New synthesis route using metal carboxylates precursor method was adopted for the synthesis of NiFe2O3 is reported. X-ray density, Tap density and powder densities of as prepared NiFe2O3 are calculated. The as synthesized NiO, Fe2O3 and NiFe2O3 are characterized by X-ray diffraction (XRD) technique. Infrared spectroscopic (IR) technique was used to know the formation of M-O and M-M bonds in prepared oxide materials.