An electrochemical flow cell for operando XPS and NEXAFS investigation of solid–liquid interfaces
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Published version
Author(s)
Type
Journal Article
Abstract
Suitable reaction cells are critical for operando near ambient pressure (NAP) soft x-ray
photoelectron spectroscopy (XPS) and near-edge x-ray absorption fine structure (NEXAFS)
studies. They enable tracking the chemical state and structural properties of catalytically active
materials under realistic reaction conditions, and thus allow a better understanding of charge
transfer at the liquid–solid interface, activation of reactant molecules, and surface intermediate
species. In order to facilitate such studies, we have developed a top-side illuminated operando
spectro-electrochemical flow cell for synchrotron-based NAP-XPS/-NEXAFS studies. Our modular
design uses a non-metal (PEEK) body, and replaceable membranes which can be either of x-ray
transparent silicon nitride (SiNx) or of water permeable polymer membrane materials (e.g.
NafionTM). The design allows rapid sample exchange and simultaneous measurements of total
electron yield, Auger electron yield and fluorescence-yield. The developed system is highly
modular and can be used in the laboratory or directly at the beamline for operando XPS/ x-ray
absorption spectroscopy investigations of surfaces and interfaces. We present examples to
demonstrate the capabilities of the flow cell. These include an operando NEXAFS study of the
Cu-redox chemistry using a SiNx/Ti-Au/Cu working electrode assembly (WEA) and a
NAP-XPS/-NEXAFS study of water adsorption on a NafionTM polymer membrane based WEA
(NafionTM/C/IrOx catalyst). More importantly, the spectro-electrochemical flow cell is available for
user community of B07 beamlines at Diamond Light Source.
photoelectron spectroscopy (XPS) and near-edge x-ray absorption fine structure (NEXAFS)
studies. They enable tracking the chemical state and structural properties of catalytically active
materials under realistic reaction conditions, and thus allow a better understanding of charge
transfer at the liquid–solid interface, activation of reactant molecules, and surface intermediate
species. In order to facilitate such studies, we have developed a top-side illuminated operando
spectro-electrochemical flow cell for synchrotron-based NAP-XPS/-NEXAFS studies. Our modular
design uses a non-metal (PEEK) body, and replaceable membranes which can be either of x-ray
transparent silicon nitride (SiNx) or of water permeable polymer membrane materials (e.g.
NafionTM). The design allows rapid sample exchange and simultaneous measurements of total
electron yield, Auger electron yield and fluorescence-yield. The developed system is highly
modular and can be used in the laboratory or directly at the beamline for operando XPS/ x-ray
absorption spectroscopy investigations of surfaces and interfaces. We present examples to
demonstrate the capabilities of the flow cell. These include an operando NEXAFS study of the
Cu-redox chemistry using a SiNx/Ti-Au/Cu working electrode assembly (WEA) and a
NAP-XPS/-NEXAFS study of water adsorption on a NafionTM polymer membrane based WEA
(NafionTM/C/IrOx catalyst). More importantly, the spectro-electrochemical flow cell is available for
user community of B07 beamlines at Diamond Light Source.
Date Issued
2024-07-01
Date Acceptance
2024-06-06
Citation
Journal of Physics: Energy, 2024, 6 (3)
ISSN
2515-7655
Publisher
IOP Publishing
Journal / Book Title
Journal of Physics: Energy
Volume
6
Issue
3
Copyright Statement
© 2024 The Author(s). Published by IOP Publishing Ltd Original content from this work may be used under the terms of the Creative Commons Attribution 4.0 licence. Any further distribution of this work must maintain attribution to the author(s) and the title of the work, journal citation and DOI.
License URL
Identifier
10.1088/2515-7655/ad54ee
Subjects
operando XPS
electrochemistry
spectroscopy
NEXAFS
surfaces and interfaces
operando electrochemistry
energy materials
Publication Status
Published
Article Number
036001
Date Publish Online
2024-06-21