Monodispersed NiFe2O4 nanoparticles are synthesized using both organic and inorganic precursors via a nonaclueous solvothermal method. X-ray diffraction (XIRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR) and atomic absorption spectroscopy (AAS) have confirmed the formation of single-phase monodispersed NiFe2O4 nanoparticles. The synthesized particles are highly dispersible in nonpolar organic solvents like hexane, toluene etc. A detailed study on the variation of size and shape of the synthesized particles by slight variation of the reaction conditions has been carried out. (C) 2008 Elsevier B.V. All rights reserved.