Oxides with spinel structures have been studied for many decades as they have been used in a variety of applications like pigments and refractories. They have also been used as a model structure to evaluate the relative stability of ions in octahedral and tetrahedral sites. Zinc-antimony spinels (Zn 7 Sb 2 O 12 ) were synthesized by the Pechini method and the cation Zn 2+ was substituted by Co
2+, taking into consideration the stoichiometry of Co x Zn 7-x Sb 2 O 12 (x = 0 -7). Characterization of the thermal properties of pyrolyzed powders was carried out with a TG/DTA analyzer, and mass losses were determined as a function of the cobalt content in the resin. The powders were calcined at temperatures in the range 600 to 1000 °C and characterized by XRD, BET and IR spectroscopy. Maximum cristalinity was obtained in powders calcined at 1000 °C. Materials with x = 5 -7 revealed the presence of a secondary phase (Co, Zn)Sb 2 O 6 . Infrared analysis facilitated in the determination of the possible sites of Zn 2+ , Co 2+ and Sb 2+ ions in the lattice.