甲基-1-[4-(1-甲基乙烯基)苯基]丙酮、二氢-5-(2-羟基-2-甲基-1-氧代丙基)-1,1,3-三甲基-3-(4-(2-羟基-2-甲基-1-氧代丙基)苯基)-1H-茚、以及双-二苯甲酮、α-[(4-苯甲酰基苯氧基)-乙酰基]-ω-[[2-(4-苯甲酰基苯氧基)-乙酰基]氧基]-聚(氧基-1,4-丁烷二基))、双(环己基磺酰基)重氮甲烷、双(叔丁基磺酰基)重氮甲烷、双(4-甲基苯基磺酰基)重氮甲烷、二苯基-4-甲基苯基锍鎓三氟甲烷磺酸盐、二苯基-2,4,6-三甲基苯基锍鎓对甲苯磺酸盐、及其组合。
合适的辐射可以存在于例如太阳光或来自人造光源的光中。光源没有特别的限制并且可以根据目的适当地选择。点光源和阵列(“灯罩(lamp carpet)”)均是合适的。其实例包括碳弧灯,氙弧灯,可能具有金属卤化物掺杂物的低、中、高和超高压汞灯(金属卤素灯),微波刺激的金属蒸气灯,准分子灯,超光化荧光灯管,荧光灯,氩气白炽灯,电子手电筒,摄影泛光灯,发光二极管(LED),电子束和X射线。所使用的特定波长将取决于STF中所使用的特定的一种或多种自由基引发剂。此类波长选择和光剂量完全在本领域技术人员的能力范围内。本发明的STF中所使用的光剂量可以从30至8,000mJ/cm2、200至8,000mJ/cm2、或从400至6,000mJ/cm2、或从500至5,000mJ/cm2、或从550至3,000mJ/cm2变化。在一个实施例中,使用以0.24m/s的速度的配备有D灯泡的融合系统紫外线(UV)带系统装置(马里兰州盖瑟斯堡的贺利氏特种光源美国有限公司(Heraeus Noblelight American,LLC,Gaithersburg,MD))。
至少一种聚合物可以以基于STF的总重量10-25wt.%、或15-20wt.%的量存在。
本文所述的固体纳米颗粒具有100nm或更小的平均粒度。当固体纳米颗粒大于100nm时,STF变得模糊并且不是光学透明的。在一些实施例中,固体纳米颗粒具有5-100nm、或10-100nm、或20-100nm、或30-100nm、或40-100nm、50-100nm、或60-100nm、或70-100nm、或10-75nm、或30-75nm、或50-70nm的平均粒度。
在一些实施例中,固体纳米颗粒具有1.3至2.0、或1.3至1.8、或1.3至1.7的折射率(在550nm下测量的)。在一个实施例中,至少一种聚合物具有与固体纳米颗粒相同的折射率。
固体纳米颗粒可以是无机或有机纳米颗粒。在一些实施例中,有机纳米颗粒选自由以下组成的组:羟基化的乙烯基或丙烯酸酯聚合物、聚苯乙烯、聚甲基丙烯酸甲酯、聚环氧乙烷、及其组合。
在一些实施例中,无机纳米颗粒选自由以下组成的组:二氧化硅、碳酸钙、氧化铁、高岭土、氧化铝、及其组合。
在一个实施例中,无机纳米颗粒可以是二氧化硅纳米颗粒。二氧化硅纳米颗粒可以是单分散的均匀尺寸的二氧化硅纳米颗粒并且是通过原硅酸四乙酯(TEOS)在溶剂(如醇)中的水解而合成的。醇可以是甲醇、乙醇、正丙醇、异丙醇、丁醇或其混合醇。可以存在酸和碱催化剂用于合成。碱催化剂可以是氨。单分散的均匀尺寸的二氧化硅纳米颗粒的合成公开在胶体与界面科学杂志[Journal of Colloid and Interface Science],26,62-29(1968)中,将其通过引用以其全文特此并入本文。溶剂中的二氧化硅纳米颗粒可以直接用于光学透明的STF流体.
