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

Title: Using “Tender” x-ray ambient pressure x-Ray photoelectron spectroscopy as a direct probe of solid-liquid interface

Abstract

We report a new method to probe the solid-liquid interface through the use of a thin liquid layer on a solid surface. An ambient pressure XPS (AP-XPS) endstation that is capable of detecting high kinetic energy photoelectrons (7 keV) at a pressure up to 110 Torr has been constructed and commissioned. Additionally, we have deployed a “dip & pull” method to create a stable nanometers-thick aqueous electrolyte on platinum working electrode surface. Combining the newly constructed AP-XPS system, “dip & pull” approach, with a “tender” X-ray synchrotron source (2 keV–7 keV), we are able to access the interface between liquid and solid dense phases with photoelectrons and directly probe important phenomena occurring at the narrow solid-liquid interface region in an electrochemical system. Using this approach, we have performed electrochemical oxidation of the Pt electrode at an oxygen evolution reaction (OER) potential. Under this potential, we observe the formation of both Pt²⁺ and Pt⁴⁺ interfacial species on the Pt working electrode in situ. We believe this thin-film approach and the use of “tender” AP-XPS highlighted in this study is an innovative new approach to probe this key solid-liquid interface region of electrochemistry.

Authors:
 [1];  [1];  [2];  [1];  [2];  [3];  [3];  [3];  [3];  [1];  [1];  [4]
  1. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
  2. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Chinese Academy of Sciences, Shanghai (Republic of China)
  3. VG Scienta,Uppsala (Sweden)
  4. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Chinese Academy of Sciences, Shanghai (Republic of China); Shanghai Tech Univ., Shanghai (China)
Publication Date:
Research Org.:
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
1187106
Grant/Contract Number:  
AC02-05CH11231
Resource Type:
Accepted Manuscript
Journal Name:
Scientific Reports
Additional Journal Information:
Journal Volume: 5; Journal Issue: 5; Journal ID: ISSN 2045-2322
Publisher:
Nature Publishing Group
Country of Publication:
United States
Language:
English
Subject:
25 ENERGY STORAGE; batteries; surface spectroscopy; electrocatalysis

Citation Formats

Axnanda, Stephanus, Crumlin, Ethan J., Mao, Baohua, Rani, Sana, Chang, Rui, Karlsson, Patrik G., Edwards, Mårten O. M., Lundqvist, Måns, Moberg, Robert, Ross, Phil, Hussain, Zahid, and Liu, Zhi. Using “Tender” x-ray ambient pressure x-Ray photoelectron spectroscopy as a direct probe of solid-liquid interface. United States: N. p., 2015. Web. doi:10.1038/srep09788.
Axnanda, Stephanus, Crumlin, Ethan J., Mao, Baohua, Rani, Sana, Chang, Rui, Karlsson, Patrik G., Edwards, Mårten O. M., Lundqvist, Måns, Moberg, Robert, Ross, Phil, Hussain, Zahid, & Liu, Zhi. Using “Tender” x-ray ambient pressure x-Ray photoelectron spectroscopy as a direct probe of solid-liquid interface. United States. doi:10.1038/srep09788.
Axnanda, Stephanus, Crumlin, Ethan J., Mao, Baohua, Rani, Sana, Chang, Rui, Karlsson, Patrik G., Edwards, Mårten O. M., Lundqvist, Måns, Moberg, Robert, Ross, Phil, Hussain, Zahid, and Liu, Zhi. Thu . "Using “Tender” x-ray ambient pressure x-Ray photoelectron spectroscopy as a direct probe of solid-liquid interface". United States. doi:10.1038/srep09788. https://www.osti.gov/servlets/purl/1187106.
@article{osti_1187106,
title = {Using “Tender” x-ray ambient pressure x-Ray photoelectron spectroscopy as a direct probe of solid-liquid interface},
author = {Axnanda, Stephanus and Crumlin, Ethan J. and Mao, Baohua and Rani, Sana and Chang, Rui and Karlsson, Patrik G. and Edwards, Mårten O. M. and Lundqvist, Måns and Moberg, Robert and Ross, Phil and Hussain, Zahid and Liu, Zhi},
abstractNote = {We report a new method to probe the solid-liquid interface through the use of a thin liquid layer on a solid surface. An ambient pressure XPS (AP-XPS) endstation that is capable of detecting high kinetic energy photoelectrons (7 keV) at a pressure up to 110 Torr has been constructed and commissioned. Additionally, we have deployed a “dip & pull” method to create a stable nanometers-thick aqueous electrolyte on platinum working electrode surface. Combining the newly constructed AP-XPS system, “dip & pull” approach, with a “tender” X-ray synchrotron source (2 keV–7 keV), we are able to access the interface between liquid and solid dense phases with photoelectrons and directly probe important phenomena occurring at the narrow solid-liquid interface region in an electrochemical system. Using this approach, we have performed electrochemical oxidation of the Pt electrode at an oxygen evolution reaction (OER) potential. Under this potential, we observe the formation of both Pt²⁺ and Pt⁴⁺ interfacial species on the Pt working electrode in situ. We believe this thin-film approach and the use of “tender” AP-XPS highlighted in this study is an innovative new approach to probe this key solid-liquid interface region of electrochemistry.},
doi = {10.1038/srep09788},
journal = {Scientific Reports},
number = 5,
volume = 5,
place = {United States},
year = {2015},
month = {5}
}

