University of Oulu

Palanivel Molaiyan, Sarah E. Mailhiot, Kevin Voges, Anu M. Kantola, Tao Hu, Peter Michalowski, Arno Kwade, Ville-Veikko Telkki, Ulla Lassi, Investigation of the structure and ionic conductivity of a Li3InCl6 modified by dry room annealing for solid-state Li-ion battery applications, Materials & Design, Volume 227, 2023, 111690, ISSN 0264-1275,

Investigation of the structure and ionic conductivity of a Li₃InCl₆ modified by dry room annealing for solid-state Li-ion battery applications

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Author: Molaiyan, Palanivel1; Mailhiot, Sarah E.2; Voges, Kevin3,4;
Organizations: 1Research Unit of Sustainable Chemistry, University of Oulu, 90570 Oulu, Finland
2NMR Research Unit, University of Oulu, 90570 Oulu, Finland
3Institute for Particle Technology, Technische Universität Braunschweig, Volkmaroder Str, 5, 38104 Braunschweig, Germany
4Battery LabFactory Braunschweig (BLB), Technische Universität Braunschweig, Langer Kamp, 19, 38106 Braunschweig, Germany
Format: article
Version: published version
Access: open
Online Access: PDF Full Text (PDF, 2.3 MB)
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Language: English
Published: Elsevier, 2023
Publish Date: 2023-09-25


Progress in new sustainable technologies depends on the development of battery materials, specifically on safer, low-cost, and higher energy density batteries. One new type of materials are the halide solid electrolytes (HSEs), which have been shown to exhibit high ionic conductivity, deformability, and oxidative stability. Here, the synthesis of Li₃InCl₆ (LIC) HSEs by ball-milling followed by dry room annealing is investigated. Crystal structure, particle size, and ionic conductivity are analyzed using a combination of X-ray diffraction, transmission electron microscopy, and electrochemical impedance spectroscopy. Dry room annealing increases the presence of impurities in the sample but also increases the Li⁺ ionic conductivity up to 1.03 mS cm⁻¹. Additional pulsed-field gradient and relaxation time NMR measurements were performed to understand the lithium diffusion in the LIC samples. Two-dimensional diffusion — T₂ relaxation correlation and T₂ relaxation exchange measurements showed that there are multiple unique Li atomic motion sites, which are correlated to different rates of diffusive, micrometer-scale motion. This work outlines a simple solid-state synthesis approach and a novel strategy for designing advanced materials, understanding the ionic conduction, as well as the challenges in scalable wet processing of halide-based cathode sheets for solid-state battery applications.

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Series: Materials & design
ISSN: 0264-1275
ISSN-E: 1873-4197
ISSN-L: 0264-1275
Volume: 227
Article number: 111690
DOI: 10.1016/j.matdes.2023.111690
Type of Publication: A1 Journal article – refereed
Field of Science: 116 Chemical sciences
Funding: This work was supported and funded by EU/EURF (PASS, A76178) and EU/Interreg Nord (SolBat, grant no. 20202885) projects. The research work was also supported by the German Federal Ministry of Education and Research (BMBF) within the project FestBatt under grant number 03XP0177C and the project EProFest under grant number 03XP0346C. Sarah Mailhiot gratefully acknowledges Academy of Finland (321701) and Marie Sklodowska-Curie Actions (896824). Ville-Veikko Telkki gratefully acknowledges financial support from the European Research Council (Project number 772110) and Academy of Finland (grant no. 340099).
EU Grant Number: (896824) NMRCement - Zero-CO2 cement concept evaluated with novel Nuclear Magnetic Resonance (NMR)
(772110) UFLNMR - Ultrafast Laplace NMR
Academy of Finland Grant Number: 321701
Detailed Information: 321701 (Academy of Finland Funding decision)
340099 (Academy of Finland Funding decision)
Copyright information: © 2023 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY license (