skip to main content
OSTI.GOV 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

Journal Article · · Scientific Reports
DOI:https://doi.org/10.1038/srep09788· OSTI ID:1187106
 [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)

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.

Research Organization:
Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States)
Sponsoring Organization:
USDOE
Grant/Contract Number:
AC02-05CH11231
OSTI ID:
1187106
Journal Information:
Scientific Reports, Vol. 5, Issue 5; ISSN 2045-2322
Publisher:
Nature Publishing GroupCopyright Statement
Country of Publication:
United States
Language:
English
Citation Metrics:
Cited by: 227 works
Citation information provided by
Web of Science

References (56)

Photoelectron spectroscopy under ambient pressure and temperature conditions
  • 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 https://doi.org/10.1016/j.nima.2008.12.155
journal March 2009
In situ investigation of electrochemical devices using ambient pressure photoelectron spectroscopy journal October 2013
Accurate Electron Inelastic Cross Sections and Stopping Powers for Liquid Water over the 0.1-10 keV Range Based on an Improved Dielectric Description of the Bethe Surface journal January 2007
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
A differentially pumped electrostatic lens system for photoemission studies in the millibar range journal November 2002
Formation of Nanometer-Sized Surface Platinum Oxide Clusters on a Stepped Pt(557) Single Crystal Surface Induced by Oxygen: A High-Pressure STM and Ambient-Pressure XPS Study journal February 2012
Multielement Activity Mapping and Potential Mapping in Solid Oxide Electrochemical Cells through the use of operando XPS journal September 2012
In Situ Characterization of Ceria Oxidation States in High-Temperature Electrochemical Cells with Ambient Pressure XPS journal November 2010
Photoelectron Spectroscopy book January 2003
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
Methanol Oxidation on a Copper Catalyst Investigated Using in Situ X-ray Photoelectron Spectroscopy journal September 2004
Electron transport in solids for quantitative surface analysis journal January 2001
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
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
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
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
Measuring individual overpotentials in an operating solid-oxide electrochemical cell journal January 2010
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
Quantitative electron spectroscopy of surfaces: A standard data base for electron inelastic mean free paths in solids journal February 1979
X-ray photoelectron spectroscopy and electron microscopy of Pt$z.sbnd;Rh gauzes used for catalytic oxidation of ammonia journal June 1977
In Situ Study of the Gas-Phase Electrolysis of Water on Platinum by NAP-XPS journal September 2013
Investigation of solid/vapor interfaces using ambient pressure X-ray photoelectron spectroscopy journal January 2013
Measure of Surface Potential at the Aqueous–Oxide Nanoparticle Interface by XPS from a Liquid Microjet journal October 2013
Kinetics of CO oxidation on high-concentration phases of atomic oxygen on Pt(111) journal December 2005
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
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
In Situ Oxidation Study of Pt(110) and Its Interaction with CO journal December 2011
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
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
Ellipsometric Study of Oxygen‐Containing Films on Platinum Anodes journal January 1968
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
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
New ambient pressure photoemission endstation at Advanced Light Source beamline 9.3.2 journal May 2010
An ESCA Study on the Electrochemical Double Layer of Emersed Electrodes journal December 1983
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
In Situ Ambient Pressure X-ray Photoelectron Spectroscopy Studies of Lithium-Oxygen Redox Reactions journal October 2012
Electrochemical Equilibria book January 1973
Observation of systematic electrochemically induced binding energy shift in the XPS spectra of emersed Cs+ double layer species journal January 1986
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
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
Influence of the Local Surface Structure on the 5 p Photoemission of Adsorbed Xenon journal September 1979

Cited By (40)

