BiFeO3-PbTiO3 powders were synthesized by a novel sol-gel auto-combustion method. The gels, transformed from the aqueous solutions of metal nitrate and citric acid, undergo a selfpropagatingcombustion process when being ignited and yield voluminous ashes. These ashes are single phase perovskite BiFeO3-PbTiO3 powders. The redox behaviors of the dried gels were studied by DTA-TG technique and IR spectra. The synthesized powders were characterized in terms of XRD, SEM and BET techniques.