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[en] Nanostructured nickel ferrite stoichiometric spinel NiFe2O4 is intensively studied as a material suitable for catalysts or medical applications. Thus, it is very important to find a simple and cost-effective method for the synthesis of nanoparticles with homogenous and tunable particle size. In this work, we successfully synthetized nickel ferrite nanoparticles by thermal decomposition of nickel-iron glycerolate in a dynamic air atmosphere at different temperatures. We studied the thermal decomposition process by STA. The nickel-iron glycerolate precursor was analyzed by XRD, XPS, AAS, Raman spectroscopy, EDS and SEM to obtain exact composition and information about the morphology. The particle size of the obtained nanoparticles was determined from XRD diffraction patterns using Scherrer equation and also by TEM. Magnetic properties were studied using VSM in PPMS. - Highlights: • Nickel ferrite spinel NiFe2O4 nanoparticles. • Synthesis by thermal decomposition of nickel-iron glycerolate. • Characterization by XRD, XPS, AAS, Raman spectroscopy, EDS, and TEM. • Magnetic properties were studied using VSM in PPMS.