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Operando identification of site-dependent water oxidation activity on ruthenium dioxide single-crystal surfaces

Nature Catalysis volume 3, pages 516–525 (2020)Cite this article

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Abstract

Understanding the nature of active sites is central to controlling (electro)catalytic activity. Here we employed surface X-ray scattering coupled with density functional theory and surface-enhanced infrared absorption spectroscopy to examine the oxygen evolution reaction on RuO2 surfaces as a function of voltage. At 1.5 VRHE, our results suggest that there is an –OO group on the coordinatively unsaturated ruthenium (RuCUS) site of the (100) surface (and similarly for (110)), but adsorbed oxygen on the RuCUS site of (101). Density functional theory results indicate that the removal of –OO from the RuCUS site, which is stabilized by a hydrogen bond to a neighbouring –OH (–OO–H), could be the rate-determining step for (100) (similarly for (110)), where its reduced binding on (100) increased activity. A further reduction in binding energy on the RuCUS site of (101) resulted in a different rate-determining step (–O + H2O – (H+ + e−) → –OO–H) and decreased activity. Our study provides molecular details on the active sites, and the influence of their local coordination environment on activity.

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Fig. 1: The coordination and electronic structure of surface ruthenium and oxygen atoms on different facets of RuO2.
Fig. 2: A DFT-calculated reaction free energy diagram at 1.5 VDFT-RHE.
Fig. 3: Potential-dependent surface structures for RuO2(100).
Fig. 4: Potential-dependent surface structures for RuO2(101).
Fig. 5: Surface-dependent water oxidation kinetics on RuO2.
Fig. 6: The reaction mechanism and water oxidation activity on polycrystalline RuO2 surfaces.

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The data supporting the findings of this study are available in the paper and its Supplementary Information. Extra data are available from the corresponding authors on reasonable request.

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Acknowledgements

This work was supported in part by the Toyota Research Institute through the Accelerated Materials Design and Discovery programme. We thank B. Han for transmission electron microscopy characterization of RuO2 nanoparticles and J. Corchado-Garcia for help during the CTR data collection. This work was supported in part by the Skoltech-MIT Center for Electrochemical Energy and the Cooperative Agreement between the Masdar Institute, UAE and the Massachusetts Institute of Technology, USA (grant no. 02/MI/MIT/CP/11/07633/GEN/G/00). The work by H.Y. was supported by US Department of Energy (DOE), Basic Energy Sciences (BES), Materials Sciences and Engineering Division, and the work by H.Z. and the use of the Advanced Photon Source were supported by DOE, BES, Scientific User Facility Division (SUFD) under contract no. DE-AC02-06CH11357. The work by A.M. was supported by DOE, BES, SUFD under contract no. DE-AC02-76SF00515. A.F.P. acknowledges the Danish Ministry for Higher Education and Science for an EliteForsk travel grant and the Strategic Research’s project NACORR (grant no. 12-133817). This work used the Extreme Science and Engineering Discovery Environment (XSEDE), which is supported by National Science Foundation grant no. ACI-154856283. This research also used resources of the National Energy Research Scientific Computing Center, a DOE Office of Science User Facility supported by the Office of Science of the US DOE under contract no. DE-AC02-05CH11231. T.V. and N.B.H acknowledge support through V-Sustain: the VILLUM Centre for the Science of Sustainable Fuels and Chemicals (grant no. 9455) from VILLUM FONDEN. I.E.L.S acknowledges the Peabody Visiting Associate Professorship, awarded by the Department of Mechanical Engineering at Massachusetts Institute of Technology.

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Author notes

  1. Reshma R. Rao

    Present address: Research Laboratory of Electronics, Massachusetts Institute of Technology, Cambridge, Massachusetts, USA

  2. Yu Katayama

    Present address: Department of Applied Chemistry, Graduate School of Sciences and Technology for Innovation, Yamaguchi University, Tokiwadai, Japan

  3. Ifan E. L. Stephens

    Present address: Royal School of Mines, Imperial College London, South Kensington Campus, London, UK

  4. These authors contributed equally: Reshma R Rao, Manuel J Kolb.

Authors and Affiliations

  1. Department of Mechanical Engineering, Massachusetts Institute of Technology, Cambridge, Massachusetts, USA

    Reshma R. Rao, Livia Giordano & Yang Shao-Horn

  2. Research Laboratory of Electronics, Massachusetts Institute of Technology, Cambridge, Massachusetts, USA

    Manuel J. Kolb, Livia Giordano, Yu Katayama & Yang Shao-Horn

  3. Section for Surface Physics and Catalysis, Department of Physics, Technical University of Denmark, Kongens Lyngby, Denmark

    Anders Filsøe Pedersen, Ib Chorkendorff & Ifan E. L. Stephens

  4. Department of Materials Science and Engineering, Massachusetts Institute of Technology, Cambridge, Massachusetts, USA

    Jonathan Hwang, Jaclyn R. Lunger & Yang Shao-Horn

  5. SLAC National Accelerator Laboratory, Menlo Park, California, USA

    Apurva Mehta

  6. Materials Science Division, Argonne National Laboratory, Lemont, Illinois, USA

    Hoydoo You

  7. X-ray Science Division, Argonne National Laboratory, Lemont, Illinois, USA

    Hua Zhou

  8. Department of Energy Conversion and Storage, Technical University of Denmark, Kongens Lyngby, Denmark

    Niels Bendtsen Halck & Tejs Vegge

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Contributions

Y.S.H. and R.R.R. conceived and designed the experiments. R.R.R. performed the electrochemical measurements. R.R.R., A.F.P., J.H., A.M., H.Y. and H.Z. participated in the surface diffraction measurements. M.J.K., L.G., J.R.L., N.B.H. and T.V. performed the DFT calculations and analysis. Y.K., J.H. and R.R.R. performed the in situ surface-enhanced FT–IR spectroscopy measurements. I.E.L.S. and I.C. participated in the discussion and interpretation of experimental and theoretical data. Y.S.H. and R.R.R. wrote the manuscript. All of the authors discussed the results and commented on the manuscript.

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Correspondence to Reshma R. Rao or Yang Shao-Horn.

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Supplemental Information

Supplementary Notes 1–9, Figs. 1–35 and Tables 1–24.

Supplementary Data 1

Surface structures from DFT calculations

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Rao, R.R., Kolb, M.J., Giordano, L. et al. Operando identification of site-dependent water oxidation activity on ruthenium dioxide single-crystal surfaces. Nat Catal 3, 516–525 (2020). https://doi.org/10.1038/s41929-020-0457-6

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