This article describes a novel hydrothermal deposition method for preparing highly dispersed NiW/gamma-Al2O3 catalysts and demonstrates its advantages over the conventional impregnation method. Via the hydrothermal precipitation reactions between sodium tungstate and hydrochloric acid and between nickel nitrate and urea, respectively, the active species W and Ni were deposited on gamma-Al2O3. In the hydrothermal deposition Of WO3, a surfactant hexadecyltrimethyl ammonium bromide (CTAB) was used to prevent the aggregation of WO3. The characterization results obtained by means of X-ray photoelectron spectroscopy (XPS), N-2 adsorption and high-resolution transmission electron microscopy (HRTEM) measurements showed that compared with the catalyst prepared by the conventional impregnation method, the catalyst with the same metal contents prepared by the hydrothermal deposition had much higher Wand Ni dispersion, higher specific surface area, larger pore volume, the significantly decreased slab length and slightly increased stacking degree of sulfided W species, leading to the significantly enhanced dibenzothiophene (DBT) hydrodesulfurization (HDS) activity. The DBT HDS assessment results also revealed that the catalyst containing 17.7 wt% WO3 and 2.4 wt% NiO prepared by the hydrothermal deposition method had the similar DBT HDS activity as a commercial NiW/gamma-Al2O3 catalyst containing 23 wt% WO3 and 2.6 wt% NiO, resulting in the greatly decreased amount of active metals for achieving the same HDS activity. (C) 2007 Elsevier B.V. All rights reserved.