We have measured the dielectric properties of nickel ferrite (NiFe 2 O 4 ) synthesized by the micelles mixing method, prepared in suspension of coconut oil and annealing for 4 h at different temperatures. The as-grown ferrites presented highly amorphous X-ray spectrum. Post preparation annealing was applied to induce the increase in the size of the nanoparticles in order to tune the dielectric responses of the samples at the microwave frequencies.The X-ray diffraction (XRD) was applied to investigate the nanoparticle size dependence on the annealing temperature, allowing the correlation between the nanoparticle size and the observed microwave dielectric response.The micelles mixing method of preparation is then a cheap procedure to obtain high quality nanostructured nickel ferrites with low dielectric losses, and dielectric constant between 2.4 and 3.6. Zn-substituted Ni-Mg ferrites, J Magn Magn Mater 192 (1999), 305-313. 11. E.M. Mohammed, K.A. Malini, P. Kurian, and M.R. Anantharaman, Modification of dielectric and mechanical properties of rubber