Using nickel, zinc and ferric nitrates, and glycine in a fuel-rich composition, Ni 1-x Zn x Fe 2 O 4 nanoparticles were prepared by a simple low-temperature auto-combustion method without further sintering at high temperatures. The auto-combusted powders obtained were characterized by X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy, energy-dispersive X-ray (EDAX) analysis and vibrating scanning magnetometer measurements. XRD confirms the formation of pure nanocrystalline spinel phases with an average diameter of about 55 nm. Raman spectra show tetrahedral and octahedral sites in the structure of Ni 1-x Zn x Fe 2 O 4 and also imply the doping of Zn 2+ and displacement of Fe 3+ ions from the tetrahedral site. EDAX showed that the samples were close to the nominal compositions. The magnetic measurement shows that the saturation magnetization and remanence magnetization decreases with the increase in the zinc content.