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Microwave-assisted hydrothermal synthesis and electrochemical studies of α- and h-MoO3

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Abstract

Two modifications of molybdenum trioxide with orthorhombic (α-MoO3) and hexagonal (h-MoO3) crystal structure have been synthesized by a microwave-assisted hydrothermal method, facilitated by formic acid. Characterization by means of X-ray diffraction, scanning electron microscopy, specific surface analysis, and Fourier-transform infrared, Raman, and UV-Vis spectroscopy reveals phase-pure crystalline powder samples of hexagonal h-MoO3 microrods and of α-MoO3 nanobelt bundles, respectively. The electrochemical properties of the MoO3 compounds, studied by cyclic voltammetry and galvanostatic cycling vs. Li/Li+, strongly depend on the structure and the applied potential range. In the range of 1.5–3.5 V, Li+-ions can be reversibly intercalated into the α-MoO3 nanobelts. Utilizing the material in this way as intercalation cathode material yields an initial discharge capacity of 295 mA h g−1 at 100 mA g−1 and comparably moderate capacity fading of 25% between cycles 20 and 100. Extending the potential range to 0.01–3.0 V induces the conversion reaction to Mo, which for both modifications yields high initial capacities of around 1500 mA h g−1 but is associated with much stronger capacity fading.

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Acknowledgements

GZ acknowledges support by the UD RAS project No. 18-10-3-32. GZ acknowledges financial support by the Excellence Initiative of the German Federal Government and States. AO and RK are grateful to the CleanTech-Initiative of the Baden-Württemberg-Stiftung (Project CT-3 Nanostorage). Support by the Deutsche Forschungsgemeinschaft via project KL1824/12-1 is acknowledged.

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Authors and Affiliations

  1. Kirchhoff Institute of Physics, Heidelberg University, INF 227, 69120, Heidelberg, Germany

    Galina S. Zakharova, Christina Schmidt, Alexander Ottmann & Rüdiger Klingeler

  2. Institute of Solid State Chemistry, Ural Division, Russian Academy of Sciences, Yekaterinburg, Russia, 620990

    Galina S. Zakharova

  3. Institute of Chemical and Environmental Engineering, West Pomeranian University of Technology, al. Piastów 45, 70-322, Szczecin, Poland

    Ewa Mijowska

  4. Centre for Advanced Materials (CAM), Heidelberg University, INF 225, 69120, Heidelberg, Germany

    Rüdiger Klingeler

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  1. Galina S. Zakharova
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  2. Christina Schmidt
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Correspondence to Alexander Ottmann.

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Zakharova, G.S., Schmidt, C., Ottmann, A. et al. Microwave-assisted hydrothermal synthesis and electrochemical studies of α- and h-MoO3. J Solid State Electrochem 22, 3651–3661 (2018). https://doi.org/10.1007/s10008-018-4073-1

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  • DOI: https://doi.org/10.1007/s10008-018-4073-1

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