In the present work, a series of zinc ferrite nanoparticles of 11 nm on average size were synthesized following an electrochemical method in aqueous medium. The nanoparticles were structurally characterized by X-ray diffraction (XRD), inductively coupled plasma spectroscopy (ICP), transmission electron microscopy (TEM), X-ray absorption spectroscopy (XAS) and neutron diffraction (ND). The magnetic characterization was carried out by vibrating sample magnetometer (VSM) and superconducting quantum interference device (SQUID) measurements. The electrochemical synthetic methodology used in this paper yields zinc ferrite monocrystalline nanoparticles with a controlled size, shape and composition, in a reproducible manner. The control of such parameters enables obtaining ferrite nanoparticles with tuneable magnetic properties. The results show that the Zn cations are situated in tetrahedral sites in the crystalline spinel structure, which causes a progressive decrease in the magnetic moments of the ferrites with Zn content due to the breakdown of the super-exchange interactions.
We acknowledge financial support from the Spanish Ministerio de Ciencia, Innovación y Universidades through the projects PGC2018–095642-B-I00, PIB2019–104600RB-I00, MAT2017–86540- C4–1-R and RTI2018–095303-A-C52 and Spanish Ministry of Economy and Competitiveness under project MAT2015–67557- C2–2-P. A.S. acknowledges the Comunidad de Madrid for an “Atracción de Talento Investigador” contract (No. 2017- t2/IND5395). The European Synchrotron (ESRF), Institut Laue-Langevin (ILL) and Consejo Superior de Investigaciones Científicas (CSIC) are also ac- knowledged for the provision of synchrotron radiation facilities and neutron diffraction experiments. We also thank the BM25-SpLine and ILL staff for the technical support beyond their dutie