Proceedings of MATSUS Spring 2025 Conference (MATSUSSpring25)
DOI: https://doi.org/10.29363/nanoge.matsusspring.2025.441
Publication date: 16th December 2024
Unlocking the secrets of electrochemical interfaces is key to advancing energy storage materials, yet these processes remain a complex and critical challenge. Among the tools for probing these elusive regions, X-ray photoelectron spectroscopy (XPS) stands out for its ability to analyze electronic structures and characterize the solid-electrolyte interphase (SEI) formed between electrodes and electrolytes. Traditional ex-situ studies (conducted postmortem on electrodes cycled in liquid electrolytes) have showcased XPS as the go-to technique for SEI analysis, thanks to its probing depth (up to 10 nm) matching typical SEI thicknesses [1, 2]. However, these methods often miss transient or intermediate species, crucial for unraveling charge transfer dynamics.
For solid-state batteries, the challenge deepens: the SEI formed between lithium metal anodes and solid electrolytes is buried, inaccessible to direct analysis. Preparing ex-situ samples without disrupting the SEI [3] further complicates the picture. Understanding this buried interphase demands alternative approaches that can monitor its formation and evolution in real time.
Herein, a virtual charging operando XPS (OpXPS) technique was deployed to electrodeposit lithium directly on a halide-based solid electrolyte within the XPS chamber, enabling real-time tracking of SEI formation. Halide solid electrolytes are promising for next-generation all-solid-state batteries, thanks to their outstanding properties such as high ionic conductivity, oxidative stability and ductility. However, their reactivity with lithium metal remains a major challenge [4].
OpXPS revealed the formation of a dynamic mixed ionic-electronic conductive (MIEC) interphase between the halide electrolyte and lithium metal anode. Complementary Electrochemical Impedance Spectroscopy (EIS) and Distribution of Relaxation Times (DRT) analyses provided critical correlations between interfacial resistance and evolving chemical composition. These techniques demonstrate the powerful capabilities of OpXPS in decoding the complex dynamics of buried interfaces, paving the way for designing stable and efficient solid-state battery systems.
Funded by the European Union`s Horizon Europe research and innovation program under grant agreement No 101069681 (HELENA Project).
Saint-Gobain is acknowledged for providing Solid Electrolyte powder material.
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