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In this study, a facile method for the synthesis of bulk and alumina-supported Ni2Mo3N is described. The synthesis is based on the heat treatment of a mixed-salt precursor in a H2 flow at 873 K. The mixed-salt precursor is obtained by evaporating ammonia solution of Ni(CH3COO)2 and (NH4)6Mo7O24 with a fixed Ni/Mo molar ratio of 2 : 3. The formation process of the bimetallic molybdenum nitride has been investigated, which indicates that the labile NH4+ contained in the inorganic salt precursor is utilized as N source to form Ni2Mo3N in the H2 flow when elemental nickel is present. The high NH3 flow rate required in the conventional temperature-programmed nitridation method is not necessary in this hydrogen thermal treatment method. Alumina-supported Ni2Mo3N has also been successfully prepared by this method. The resultant catalyst has better dispersion of Ni2Mo3N and exhibits higher catalytic activity compared to the catalyst prepared by the conventional method. [ABSTRACT FROM AUTHOR]