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

Citation Metrics:
Cited by: 59 works
Citation information provided by
Web of Science

Save / Share:

Works referenced in this record:

Photoelectron spectroscopy under ambient pressure and temperature conditions
journal, March 2009

  • Frank Ogletree, D.; Bluhm, Hendrik; Hebenstreit, Eleonore D.
  • Nuclear Instruments and Methods in Physics Research Section A: Accelerators, Spectrometers, Detectors and Associated Equipment, Vol. 601, Issue 1-2
  • DOI: 10.1016/j.nima.2008.12.155

In situ investigation of electrochemical devices using ambient pressure photoelectron spectroscopy
journal, October 2013

  • Crumlin, Ethan J.; Bluhm, Hendrik; Liu, Zhi
  • Journal of Electron Spectroscopy and Related Phenomena, Vol. 190
  • DOI: 10.1016/j.elspec.2013.03.002

Electronic Effects in the Electric Double Layer
journal, January 1996


Ultra-high vacuum techniques in the study of single-crystal electrode surfaces
journal, April 1992


Atomic subshell photoionization cross sections and asymmetry parameters: 1 ⩽ Z ⩽ 103
journal, January 1985


Influence of Hydrocarbon and CO 2 on the Reversibility of Li–O 2 Chemistry Using In Situ Ambient Pressure X-ray Photoelectron Spectroscopy
journal, December 2013

  • Lu, Yi-Chun; Crumlin, Ethan J.; Carney, Thomas J.
  • The Journal of Physical Chemistry C, Vol. 117, Issue 49
  • DOI: 10.1021/jp409453s

A differentially pumped electrostatic lens system for photoemission studies in the millibar range
journal, November 2002

  • Ogletree, D. Frank; Bluhm, Hendrik; Lebedev, Gennadi
  • Review of Scientific Instruments, Vol. 73, Issue 11
  • DOI: 10.1063/1.1512336

An ESCA study on emersed electrodes
journal, July 1980

  • Hansen, W. N.; Kolb, D. M.; Rath, D. L.
  • Journal of Electroanalytical Chemistry and Interfacial Electrochemistry, Vol. 110, Issue 1-3
  • DOI: 10.1016/S0022-0728(80)80391-3

Multielement Activity Mapping and Potential Mapping in Solid Oxide Electrochemical Cells through the use of operando XPS
journal, September 2012

  • Zhang, Chunjuan; Grass, Michael E.; Yu, Yi
  • ACS Catalysis, Vol. 2, Issue 11
  • DOI: 10.1021/cs3004243

In Situ Characterization of Ceria Oxidation States in High-Temperature Electrochemical Cells with Ambient Pressure XPS
journal, November 2010

  • DeCaluwe, Steven C.; Grass, Michael E.; Zhang, Chunjuan
  • The Journal of Physical Chemistry C, Vol. 114, Issue 46
  • DOI: 10.1021/jp107694z

Reaction-Driven Restructuring of Rh-Pd and Pt-Pd Core-Shell Nanoparticles
journal, November 2008


Mechanistic Studies of Water Electrolysis and Hydrogen Electro-Oxidation on High Temperature Ceria-Based Solid Oxide Electrochemical Cells
journal, July 2013

  • Zhang, Chunjuan; Yu, Yi; Grass, Michael E.
  • Journal of the American Chemical Society, Vol. 135, Issue 31
  • DOI: 10.1021/ja402604u

Methanol Oxidation on a Copper Catalyst Investigated Using in Situ X-ray Photoelectron Spectroscopy
journal, September 2004

  • Bluhm, Hendrik; Hävecker, Michael; Knop-Gericke, Axel
  • The Journal of Physical Chemistry B, Vol. 108, Issue 38
  • DOI: 10.1021/jp040080j

