CN111399300B - 具有边缘保护的电致变色膜 - Google Patents
具有边缘保护的电致变色膜 Download PDFInfo
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- CN111399300B CN111399300B CN201911095986.4A CN201911095986A CN111399300B CN 111399300 B CN111399300 B CN 111399300B CN 201911095986 A CN201911095986 A CN 201911095986A CN 111399300 B CN111399300 B CN 111399300B
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- electrochromic
- edge
- electrochromic film
- film
- edge protection
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Abstract
本申请公开了一种用于制备电致变色装置的方法。该方法包括在第一基板和第二基板上设置边缘保护材料，在第一基板和第二基板上的边缘保护材料内分别设置第一中间层和第二中间层，其中边缘保护材料围绕第一中间层和第二中间层的边缘，并且在第一中间层和第二中间层之间插入电致变色膜。边缘保护材料防止第一中间层和第二中间层中的化学物进入电致变色膜。
Description
技术领域
本发明总体涉及电致变色装置，并且尤其涉及具有边缘保护的电致变色装置以及用于制造该电致变色装置的方法。
背景技术
电致变色通常是指在施加电势时材料的光学性质的可逆变化。特别地，由于施加电场引起的电化学氧化还原反应，电致变色材料表现出可逆的颜色变化。
电致变色材料可用于多种应用，包括光伏器件、场效应晶体管、有机发光二极管、通用印刷电子产品、防眩窗、显示系统等。
通常，将电致变色材料夹在刚性基板之间以制造装置。基于柔性基板的电致变色膜在重量、运输方便性、曲面上的应用能力等方面均优于传统电致变色玻璃。
对于涉及智能窗技术的应用，电致变色材料需要与玻璃基板(例如，玻璃窗)集成来供使用。集成工艺通常要求将电致变色膜夹在两个具有中间层(例如，聚乙烯醇缩丁醛(PVB)和SentryGlas等)的玻璃板之间。然后，在一定压力和温度下对这些封装件加压和加热。在层压工艺之后，中间层将被固化并且将电致变色膜固定在玻璃板之间。为了化学和物理性质的改变，在中间层内存在某些添加剂。这些添加剂能够渗透到多层电致变色膜中并且不利地影响电致变色膜。结果，电致变色膜的性能和寿命会受到严重损害。
因此，需要一种改进的电致变色膜设计以解决上述和其它问题。
发明内容
本公开提出一种制备具有边缘保护的电致变色膜的方法，以防止不期望的材料以及氧气和水分渗入电致变色膜的边缘。电致变色膜可以包括第一电极、第二电极、沉积在至少第一电极上的电致变色材料、沉积在第二电极上的电荷存储层以及设置在电致变色材料和电荷存储层之间的固体聚合物电解质。
通常电致变色膜可以插入两个中间层之间并且层压在两个玻璃板之间。在一些实施例中，电致变色膜的边缘和中间层由边缘保护材料覆盖以防止电致变色膜暴露于来自中间层和周围环境的不期望的材料。这些不期望的材料包括中间层内的某些添加剂以及来自周围环境的氧气和水分，这些可能不利地影响电致变色膜的性能和寿命。
根据本公开的一个实施例，用于制备电致变色装置的方法包括在第一基板和第二基板上设置边缘保护材料，在第一基板和第二基板上的边缘保护材料内分别设置第一中间层和第二中间层，其中边缘保护材料围绕第一中间层和第二中间层的边缘，在第一中间层和第二中间层之间插入电致变色膜，其中边缘保护材料防止第一中间层和第二中间层中的化学物进入电致变色膜。该方法还可以包括：将第一基板和第二基板朝向彼此按压并且加热第一中间层和第二中间层以将电致变色膜固定在第一基板和第二基板之间。
