Nanocrystalline nickel ferrite has been synthesized by novel combustion method using hexamine as a fuel and metal nitrates as oxidizers. The prepared compounds were sintered at 750°C. The synthesized ferrite powders were characterized by XRD, FTIR, EDAX, and SEM. XRD data confirm the formation of single-phase spinel nickel ferrite compound. FTIR spectra show the stretching and bending vibrations of Ni-O and Fe-O bonds in nickel ferrite. The elemental composition of the synthesized compound was assessed by EDAX analysis. The morphological features of the ferrite powders were scrutinized by SEM.