Publication date: 10th April 2024
The oxyhalide materials, LiMOCl4 (M = Nb and Ta), have emerged as potential solid-state Li ion conductors for use in all-solid-state batteries (ASSBs). This is due to their high room temperature ionic conductivities and good oxidation stability [1]. Despite this, their structure-property relationships are poorly understood as the required mechnochemical synthesis route produces products with poor crystallinity. As a result, these materials have debated crystal structures [1,2]. In this study, we show that the crystallinity and ionic conductivity of LiNbOCl4 can be tuned by synthesising it off-stoichiometry from the nominal composition. In doing so, we provide insight into the crystal structure of LiNbOCl4 through a combination of X-ray, neutron, and PDF methods. Specifically, we demonstrate how controlling the lithium content in Li1−xNbO1−xCl4+x influences the crystallinity and ionic conductivity of the material. In addition, we show how these affects influence the cycling capability of ASSBs containing LiNbOCl4 solid electrolytes.
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