Microwave-induced combustion with glycine, CTAB-assisted hydrothermal process with NaOH and NH3, EDTA assisted-hydrothermal methods have been applied to prepare NiFe2O4 nanoparticles for the first time. Structural and magnetic properties of the products were investigated by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmison electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), and electron spin resonance spectrometry (EPR). TEM measurements showed that morphology of the product depends on the synthesis method employed. The average cystallite size of NiFe2O4 nanoparticles was in the range of 14-59 nm as measured by XRD. The uncoated sample (Method A) had an EPR linewidth of 1973 Oe, the coated samples reached lower values. The magnetic dipolar interactions existing among the Ni ferrite nanoparticles are reduced by the coatings, which could cause the decrease in the linewidth of the EPR signals. Additionally, the linewidth increases with an increase in the size and the size distribution of nanoparticles.