硅酸盐学报

基于溶胶-凝胶法制备的离子导体层的电致变色器件及性能

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苏文敬 ¹^,² , 王天齐 ¹^,² , 金克武 ¹^,² , 汤永康 ¹^,² , 沈洪雪 ¹^,² , 李刚 ¹^,²

硅酸盐学报 | 先进玻璃材料技术与产业发展专题—研究论文 2025,53(10): 2861-2869

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硅酸盐学报 |先进玻璃材料技术与产业发展专题—研究论文 2025 , 53 (10) : 2861 -2869

基于溶胶-凝胶法制备的离子导体层的电致变色器件及性能

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苏文敬¹^,², 王天齐¹^,², 金克武¹^,², 汤永康¹^,², 沈洪雪¹^,², 李刚¹^,²

作者信息

^1．中建材玻璃新材料研究院集团有限公司，先进玻璃材料全国重点实验室，安徽蚌埠 233018

^2．安徽省硅基材料实验室，安徽蚌埠 233018

作者简介:

苏文敬（1987—），男，硕士，高级工程师。

Electrochromic Devices with Ion Conductor Layers Prepared by Sol-gel Method and Their Performances

Wenjing SU¹^,², Tianqi WANG¹^,², Kewu JIN¹^,², Yongkang TANG¹^,², Hongxue SHEN¹^,², Gang LI¹^,²

Affiliations

^1.State Key Laboratory of Advanced Glass Materials, CNBM Research Institute for Advanced Glass Materials Group Co., Ltd., Bengbu 233018, Anhui, China

^2.Silica-based Materials Laboratory of Anhui Province, Bengbu 233018, Anhui, China

SU Wenjing (1987-), male, Master, Senior Engineer. E-mail: 281226975@qq.com

出版时间: 2025-10-20 doi: 10.14062/j.issn.0454-5648.20250201

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摘要

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开发了离子导体材料钽酸锂的溶胶-凝胶法合成工艺并采用旋涂法制备了钽酸锂薄膜，采用X射线衍射仪、原子力显微镜及电化学工作站等对薄膜进行了物相形貌及电化学性能表征。其中溶胶-凝胶法制备的钽酸锂薄膜室温离子电导率可以达到7.44×10^-7 S/cm。采用旋涂法分别在ITO/NiO和ITO/WO₃基底上制备了钽酸锂薄膜，并采用磁控溅射法制备相应的电致变色层和离子存储层及透明导电电极，通过液相法与PVD法结合制备出了结构为ITO/NiO/LiTaO₃/WO₃/ITO的电致变色器件，研究发现以ITO/NiO为基底旋涂钽酸锂制备的电致变色器件具有较高的变色幅度和较快的转变速率，在施加5 V外加电压时，可见光调节幅度可以达到26%，着色时间约为50 s，褪色时间为56 s。而在氧化钨薄膜表面旋涂钽酸锂制备的器件对近红外波段有较好的调控，但是相同电压下器件褪色和着色速率大幅下降，相同电压下可见光调节幅度也有所降低。

关键词

溶胶-凝胶法 / 锂离子导体层 / 电致变色 / 全固态无机电致变色器件 / 局域表面等离激元振荡 / 近红外波段调控

Abstract

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Introduction

Electrochromic device (ECD) is comprised of five superimposed layers, i.e., transparent conducting layer, electrochromic layer, ion conductor layer, ion storage layer and another transparent conducting layer, respectively. It can modulate the amount of solar radiation transmitting through it under applied voltage, often used as smart windows or facades to adjust the light and heat entering buildings proactively, which can sufficiently reduce the energy consumption. The existing ECDs are mainly fabricated by a magnetron sputtering method, which has a low productivity and high cost, especially for the ion conductor layer. Sol-gel method is a simple and relatively cheap method for preparing thin films, and massive researches are conducted on sol-gel electrochromic thin films such as tungsten oxide, nickel oxide etc.. In this work, an ion conductor layer was prepared by a sol-gel method, and its application in electrochromic device and their performance were also investigated.

Methods

Lithium tantalite sol was synthesized with lithium acetate (LiAc) and tantalum pentaethoxide (TaEt) as precursors and 1,2-Propanediol as a solvent. The molar ratio of LiAc and TaEt was 1∶1. Lithium tantalite thin films were prepared by a spin coating method and heat-treated in air at 400 ℃ for 2 h. Some of the sol was dried and the subsequently formed powder was heated at 600-700 ℃. The phase compositions of the films and powders were characterized by X-ray diffraction (XRD), and the electrochemical properties of thin films were analyzed.

