CN112327555A - 一种电致变色器件及其制备方法和在智能窗中的应用 - Google Patents
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Abstract
本发明提供了一种电致变色器件及其制备方法和在智能窗中的应用。所述电致变色器件包括相对设置的阳极和阴极透明导电基底,以及设置于阳极与阴极透明导电基底之间的电致变色层和电解质层,所述的阳极透明导电基底与阴极透明导电基底之间不包括离子存储层;所述的电解质层是通过将含有金属离子的溶液滴在电致变色层上而获得,所述的金属离子为具有氧化作用的金属阳离子。本发明提供了所述电致变色器件在智能窗中的应用。本发明所述电致变色器件将传统电致变色器件中的电解质层和离子存储层的功能二合为一,使之既有氧化作用又有离子传输作用,简化了结构,制备的电致变色器件具有好的稳定性以及快的响应时间,在智能窗等领域具有很好的应用价值。
Description
(一)技术领域
本发明涉及一种电致变色器件及其制备方法和在智能窗中的应用。
(二)背景技术
“电致变色”(Electrochromism,EC)是指材料的光学属性,如透射率、反射率、吸收率等在外加电场作用下发生稳定、可逆变化的现象,宏观上表现为颜色和透明度的可逆变化。具有电致变色性能的材料被称为电致变色材料,由电致变色材料制成的器件为电致变色器件。
传统的电致变色器件为常见的“三明治”结构,结构依次为导电基底、电致变色层、电解质层、离子存储层以及导电基底。传统的电致变色器件的性能不仅与电致变色材料有关,还很大程度上与离子存储层有关,该类电致变色器件稳定性、响应时间等性能有待提高,并且由于结构复杂,加工难度较大,这提高了电致变色器件商业化的难度。
因此,对目前电致变色器件进行改善以解决上述问题成为了该领域技术人员急需解决的难题。
(三)发明内容
本发明的目的是提供一种新型电致变色器件及其制备方法和应用,该电致变色器件具有高的稳定性和更简单的器件结构。
为实现上述发明目的,本发明采用如下技术方案:
第一方面,本发明提供了一种电致变色器件,包括相对设置的阳极透明导电基底和阴极透明导电基底,以及设置于阳极透明导电基底与阴极透明导电基底之间的电致变色层和电解质层,所述的阳极透明导电基底与阴极透明导电基底之间不包括离子存储层;
所述的电解质层是通过将含有金属离子的溶液滴在电致变色层上而获得,所述的金属离子为具有氧化作用的金属阳离子,所述含有金属离子的溶液的溶剂为乙腈、甲醇、乙醇中的一种或多种,所述的含有金属离子的溶液的浓度为0.01~0.5M。
作为优选,所述电致变色器件由相对设置的阳极透明导电基底和阴极透明导电基底,以及设置于阳极透明导电基底与阴极透明导电基底之间的电致变色层和电解质层组成。
作为优选,所述的金属离子为铁离子或铜离子。本发明对于与金属离子形成化合物的阴离子没有特别要求,如Cl-、NO3-等均可,只要形成的金属离子化合物能溶于相应的溶剂即可。
作为优选,所述的电解质层的厚度为0.1~0.3mm。
本发明中,所述的阳极透明导电基底、阴极透明导电基底和电致变色层均可根据实际需要进行常规选择。所述的阳极透明导电基底可以是ITO、FTO或PET的一种,所述的阴极透明导电基底可以是ITO、FTO或PET的一种。所述的电致变色层采用的电致变色材料可以根据电致变色器件的应用场景进行选择,如在智能窗领域,优选黑色到高透射或高透射到黑色转变的电致变色材料。
作为一种优选的实施方式,所述的电致变色材料的结构如下所示:
所述电致变色聚合物的数均分子量Mn=5000~200000,多分散系数D=1.0~5.0。
上述电致变色材料可通过专利CN111393616A公开的方法进行制备,本发明对该专利做全文引用。
本发明提供了一种电致变色器件的制备方法,包括如下步骤:
将电致变色材料通过溶液加工成膜的方式制备在阳极透明导电基底上,将含有金属离子的溶液滴在电致变色层上,再将阴极基底置于电解质层上,封装器件即得电致变色器件。
作为优选,所述的溶液加工成膜具体为:将电致变色材料溶于溶剂中得到电致变色层溶液,然后将电致变色层溶液涂覆于阳极透明导电基底上,去除溶剂后得到电致变色层。
作为进一步的优选,所述的电致变色层溶液的溶剂为二氯甲烷、三氯甲烷、四氢呋喃、甲苯或二甲基甲酰胺。
作为进一步的优选,涂覆方式是喷涂、旋涂、丝网印刷等。
作为优选,将含有金属离子的溶液滴在电致变色层上使液层厚度达到0.1~0.3mm。
第三方面,本发明提供了所述电致变色器件在智能窗中的应用。
与现有的技术相比,本发明具有以下优点和有益效果:
