CN110383164A - 用于电泳介质的光热诱导的聚合的抑制剂 - Google Patents
用于电泳介质的光热诱导的聚合的抑制剂 Download PDFInfo
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- CN110383164A CN110383164A CN201880016148.0A CN201880016148A CN110383164A CN 110383164 A CN110383164 A CN 110383164A CN 201880016148 A CN201880016148 A CN 201880016148A CN 110383164 A CN110383164 A CN 110383164A
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Classifications
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- G—PHYSICS
- G02—OPTICS
- 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
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/165—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on translational movement of particles in a fluid under the influence of an applied field
- G02F1/166—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on translational movement of particles in a fluid under the influence of an applied field characterised by the electro-optical or magneto-optical effect
- G02F1/167—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on translational movement of particles in a fluid under the influence of an applied field characterised by the electro-optical or magneto-optical effect by electrophoresis
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C243/00—Compounds containing chains of nitrogen atoms singly-bound to each other, e.g. hydrazines, triazanes
- C07C243/04—N-nitroso compounds
- C07C243/06—N-nitroso-amines
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C39/00—Compounds having at least one hydroxy or O-metal group bound to a carbon atom of a six-membered aromatic ring
- C07C39/02—Compounds having at least one hydroxy or O-metal group bound to a carbon atom of a six-membered aromatic ring monocyclic with no unsaturation outside the aromatic ring
- C07C39/08—Dihydroxy benzenes; Alkylated derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C50/00—Quinones
- C07C50/02—Quinones with monocyclic quinoid structure
- C07C50/04—Benzoquinones, i.e. C6H4O2
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
- C09D5/4407—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications with polymers obtained by polymerisation reactions involving only carbon-to-carbon unsaturated bonds
- C09D5/4411—Homopolymers or copolymers of acrylates or methacrylates
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Abstract
