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Convenient synthesis of nanocrystalline powders of phase-pure manganese nitride η-Mn3N2

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Abstract

Manganese bis(trimethylsilyl)amide Mn[N(Si(CH3)3)2]2 was used as a convenient material precursor to prepare pure manganese nitride nanopowders with reaction-controlled average crystallite sizes. The precursor was first reacted with liquid ammonia under reflux conditions and the resulting by-product was pyrolyzed under an ammonia flow at temperatures in the range 150–900 °C. The powder products were characterized mainly by powder X-ray diffraction (XRD) diffraction, SEM/EDX examinations, and FT-IR and micro-Raman spectroscopies. In all cases, a pure phase of nanocrystalline η-Mn3N2 was detected by XRD as the exclusive manganese nitride product. The compound’s nanopowders were extremely reactive toward air. Upon oxidation, they formed either MnO for a relatively better crystallized nitride from higher synthesis temperatures or Mn3O4 after self-ignition of a poorly crystalline nitride from a lower synthesis temperature.

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Acknowledgements

The study was supported by Polish NCN Grant 2011/01/B/ST5/06592.

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Authors and Affiliations

  1. Faculty of Energy and Fuels, AGH University of Science and Technology, al. Mickiewicza 30, 30-059, Krakow, Poland

    Mariusz Drygaś, Michał Musiał & Jerzy F. Janik

  2. Faculty of Materials Science and Ceramics, AGH University of Science and Technology, al. Mickiewicza 30, 30-059, Krakow, Poland

    Mirosław M. Bućko

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  1. Mariusz Drygaś
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  2. Mirosław M. Bućko
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  4. Jerzy F. Janik
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Correspondence to Mariusz Drygaś.

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Drygaś, M., Bućko, M.M., Musiał, M. et al. Convenient synthesis of nanocrystalline powders of phase-pure manganese nitride η-Mn3N2 . J Mater Sci 51, 8177–8186 (2016). https://doi.org/10.1007/s10853-016-0094-2

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