在一些实施例中,二氧化硅纳米颗粒可以通过有机硅化合物改性.有机硅化合物可以是有机烷氧基硅烷或甲基烯丙基硅烷。有机烷氧基硅烷可以包含一个、两个或三个与硅连接的烷氧基,如以下所示。
其中R是烷基或芳基;X1-X3相同或不同并且各自独立地是R或烷氧基。有机烷氧基硅烷的实例可以包括但不限于3-氨基丙基三甲氧基硅烷(APTMS)、3-氨基丙基三乙氧基硅烷(APTES)、3-氨基丙基三甲氧基-乙氧基乙氧基硅烷、3-氨基丙基三乙氧基-甲氧基乙氧基硅烷、3-氨基丙基-甲基-二乙氧基硅烷、N-甲基-3-氨基丙基三甲氧基硅烷、N-丁基-3-氨基丙基三甲氧基硅烷、3-巯基丙基三甲氧基硅烷、3-巯基丙基三乙氧基硅烷、3-巯基丙基-甲基二甲氧基硅烷、氨基乙基-氨基丙基-三甲氧基硅烷、(3-缩水甘油基氧基丙基)三甲氧基硅烷)、(N-环己基氨基甲基)甲基二-乙氧基硅烷、(N-环己基氨基甲基)三乙氧基硅烷、(N-苯基氨基甲基)甲基二甲氧基硅烷、(N-苯基氨基甲基)三甲氧基硅烷、N-乙基-氨基异丁基三甲氧基硅烷、4-氨基-3,3-二甲基丁基三甲氧基硅烷、(3-氯丙基)三甲氧基硅烷、(3-缩水甘油基氧基丙基)三甲氧基硅烷、乙基三乙酰氧基硅烷、三乙氧基(异丁基)硅烷、三乙氧基(辛基)硅烷、三(2-甲氧基乙氧基)(乙烯基)硅烷、苯基三甲氧基硅烷、氯三乙氧基硅烷、乙烯基-三甲氧基硅烷、3-丙烯酰基氧基三甲氧基硅烷、甲基三甲氧基硅烷、8-甲基丙烯酰基氧基三甲氧基硅烷、或以上的任何组合。
为了当受到外力或外部冲击时使STF为装置提供足够的保护,固体纳米颗粒可以以基于STF的总重量50-75wt.%的量存在。在一些实施例中,固体纳米颗粒可以以基于STF的总重量50-70wt.%、或54-70wt.%、或50-60wt.%、或60-70wt.%的量存在。
液体介质是光学透明的。液体介质具有与固体纳米颗粒相同或接近的折射率,并且其中可以使固体纳米颗粒分散。在一个实施例中,液体介质具有1.47±0.05的折射率(在550nm下测量的)。
在一个实施例中,液体介质可以选自由以下组成的组:亚烷基二醇、聚亚烷基二醇、甘油、多元醇及其组合。液体介质的实例可以包括但不限于乙二醇、丙二醇、聚乙二醇和聚丙二醇。
存在的液体介质的量足以分散固体纳米颗粒并溶解一种或多种聚合物。在一些实施例中,液体介质可以以基于STF的总重量25至50wt.%、或15至25wt.%的量存在。
在一个实施例中,STF可以通过将固体纳米颗粒和至少一种具有可交联基团的聚合物或至少一种聚合物和交联剂添加到液体介质中;并且将它们混合在一起来制备。
在另一个实施例中,STF可以通过以下来制备:将至少一种具有可交联基团的聚合物或至少一种聚合物和交联剂溶解在液体介质中以形成聚合物溶液。并且然后将固体纳米颗粒添加并分散在聚合物溶液中。
本公开的STF在剪切应力的作用之前是粘性液体。在一些实施例中,STF在没有任何剪切应力下可以具有2,000至200,000mPa.s、或5,000至200,000mPa.s、或10,000至200,000mPa.s、或15,000至200,000mPa.s、或20,000至150,000mPa.s、或50,000至100,000mPa.s的粘度。
以上针对STF的实施例中的任一个可以与一个或多个其他实施例组合,只要它们不是互相排斥的。本领域普通技术人员将理解哪些实施例是相互排斥的并且因此将容易地能够确定本申请所考虑的实施例的组合。
