We evaluated the optimal conditions for fluidization of nickel oxide (NiO) and its reduction into highpurity Ni during hydrogen reduction in a laboratory-scale fluidized bed reactor. A comparative study was performed through structural shape analysis using scanning electron microscopy (SEM); variance in pressure drop, minimum fluidization velocity, terminal velocity, reduction rate, and mass loss were assessed at temperatures ranging from 400 to 600 °C and at 20, 40, and 60 min in reaction time. We estimated the sample weight with most active fluidization to be 200 g based on the bed diameter of the fluidized bed reactor and height of the stocked material. The optimal conditions for NiO hydrogen reduction were found to be height of sample H to the internal fluidized bed reactor diameter D was H/D=1, reaction temperature of 550 °C, reaction time of 60 min, superficial gas velocity of 0.011 m/s, and pressure drop of 77 Pa during fluidization. We determined the best operating conditions for the NiO hydrogen reduction process based on these findings.