CN111875823A - 一种厚度可控的全透光离子液体凝胶薄膜的制备方法 - Google Patents
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Abstract
本发明公开了一种厚度可控的全透光离子液体凝胶薄膜的制备方法,包括以下步骤:第一步:在容器中加入离子液体与聚合物,再放入溶剂,以使聚合物和离子液体溶解,将溶解后的混合溶液进行磁力搅拌,使其混合均匀;第二步:将基底吸附在匀胶机仪器上,将第一步得到的混合溶液滴在基底上,通过设定不同的转速进行旋涂,得到旋涂有离子液体凝胶的基底;第三步,将第二步得到的旋涂有离子液体凝胶的基底放至真空烤箱中烘烤,得到所述全透光离子液体凝胶薄膜。本发明极大的提升了凝胶类离子凝胶薄膜的制备简易性,在保留了离子液体性能的同时,凝胶薄膜的物理形态克服了离子液体易流动的缺陷且厚度均匀可控,可获得100%透光率的离子凝胶薄膜。
Description
技术领域
本发明属于电解质材料领域,具体涉及一种厚度可控的全透光离子液体凝胶薄膜电解质的制备方法。
背景技术
由于离子液体具有许多优良的性质,例如高热稳定性、宽电化学窗口、无毒、超级电容等,因此其在各个领域有着重要的应用价值,随着材料发展的需求,如何保持离子液体原有的物理化学性质,同时将其集成于固体器件中是目前研究的热点。作为一种新型的混合材料,离子液体凝胶不仅保持了离子液体原有的理化性质,而且解决了离子液体外溢的问题,同时其较高的形状可塑性满足了人们对特殊材料的需求,因此拓展了离子液体的应用范围。
离子液体凝胶具有离子液体的本征性质,具有低蒸汽压、较高的热稳定性和化学稳定性、宽电化学窗口等独特优点。
现阶段仍然缺乏一种简易的、高效的方法来制备兼具高透明性、高杨氏模量、高电容以及环境稳定性的厚度可控柔性离子凝胶薄膜。
发明内容
本发明的目的是提供一种厚度可控的全透光离子液体凝胶薄膜的制备方法,以解决离子液体易流动、不易应用的问题。
为实现上述目的,本发明采用的技术方案如下:
一种厚度可控的全透光离子液体凝胶薄膜的制备方法,包括以下步骤:
第一步:在容器中加入离子液体与聚合物,再放入溶剂,以使聚合物和离子液体溶解,将溶解后的混合溶液进行磁力搅拌,使其混合均匀;
第二步:将基底吸附在匀胶机仪器上,将第一步得到的混合溶液滴在基底上,通过设定不同的转速进行旋涂,得到旋涂有离子液体凝胶的基底;
第三步:将第二步得到的旋涂有离子液体凝胶的基底放至真空烤箱中烘烤,得到所述全透光离子液体凝胶薄膜。
优选的,所述第一步中,离子液体为N,N-二乙基-N-甲基-N-(2-甲氧乙基)铵基双(三氟甲基磺酰)酰亚胺,其结构式为:
优选的,所述第一步中,聚合物为聚偏二氟乙烯-六氟丙烯(P(VDF-HFP)),其结构式为:
优选的,所述第一步中,溶剂为丙酮。
优选的,所述第一步中,离子液体、聚合物、溶剂的质量比为4:1:10。
优选的,所述第一步中,磁力搅拌的温度为70℃,时间为一小时,目的是为了将离子液体与结构化聚合物共混以形成化学或物理交联的网络。
优选的,所述第二步中,基底为硅片或石英片。
优选的,所述第二步中,通过改变匀胶机仪器的转速来调整所得全透光离子液体凝胶薄膜的厚度,转速越快,厚度越小。
优选的,所述第二步中,烘烤的温度为70℃,时间为24小时。烘烤的目的是去除溶剂。
