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Combined EXAFS, XRD, DRIFTS, and DFT Study of Nano Copper-Based Catalysts for CO2 Hydrogenation

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    Research Article

    Combined EXAFS, XRD, DRIFTS, and DFT Study of Nano Copper-Based Catalysts for CO2 Hydrogenation
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    † Department of Chemistry, Christopher Ingold Laboratories, University College London, 20 Gordon Street, London WC1H 0AJ, United Kingdom
    ‡ Department of Chemical Engineering and Technology, KTH-Royal Institute of Technology, Teknikringen 42, 100 44 Stockholm, Sweden
    § School of Chemical Engineering and Analytical Science, The University of Manchester, Oxford Road, Manchester M13 9PL, U.K.
    ∥ School of Chemistry, Cardiff University, Main Building, Park Place, Cardiff CF10 3AT, U.K.
    *J.A.D.: e-mail, [email protected]; tel, +44 (0)20 7679 4345.
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    ACS Catalysis

    Cite this: ACS Catal. 2016, 6, 9, 5823–5833
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    https://doi.org/10.1021/acscatal.6b01529
    Published July 21, 2016
    Copyright © 2016 American Chemical Society
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    Abstract

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    Highly monodispersed CuO nanoparticles (NPs) were synthesized via continuous hydrothermal flow synthesis (CHFS) and then tested as catalysts for CO2 hydrogenation. The catalytic behavior of unsupported 11 nm sized nanoparticles from the same batch was characterized by diffuse reflectance infrared fourier transform spectroscopy (DRIFTS), extended X-ray absorption fine structure (EXAFS), X-ray diffraction (XRD), and catalytic testing, under CO2/H2 in the temperature range 25–500 °C in consistent experimental conditions. This was done to highlight the relationship among structural evolution, surface products, and reaction yields; the experimental results were compared with modeling predictions based on density functional theory (DFT) simulations of the CuO system. In situ DRIFTS revealed the formation of surface formate species at temperatures as low as 70 °C. DFT calculations of CO2 hydrogenation on the CuO surface suggested that hydrogenation reduced the CuO surface to Cu2O, which facilitated the formation of formate. In situ EXAFS supported a strong correlation between the Cu2O phase fraction and the formate peak intensity, with the maxima corresponding to where Cu2O was the only detectable phase at 170 °C, before the onset of reduction to Cu at 190 °C. The concurrent phase and crystallite size evolution were monitored by in situ XRD, which suggested that the CuO NPs were stable in size before the onset of reduction, with smaller Cu2O crystallites being observed from 130 °C. Further reduction to Cu from 190 °C was followed by a rapid decrease of surface formate and the detection of adsorbed CO from 250 °C; these results are in agreement with heterogeneous catalytic tests where surface CO was observed over the same temperature range. Furthermore, CH4 was detected in correspondence with the decomposition of formate and formation of the Cu phase, with a maximum conversion rate of 2.8% measured at 470 °C (on completely reduced copper), supporting the indication of independent reaction pathways for the conversion of CO2 to CH4 and CO that was suggested by catalytic tests. The resulting Cu NPs had a final crystallite size of ca. 44 nm at 500 °C and retained a significantly active surface.

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    The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acscatal.6b01529.

    • Schematic representation of the continuous hydrothermal flow synthesis (CHFS) process, DFT model surfaces, and heterogeneous test results for WHSV = 4900 mL h–1 g–1 (PDF)

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    Cite this: ACS Catal. 2016, 6, 9, 5823–5833
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    https://doi.org/10.1021/acscatal.6b01529
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    Citations are the number of other articles citing this article, calculated by Crossref and updated daily. Find more information about Crossref citation counts.

    The Altmetric Attention Score is a quantitative measure of the attention that a research article has received online. Clicking on the donut icon will load a page at altmetric.com with additional details about the score and the social media presence for the given article. Find more information on the Altmetric Attention Score and how the score is calculated.