Solvent-assisted ball milling for synthesizing solid electrolyte Li7P3S11

Solvent-assisted ball milling for synthesizing solid electrolyte Li7P3S11
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溶剂辅助球磨合成固体电解质Li7P3S11

DOI:
10.1111/jace.16249
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发表时间:
2019-06-01
影响因子:
3.9
通讯作者:
Ma, Hongli
Ma, Hongli
中科院分区:
材料科学2区
文献类型:
--
作者:
Xue, Bai;Fan, Bo;Ma, Hongli

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采用溶剂辅助球磨法制备硫化物固体电解质Li7P3S11。与干法球磨和简单的液相合成相比,溶剂辅助球磨可以显着促进起始原料的反应从数十小时缩短至仅几个小时。以二甲氧基乙烷为辅助溶剂时,球磨8小时,180℃真空干燥2小时,230℃热处理4小时,可合成较纯的Li7P3S11,离子电导率为1.0×10(-4)S/cm。结果表明,从前体到 Li7P3S11 的转变是一个两步过程,中间体由硫代-LISICON III 类似相和非晶相组成。这项工作不仅提供了一种缩短合成时间的Li7P3S11的合成路线,而且还为硫化物固体电解质的溶剂基合成过程中的相演化提供了指导性的见解。
Solvent-assisted ball milling is used to prepare the sulfide solid electrolyte Li7P3S11. Comparing with dry ball milling and simple liquid phase synthesis, solvent-assisted ball milling can significantly promote the reaction of the starting materials from tens of hours to only several hours. When using dimethoxyethane as the assistant solvent, relatively pure Li7P3S11 with ionic conductivity of 1.0 x 10(-4) S/cm can be synthesized after 8-hour ball milling with following 2-hour 180 degrees C vacuum drying and 4-hour 230 degrees C heat treatment. It is revealed that the transition from the precursor to Li7P3S11 is a two-step process, with an intermediate composed of a thio-LISICON III analogous phase and an amorphous phase. This work not only provides a synthesis route of Li7P3S11 which reduces synthesis duration, but also offers an instructive insight into the phase evolution in solvent-based synthesis process of sulfide solid electrolytes.