Topics in Catalysis

, Volume 61, Issue 20, pp 2152–2160 | Cite as

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

  • Kelsey A. Stoerzinger
  • Marco Favaro
  • Philip N. Ross
  • Zahid Hussain
  • Zhi Liu
  • Junko Yano
  • Ethan J. CrumlinEmail author
Original Article


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.


Ambient pressure XPS Electrocatalysis Oxygen evolution reaction Hydrogen evolution reaction Solid/liquid interface stability 



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.

Supplementary material

11244_2018_1063_MOESM1_ESM.pdf (485 kb)
Supplementary material 1 (PDF 485 KB)


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Copyright information

© Springer Science+Business Media, LLC, part of Springer Nature 2018

Authors and Affiliations

  1. 1.Physical and Computational Sciences DirectoratePacific Northwest National LaboratoryRichlandUSA
  2. 2.Advanced Light SourceLawrence Berkeley National LaboratoryBerkeleyUSA
  3. 3.Joint Center for Artificial PhotosynthesisLawrence Berkeley National LaboratoryBerkeleyUSA
  4. 4.Chemical Sciences DivisionLawrence Berkeley National LaboratoryBerkeleyUSA
  5. 5.Materials Sciences DivisionLawrence Berkeley National LaboratoryBerkeleyUSA
  6. 6.Molecular Biophysics and Integrated Bioimaging DivisionLawrence Berkeley National LaboratoryBerkeleyUSA
  7. 7.State Key Laboratory of Functional Materials for Informatics, Shanghai Institute of Microsystem and Information TechnologyChinese Academy of SciencesShanghaiPeople’s Republic of China
  8. 8.Division of Condensed Matter Physics and Photon Science, School of Physical Science and TechnologyShanghaiTech UniversityShanghaiChina
  9. 9.Joint Center for Energy Storage ResearchLawrence Berkeley National LaboratoryBerkeleyUSA
  10. 10.School of Chemical, Biological and Environmental Engineering, Johnson HallOregon State UniversityCorvallisUSA
  11. 11.Helmholtz Zentrum Berlin für Materialien und Energie GmbH, Institute for Solar FuelsBerlinGermany

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