A powder of nominal composition (ZrO2)(0.886)(Sc2O3)(0.104)(Al2O3)(0.01) was synthesized by spray drying with the purpose of testing the performance of solid oxide fuel cells containing scandia-stabilized zirconia (ScSZ) as electrolyte. The phases resulting from calcination and sintering at different temperatures were investigated by XRD, impedance and Raman spectroscopy. At sintering temperatures of 1200-1400 degrees C nearly equal amounts of cubic and rhombohedral ScSZ were detected, whereas heat treatment higher than 1500 degrees C led to a cubic single-phase material. A preliminary reaction mechanism of phase formation is proposed with respect to the various results depending on heat treatment.