A novel and facile route to bimetallic molybdenum phosphides was described. Both NiMoP and CoMoP phosphides were successfully prepared by a hexamethylenetetramine (HMT) route. Mixed-salt precursors containing HMT, M-HMT (M = Ni, Co or Mo) complexes, MMo-HMT (M = Ni or Co) complexes and P-containing species can be directly converted to bimetallic molybdenum phosphides under a flow of Ar at 800 degrees C. It was proposed that the bimetallic phosphides were formed via two possible reaction pathways: (i) MMo-HMT complexes/P -> MMoP (M = Ni or Co) and (ii) M-HMT (M = Ni, Co or Mo) complexes/P -> M2P/MoP -> MMoP (M = Ni or Co). Additionally, it was found that the dispersions and surface areas of NiMoP and CoMoP prepared by HMT route were higher than those of corresponding bimetallic phosphides prepared by traditional H-2 reduction method.