可被掺入到电泳显示器中的电泳介质包括可以包含在多个微囊或微单元或聚合物连续相中的分散液。所述分散液可包括非极性流体、多个第一带电粒子;和光热诱导的聚合的抑制剂,所述抑制剂抑制粒子和/或微单元或聚合物连续相之间的潜在交联。所述抑制剂可以是具有不饱和烃环和羟基基团、羰基基团和亚硝基基团中的至少一种的化合物。多个微单元或聚合物连续相和粒子的涂层可包含含有(甲基)丙烯酸酯的聚合物材料。
Description
相关申请的交叉引用
本申请要求于2017年3月9日提交的申请号为62/469,082的美国临时申请的优先权和权益,其内容通过引用整体并入本文。
发明背景
本发明涉及电泳显示器和抑制电泳介质中抑制不期望的光热诱导的聚合反应以在用于显示器中时改善介质的性能的添加剂。例如,本发明的添加剂能改善电泳显示器的热和光学可靠性。
基于粒子的电泳显示器多年来一直是重点研究和开发的主题。在这种显示器中,多个带电粒子(有时称为颜料粒子)在电场的影响下移动通过流体。电场通常由导电膜或晶体管,例如场效应晶体管提供。与液晶显示器相比,电泳显示器具有良好的亮度和对比度、宽视角、状态双稳态性和低功耗。然而,这种电泳显示器具有比LCD显示器更慢的切换速度,并且电泳显示器通常太慢而不能显示实时视频。另外,电泳显示器在低温下可能迟滞,因为流体的粘度限制了电泳粒子的移动。尽管有这些缺点,但电泳显示器仍可见于日常产品,例如电子书(电子阅读器)、移动电话和移动电话壳、智能卡、标牌、手表、货架标签和闪存驱动器。
电泳图像显示器(EPID)通常包括一对间隔开的板状电极。通常观看侧上的至少一个电极板是透明的。由介电溶剂与分散在其中的带电颜料粒子组成的电泳流体封闭在两个电极板之间。电泳流体可以具有分散在对比色的溶剂或溶剂混合物中的一类带电颜料粒子。在这种情况下,当在两个电极板之间施加电压差时,颜料粒子通过吸引到极性与颜料粒子极性相反的板迁移。因此,在透明板上显示的颜色可以是溶剂的颜色或颜料粒子的颜色。板极性的反转将使粒子迁移到相对的板,从而反转颜色。供选择地,电泳流体可具有两类具有对比色并带有相反电荷的颜料粒子,并且两类颜料粒子分散在透明溶剂或溶剂混合物中。在这种情况下,当在两个电极板之间施加电压差时,两类颜料粒子将移动到显示单元中的相对端(顶部或底部)。因此,在显示单元的观看侧将看到两类颜料粒子的颜色中的一种。
授让给麻省理工学院(MIT)、E Ink公司,E Ink California,LLC和相关公司或麻省理工学院(MIT)、E Ink公司,E Ink California,LLC和相关公司署名的许多专利和申请描述了封装的、微单元电泳和其他电光介质中使用的各种技术。在微单元电泳显示器中,带电颜料粒子保留在通常为聚合物膜的载体介质内形成的多个腔内。这些专利和申请中描述的技术包括:
(a)电泳粒子、流体和流体添加剂;参见例如第7002728和7679814号美国专利;
(b)微单元结构、壁材料和形成微单元的方法;参见例如第7072095和9279906号美国专利;
(d)用于填充和密封微单元的方法;参见例如第6545797;6751008;6788449;6831770;6833943;6859302;6867898;6914714;6972893;7005468;7046228;7052571;7144942;7166182;7374634;7385751;7408696;7522332;7557981;7560004;7564614;7572491;7616374;7684108;7715087;7715088;8179589;8361356;8520292;8625188;8830561;9081250;和9346987号美国专利;和第2002/0188053;2004/0120024;2004/0219306;2006/0132897;2006/0164715;2006/0238489;2007/0035497;2007/0036919;2007/0243332;2015/0098124;和2016/0109780号美国专利申请公开文件;
(e)含有电光材料的膜和子组件;参见例如第6982178和7839564号美国专利;
(f)显示器中使用的背板、粘合层和其他辅助层和方法;参见例如第7116318和7535624号美国专利;
(g)颜色形成和颜色调整;参见例如第7075502和7839564号美国专利;
(h)用于驱动显示器的方法;参见例如第7012600和7453445号美国专利;
(i)显示器的应用;参见例如第7312784和8009348号美国专利;和
(j)非电泳显示器,如第6241921号美国专利和第2015/0277160号美国专利申请公开文件中所述;和除显示器以外的封装和微单元技术的应用;参见例如第2015/0005720和2016/0012710号美国专利申请公开文件。
许多商用电泳介质基本上仅显示两种颜色,在极黑和极白之间具有梯度,称为“灰阶”。这种电泳介质或者使用在具有第二不同颜色的有色流体中具有第一颜色的单一类型的电泳粒子(在此情形下,在粒子位于邻近显示器的观看表面时显示第一颜色,并且在粒子被从观看表面隔开时显示第二颜色),或者使用无色流体中具有不同的第一颜色和第二颜色的第一类和第二类电泳粒子。在后面的情形下,当第一类粒子位于邻近显示器的观看表面时显示第一颜色,并且当第二类粒子位于邻近观看表面时显示第二颜色。通常,两种颜色为黑色和白色。
如果期望为全彩显示器,则可将彩色滤光片阵列沉积在单色(黑与白)显示器的观看表面上。具有彩色滤光片阵列的显示器依赖面积共享和颜色掺合以创造颜色刺激。三或四原色,如红/绿/蓝(RGB)或红/绿/蓝/白(RGBW)共享可用的显示器区域,并且滤光片可按一维(条状)或二维(2×2)重复图案布置。原色或超过三原色的其他选择在本领域中也是已知的。选择足够小的三种(在RGB显示器的情况下)或四种(在RGBW显示器的情况下)子像素,使得在预期的观看距离处它们在视觉上掺合在一起成为颜色刺激均匀(“颜色掺合”)的单一像素。
