CN112521555B - 一种用于电致变色器件的抗冻耐热型水凝胶电解质 - Google Patents
一种用于电致变色器件的抗冻耐热型水凝胶电解质 Download PDFInfo
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Abstract
本发明涉及一种用于电致变色器件的抗冻耐热型水凝胶电解质。以去离子水为溶剂，羧化壳聚糖、丙烯酰胺为主单体，以N，N‑亚甲基双丙烯酰胺为交联剂，锂盐为电解质，聚乙二醇和丙三醇为添加剂，以2‑羟基‑2‑甲基‑1‑苯基‑1‑丙酮为光引发剂，在紫外灯照射下自由基聚合，通过调节聚乙二醇和丙三醇的加入量，制备抗冻和耐热性能良好的水凝胶电解质。进一步将该水凝胶电解质用于制备三明治结构电致变色器件，器件具有较宽的工作温度范围，在‑40℃～60℃温度区间表现出很好的循环稳定性，并且适用于柔性器件的制备。本发明涉及的新型水凝胶电解质制备方法简单，原料价廉易得，离子电导率高，透明度高，稳定性高，高低温耐受性能优异，具有广泛的应用前景。
Description
技术领域
本发明涉及一种新型水凝胶电解质的制备及应用，尤其涉及一种抗冻耐热型羧化壳聚糖改性聚丙烯酰胺类水凝胶电解质的制备，属于电致变色技术领域。
背景技术
电致变色现象自1969年发现以来受到广泛关注，在显示和光辐射及透过管理中具有潜在应用。在倡导节能减排的时代背景下，电致变色智能窗在节能建筑中的应用更是前景广泛。基于电化学氧化还原，离子脱嵌等机理，科学家们设计并开发了一系列优异的电致变色材料，表现出优异的电致变色性能。除此之外，为了获得更好的器件性能以满足实际应用需求，固态电解质通常被引入制成三明治结构器件。在三明治电致变色器件中，固态电解质因其组分多样化、化学键、物理键等相互作用比较复杂，使得工作性能更加具有环境敏感性，从而降低了器件的循环稳定性。因此，开发性能优异的固态电解质对推进电致变色器件的实用化尤为重要。
水凝胶是以水为分散介质，由亲水聚合物形成的具有三维网络结构的功能高分子材料。高度交联的聚合物网络使水凝胶具有优异机械性能和形变能力。由于水凝胶中包含着大量自由水分子，通常具有较高的离子电导率，在电致变色器件中具有广泛应用。
作为户内外光辐射环境下工作的光电器件，电致变色器件必须具有很强的环境耐受性以保证器件的适用性和稳定性。如季节性的温度变化，区域性气温差异等。因此，水凝胶电解质的高低温工作性能是电致变色器件无法逃避的重点。然而，目前仍然没有相关电致变色研究案例被报道。再者，由于水凝胶中自由水的存在，通常存在低温结冰，高温气化脱水的可能，大大降低器件性能。因此，开发防冻耐热型水凝胶电解质对推进电致变色器件的实际应用具有非常重要的意义。
发明内容
针对环境对于电致变色器件中电解质的影响，本发明提供了一种用于电致变色器件的抗冻耐热型水凝胶电解质的制备方法。
本发明的另一目的在于提供一种简便的电致变色器件制作方法，用3M双面胶在两种电极间固定出中空隔槽，灌入水凝胶溶液，紫外灯照射条件下使其在器件内部固化；不仅可以保证电解质层很薄，还能增加器件的使用寿命。
一种用于电致变色器件的抗冻耐热型水凝胶电解质及器件制备包括以下步骤：
(1)水凝胶电解质的制备：室温条件下，将锂盐加入到去离子水中，充分搅拌溶解得到盐溶液，依次加入主单体、光引发剂、交联剂和添加剂，搅拌溶解后得到水凝胶溶液；
(2)电极材料的制备：运用恒电流沉积法和恒电压电沉积法在导电玻璃上沉积上普鲁士蓝和聚紫罗精薄膜，分别作为电致变色器件的阳极和阴极；
