The combustion reaction is an important powder preparation process by which several hundred compounds may be prepared. Ni-Zn ferrite nano. particles (Ni1-xZnxFe2O4, x = 0,3; 0,5 and 0,7 mol) have been prepared by a single step solution combustion reaction using nitrates and urea as fuel. XRD, BET, SEM, and helium pycnometer characterized the as-prepared powders. Ni-Zn ferrite nanoparticles prepared by the present method can easily form the well-crystallized particles with a large surface area in the range of 42-64 m(2)/g. The resulting powders showed extensive XRD line broadening and the crystallite sizes calculated from the XRD fine broadening were in the nanometer range (19-25 nm). The results evidenced the influence of different compositional variables on the powders characteristic.