The efficient synthesis of polycrystalline filled beta-Mn structured Ni2Mo3N, and the etacarbides Fe3Mo3N and Co3Mo3N, by a single heating of metal powders at 975 ºC under a hydrogen-nitrogen mixture is reported. Rietveld analysis of high-resolution X-ray powder diffraction data shows that the reduction-nitridation of NiMoO4 produces Ni2Mo3N and nickel; Ni3Mo3N is not obtained in this way and its existence is disproved.
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