Abstract: The amorphous Ni-Mo-B catalysts were prepared by ultrasonic as well as regular chemical reduction and characterized by BET, SEM, XRD, XPS, and FT-IR. Their catalytic activity in the hydrodeoxygenation of phenol was evaluated. The influences of the catalyst preparation conditions and the reaction temperature on the phenol hydrodeoxygenation were investigated, and a reaction mechanism was proposed. The results showed that the particle size, agglomeration phenomenon, surface area, and MoO₂ and B content of the Ni-Mo-B catalysts can be regulated by introducing the ultrasonic treatment into the chemical reduction, which is effective to enhance their catalytic activity in phenol hydrodeoxygenation. At 498 K, the conversion of phenol is 81.08% and the hydrodeoxygenation selectivity reaches 93.39%.