Nickel oxide – 8 mol% yttria stabilized zirconia (NiO-8YSZ) powders containing 25 to 75 wt% of NiO were prepared by coprecipitation. The entire process includes the reaction of metals aqueous chloride solutions (heated at 95 oC) with ammonium hydroxide, washing steps of the resulting gel, butanol azeotropic distillation treatment to prevent the formation of hard agglomerates, drying, calcination and ball milling. The yield of precipitation of metals was determined by inductively coupled plasma atomic emission spectroscopy analysis (ICP-AES). Powders were characterized by X-ray and laser diffraction, infrared analysis, gas adsorption (BET) and scanning electron microscopy. It was observed that zirconium and yttrium hydroxides are easily precipitated in alkaline medium, while nickel precipitation yield is in the range of 80 to 95% due to the formation of soluble complexes. NiO appears as a second phase in synthesized powders and contributes to decreasing of specific surface area and agglomerate mean size.