A recently reported promising new perovskite oxide cathode material, Ba0.2Sr0.8Co0.8Fe0.2O3−δ, (BSCF) (with x = 0.2 and y = 0.8) of high purity for intermediate-temperature solid oxide fuel cells (IT-SOFCs) was synthesised in the current work by using the co-precipitation method. The result indicated a precursor with a well-deﬁned composition of ﬁne particle size, high homogeneity, and high reactivity. After calcining has been developed at 900°C, the individual oxides from ammonium oxalate were alloyed into nanostructured perovskite (with x = 0.2 and y = 0.8) Ba0.2Sr0.8Co0.8Fe0.2O3 of high purity. The thermal properties, phase constituents, surface area and microstructure of the samples were characterised by TGA, XRD, BET, SEM and EDX techniques respectively. The results show that the BSCF powders have cubic perovskite-type structure with fine particle size, high surface area and high homogeneity. The current method employed is found to be very reliable for the synthesis of BSCF.