A new carbonitride Ni2Mo3(CxNy) has been synthesized by temperature-programmed carburization of the Ni2Mo3N precursor with a CH4/H2/Ar gas mixture at 923 K. This compound has been characterized by X-ray diffraction, elemental analysis, Auger electron spectroscopy, laser Raman spectroscopy, thermogravimetric analysis and field-emission scanning electron microscopy. Ni2Mo3(CxNy) crystallizes in the cubic space groupP4132, with a lattice parameter of a = 6.64575(3) Å, corresponding to the unusual filled β-Mn structure. Its formation occurs by partial substitution of N by Cvia a topotactic and pseudomorphic reaction and its stability in air is higher that of Ni2Mo3N. A two-phase mixture with a cubic structure has always been obtained by the same synthetic method applied to the V2Mo(OxNy) precursor. One of these would be of carbidic nature formed at 1153 K following a reaction similar to that proposed for Ni2Mo3(CxNy).
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