虽然看似简单,但电泳介质和电泳装置显示出复杂的行为。例如,已发现简单的“开/关”电压脉冲不足以在电子阅读器中获得高质量文本。而是需要复杂的“波形”在状态之间驱动粒子以及确保新显示的文本不保留先前文本的记忆,即“重影”。参见例如第20150213765号美国专利申请。结合电场的复杂性,内相,即粒子(颜料)与流体的混合物在施加电场时可表现出由于带电物质与周围环境(如封装介质)之间的相互作用所造成的预料不到的行为。另外,预料不到的行为可能由流体、颜料、或封装介质中的杂质造成。因此,难以预测电泳显示器会如何响应内相组成的变化。
当前显示器被确认的一个具体缺点为不期望的颜料粒子之间的反应,以及颜料粒子与用以形成微单元的聚合物材料之间的潜在反应。为了向粒子的表面赋予某种功能性,颜料粒子常被涂覆聚合物。当聚合粒子涂层或微单元聚合膜含有(甲基)丙烯酸酯基团时,粒子可能固化在一起且团聚,或者颜料涂层与微单元的聚合材料例如在暴露于热或UV光时可能交联,因此抑制/防止颜料移动。
因此,需要改善的电泳介质和掺入该介质的显示器。
发明概述
本发明包括改善的电泳介质制剂。改善的性能是由于包括光热诱导的聚合的抑制剂造成的,其防止颜料粒子的聚合物涂层彼此不希望的交联、或颜料粒子的聚合物涂层与形成电泳显示器的多个微单元的聚合物膜或形成聚合物分散型电泳显示器的连续相的聚合物材料的不希望的交联。当包含在用于反射型显示器的电泳粒子分散液中时,包含这些抑制剂中的一些还可提供另外的益处,如改善的白色状态。具体地,本发明包括包含以下的电泳介质:(a)非极性流体、(b)多个第一带电粒子和(c)光热诱导的聚合的抑制剂。
除了第一带电粒子,本发明的电泳介质还可包含另外类型的粒子。例如,该电泳介质可包含第二、第三、第四、第五或第六类带电粒子。所述粒子的电荷、密度、疏水性及/或ζ电位可不同。所述粒子可具有不同的颜色,如洋红色、红色、橙色、黄色、绿色、青色、蓝色、紫色、黑色和白色。所述粒子可为无色的或透明的。该电泳介质可另外包含表面活性剂,如离子表面活性剂,即具有季铵头基的表面活性剂。
本发明的电泳介质可被封装在例如微单元或蛋白质凝聚体中,如背景部分所讨论的。另外,本发明的电泳介质可被分散在聚合物基体中。该封装的或聚合物分散的电泳介质可掺入前面层压板(FPL)和/或电光显示器中,如背景所讨论的。这种材料可用于制造电泳图像显示器(EPID)、标牌或在接收信号时将改变外观的建筑材料。
附图简述
附图仅以示例的方式而非通过限制方式描述了根据本发明构思的一个或多个实施方式。
图1是绘制各种电泳显示样品、一种对照样品和包含含有根据本发明各个实施方案的抑制剂的分散液的七种样品的白色状态(WL*)的图。
发明详述
各类电泳介质的性能可通过包含本文所述的抑制剂得到改善。例如,对于多种用于电泳显示器的颜料,本发明的抑制剂可在暴露于热和/或光之后保留亮(开)与暗(关)状态之间的对比。另外,该抑制剂降低被称为“重影”的现象的在显示器已在图像之间切换之后残余图像的入射和强度。
如背景所讨论的,被掺入电泳介质的分散液的颜料可包括聚合壳或涂层,以赋予某种功能性或提供反应性基团以改变颜料粒子的表面化学。该聚合物通常包括(甲基)丙烯酸酯基团。类似地,用以形成封装该分散液的微单元或粘结剂的聚合物材料也可包含含(甲基)丙烯酸酯基团的聚合物。如本文在整个说明书和权利要求书中所使用的,“(甲基))丙烯酸酯”意指甲基丙烯酸酯和/或丙烯酸酯。被掺入根据本发明的各实施方案的电泳介质中的抑制剂抑制和/或防止颜料的(甲基)丙烯酸酯基团与微单元之间交联的可能性,所述交联可能在电泳显示器暴露于热和/或光时发生。通过降低/消除颜料粒子彼此固化或固化到微单元或粘结剂的可能性,可保留颜料粒子的移动,从而得到暴露于热和/或光的显示器随时间改善的性能。
一般地,可包含在本发明的各实施方案中的光热诱导的聚合的抑制剂可包括但不限于具有不饱和烃环和羟基基团、羰基基团和亚硝基基团中的至少一种的化合物。更具体地,该抑制剂可包括但不限于酚/含苯氧基化合物(例如二叔丁基对甲酚、2,6-二叔丁基-4-甲基酚、4,4’-亚甲基双(2,6-二叔丁基酚)、1,5-萘二酚、2,6-二叔丁基对甲酚、2,2’-亚甲基双(6-叔丁基对甲酚)、4,4’-双酚、4,4’-亚丁基双(6-叔丁基-3-甲基酚)、4-叔丁基酚、4-甲氧基酚、硫代双(二仲戊基酚)和3,5-二叔丁基-4-羟基苄醇)、儿茶酚(例如1,4-双(3,4-二羟基苯基)-2,3-二甲基丁烷、4-甲基儿茶酚和4-叔丁基-5-甲氧基儿茶酚)、间苯二酚(例如4-甲基间苯二酚、4-丁基间苯二酚、5-十三基间苯二酚、5-十五基间苯二酚和5-(1,2-二甲基庚基)-1,3-苯二酚)、氢醌(例如叔丁基氢醌、2,5-二叔丁基氢醌、2,5-双-(1,1,3,3-四甲基丁基)-苯-1,4-二酚、甲基氢醌、三甲基氢醌、2,3-二甲基氢醌和2,5-二叔戊基氢醌)、苯醌(例如3,5-二叔丁基邻苯醌、2,6-二叔丁基-1,4-苯醌、2,5-二叔丁基-1,4-苯醌、2-叔丁基-1,4-苯醌、4-叔丁基-5-甲氧基邻苯醌、3,6-二叔丁基-1,2-苯醌、甲基对苯醌和3-叔丁基-5-甲氧基邻苯醌)、含亚硝基基团的芳族化合物(例如三(N-亚硝基-N-苯基羟基胺)铝盐、4-亚硝基二甲基苯胺和1,3,5-三叔丁基-2-亚硝基苯)、及其组合。该抑制剂可以以基于分散液的总重量0.01%至10%的浓度加入电泳介质,更优选地,添加剂的重量百分比为基于分散液的总重量为0.1%至5%。
