CN108363255A - 一种电致变色膜材料及其制备的电致变色膜器件 - Google Patents

一种电致变色膜材料及其制备的电致变色膜器件 Download PDF

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CN108363255A
CN108363255A CN201810255791.0A CN201810255791A CN108363255A CN 108363255 A CN108363255 A CN 108363255A CN 201810255791 A CN201810255791 A CN 201810255791A CN 108363255 A CN108363255 A CN 108363255A
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electrochromism
electrochromism membrane
cohesive force
electrochromic
oxidation
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CN108363255B (zh
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曾西平
杨改丽
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China Tech Powerise Technology Co Ltd Of Shenzhen
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Priority to US17/040,049 priority patent/US11326094B2/en
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Abstract

本发明属于电致变色器件技术领域，具体涉及一种新型电致变色膜材料，并进一步公开其制备的电致变色膜器件。本发明所述的电致变色膜器件，首次以高粘结力组合物和电致变色组合物为原料进行制备电致变色膜材料，通过高粘结力组合物的固化反应将电致变色组合物于所述导电基板之间进行分散并固化，经测试，本发明制得的电致变色膜器件，的变色响应时间在7‑11秒之间、循环次数在14‑16万次之间、色差b值在‑20到+30之间，具有变色速度快、寿命高、性能稳定的，最高循环寿命可达16万次，具有较好的应用性能。

Description

一种电致变色膜材料及其制备的电致变色膜器件
技术领域
本发明属于电致变色器件技术领域，具体涉及一种新型电致变色膜材料，并进一步公开其制备的电致变色膜器件。
背景技术
电致变色技术是一种电驱动变色技术，是指是材料在外加电源作用下通过得失电子(氧化还原)使其状态发生改变，使得材料自身颜色发生变化的过程。我们将具有这种电致变色性质的材料称之为电致变色材料，并将利用这种电致变色材料制备的器件命名为电致变色器件(electro chromic device，ECD)。
ECD可以通过对光的透过和吸收而改变其颜色，这种技术有着很广泛的应用领域及发展前景，如现有技术中已经开发的电致变色窗、电致变色显示屏、电致变色眼镜等。电致变色窗能够通过自身的颜色和部分红外线辐照的开关效应在强光直射时改变光的辐照强度，达到调节室内光线和温度的作用，可以部分降低用于取暖、降温等消耗的能源，并由此降低带来的环境污染；电致显示屏是利用电致变色技术制备的显示屏，由于电致变色器件的记忆效果，即一旦变色不需要外加电源仍可维持其变色状态的功能，使得在显示静态图像时无需外加电压，从而达到节能的目的；电致变色眼镜基于电致变色技术，打破传统产品的光线控制，可随时随地通过改变电压而变换颜色，具有较大的可调性。