根据本公开的另一实施例，电致变色膜包括第一电极、第二电极、沉积在至少第一电极上的电致变色材料、沉积在第二电极上的电荷存储层以及设置在电致变色材料和电荷存储层之间的固体聚合物电解质。在该实施例中，至少电致变色材料的边缘由边缘保护材料覆盖。
根据本公开的又一实施例，电致变色装置包括第一玻璃板、位于第一玻璃板上的第一中间层、第二玻璃板、位于第二玻璃板上的第二中间层以及位于第一中间层和第二中间层之间的电致变色膜。电致变色膜可以包括第一电极、第二电极、沉积在至少第一电极上的电致变色材料、沉积在第二电极上的电荷存储层以及设置在电致变色材料和电荷存储层之间的固体聚合物电解质。至少电致变色材料的边缘由边缘保护材料覆盖。
附图说明
通过参考附图，可以更容易地理解本发明的优选非限制性实施例，其中：
图1是根据一个示例性实施例的在其中设置有电致变色膜的层压结构的简化示意图。
图2是根据一个示例性实施例的电致变色膜的简化示意图。
图3是根据一个示例性实施例的电致变色膜的透视图。
图4A至4C示出根据示例性实施例的制备具有边缘保护的电致变色膜的方法。
图5示出根据示例性实施例的制备电致变色装置的方法的流程图。
图6示出根据示例性实施例的具有边缘保护的电致变色膜。
图7示出根据一个示例性实施例的具有边缘保护的层压电致变色膜。
图8示出根据另一示例性实施例的具有边缘保护的非层压电致变色膜。
图9示出根据另一示例性实施例的具有边缘保护的另一层压电致变色膜。
图10A示出根据实施例的具有边缘保护的层压电致变色膜和不具有边缘保护的层压电致变色膜的性能和寿命的比较。
图10B示出根据实施例的具有边缘保护的非层压电致变色膜和不具有边缘保护的非层压电致变色膜的性能和寿命的比较。
具体实施方式
在以下描述中，阐述了一些具体细节以提供对本发明的各种实施例的充分理解。然而，本领域技术人员将理解，可以在没有这些细节的情况下实践本发明。此外，尽管本文公开了本发明的各种实施例，但是根据本领域技术人员的公知常识，可以在本发明的范围内做出许多调整和修改。这样的修改包括用已知等效物替代本发明的任何方面，以便以基本上相同的方式获得相同的结果。
除非上下文另有要求，否则在整个说明书和权利要求中，词语“包括(comprise)”及其变体，例如“包括(comprises)”和“包括(comprising)”应被解释为开放的包括含义，即“包括，但是不限于”。在整个说明书中，数值范围的记载旨在用作分别表示在包括限定范围的值的范围内的每个单独值的简化符号，并且每个单独值如单独在本文中记载的那样并入说明书中。另外，单数形式“一(a)”、“一(an)”和“该”包括复数指示物，除非上下文另有明确规定。
在本说明书中，提到“一个实施例”或者“实施例”时，指的是结合该实施例描述的特定特征、结构或者特性包含在本发明的至少一个实施例中。因此，在本说明书中各个地方出现的短语“在一个实施例中”或者“在实施例中”不一定都是指同一实施例，而是在某些情况下可能是这样。此外，特定特征、结构或者特性可以以任何合适的方式结合在一个或更多个实施例中。
图1示出根据一个示例性实施例的在其中插入有电致变色膜的层压结构的简化示意图。仅为了清楚起见，间隔开地示出层压结构的各种组件(例如，基板层、粘合剂层和电致变色膜)。
如图1所示，层压结构100包括第一粘合剂中间层102，第一粘合剂中间层102插入电致变色膜106的第一表面104和第一基板108。层压结构100还包括第二粘合剂中间层110，第二粘合剂中间层110插入电致变色膜106的第二表面112和第二基板114之间。如图1的实施例中所示，第一表面104和第二表面112对应于电致变色膜106的相反表面。
第一粘合剂中间层102和/或第二粘合剂中间层110可以包括配置为将电致变色膜106与第一基板108和第二基板114牢固黏合(例如，交联)的材料(例如，热固性聚合物材料)。因此，第一粘合剂中间层102和/或第二粘合剂中间层110配置为即使在破碎/断裂时也将层压结构100保持在一起，并且防止层压结构100断裂成大的、尖锐的碎片。
