In this study, Ni2Mo3N cube-like particles have been synthesized by a solid-state reaction of metallic molybdenum, nickel chloride hexahydrate, and sodium azide in a sealed autoclave at 750 degrees C. The structures and morphologies of the obtained product are derived from X-ray diffraction, field-emission scanning electron microscopy, and transmission electron microscopy. Furthermore, the thermal stability and oxidation resistance of the obtained product are investigated.