该抑制剂可用于包含在有机溶剂中的官能化颜料的电泳介质。该介质可被掺入显示器中、或掺入连接至背板以制造显示器的前面层压板或倒置前面层压板中。本发明的电泳介质,即含光热诱导的聚合的抑制剂的电泳介质可仅包括例如用于黑/白显示器的黑色颜料和白色颜料。本发明的电泳介质也可用于彩色显示器中,且含有例如三、四、五、六、七或八种不同类型的粒子。在一个实施方案中,可构建一种电泳显示器,其中,电泳介质中的粒子包括黑色、白色和红色,或黑色、白色和黄色。供选择地,该介质可包括红色、绿色和蓝色粒子,或青色、洋红色和黄色粒子,或红色、绿色、蓝色和黄色粒子。
术语灰色状态在本文中以其在成像领域的常规意义使用,以指代像素的两个极端光学状态中间的状态,且未必暗示这两种极端状态之间的黑-白过渡。例如几个以下参考的E Ink专利和公开申请描述了其中极端状态为白色和深蓝色,使得中间灰色状态实际上为浅蓝色的电泳显示器。事实上,如所提到的,光学状态变化可能根本不是颜色变化。术语黑和白可在下文用以指代显示器的两个极端光学状态,且应理解为通常包括并非为严格的黑和白的极端光学状态,例如前面的白色与深蓝色状态。
术语“双稳态的”和“双稳态性”在本文中以其在本领域中的常规含义使用,以指代包括具有在至少一种光学性质上不同的第一和第二显示状态的显示元件的显示器,并且使得已经在通过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,在寻址脉冲终止后,该状态将持续改变显示元件的状态所需寻址脉冲的最小持续时间的至少几倍,例如至少四倍。第7170670号美国专利中示出了一些基于粒子的能显示灰阶的电泳显示器不仅在它们的极端黑色和白色状态下稳定,而且在它们的中间灰度状态下也是稳定的,并且对于一些其它类型的电光显示器也是如此。这种类型的显示器被适当地称为“多稳态的”,而不是双稳态的,但是为了方便,术语“双稳态的”在本文中可以用于涵盖双稳态的显示器和多稳态的显示器两者。
内相的封装可以以许多种不同的方式完成。许多合适的微封装步骤详述于微封装、方法和应用(Microencapsulation,Processes and Applications),(I.E.Vandegaer编辑),Plenum出版社,New York,N.Y.(1974)和Gutcho的微囊和微封装技术(Microcapsulesand Microencapsulation Techniques),Noyes Data Corp.,Park Ridge,N.J.(1976)。该方法落入几个大类,其均可适用于本发明:界面聚合、原位聚合、物理方法,如共挤出及其他相分离方法、在液体中固化(in-liquid curing)和简单/复杂凝聚。
许多材料及方法将被证明在本发明的显示器配制中有用。用于简单凝聚方法以形成囊的有用材料包括但不限于明胶、聚(乙烯醇)、聚(乙酸乙烯酯)和纤维素衍生物,例如羧甲基纤维素。用于复杂凝聚方法的有用材料包括但不限于明胶、***胶、卡拉胶、羧甲基纤维素、水解苯乙烯酐共聚物、琼脂、藻酸盐、酪蛋白、白蛋白、甲基乙烯基醚共聚顺丁烯二酐和纤维素苯二甲酸酯。用于相分离方法的有用材料包括但不限于聚苯乙烯、聚(甲基丙烯酸甲酯)(PMMA)、聚(甲基丙烯酸乙酯)、聚(甲基丙烯酸丁酯)、乙基纤维素、聚(乙烯基吡啶)和聚丙烯腈。用于原位聚合方法的有用材料包括但不限于聚羟基酰胺类与醛类、三聚氰胺、或脲与甲醛;三聚氰胺的缩合物的水溶性低聚物、或脲和甲醛;和乙烯基单体,例如苯乙烯、甲基丙烯酸甲酯(MMA)和丙烯腈。最后,用于界面聚合方法的有用材料包括但不限于二酰氯,例如癸二酰基、己二酰基、和二胺或多胺或醇、和异氰酸酯。有用的乳化聚合材料可包括但不限于苯乙烯、乙酸乙烯酯、丙烯酸、丙烯酸丁酯、丙烯酸叔丁酯、甲基丙烯酸甲酯和甲基丙烯酸丁酯。
所产生的囊可以分散在可固化的载体中,得到的油墨可以使用常规的印刷和涂覆技术印刷或涂覆在大的和任意形状或弯曲的表面上。
在本发明的上下文中,本领域技术人员将基于期望的囊性质选择封装过程和壁材料。这些性质包括囊半径的分布;囊壁的电、机械、扩散和光学性质;和与囊的内相的化学相容性。
囊壁通常具有高电阻率。尽管可以使用具有相对低电阻率的壁,但这可能限制需要相对较高寻址电压的性能。囊壁还应该是高机械强度的(尽管如果将完成的囊粉末分散在可固化聚合物粘结剂中用于涂覆,则机械强度不是那么关键)。囊壁通常不应是多孔的。然而,如果期望使用产生多孔囊的封装过程,则可以在后处理步骤(即第二次封装)中对它们进行外涂。此外,如果囊将分散在可固化的粘结剂中,则粘结剂将用于封闭孔。囊壁应该是光学透明的。然而,可选择壁材料以匹配囊的内相(即悬浮流体)或囊待分散于其中的粘结剂的折射率。对于一些应用(例如,两个固定电极之间的***),单分散的囊半径是理想的。
适于本发明的封装技术涉及在带负电荷的羧基取代的直链烃聚电解质材料存在下,在油/水乳液的水相中脲和甲醛之间的聚合。得到的囊壁是脲/甲醛共聚物,其离散地封闭内相。囊透明,机械强度高,并具有良好的电阻性质。
相关的原位聚合技术使用油/水乳液,其通过将电泳流体(即含有颜料粒子的悬浮液的介电液)分散在水性环境中而形成。单体聚合以形成聚合物,其对内相的亲和力高于对水相的亲和力,因此在乳化的油性液滴周围凝结。在一种原位聚合方法中,脲和甲醛在聚(丙烯酸)存在下缩合(参见例如第4001140号美国专利)。在第4273672号美国专利中描述的其他方法中,在水溶液中承载的各种交联剂中的任何一种都沉积在微观油滴周围。这种交联剂包括醛,尤其是甲醛、乙二醛或戊二醛;明矾;锆盐;和多异氰酸酯。
