An unsupported nickel phosphide catalyst with high surface area (130 m(2)/g) and high hydrotreating activity was prepared in the presence of a polymer surfactant (Triton X-114) and ethylene glycol. The resulting catalyst was characterized by XRD, SEM, TEM, CO and O-2 chemisorption, and P-31 MAS NMR spectroscopy. Both polymer surfactant and ethylene glycol are necessary to obtain good texture properties and hydrotreating activities of bulk nickel phosphide catalysts. (c) 2006 Elsevier Inc. All rights reserved.