目前，以电致变色技术为主的企业主要有美国Sage Glass、Gentex、德国的E-control Glas、Gesimat和瑞典的Chromo Genie。但是，由于现有生产的电致变色膜器件的性能并不稳定，而且生产工艺较为复杂，导致其生产成本较高，限制电致变色膜器件的广泛应用及发展。
发明内容
为此，本发明所要解决的技术问题在于提供一种电致变色膜材料，并进一步公开其制备的电致变色膜器件。
为解决上述技术问题，本发明所述的一种用于制备电致变色膜材料的高粘结力组合物，其特征在于，包括如下重量份的组分：
所述的用于制备电致变色膜材料的高粘结力组合物中：
所述树脂包括丙烯酸酯树脂、聚氨酯树脂、聚酯树脂或环氧树脂等带有容易进行自由基反应的双键的树脂；并优选聚氨酯丙烯酸酯树脂；更具体可选自聚氨酯丙烯酸树脂CN704、聚氨酯丙烯酸树脂CN966J75NS、聚氨酯丙烯酸树脂UV65等；
所述单体包括丙烯酸(酯)类单体、乙烯基单体、环氧单体或环氧丙烯酸酯单体；
所述交联剂包括多官能团功能性单体；如双官能团交联单体，HDDA、BDDA、DEGDA、TEGDA等，或三官能团交联单体，TMPTA、TEGDA、PETA等；
所述引发剂包括光引发剂或热引发剂；如光引发剂I-1173、I-184、I-369、I-2959、I-819、EDB、ITX、TPO，或热引发剂AIBN等自由基型引发剂，并优选光引发剂两两共混的体系；
所述间隔子包括刚性微珠，并优选直径在10微米到100微米之间的微珠；两片导电基材之间的距离由间隔子控制，可通过加入不同直径的间隔子调节电致电色器件的厚度，具体的为10微米、20微米、30微米、50微米、100微米。
本发明还公开了一种用于制备电致变色膜材料的氧化还原型液态电致变色组合物，包括如下重量份的组分：
电致变色材料 0.01-10重量份；
离子储存材料 0.01-10重量份；
液态电解质材料 50.01-102.5重量份。
所述的用于制备电致变色膜材料的氧化还原型液态电致变色组合物中：
所述电致变色材料包括有机高分子、有机小分子以及金属氧化物或金属络合物类电致变色材料；
其中，所述有机高分子电致变色材料具体选自聚噻吩、聚吡置、聚苯胺、侧链带有电致变色结构的高分子聚合物、高分子金属配合物中的至少一种；所述有机小分子电致变色材料具体选自紫精化合物、三苯胺、三苯胺衍生物、咔唑、咔唑衍生物、蒽醌、蒽醌衍生物、吩噻嗪、吩噻嗪衍生物等的一种；所述金属氧化物类电致变色材料主要是过渡金属氧化物，具体选自：五氧化二钒、氧化钨、氧化鈰、氧化铟锡等的其中一种；所述金属络合物物具体选自：普鲁士蓝、普鲁士黑、普鲁士白、普鲁士绿、亚硝酰基含氧钼络合物等的其中一种；
所述离子储存材料包括五氧化二钒、氧化钨、氧化鈰、氧化铟锡、普鲁士蓝、聚苯胺、三苯胺、吩嗪或紫精类化合物；
所述液态电解质材料由50-99重量份的液态导电介质和0.1-3.5重量份的电解质盐组成；
所述液态导电介质包括液态有机溶剂、离子液体或凝胶状的交联高分子材料，如碳酸丙烯酯、碳酸乙二醇酯等；
所述电解质盐选自高氯酸锂、六氟磷酸锂、四氟磷酸离、二草酸硼酸锂、双(三氟甲基磺酰)亚胺锂中的至少一种。
本发明还公开了所述的高粘结力组合物用于制备电致变色膜材料的用途。
本发明还公开了所述的氧化还原型液态电致变色组合物用于制备电致变色膜材料的用途。
本发明还公开了一种电致变色膜材料，其原料组分包括所述的高粘结力组合物和所述的氧化还原型液态电致变色组合物，所述高粘结力组合物和所述的氧化还原型液态电致变色组合物的质量比为1：0.01-50。
本发明还公开了一种制备所述电致变色膜材料的方法，包括按照选定量将所述高粘结力组合物和所述的氧化还原型液态电致变色组合物的各组分进行混匀的步骤，并经过固化，即得。
