In the proposed method, we could complete the synthesis with only 3 h of thermal treatment, which is relatively fast in comparison to the previously reported procedure, without an expensive gascontrolled chamber system. The compound comprises Re₂O₃ and NiO₃ powders that were mixed thoroughly in a stoichiometric ratio in a ball mill for 24 h and then dried in an oven at a 100 °C. The powder mixture was quickly calcined at various temperature for at least 3 h in an oxygen gas flow compared to conventional annealing method. After calcination at 1100 °C, the detected XRD peaks matched well with peaks of the standard ABO₃ perovskite structure. Moreover, EDX and FT-IR spectral analysis results confirmed that the mixture had formed stoichiometry ReNiO₃. All prepared samples comprised plate-like grains with a random orientation, and their average particle size was in the range of 1 to 3 μm calculated from FE-SEM images.