Ni-Based materials are one of the most promising candidates for hydrogen oxidation reaction (HOR) in anion exchange membrane fuel cells (AEMFC). However, the performance for pure Ni is limited. In this work, Ni mixed CeO₂ nanoparticles supported on carbon black were synthesized for the first time by Reactive Spray Deposition Technology (RSDT) and followed by an oxygen reduction process in a furnace. By controlling the reaction parameters during the RSDT fabrication process, the particle size of Ni/CeO₂/C is set at 3 nm. The resultant 3 nm catalyst Ni/CeO₂/C catalyst exhibits excellent mass activity (14.92 mA mg^-1_Ni) compared to the catalyst without the addition of CeO₂ (which is Ni/C 4.39mA mg^-1_Ni) as well as the activity of most of the other non-precious metal-based materials for HOR. The excellent electrocatalytic performance indicates that Ni/CeO₂/C can be considered as a potential non-precious metal at the anodes for AMEFCs.