本公开还涉及一种保护组件。保护组件包括第一光学透明的层以及布置在所述第一光学透明的层上的STF。STF与先前所述的相同。在一些实施例中,将STF涂覆在第一光学透明的层上,干燥以除去任何溶剂(如果存在的话)以形成STF层。在一个实施例中,然后将STF层交联以形成交联的STF层。
保护组件可以进一步包括布置在STF层上的第二光学透明的层。在一个实施例中,可以将第二光学透明的层层压在STF层之上。可以在第二光学透明的层的层压之前或之后进行交联以形成交联的STF层。在另一个实施例中,可以将STF密封在第一与第二光学透明的层之间并且然后交联。在密封之前除去溶剂。
第一和第二光学透明的层可以由相同或不同的材料制成。合适的材料可以包括但不限于聚酰亚胺、聚酰亚胺-酰胺、聚酯、聚氨酯、聚乙烯、聚丙烯、聚碳酸酯、聚对苯二甲酸乙二醇酯、聚苯乙烯、聚甲基丙烯酸甲酯、乙烯-四氟乙烯共聚物、及其组合。在一些实施例中,光学透明的层可以具有10至400μm、或25至400μm、或25至350μm、或25至300μm、或25至250μm、或30至100μm、或40至75μm、或50至70μm的厚度。
在一些实施例中,STF层可以具有1至400μm、或3至400μm、或3至350μm、或5至400μm、或5至300μm、或10至400μm、或10至250μm、或20至400μm、或20至200μm、或25至400μm、或25至350μm、25至300μm、或25至250μm、或25至200μm、或25至150μm、或5至100μm、或5至50μm、或5至30μm、或5至20μm、或7至25μm、或7至20μm、或7至15μm的厚度。
本公开的保护组件是透明且无色的。保护组件的光学特性(透射率、雾度、黄度指数、b*)可以用UV-VIS光谱仪测量。可以基于395至700nm的吸光度光谱计算黄度指数。可以基于380至780nm的%透射率计算b*(与感知到的黄化度相关)。
在本公开中,含有STF层的保护组件的光学特性可以通过将STF层放置在两个透明的聚合物膜之间来确定。保护组件可以具有5%或更小、或3%或更小、或2%或更小、或1%或更小的雾度值。保护组件可以具有至少80%、或至少85%、或至少90%、或至少93%、或至少94%、或至少95%、或至少97%、或至少98%、或至少99%的透射率。
STF在剪切应力下在硬化中的有效性可以通过使用应变控制的流变仪测量STF的粘度随剪切速率的变化来确定。STF的有效性还可以以戳破测试确定。在戳破测试中,用塑料移液管以约10sec-1的速率敲击流体。如果流体在冲击时立即变成固体,则STF将通过此测试。通常不希望的是STF在小于1sec-1的时间尺度上变成固体。
本公开进一步涉及一种用于制造保护组件的方法。在一些实施例中,所述方法包括以下步骤:(a)提供至少一种具有可交联基团的聚合物;(b)将所述至少一种聚合物溶解在液体介质中以形成聚合物溶液;(c)将具有等于或小于100nm的平均粒度的固体纳米颗粒分散在所述聚合物溶液中以形成光学透明的剪切增稠流体(STF);(d)将所述剪切增稠流体涂覆在第一光学透明的层上以形成STF层;以及(e)将所述STF层暴露于一定量的固化能量以形成经固化的STF层。
在一些实施例中,所述方法包括以下步骤:(a)提供至少一种聚合物和交联剂;(b)将所述至少一种聚合物和所述交联剂溶解在液体介质中以形成聚合物溶液;(c)将具有等于或小于100nm的平均粒度的固体纳米颗粒分散在所述聚合物溶液中以形成光学透明的剪切增稠流体(STF);(d)将所述剪切增稠流体涂覆在第一光学透明的层上以形成STF层;以及(e)将所述STF层暴露于一定量的固化能量以形成经固化的STF层。交联剂与先前所述的那些相同。
