High surface area nanocrystalline hausmannite synthesized by a solvent-free route

Nanocrystalline high surface area Mn3O4 powder was obtained at low temperature by a solvent-free route. The precursor was a mixture of manganese (II) acetate, 3,6,9-trioxadecanoic acid (TODA) and ammonium acetate that were intimately mixed by grounding in an agate mortar. Nanocrystalline Mn3O4 was obtained by thermal treatment at 120 °C. Powder X-ray diffraction, selected area electron diffraction, high resolution transmission electron microscopy, and Fourier transformed infrared characterization confirmed the formation of the hausmannite phase. The as-prepared mesoporous material has high specific surface area (120 m2 g−1). The performances of tape casted Mn3O4 nanopowder electrodes were investigated as anode material for lithium ion batteries. High capacity values were achieved at diverse C rates. Capacity fading was found to be dependent on the upper cut off voltage, the presence of a plateau at 2.25 V vs. Li+/Li being detrimental for long term cyclability.

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► High surface area Mn3O4 nanoparticles obtained by a solvent-free low temperature route.
► 3,6,9-Trioxadecanoic acid allows to obtain nanocrystalline hausmannite.
► Tape casted electrodes show up to 300 mAh g−1 capacity after more than 40 cycles at a C/3 rate.
► Upper cut off voltage strongly influences capacity retention upon cycling at high C rates.