In-situ X-ray diffraction study of carbonate formation and decomposition in perovskite-type BCFZ
The effect of CO{sub 2} on the two phase perovskite with average composition of BaCo{sub 0.4}Fe{sub 0.4}Zr{sub 0.2}O{sub 3-{delta}} is investigated by in-situ X-ray diffraction (XRD) as well as transmission electron microscopy (TEM). Partial decomposition of the BCFZ into high-temperature rhombohedral BaCO{sub 3} polymorph was observed during annealing in an atmosphere, which contained 50 vol% CO{sub 2}/50 vol% N{sub 2} at 1173 K. This carbonate structure is not quenchable and cannot be detected by ex-situ methods. Additionally, the reversible phase transition of BaCO{sub 3} from orthorhombic to rhombohedral to cubic at different temperatures accompanied by formation of CoO was shown by in-situ XRD and TEM. Furthermore, complete regeneration of perovskite phase was obtained after high-temperature treatment under CO{sub 2}-free conditions. -- Graphical abstract: In-situ XRD of BCFZ powder in the atmosphere containing 50% CO{sub 2} and 50% N{sub 2} at different temperatures showing formation of BaCO{sub 3} and their phase transition. Display Omitted Highlights: {yields} Partial BCFZ decomposition. {yields} Rapid formation of rhombohedral BaCO{sub 3} after exposure of the CO{sub 2} at 1173 K. {yields} Reversible phase transition of BaCO{sub 3}. {yields} Formation of CoO and tetragonal disordered Fe-enriched perovskite phase. {yields} Complete regeneration of BCFZ after removing of CO{sub 2}.