(1)本发明所述电致变色器件通过独特的电解质层的设计,将传统电致变色器件中的电解质层和离子存储层的功能二合为一,使之既有氧化作用又有离子传输作用,简化了电致变色器件的结构。
(2)本发明制备的电致变色器件具有好的稳定性以及快的响应时间。
(3)本发明电致变色器件的制备相较于传统电致变色更简单,在智能窗等领域具有很好的应用价值。
(四)附图说明
图1:实施例1中所制备的电致变色器件在不同电压下的光谱曲线。
图2、3和4:实施例1中所制备的电致变色器件在具体波长下-2.0-0.8V多电位阶跃下透射率随时间变化的曲线。
(五)具体实施方式
下面以具体实施例对本发明的技术方案作进一步的说明,但本发明的保护范围不限于此。
实施例1
所使用的电致变色层材料结构如下所示:
电致变色层材料合成方法如下:
将P(3.65g,1eq.)加入到含有Br-PC-Br(1.75g,0.5eq)的30ml四氢呋喃溶液中,加入Pd(PPh3)2Cl2(105mg,0.03eq.),回流下反应12小时,反应结束后用水和二氯甲烷萃取,干燥,经过柱层析分离得到PPCP。
将PPCP(1.42g,1eq.)与Br-PBTP-Br(1.17g,1eq.)加入到含有新戊酸(30mg,0.3eq.) 和碳酸钾(0.34g,2.5eq.)的30mlDMAc溶液中,最后加入Pd(OAc)2(7mg,0.03eq.)催化剂,120℃反应24小时。反应结束后,将溶液倒入甲醇中,过滤,烘干,依次用甲醇、丙酮、己烷、三氯甲烷索提,收集三氯甲烷中溶解的聚合物,旋干即得电致变色层材料。
本发明电致变色器件制备如下:
将电致变色层材料溶于三氯甲烷中得到浓度为30mg/mL的溶液,在4×2.5cm的ITO导电基底上进行旋涂制膜,旋涂溶液浓度为30mg/ml,旋涂溶液体积为0.5ml,转速为800r/min,时间为1min。再将0.1M的FeCl3/ACN溶液滴在电致变色层上形成0.2mm后的电解质层,最后将ITO导电基底置于电解质层上,3M胶封装即得电致变色器件。
所得器件的电致变色性能测试如下:
使用电化学工作站与紫外-可见分光光度仪联用装置,分别测试所制备的器件-2.0V和 0.8V电压下的紫外-可见光吸收,在特定波长下的透射率和时间的关系,以及在阶跃电压下器件稳定性测试,数据处理结果如图1-3所示。从图1可以看出该器件在-2.0V状态下呈黑色,在电压0.8V下氧化后呈高透射状态。图2、3为器件在497nm下从-2.0-0.8V多电位阶跃透射率随时间变化的曲线,可以看出器件在497nm处的对比度为44.5%,着色时间和褪色时间分别为2.8s和0.6s。从图4器件稳定性测试,可以看出在1000个循环后,对比度基本不变,说明器件稳定性非常好。该电致变色器件在智能窗领域具有很好的潜在商业价值。
Claims (10)
1.一种电致变色器件,包括相对设置的阳极透明导电基底和阴极透明导电基底,以及设置于阳极透明导电基底与阴极透明导电基底之间的电致变色层和电解质层,所述的阳极透明导电基底与阴极透明导电基底之间不包括离子存储层;
所述的电解质层是通过将含有金属离子的溶液滴在电致变色层上而获得,所述的金属离子为具有氧化作用的金属阳离子,所述含有金属离子的溶液的溶剂为乙腈、甲醇、乙醇中的一种或多种,所述的含有金属离子的溶液的浓度为0.01~0.5M。
2.如权利要求1所述的电致变色器件,其特征在于:所述电致变色器件由相对设置的阳极透明导电基底和阴极透明导电基底,以及设置于阳极透明导电基底与阴极透明导电基底之间的电致变色层和电解质层组成。
3.如权利要求1或2所述的电致变色器件,其特征在于:所述的金属离子为铁离子或铜离子。
4.如权利要求1或2所述的电致变色器件,其特征在于:所述的电解质层的厚度为0.1~0.3mm。
5.如权利要求1或2所述的电致变色器件,其特征在于:所述的阳极透明导电基底是ITO、FTO或PET的一种,所述的阴极透明导电基底是ITO、FTO或PET的一种。
7.一种如权利要求1所述的电致变色器件的制备方法,包括如下步骤:
将电致变色材料通过溶液加工成膜的方式制备在阳极透明导电基底上,将含有金属离子的溶液滴在电致变色层上,再将阴极基底置于电解质层上,封装器件即得电致变色器件。
8.如权利要求7所述的制备方法,其特征在于:所述的溶液加工成膜具体为:将电致变色材料溶于溶剂中得到电致变色层溶液,然后将电致变色层溶液涂覆于阳极透明导电基底上,去除溶剂后得到电致变色层。
9.如权利要求7所述的制备方法,其特征在于:将含有金属离子的溶液滴在电致变色层上使液层厚度达到0.1~0.3mm。
10.如权利要求1所述的电致变色器件在智能窗中的应用。
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