Microwave synthesis of ferrite materials integrates the synthetic technology for information storage materials. Microwave route is adopted for the synthesis of nanosized NiFe2O4 using urea as a fuel. Nickel oxalates and iron oxalates were prepared by dissolving nickel and iron salt in oxalic acid solution. These two oxalates are irradiated with microwaves using urea as a fuel to get cubic NiFe2O4 particles. The structure of the prepared sample is studied by X-ray diffraction (XRD) which shows crystalline cubic structure, Morphology of the sample is viewed by Scanning electron micrograph (SEM) which shows spherical particles with compact and globular arrangement. Metal-Oxygen and metal-metal bonding is studied by infrared (IR) technique.