Transition-metal spinels are efficient catalysts in a number of heterogeneous processes, such as CO oxidation, catalytic combustion of hydrocarbons and oxychlorination of methane. The properties of catalytic materials are highly dependent on the synthesis route. Spinels are often produced at high temperatures by the calcination of precursors such as powder mixtures, slurries or resins. Combustion synthesis is a cost-efficient method used to produce homogeneous and fine particles with high reproducibility. Cu0.8Ni0.2Cr2O4 spinel was obtained by the combustion of metallic nitrates using urea as fuel. The resulting powders were calcinated at different temperatures and characterized by thermogravimetric and particle size analyses, X ray diffraction, and scanning electron microscopy. The effect of urea on the control of the process and particle morphology was investigated. The results revealed the formation of porous powders with increasing crystallinity as the calcination temperature increased. Crystallization of spinel started at 700 degrees C.