Nano-crystalline NiO-YSZ composite powders have been successfully prepared by microwave-assisted combustion of a gel derived from an aqueous solution containing ZrO(NO3)(2) center dot 6H(2)O, Y(NO3)(3) center dot 6H(2)O, Ni (NO3)(2) center dot 6H(2)O and glycine. The as-prepared powders were examined using X-ray diffraction (XRD), scanning electron microscope (SEM) and transmission electron microscope (TEM) techniques. It was found that the process took only a few seconds to obtain NiO-YSZ composite powders. The as synthesized composite powder was a homogeneous mixture of YSZ, NiO and Ni phases with crystallite size of 24.2, 33.6 and 25.3 nm respectively. (c) 2008 Elsevier B.V. All rights reserved.