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

• Published in: Chemistry : a European journal Vol. 28; no. 34; pp. e202104331 - n/a
• Main Authors: Lisníková, Soňa, Kopp, Josef, Vrba, Vlastimil, Novák, Petr
• Format: Journal Article
• Language: English
• Published: Germany Wiley Subscription Services, Inc 15-06-2022
• Subjects: Cations; Chemistry; Cobalt; Cobalt ferrites; Decomposition; Fe/Co oxalates; in situ XRD; Metal ions; Mixtures; Mossbauer spectroscopy; Mössbauer spectroscopy; Oxalates; Oxalic acid; Physical properties; Precursors; solid solution; Solid solutions; Spectroscopy; Spinel; structural analysis; Thermal decomposition; X-ray diffraction; Fe/Co oxalates; structural analysis; solid solution; in situ XRD; Mössbauer spectroscopy
• ISSN: 0947-6539; 1521-3765
• DOI: 10.1002/chem.202104331

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 N2 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.
We report the benefits of single‐phase oxalate precursors for the preparation of spinel ferrites by thermal decomposition. Various characterization techniques are employed to study the bimetallic nature of the oxalate precursor. The thermal decomposition of the bimetallic oxalate is investigated using in situ XRD. The products of decomposition are further examined by Mössbauer spectroscopy, XRD and N2 adsorption.