图2示出根据一个实施例的电致变色膜200的示例性、非限制性示意图。值得注意的是，可以结合本文所述的其它装置/特征/组件，例如，参考其它实施例/方面描述的那些装置/特征/组件来实现图2的电致变色膜200。电致变色膜200可以用在各种应用和/或排列中，这些应用和/或排列在本文描述的说明性实施例/方面中可能被提到或未被提到。例如，在一些实施例中，电致变色膜200可以包括比图2中所示的特征/组件更多或更少的特征/组件。另外，除了另外指定，如本领域技术人员在阅读本公开后将认识到的，电致变色膜200的一个或更多个组件可以是常规材料、设计和/或使用已知技术(例如，溅射、化学气相沉积(CVD)、物理气相沉积(PVD)、等离子增强化学气相沉积(PECVD)、喷涂、槽模涂覆、浸涂、旋涂、印刷等)制造。
如图2所示，电致变色膜200包括彼此平行、间隔开的第一透明基板202和第二透明基板204。第一基板202和第二基板204可以具有相同或不同尺寸，包括相同或不同材料等。用于第一基板202和/或第二基板204的合适材料可以包括，但不限于，玻璃、聚合物材料、塑料材料和/或在电磁光谱的可视区域的至少一部分中透明的其它材料。在一些实施例中，第一基板202和第二基板204可以包括玻璃。
如图2所示，第一透明导电膜206沉积在第一基板202的内表面208上以用作电极。第二透明导电膜210也沉积在第二基板204的内表面212上以用作电极。第一导电膜206和第二导电膜210可以具有相同或不同尺寸，包括相同或不同材料等。第一导电膜206和第二导电膜210还可以各自独立地具有单层或多层结构。用于第一导电膜206和第二导电膜210的合适材料可以包括，但不限于掺锡氧化铟(ITO)、掺氟氧化铟、掺锑氧化铟、掺锌氧化铟、掺铝氧化锌、银纳米线、金属网及其组合和/或呈现出足够电导率的其它这种透明材料。在优选方面，第一导电膜206和第二导电膜210可以各自包括含有掺锡氧化铟(ITO)的电极层。
电致变色装置200还可以包括被配置为在第一导电膜206和第二导电膜210之间供应电压的电源(未示出)。
如图2进一步所示，电致变色材料层214沉积在第一导电膜206的内表面216上。电致变色材料层214配置为在由施加的电流引起还原(获得电子)或氧化(失去电子)时导致可逆的颜色变化。在一些实施例中，电致变色材料层214可以配置为在氧化或还原时从透明状态改变为有色状态，或从一有色状态改变为另一有色状态。在一些实施例中，电致变色材料层214可以是其中可能有多于两种氧化还原状态的多电致变色材料(polyelectrochromicmaterial)，并且因此可以呈现几种颜色。
在一些实施例中，电致变色材料层214可以包括有机电致变色材料、无机电致变色材料、两者的混合物等。电致变色材料层214也可以是还原有色材料(即，在获得电子时变成有色的材料)或氧化有色材料(即，在失去电子时变成有色的材料)。
在一些实施例中，电致变色材料层214可以包括金属氧化物，例如MoO3、V2O5、Nb2O5、WO3、TiO2、Ir(OH)x、SrTiO3、ZrO2、La2O3、CaTiO3、钛酸钠、铌酸钾及其组合等。在一些实施例中，电致变色材料层214可以包括导电聚合物，例如，聚-3,4-乙烯二氧噻吩(PEDOT)、聚-2,2’-联噻吩、聚吡咯、聚苯胺(PANI)、聚噻吩、聚异苯并噻吩、聚(邻氨基苯酚)、聚吡啶、聚吲哚、聚咔唑、聚醌、八氰基酞菁及其组合等。此外，在一些实施例中，电致变色材料层214可以包括诸如紫精、蒽醌、吩噻嗪及其组合等的材料。电致变色材料的另外示例、尤其是包括多色电致变色聚合物的那些可以在2017年1月6日提交的第15/399,839号美国专利申请中找到，该申请的全部内容通过引用并入本文。
如图2另外所示，电荷存储层218沉积在第二导电膜210的内表面220上。用于电荷存储层218的合适材料可以包括，但不限于氧化钒、二元氧化物(例如，CoO、IrO2、MnO、NiO和PrOx)、三元氧化物(例如，CexVyOz)等。
在一些实施例中，电荷存储层218可以用可选的第二电致变色材料层代替。该可选的第二电致变色材料层可以具有与第一电致变色材料层214相同或不同的尺寸，包括与第一电致变色材料层214相同或不同的组分等。