如前所述,固化能量可以包括热和/或光化辐射。在一个实施例中,在上述方法中,可以在步骤(e)之前增加步骤(d')。步骤(d')包括将第二光学透明的层添加到STF层的顶表面上。在另一个实施例中,如上所述的方法进一步包括将第二光学透明层添加在经固化的STF层的顶表面上的步骤(f)。
第一和第二光学透明的层可以由相同或不同的材料(如前所述)制成。此外,STF与先前所述的那些相同。
本公开还涉及包括如上所述的保护组件的显示装置。在一些实施例中,显示装置可以是柔性显示装置。示例性装置在图1中示出。装置1000具有柔性基板100、显示面板200和保护组件300,其中,所述保护组件位于所述显示面板的观看侧。保护组件300包括第一透明柔性膜10,光学透明的STF层20和第二透明柔性膜30。透明柔性膜和STF层与先前所述的相同。柔性基板100可以是聚合物膜或玻璃层,并且是本领域众所周知的。显示面板200可以是任何已知类型的显示器。示例性显示面板可以包括但不限于LCD和OLED。
实例
本文描述的概念将在以下实例中进一步描述,这些实例不限制权利要求中所述的本发明的范围。除非另有说明,否则所有温度单位均是室温(20℃-25℃),并且所有压力单位均是标准压力或101kPa。
材料
ORGANOSILICASOLTMMA-ST-ZL:在甲醇中具有30wt.%的固体负载量的粒度为70至100nm的胶体二氧化硅单分散的纳米颗粒,从得克萨斯州休斯敦的日产化学美国公司(Nissan Chemical America Corporation,Houston,Texas)可商购的。
V65 HP:2,2'-偶氮双(2.4-二甲基戊腈),从日本东京市的富士胶片和光化学美国公司(FUJIFILM Wako Pure Chemicals Corporation,Tokyo,Japan)可商购的。
聚合物的制备
实例1
如下制备衍生自丙烯酸羟乙酯(“HEA”)和甲基丙烯酸缩水甘油酯(“GMA”)的共聚物。
在40ml玻璃小瓶中,将1.6292g的GMA与18.4220g的HEA和15.0123g的异丙醇(“IPA”)混合。将小瓶放置在冰/水浴中以与浴达到温度平衡。然后将0.6062g的V65 HP添加到小瓶中。然后将小瓶放入振荡器中以溶解V65 HP以形成溶液。然后将小瓶放回浴中。在到100ml三颈圆底烧瓶的反应器的整个进料过程中,将溶液保持在浴中。三个颈分别连接到热电偶、冷凝器和溶液的进料口。反应器通过加热套加热。加热套位于磁力搅拌器上,以用磁力搅拌子为反应器提供搅拌。向反应器中装入15.0g的IPA。然后将反应器加热至80℃并保持在80℃。在90分钟内将溶液进料到反应器中。将溶液进料后,将反应器在80℃下保持两小时。然后将反应器冷却至20℃-25℃。获得反应器中的聚合物溶液并直接使用。聚合物溶液中的聚合物含量是41.6wt.%。
实例2
如下制备衍生自丙烯酸羧乙酯(“CEA”)和GMA的共聚物。
进行与实例1相同的程序,除了通过混合2.0223g的CEA,18.0062g的GMA,14.8159g的IPA和0.6039g的V65 HP来制备溶液外。最终产物的聚合物溶液中的聚合物含量是38.3wt.%。
实例3
如下制备衍生自HEA、CEA和GMA的共聚物。
进行与实例1相同的程序,除了通过混合5.772g的HEA,7.16g的CEA,7.064g的GMA,15g的IPA和0.6g的V65 HP制备溶液外。
50μm聚酰亚胺(PI)膜的制备
实例4
