The synthesis of micro-sized, uniformly distributed Al₂O₃-15Vol% Ni powders were studied through three step co-precipitation of hydroxides mixtures from proper solution, calcination at air atmosphere and final step of calcined powders in a carbon bed. Al and Ni hydroxide and amorphous phase were first obtained from their salt’s solutions through chemical co-precipitation method by adjusting pH. The precipitated powders were then calcined to obtain a mixture of their oxides as NiO and NiAl₂O₄ which were reduced in a carbon bed at various temperatures up to 1300. Proper temperature for calcination in air was determined through TG analysis; 900. SEM observation of powders after reduction, revealed micro-sized Ni particles, along with fin distribution of Ni and Al₂O₃ elements. XRD analysis of the calcined sample showed the presence of NiAl₂O₄ and NiO and the same analysis for the reduced sample confirmed the formation of Al₂O₃ and Ni.