凝聚方法也使用油/水乳液。一种或多种胶体从水相中凝聚(即团聚)出来,并通过控制温度、pH和/或相对浓度作为壳沉积在油滴周围,从而产生微囊。适合凝聚的材料包括明胶和***树胶。参见,例如第2800457号美国专利。
界面聚合方法依赖于电泳组合物中油溶性单体的存在,其再次作为乳液存在于水相中。微小疏水液滴中的单体与引入水相中的单体反应,在液滴和周围水性介质之间的界面处聚合,并在液滴周围形成壳。尽管所得到的壁相对较薄并且可能是可渗透的,但是该方法不需要某些其他方法的升温特性,且因此在选择介电液体方面提供了更大的灵活性。
供选择地,电泳介质可以包含在微制造的单元,即微单元中,例如由E Ink以商品名MICROCUP制造的。例如,如第6930818号美国专利中所述,可以使用阳模以压印导电基材,在导电基材上形成透明导体膜。然后将一层热塑性或热固性前体涂覆在导体膜上。热塑性或热固性前体层在高于热塑性或热固性前体层的玻璃化转变温度的温度下通过辊、板或带形式的阳模进行压花。一旦形成,在前体层硬化期间或之后释放模具以露出微单元阵列。前体层的硬化可以通过冷却、通过辐射、热或湿气交联完成。如果通过UV辐射实现热固性材料前体的固化,则UV可以从网的底部或顶部辐射到透明导体膜上,如两幅图所示。供选择地,可以将UV灯放置在模具内。在这种情况下,模具必须是透明的,以允许UV光通过预先图案化的阳模辐射到热固性前体层上。
用于制备微单元的热塑性或热固性前体可以是多官能丙烯酸酯或甲基丙烯酸酯、乙烯基醚、环氧化物及其低聚物、聚合物等。通常还添加赋予柔韧性的可交联低聚物,例如氨基甲酸酯丙烯酸酯或聚酯丙烯酸酯,以改善压花的微杯的抗弯曲性。该组合物可含有聚合物、低聚物、单体和添加剂或仅含有低聚物、单体和添加剂。
通常,微单元可以是任何形状,并且它们的尺寸和形状可以变化。微单元在一个***中可具有基本均匀的尺寸和形状。然而,为了使光学效果最大化,可以制备具有不同形状和尺寸的混合物的微单元。例如,填充有红色分散液的微单元可以具有与绿色微单元或蓝色微单元不同的形状或尺寸。此外,像素可以由不同数量的不同颜色的微单元组成。例如,像素可以由许多小的绿色微单元,许多大的红色微单元和许多小的蓝色微单元组成。三种颜色的形状和数量不必相同。
微单元的开口可以是圆形、方形、矩形、六边形或任何其他形状。优选保持小的开口之间的分隔区域,以便在保持期望的机械性能的同时实现高色彩饱和度和对比度。因此,蜂窝状开口优于例如圆形开口。
对于反射型电泳显示器,每个单独的微单元的尺寸范围可以为约102至约5×105μm2,优选约103至约5×104μm2。微单元的深度范围为约3至约100微米,优选约10至约50微米。开口与壁的比率范围为约0.05至约100,优选约0.4至约20。开口的距离范围从开口的边缘到边缘通常为约15至约450微米,优选约25至约300微米。
许多上述专利和申请认识到,封装的电泳介质中的离散微囊周围的壁可以被连续相代替,由此产生所谓的聚合物分散的电泳显示器,其中电泳介质包括多个离散的电泳流体滴和聚合物材料的连续相,并且即使没有离散的囊膜与每个单独的液滴相关联,这种聚合物分散的电泳显示器内的电泳流体的离散液滴也可以被认为是囊或微囊;例如,参见第6866760号美国专利。因此,出于本申请的目的,这种聚合物分散的电泳介质被认为是封装的电泳介质的子种类。
如上所述,电泳介质需要存在流体。在大多数现有技术的电泳介质中,该流体是液体,但是电泳介质可以使用气态流体制备。例如,参见Kitamura,T.等人,Electrical tonermovement for electronic paper-like display,IDW日本,2001,论文HCS1-1,和Yamaguchi,Y.等人,Toner display using insulative particles chargedtriboelectrically,IDW日本,2001年,论文AMD4-4)。还参见第7321459和7236291号美国专利。当介质以允许像基于液体的电泳介质那样的粒子沉降的方向使用时,例如在介质被设置在竖直平面的标牌中,这种基于气体的电泳介质似乎易于受到因这种粒子沉降造成的相同类型问题的影响。实际上,粒子沉降在基于气体的电泳介质中似乎是比在基于液体的介质中更严重的问题,因为与液体悬浮液相比,气态悬浮流体的较低粘度使得电泳粒子更快速沉降。
封装的电泳显示器通常不会遭受传统电泳装置的聚集和沉降失效模式的问题,并且提供了进一步的优点,例如在多种柔性和刚性基材上印刷或涂覆显示器的能力。(打印一词的使用旨在包括所有形式的印刷和涂布,包括但不限于:预计量涂布,诸如小块模具涂布(patch die coating)、狭缝或挤出涂布,坡流或阶流涂布,幕式涂布;辊涂,诸如辊衬刮刀涂布、正向和反向辊涂;凹版涂布;浸渍涂布;喷涂;弯月面涂布;旋涂;刷涂;气刀涂布;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(参见第7339715号美国专利);和其它类似技术)。因此,所得到的显示器可以是柔性的。此外,因为可以(使用各种方法)印刷显示介质,所以可以廉价地制造显示器本身。
