Nanocrystalline forms of nickel ferrite (NiFe2O4) have been synthesized with the aid of single step chemical combustion method using citric acid as fuel in the 1:1 ratio. The single phase formation of nickel ferrite was confirmed through powder X-ray diffraction (XRD). The presence of various functional groups was confirmed through Fourier transform infrared spectroscopic (FTIR) analysis and the compositional analysis was performed through Energy dispersive X-ray studies (EDX). The micro structural features of nanocrystallites were examined by scanning electron microscope (SEM). Surface morphology of the nanocrystalline form of NiFe2O4 was also investigated through transmission electron microscopic (TEM) analysis. Magnetic measurements have showed the ferrimagnetic properties with Curie temperature @ 500 °C. The obtained results are in good agreement with the reported values. The other results have been discussed in detail.