Electron transport in solids for quantitative surface analysis
journal, January 2001

  • Werner, Wolfgang S. M.
  • Surface and Interface Analysis, Vol. 31, Issue 3
  • DOI: 10.1002/sia.973

Break-Up of Stepped Platinum Catalyst Surfaces by High CO Coverage
journal, February 2010


Ambient pressure photoelectron spectroscopy: A new tool for surface science and nanotechnology
journal, April 2008


Electron spectroscopy of platinum-oxygen surfaces and application to electrochemical studies
journal, November 1971

  • Kim, K. S.; Winograd, N.; Davis, R. E.
  • Journal of the American Chemical Society, Vol. 93, Issue 23
  • DOI: 10.1021/ja00752a065

In situ x-ray photoelectron spectroscopy studies of water on metals and oxides at ambient conditions
journal, April 2008


In situ x-ray photoelectron spectroscopy for electrochemical reactions in ordinary solvents
journal, September 2013

  • Masuda, Takuya; Yoshikawa, Hideki; Noguchi, Hidenori
  • Applied Physics Letters, Vol. 103, Issue 11
  • DOI: 10.1063/1.4821180

Observation of systematic electrochemically induced binding energy shift in the XPS spectra of emersed Cs+ double layer species
journal, January 1986


In situ study of an oxidation reaction on a Pt/C electrode by ambient pressure hard X-ray photoelectron spectroscopy
journal, September 2014

  • Takagi, Yasumasa; Wang, Heng; Uemura, Yohei
  • Applied Physics Letters, Vol. 105, Issue 13
  • DOI: 10.1063/1.4897007

UHV Techniques in the Study of Electrode Surfaces
journal, January 1987


Electron spectroscopy for chemical analysis of liquids and solutions
journal, March 1985


ESCA study of sputtered platinum films
journal, March 1975

  • Bancroft, G. Michael.; Adams, Ian.; Coatsworth, Leighton L.
  • Analytical Chemistry, Vol. 47, Issue 3
  • DOI: 10.1021/ac60353a050

Measuring individual overpotentials in an operating solid-oxide electrochemical cell
journal, January 2010

  • El Gabaly, Farid; Grass, Michael; McDaniel, Anthony H.
  • Physical Chemistry Chemical Physics, Vol. 12, Issue 38
  • DOI: 10.1039/c003581e

A few selected applications of surface nonlinear optical spectroscopy.
journal, October 1996


Effect of pretreatment on a platinized tin oxide catalyst used for low-temperature Co oxidation
journal, July 1990

  • Drawdy, Jean E.; Hoflund, Gar B.; Gardner, Steven D.
  • Surface and Interface Analysis, Vol. 16, Issue 1-12
  • DOI: 10.1002/sia.740160178

Quantitative electron spectroscopy of surfaces: A standard data base for electron inelastic mean free paths in solids
journal, February 1979


In Situ Study of the Gas-Phase Electrolysis of Water on Platinum by NAP-XPS
journal, September 2013

  • Arrigo, Rosa; Hävecker, Michael; Schuster, Manfred E.
  • Angewandte Chemie International Edition, Vol. 52, Issue 44
  • DOI: 10.1002/anie.201304765

Investigation of solid/vapor interfaces using ambient pressure X-ray photoelectron spectroscopy
journal, January 2013

  • Starr, D. E.; Liu, Z.; Hävecker, M.
  • Chemical Society Reviews, Vol. 42, Issue 13
  • DOI: 10.1039/c3cs60057b

Measure of Surface Potential at the Aqueous–Oxide Nanoparticle Interface by XPS from a Liquid Microjet
journal, October 2013

  • Brown, Matthew A.; Beloqui Redondo, Amaia; Sterrer, Martin
  • Nano Letters, Vol. 13, Issue 11
  • DOI: 10.1021/nl402957y

Kinetics of CO oxidation on high-concentration phases of atomic oxygen on Pt(111)
journal, December 2005

  • Gerrard, Alex L.; Weaver, Jason F.
  • The Journal of Chemical Physics, Vol. 123, Issue 22
  • DOI: 10.1063/1.2126667

A Reactive Oxide Overlayer on Rhodium Nanoparticles during CO Oxidation and Its Size Dependence Studied by In Situ Ambient-Pressure X-ray Photoelectron Spectroscopy
journal, November 2008

  • Grass, Michael E.; Zhang, Yawen; Butcher, Derek R.
  • Angewandte Chemie International Edition, Vol. 47, Issue 46
  • DOI: 10.1002/anie.200803574

