Iron oxides currently attract considerable attention due to their potential applications in the fields of lithiumion batteries, bio-medical sensors, and hyperthermia therapy materials. Magnetite (Fe3O4) is a particularly interesting research target due to its low cost, good biocompatibility, outstanding stability in physiological conditions. Hydrothermal synthesis is one of several liquid-phase synthesis methods with water or an aqueous solution under high pressure and high temperature. This paper reports the growth of magnetic Fe3O4 particles from iron powder (spherical, <10 μm) through an alkaline hydrothermal process under the following conditions: (1) Different KOH molar concentrations and (2) different synthesis time for each KOH molar concentrations. The optimal condition for the synthesis of Fe3O4 using Fe powders is hydrothermal oxidation with 6.25 M KOH for 48 h, resulting in 89.2 emu/g of saturation magnetization at room temperature. The structure and morphologies of the synthesized particles are characterized by X-ray diffraction (XRD, 2θ = 20°–80°) with Cu-kα radiation and field emission scanning electron microscopy (FE-SEM), respectively. The magnetic properties of magnetite samples are investigated using a vibrating sample magnetometer (VSM). The role of KOH in the formation of magnetite octahedron is observed.
In this study, the reduction kinetics and behaviors of oxides in the water-atomized iron powder have been evaluated as a function of temperature ranging 850-1000˚C in hydrogen environment, and compared to the reduction behaviors of individual iron oxides including Fe2O3, Fe3O4 and FeO. The water-atomized iron powder contained a significant amount of iron oxides, mainly Fe3O4 and FeO, which were formed as a partially-continuous surface layer and an inner inclusion. During hydrogen reduction, a significant weight loss in the iron powder occurred in the initial stage of 10 min by the reduction of surface oxides, and then further reduction underwent slowly with increasing time. A higher temperature in the hydrogen reduction promoted a high purity of iron powder, but no significant change in the reduction occurred above 950˚C. Sequence reduction process by an alternating environment of hydrogen and inert gases effectively removed the oxide scale in the iron powder, which lowered reduction temperature and/or shortened reduction time.