电致变色装置200还包括设置在电致变色材料层214和电荷存储层218之间的电解质层222。在一些实施例中，电解质层222可以包括本领域已知的液体电解质。在一些实施例中，电解质层222可以包括固态电解质，包括但不限于Ta2O5、MgF、Li3N、LiPO4、LiBO2-Li2SO4等。在一些实施例中，电解质层222可以包括基于聚合物的电解质，其包括电解质盐(例如，LiTFSI、LiPF6、LiBF4、LiClO4、LiCF3SO3、LiN(CF3SO2)2、LiSbFg、LiAsF6、LiN(CF3CF2SO2)2、(C2H5)4NBF4、(C2H5)3CH3NBF4、LiI等)、聚合物基质(例如，聚环氧乙烷、聚偏二氟乙烯(PVDF)、聚甲基丙烯酸甲酯(PMMA)、聚环氧乙烷(PEO)、聚丙烯腈(PAN)、聚乙烯腈等)以及一种或更多种可选的增塑剂(例如，戊二腈、丁二腈、己二腈、富马酸腈等)。电介质材料的另外示例、尤其是包括固体聚合物电解质的那些可以在2017年1月6日提交的第15/399,852号和2017年4月13日提交的第15/487,325号美国专利申请中找到，以上两个申请的全部内容通过引用并入本文。
图3是根据一个示例性实施例的电致变色膜300的透视图。图2和图3的不同在于，在图3中仅以透视图示出电致变色膜300，而不具有图2中的第一透明基板202和第二透明基板204。与图2类似，电致变色膜300包括第一透明导电膜306和第二透明导电膜310。在第一透明导电膜306和第二透明导电膜310之间，电致变色膜300还包括电介质层322，该电介质层设置在电致变色材料层314和电荷存储层318之间。在一些实施例中，聚合物电介质层322是固体聚合物电解质，并且固体聚合物电解质包括以上关于图2中的实施例所述的电解质盐和聚合物基质。
图4A至4C示出根据一个示例性实施例的制备具有边缘保护的层压电致变色装置的方法400。图4A示出制造具有边缘保护的玻璃板以用于与电致变色膜层压的工艺。在图4A中，首先制备玻璃板402。然后，将由边缘保护材料制成的四条边缘密封件405设置在四个边缘中的每一个上和玻璃板402的顶部。边缘保护材料可选自聚乙烯基硅氧烷(PVS)、SentryGlas、热塑性聚氨酯(TPU)、乙烯乙酸乙烯酯(EVA)等。接着，在玻璃板402的中心上、由四条边缘密封件405限定的区域内设置中间层403以形成第一中间层基板部分410。中间层403可以由聚乙烯醇缩丁醛(PVB)、紫外线额外保护的PVB等。如上所述，中间层可能包含会不利地影响电致变色膜的性能和寿命的不期望的化学物。通常，这些化学物可以经常经由电介质层通过膜的接合而渗入电致变色膜。通过边缘保护，中间层403的边缘被密封，并且化学物将不能够进入电致变色膜。能够使用相同工艺形成另一个中间层基板。如图4B所示，形成各自具有被边缘保护材料围绕的中间层的两个中间层基板部分410a、410b。电致变色膜401设置且层压在两个中间层基板部分410a、410b之间。能够如上所述参考图1至图3制造电致变色膜401。在图4C中，示出层压在两个玻璃板内的具有边缘保护的电致变色膜420。能够通过按压玻璃板和加热电致变色装置来固化中间层。
图5示出概括图4A至图4C所示的步骤的流程图500。在步骤502中，在第一基板和第二基板上设置边缘保护材料。在步骤504中，将第一中间层和第二中间层分别设置在第一基板和第二基板上的边缘保护材料内，其中，边缘保护材料围绕第一中间层和第二中间层的边缘。在步骤506中，在第一中间层和第二中间层之间插入电致变色膜。边缘保护材料可以防止第一中间层和第二中间层中的化学物进入电致变色膜。方法500还可以包括可选的步骤508，该步骤将第一基板和第二基板朝向彼此接压并加热第一中间层和第二中间层以在第一基板和第二基板之间固定电致变色膜。
图6是两个电致变色膜606和610的剖面图600，其中两个电致变色膜的接合处和边缘被边缘保护材料(例如，环氧树脂层605)覆盖。在图6中，电致变色材料层614、电介质层622和电荷存储层618夹在两个电致变色膜606和610间。在利用热或紫外线固化后，环氧树脂605能够用作有效的氧气和水分阻滞剂。使用该方法，能够在不牺牲性能和寿命的情况下将电致变色膜卷储存在周围环境中更长时间。环氧树脂也能够替代为其它合适的材料。在一些实施例中，至少第一电极和第二电极中的一个、电致变色材料、固体聚合物电介质和电荷存储层的边缘由边缘保护材料覆盖。