有益效果:本发明通过选择性溶解共聚物来使离子液体胶化,其中聚偏二氟乙烯-六氟丙烯晶体不溶于液体。凝胶化是通过溶解在溶液中的聚合物桥连这些晶体而发生的。采用向离子液体中加入聚偏二氟乙烯-六氟丙烯,可以一定程度提升电解质的柔性,特别地,本发明实现了离子液体凝胶的薄膜化,使其可轻易的机械切割下来直接应用到器件中,并且实现了离子液体凝胶厚度的可控性,可根据具体器件需要按已知规律选择所需的厚度,大大拓展了离子液体在柔性电子器件领域的应用。本发明的薄膜透光率在300-900纳米波段高达100%,在可见光波段(390-770纳米)可达到高透光率,且高透光性可以维持到900nm的高波长范围。
利用本发明制备的离子液体凝胶薄膜具有以下显著特点:(1)高透光性,在波长为300-900纳米甚至更高的波段均显示出100%的全透光性;(2)厚度可控,与转速成规律性。(3)片式的离子凝胶薄膜便于保存和使用。(4)良好的拉伸性和回弹性;(5)良好的化学稳定性,不腐蚀金属,可与铜、铝等金属复合制备复杂的器件。(6)制备流程简单,易于操作;(7)工作电压窗口高,分解电压>3V,支持其在凝胶电解质领域中正常工作;
本方法极大的提升了凝胶类离子凝胶薄膜的制备简易性,通过以上方法可获得100%透光率的薄膜化离子液体凝胶,在保留了离子液体性能的同时,凝胶薄膜的物理形态克服了离子液体易流动的缺陷,大大拓展了它们的应用范围(如聚合物固态电解质、超级电容、锂电池、电化学发光材料等),“即用即旋”即可获得薄膜的方式也大大提高了操作的便利性,其柔性和厚度可控的特质也为柔性电子领域提供了新的机会。
附图说明
图1为实施例1制备的离子液体凝胶薄膜的实物图;
图2为实施例1中匀胶转速与离子液体凝胶薄膜厚度的关系;
图3为实施例1中离子液体凝胶薄膜波长与透光率的关系;
图4为实施例1中离子液体凝胶薄膜电容与频率的关系;
图5为实施例2中匀胶转速与离子液体凝胶薄膜厚度的关系。
具体实施方式
下面结合实施例对本发明做更进一步的解释。
实施例1
本实例包括以下步骤:
第一步:称取4g N,N-二乙基-N-甲基-N-(2-甲氧乙基)铵基双(三氟甲基磺酰)酰亚胺和1g聚偏二氟乙烯-六氟丙烯加入到50mL的烧杯中,再称取10g丙酮溶剂加入烧杯中,加入洗净的磁转子,用锡纸盖住烧杯口,并用镊子戳出若干个孔,以便于丙酮挥发。将烧杯放置于70℃的磁力搅拌器上搅拌一小时。
第二步:取1.5×1.5cm的干净硅片或石英片吸附在匀胶机仪器上,将配置好的离子液体滴在硅片上,转速为2000转/分钟,匀胶时间为60s,所得薄膜的厚度与转速遵循一定的规律,转速越快,凝胶薄膜厚度越小。
第三步,将旋涂了离子液体凝胶的硅片或玻璃片放至真空烤箱中以70℃条件烘烤24小时,以去除多余的丙酮。此时硅片上的离子凝胶薄膜可轻松用镊子夹取,独立操作。
本实施例得到的离子液体凝胶薄膜及其性能测试如图1-图4:图1为实施例1制备的离子液体凝胶薄膜的实物图;图2为匀胶转速与离子液体凝胶薄膜厚度的关系,匀胶时长为60s,改变第二步匀胶的转速,分别为1000转/分钟、2000转/分钟、5000转/分钟、9000转/分钟,图2展示了按照实施例1过程配置匀胶转速与离子液体凝胶薄膜厚度的规律性;图3为离子液体凝胶薄膜波长与透光率的关系;图4为离子液体凝胶薄膜电容与频率的关系,可知本发明所制备的离子液体凝胶薄膜的电容可达微法/平方厘米级别。
