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Investigation of the lithium-rich boundary of the Li1+x Mn2−x O4 cubic spinel phase in air

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Abstract

Several compositions of the cubic spinel Li1+x Mn2−x O4−δ phase in the lithium–manganese–oxygen (Li–Mn–O) system were synthesized at 700, 750, and 800 °C in air (\( p_{{{\text{O}}_{2} }} \) = 0.2 atm) to investigate the Li-rich boundary of the cubic spinel phase at these temperatures. The lattice parameters of the several compositions were determined by Rietveld analysis of the measured X-ray patterns, and the Li and Mn contents of the samples were measured using inductively coupled plasma with optical emission spectroscopy (ICP-OES). A Vegard-like dependence of the measured lattice parameter of the cubic spinel phase with Li to Mn ratio exists in the homogeneity range of the cubic spinel. This dependence could be used to derive the boundary of the single phase cubic spinel field in the Li–Mn–O system at 700 and 750 °C at \( p_{{{\text{O}}_{2} }} \) = 0.2 atm and to estimate the Li-rich boundary at 800 °C. The results of the present study are compared with two other experimental studies on the homogeneity range of the cubic spinel phase in an attempt to resolve the contradiction between these two studies.

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Acknowledgements

The authors would like to thank the German Research Foundation (DFG) Priority Program 1473 WenDeLib—Materials with New design for Improved Lithium Ion Batteries for the financial support.

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  1. Toni Lehmann

    Present address: Fraunhofer Technology Center for Semiconductor Materials, Am St. Niclas Schacht 13, 09599, Freiberg, Germany

Authors and Affiliations

  1. Karlsruhe Institute of Technology, Institute for Applied Materials—Applied Materials Physics (IAM-AWP), Hermann-von-Helmholtz-Platz 1, 76344, Eggenstein-Leopoldshafen, Germany

    Damian M. Cupid, Thomas Bergfeldt, Harald Berndt & Hans J. Seifert

  2. Technische Universität Bergakademie Freiberg, Institute of Materials Science, Gustav-Zeuner-Strasse 5, 09599, Freiberg, Germany

    Toni Lehmann

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  1. Damian M. Cupid
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Correspondence to Damian M. Cupid.

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Cupid, D.M., Lehmann, T., Bergfeldt, T. et al. Investigation of the lithium-rich boundary of the Li1+x Mn2−x O4 cubic spinel phase in air. J Mater Sci 48, 3395–3403 (2013). https://doi.org/10.1007/s10853-012-7126-3

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  • DOI: https://doi.org/10.1007/s10853-012-7126-3

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