Monitoring metallic sub-micrometric lithium structures in Li-ion batteries by in situ electron paramagnetic resonance correlated spectroscopy and imaging

Charles-Emmanuel Dutoit (), Mingxue Tang, Didier Gourier, Jean-Marie Tarascon, Hervé Vezin () and Elodie Salager
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Charles-Emmanuel Dutoit: CNRS, CEMHTI UPR3079, Université d’Orléans
Mingxue Tang: CNRS, CEMHTI UPR3079, Université d’Orléans
Didier Gourier: Chimie-ParisTech, PSL Université, CNRS, Institut de Recherche de Chimie-Paris (IRCP)
Jean-Marie Tarascon: Réseau sur le Stockage Electrochimique de l’Energie (RS2E), FR CNRS 3459
Hervé Vezin: Université Lille Nord de France, CNRS UMR8516, LASIRE
Elodie Salager: CNRS, CEMHTI UPR3079, Université d’Orléans

Nature Communications, 2021, vol. 12, issue 1, 1-6

Abstract: Abstract Monitoring the formation of dendrites or filaments of lithium is of paramount importance for Li-based battery technologies, hence the intense activities in designing in situ techniques to visualize their growth. Herein we report the benefit of correlating in situ electron paramagnetic resonance (EPR) spectroscopy and EPR imaging to analyze the morphology and location of metallic lithium in a symmetric Li/LiPF6/Li electrochemical cell during polarization. We exploit the variations in shape, resonance field and amplitude of the EPR spectra to follow, operando, the nucleation of sub-micrometric Li particles (narrow and symmetrical signal) that conjointly occurs with the fragmentation of bulk Li on the opposite electrode (asymmetrical signal). Moreover, in situ EPR correlated spectroscopy and imaging (spectral-spatial EPR imaging) allows the identification (spectral) and localization (spatial) of the sub-micrometric Li particles created by plating (deposition) or stripping (altered bulk Li surface). We finally demonstrate the possibility to visualize, via in situ EPR imaging, dendrites formed through the separator in the whole cell. Such a technique could be of great help in mastering the Li-electrolyte interface issues that plague the development of solid-state batteries.

Date: 2021
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DOI: 10.1038/s41467-021-21598-2

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