Nickel zinc ferrite nanoparticles of the composition NixZn1-xFe2O4 (x = 0.1, 0.3, 0.5) have been synthesized by the chemical co-precipitation method. The samples were characterized by X-ray diffraction, TEM, EPR, DC magnetization and AC susceptibility measurements. The X-ray diffraction patterns confirm the synthesis of single crystalline phase of NixZn1-xFe2O4 (x = 0.1, 0.3, 0.5) nanoparticles. Lattice parameter decreases with the increase in nickel content. The magnetic measurements shows superparamagnetic nature of the samples for x = 0.1 and 0.3 whereas for x = 0.5 the material shows ferromagnetic nature. The saturation magnetization is low and increases with increase in nickel content. The superparamagnetic nature of the samples is supported by the EPR and ac susceptibility measurement studies. The blocking temperature increases with the nickel concentration. The changes in the magnetic properties have been explained by the redistribution of the cations on A and B sites.