(3)电致变色器件的制作：用3M双面胶在步骤(2)制备的两种电极间固定出一个中空隔槽，将步骤(1)制备的水凝胶溶液滴加进去，紫外灯下照射使水凝胶固化，得到基于羧化壳聚糖改性聚丙烯酰胺类抗冻耐热型水凝胶的电致变色器件。
步骤(1)中锂盐为氯化锂、溴化锂或四氟硼酸锂其中的一种，浓度为1mol/L。
步骤(1)中主单体为羧化壳聚糖和丙烯酰胺，羧化壳聚糖和丙烯酰胺的质量比为1∶1～3。
步骤(1)中交联剂为N，N-亚甲基双丙烯酰胺，其占丙烯酰胺质量的1～10％。
步骤(1)中光引发剂为2-羟基-2-甲基-1-苯基-1-丙酮(HMPP)，其加入量为10～50μL。
步骤(1)中添加剂为聚乙二醇和丙三醇；聚乙二醇作为互穿网络链段，其质量分数为羧化壳聚糖质量的0％～25％；丙三醇作为耐温溶剂，其体积分数为0％～60％。
步骤(2)电沉积过程中，均以ITO导电玻璃作为工作电极，铂丝为对电极，银丝为参比电极。
本发明具有以下优势：
本发明中制备水凝胶电解质的方法简便，且该水凝胶具有抗冻耐热性能，在-40℃～60℃的范围可以保持完整的形貌特征和很高的离子电导率，基于该水凝胶的器件也可以在-40℃～60℃的范围内具有很优异的电致变色性能，在智能变色窗以及柔性电子设备领域具有很好的应用前景。
附图说明
图1为电致变色器件的结构图。
图2为实施例1、2、3的水凝胶电解质在-40℃条件下外观形貌照片；结果表明水凝胶电解质在低温条件下可以保持良好的透明度和柔软性。
图3为实施例1、2、3的水凝胶电解质分别在室温、-40℃、60℃条件下，离子电导率的情况；由图可知，该水凝胶电解质无论在高温或者低温条件下，水凝胶仍可以拥有较好的离子电导率。
图4为以实例1的水凝胶制作成电致变色器件后在室温条件下的紫外吸收光谱和循环稳定性；由图可知，在最大吸收波长680nm处，电致变色器件循环了1000圈以后透光率差值仍然可以保持初始状态的94.8％。
图5为电致变色器件在-40℃和60℃条件下的循环稳定性；结果表明，由于水凝胶电解质的抗冻耐热性能优异，从而电致变色器件在极端条件下仍然维持其良好的循环稳定性。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例，对本发明进行进一步说明。
实施例1
(1)水凝胶电解质的制备：
将0.4g羧化壳聚糖和20μL光引发剂2-羟基-2-甲基-1-苯基-1-丙酮加入到5mL的溴化锂水溶液中，搅拌至溶解；称取0.8g的丙烯酰胺和0.04g的N，N-亚甲基双丙烯酰胺加入到该溶液中，继续搅拌2h；再加入0.06g聚乙二醇-1000搅拌至完全溶解；最后加入体积分数为50％的丙三醇，搅拌30min后得到水凝胶溶液；
(2)电极的制备：
采用恒电流沉积法制备普鲁士蓝薄膜，称取0.329g的K3Fe(CN)6、0.162g的FeCl3、1.491g的KCl和1mol/L HCl溶于100mL去离子水中得到电沉积液，在50μA的恒电流下沉积800s；采用恒电压沉积法制备聚紫罗精薄膜，称取0.848g的BVBr2、0.136g的KH2PO4、1.567g的K2HPO4和3.683g的K4Fe(CN)6溶于100mL去离子水中，在-0.75V的恒电压下沉积直至总电荷量达到150mC；以上电沉积过程中，均以ITO导电玻璃作为工作电极，以铂丝为对电极，银丝为参比电极；
(3)电致变色器件的制备：
用3M双面胶在沉积有聚紫罗精薄膜的ITO导电玻璃上固定出一个具有一定大小和厚度的中空隔槽，将上述得到的均一的水凝胶溶液滴加进隔槽中，再将沉积有普鲁士蓝薄膜的ITO导电玻璃贴上，紫外灯下照射2min使水凝胶固化，得到基于羧化壳聚糖改性聚丙烯酰胺类抗冻耐热型水凝胶的电致变色器件。
