Structural Evolution and Li Dynamics in Nanophase Li3PS4 by Solid-State and Pulsed-Field Gradient NMR

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• 作者：Mallory Gobet ; Steve Greenbaum ; Gayatri Sahu ; Chengdu Liang
• 刊名：Chemistry of Materials
• 出版年：2014
• 出版时间：June 10, 2014
• 年：2014
• 卷：26
• 期：11
• 页码：3558-3564
• 全文大小：287K
• 年卷期：v.26,no.11(June 10, 2014)
• ISSN：1520-5002

文摘

The ceramic lithium ion conductor 尾-Li₃PS₄ has a disordered and nanoporous structure that leads to an enhancement in ionic conductivity by some 3 orders of magnitude compared to the crystalline 纬 phase. The 尾 phase is prepared by thermal treatment of an inorganic鈥搊rganic complex based on Li₃PS₄ and THF. Multinuclear (¹H, ^6,7Li, ³¹P) solid-state NMR spectroscopy is used to characterize the structural phase evolution of the starting material at various steps in the thermal treatment. The 尾 phase formed after high temperature treatment is recognized as spectroscopically distinct from the bulk 纬-Li₃PS₄ compound. Also formed is an amorphous lithium thiophosphate phase that is metastable as verified by annealing over an extended period. Lithium ion self-diffusion coefficients are measurable by standard pulsed-field gradient NMR methods at 100 掳C and with values consistent with the high ionic conductivity previously reported for this material.