Abstract FeTiO3 powders were prepared from (Fe+Ti) mixed carbonate precursor by the microwave-assisted calcination method. The thermal analysis of the precursor was conducted by TG/DSC. It is demonstrated that the calcination process can be divided into three different stages: the removal of water, the decomposition of precursor and the formation of FeTiO3. A variety of techniques, such as XRD, FT-IR, SEM and EDS were utilized to characterize the samples. The results indicated that FeTiO3 powders can be prepared by microwave-assisted calcination for 20min at 450°C, while those cannot be obtained by conventional one until reaction time exceeds 120min at 600°C. The FeTiO3 powders prepared by microwave-assisted calcination are nearly spherical with limited aggregation and have a mean particle size of 400–500nm.