实施例2
(1)水凝胶电解质的制备：
将0.6g羧化壳聚糖和30μL光引发剂2-羟基-2-甲基-1-苯基-1-丙酮加入到5mL的氯化锂水溶液中，搅拌至溶解；称取1.2g的丙烯酰胺和0.05g的N，N-亚甲基双丙烯酰胺加入到该溶液中，继续搅拌2h；再加入0.1g聚乙二醇-1000搅拌至完全溶解；最后加入体积分数为50％的丙三醇，搅拌均匀后得到水凝胶溶液；
(2)电极及电致变色器件的制备方法与实例1相同。
实施例3
(1)水凝胶电解质的制备：
将0.6g羧化壳聚糖和20μL光引发剂2-羟基-2-甲基-1-苯基-1-丙酮加入到5mL的四氟硼酸锂水溶液中，搅拌至溶解；称取1.2g的丙烯酰胺和0.05g的N，N-亚甲基双丙烯酰胺加入到该溶液中，继续搅拌2h；再加入0.12g聚乙二醇-1000搅拌至完全溶解；最后加入体积分数为50％的丙三醇，搅拌30min；
(2)电极及电致变色器件的制备方法与实例1相同。
以上所述实施例目的在于让熟悉此领域技术的人士能够了解本发明的内容并加以实施，并不能以此限制本发明的保护范围，凡根据本发明的精神实质所作的等效变化或修饰，都应涵盖在本发明的保护范围内。
Claims (7)
1.一种基于羧化壳聚糖改性聚丙烯酰胺类抗冻耐热型水凝胶的电致变色器件的制备方法，其特征在于，包括如下步骤：
(1)水凝胶电解质的制备：室温条件下，将锂盐加入到去离子水中，充分搅拌溶解得到锂盐溶液，依次加入主单体、光引发剂、交联剂和添加剂，搅拌溶解后得到水凝胶溶液；主单体为羧化壳聚糖和丙烯酰胺，羧化壳聚糖和丙烯酰胺的质量比为1:1～3；
(2)电极材料的制备：运用恒电流沉积法和恒电压电沉积法在导电玻璃上沉积上普鲁士蓝和聚紫罗精薄膜，分别作为电致变色器件的阳极和阴极；
(3)电致变色器件的制作：用3M双面胶在步骤(2)制备的两种电极间固定出一个中空隔槽，将步骤(1)制备的水凝胶溶液滴加进去，紫外灯下照射使水凝胶固化，得到基于羧化壳聚糖改性聚丙烯酰胺类抗冻耐热型水凝胶的电致变色器件。
2.根据权利要求1所述的基于羧化壳聚糖改性聚丙烯酰胺类抗冻耐热型水凝胶的电致变色器件的制备方法，其特征在于，步骤(1)中锂盐为氯化锂、溴化锂或四氟硼酸锂其中的一种，浓度为1mol/L。
3.根据权利要求1所述的基于羧化壳聚糖改性聚丙烯酰胺类抗冻耐热型水凝胶的电致变色器件的制备方法，其特征在于，步骤(1)中交联剂为N,N-亚甲基双丙烯酰胺，其占丙烯酰胺质量的1～10％。
4.根据权利要求1所述的基于羧化壳聚糖改性聚丙烯酰胺类抗冻耐热型水凝胶的电致变色器件的制备方法，其特征在于，步骤(1)中光引发剂为2-羟基-2-甲基-1-苯基-1-丙酮(HMPP)，其加入量为10～50μL。
5.根据权利要求1所述的基于羧化壳聚糖改性聚丙烯酰胺类抗冻耐热型水凝胶的电致变色器件的制备方法，其特征在于，步骤(1)中添加剂为聚乙二醇和丙三醇；聚乙二醇作为互穿网络链段，其质量分数为羧化壳聚糖质量的0％～25％；丙三醇作为耐温溶剂，其体积分数为0％～60％。
6.根据权利要求1所述的基于羧化壳聚糖改性聚丙烯酰胺类抗冻耐热型水凝胶的电致变色器件的制备方法，其特征在于，步骤(2)电沉积过程中，均以氧化铟锡ITO导电玻璃作为工作电极，铂丝为对电极，银丝为参比电极。
7.一种基于羧化壳聚糖改性聚丙烯酰胺类抗冻耐热型水凝胶的电致变色器件，由权利要求1-6任意一项所述的制备方法制得，其特征在于，由两层沉积有电致变色材料的ITO电极以及一层透明的抗冻耐热水凝胶电解质构成。
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