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

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

CHEN Cong-Cong ^1,2 ,
LI Jia-Yu ^1,2 ,
HUANG Yu-Hao ^1,2 ,
ZHANG Lei ^1,2 ,
WANG Yun-Ju ^1,2 ,
WANG Hong-Yu ^1,2,,

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).

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