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Article

Surface Fluorination for the Stabilization in Air of Garnet-Type Oxide Solid Electrolyte for Lithium Ion Battery

1
Institut de Chimie de Clermont-Ferrand (UMR 6296), Université Clermont Auvergne, CNRS, BP 10448, F-63000 Clermont-Ferrand, France
2
Centre de Recherche & Innovation, Syensqo, 52 Rue de la Haie Coq, 93300 Aubervilliers, France
3
Solvay, 9 rue des Cuirassiers, 69003 Lyon, France
*
Author to whom correspondence should be addressed.
Batteries 2025, 11(7), 268; https://doi.org/10.3390/batteries11070268
Submission received: 23 May 2025 / Revised: 7 July 2025 / Accepted: 8 July 2025 / Published: 16 July 2025

Abstract

After reviewing the state of the art of the fluorination of inorganic solid electrolytes, an application of gas/solid fluorination is given and how it can be processed. Garnet-type oxide has been chosen. These oxides with an ideal structure of chemical formula A3B2(XO4)3 are mainly known for their magnetic and dielectric properties. Certain garnets may have a high enough Li+ ionic conductivity to be used as solid electrolyte of lithium ion battery. The surface of LLZO may be changed in contact with the moisture and CO2 present in the atmosphere that results in a change of the conductivity at the interface of the solid. LiOH and/or lithium carbonate are formed at the surface of the garnet particles. In order to allow for handling and storage under normal conditions of this solid electrolyte, surface fluorination was performed using elemental fluorine. When controlled using mild conditions (temperature lower or equal to 200 °C, either in static or dynamic mode), the addition of fluorine atoms to LLZO with Li6,4Al0,2La3Zr2O12 composition is limited to the surface, forming a covering layer of lithium fluoride LiF. The effect of the fluorination was evidenced by IR, Raman, and NMR spectroscopies. If present in the pristine LLZO powder, then the carbonate groups disappear. More interestingly, contrary to the pristine LLZO, the contents of these groups are drastically reduced even after storage in air up to 45 days when the powder is covered with the LiF layer. Surface fluorination could be applied to other solid electrolytes that are air sensitive.
Keywords: garnet-type oxides; lithium ion battery; solid electrolyte; fluorination; surface treatment garnet-type oxides; lithium ion battery; solid electrolyte; fluorination; surface treatment

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MDPI and ACS Style

Herraiz, M.; Moumen, S.; Lemoine, K.; Jouffret, L.; Guérin, K.; Petit, E.; Gaillard, N.; Bertry, L.; Toth, R.; Le Mercier, T.; et al. Surface Fluorination for the Stabilization in Air of Garnet-Type Oxide Solid Electrolyte for Lithium Ion Battery. Batteries 2025, 11, 268. https://doi.org/10.3390/batteries11070268

AMA Style

Herraiz M, Moumen S, Lemoine K, Jouffret L, Guérin K, Petit E, Gaillard N, Bertry L, Toth R, Le Mercier T, et al. Surface Fluorination for the Stabilization in Air of Garnet-Type Oxide Solid Electrolyte for Lithium Ion Battery. Batteries. 2025; 11(7):268. https://doi.org/10.3390/batteries11070268

Chicago/Turabian Style

Herraiz, Michael, Saida Moumen, Kevin Lemoine, Laurent Jouffret, Katia Guérin, Elodie Petit, Nathalie Gaillard, Laure Bertry, Reka Toth, Thierry Le Mercier, and et al. 2025. "Surface Fluorination for the Stabilization in Air of Garnet-Type Oxide Solid Electrolyte for Lithium Ion Battery" Batteries 11, no. 7: 268. https://doi.org/10.3390/batteries11070268

APA Style

Herraiz, M., Moumen, S., Lemoine, K., Jouffret, L., Guérin, K., Petit, E., Gaillard, N., Bertry, L., Toth, R., Le Mercier, T., Buissette, V., & Dubois, M. (2025). Surface Fluorination for the Stabilization in Air of Garnet-Type Oxide Solid Electrolyte for Lithium Ion Battery. Batteries, 11(7), 268. https://doi.org/10.3390/batteries11070268

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