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Stabilizing the Meniscus for Operando Characterization of Platinum During the Electrolyte-Consuming Alkaline Oxygen Evolution Reaction

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Abstract

Achieving a molecular-level understanding of interfacial (photo)electrochemical processes is essential in order to tailor novel and highly-performing catalytic systems. The corresponding recent development of in situ and operando tools has posed new challenges on experimental architectures. In this study, we use ambient pressure X-ray photoelectron spectroscopy (AP-XPS) to probe the solid/liquid electrified interface of a polycrystalline Pt sample in contact with an alkaline electrolyte during hydrogen and oxygen evolution reactions. Using the “dip-and-pull” technique to probe the interface through a thin liquid layer generated on the sample surface, we observe that the electrolyte meniscus becomes unstable under sustained driving of an electrolyte-consuming reaction (such as water oxidation). The addition of an electrochemically inert supporting electrolyte mitigates this issue, maintaining a stable meniscus layer for prolonged reaction times. In contrast, for processes in which the electrolyte is replenished in the reaction pathway (i.e. water reduction in alkaline conditions), we find that the solid/liquid interface remains stable without addition of a secondary supporting electrolyte. The approach described in this work allows the extension of operando AP-XPS capabilities using the “dip-and-pull” method to a broader class of reactions consuming ionic species during complex interfacial faradaic processes.

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References

  1. Reier T, Nong HN, Teschner D, Schlögl R, Strasser P (2017) Electrocatalytic oxygen evolution reaction in acidic environments—reaction mechanisms and catalysts. Adv Energy Mat 7(1):1601275

    Article  Google Scholar 

  2. Cherevko S, Geiger S, Kasian O, Kulyk N, Grote J-P, Savan A, Shrestha BR, Merzlikin S, Breitbach B, Ludwig A, Mayrhofer KJJ (2016) Oxygen and hydrogen evolution reactions on Ru, RuO2, Ir, and IrO2 thin film electrodes in acidic and alkaline electrolytes: a comparative study on activity and stability. Catal Today 262(Supplement C):170–180

    Article  CAS  Google Scholar 

  3. Karlsson RKB, Cornell A (2016) Selectivity between oxygen and chlorine evolution in the chlor-alkali and chlorate processes. Chem Rev 116(5):2982–3028

    Article  CAS  Google Scholar 

  4. Trasatti S (1984) Electrocatalysis in the anodic evolution of oxygen and chlorine. Electrochim Acta 29(11):1503–1512

    Article  CAS  Google Scholar 

  5. Clancy M, Bettles CJ, Stuart A, Birbilis N (2013) The influence of alloying elements on the electrochemistry of lead anodes for electrowinning of metals: a review. Hydrometallurgy 131–132(Supplement C):144–157

    Article  Google Scholar 

  6. Carpenter BK, Harvey JN, Orr-Ewing AJ (2016) The study of reactive intermediates in condensed phases. J Am Chem Soc 138(14):4695–4705

    Article  CAS  Google Scholar 

  7. Crumlin EJ, Liu Z, Bluhm H, Yang W, Guo J, Hussain Z (2015) X-ray spectroscopy of energy materials under in situ/operando conditions. J Electron Spectrosc Relat Phenom 200:264–273

    Article  CAS  Google Scholar 

  8. Kaya S, Ogasawara H, Näslund L-Å, Forsell J-O, Casalongue HS, Miller DJ, Nilsson A (2013) Ambient-pressure photoelectron spectroscopy for heterogeneous catalysis and electrochemistry. Catal Today 205:101–105

    Article  CAS  Google Scholar 

  9. Kornienko N, Resasco J, Becknell N, Jiang C-M, Liu Y-S, Nie K, Sun X, Guo J, Leone SR, Yang P (2015) Operando spectroscopic analysis of an amorphous cobalt sulfide hydrogen evolution electrocatalyst. J Am Chem Soc 137(23):7448–7455

    Article  CAS  Google Scholar 

  10. Ramaker DE, Korovina A, Croze V, Melke J, Roth C (2014) Following ORR intermediates adsorbed on a Pt cathode catalyst during break-in of a PEM fuel cell by in operando X-ray absorption spectroscopy. Phys Chem Chem Phys 16(27):13645–13653

    Article  CAS  Google Scholar 

  11. Schlögl R (2015) Heterogeneous catalysis. Angew Chem Int Ed 54(11):3465–3520

    Article  Google Scholar 

  12. Zandi O, Hamann TW (2016) Determination of photoelectrochemical water oxidation intermediates on haematite electrode surfaces using operando infrared spectroscopy. Nat Chem 8(8):778–783

