<i>In situ</i> observation of the deterioration process of sulfide-based solid electrolytes using airtight and air-flow TEM systems

  • Hirofumi Tsukasaki
    Department of Material Science, Graduate School of Engineering, Osaka Prefecture University, Sakai, Osaka 599-8531, Japan
  • Keisuke Igarashi
    Hitachi High-Tech Corporation, 1040, Ichige, Hitachinaka-shi, Ibaraki 312-0033, Japan
  • Akiko Wakui
    Hitachi High-Tech Corporation, 1040, Ichige, Hitachinaka-shi, Ibaraki 312-0033, Japan
  • Toshie Yaguchi
    Hitachi High-Tech Corporation, 1040, Ichige, Hitachinaka-shi, Ibaraki 312-0033, Japan
  • Hiroshi Nakajima
    Department of Material Science, Graduate School of Engineering, Osaka Prefecture University, Sakai, Osaka 599-8531, Japan
  • Takuya Kimura
    Department of Applied Chemistry, Graduate School of Engineering, Osaka Prefecture University, Sakai, Osaka 599-8531, Japan
  • Atsushi Sakuda
    Department of Applied Chemistry, Graduate School of Engineering, Osaka Prefecture University, Sakai, Osaka 599-8531, Japan
  • Masahiro Tatsumisago
    Department of Applied Chemistry, Graduate School of Engineering, Osaka Prefecture University, Sakai, Osaka 599-8531, Japan
  • Akitoshi Hayashi
    Department of Applied Chemistry, Graduate School of Engineering, Osaka Prefecture University, Sakai, Osaka 599-8531, Japan
  • Shigeo Mori
    Department of Material Science, Graduate School of Engineering, Osaka Prefecture University, Sakai, Osaka 599-8531, Japan

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<jats:title>Abstract</jats:title> <jats:p>Sulfide-based solid electrolytes (SEs) exhibiting high ionic conductivity are indispensable battery materials for next-generation all-solid-state batteries. However, sulfide-based SEs have a major drawback in their low chemical stability in air. When exposed to H2O or O2 gas, toxic H2S is generated, and their ionic conductivity considerably declines. However, their degradation mechanism caused by air exposure has not been understood yet. To clarify the degradation process, in this study, we developed a transmission electron microscope (TEM) system to evaluate the air stability of battery materials. Using a vacuum transfer double-tilt TEM holder with a gas-flow system, the in situ observation of the degradation process was conducted for a sulfide-based Li4SnS4 glass ceramic under an air-flow environment. Consequently, electron diffraction (ED) patterns and TEM images could clearly capture morphological changes and the amorphization process caused by air exposure. Moreover, based on the analysis of ED patterns, it is observed that Li4SnS4 is likely to decompose because of the reaction with H2O in air. Therefore, this airtight and air-flow TEM system should be effective in clarifying the process of the deterioration of sulfur-based SEs during exposure to air.</jats:p>

収録刊行物

  • Microscopy

    Microscopy 70 (6), 519-525, 2021-06-22

    Oxford University Press (OUP)

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