上述第6982178、6672921、6788449和6866760号美国专利描述了组装电泳显示器(包括封装的电泳显示器)的方法。基本上,这些专利描述了一种层压板,其包括透光导电层和与导电层电接触的固体电光介质层。通常,透光导电层将承载在透光基材上,在基材可以手动缠绕在直径为10英寸(254mm)的鼓上而不永久变形的意义上,该基材优选是柔性的。在本专利中使用术语“透光的”,并且在本文中意指由此指定的层透射足够的光以使观察者能够通过该层观看,以观察电光介质的显示状态的变化,这通常是通过导电层和相邻基材(如果存在)观看的;在电光介质在不可见波长处显示反射率变化的情况下,术语透光的当然应该被解释为指相关非可见波长的透射。基材通常是聚合物膜,并且通常具有范围为约1至约25密耳(25至634μm),优选约2至约10密耳(51至254μm)的厚度。导电层适合为薄金属或金属氧化物层,例如铝或氧化铟锡(ITO)层,或者可以是导电聚合物。涂覆有铝或ITO的聚(对苯二甲酸乙二醇酯)(PET)膜可商购,例如来自E.I.du Pont de Nemours&Company,Wilmington DE的铝化Mylar(Mylar是注册商标),并且这种商业材料可以在前面层压板中使用,具有良好的结果。
电光显示器的组装可以通过在有效使粘合层粘附到背板的条件下用粘合剂将上述层压板连接到背板上,从而使粘合层、电光介质层和导电层固定到背板实现。该方法非常适于大规模生产,因为前面层压板可以批量生产,通常使用卷对卷涂布技术,然后切割成与特定背板一起使用所需的任何尺寸的片。
除了掺入本发明各种实施方案中的光热诱导的聚合的抑制剂之外,电泳介质还可包含电荷控制剂(CCA)。例如,颜料粒子可以用带电基团或可带电基团官能化或表面涂覆。CCA可以被吸收到粒子中,它们可以共价地结合到粒子的表面,并且它们可以存在于电荷复合物中,或者通过范德华力松散地结合。电荷控制剂通常通过难以理解和不受控制的过程使粒子带电,并且可以导致电泳介质的不期望的高导电性。而且,因为电荷控制剂仅被物理吸附在粒子上而不与粒子结合,所以条件的变化可能引起电荷控制剂从粒子部分或完全解吸,结果是粒子的电泳特性的不期望的变化。解吸的电荷控制剂可能再吸收到电泳介质内的其他表面上,并且这种再吸收有可能引起其他问题。
优选包含季胺和包含长度为至少10个碳原子的单体的不饱和聚合物尾部的电荷控制剂。季胺包含与有机分子,例如烷基基团或芳基基团结合的季铵阳离子[NR1R2R3R4]+。季胺电荷控制剂通常包括与带电铵阳离子连接的长的非极性尾部,例如由Akzo Nobel以商品名ARQUAD提供的脂肪酸季胺的家族。季胺电荷控制剂可以以纯化形式购买,或者电荷控制剂可以作为已形成季胺电荷控制剂的反应产物购买。例如,可以购买作为12-羟基-十八烷酸均聚物与N,N-二甲基-1,3-丙二胺和甲基二硫酸盐的反应产物的SOLSPERSE 17000(Lubrizol Corporation)。其它有用的离子电荷控制剂包括但不限于十二烷基苯磺酸钠,金属皂,聚丁烯琥珀酰亚胺,马来酸酐共聚物,乙烯基吡啶共聚物,乙烯基吡咯烷酮共聚物,(甲基)丙烯酸共聚物或N,N-二甲基氨基乙基(甲基)丙烯酸酯共聚物,Alcolec LV30(大豆卵磷脂),Petrostep B100(石油磺酸盐)或B70(磺酸钡),OLOA 11000(琥珀酰亚胺无灰分散剂),OLOA 1200(聚异丁烯琥珀酰亚胺),Unithox 750(乙氧基化物),Petronate L(磺酸钠),Disper BYK 101、2095、185、116、9077和220以及ANTITERRA系列。
对于每100g带电粒子,电荷控制剂可以以大于1g电荷控制剂的浓度添加到电泳介质中。例如,电荷控制剂与带电粒子比可以是1:30(wt/wt),例如1:25(wt/wt),例如1:20(wt/wt)。电荷控制剂的平均分子量可以大于12000克/摩尔,例如大于13000克/摩尔,例如大于14000克/摩尔,例如大于15000克/摩尔,例如大于16000克/摩尔,例如大于17000克/摩尔,例如大于18000克/摩尔,例如大于19000克/摩尔,例如大于20000克/摩尔,例如大于21000克/摩尔。例如,电荷控制剂的平均分子量可以为14000克/摩尔至22000克/摩尔,例如15000克/摩尔至20000克/摩尔。在一些实施方案中,电荷控制剂的平均分子量为约19000克/摩尔。
可以使用另外的电荷控制剂,在聚合物涂层中具有或不具有带电基团,以向电泳粒子提供良好的电泳迁移率。稳定剂可用于防止电泳粒子的聚集,以及防止电泳粒子不可逆地沉积在囊壁上。任一组分都可以由跨宽范围分子量的材料(低分子量、低聚的或聚合的)构成,并且可以是单一纯化合物或混合物。可以使用任选的电荷控制剂或电荷导向剂。这些组分通常由低分子量表面活性剂、聚合试剂或一种或多种组分的共混物组成,并用于稳定或以其它方式改变电泳粒子上电荷的符号和/或大小。可能相关的其他颜料性质是粒度分布、化学组成和耐光性。
如已经指出的,应该基于诸如密度、折射率和溶解度的性质来选择含有粒子的悬浮流体。优选的悬浮流体具有低介电常数(约2)、高体积电阻率(约1015欧姆-厘米)、低粘度(低于5厘沲(“cst”))、低毒性和环境影响、低水溶性(低于百万分之10份(“ppm”))和低折射率(小于1.2)。
非极性流体的选择可以基于对化学惰性、与电泳粒子的密度匹配、或与电泳粒子和结合囊的化学相容性(在封装的电泳显示器的情况下)的关注。当期望移动粒子时,流体的粘度应该低。
非极性有机溶剂,如卤代有机溶剂,饱和直链或支链烃(如C6-C18支链烷烃或C7-C10支链烷烃),硅油和低分子量含卤素聚合物是一些有用的非极性流体。非极性流体可包括单一流体。然而,非极性流体通常是多于一种流体的共混物,以调节其化学和物理性质。此外,非极性流体可包含另外的表面改性剂以改进电泳粒子或结合囊的表面能或电荷。用于微封装过程的反应物或溶剂(例如油溶性单体)也可以包含在悬浮流体中。还可以将另外的电荷控制剂添加到悬浮流体中。
