A new method for the preparation of bimetal phosphides was reported. Bulk and SiO(2)-supported porous NiCoP were obtained from the direct thermal treatment of precursors containing nickel, cobalt salts, and sodium hypophosphite mixed mechanically under flowing nitrogen. Compared with traditional H(2)-temperature-programmed reduction method, the method developed provided a simple one-step way to produce bimetal phosphides with a relatively low temperature. In the report, a possible preparation mechanism was discussed to form NiCoP. The route and mechanism could also be applied to the preparation of other bimetal phosphides. In comparison with the Ni(2)P/SiO(2) catalyst, the NiCoP/SiO(2) showed a higher hydrodesulfurization activity for dibenzothiophene. Crown Copyright 0 2011 Published by Elsevier B.V. All rights reserved.