Abstract Pechini method was applied for the first time to synthesize CeNb3O9 perovskite at different calcination temperatures (600, 800 and 1000 °C). A solution of water, citric acid, ethylene glycol, ammonium niobium oxalate and cerium ions was polymerized and calcined at 300 °C for 2 h. The precursor gels were submitted to a second calcination at 600, 800 and 1000 °C to obtain perovskite at different temperatures. These materials were characterized through X-ray diffraction (XRD), thermogravimetric analysis (TGA), N2 physisorption, scanning electron microscopy (SEM) coupled with energy dispersive spectroscopy (EDS), diffuse reflectance spectroscopy (DRS-UVvis) and Fourier transform infrared spectroscopy (FTIR). Results showed the formation of perovskite only at 1000 °C and Nb2O5-CeO2 mixed oxides at lower temperatures with some interesting characteristics. Pechini technique allows the synthesis of cerium niobate perovskite at lower temperatures than those presented in the literature (prepared by different methods).