Abstract
A method combining cyclic voltammetry (CV) with x-ray absorption fine structure (XAFS) spectroscopy, viz. CV-XAFS, has been developed to enable in situ real-time investigation of atomic and electronic structures related to electrochemical reactions. We use this method to study the reaction of a Pt/C cathode catalyst in the oxygen reduction reaction (ORR) in an alkaline electrolyte, using x-ray energies near the Pt LIII edge for XAFS measurements. It was found that the current induced by the ORR was first observed at approximately 0.08 V versus Hg/HgO, although the Pt valence, which is reflected in the oxidation states, remained almost unchanged. The electronic structure of the catalytic surface in the ORR was observed to be different in the negative and positive scan directions of CV measurements. Hydrogen adsorption is also discussed on the basis of the observation of this spectral change. We have demonstrated that CV-XAFS provides dynamical structural and electronic information related to electrochemical reactions and can be used for in situ real-time measurements of a catalyst.
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References
N.M. Marković, H.A. Gasteiger, and P.N. Ross Jr., J. Phys. Chem. 100, 6715 (1996).
A.J. Bard and L.R. Faulkner, Electrochemical Methods: Fundamentals and Applications, 2nd ed. (New York: Wiley, 2001).
N.M. Marković and P.N. Ross Jr., Surf. Sci. Rep. 45, 117 (2002).
W. Jin, H. Du, S. Zheng, H. Xu, and Y. Zheng, J. Phys. Chem. B 114, 6542 (2010).
E.J. Coleman, M.H. Chowdhury, and A.C. Co, ACS Catal. 5, 1245 (2015).
L.R. Merte, F. Behafarid, D.J. Miller, D. Friebel, S. Cho, F. Mbuga, D. Sokaras, R. Alonso-Mori, T. Weng, D. Nordlund, A. Nilsson, and B.R. Cuenya, ACS Catal. 2, 2371 (2012).
S. Nagamatsu, T. Arai, M. Yamamoto, T. Ohkura, H. Oyanagi, T. Ishizaka, H. Kawanami, T. Uruga, M. Tada, and Y. Iwasawa, J. Phys. Chem. C 117, 13094 (2013).
T. Masuda, H. Fukumitsu, K. Fugane, H. Togasaki, D. Matsumura, K. Tamura, Y. Nishihata, H. Yoshikawa, K. Kobayashi, T. Mori, and K. Uosaki, J. Phys. Chem. C 116, 10098 (2012).
D.E. Ramaker, A. Korovina, V. Croze, J. Melke, and C. Roth, Phys. Chem. Chem. Phys. 16, 13645 (2014).
T.M. Arruda, B. Shyam, J.M. Ziegelbauer, S. Mukerjee, and D.E. Ramaker, J. Phys. Chem. C 112, 18087 (2008).
S. Kityakarn, T. Saida, A. Sode, N. Ishiguro, O. Sekizawa, T. Uruga, K. Nagasawa, T. Yamamoto, T. Yokoyama, and M. Tada, Top. Catal. 57, 903 (2014).
M. Tada, S. Murata, T. Asakoka, K. Hiroshima, K. Okumura, H. Tanida, T. Uruga, H. Nakanishi, S. Matsumoto, Y. Inada, M. Nomura, and Y. Iwasawa, Angew. Chem. Int. Ed. 46, 4310 (2007).
T. Matsushita and R.P. Phizackerley, Jpn. J. Appl. Phys. 20, 2223 (1981).
U. Kaminaga, T. Matsushita, and K. Kohra, Jpn. J. Appl. Phys. 20, L355 (1981).
Acknowledgements
The present experiment was performed under the approval of Japan Synchrotron Radiation Research Institute (Proposal Nos. 2012B3609, 2013A3610, and 2014A3609). This work was partly supported by JSPS KAKENHI Grant Nos. 2600322, 25790083, and 16K17540.
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Kusano, S., Matsumura, D., Asazawa, K. et al. Study of Catalytic Reaction at Electrode–Electrolyte Interfaces by a CV-XAFS Method. J. Electron. Mater. 46, 3634–3638 (2017). https://doi.org/10.1007/s11664-016-5259-x
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DOI: https://doi.org/10.1007/s11664-016-5259-x