NiO/YSZ powders prepared by the citrate route were characterized in order to check the effectiveness of this method for the preparation of materials suitable for solid oxide fuel cell application. Powders were obtained in the form of agglomerates of small YSZ and NiO particles (dimensions < 0.1 mum). Both stoichiometry of YSZ and NiO content derived by quantitative XRD analysis are consistent with the results of chemical analysis.