Noble metal (Ru, Pd, and Pt) catalyzed preparation of Ni₂P/α-Al₂O₃ was proved by XRD characterization. As is known from H₂-TPR experiments, Pd exhibits superior catalytic activity over Ru and Pt. These noble metal catalysts can be uniformly deposited on nickel phosphate precursors, and generate spillover hydrogen. Such a surface catalytic effect promotes the preparation of Ni₂P/α-Al₂O₃, without avoiding the formation of the minor phase Ni₁₂P₅. They can also be homogeneously dispersed in nickel phosphate precursors, and boost bulk diffusion of oxygen during reduction process, this is termed the “bulk catalytic effect”. It is feasible to produce pure phase Ni₂P by the latter preparation method using 0.05 wt% Pd or 0.1 wt% Ru at 768 K. The bulk catalytic effect may be considered as a meaningful option for developing catalytic materials.