所述固化反应步骤中，若使用光引发剂则固化反应条件为紫外光，所述光的能量为0.5mW/cm2-5.5mW/cm2，更优为2.5mW/cm2，固化时间为30s-5min，更优为2min；若使用热引发剂则固化反应条件为烘箱加热，其中加热温度为30-80℃，更优为55℃，固化时间为10s-30min，更优为10min。
本发明还公开了一种电致变色膜器件，包括两层导电基材，以及分散固定于两层所述导电基材之间的所述的电致变色膜材料。
所述导电基材包括氧化铟锡(ITO)导电玻璃、氧化铟锡(ITO)导电薄膜、纳米银线导电薄膜、氟化掺杂氧化锡玻璃或聚合物导电膜。
本发明还公开了一种制备所述的电致变色膜器件的方法，包括按照选定量将所述高粘结力组合物和所述的氧化还原型液态电致变色组合物的各组分进行混匀的步骤，并所得混合物涂布于选定的两层所述导电基材之间，经固化反应，得到所需的电致变色膜器件。
所述固化反应步骤中，若使用光引发剂则固化反应条件为紫外光，所述光的能量为0.5mW/cm2-5.5mW/cm2，更优为2.5mW/cm2，固化时间为30s-5min，更优为2min；若使用热引发剂则固化反应条件为烘箱加热，其中加热温度为30-80℃，更优为55℃，固化时间为10s-30min，更优为10min。
本发明所述的电致变色膜器件，首次以高粘结力组合物和电致变色组合物为原料进行制备电致变色膜材料，通过高粘结力组合物的固化反应将电致变色组合物于所述导电基板之间进行分散并固化，经测试，本发明制得的电致变色膜器件，的变色响应时间在7-11秒之间、循环次数在14-16万次之间、色差b值在-20到+30之间，具有变色速度快、寿命高、性能稳定的，最高循环寿命可达16万次，具有较好的应用性能。
本发明所述电致变色膜器件生产工艺简单且固化前后基本不改变原导电基材的透光度，电致变色器件的透光率都在80以上，可以解决用户对色度、透光度调节的需求。同时，相比于市场上现有的调光器件，本发明中器件利用高粘结力组合物将电致变色溶液分散固定的技术有效减低了生产成本，具有较好的经济效益。
具体实施方式
本发明下述各实施例中对所得电致变色膜器件性能的测试条件及测试方法具体包括：
电致变色性能：日本分光计器株式会社提供的紫外-可见-分光光度计(Jesco-V670)；
电致变色器件在不同状态下的色度变化：飞利浦15-4460色差仪；
循环次数：利用多电位阶跃方法实现电致变色器件的循环，同时结合V-670对其循环过程进行实时监测以测试电致变色器件的工作性能；
驱动电压：上海辰华仪器有限公司提供的CHI-660D电化学分析仪。
实施例1
本实施例所述电致变色膜器件，包括两层氧化铟锡(ITO)导电薄膜为导电基材，两层所述氧化铟锡(ITO)导电薄膜之间分散固化有电致变色膜材料。
本实施例所述电致变色膜材料包括高粘结力组合物和氧化还原型液态电致变色组合物，所述电致变色膜材料具体包括如下制备原料：
聚氨酯丙烯酸酯树脂10kg；
甲基丙烯酸酯单体10kg；
三官能团交联剂PETA 3kg；
光引发剂TPO 0.003kg；
10微米间隔子0.003kg；
三苯胺1kg；
普鲁士蓝1kg；
碳酸丙烯酯74kg；
高氯酸锂0.5kg。
本实施例所述电致变色膜器件的制备方法包括：按照上述选定量取各个原料组分，将其混合均匀后，用滚涂机涂布在两片长3米宽3米的氧化铟锡(ITO)导电薄膜之间，用能量为2.5mW/cm2的紫外光固化2分钟，得电致变色膜器件1。
将所得器件连接直流电压5V，该器件由蓝色变黄绿色，响应时间为11秒，器件光透过率由84.4变到84.3，色差b值由-20变到+30，循环次数151154次。
实施例2
本实施例所述电致变色膜器件，包括两层氧化铟锡(ITO)导电薄膜为导电基材，两层所述氧化铟锡(ITO)导电薄膜之间分散固化有电致变色膜材料。