The electrochromic devices with a structure of ITO/NiO/LiTaO₃/WO₃/ITO were prepared by PVD method and subsequent sol-gel method. The tungsten oxide or nickel oxide thin film layer was firstly sputtered on the ITO glass and then lithium tantalite thin films were spin-coated onto the as prepared films. After heating process at 400 ℃ for 2 h, another layer of the tungsten oxide or nickel oxide films were sputtered, and another layer of ITO thin film was finally sputtered as a conducting electrode. The electrochromic devices were noted as EC-N when lithium tantalite was spin-coated onto nickel oxide films and as EC-W when lithium tantalite was spin-coated onto tungsten oxide films. The transmittance changes were measured by UV-vis-IR spectrometer.

Results and discussion

The XRD patterns show that powders dried and heated from the sol are a polycrystalline lithium tantalite, and thin films are amorphous. The analysis of electrochemical impedance spectroscopy indicates that the sol-gel lithium tantalite thin film has an ionic conductivity of 7.44×10^-7 S/cm at room temperature, which is comparable to that of sputtered film. As for the devices, the XRD patterns show that nickel oxide thin film layers are both polycrystalline in EC-N and EC-W, while tungsten oxides is polycrystalline in EC-W and amorphous in EC-N. The XRD patterns and XPS spectra also show the existence of WO_3-_x phase in polycrystalline tungsten oxide films.

For electrochromic properties of the two groups of devices, transmittance regulations are measured at a fixed wavelength of 550 nm. For both groups, the differences of transmittance between colored and bleached state increase with increasing voltage. The maximum of transmittance change for EC-N is 26% at 5 V, with transmittance of around 72% at bleached state and 46% at colored state. Its coloring time is 50 s and bleaching time is 56 s. The results of cyclic test show that the differences of colored and bleached states keep stable, no obvious degeneration occurs after 60 cycles. The transmittance changes for EC-W have a lower value when applied the same voltages as in EC-N, and the switching speed is much slower. Its transmittance change is 14% at 3 V, while the coloring and bleaching time are both larger than 2 min, exceeding the setting range. It can be concluded that EC-N has a better property for regulation of visible light, and crystallinity can slow the switching process.

The transmittance spectra of colored states in vis-NIR range show that EC-W has a significant modulating performance for NIR, which can be attributed to the existence of WO_3-_x components. As reported, oxygen deficient components can generate a local surface plasmon resonance effect that can result in absorption in the spectral range of NIR.

Conclusions

Electrochromic devices fabricated by a process that lithium tantalite was spin-coated on nickel oxide had better electrochromic properties in a visible spectral range, with larger optical modulations and a higher switching speed less than 1 min. The devices with lithium tantalite spin-coated on the tungsten oxide films could have a slower coloring and bleaching rate, while showing a better near-infrared modulation effect. These results indicated a routine for the realization of electrochromic devices that could modulate light and heat simultaneously and independently.

Key words

sol-gel method / lithium ion conductor layer / electrochromism / all solid state inorganic electrochromic device / localized surface plasmon resonance / near-infrared modulation

引用本文

苏文敬, 王天齐, 金克武, 汤永康, 沈洪雪, 李刚. 基于溶胶-凝胶法制备的离子导体层的电致变色器件及性能. 硅酸盐学报, 2025 , 53 (10) : 2861 -2869 . DOI: 10.14062/j.issn.0454-5648.20250201

Wenjing SU, Tianqi WANG, Kewu JIN, Yongkang TANG, Hongxue SHEN, Gang LI. Electrochromic Devices with Ion Conductor Layers Prepared by Sol-gel Method and Their Performances[J]. Journal of the Chinese Ceramic Society, 2025 , 53 (10) : 2861 -2869 . DOI: 10.14062/j.issn.0454-5648.20250201

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2025年第53卷第10期

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doi: 10.14062/j.issn.0454-5648.20250201

接收时间：2025-03-24
首发时间：2026-10-21
出版时间：2025-10-20

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收稿日期：2025-03-24
修回日期：2025-04-17

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^1．中建材玻璃新材料研究院集团有限公司，先进玻璃材料全国重点实验室，安徽蚌埠 233018

^2．安徽省硅基材料实验室，安徽蚌埠 233018

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2种不同金属材料的力学参数

科 Family	属数 Number of genus	种数 Number of species	占总种数比例 Percentage of total species (%)	属 Genus	种数 Number of species	占总种数比例 Percentage of total species (%)
鹅膏菌科Amanitaceae	2	11	5.26	鹅膏菌属 Amanita	10	4.78
小菇科 Mycenaceae	2	12	5.74	丝盖伞属 Inocybe	5	2.39
多孔菌科 Polyporaceae	8	14	6.70	蜡蘑属 Laccaria	5	2.39
红菇科 Russulaceae	3	23	11.00	小皮伞属 Marasmius	6	2.87
				小菇属 Mycena	11	5.26
				光柄菇属 Pluteus	5	2.39
				红菇属 Russula	17	8.13
				栓菌属 Trametes	5	2.39

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