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Nanoscale Nickel ferrite particles were prepared by combustion method using nickel nitrate as oxidizer and urea as a fuel. The structure of the sample is studied with X-ray diffraction (XRD) using Cu-Kα radiation. The X-ray diffraction analysis revealed the nanocrystalline nature in the prepared ferrite samples. Dielectric studies have been undertaken over a wide range of frequencies (100Hz-5MHz) for Nickel nanoferrites at room temperature. Dielectric properties such as dielectric loss tangent (D), dielectric constant (ε′ ) and dielectric loss factor (ε″) are found to decrease with the increase in the frequency. Observed variations are understood on the basis of Koop’s phenomenological model. Further, a. c. conductivity of the Nickel nanoferrite was found to increase with the increase in the frequency. Observed variation in the a. c. conductivity with the frequency has been understood on the basis of electron hopping model.