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

Abstract

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. © 2022 by the authors.