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Published on: November 11, 2013
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Operando XPS: A Novel Approach for Probing the Lithium/Electrolyte Interphase Dynamic Evolution.
A Benayad1, J E Morales-Ugarte1,2, C C Santini3
1Université Grenoble Alpes, CEA-LITEN, 17 rue des Martyrs, 38054 Grenoble Cedex 9, France.
The Journal of Physical Chemistry. A
|January 21, 2021
Summary
This study introduces a novel operando cell for X-ray photoemission spectroscopy (XPS) to analyze lithium-ion battery (LIB) interfaces. The new design enables real-time monitoring of lithium metal reactivity with ionic liquid electrolytes, improving understanding of LIB degradation.
Area of Science:
- Materials Science
- Electrochemistry
- Surface Science
Background:
- Coupling photoemission spectroscopy with other characterization methods advances materials science but often involves sequential, separate analyses, raising surface equivalence concerns.
- Operando techniques are crucial for studying lithium-ion battery (LIB) materials and interfaces, yet limitations in material sensitivity and characterization methods hinder understanding of performance degradation.
- Investigating electrode-electrolyte interfaces in LIBs requires advanced techniques to probe dynamic chemical and electronic changes.
Purpose of the Study:
- To develop and demonstrate a novel operando cell for X-ray photoemission spectroscopy (XPS) specifically designed for electrochemical applications.
- To investigate the reactivity of lithium metal interfaces with ionic liquid electrolytes under various electrochemical conditions.
- To overcome limitations in current operando techniques for studying dynamic interfacial processes in lithium-ion batteries.
Main Methods:
- Designed and implemented a new operando cell compatible with X-ray photoemission spectroscopy (XPS) under electrochemical control.
- Utilized Li/Li symmetrical cells with two distinct ionic liquid electrolytes (C1C6ImTFSI and C1C6ImFSI) containing LiTFSI salt.
- Performed XPS measurements under open circuit voltage and polarization conditions to monitor lithium metal surface reactivity.
Main Results:
- Successfully demonstrated the capability of the operando cell to probe the lithium metal-electrolyte interface in dynamic mode.
- Tracked the evolution of chemical structure and surface potential at the lithium/electrolyte interface during electrochemical cycling.
- Identified and optimized blocking issues to enable accurate operando XPS (OXPS) measurements for interfacial studies.
Conclusions:
- The developed operando cell provides a powerful tool for real-time interfacial analysis in lithium-ion battery research.
- This technique facilitates a deeper understanding of lithium metal reactivity and degradation mechanisms in ionic liquid electrolytes.
- The study highlights the importance of in-situ/operando characterization for advancing battery technology and addressing performance limitations.
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