We report on the synthesis of Zn0.7Ni0.3Fe2O4 nanoparticles via microwave assisted combustion route by using urea as fuel. XRD and FT-IR analyses confirm the composition and structure as spinel ferrite. The crystallite size estimated from XRD (16.4nm) and the magnetic core size(15.04nm) estimated from VSM agree well, while a slightly smaller magnetic diameterre reflects a very thin magnetically dead layer on the surface of the nanoparticles. Morphological investigation of the products was done by TEM which revealed the existence of irregular shapes such spherical, spherodial and polygon. Magnetization measurements performed on Zn0.7Ni0.3Fe2O4 nanoparticles showed that saturation was not attained at even in the high magnetic field. The sample shows superparamagnetic behavior at around the room temperature and ferromagnetic behavior below the blocking temperature which is measured as 284 K. (C) 2009 Elsevier B.V. All rights reserved.