Abstract: A series of NiV/Al2O3 catalysts with different Ni/(Ni+V) atomic ratios were prepared by pore saturation impregnation method. The catalysts were characterized by Raman spectrometry and H2-TPR technique. The hydrodemetallization (HDM) and hydrodesulfurization (HDS) activities of the prepared NiV/Al2O3 catalysts after sulfidation were assessed using Kuwait atmospheric residue as feed. Results showed that the existence of nickel could promote the agglomeration of vanadium and reduce the interaction between vanadium and alumina support. It can be concluded that a positive synergetic effect of nickel and vanadium existed in catalyst having Ni/(Ni+V) atomic ratio of 0.25, its HDM activity was much higher than those of the other NiV/Al2O3 catalysts, and its HDS activity was also slightly higher.