本实施例所述电致变色膜材料包括高粘结力组合物和氧化还原型液态电致变色组合物，所述电致变色膜材料具体包括如下制备原料：
聚氨酯丙烯酸酯树脂10kg；
环氧丙烯酸酯8kg；
三官能团交联剂TMPTA 3kg；
光引发剂TPO 0.003kg；
10微米间隔子0.003kg；
聚噻吩3kg；
普鲁士蓝1kg；
碳酸丙烯酯74kg；
高氯酸锂0.5kg。
本实施例所述电致变色膜器件的制备方法包括：按照上述选定量取各个原料组分，将其混合均匀后，用滚涂机涂布在两片长3米宽3米的氧化铟锡(ITO)导电薄膜之间，用能量为2.5mW/cm2的紫外光固化3分钟，得电致变色膜器件2。
将所得器件连接直流电压5.5V，该器件由蓝色变黄绿色，响应时间10秒，器件光透过滤由84.4变到84.1，色差b值由-20变到+20，循环次数148958次。
实施例3
本实施例所述电致变色膜器件，包括两层氧化铟锡(ITO)导电薄膜为导电基材，两层所述氧化铟锡(ITO)导电薄膜之间分散固化有电致变色膜材料。
本实施例所述电致变色膜材料包括高粘结力组合物和氧化还原型液态电致变色组合物，所述电致变色膜材料具体包括如下制备原料：
聚氨酯丙烯酸酯树脂10kg；
环氧丙烯酸酯8kg；
三官能团交联剂TMPTA 3kg；
热引发剂AIBN 0.003kg；
10微米间隔子0.003kg；
聚吡置3kg；
普鲁士蓝1kg；
碳酸丙烯酯74kg；
高氯酸锂0.5kg。
本实施例所述电致变色膜器件的制备方法包括：按照上述选定量取各个原料组分，将其混合均匀后，用滚涂机涂布在两片长3米宽3米的氧化铟锡(ITO)导电薄膜之间，用烘箱在60摄氏度固化5分钟，得电致变色膜器件3。
将所得器件连接直流电压5.5V，该器件由蓝色变黄绿色，响应时间为8秒，器件光透过滤由84.4变到81.5，色差b值由-18变到+11，循环次数144650次。
实施例4
本实施例所述电致变色膜器件，包括两层纳米银线导电薄膜为导电基材，两层所述纳米银线导电薄膜之间分散固化有电致变色膜材料。
本实施例所述电致变色膜材料包括高粘结力组合物和氧化还原型液态电致变色组合物，所述电致变色膜材料具体包括如下制备原料：
聚氨酯丙烯酸酯树脂10kg；
环氧丙烯酸酯8kg；
三官能团交联剂TMPTA 3kg；
热引发剂AIBN 0.003kg；
10微米间隔子0.003kg；
聚吡置3kg；
二茂铁1kg；
碳酸乙二醇酯95kg；
高氯酸锂0.5kg。
本实施例所述电致变色膜器件的制备方法包括：按照上述选定量取各个原料组分，将其混合均匀后，用滚涂机涂布在两片长3米宽3米的纳米银线导电薄膜之间，用烘箱在60摄氏度固化5分钟，得电致变色膜器件4。
将该器件连接直流电压5.0V，该器件由蓝色变黄绿色，响应时间为9秒，器件光透过滤由84.6变到82.9，色差b值由-17变到+11，循环次数144920次。
实施例5
本实施例所述电致变色膜器件，包括两层氟化掺杂氧化锡玻璃为导电基材，两层所述氟化掺杂氧化锡玻璃之间分散固化有电致变色膜材料。
本实施例所述电致变色膜材料包括高粘结力组合物和氧化还原型液态电致变色组合物，所述电致变色膜材料具体包括如下制备原料：
环氧树脂1kg；
环氧丙烯酸酯单体0.01kg；
双官能团交联单体HDDA 0.01kg；
光引发剂EDB 0.001kg；
20微米间隔子0.001kg；
聚苯胺0.01kg；
五氧化二钒0.01kg；
碳酸乙二醇酯50kg；
六氟磷酸锂0.1kg。
本实施例中所述电致变色膜器件的制备方法同实施例1。
实施例6
本实施例所述电致变色膜器件，包括两层氧化铟锡(ITO)导电薄膜为导电基材，两层所述氧化铟锡(ITO)导电薄膜之间分散固化有电致变色膜材料。
本实施例所述电致变色膜材料包括高粘结力组合物和氧化还原型液态电致变色组合物，所述电致变色膜材料具体包括如下制备原料：
聚氨酯丙烯酸树脂CN966J75NS 60kg；