Surface science studies of model fuel cell electrocatalysts
journal, April 2002


Surface Chemistry of Late Transition Metal Oxides
journal, December 2012


Different Reactivity of the Various Platinum Oxides and Chemisorbed Oxygen in CO Oxidation on Pt(111)
journal, April 2014

  • Miller, Daniel; Sanchez Casalongue, Hernan; Bluhm, Hendrik
  • Journal of the American Chemical Society, Vol. 136, Issue 17
  • DOI: 10.1021/ja413125q

In Situ Oxidation Study of Pt(110) and Its Interaction with CO
journal, December 2011

  • Butcher, Derek R.; Grass, Michael E.; Zeng, Zhenhua
  • Journal of the American Chemical Society, Vol. 133, Issue 50
  • DOI: 10.1021/ja207261s

Oxidation of Pt(111) under Near-Ambient Conditions
journal, November 2011


Measuring fundamental properties in operating solid oxide electrochemical cells by using in situ X-ray photoelectron spectroscopy
journal, September 2010

  • Zhang, Chunjuan; Grass, Michael E.; McDaniel, Anthony H.
  • Nature Materials, Vol. 9, Issue 11
  • DOI: 10.1038/nmat2851

In Situ Characterizations of Nanostructured SnO x /Pt(111) Surfaces Using Ambient-Pressure XPS (APXPS) and High-Pressure Scanning Tunneling Microscopy (HPSTM)
journal, January 2014

  • Axnanda, Stephanus; Zhu, Zhongwei; Zhou, Weiping
  • The Journal of Physical Chemistry C, Vol. 118, Issue 4
  • DOI: 10.1021/jp409272j

Ellipsometric Study of Oxygen‐Containing Films on Platinum Anodes
journal, January 1968

  • Reddy, A. K. N.; Genshaw, M. A.; Bockris, J. O'M.
  • The Journal of Chemical Physics, Vol. 48, Issue 2
  • DOI: 10.1063/1.1668699

Importance of the Metal-Oxide Interface in Catalysis: In Situ Studies of the Water-Gas Shift Reaction by Ambient-Pressure X-ray Photoelectron Spectroscopy
journal, April 2013

  • Mudiyanselage, Kumudu; Senanayake, Sanjaya D.; Feria, Leticia
  • Angewandte Chemie International Edition, Vol. 52, Issue 19
  • DOI: 10.1002/anie.201210077

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


An analytical SEM and XPS study of platinum-rhodium gauzes used in high pressure ammonia burners
journal, October 1988

  • Fierro, J. L. G.; Palacios, J. M.; Tomas, F.
  • Surface and Interface Analysis, Vol. 13, Issue 1
  • DOI: 10.1002/sia.740130107

New ambient pressure photoemission endstation at Advanced Light Source beamline 9.3.2
journal, May 2010

  • Grass, Michael E.; Karlsson, Patrik G.; Aksoy, Funda
  • Review of Scientific Instruments, Vol. 81, Issue 5
  • DOI: 10.1063/1.3427218

An ESCA Study on the Electrochemical Double Layer of Emersed Electrodes
journal, December 1983

  • Kolb, P. M.; Rath, D. L.; Wille, R.
  • Berichte der Bunsengesellschaft für physikalische Chemie, Vol. 87, Issue 12
  • DOI: 10.1002/bbpc.19830871206

Influence of the Local Surface Structure on the 5 p Photoemission of Adsorbed Xenon
journal, September 1979


Simulation of electron spectra for surface analysis (SESSA): a novel software tool for quantitative Auger-electron spectroscopy and X-ray photoelectron spectroscopy
journal, January 2005

  • Smekal, Werner; Werner, Wolfgang S. M.; Powell, Cedric J.
  • Surface and Interface Analysis, Vol. 37, Issue 11
  • DOI: 10.1002/sia.2097

In Situ Ambient Pressure X-ray Photoelectron Spectroscopy Studies of Lithium-Oxygen Redox Reactions
journal, October 2012

  • Lu, Yi-Chun; Crumlin, Ethan J.; Veith, Gabriel M.
  • Scientific Reports, Vol. 2, Issue 1
  • DOI: 10.1038/srep00715

    Works referencing / citing this record:

    Water-mediated photo-induced reduction of platinum films
    journal, June 2019

    • Fraxedas, Jordi; Zhang, Kuan; Sepúlveda, Borja
    • Journal of Synchrotron Radiation, Vol. 26, Issue 4
    • DOI: 10.1107/s1600577519004685