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A transfer cell for ultrahigh vacuum surface analysis of samples exposed to electrochemical environments

Lira, E. LU ; Grespi, A. LU orcid ; Paoletti, N. ; Ti, A. LU orcid ; Rodriguez, A. M. ; Larsson, A. LU orcid ; Merte, L. R. LU and Lundgren, E. LU (2026) In Review of Scientific Instruments 97(3).
Abstract

We present the design and implementation of a portable transfer system equipped with an integrated electrochemical cell that enables the controlled transfer of samples between an electrochemical environment and an ultrahigh vacuum (UHV) system without air exposure. This setup allows for the preparation of well-defined model surfaces, their electrochemical modification, and subsequent structural and chemical characterization using surface-sensitive UHV techniques. The system’s performance was validated using Au(111) as a model electrode. Cyclic voltammetry performed in a hanging meniscus configuration reproduced the characteristic oxidation and reduction features of Au(111), while scanning tunneling microscopy, low-energy electron... (More)

We present the design and implementation of a portable transfer system equipped with an integrated electrochemical cell that enables the controlled transfer of samples between an electrochemical environment and an ultrahigh vacuum (UHV) system without air exposure. This setup allows for the preparation of well-defined model surfaces, their electrochemical modification, and subsequent structural and chemical characterization using surface-sensitive UHV techniques. The system’s performance was validated using Au(111) as a model electrode. Cyclic voltammetry performed in a hanging meniscus configuration reproduced the characteristic oxidation and reduction features of Au(111), while scanning tunneling microscopy, low-energy electron diffraction, and Auger electron spectroscopy confirmed the structural and chemical integrity of the surface after transfer. Progressive surface roughening with increasing numbers of oxidation-reduction cycles followed an approximately linear trend, consistent with previous studies. In addition, we investigated the stability of gold oxide under vacuum and demonstrated that the thin oxide formed during anodic polarization, prior to the onset of the oxygen evolution reaction, is partially reduced during UHV transfer. X-ray photoelectron spectroscopy and Auger spectroscopy data indicate that the oxidized phase is stable in vacuum only after polarization at sufficiently high potentials, when continuous oxygen evolution is achieved via water electrolysis. Finally, successful integration and testing of the system at the FlexPES beamline at MAX IV confirmed its compatibility with synchrotron-based spectroscopy.

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author
; ; ; ; ; ; and
organization
publishing date
type
Contribution to journal
publication status
published
subject
in
Review of Scientific Instruments
volume
97
issue
3
article number
033903
publisher
American Institute of Physics (AIP)
external identifiers
  • scopus:105032050183
  • pmid:41784501
ISSN
0034-6748
DOI
10.1063/5.0313826
language
English
LU publication?
yes
id
575aa7c6-f46c-4826-b18e-d0729b1f834d
date added to LUP
2026-04-22 12:04:27
date last changed
2026-05-05 09:00:26
@article{575aa7c6-f46c-4826-b18e-d0729b1f834d,
  abstract     = {{<p>We present the design and implementation of a portable transfer system equipped with an integrated electrochemical cell that enables the controlled transfer of samples between an electrochemical environment and an ultrahigh vacuum (UHV) system without air exposure. This setup allows for the preparation of well-defined model surfaces, their electrochemical modification, and subsequent structural and chemical characterization using surface-sensitive UHV techniques. The system’s performance was validated using Au(111) as a model electrode. Cyclic voltammetry performed in a hanging meniscus configuration reproduced the characteristic oxidation and reduction features of Au(111), while scanning tunneling microscopy, low-energy electron diffraction, and Auger electron spectroscopy confirmed the structural and chemical integrity of the surface after transfer. Progressive surface roughening with increasing numbers of oxidation-reduction cycles followed an approximately linear trend, consistent with previous studies. In addition, we investigated the stability of gold oxide under vacuum and demonstrated that the thin oxide formed during anodic polarization, prior to the onset of the oxygen evolution reaction, is partially reduced during UHV transfer. X-ray photoelectron spectroscopy and Auger spectroscopy data indicate that the oxidized phase is stable in vacuum only after polarization at sufficiently high potentials, when continuous oxygen evolution is achieved via water electrolysis. Finally, successful integration and testing of the system at the FlexPES beamline at MAX IV confirmed its compatibility with synchrotron-based spectroscopy.</p>}},
  author       = {{Lira, E. and Grespi, A. and Paoletti, N. and Ti, A. and Rodriguez, A. M. and Larsson, A. and Merte, L. R. and Lundgren, E.}},
  issn         = {{0034-6748}},
  language     = {{eng}},
  number       = {{3}},
  publisher    = {{American Institute of Physics (AIP)}},
  series       = {{Review of Scientific Instruments}},
  title        = {{A transfer cell for ultrahigh vacuum surface analysis of samples exposed to electrochemical environments}},
  url          = {{http://dx.doi.org/10.1063/5.0313826}},
  doi          = {{10.1063/5.0313826}},
  volume       = {{97}},
  year         = {{2026}},
}