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In situ XRD study of nanocrystalline cobalt oxide reduction

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Abstract

The reduction of nanocrystalline cobalt oxide samples (single-phase and supported on γ-Al2O3) was studied using in situ X-ray diffraction (XRD) analysis. The atomic structures of single-phase and supported Co3O4 samples were refined, and the occurrence of cationic vacancies was demonstrated. A set of methods (XRD, temperature-programmed reduction, and differential dissolution) was used to find that the reduction of supported and unsupported model cobalt oxide was considerably different. The single-phase sample was reduced in undiluted hydrogen to cobalt metal with a hexagonal closely packed structure. The reduction of the supported sample (unlike the single-phase sample) occurred through the formation of a crystalline CoO phase to the formation of cobalt metal with a face-centered cubic structure. Interaction of cobalt oxide with the γ-Al2O3 support, which hinders the reduction to cobalt metal, was detected.

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Correspondence to A. V. Ishchenko.

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Original Russian Text © O.A. Bulavchenko, S.V. Cherepanova, V.V. Malakhov, L.S. Dovlitova, A.V. Ishchenko, S.V. Tsybulya, 2009, published in Kinetika i Kataliz, 2009, vol. 50, No. 2, pp. 205–211.

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Bulavchenko, O.A., Cherepanova, S.V., Malakhov, V.V. et al. In situ XRD study of nanocrystalline cobalt oxide reduction. Kinet Catal 50, 192–198 (2009). https://doi.org/10.1134/S0023158409020086

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