电化学膨胀计联用现场X-射线衍射表征螺环季铵盐插嵌石墨负极

引用本文: 陈聪聪, 李家玉, 黄玉豪, 张磊, 王云举, 王宏宇. 电化学膨胀计联用现场X-射线衍射表征螺环季铵盐插嵌石墨负极[J]. 分析化学, 2022, 50(3): 413-423. doi: 10.19756/j.issn.0253-3820.211138 shu

Citation: CHEN Cong-Cong, LI Jia-Yu, HUANG Yu-Hao, ZHANG Lei, WANG Yun-Ju, WANG Hong-Yu. Study on Quaternary Alkyl Ammonium Intercalation into Graphite Negative Electrodes by In-Situ X-ray Diffraction and Electrochemical Dilatometry[J]. Chinese Journal of Analytical Chemistry, 2022, 50(3): 413-423. doi: 10.19756/j.issn.0253-3820.211138 shu

电化学膨胀计联用现场X-射线衍射表征螺环季铵盐插嵌石墨负极

¹中国科学院长春应用化学研究所, 电分析化学国家重点实验室, 长春 130022;
²中国科学技术大学, 合肥 230026

通讯作者: 王宏宇,E-mail:hongyuwang@ciac.ac.cn

基金项目:
国家自然科学基金项目（No.21975251）资助。

摘要: 以活性炭/石墨电容器为平台，通过电化学膨胀计（ECD）和原位X射线衍射（XRD）技术，对螺环季铵盐阳离子（SBP⁺）电化学插嵌不同石墨负极过程中的膨胀现象进行了研究。ECD能准确监测石墨电极的宏观厚度变化，而原位XRD可以实时探测石墨电极微观晶体结构的变化。通过两者数据相互对照，发现微观尺度上因离子插嵌导致的石墨XRD数据非常接近（晶格膨胀程度为56%~59%），但在宏观上却展现出截然不同的膨胀现象，大颗粒片层状石墨电极表现出更大幅度的膨胀（12%），而小粒径的片层状石墨和球状石墨电极的膨胀幅度却很小（5%~6%）。通过扫描电子显微镜观测发现，造成此现象的原因与石墨形貌结构以及其在集流体上的排列密切相关。大颗粒片层状石墨结构和排列上的高度有序性导致电极膨胀相对更大，而小粒径片层石墨杂乱的排列以及天然球状石墨独特的结构会使膨胀向各个方向分散，造成整体膨胀幅度更小。

关键词:

English

Study on Quaternary Alkyl Ammonium Intercalation into Graphite Negative Electrodes by In-Situ X-ray Diffraction and Electrochemical Dilatometry

¹State Key Laboratory of Electroanalytical Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022, China;
²University of Science and Technology of China, Hefei 230026, China

Corresponding author: WANG Hong-Yu, hongyuwang@ciac.ac.cn

Received Date: 22 February 2021
Revised Date: 30 March 2021
Fund Project:
Supported by the National Natural Science Foundation of China (No.21975251).

Abstract: In activated carbon/graphite capacitors, electrochemical dilatometry and in-situ X-ray diffraction (XRD) were used to investigate the expansion of graphite negative electrodes during the storage of spiro-(1,1') bipyrrolidinium cation (SBP⁺) from both macro and micro perspectives. The electrochemical dilatometry can accurately monitor the changes in the macroscopic thickness of the graphite electrode, while in-situ XRD can detect the changes in the microscopic crystal structure of the graphite electrode in real time. Through the comparison of the two set of data, it was found that the relative lattice expansion of graphite caused by ion intercalation on the microscopic scale was very close (56%-59%), with a completely different expansion phenomenon from a macroscopic point of view. Large graphite flakes exhibited a greater expansion (12%), while graphite flakes with a smaller size and spherical graphite demonstrated a very small expansion (5%-6%). The scanning electron microscope test showed that this tendency was closely related to the morphology of graphite and the arrangement of graphite particles on the current collector. The high orientation of large graphite flakes led to the relatively larger electrode expansion, while the disorderly arrangement of thin graphite flakes and the isotropic structure of natural spherical graphite would cause the expansion to be dispersed in all directions, and then made the overall expansion smaller.

Key words:

Electrochemical dilatometer
/ In-situ X-ray diffraction
/ Spiro-(1,1')-bipyrrolidinium tetrafluoroborate
/ Graphite intercalation compounds

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沈阳化工大学材料科学与工程学院沈阳 110142

电化学膨胀计联用现场X-射线衍射表征螺环季铵盐插嵌石墨负极

通讯作者: 王宏宇,E-mail:hongyuwang@ciac.ac.cn

English

Study on Quaternary Alkyl Ammonium Intercalation into Graphite Negative Electrodes by In-Situ X-ray Diffraction and Electrochemical Dilatometry

Corresponding author: WANG Hong-Yu, hongyuwang@ciac.ac.cn

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

电化学膨胀计联用现场X-射线衍射表征螺环季铵盐插嵌石墨负极

通讯作者: 王宏宇,E-mail:hongyuwang@ciac.ac.cn

English

Study on Quaternary Alkyl Ammonium Intercalation into Graphite Negative Electrodes by In-Situ X-ray Diffraction and Electrochemical Dilatometry

Corresponding author: WANG Hong-Yu, hongyuwang@ciac.ac.cn

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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