Publication date: 10th April 2024
Lithium thioborates have garnered significant attention as promising solid electrolyte (SE) materials for all-solid-state lithium batteries due to their high ionic conductivity, electrochemical stability, and unique structural features that facilitate efficient lithium-ion transport [1,2]. In this work, samples with the formula Li10B10S20-xIx (x = 0, 1, 2, 4) were prepared, where iodine substitution was employed to investigate its impact on the structural and dynamic properties of these materials. Solid-state nuclear magnetic resonance (NMR) spectroscopy was used as a powerful technique for probing the local structures, lithium-ion dynamics, and ionic conduction mechanisms in solid-state electrolytes [3,4]. Single-pulse 6Li magic-angle spinning (MAS) NMR experiments were conducted to observe changes in the lithium environments, as well as the appearance of any new lithium resonances, along the substitution series. Complementary single-pulse 11B MAS NMR experiments were used to probe the local boron environments and their evolution with increasing iodine content. This allowed the presence of B10S20 macro-tetrahedra structural motif along other boron environments to be confirmed, where multiple-quantum (MQ) 11B MAS NMR experiments were deployed to better enable the distinction between different boron sites and help elucidate the complex anionic framework of the lithium thioborates. Furthermore, static variable-temperature (VT) single-pulse and saturation-recovery 7Li NMR experiments were employed to study the lithium-ion dynamics in these materials. These experiments provide valuable information on lithium-ion mobility, activation energies for ion conduction, and the correlation between structural features and observed ionic conductivity properties. By combining these complementary solid-state NMR techniques, an understanding of the structure-property relationships in iodine-substituted lithium thioborates can be achieved.
J.K. is a member of the International Graduate School for Battery Chemistry, Characterization, Analysis, Recycling and Application (BACCARA), which is funded by the Ministry for Culture and Science of North Rhine-Westphalia, Germany.
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