有用的有机溶剂包括但不限于环氧化物,例如癸烷环氧化物和十二烷环氧化物;乙烯基醚,例如环己基乙烯基醚和Decave(International Flavors&Fragrances,Inc.,NewYork,N.Y.的注册商标);和芳烃,如甲苯和萘。有用的卤代有机溶剂包括但不限于四氟二溴乙烯、四氯乙烯、三氟氯乙烯、1,2,4-三氯苯和四氯化碳。这些材料具有高密度。有用的烃包括但不限于十二烷、十四烷、Isopar(注册商标)系列中的脂族烃(Exxon,Houston,Tex.)、Norpar(注册商标)(一系列正链烷烃液体)、Shell-Sol(注册商标)(Shell,Houston,Tex.)和Sol-Trol(注册商标)(Shell)、石脑油和其他石油溶剂。这些材料通常具有低密度。硅油的有用实例包括但不限于八甲基环硅氧烷和更高分子量的环状硅氧烷、聚(甲基苯基硅氧烷)、六甲基二硅氧烷和聚二甲基硅氧烷。这些材料通常具有低密度。有用的低分子量含卤素聚合物包括但不限于聚(三氟氯乙烯)聚合物(Halogenated Hydrocarbon Inc.,RiverEdge,N.J.)、Galden(注册商标)(来自Ausimont,Morristown,N.J.的全氟醚)、或来自duPont(Wilmington,Del.)的Krytox(注册商标)。在优选的实施方案中,悬浮流体是聚(三氟氯乙烯)聚合物。在特别优选的实施方案中,该聚合物的聚合度为约2至约10。可获得一系列粘度、密度和沸点的许多上述材料。
在一些实施方案中,非极性流体将包括光学吸收染料。该染料必须可溶于流体中,但通常不溶于囊的其它组分。染料材料的选择有很大的灵活性。染料可以是纯化合物、或染料的共混物以实现特定的颜色,包括黑色。染料可以是荧光的,这将产生其中荧光性质取决于粒子的位置的显示器。染料可以是光活性的,在用可见光或紫外光照射时变成另一种颜色或变成无色,提供另一种获得光学响应的手段。染料也可以通过例如热、光化学或化学扩散方法聚合,在结合壳内形成固体吸收性聚合物。
电泳显示器领域的技术人员已知的许多染料将证明是有用的。有用的偶氮染料包括但不限于:油红染料及苏丹红和苏丹黑系列染料。有用的蒽醌染料包括但不限于:油蓝染料和Macrolex Blue系列染料。有用的三苯基甲烷染料包括但不限于Michler's hydrol、孔雀石绿、结晶紫和金胺(Auramine)O。核粒子可以是无机颜料,例如TiO2、ZrO2、ZnO、Al2O3、CI颜料黑26或28或类似物(例如,铁锰黑尖晶石或铜铬黑尖晶石),或有机颜料,例如酞菁蓝、酞菁绿、二芳基黄、二芳基AAOT黄、和喹吖啶酮、偶氮、罗丹明、来自Sun Chemical的苝(perylene)颜料系列,来自Kanto Chemical的Hansa黄G粒子和来自Fisher的碳灯黑(Carbon Lampblack)等。
还可以加入粒子分散稳定剂以防止粒子絮凝或附着到囊壁上。对于在电泳显示器中用作悬浮流体的典型高电阻率液体,可以使用非水表面活性剂。这些包括但不限于乙二醇醚、乙炔二醇、链烷醇酰胺、山梨糖醇衍生物、烷基胺、季胺、咪唑啉、二烷基氧化物和磺基琥珀酸酯。
如果需要双稳态电泳介质,可能期望在悬浮流体中包括数均分子量超过约20000的聚合物,该聚合物在电泳粒子上基本上不吸收;聚(异丁烯)是用于此目的的优选聚合物。参见第7170670号美国专利,其全部公开内容通过引用并入本文。
一旦被封装,根据本发明的各个实施方案的电泳介质可以与粘结剂和/或施加剂组合以改善电泳显示器的构造。例如,涂布助剂可用于改善涂布或印刷的电泳油墨材料的均匀性和质量。可加入润湿剂以调节涂层/基材界面处的界面张力并调节液体/空气表面张力。润湿剂包括但不限于阴离子和阳离子表面活性剂,和非离子物质,例如硅氧烷或含氟聚合物基材料。分散剂可用于改进囊和粘结剂之间的界面张力,提供对絮凝和粒子沉降的控制。
实施例
现在给出实施例,但仅通过说明的方式给出,以显示本发明的优选电泳介质的细节。
实施例1-
如第6930818号美国专利所述制备2片微单元膜,该美国专利的内容通过引用整体并入本文。通过将电泳介质涂覆在具有该微单元膜的前面层压板上随后将前面层压板层压于具有TFT阵列的背板,制备含有7,2,6-二叔丁基对甲酚(TBPC)或三(N-亚硝基-N-苯基羟基胺)铝盐(NNNPA)相对于电泳粒子的浓度为1:200(重量/重量)的电泳介质,用于测试显示器。
首先将该显示器以5伏波形(LV)驱动到白色状态(W)或黑色状态(K),然后置于Qsun室持续3天,之后再测试性能。使用具有D65照射的X-rite iOne分光光度计(GrandRapids,MI的X-rite),评估显示器在明暗状态的相对反射和色彩。使用CIExyY及CIELAB色彩空间算法报告数据。通过在明暗图像之间驱动显示器且评估当从明图像到暗图像时的剩余反射量和当从暗图像到明图像时的反射减少量而确定重影程度。实际上,在正与负棋盘图案之间驱动每个显示器,同时在数个位置测量L*变化,从而实现在少量时间内收集许多相关数据点。结果提供于表1中。
表1.在Q-sun之后有/无TBPC的LV性能比较
表1的结果证实,当以1:200重量/重量添加时,添加TBPC将Qsun暴露3天后的K衰减降低大约50%,以及将K重影降低大约40%。TBPC还导致稍微改善的白色状态反射率。
实施例2-
依照实施例1的过程制备电泳介质并将其掺入显示器样品中,除了使用的光热诱导的聚合的抑制剂为三(N-亚硝基-N-苯基羟基胺)铝盐(NNNPA)而非TBPC之外。然后使用类似实施例1的方法测试样品,结果提供于表3中,以及使用其中将显示器样品置于60C的室持续3天的改进测试来测试样品,结果提供于表2中。
表2.暴露于60C热后有/无NNNPA的LV性能比较
