A chemical route was used to synthesize perovskite bismuth ferrite and spinel nickel ferrite of bismuth ferrite-nickel ferrite nanocomposites. The precursors mixed were made to undergo thermal analyses to observe the crystallization temperature. Then the precursor samples were heated at 550, 600 and 700 °C for 4 h, followed by XRD analyses to determine phase formation. Crystallite size, strain analyses by the Williamson-Hall plot and planes of orientations were noted from XRD analysis. It was observed that 600 °C was the optimum temperature for phase development. Morphology analyses exhibited an agglomerated mass of particulates, while individual phase particulates were polygonal and irregularly shaped. EDX analysis confirmed the elemental compositions of the sample synthesized, while FTIR analysis confirmed the presence of M-O octahedral and tetrahedral coordinations of the M-O bonds formed.