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In Situ Lithiated Reference Electrode: Four Electrode Design for In-operando Impedance Spectroscopy

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Operando Raman spectroscopy for investigating lithium deposition/dissolution and diffusion at the microelectrode

Hayate Mukofukasawa¹, Koji Hiraoka¹, Shiro Seki¹

¹Graduate School of Applied Chemistry and Chemical Engineering, Kogakuin University 2665-1 Nakano-machi Hachioji-shi Tokyo 192-0015 Japan shiro-seki@cc.kogakuin.ac.jp.

|July 14, 2025

Summary

We visualized lithium deposition and diffusion using operando Raman spectroscopy. This technique reveals insights into lithium-ion battery interfaces, showing how electrolyte components change during cycling.

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Area of Science:

Electrochemistry
Materials Science
Spectroscopy

Background:

Understanding lithium deposition and diffusion is critical for lithium-ion battery performance and safety.
Microelectrode interfaces present unique challenges for in-situ analysis.

Purpose of the Study:

To develop and apply an operando Raman spectroscopy method for visualizing lithium deposition and diffusion at the microelectrode interface.
To investigate the behavior of electrolyte components during lithium deposition and dissolution.

Main Methods:

Developed an operando Raman spectroscopy technique.
Utilized microelectrode setups for in-situ measurements.
Analyzed spectral changes associated with lithium deposition and dissolution.

Main Results:

Visualized lithium deposition and diffusion processes at the microelectrode interface.
Observed the release of free ethylene carbonate (EC) and fluoroethylene carbonate (FSC) during lithium deposition.
Detected rapid lithium-ion (Li+) coordination changes during dissolution.
Validated diffusion layer thickness estimations against theoretical predictions.

Conclusions:

Operando Raman spectroscopy is a powerful tool for studying lithium-ion battery interfaces.
The method provides insights into electrolyte-electrode interactions during cycling.
This technique can advance the understanding of battery degradation and performance limitations.