Electronic Structure Characterization of Soft Semiconductors journal June 2019
NiFe-Based (Oxy)hydroxide Catalysts for Oxygen Evolution Reaction in Non-Acidic Electrolytes journal July 2016
Electrode Architecture in Galvanic and Electrolytic Energy Cells journal March 2016
Ambient Pressure Photoelectron Spectroscopy: Opportunities in Catalysis from Solids to Liquids and Introducing Time Resolution journal January 2018
In‐Situ/Operando X‐ray Characterization of Metal Hydrides journal March 2019
External RBS analysis setup at University of Göttingen: RBS analysis for liquid samples journal February 2018
Single-Atom Electrocatalysts for Water Splitting book January 2020
In Situ Electrochemical Cells to Study the Oxygen Evolution Reaction by Near Ambient Pressure X-ray Photoelectron Spectroscopy journal October 2018
Stabilizing the Meniscus for Operando Characterization of Platinum During the Electrolyte-Consuming Alkaline Oxygen Evolution Reaction journal October 2018
Various spectroelectrochemical cells for in situ observation of electrochemical processes at solid–liquid interfaces journal October 2018
Speciation and Electronic Structure of La1−xSrxCoO3−δ During Oxygen Electrolysis journal October 2018
An APXPS endstation for gas–solid and liquid–solid interface studies at SSRF journal April 2019
Unravelling the electrochemical double layer by direct probing of the solid/liquid interface journal August 2016
Probing a battery electrolyte drop with ambient pressure photoelectron spectroscopy journal July 2019
Multiphase carbon mineralization for the reactive separation of CO2 and directed synthesis of H2 journal January 2020
Frontiers of water oxidation: the quest for true catalysts journal January 2017
Molecular species forming at the α-Fe 2 O 3 nanoparticle–aqueous solution interface journal January 2018
Electronic structure of aqueous-phase anatase titanium dioxide nanoparticles probed by liquid jet photoelectron spectroscopy journal January 2019
2D oxides on metal materials: concepts, status, and perspectives journal January 2019
The effect of grain size on the hydration of BaZr 0.9 Y 0.1 O 3−δ proton conductor studied by ambient pressure X-ray photoelectron spectroscopy journal January 2020
Atmospheric pressure X-ray photoelectron spectroscopy apparatus: Bridging the pressure gap journal May 2016
Advances in liquid phase soft-x-ray photoemission spectroscopy: A new experimental setup at BESSY II journal July 2017
Revealing the formation dynamics of the electric double layer by means of in - situ Rutherford backscattering spectrometry journal August 2019
Restructuring of silica supported vanadia during propane oxidative dehydrogenation studied by combined synchrotron radiation based in situ soft X-ray absorption and photoemission journal March 2017
Ambient pressure photoelectron spectroscopy: Practical considerations and experimental frontiers journal December 2016
The offset droplet: a new methodology for studying the solid/water interface using x-ray photoelectron spectroscopy journal October 2017
Beyond Koopmans’ theorem: electron binding energies in disordered materials journal December 2018
In-depth study of the chemical/electronic structures of two-dimensional molybdenum disulfide materials with sub-micrometer-resolution scanning photoelectron microscopy journal January 2020
Water-mediated photo-induced reduction of platinum films journal June 2019
Perovskites in catalysis and electrocatalysis journal November 2017
A high-pressure x-ray photoelectron spectroscopy instrument for studies of industrially relevant catalytic reactions at pressures of several bars text January 2019
Interface Science Using Ambient Pressure Hard X-ray Photoelectron Spectroscopy journal January 2019
A high-pressure x-ray photoelectron spectroscopy instrument for studies of industrially relevant catalytic reactions at pressures of several bars journal October 2019
Water-mediated photo-induced reduction of platinum films text January 2019
Probing a battery electrolyte drop with ambient pressure photoelectron spectroscopy text January 2019
Restructuring of silica supported vanadia during propane oxidative dehydrogenation studied by combined synchrotron radiation based in situ soft X-ray absorption and photoemission text January 2017
A high-pressure x-ray photoelectron spectroscopy instrument for studies of industrially relevant catalytic reactions at pressures of several bars text January 2019
Restructuring of silica supported vanadia during propane oxidative dehydrogenation studied by combined synchrotron radiation based in situ soft X-ray absorption and photoemission text January 2017
Nanocarbon-Edge-Anchored High-Density Pt Atoms for 3-nitrostyrene Hydrogenation: Strong Metal-Carbon Interaction journal March 2019
The Oxidation of Platinum under Wet Conditions Observed by Electrochemical X-ray Photoelectron Spectroscopy journal March 2019