实施例2
本实例包括以下步骤:
第一步:称取4gN,N-二乙基-N-甲基-N-(2-甲氧乙基)铵基双(三氟甲基磺酰)酰亚胺和0.75g聚偏二氟乙烯-六氟丙烯加入到50mL的烧杯中,再称取10g丙酮溶剂加入烧杯中,加入洗净的磁转子,用锡纸盖住烧杯口,并用镊子戳出若干个孔,以便于丙酮挥发。将烧杯放置于70℃的磁力搅拌器上搅拌一小时,搅拌时间和转速可根据所配置的溶液量来定。
第二步:取1.5×1.5cm的干净硅片或玻璃片吸附在匀胶机仪器上,将配置好的离子液体滴在硅片上,转速为2000转/分钟,匀胶时间为60s,其厚度与转速遵循一定的规律,转速越快,凝胶薄膜厚度越小。
第三步,将旋涂了离子液体凝胶的硅片或玻璃片放至真空烤箱中以70℃条件烘烤24小时,以去除多余的丙酮。此时硅片上的离子凝胶薄膜可轻松用镊子夹取,独立操作。
图5为按照实施例2过程配置的匀胶转速与离子液体凝胶薄膜厚度的关系,可看出减少聚合物在配置中的比重之后,厚度均比实例1的薄。五幅图可以看出本实例得到的离子液体凝胶薄膜具有高透明度、高拉伸性、高独立性以及较高的电容,是可以作为柔性导电器件以及凝胶电解质的离子导体。
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (9)
1.一种厚度可控的全透光离子液体凝胶薄膜的制备方法,其特征在于:包括以下步骤:
第一步:在容器中加入离子液体与聚合物,再放入溶剂,以使聚合物和离子液体溶解,将溶解后的混合溶液进行磁力搅拌,使其混合均匀;
第二步:将基底吸附在匀胶机仪器上,将第一步得到的混合溶液滴在基底上,通过设定不同的转速进行旋涂,得到旋涂有离子液体凝胶的基底;
第三步:将第二步得到的旋涂有离子液体凝胶的基底放至真空烤箱中烘烤,得到所述全透光离子液体凝胶薄膜。
2.根据权利要求1所述的厚度可控的全透光离子液体凝胶薄膜的制备方法,其特征在于:所述第一步中,离子液体为N,N-二乙基-N-甲基-N-(2-甲氧乙基)铵基双(三氟甲基磺酰)酰亚胺。
3.根据权利要求1所述的厚度可控的全透光离子液体凝胶薄膜的制备方法,其特征在于:所述第一步中,聚合物为聚偏二氟乙烯-六氟丙烯。
4.根据权利要求1所述的厚度可控的全透光离子液体凝胶薄膜的制备方法,其特征在于:所述第一步中,溶剂为丙酮。
5.根据权利要求1-3任一所述的厚度可控的全透光离子液体凝胶薄膜的制备方法,其特征在于:所述第一步中,离子液体、聚合物、溶剂的质量比为4:1:10。
6.根据权利要求1所述的厚度可控的全透光离子液体凝胶薄膜的制备方法,其特征在于:所述第一步中,磁力搅拌的温度为70℃,时间为一小时。
7.根据权利要求1所述的厚度可控的全透光离子液体凝胶薄膜的制备方法,其特征在于:所述第二步中,基底为硅片或石英片。
8.根据权利要求1所述的厚度可控的全透光离子液体凝胶薄膜的制备方法,其特征在于:所述第二步中,通过改变匀胶机仪器的转速来调整所得全透光离子液体凝胶薄膜的厚度,转速越快,厚度越小。
9.根据权利要求1所述的厚度可控的全透光离子液体凝胶薄膜的制备方法,其特征在于:所述第二步中,烘烤的温度为70℃,时间为24小时。
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