NiFe2O4 nanoparticles were synthesized using the microwave assisted combustion method based on metal nitrate salts and urea. To remain of organic matters and to stabilize the particles, samples were thermally treated at various temperatures from 300-800 degrees C. The prepared samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX) thermogravimetric analysis (TGA) and vibrating sample magnetometry (VSM). The heat treated samples show the reflection planes of (111), (220), (222), (311), (400), (422), (511), and (440) which perfectly confirm to a cubic spinel phase of NiFe2O4 and no secondary phases were detected in the XRD patterns of the samples. The crystallite sizes calculated using the Debye-Scherrer formula were found to increase with the heat treatment temperature, from about 4 nm at 300 degrees C-85 nm at 800 degrees C. EDX results verify that the compositional mass rations were relevant, as expected from the synthesis. The micrographs of SEM and TEM showed that all of the samples have nano-crystalline behavior and particles indication cubic shape. Magnetization measurements were obtained at room temperature by using a VSM, which demonstrated that the all of the samples synthesized with heat treatment exhibited ferromagnetic behaviors. (C) 2014 Elsevier B.V. All rights reserved.