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1、分类号：O69 密 级：公开档案号：2021-06-09-081704-24-012 学 号：1111091012 硕 士 学 位 论 文(学术学位含联吡啶类电致变色材料的制备与全固态器件性能研究学 生 姓 名：指导教师姓名：学 科 门 类：工 学专 业 名 称：应用化学研 究 方 向：材料化学及其应用二一四年六月含联吡啶类电致变色材料的制备与全固态器件性能研究学 生 姓 名：指导教师姓名：专 业 名 称：应用化学Preparation of the Electrochromic Materials Containing Bipyridine Derivatives and Propertie
2、s of the Solid-state DevicesMaster Candidate: Supervisor: Professor Major: Applied Chemistry June,2021 摘要摘 要联吡啶类有机电致变色材料因其丰富的色彩和较快的颜色转换速度成为当前绿色光电材料的研究热点。本文以4,4-联吡啶和取代三联吡啶为前驱体，合成了4类不同类型的联吡啶化合物，共计13个目标化合物，并对其结构做了表征。运用紫外和电化学分析了各化合物的光电性质和电致变色机理。结果说明：小分子紫精是通过氧化复原使分子结构在苯式和醌式间相互转换实现电致变色的，而联吡啶金属配合物的电致变色那么是通
3、过金属离子与配体间电荷迁移来实现的。分别通过旋转涂布和电化学沉积法在ITO导电玻璃上制备了联吡啶化合物的电致变色薄膜，并对其光电性能做了测试。以LiClO4-PMMA/PEO聚合物电解质为PE层制作了基于ITO玻璃的全固态电致变色器件，对器件的性能进行了测试。结果说明：以4,4-双三苯胺紫精为EC材料的电致变色能够在0-0.8V之间实现由无色到蓝绿色的可逆变化；以联吡啶的Fe()配合物和Ru()配合物为EC材料的电致变色器件在03V之间分别能够实现由紫色到蓝绿色和由橙红色到绿色的可逆变化。所有器件在不超过3 V的驱动电压下，可以在着色和褪色两种状态下稳定可逆变化，着色/褪色时间响应较快，开路记
4、忆时间长达300min，说明本文所制备的器件均具有优良的电致变色性能，有望制作实用的电致变色器件。关键词：联吡啶 紫精 电致变色 循环伏安 固体电解质 全固态电致变色器件 AbstractAbstractOrganic electrochromic materials with bipyridine group are the hot issue of focus in green photovoltaic materials due to its rich colors and fast color conversion speed. In this paper, four kinds of
5、 different bipyridine-based compounds, totaling 13 target compounds, were synthesized using 4,4-bipyridine and substituted terpyridine as precursors, and their structures were characterized. The optical performance and electrochromic mechanism of the compounds were tested via UV-visible spectrophoto
6、metry and cyclic voltammetry. The results showed that: the small molecule viologen achieves electrochromic when its molecule structure change between benzene and quinone by redox, while the electrochromic of bipyridine metal complexes are achieved through charge transferring between the metal ions a
7、nd the ligands.Electrochromic films of bipyridine compounds were prepared by spin coating and electrochemical deposition on ITO conductive glass respectively, and their optical performance were tested. All-solid-state electrochromic devices based on conductive ITO glass were fabricated using LiClO4-
8、PMMA/PEO polymer electrolyte as PE layer, and the performances of the devices were tested. The results showed: the electrochromic device of 4,4-bis-triphenylamine viologen has reversible color change from colorless to blue-green between 0V and -0.8V; while the devices of Fe() bipyridine metal comple
9、xes and Ru() bipyridine metal complexes have reversible color change from purple to blue-green and orange to green respectively under the potential of 0 3V. All the devices can stably shift in two states of coloring and fading under a driving potential which is not higher than 3V. All the devices re
10、sponse fast while coloring and fading. And the open memory time of the ECD is as long as 300min. All of these proved that the ECDs have excellent electrochromic properties, which are expected to produced to practical electrochromic devices. Keywords: bipyridine, viologen, electrochromic, cyclic volt
11、ammetry, solid electrolyte, all-solid electrochromic devicesII 目录目录摘 要IAbstractII目录III第一章 绪论11.1电致变色简介11.2电致变色材料31.2.1 无机电致变色材料31.2.2有机电致变色材料41.3 电致变色器件71.3.1电致变色器件的结构71. 3.2 电致变色技术的应用91.4 联吡啶衍生物电致变色材料的研究进展101.5 选题意义和研究内容12第二章 联吡啶化合物的合成与表征142.1 引言142.2仪器与药品142.3 三联吡啶金属配合物的制备与表征152.3.1 配体的制备及表征152.3.
12、2 三联吡啶金属配合物1a、1b、2a、2b的制备及表征182.4 三联吡啶-三苯胺金属配合物的制备与表征192.4.1 三联吡啶-三苯胺配体4、5、6的合成与表征202.4.2 三联吡啶-三苯胺配体金属配合物4a、4b，5a、5b和6a、6b的合成与表征222.5 4,4-双三苯胺紫精的制备与表征232.6三联吡啶-芴类衍生物金属配合物的制备与表征242.6.1 配体2,7-双(苯基-4-(2,2 :6,2 - 三联吡啶)-9,9-二己基芴的制备24 金属配合物7a和7b的合成252.7 本章小结26第三章 联吡啶化合物的性能测试273.1 引言273.2 紫外吸收273.3 循环伏安测试3
13、13.4 结果与讨论363.4.1紫外可见吸收光谱的比拟363.4.2电化学性质的比拟383.5 本章小结39第四章 用于全固态电致变色器件的聚合物电解质的制备与性能研究404.1 引言404.2 聚合物电解质的制备414.2.1 制备聚合物电解质所需仪器与药品414.2.2聚合物电解质的制备414.3 聚合物电解质的结构表征与性能测试414.3.1 PE膜的结构表征414.3.2 PE膜的厚度测试424.3.3 PE膜的热稳定性分析434.3.4 PE膜的电导率研究444.3.5 PE膜的光学性能454.4本章小结46第五章 联吡啶电致变色薄膜与全固态电致变色器件475.1引言475.2 联
14、吡啶化合物电致变色薄膜的制备与讨论475.2.1 电致变色薄膜材料的制备475.2.2 电致变色膜的紫外-可见光谱测试485.3 全固态ECDs的制作515.4 全固态ECDs的性能测试525.4.1 ECDs的驱动电压525.4.2着色时间和褪色时间555.4.3 ECDs的开路记忆时间555.4本章小结55第六章 总结与展望576.1 全文总结576.2 展望58参考文献59附表一：文中常用英文缩写67致 谢68作者简介69III 第一章 绪论第一章 绪论1.1电致变色简介随着地球资源的过渡消耗及人类生产活动对环境的影响，绿色环保、节能低碳的新型功能性材料已经越来越受到人们的重视。人们对于产品制造从最初的材料强度，硬度，刚性和柔韧性等机械特性外，人们逐渐要