向氮气吹扫过的80加仑的反应器中在搅拌下添加12.837kg的三氟甲基联苯胺(TFMB,赛卡公司(Seika Corporation),Wakayam Seika Kogyo有限公司,日本)和107.5kg的二甲基乙酰胺(DMAC)。将溶液搅拌至使得TFMB完全溶解在DMAC溶剂中,并在所有后续步骤期间继续搅拌。将反应混合物加热至约40℃。将1.11kg的联苯四甲酸二酐(BPDA,三菱化学公司(Mitsubishi Chemical Co.),日本)和15.079kg的4,4’-(六氟异亚丙基)二邻苯二甲酸酐(6FDA,新纳希公司(Synasia),麦塔城(Metuchen),新泽西州)以四个单独的等分部分在6小时时间段内添加。将三个另外等分部分的1.831g的BPDA和24.881g的6FDA在约3小时的时间段内添加到反应混合物中。预聚物在25℃下的粘度为约89泊。在氮气吹扫的反应器中使用在DMAC中的6wt.%均苯四甲酸二酐(PMDA)的混合物将一部分聚合物聚合(“加工(finish)”)至约1200-1300泊。将所述材料在40℃下在约24小时期间与PMDA溶液聚合以形成聚酰胺酸溶液。
将聚酰胺酸溶液流延到移动带上并在约95℃至约150℃的烘箱温度下干燥。将自支撑膜从带剥离并且在约110℃至约675℃的温度(辐射加热器表面温度)的拉幅机烘箱中用辐射加热器加热以使聚合物膜干燥并酰亚胺化。获得了50μm PI膜。
STF、保护组件制备和表征
实例5
将ORGANOSILICASOLTMMA-ST-ZL(MA-ST-ZL),二乙二醇和由实例1和2制备的合成共聚物以表1所列的量混合以形成混合物。将甲醇在30℃下用旋转蒸发仪从混合物中除去,以形成液体STF配制品作为对照和样品1-3。
表1
将由对照和样品1-3制备的液体STF配制品用刮涂棒涂覆器涂覆到由实例4制备的第一50μm无色聚酰亚胺膜上以形成STF层上。将由实例4制备的50μm无色聚酰亚胺膜的第二膜放置在STF层之上以形成保护组件,然后将其在戳破测试中以约10sec-1的速率进行测试。结果在表2中示出。
表2
样品 | 剪切增稠作用 | 戳破测试 |
对照 | 否 | 失败 |
1 | 显著的 | 通过 |
2 | 有 | 失败 |
3 | 有 | 通过 |
用Agilent/Hewlett Packard 8453 UV-VIS光谱仪(从加利福尼亚州圣克拉拉的安捷伦科技公司(Agilent Technologies Inc,Santa Clara,CA)可商购的)测量样品1的透射率和雾度。在400至800nm波长处测量透射率。将含有两个由实例4制备的50μm PI膜与填充在两个膜之间的二乙二醇的空白样品基线化为100%的400至800nm波长的透射率。样品1的透射率为94%,并且雾度小于0.84。
实例6
将57.4wt.%的ORGANOSILICASOLTMMA-ST-ZL,25.7wt.%的二乙二醇,8.5wt.%的由实例1制备的共聚物和8.4wt.%的由实施例2制备的共聚物混合以形成混合物。将甲醇用旋转蒸发仪在30℃下从混合物中除去,以形成液体STF配制品。
将STF配制品涂覆在由实例4制备的50μm PI膜上,并干燥以在PI膜上形成STF层。将STF层连同PI膜在150℃下烘烤5-15分钟,以在第一50μm PI膜上形成交联的STF层。将由实例4制备的第二50μm PI膜层压在交联的STF层之上以形成保护组件。保护组件通过了以10sec-1的速率的戳破测试。
Claims (16)
1.一种光学透明的剪切增稠流体,其包含:
具有等于或小于100nm的平均粒度的固体纳米颗粒;
