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

  • Heike Stöffler*
    Heike Stöffler
    Institute for Applied Materials − Energy Storage Systems (IAM-ESS), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany
    *E-mail: [email protected]. Tel.: +49-721-680-28502.
    More by Heike Stöffler
    Orcidhttp://orcid.org/0000-0002-7987-8646
  • , 
  • Tatiana Zinkevich
    Tatiana Zinkevich
    Institute for Applied Materials − Energy Storage Systems (IAM-ESS), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany
    Helmholtz Institute Ulm, Helmholtzstraße 11, 89081 Ulm, Germany
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  • , 
  • Murat Yavuz
    Murat Yavuz
    Institute for Applied Materials − Energy Storage Systems (IAM-ESS), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany
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  • , 
  • Anna-Lena Hansen
    Anna-Lena Hansen
    Institute for Applied Materials − Energy Storage Systems (IAM-ESS), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany
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  • , 
  • Michael Knapp
    Michael Knapp
    Institute for Applied Materials − Energy Storage Systems (IAM-ESS), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany
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  • , 
  • Jozef Bednarčík
    Jozef Bednarčík
    Deutsches Elektronen Synchrotron DESY, Notkestrasse 85, 22607 Hamburg, Germany
    Department of Condensed Matter Physics, Institute of Physics, P. J. Safarik University, Park Angelinum 9, 041 54 Kosice, Slovakia
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  • , 
  • Simon Randau
    Simon Randau
    Institute of Physical Chemistry, Justus-Liebig-University Giessen, Heinrich-Buff-Ring 17, 35392 Giessen, Germany
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  • , 
  • Felix H. Richter
    Felix H. Richter
    Institute of Physical Chemistry, Justus-Liebig-University Giessen, Heinrich-Buff-Ring 17, 35392 Giessen, Germany
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  • , 
  • Jürgen Janek
    Jürgen Janek
    Institute of Physical Chemistry, Justus-Liebig-University Giessen, Heinrich-Buff-Ring 17, 35392 Giessen, Germany
    BELLA-Batteries and Electrochemistry Laboratory, Institute of Nanotechnology, Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany
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  • , 
  • Helmut Ehrenberg
    Helmut Ehrenberg
    Institute for Applied Materials − Energy Storage Systems (IAM-ESS), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany
    Helmholtz Institute Ulm, Helmholtzstraße 11, 89081 Ulm, Germany
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  • , and 
  • Sylvio Indris
    Sylvio Indris
    Institute for Applied Materials − Energy Storage Systems (IAM-ESS), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany
    Helmholtz Institute Ulm, Helmholtzstraße 11, 89081 Ulm, Germany
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    Orcidhttp://orcid.org/0000-0002-5100-113X
Cite this: J. Phys. Chem. C 2019, 123, 16, 10280–10290
Publication Date (Web):April 1, 2019
https://doi.org/10.1021/acs.jpcc.9b01425
Copyright © 2019 American Chemical Society
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    Abstract

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    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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    The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acs.jpcc.9b01425.

    • X-ray diffraction pattern (Mo Kα1) of P4S10 with Rietveld refinement, Raman spectra of initial compounds and empty capillary, in situ HT-XRD patterns (Mo Kα1) of the amorphous sample. The patterns were recorded at temperatures from 298 to 773 K (in red for increasing temperature) and at 298 K (in blue after cooling), in situ HT-XRD patterns (Mo Kα1) of the Li2S–P2S5 glass heated at 413 and 433 K, Nyquist plot of electrochemical impedance for the (a) amorphous and (b) calcined samples at selected temperatures, nitrogen physisorption isotherm of (a) amorphous and (b) calcined samples (PDF)

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