skip to main content
OSTI.GOV title logo U.S. Department of Energy
Office of Scientific and Technical Information

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

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.

Authors:
ORCiD logo [1]; ORCiD logo [1];  [1];  [1];  [2];  [1]; ORCiD logo [1]
  1. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
  2. Chinese Academy of Sciences (CAS), Beijing (China); Shanghai Tech Univ., Shanghai (China)
Publication Date:
Research Org.:
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
Sponsoring Org.:
USDOE Office of Science (SC)
OSTI Identifier:
1580347
Grant/Contract Number:  
AC02-05CH11231
Resource Type:
Journal Article: Accepted Manuscript
Journal Name:
Topics in Catalysis
Additional Journal Information:
Journal Volume: 61; Journal Issue: 20; Journal ID: ISSN 1022-5528
Publisher:
Springer
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; Ambient pressure XPS; Electrocatalysis; Oxygen evolution reaction; Hydrogen evolution reaction; Solid/liquid interface stability

Citation Formats

Stoerzinger, Kelsey A., Favaro, Marco, Ross, Philip N., Hussain, Zahid, Liu, Zhi, Yano, Junko, and Crumlin, Ethan J. Stabilizing the Meniscus for Operando Characterization of Platinum During the Electrolyte-Consuming Alkaline Oxygen Evolution Reaction. United States: N. p., 2018. Web. doi:10.1007/s11244-018-1063-6.
Stoerzinger, Kelsey A., Favaro, Marco, Ross, Philip N., Hussain, Zahid, Liu, Zhi, Yano, Junko, & Crumlin, Ethan J. Stabilizing the Meniscus for Operando Characterization of Platinum During the Electrolyte-Consuming Alkaline Oxygen Evolution Reaction. United States. https://doi.org/10.1007/s11244-018-1063-6
Stoerzinger, Kelsey A., Favaro, Marco, Ross, Philip N., Hussain, Zahid, Liu, Zhi, Yano, Junko, and Crumlin, Ethan J. Tue . "Stabilizing the Meniscus for Operando Characterization of Platinum During the Electrolyte-Consuming Alkaline Oxygen Evolution Reaction". United States. https://doi.org/10.1007/s11244-018-1063-6. https://www.osti.gov/servlets/purl/1580347.
@article{osti_1580347,
title = {Stabilizing the Meniscus for Operando Characterization of Platinum During the Electrolyte-Consuming Alkaline Oxygen Evolution Reaction},
author = {Stoerzinger, Kelsey A. and Favaro, Marco and Ross, Philip N. and Hussain, Zahid and Liu, Zhi and Yano, Junko and Crumlin, Ethan J.},
abstractNote = {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.},
doi = {10.1007/s11244-018-1063-6},
url = {https://www.osti.gov/biblio/1580347}, journal = {Topics in Catalysis},
issn = {1022-5528},
number = 20,
volume = 61,
place = {United States},
year = {2018},
month = {10}
}

Journal Article:
Free Publicly Available Full Text
Publisher's Version of Record

Citation Metrics:
Cited by: 4 works
Citation information provided by
Web of Science

Save / Share:

Works referenced in this record:

How Much Supporting Electrolyte Is Required to Make a Cyclic Voltammetry Experiment Quantitatively “Diffusional”? A Theoretical and Experimental Investigation
journal, June 2009


Addressing the terawatt challenge: scalability in the supply of chemical elements for renewable energy
journal, January 2012


Thermal performance of a commercial alkaline water electrolyzer: Experimental study and mathematical modeling
journal, December 2008


Probing the Surface of Platinum during the Hydrogen Evolution Reaction in Alkaline Electrolyte
journal, November 2017


Unravelling the electrochemical double layer by direct probing of the solid/liquid interface
journal, August 2016


Elucidating the alkaline oxygen evolution reaction mechanism on platinum
journal, January 2017


Thermodynamic studies of chloride adsorption at the Pt(111) electrode surface from 0.1 M HClO4 solution
journal, February 2005


Operando Analyses of Solar Fuels Light Absorbers and Catalysts
journal, September 2016


Operando Spectroscopic Analysis of an Amorphous Cobalt Sulfide Hydrogen Evolution Electrocatalyst
journal, June 2015


X-ray photoelectron spectroscopy: Progress and perspectives
journal, May 2010


Engineering Pt/Pd Interfacial Electronic Structures for Highly Efficient Hydrogen Evolution and Alcohol Oxidation
journal, May 2017


Ambient-Pressure XPS Study of a Ni–Fe Electrocatalyst for the Oxygen Evolution Reaction
journal, January 2016


The Study of Reactive Intermediates in Condensed Phases
journal, March 2016


Benchmarking Heterogeneous Electrocatalysts for the Oxygen Evolution Reaction
journal, October 2013


X-ray spectroscopy of energy materials under in situ/operando conditions
journal, April 2015


Light-Induced Surface Reactions at the Bismuth Vanadate/Potassium Phosphate Interface
journal, September 2017


Electrocatalytic Oxygen Evolution Reaction in Acidic Environments - Reaction Mechanisms and Catalysts
journal, October 2016


Meniscus shape and lateral wetting at the hanging meniscus rotating disc (HMRD) electrode
journal, March 1996


Ambient-pressure photoelectron spectroscopy for heterogeneous catalysis and electrochemistry
journal, April 2013


Precise tuning in platinum-nickel/nickel sulfide interface nanowires for synergistic hydrogen evolution catalysis
journal, February 2017


Hydrogen production by alkaline water electrolysis
journal, January 2013


Using “Tender” X-ray Ambient Pressure X-Ray Photoelectron Spectroscopy as A Direct Probe of Solid-Liquid Interface
journal, May 2015


Electrocatalysis in the anodic evolution of oxygen and chlorine
journal, November 1984


Heterogeneous Catalysis
journal, February 2015


Pt–Ni octahedral nanocrystals as a class of highly active electrocatalysts toward the hydrogen evolution reaction in an alkaline electrolyte
journal, January 2016


Direct observation of the energetics at a semiconductor/liquid junction by operando X-ray photoelectron spectroscopy
journal, January 2015


Insights into Electrochemical Reactions from Ambient Pressure Photoelectron Spectroscopy
journal, August 2015


Selectivity between Oxygen and Chlorine Evolution in the Chlor-Alkali and Chlorate Processes
journal, February 2016


Subsurface Oxygen in Oxide-Derived Copper Electrocatalysts for Carbon Dioxide Reduction
journal, December 2016


    Works referencing / citing this record:

    Interface Science Using Ambient Pressure Hard X-ray Photoelectron Spectroscopy
    journal, January 2019