至少一种聚合物;以及
液体介质,
其中所述至少一种聚合物基本上可溶于所述液体介质。
2.如权利要求1所述的剪切增稠流体,其中,所述至少一种聚合物包含选自由以下组成的组的可交联基团:羟基、羧基、环氧、丙烯酸酯及其组合。
3.如权利要求2所述的剪切增稠流体,其中,所述至少一种聚合物选自由以下组成的组:聚(丙烯酸2-羟乙酯-共-甲基丙烯酸缩水甘油酯-共-甲基丙烯酸)、聚(丙烯酸2-羟乙酯-共-甲基丙烯酸缩水甘油酯-共-丙烯酸2-羧乙酯)、部分地用丙烯酸酯官能团封端的聚(丙烯酸2-羟乙酯)、聚乙二醇二丙烯酸酯、聚乙二醇二甲基丙烯酸酯、聚乙二醇单丙烯酸酯、聚乙二醇单甲基丙烯酸酯、丙烯酸2-羟乙酯的共聚物、及其组合。
4.如权利要求1所述的剪切增稠流体,其进一步包含选自由以下组成的组的交联剂:四(甲氧基甲基)甘脲、六甲氧基甲基三聚氰胺、聚乙二醇二缩水甘油醚、丁烷二缩水甘油醚、琥珀酸、丙烷三甲酸、异氰酸酯以及封端的异氰酸酯。
5.如权利要求1至4中任一项所述的剪切增稠流体,其中,所述固体纳米颗粒具有1.3至2.0的折射率并且所述至少一种聚合物具有与所述固体纳米颗粒相同的折射率。
6.如权利要求2所述的剪切增稠流体,其中,所述至少一种聚合物包含具有第一可交联基团的第一聚合物和具有第二可交联基团的第二聚合物,其中将所述第一聚合物与所述第二聚合物交联。
7.如权利要求2或4所述的剪切增稠流体,其中,将所述至少一种聚合物在低于250℃的温度下交联。
8.如权利要求2或4所述的剪切增稠流体,其中,将所述至少一种聚合物紫外线(UV)交联。
9.如权利要求1至8中任一项所述的剪切增稠流体,其中,所述液体介质选自由以下组成的组:亚烷基二醇、聚亚烷基二醇、甘油、多元醇及其组合。
10.如权利要求1至9中任一项所述的剪切增稠流体,其中,所述固体纳米颗粒是无机或有机纳米颗粒。
11.如权利要求10所述的剪切增稠流体,其中,所述无机纳米颗粒是二氧化硅纳米颗粒并且所述二氧化硅纳米颗粒是通过原硅酸四乙酯在醇中的水解而制成的单分散的均匀尺寸的二氧化硅纳米颗粒。
12.如权利要求11所述的剪切增稠流体,其中,所述二氧化硅纳米颗粒通过有机烷氧基硅烷或甲基烯丙基硅烷的有机硅化合物改性。
13.一种保护组件,其包括第一光学透明的层和布置在所述第一光学透明的层上的如权利要求1至12中任一项所述的剪切增稠流体。
14.如权利要求13所述的保护组件,其进一步包括布置在所述剪切增稠流体上的第二光学透明的层。
15.一种用于生产保护组件的方法,所述方法包括以下步骤:
(a)提供至少一种具有可交联基团的聚合物;
(b)将所述至少一种聚合物溶解在液体介质中以形成聚合物溶液;
(c)将具有等于或小于100nm的平均粒度的固体纳米颗粒分散在所述聚合物溶液中以形成光学透明的剪切增稠流体(STF);
(d)将所述剪切增稠流体涂覆在第一光学透明的层上以形成STF层;以及
(e)将所述STF层暴露于一定量的固化能量以形成经固化的STF层。
16.一种用于生产保护组件的方法,所述方法包括以下步骤:
(a)提供至少一种聚合物和交联剂;
(b)将所述至少一种聚合物和所述交联剂溶解在液体介质中以形成聚合物溶液;
(c)将具有等于或小于100nm的平均粒度的固体纳米颗粒分散在所述聚合物溶液中以形成光学透明的剪切增稠流体(STF);
(d)将所述剪切增稠流体涂覆在第一光学透明的层上以形成STF层;以及
(e)将所述STF层暴露于一定量的固化能量以形成经固化的STF层。
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