Spherical La0.8Sr0.2Ga0.8Mg0.2O3-δ (LSGM) precursor powders were synthesized by aerosol plasma pyrolysis using an aqueous solution of metal nitrate. As-prepared powders obtained by this method were found to have a spherical morphology with a bimodal size distribution of nanosized (primary) and submicron-sized (secondary) particles. The average size of the primary particles was less than 100 nm. X-ray diffraction (XRD) patterns showed that as-prepared powders crystallized to LSGM and other phases. XRD revealed that LSGM pellets were crystallized to a perovskite structure after sintering at 1300 °C for 10 h.