Single‐Phase Precursors for the Preparation of Spinel Ferrites via Oxalate Route: the Study of Cobalt Ferrite Synthesis

Abstract This work explores the benefits of single‐phase oxalate precursors for the preparation of spinel ferrites by thermal decomposition. A direct comparison between the genuine oxalate solid solution and the physical mixture of simple oxalates is presented using the case study of cobalt ferrite preparation. The mixing of metal cations within a single oxalate structure could be verified prior to its thermal decomposition by several non‐destructive experimental techniques, namely Mössbauer spectroscopy, X‐ray powder diffraction (XRD) and energy‐dispersive X‐ray spectroscopy. In situ XRD experiments were conducted to compare the decomposition processes of the solid solution and the physical mixture. Additionally, the decomposition products of the FeCo oxalate solid solution were studied ex situ by means of N 2 adsorption, Mössbauer spectroscopy and XRD. The results obtained for different reaction temperatures demonstrate the possibilities to easily control the physical properties of the prepared oxides.