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Related Concept Videos

Electrochemical Systems01:24

Electrochemical Systems

Electrochemical systems provide a fascinating insight into the dynamic interplay of charged species within various phases. One notable example is the interaction between a membrane permeable to K⁺ ions but not to Cl⁻ ions, separating an aqueous KCl solution from pure water. As K⁺ ions diffuse through the membrane, they generate net charges on each phase, leading to a potential difference between them.Similarly, when a piece of Zn is immersed in an aqueous ZnSO₄ solution, the Zn metal, composed...
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In the region where two bulk phases meet, an intricate electric charge distribution arises due to charge transfer, ion adsorption, molecular orientation, and charge distortion. This complex distribution is commonly referred to as the electrical double layer.When a solid electrode interfaces with ions in an electrolyte solution, the speed of electron transfer dictates the rates of oxidation and reduction. The electrode acquires a charge through the escape of atoms into the solution as cations or...

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Updated: Jun 18, 2026

Characterization of Electrode Materials for Lithium Ion and Sodium Ion Batteries Using Synchrotron Radiation Techniques
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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
PubMed
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.

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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.