Study of structural and electrochemical evolution of LPSCL during “cold sintering” process
Ove Korjus a b, Saptarshee Mitra b, Quentin Berrod a b, Victor Vanpeene a, Markus Appel a, Emanuelle Suard a, Sandrine Lyonnard b, Claire Villevieille c
a Institut Laue-Langevin - 71 avenue des Martyrs CS 20156, 38042 GRENOBLE Cedex
b CEA Grenoble, 17 rue des Martyrs, Grenoble, France
c Univ. Grenoble Alpes, Univ. Savoie Mont Blanc, CNRS, Grenoble INP*, LEPMI, 38000 Grenoble, France
Proceedings of 24th International Conference on Solid State Ionics (SSI24)
Advanced characterisation techniques: fundamental and devices
London, United Kingdom, 2024 July 14th - 19th
Organizers: John Kilner and Stephen Skinner
Poster, Ove Korjus, 623
Publication date: 10th April 2024

Solid-state lithium-ion batteries (SLIBs) are envisaged as next-generation to conventional Li-ion batteries. However, to date, they have suffered several issues arising from the engineering and control of their solid-solid interfaces.

Li6PS5Cl (LPSCL), one material from the thiophosphate family, possesses several advantages, such as high ionic conductivity and a “cold sintered” ability1. However, the ionic conductivity can range from 0.06 to 4.73 at room temperature2,3 based on materials quality, granulometry surface chemistry, etc., which explains such an extensive results dispersion.

In this study, we conducted in situ “cold sintering” of Li6PS5Cl electrolyte while simultaneously measuring Electrochemical Impedance Spectroscopy and micro X-ray tomography at ID19 in the European Synchrotron Radiation Facility (ESRF) to understand the “cold sintering” process of LPSCL electrolyte and establish the relationship between tortuosity, electrolyte microstructure and ionic conductivities.

One of the things we saw from the in situ “cold sintering” experiment was the intense cracking of big LPSCL secondary particles (Fig. 2a.), and at the same time, not many changes to the particle shape of the secondary particles. We saw an evolution of electrolyte conductivity from the simultaneous electrochemical impedance spectroscopy measurements (Fig. 2b.). To get more information about the nature of the conductivity change during the “cold sintering” of the electrolyte, additional advanced laboratory experiments using electrochemical impedance spectroscopy at very low temperatures were carried out. It helped us to separate the grain boundaries evolution to one of the bulk ionic conductivity, giving a new correlation between electrode microstructure and electrochemical measurement.

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