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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 Laboratory (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. https://doi.org/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. https://doi.org/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 = {Thu May 07 00:00:00 EDT 2015},
month = {Thu May 07 00:00:00 EDT 2015}
}

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Different Reactivity of the Various Platinum Oxides and Chemisorbed Oxygen in CO Oxidation on Pt(111)
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Influence of Hydrocarbon and CO 2 on the Reversibility of Li–O 2 Chemistry Using In Situ Ambient Pressure X-ray Photoelectron Spectroscopy
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  • Lu, Yi-Chun; Crumlin, Ethan J.; Carney, Thomas J.
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Measure of Surface Potential at the Aqueous–Oxide Nanoparticle Interface by XPS from a Liquid Microjet
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Measuring fundamental properties in operating solid oxide electrochemical cells by using in situ X-ray photoelectron spectroscopy
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Investigation of solid/vapor interfaces using ambient pressure X-ray photoelectron spectroscopy
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Ellipsometric Study of Oxygen‐Containing Films on Platinum Anodes
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Kinetics of CO oxidation on high-concentration phases of atomic oxygen on Pt(111)
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  • Gerrard, Alex L.; Weaver, Jason F.
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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

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

  • Masuda, Takuya; Yoshikawa, Hideki; Noguchi, Hidenori
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  • DOI: 10.1063/1.4821180

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

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  • Applied Physics Letters, Vol. 105, Issue 13
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  • Ali, Hebatallah; Seidel, Robert; Pohl, Marvin N.
  • Chemical Science, Vol. 9, Issue 19
  • DOI: 10.1039/c7sc05156e

Electronic structure of aqueous-phase anatase titanium dioxide nanoparticles probed by liquid jet photoelectron spectroscopy
journal, January 2019

  • Ali, Hebatallah; Seidel, Robert; Bergmann, Arno
  • Journal of Materials Chemistry A, Vol. 7, Issue 12
  • DOI: 10.1039/c8ta09414d

2D oxides on metal materials: concepts, status, and perspectives
journal, January 2019

  • Barcaro, Giovanni; Fortunelli, Alessandro
  • Physical Chemistry Chemical Physics, Vol. 21, Issue 22
  • DOI: 10.1039/c9cp00972h

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

  • Jarry, Angelique; Jackson, Gregory S.; Crumlin, Ethan J.
  • Physical Chemistry Chemical Physics, Vol. 22, Issue 1
  • DOI: 10.1039/c9cp04335g

Atmospheric pressure X-ray photoelectron spectroscopy apparatus: Bridging the pressure gap
journal, May 2016

  • Velasco-Vélez, J. J.; Pfeifer, V.; Hävecker, M.
  • Review of Scientific Instruments, Vol. 87, Issue 5
  • DOI: 10.1063/1.4951724

Advances in liquid phase soft-x-ray photoemission spectroscopy: A new experimental setup at BESSY II
journal, July 2017

  • Seidel, Robert; Pohl, Marvin N.; Ali, Hebatallah
  • Review of Scientific Instruments, Vol. 88, Issue 7
  • DOI: 10.1063/1.4990797

Revealing the formation dynamics of the electric double layer by means of in - situ Rutherford backscattering spectrometry
journal, August 2019

  • Khojasteh, Nasrin B.; Apelt, Sabine; Bergmann, Ute
  • Review of Scientific Instruments, Vol. 90, Issue 8
  • DOI: 10.1063/1.5100216

Ambient pressure photoelectron spectroscopy: Practical considerations and experimental frontiers
journal, December 2016

  • Trotochaud, Lena; Head, Ashley R.; Karslıoğlu, Osman
  • Journal of Physics: Condensed Matter, Vol. 29, Issue 5
  • DOI: 10.1088/1361-648x/29/5/053002

The offset droplet: a new methodology for studying the solid/water interface using x-ray photoelectron spectroscopy
journal, October 2017

  • Booth, S. G.; Tripathi, A. M.; Strashnov, I.
  • Journal of Physics: Condensed Matter, Vol. 29, Issue 45
  • DOI: 10.1088/1361-648x/aa8b92

Beyond Koopmans’ theorem: electron binding energies in disordered materials
journal, December 2018


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

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

  • Amann, Peter; Degerman, David; Lee, Ming-Tao
  • Deutsches Elektronen-Synchrotron, DESY, Hamburg
  • DOI: 10.3204/pubdb-2019-04318

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

  • Amann, Peter; Degerman, David; Lee, Ming-Tao
  • Review of Scientific Instruments, Vol. 90, Issue 10
  • DOI: 10.1063/1.5109321

Water-mediated photo-induced reduction of platinum films
text, January 2019


Probing a battery electrolyte drop with ambient pressure photoelectron spectroscopy
text, January 2019


A high-pressure x-ray photoelectron spectroscopy instrument for studies of industrially relevant catalytic reactions at pressures of several bars
text, January 2019

  • Amann, Peter; Degerman, David; Lee, Ming-Tao
  • Deutsches Elektronen-Synchrotron, DESY, Hamburg
  • DOI: 10.3204/pubdb-2019-04325

The Oxidation of Platinum under Wet Conditions Observed by Electrochemical X-ray Photoelectron Spectroscopy
journal, March 2019

  • Mom, Rik; Frevel, Lorenz; Velasco-Vélez, Juan-Jesús
  • Journal of the American Chemical Society, Vol. 141, Issue 16
  • DOI: 10.1021/jacs.8b12284

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

  • Favaro, Marco; Jeong, Beomgyun; Ross, Philip N.
  • Nature Communications, Vol. 7, Issue 1
  • DOI: 10.1038/ncomms12695

Probing a battery electrolyte drop with ambient pressure photoelectron spectroscopy
text, January 2019