Nanocrystalline composite powders, NiO-YSZ were prepared by the succinic acid-containing gel-combustion method at a temperature as low as 310 degrees C. FT-IR, XRD, DTA/TGA, SEM and TEM were employed to characterize the thermal decomposition of the precursor and the phase evolution and morphology of the calcined powders. The results of FT-IR and thermal analysis showed that the pyrolysis of the precursor began at 171 degrees C followed by the decomposition of carbonate-containing residues at 245 degrees C and finally the removal of all pyrolyzed species was completed at 302 degrees C, accompanied by the crystallization of the metallic nickel, NiO and cubic YSZ phases. The examination of TEM also showed that the nanocrystallites were closely bonded and homogeneously distributed at the nanometric scale. (c) 2006 Elsevier B.V All rights reserved.