Zinc–ferrite, nickel–ferrite and mixed nickel–zinc ferrites were successfully synthesized via the thermal decomposition method from acetylacetonate complexes. To control the particle size and enhance dispersibility in an aqueous medium, starch, a natural and biocompatible compound, was used for the first time for coating such magnetic powders. X-ray powder diffraction (XRPD) was performed to study the structural properties of all samples. The presence of a single-phase spinel structure as well as the cation distribution in both sites of all investigated magnetic powders was confirmed. The values of unit cell parameters obtained from the results of the Rietveld analysis decreased, while the average crystallite size increased with increasing Ni2+ content. The average microstrain parameters unambiguously showed a change in the spinel structure with cation distribution. Scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS) and Fourier transform infrared spectroscopy (FTIR) analyses were also utilized to characterize the synthesized materials, corroborating the XRPD data. The obtained results indicated that functionalization by starch was successfully achieved.
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