A combined electrochemical/chemical method has been developed for synthesize manganese ferrite nanoparticles. This is able to obtain MnxFe3−xO4 ferrite, where x = 0.5. This low amount of Mn in the structure was similar in samples obtained by electrochemical synthesis. The size of the manganese ferrite was around 23 ± 6 nm and X-ray diffraction confirmed the spinel structure without impurities.
Mn cations were found to possess high crystallographic order with the first and second neighbor and a mixture of Mn2 + and Mn3 + was confirmed. Also XANES and EXAFS have demonstrated the presence of Fe2 + and Fe3 + in the structure. The comparison of nanoparticles obtained electrochemically and by the method developed in this work has shown similar structural and magnetic characteristics. Therefore, the most important conclusion of this work is that this methodology, which replaces the manganese anode in the electrosynthesis process by a Mn2 + electrolyte, is perfectly viable and allows obtaining materials with the same characteristics and properties. This is a major breakthrough, taking into account the cost of the metal and its rapid degradation over time.