乙烯基单体50kg；
双官能团交联单体TEGDA 50kg；
热引发剂AIBN 5kg；
30微米间隔子0.01kg；
吩噻嗪10kg；
聚苯胺10kg；
碳酸丙烯酯99kg；
二草酸硼酸锂3.5kg。
本实施例中所述电致变色膜器件的制备方法同实施例3。
由以上测试数据可知，本发明提供的电致变色膜器件的变色响应时间在7-11秒之间、循环次数在14-16万次之间、色差b值在-20到+30之间，具有较好的性能。
本发明所述电致变色膜器件生产工艺简单且固化前后基本不改变原导电基材的透光度，电致变色器件的透光率都在80以上，可以解决用户对色度、透光度调节的需求。同时，相比于市场上现有的调光器件，本发明中器件利用高粘结力组合物将电致变色溶液分散固定的技术有效减低了生产成本，具有较好的经济效益。
显然，上述实施例仅仅是为清楚地说明所作的举例，而并非对实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引伸出的显而易见的变化或变动仍处于本发明创造的保护范围之中。

Claims (10)

1.一种用于制备电致变色膜材料的高粘结力组合物，其特征在于，包括如下重量份的组分：
2.根据权利要求1所述的用于制备电致变色膜材料的高粘结力组合物，其特征在于：
所述树脂包括丙烯酸酯树脂、聚氨酯树脂、聚酯树脂或环氧树脂；
所述单体包括丙烯酸(酯)类单体、乙烯基单体、环氧单体或环氧丙烯酸酯单体；
所述交联剂包括多官能团功能性单体；
所述引发剂包括光引发剂或热引发剂；
所述间隔子包括刚性微珠。
3.一种用于制备电致变色膜材料的氧化还原型液态电致变色组合物，其特征在于，包括如下重量份的组分：
电致变色材料0.01-10重量份；
离子储存材料0.01-10重量份；
液态电解质材料50.01-102.5重量份。
4.根据权利要求3所述的用于制备电致变色膜材料的氧化还原型液态电致变色组合物，其特征在于：
所述电致变色材料包括有机高分子、有机小分子以及金属氧化物或金属络合物类电致变色材料；
所述离子储存材料包括五氧化二钒、氧化钨、氧化鈰、氧化铟锡、普鲁士蓝、聚苯胺、三苯胺、吩嗪或紫精类化合物；
所述液态电解质材料由50-99重量份的液态导电介质和0.1-3.5重量份的电解质盐组成；
所述液态导电介质包括液态有机溶剂、离子液体或凝胶状的交联高分子材料；
所述电解质盐选自高氯酸锂、六氟磷酸锂、四氟磷酸离、二草酸硼酸锂、双(三氟甲基磺酰)亚胺锂中的至少一种。
5.权利要求1或2所述的高粘结力组合物或权利要求3或4所述的氧化还原型液态电致变色组合物用于制备电致变色膜材料的用途。
6.一种电致变色膜材料，其特征在于，其原料组分包括权利要求1或2所述的高粘结力组合物和权利要求3或4所述的氧化还原型液态电致变色组合物，所述高粘结力组合物和所述的氧化还原型液态电致变色组合物的质量比为1：0.01-50。
7.一种制备权利要求5或6所述电致变色膜材料的方法，其特征在于，包括按照选定量将所述高粘结力组合物和所述的氧化还原型液态电致变色组合物的各组分进行混匀的步骤，并经过固化，即得。
8.一种电致变色膜器件，其特征在于，包括两层导电基材，以及分散固定于两层所述导电基材之间的权利要求5或6所述的电致变色膜材料。
9.根据权利要求8所述的电致变色膜器件，其特征在于，所述导电基材包括氧化铟锡(ITO)导电玻璃、氧化铟锡(ITO)导电薄膜、纳米银线导电薄膜、氟化掺杂氧化锡玻璃或聚合物导电膜。
10.一种制备权利要求8或9所述的电致变色膜器件的方法，其特征在于，包括按照选定量将所述高粘结力组合物和所述的氧化还原型液态电致变色组合物的各组分进行混匀的步骤，并所得混合物涂布于选定的两层所述导电基材之间，经固化反应，得到所需的电致变色膜器件。
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