Spinel Iron Oxide by the Co-Precipitation Method: Effect of the Reaction Atmosphere

Synthesis atmosphere (i.e., air and nitrogen) effects on the physical properties and formation mechanism of spinel iron oxide nanoparticles prepared via the co-precipitation method have been investigated using a multi-technique approach. The obtained magnetic nanoparticles (MNPs) were characterized using the X-ray diffraction, transmission electron microscopy (TEM), SQUID magnetometry, Mossbauer spectroscopy and X-ray absorption near-edge Structure spectroscopy techniques. The synthesis procedure leads to the formation of a spinel structure with an average crystallite size of 9.0(9) nm. The morphology of the particles synthetized under an inert atmosphere was quasi-spherical, while the nanoparticles prepared in air present a faceted shape. The small differences observed in morphological properties are explained by the influence of the reaction atmosphere on the formation mechanism of the MNPs. The magnetic characterization indicates that both samples exhibit superparamagnetic behavior at 300 K. The investigation by means of the Langevin approach at 300 K also leads to equal values for the mean size of the magnetic cores (Dm). Additionally, the analysis of the Mossbauer spectra revealed the lack of spin disorder for both samples, resulting in a high saturation magnetization. The fit of XANES spectrum suggests that about 2/3 of the iron ions reside in a local environment close to that of γ-Fe2O3 and about 1/3 close to that of Fe3O4 for the sample synthetized in inert atmosphere.