Nanoparticles nickel ferrite of size 6 -8 nm, synthesized by the coprecipitation method with x varying from 0 to 1.0. The powder samples were characterized by XRD, VSM and FTIR. The average crystallite sizes of the particles were determined from X-ray diffraction. X-ray analysis showed that the samples were cubic spinel. The lattice constant (a o ) increased with the increase in zinc substitution. The specific saturation magnetization (M S ) of the particles was measured at room temperature. The magnetic parameter of M S , was found to decrease with the increase in zinc substitution. Fourier transform infrared spectroscopy (FTIR) spectra of the Ni 1-x Zn x Fe 2 O 4 with x = 0, 0.5, 1 in the range 400 -4000 cm -1 were reported. The spinel structure and the crystalline water adsorption of Ni 1-x Zn x Fe 2 O 4 nanoparticles were studied by using FTIR.