Abstract. In this study, BaFe 1−x Al x O 3-δ (0 ≤ x ≤ 0.3) perovskite-type oxides were prepared by sol-gel method using citric acid as chelating agent. The samples were subjected to various calcination temperatures in order to investigate the physicochemical properties of the oxide affected by the parameter. Thermogravimetric analysis, Fourier transform infrared spectroscopy and X-ray diffraction (XRD) techniques are used to explore precursor decomposition and to establish adequate calcination temperature for the preparation of the nanopowders. The studied compounds have hexagonal crystal structure at the temperature of 1123 K. The samples obtained after calcination at 1123 K were characterized by XRD, Brunauer-Emmett-Teller surface area analysis, scanning electron microscopy, powder size distribution and electrical conductivity. The microstructure and morphology of the compounds show that the particles are nearly spherical in shape and are partially agglomerated. The highest surface area and total pore volume are achieved for BaFe 0.8 Al 0.2 O 3-δ oxide. Temperature dependence of electrical conductivity shows a semiconducting behavior.