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Cerium molybdate semiconductive nanoparticles were synthesized by the EDTA-citrate combined complexation method. Gel thermal degradation behavior, phase formation, morphology, composition and band gap of cerium molybdate powders were characterized by TG/DSC, XRD, SEM/EDS and DRS analysis, respectively. The nanoparticles were synthesized by fixing the pH of the reaction medium to 9, producing an organometallic gel which was heated to 230 ºC obtaining a precursor powder. The precursors were calcined in a temperature range of 450 -800 ºC for 3 h. The cerium molybdate powders were characterized and the phase evolution, morphology and band gap changes with the increase of calcining temperature were investigated. It was observed that the calcining temperature directly influences the formation of the crystalline structure, appearance of other phases in the materials and the particle size.