静电喷雾法/原位洗脱法结合制备电致变色薄膜

doi:10.11868/j.issn.1001-4381.2020.001087

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电致变色材料在提倡低碳节能的发展理念下有很好的发展前景, 而探索一种高效简单且性能优异的制备工艺尤为重要。利用静电喷雾法结合原位洗脱法制备了聚合物电致变色薄膜。根据电解质盐的颜色适配性和溶解性, 选择四丁基高氯酸铵(TBAP)作为模板剂, 在易加工的TPA-OMe-PA溶液中添加不同比例的电解质盐, 然后利用静电喷雾技术在ITO玻璃表面沉积制备薄膜, 再通过原位洗脱法去除其中的模板剂-电解质盐, 最终制备出含有多层级孔结构的聚合物薄膜。采用电子扫描显微镜对其形貌进行分析, 利用电化学工作站结合紫外/可见/红外光谱仪研究了薄膜的电致变色性能。研究结果表明, 利用静电喷雾技术与原位洗脱法制备的聚合物薄膜具备多层级孔结构和良好的电致变色性能。其中电解质含量为33.3%(质量分数)时, 多层级孔隙率最高, 且电致变色性能最为优异, 漂白时间/着色时间缩减至0.6 s/1 s, 着色效率达到608.2 cm²·C^-1, 为已报道基于相同材料的电致变色薄膜的最快响应速度。

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	朱陈杰
	陈海权
	于有海

关键词 ：电致变色薄膜, 静电喷雾沉积, 原位洗脱法, 多层级孔结构, 电化学性能

Abstract：

Electrochromic materials have good development prospect under the development concept of promoting low carbon and energy saving. In order to explore the efficient, simple and excellent preparation process, the polymer electrochromic film was prepared by the electrostatic spray method combined with the in-situ elution method. According to the color adaptability and solubility of the electrolyte salt, tetrabutylammonium perchlorate (TBAP) was selected as the template, and different proportions of electrolyte salt were added to the easy-to-process TPA-OMe-PA solution, then film was deposited on the surface of the ITO glass by electrostatic spray technology. After that, the electrolyte salt was precipitated by in-situ washing method. The morphology of the film was analyzed using scanning electron microscope, and the electrochromic properties of the film were studied using the electrochemical workstation combined with ultraviolet/visible/infrared spectrometer. The research results show that the polymer film prepared by electrostatic spray technology and in-situ elution method have multi-level pore structure and excellent electrochromic properties. Especially when the electrolyte content is 33.3%(mass fraction), the multi-layer porosity is the highest, and the electrochromic performance is the best. The bleaching time/coloration time is reduced to 0.6 s/1 s, and the coloration efficiency reaches 608.2 cm²·C^-1, which is the best record for the polyamide based electrochromic film.

Key words： electrochromic film electrostatic spray deposition in-situ washing method multi-level pore structure electrochemical performance

收稿日期: 2020-11-26 出版日期: 2022-01-19

中图分类号:

TQ150.7

通讯作者: 于有海 E-mail: yuyouhai@dhu.edu.cn

作者简介: 于有海(1977—), 男, 研究员, 博士, 研究方向为电致变色、导电高分子等, 联系地址: 上海市松江区人民北路2999号东华大学民用航空复合材料协同创新中心B556(201620), E-mail: yuyouhai@dhu.edu.cn

引用本文:

朱陈杰, 陈海权, 于有海. 静电喷雾法/原位洗脱法结合制备电致变色薄膜[J]. 材料工程, 2022, 50(1): 109-116.
Chenjie ZHU, Haiquan CHEN, Youhai YU. Preparation of electrochromic film by combination of electrostatic spray method/in-situ washing method. Journal of Materials Engineering, 2022, 50(1): 109-116.

链接本文:

http://jme.biam.ac.cn/CN/10.11868/j.issn.1001-4381.2020.001087 或 http://jme.biam.ac.cn/CN/Y2022/V50/I1/109

Fig.1 静电喷雾沉积法-原位洗脱法制备电致变色薄膜的流程示意图

Fig.2 不同含量TBAP及TBAP-33.3%未洗脱盐的薄膜的SEM图
(a)9.1%；(b)23.1%；(c)33.3%；(d)：41.2%；(e)TBAP-33.3%未洗脱盐；(1)表面；(2)截面

Fig.3 不同TBAP含量的电致变色薄膜的循环伏安图

Table 1 薄膜的循环伏安曲线图的氧化电位、还原电位及电位差

Fig.4 不同TBAP含量薄膜的交流阻抗图

Fig.5 电极反应过程的机理研究
(a)不同扫描速率下的CV曲线图；(b)阳极、阴极峰值电流与扫描速率的关系；(c)阳极、阴极峰值电流与扫描速率的平方根的关系

Fig.6 不同含量TBAP薄膜的光谱仪-电化学工作站联用测试图
(1)吸收光谱图；(2)电位在-0.25 V/0.95 V之间以40 s间隔振荡时792 nm处的光透射率随时间变化；(3)薄膜的切换速度；
(a)9.1%；(b)23.1%；(c)33.3%；(d)41.2%

Table 2 不同TBAP含量薄膜的电致变色性能与文献中的性能参数比较

Fig.7 薄膜的着色效率图
(a)TBAP-9.1%;(b)TBAP-23.1%;(c)TBAP-33.3%;(d)TBAP-41.2%

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