图7示出根据一个示例性实施例的具有边缘保护的层压电致变色装置700。层压电致变色装置700包括位于底部的第一基板702(例如，玻璃板)、位于顶部的第二基板704(例如，玻璃板)、位于第一基板702上的第一中间层703a、位于第二基板704下的第二中间层703b、电致变色膜701以及边缘保护材料705、715，所述边缘保护材料705、715位于第一基板702和第二基板704之间并且围绕中间层703a和703b以及电致变色膜。边缘保护材料705、715与电致变色膜701和基板兼容，但是抵抗中间层703a和703b的化学物。电致变色膜701被预定位，使得其边缘适合边缘保护材料705、715。随后是正常的层压工艺，例如，高压釜，电致变色膜701的边缘将被边缘保护材料705、715保护。
图8示出根据另一示例性实施例的具有边缘保护的电致变色膜800。图8中的电致变色膜包括两个侧面801a和801b，一侧面作为阳极，另一侧面作为阴极。上侧面801a在左侧由边缘保护材料覆盖，并且下侧面801b在右侧由边缘保护材料覆盖。边缘被覆盖的电致变色膜800能够被卷起并且能够在不牺牲性能和寿命的情况下容易地储存在周围环境中更长时间。
图9示出根据另一示例性实施例的具有边缘保护的另一电致变色膜900。与图8类似，图9中的电致变色膜包括两个侧面901a和901b，一侧面作为阳极，另一侧面作为阴极。电致变色膜的边缘901a和901b由边缘保护材料(例如，环氧树脂层905和915)覆盖。在利用热或紫外线固化后，环氧树脂905和环氧树脂915能够用作有效的氧气和水分阻滞剂。然后，能够利用上述层压工艺将电致变色膜层压在两个基板(例如，玻璃板)之间。与图7类似，层压电致变色装置900包括第一基板902(例如，玻璃板)、第二基板904(例如，玻璃板)、第一基板902和第二基板904之间的中间层903以及层压在中间层903内的具有边缘保护的电致变色膜。
在一些实施例中，边缘保护材料，例如，环氧树脂805/815/905/915可以是导电的，使得其能够用作上述实施例中的电极。通过使用导电材料作为边缘保护材料，电致变色膜制造工艺能够节省关于制造电极的一个步骤。可替换地，导电边缘保护材料能够将电流传导到电极层和/或电荷存储层。
图10A示出根据实施例的具有边缘保护的层压电致变色膜和不具有边缘保护的层压电致变色膜的性能和寿命的比较。曲线1002是层压电致变色膜的原始性能，例如，未退化时的性能。该曲线示出未退化的层压电致变色膜随时间变化的归一化透明度的反应。曲线1004示出不具有边缘保护的层压电致变色膜随时间变化的归一化透明度的反应。曲线1006示出具有边缘保护的层压电致变色膜随时间变化的归一化透明度的反应。通过比较图10A中的曲线1002、1004和1006，能够发现不具有边缘保护的装置(曲线1004)显示出非常差的稳定性。在100℃处1小时的加速退化后，装置在变换响应上已经减慢。相反，具有边缘保护的装置(曲线1006)在1个月加速退化应力测试之后仅显示出有限的退化迹象。因此，利用边缘保护，能够更好地防止层压电致变色膜退化。
图10B示出根据实施例的具有边缘保护的非层压电致变色膜和不具有边缘保护的非层压电致变色膜的性能和寿命的比较。曲线1012是非层压电致变色膜的原始性能，例如，未退化时的性能。该曲线示出未退化的非层压电致变色膜随时间变化的归一化透明度的反应。曲线1014示出具有边缘保护的非层压电致变色膜随时间变化的归一化透明度的反应。如图10B中所示，在1周的加速退化应力测试之后，具有边缘保护的装置(曲线1014)仍维持合理的良好变换速度，即，与原始曲线1012类似。因此，具有边缘保护，非层压电致变色膜能够防止退化，为进一步的层压工艺保留长的工艺窗口。
