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Methodological insights into the dip-and-pull X-ray photoelectron spectroscopy technique : analysing electrochemical interfaces under in situ/operando conditions

Rotonnelli, Benjamin ; Brige, Amandine ; Oshchepkov, Alexandr G. ; Gallet, Jean Jacques ; Bournel, Fabrice ; Bonnefont, Antoine ; Yaroslavtsev, Alexander LU ; Shavorskiy, Andrey LU ; Temperton, Robert LU and Savinova, Elena R. , et al. (2026) In Journal of Synchrotron Radiation 33. p.130-141
Abstract

Gaining insight into structural and compositional transformations occurring at the electrode/electrolyte interface during the operation of electrochemical systems is fundamental to understanding and, thus, optimizing their performance. Such an analysis must be performed in operando conditions, owing to the potential, electrolyte and time dependence of these transformations. Here, the use of X-ray photoelectron spectroscopy (XPS) is particularly attractive due to its surface sensitivity and ability to provide quantitative information on the oxidation state and chemical environment of an element. In specific instrumental configurations [e.g. in `dip-and-pull' (D&P) or `meniscus' setup], it can be used to analyse not only the electrode... (More)

Gaining insight into structural and compositional transformations occurring at the electrode/electrolyte interface during the operation of electrochemical systems is fundamental to understanding and, thus, optimizing their performance. Such an analysis must be performed in operando conditions, owing to the potential, electrolyte and time dependence of these transformations. Here, the use of X-ray photoelectron spectroscopy (XPS) is particularly attractive due to its surface sensitivity and ability to provide quantitative information on the oxidation state and chemical environment of an element. In specific instrumental configurations [e.g. in `dip-and-pull' (D&P) or `meniscus' setup], it can be used to analyse not only the electrode but also the electrolyte side of the interface, under in situ/operando conditions. In this article, we discuss how D&P XPS can provide unique information on both sides of the electrode/electrolyte interface, briefly review publications demonstrating its capabilities, highlight the challenges the method faces, and share our views on its future developments. This article aims to provide a practical guide to new D&P synchrotron users and help them to understand the technique, and physical phenomena that may impede the acquisition of reliable data.

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organization
publishing date
type
Contribution to journal
publication status
published
subject
keywords
dip-and-pull XPS, electrochemistry, electrode–electrolyte interface, in situ, methodology, operando, synchrotron, X-ray photoelectron spectroscopy
in
Journal of Synchrotron Radiation
volume
33
pages
12 pages
publisher
International Union of Crystallography
external identifiers
  • pmid:41307983
  • scopus:105026870025
ISSN
1600-5775
DOI
10.1107/S1600577525008811
language
English
LU publication?
yes
additional info
Publisher Copyright: open access.
id
2adaba1f-9cee-4aef-bfe0-179a4c2972dc
date added to LUP
2026-03-19 14:22:45
date last changed
2026-09-05 23:01:05
@article{2adaba1f-9cee-4aef-bfe0-179a4c2972dc,
  abstract     = {{<p>Gaining insight into structural and compositional transformations occurring at the electrode/electrolyte interface during the operation of electrochemical systems is fundamental to understanding and, thus, optimizing their performance. Such an analysis must be performed in operando conditions, owing to the potential, electrolyte and time dependence of these transformations. Here, the use of X-ray photoelectron spectroscopy (XPS) is particularly attractive due to its surface sensitivity and ability to provide quantitative information on the oxidation state and chemical environment of an element. In specific instrumental configurations [e.g. in `dip-and-pull' (D&amp;P) or `meniscus' setup], it can be used to analyse not only the electrode but also the electrolyte side of the interface, under in situ/operando conditions. In this article, we discuss how D&amp;P XPS can provide unique information on both sides of the electrode/electrolyte interface, briefly review publications demonstrating its capabilities, highlight the challenges the method faces, and share our views on its future developments. This article aims to provide a practical guide to new D&amp;P synchrotron users and help them to understand the technique, and physical phenomena that may impede the acquisition of reliable data.</p>}},
  author       = {{Rotonnelli, Benjamin and Brige, Amandine and Oshchepkov, Alexandr G. and Gallet, Jean Jacques and Bournel, Fabrice and Bonnefont, Antoine and Yaroslavtsev, Alexander and Shavorskiy, Andrey and Temperton, Robert and Savinova, Elena R. and Asset, Tristan}},
  issn         = {{1600-5775}},
  keywords     = {{dip-and-pull XPS; electrochemistry; electrode–electrolyte interface; in situ; methodology; operando; synchrotron; X-ray photoelectron spectroscopy}},
  language     = {{eng}},
  month        = {{01}},
  pages        = {{130--141}},
  publisher    = {{International Union of Crystallography}},
  series       = {{Journal of Synchrotron Radiation}},
  title        = {{Methodological insights into the dip-and-pull X-ray photoelectron spectroscopy technique : analysing electrochemical interfaces under in situ/operando conditions}},
  url          = {{http://dx.doi.org/10.1107/S1600577525008811}},
  doi          = {{10.1107/S1600577525008811}},
  volume       = {{33}},
  year         = {{2026}},
}