Ni/YSZ cermets has been prepared by the combustion of Y(NO3)(3), Zr(NO3)(4), Ni(NO3)(2) and organic fuel, followed by hydrogen reduction at 800 degrees C. The influence of the oxidant/fuel mixture ratio of the precursors on the end reaction product characteristics was investigated. It is showed that the powders prepared by the combustion crystallize fully when oxidant/fuel is 2/3. SEM and TEM investigated the powders and Ni/YSZ cermets. It is showed that the powders were fine and homogenous, agglomerated particle size was about 0.5 mu m similar to 1 mu m. Ni/YSZ anode specimens prepared using the powders by pressing method were not only more Ni homogeneously distributed in YSZ matrix than those of samples prepared using powders synthesized by the traditional mechanical mixing method but also both Ni and YSZ phase form continuous network structure, respectively.