A Comprehensive Study of Synthesis and Analysis of Anisotropic Iron Oxide and Oxyhydroxide Nanoparticles

One-dimensional anisotropic nanoparticles are of great research interest across a wide range of biomedical applications due to their specific physicochemical and magnetic properties in comparison with isotropic magnetic nanoparticles. In this work, the formation of iron oxides and oxyhydroxide anisotropic nanoparticles (ANPs) obtained by the co-precipitation method in the presence of urea was studied. Reaction pathways of iron oxide and oxyhydroxide ANPs formation are described based on of X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), and pulse magnetometry studies. It is shown that a nonmonotonic change in the Fe₃O₄ content occurs during synthesis. The maximum content of the Fe₃O₄ phase of 47.4% was obtained at 12 h of the synthesis. At the same time, the reaction products contain ANPs of α-FeOOH and submicron isotropic particles of Fe₃O₄, the latter formation can occur due to the oxidation of Fe²⁺ ions by air-oxygen and Ostwald ripening processes. A subsequent increase in the synthesis time leads to the predominant formation of an α-FeOOH phase due to the oxidation of Fe₃O₄. As a result of the work, a methodological scheme for the analysis of iron oxide and oxyhydroxide ANPs was developed.