An electrochemical method for the synthesis of complex dispersed oxide system Al₂O₃–Fe₂O₃, based on the combined aluminum and iron anodic dissolution in aqueous solution containing chloride ions, has been suggested. The phase composition and morphology of Al₂O₃–Fe₂O₃ dispersed precipitate have been investigated by means of X-ray fluorescence, X-ray diffraction (XRD), and scanning electron microscopy (SEM). The influence of the electrolysis mode on the characteristics of the synthesized oxide system has been shown. It is found that the direct current (DC) mode allows us to adjust the phase correlation in the precipitate and to obtain a particle size which is two or more times smaller than the particle size of the samples synthesized by means of the alternating current (AC).