表3.在Q-sun室中暴露后有/无NNNPA的LV性能比较
以上表2和3的结果证实,在3天60C运行测试之后,添加1:200重量/重量的NNNPA将W状态改善33%,以及将K状态改善52%。在Qsun曝光测试之后当驱动到K状态时,添加1:200重量/重量的NNNPA还将W状态改善49%,以及将K状态改善53%。在Qsun曝光期间,当驱动到W状态和K状态时,Qsun曝光后的K重影程度也分别改善52%及33%。
实施例3-
依照实施例1所注明的过程制备微单元膜。将8种不同的电泳介质制剂涂覆在具有该微单元膜的前面层压板上,继而将前面层压板层压于ITO玻璃背板而制备显示器样品。全部8种电泳介质制剂均含有白色、黑色、红色和黄色电泳粒子。对照样品不含抑制剂,而其余7种样品中的每一种含有相对于电泳粒子的浓度为1:200(重量/重量)的以下抑制剂之一:三(3,5-二叔丁基-4-羟基苄基)异氰酸酯(“AO-20”)、4,4’,4”-(1-甲基亚丙-3-基)三[6-叔丁基间甲酚](“AO-30”)、1,3,5-三甲基-2,4,6-三(3,5-二叔丁基-4-羟基苄基)苯(“AO-330”)、4,4’-亚丁基二(6-叔丁基间甲酚)(“AO-40”)、3-(3,5-二叔丁基-4-羟基苯基)丙酸十八酯(“AO-50”))、季戊四醇四(3,5-二叔丁基-4-羟基氢肉桂酸酯)(“AO-60”)和3,9-双1,1-二甲基-2-(3-叔丁基-4-羟基-5-甲基苯基)丙酰氧基乙基-2,4,8,10-四氧杂螺[5.5]十一烷(“AO-80”)。使用具有D65照射的X-rite iOne分光光度计(MI Grand Rapids的X-rite)评估显示器在明暗状态下的相对反射及色彩。使用CIELAB色彩空间算法报告数据。
如图1所述,AO-30和AO-40样品相较于其他样品表现出改善的明状态。因此,包括特定聚合抑制剂可提供额外的益处,如当被包括于反射型显示器的电泳粒子分散液时改善的白色状态。
如上所示,本发明提供可被包括于电泳介质中以改善介质的性能的光热诱导的聚合的抑制剂。
可对上述本发明的具体实施方案进行许多变化和修改而不背离本发明的范围对所属技术领域人员是明显的。因此,以上说明书全部以示例性意义而非限制性意义解读。
Claims (20)
1.一种包含分散液的电泳介质,所述分散液包含:
(a)非极性流体;
(b)多个第一带电粒子;和
(c)光热诱导的聚合的抑制剂。
2.权利要求1所述的电泳介质,其中所述抑制剂包含不饱和烃环和羟基基团、羰基基团和亚硝基基团中的至少一种。
3.权利要求1所述的电泳介质,其中所述抑制剂选自酚、含苯氧基的化合物、儿茶酚、间苯二酚、氢醌和苯醌。
4.权利要求1所述的电泳介质,其中所述抑制剂是7,2,6-二叔丁基对甲酚。
5.权利要求1所述的电泳介质,其中所述抑制剂是三(N-亚硝基-N-苯基羟基胺)铝盐。
6.权利要求1所述的电泳介质,其中所述抑制剂是苯醌。
7.权利要求6所述的电泳介质,其中所述抑制剂是3,5-二叔丁基邻苯醌。
8.权利要求1所述的电泳介质,其中所述抑制剂是氢醌。
9.权利要求8所述的电泳介质,其中所述抑制剂是2,5-二叔丁基氢醌。
10.权利要求1所述的电泳介质,其中所述抑制剂选自4,4'-亚丁基双(6-叔丁基间甲酚)和4,4',4”-(1-甲基亚丙-3-基)三[6-叔丁基间甲酚]。
11.权利要求1所述的电泳介质,其中所述第一带电粒子包括含有(甲基)丙烯酸酯基团的聚合物涂层。
12.权利要求11所述的电泳介质,其中所述分散液被封装在包含含有(甲基)丙烯酸酯基团的聚合物材料的多个微单元或聚合物连续相内。
13.权利要求1所述的电泳介质,其中所述分散液被封装。
14.权利要求13所述的电泳介质,其中所述分散液被封装在包含含有(甲基)丙烯酸酯基团的聚合物材料的多个微单元或聚合物连续相内。
15.权利要求1所述的电泳介质,其还包含分散在所述非极性流体中的多个第二带电粒子,其中所述第一带电粒子和第二带电粒子具有相反的电荷,并且所述第一带电粒子和第二带电粒子中的至少一种包含含有(甲基)丙烯酸酯基团的聚合物涂层。
16.权利要求15所述的电泳介质,其中所述分散液被封装在包含含有(甲基)丙烯酸酯基团的聚合物材料的多个微单元或聚合物连续相中。
17.权利要求1所述的电泳介质,其中所述第一带电粒子包含二氧化钛、炭黑或亚铬酸铜。
18.权利要求1所述的电泳介质,其中添加剂的重量百分比为基于分散液的总重量的0.01%至10%。
19.权利要求1所述的电泳介质,其中添加剂的重量百分比为基于分散液的总重量的0.1%至5%。
20.权利要求1所述的电泳介质,其还包含分散在所述非极性流体中的多个第二带电粒子和多个第三带电粒子,其中,所述第一带电粒子、第二带电粒子或第三带电粒子中的每一种是选自红色、绿色、蓝色、青色、黄色和洋红色的不同颜色。
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WO2018164863A1 (en) | 2018-09-13 |
TW201903071A (zh) | 2019-01-16 |
TWI673334B (zh) | 2019-10-01 |
US20180259823A1 (en) | 2018-09-13 |
CN110383164B (zh) | 2023-05-02 |
EP3593205A4 (en) | 2020-11-25 |
EP3593205A1 (en) | 2020-01-15 |
US10585325B2 (en) | 2020-03-10 |
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