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Critical Influence of Redox Pretreatments on the CO Oxidation Activity of BaFeO3−δ Perovskites: An in-Depth Atomic-Scale Analysis by Aberration-Corrected and in Situ Diffraction Techniques

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Departamento de Química Inorgánica, Facultad de Ciencias Químicas, Universidad Complutense, 28040 Madrid, Spain
Departamento de Ciencia de los Materiales e Ingeniería Metalúrgica y Química Inorgánica, Facultad de Ciencias, Universidad de Cádiz, Campus Río San Pedro, 11510 Puerto Real, Spain
§ Instituto Universitario de Investigación en Microscopía Electrónica y Materiales (IMEYMAT), Facultad de Ciencias, Universidad Complutense, Campus Río San Pedro, 11510 Puerto Real, Spain
Centro Nacional de Microscopia Electrónica, Universidad Complutense, 28040 Madrid, Spain
*J.M.G.-C.: e-mail, [email protected]; tel, +34 91 394 41 88; fax, +34 91 394 43 52.
Cite this: ACS Catal. 2017, 7, 12, 8653–8663
Publication Date (Web):November 7, 2017
https://doi.org/10.1021/acscatal.7b02595
Copyright © 2017 American Chemical Society

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    Abstract

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    A BaFeO3−δ (δ ≈ 0.22) perovskite was prepared by a sol–gel method and essayed as a catalyst in the CO oxidation reaction. BaFeO3−δ (0.22 ≤ δ ≤ 0.42) depicts a 6H perovskite hexagonal structural type with Fe in both III and IV oxidation states and oxygen stoichiometry accommodated by a random distribution of anionic vacancies. The perovskite with the highest oxygen content, BaFeO2.78, proved to be more active than its lanthanide-based counterparts, LnFeO3 (Ln = La, Sm, Nd). Removal of the lattice oxygen detected in both temperature-programmed oxidation (TPO) and reduction (TPR) experiments at around 500 K and which leads to the complete reduction of Fe4+ to Fe3+, i.e. to BeFeO2.5, significantly decreases the catalytic activity, especially in the low-temperature range. The analysis of thermogravimetric experiments performed under oxygen and of TPR studies run under CO clearly support the involvement of lattice oxygen in the CO oxidation on these Ba-Fe perovskites, even at the lowest temperatures. Atomically resolved images and chemical maps obtained using different aberration-corrected scanning transmission electron microscopy techniques, as well as some in situ type experiments, have provided a clear picture of the accommodation of oxygen nonstoichiometry in these materials. This atomic-scale view has revealed details of both the cation and anion sublattices of the different perovskites that have allowed us to identify the structural origin of the oxygen species most likely responsible for the low-temperature CO oxidation activity.

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    The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acscatal.7b02595.

    • Experimental details including chemical analysis, microstructural characterization, powder neutron diffraction, thermogravimetric analysis, study of catalyst pretreatment conditions, study of catalyst conditions, XPS analysis, and Rietveld refinement of the XRD under vacuum conditions (PDF)

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