    Article  CAS  Google Scholar 

  13. Vesborg PCK, Jaramillo TF (2012) Addressing the terawatt challenge: scalability in the supply of chemical elements for renewable energy. RSC Adv 2(21):7933–7947

    Article  CAS  Google Scholar 

  14. Fan J, Qi K, Zhang L, Zhang H, Yu S, Cui X (2017) Engineering Pt/Pd interfacial electronic structures for highly efficient hydrogen evolution and alcohol oxidation. ACS App Mater Interfaces 9(21):18008–18014

    Article  CAS  Google Scholar 

  15. Kavian R, Choi S-I, Park J, Liu T, Peng H-C, Lu N, Wang J, Kim MJ, Xia Y, Lee SW (2016) Pt-Ni octahedral nanocrystals as a class of highly active electrocatalysts toward the hydrogen evolution reaction in an alkaline electrolyte. J Mat Chem A 4(32):12392–12397

    Article  CAS  Google Scholar 

  16. Wang P, Zhang X, Zhang J, Wan S, Guo S, Lu G, Yao J, Huang X (2017) Precise tuning in platinum-nickel/nickel sulfide interface nanowires for synergistic hydrogen evolution catalysis. Nat Comm 8:14580

    Article  CAS  Google Scholar 

  17. Fadley CS (2010) X-ray photoelectron spectroscopy: progress and perspectives. J Electron Spectrosc Relat Phenom 178–179(Supplement C):2–32

    Article  Google Scholar 

  18. Stoerzinger KA, Hong WT, Crumlin EJ, Bluhm H, Shao-Horn Y (2015) Insights into electrochemical reactions from ambient pressure photoelectron spectroscopy. Acc Chem Res 48(11):2976–2983

    Article  CAS  Google Scholar 

  19. Axnanda S, Crumlin EJ, Mao B, Rani S, Chang R, Karlsson PG, Edwards MOM, Lundqvist M, Moberg R, Ross P, Hussain Z, Liu Z (2015) Using “tender” X-ray ambient pressure X-ray photoelectron spectroscopy as a direct probe of solid-liquid interface. Sci Rep 5:9788

    Article  CAS  Google Scholar 

  20. Favaro M, Jeong B, Ross PN, Yano J, Hussain Z, Liu Z, Crumlin EJ (2016) Unravelling the electrochemical double layer by direct probing of the solid/liquid interface. Nat Commun 7:12695

    Article  CAS  Google Scholar 

  21. Lewerenz H-J, Lichterman MF, Richter MH, Crumlin EJ, Hu S, Axnanda S, Favaro M, Drisdell W, Hussain Z, Brunschwig BS, Liu Z, Nilsson A, Bell AT, Lewis NS, Friebel D (2016) Operando analyses of solar fuels light absorbers and catalysts. Electrochim Acta 211(Supplement C):711–719

    Article  CAS  Google Scholar 

  22. Favaro M, Valero-Vidal C, Eichhorn J, Toma FM, Ross PN, Yano J, Liu Z, Crumlin EJ (2017) Elucidating the alkaline oxygen evolution reaction mechanism on platinum. J Mat Chem A 5(23):11634–11643

    Article  CAS  Google Scholar 

  23. Stoerzinger KA, Favaro M, Ross PN, Yang J, Liu Z, Hussain Z, Crumlin EJ (2017) Probing the surface of platinum during the hydrogen evolution reaction in alkaline electrolyte. J Phys Chem B 112(2):864–870

    Article  Google Scholar 

  24. Santos DMF, Sequeira CAC, Figueiredo JL (2013) Hydrogen production by alkaline water electrolysis. Quim Nova 36:1176–1193

    Article  CAS  Google Scholar 

  25. Esposito DV (2017) Membraneless electrolyzers for low-cost hydrogen production in a renewable energy future. Joule. https://doi.org/10.1016/j.joule.2017.07.003

    Article  Google Scholar 

  26. Eilert A, Cavalca F, Roberts FS, Osterwalder J, Liu C, Favaro M, Crumlin EJ, Ogasawara H, Friebel D, Pettersson LGM, Nilsson A (2017) Subsurface oxygen in oxide-derived copper electrocatalysts for carbon dioxide reduction. J Phys Chem Lett 8(1):285–290

