Amorphous versus Crystalline Li3PS4: Local Structural Changes during Synthesis and Li Ion Mobility

材料科学 结晶 无定形固体 离子电导率 分析化学(期刊) 魔角纺纱 快离子导体 玻璃化转变 核磁共振波谱 结晶学 化学工程 核磁共振 物理化学 化学 电解质 聚合物 复合材料 工程类 物理 色谱法 电极
作者
Heike Stöffler,Tatiana Zinkevich,Murat Yavuz,Anna‐Lena Hansen,Michael Knapp,Jozef Bednarčík,Simon Randau,Felix H. Richter,Jürgen Janek,Helmut Ehrenberg,Sylvio Indris
出处
期刊:Journal of Physical Chemistry C [American Chemical Society]
卷期号:123 (16): 10280-10290 被引量:80
标识
DOI:10.1021/acs.jpcc.9b01425
摘要

Glass–ceramic solid electrolytes have been reported to exhibit high ionic conductivities. Their synthesis can be performed by crystallization of mechanically milled Li2S–P2S5 glasses. Herein, the amorphization process of Li2S–P2S5 (75:25) induced by ball milling was analyzed via X-ray diffraction (XRD), Raman spectroscopy, and 31P magic-angle spinning nuclear magnetic resonance (NMR) spectroscopy. Several structural building blocks such as [P4S10], [P2S6]4–, [P2S7]4–, and [PS4]3– occur during this amorphization process. In addition, high-temperature XRD was used to study the crystallization process of the mechanically milled Li2S–P2S5 glass. Crystallization of phase-pure β-Li3PS4 was observed at temperatures up to 548 K. The kinetics of crystallization was analyzed by integration of the intensity of the Bragg reflections. 7Li NMR relaxometry and pulsed field-gradient (PFG) NMR were used to investigate the short-range and long-range Li+ dynamics in these amorphous and crystalline materials. From the diffusion coefficients obtained by PFG NMR, similar Li+ conductivities for the glassy and heat-treated samples were calculated. For the glassy sample and the glass–ceramic β-Li3PS4 (calcination at 523 K for 1 h), a Li+ bulk conductivity σLi of 1.6 × 10–4 S/cm (298 K) was obtained, showing that for this system a well-crystalline material is not essential to achieve fast Li-ion dynamics. Impedance measurements reveal a higher overall conductivity for the amorphous sample, suggesting that the influence of grain boundaries is small in this case.
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