Synthesis and structural characterization of ZnxFe3−xO4 ferrite nanoparticles obtained by an electrochemical method

A series of zinc ferrite nanoparticles were synthesized following a single-step electrochemical method in aqueous medium. This strategy allowed the control of both the size and chemical composition of the nanoparticles in an easy and reproducible manner by simply varying the intensity of the applied current. The obtained nanoparticles were morphologically and structurally characterized as a function of the particle size and the Zn content in the sample by X-ray diffraction (XRD), transmission electron microscopy (TEM), inductively coupled plasma emission spectroscopy (ICP) and Raman microscopy. The formation of ZnxFe(3-x)O4 (x = 0.18-0.93) ferrite nanoparticles with crystal sizes in the range of 9 to 18 nm and with a homogeneous distribution of the Zn2+ cation in the crystalline structure was observed. However, following a thermal treatment, a migration of zinc cations was detected that led to the formation of two different crystalline phases, stoichiometric zinc ferrite and hematite. Raman microscopy revealed the formation of segregated micro-domains enriched within these crystalline phases. The study of the magnetic properties of the electro-synthesized ferrite nanoparticles with a homogeneous incorporation of Zn in the structure shows that the saturation magnetization and the coercively values are highly dependent on the chemical composition and crystal size.