    Article  CAS  Google Scholar 

  27. Lichterman MF, Hu S, Richter MH, Crumlin EJ, Axnanda S, Favaro M, Drisdell W, Hussain Z, Mayer T, Brunschwig BS, Lewis NS, Liu Z, Lewerenz H-J (2015) Direct observation of the energetics at a semiconductor/liquid junction by operando X-ray photoelectron spectroscopy. Energy Environ Sci 8(8):2409–2416

    Article  CAS  Google Scholar 

  28. Haar L, Gallagher JS, Kell GS (eds) (1984) NBS/NRC steam tables. Hemisphere Publishing Corp., New York

    Google Scholar 

  29. Diéguez PM, Ursúa A, Sanchis P, Sopena C, Guelbenzu E, Gandía LM (2008) Thermal performance of a commercial alkaline water electrolyzer: experimental study and mathematical modeling. Int J Hydrog Energy 33(24):7338–7354

    Article  Google Scholar 

  30. McCrory CCL, Jung S, Peters JC, Jaramillo TF (2013) Benchmarking heterogeneous electrocatalysts for the oxygen evolution reaction. J Am Chem Soc 135(45):16977–16987

    Article  CAS  Google Scholar 

  31. Villullas HM, Lopez Teijelo M (1996) Meniscus shape and lateral wetting at the hanging meniscus rotating disc (HMRD) electrode. J Appl Electrochem 26(3):353–359

    Article  CAS  Google Scholar 

  32. Ali-Löytty H, Louie MW, Singh MR, Li L, Sanchez Casalongue HG, Ogasawara H, Crumlin EJ, Liu Z, Bell AT, Nilsson A, Friebel D (2016) Ambient-pressure XPS study of a Ni–Fe electrocatalyst for the oxygen evolution reaction. J Phys Chem C 120(4):2247–2253

    Article  Google Scholar 

  33. Favaro M, Abdi FF, Lamers M, Crumlin EJ, Liu Z, van de Krol R, Starr DE (2017) Light-induced surface reactions at the bismuth vanadate/potassium phosphate interface. J Phys Chem B. https://doi.org/10.1021/acs.jpcb.7b06942

    Article  PubMed  Google Scholar 

  34. Dickinson EJF, Limon-Petersen JG, Rees NV, Compton RG (2009) How much supporting electrolyte is required to make a cyclic voltammetry experiment quantitatively “diffusional”? A theoretical and experimental investigation. J Phys Chem C 113(25):11157–11171

    Article  CAS  Google Scholar 

  35. Hwang I, Ahn E, Tak Y (2014) Effect of flouride ions on oxygen reduction and evolution reaction at α-MnO2 cathode. Int J Electrochem Sci 9(10):5454–5466

    Google Scholar 

  36. Soriaga MP, Chia VKF, White JH, Song D, Hubbard AT (1984) The orientation and electrochemical oxidation of hydroquinone chemisorbed on platinum electrodes in various weakly surface-active supporting electrolytes. J Electroanal Chem Interfacial Electrochem 162(1):143–152

    CAS  Google Scholar 

  37. Garcia-Araez N, Climent V, Herrero E, Feliu J, Lipkowski J (2005) Thermodynamic studies of chloride adsorption at the Pt(111) electrode surface from 0.1 M HClO4 solution. J Electroanal Chem 576(1):33–41

    Article  CAS  Google Scholar 

Download references

Acknowledgements

This work was partially supported through the Office of Science, Office of Basic Energy Science (BES), of the U.S. Department of Energy (DOE) under award no. DE-SC0004993 to the Joint Center for Artificial Photosynthesis (JCAP), a DOE Energy Innovation Hub. The Advanced Light Source is supported by the Director, Office of Science, Office of Basic Energy Sciences, of the U.S. DOE under Contract No. DE-AC02-05CH11231. K.A.S. gratefully acknowledges support from the Linus Pauling Distinguished Post-Doctoral Fellowship Pacific Northwest National Laboratory (PNNL, Laboratory Directed Research and Development Program 69319). PNNL is a multiprogram national laboratory operated for DOE by Battelle.

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Correspondence to Ethan J. Crumlin.

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Stoerzinger, K.A., Favaro, M., Ross, P.N. et al. Stabilizing the Meniscus for Operando Characterization of Platinum During the Electrolyte-Consuming Alkaline Oxygen Evolution Reaction. Top Catal 61, 2152–2160 (2018). https://doi.org/10.1007/s11244-018-1063-6

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