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Updated: May 7, 2026

Characterization of Electrode Materials for Lithium Ion and Sodium Ion Batteries Using Synchrotron Radiation Techniques
Published on: November 11, 2013
Unveiling Physical and Chemical Changes in All-Solid-State Battery: An Operando Synchrotron Chemical Imaging Study
Chayene Gonçalves Anchieta1, Barthélémy Lelotte2, Hari Vignesh Ramasamy2
1Swiss Light Source, Paul Scherrer Institut PSI, Villigen, Switzerland.
This study reveals heterogeneous lithium dynamics in all-solid-state batteries using synchrotron X-ray imaging. It identifies particle-level lithium diffusion, water-induced phase changes, and parasitic reactions impacting battery performance.
Area of Science:
- Materials Science
- Electrochemistry
- Analytical Chemistry
Background:
- Understanding complex battery material dynamics at high resolution is crucial for next-generation energy storage.
- Current operando techniques struggle to provide micrometer spatial and relevant temporal resolution for heterogeneous battery systems.
Purpose of the Study:
- To develop and apply a synchrotron-based operando chemical imaging methodology using microfocus X-ray diffraction (µ-XRD) scanning imaging.
- To investigate the dynamics of an all-solid-state battery (ASSB) with Li-rich NCM cathode under realistic operating conditions.
Main Methods:
- Utilized synchrotron-based operando µ-XRD scanning imaging.
- Integrated the ASSB within a custom-designed electrochemical cell for optimal XRD analysis.
- Performed operando XRD mapping across a large field of view with micrometer resolution.
Main Results:
- Observed heterogeneous lithiation/delithiation within individual Li-rich NCM particles, indicating differential lithium diffusion.
- Identified reversible formation of YCl2(H2O)6Cl due to water residues.
- Detected irreversible dissolution of Li2S and formation of LiOH parasitic phases.
Conclusions:
- The developed µ-XRD methodology provides unprecedented spatiotemporal resolution for battery material analysis.
- Heterogeneous intraparticle lithium diffusion and parasitic reactions are key challenges in ASSBs.
- This approach offers new insights for optimizing various battery chemistries, including Na-ion, Zn-air, Li-air, Li-ion, and Li-S batteries.
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