本说明书描述了通常通过卷对卷(roll-to-roll)工艺以低成本制造的电致变色膜的保护边缘。由于在电致变色膜的实际应用中，例如，智能窗口，电致变色膜需要层压在基板(例如，两个玻璃板)之间，因此在不使用上述方法的情况下，层压中间层材料的选择将受到限制，并且存储和运输将需要更加专门的环境和条件。上述实施例有助于促进电致变色膜在窗工业中的应用。
本文描述和要求保护的发明的范围不受本文公开的特定优选实施例的限制，因为这些实施例旨在作为本发明的几个方面的说明。实际上，除了本文中示出和描述的那些之外，根据前述描述，本发明的各种修改对于本领域技术人员来说将变得显而易见。这样的修改也意图落入所附权利要求的范围内。
Claims (6)
1.一种电致变色装置，包括：
电致变色膜（900）；
边缘保护材料（905、915），其设置在所述电致变色膜（900）的部分上，其中所述电致变色膜（900）包括上侧（901a）和下侧（901b），其中所述上侧在横向方向上相对于所述下侧偏移，并且其中所述上侧的横向边缘和所述下侧的横向边缘在横向方向上相对于彼此偏移，使得所述上侧的第一横向边缘相对于所述下侧的相邻横向边缘横向后移，并且所述下侧的第二横向边缘相对于所述上侧的相邻横向边缘横向前移，其中被所述边缘保护材料覆盖的电致变色膜的部分包括：
在所述第一横向边缘处的、具有边缘保护材料的上侧的顶部的部分和下侧的顶部的部分；
在所述第二横向边缘处的、具有边缘保护材料的上侧的底侧的部分和下侧的底侧的部分，使得上侧的第一横向边缘和下侧的第二横向边缘被边缘保护材料覆盖；
其中所述电致变色膜被中间层（903）围绕；并且所述电致变色膜和所述中间层（903）插入在第一基板（902）与第二基板（904）之间，其中所述边缘保护材料（905、915）是导电的并用作所述电致变色膜（900）的电极。
2.根据权利要求1所述的电致变色装置，其中所述边缘保护材料是环氧树脂。
3.根据权利要求1所述的电致变色装置，其中所述边缘保护材料选自：聚乙烯基硅氧烷PVS、热塑性聚氨酯TPU和乙烯乙酸乙烯酯EVA。
4.根据权利要求1所述的电致变色装置，其中所述中间层由聚乙烯醇缩丁醛PVB制成。
5.根据权利要求1所述的电致变色装置，其中所述边缘保护材料抵抗所述中间层的化学物。
6.根据权利要求1所述的电致变色装置，其中所述电致变色膜层压在中间层内。
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| JP2011095406A (ja) * | 2009-10-28 | 2011-05-12 | Tokai Rika Co Ltd | エレクトロクロミックミラー |
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| Publication number | Publication date |
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| EP3654095A1 (en) | 2020-05-20 |
| ES2946279T3 (es) | 2023-07-14 |
| EP4220293A1 (en) | 2023-08-02 |
| US20200150507A1 (en) | 2020-05-14 |
| US11969970B2 (en) | 2024-04-30 |
| US20230302771A1 (en) | 2023-09-28 |
| CN111399300A (zh) | 2020-07-10 |
| US11571878B2 (en) | 2023-02-07 |
| CN116430633A (zh) | 2023-07-14 |
| EP3654095B1 (en) | 2023-05-10 |
| US12030277B2 (en) | 2024-07-09 |
| US20240217214A1 (en) | 2024-07-04 |
| US20230158778A1 (en) | 2023-05-25 |
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