scholarly journals Time-Resolved X-ray Absorption Spectroscopy in (Photo)Electrochemistry

Surfaces ◽  
2018 ◽  
Vol 1 (1) ◽  
pp. 138-150 ◽  
Author(s):  
Martina Fracchia ◽  
Paolo Ghigna ◽  
Alberto Vertova ◽  
Sandra Rondinini ◽  
Alessandro Minguzzi
Keyword(s):  
Oxidation State ◽  
Absorption Spectroscopy ◽  
Time Resolution ◽  
Local Structure ◽  
Future Perspectives ◽  
Time Resolved ◽  
X Ray ◽  
Fixed Energy ◽  
Complete Survey ◽  
X Ray Absorption

This minireview aims at providing a complete survey concerning the use of X-ray absorption spectroscopy (XAS) for time-resolved studies of electrochemical and photoelectrochemical phenomena. We will see that time resolution can range from the femto-picosecond to the second (or more) scale and that this joins the valuable throughput typical of XAS, which allows for determining the oxidation state of the investigated element, together with its local structure. We will analyze four different techniques that use different approaches to exploit the in real time capabilities of XAS. These are quick-XAS, energy dispersive XAS, pump & probe XAS and fixed-energy X-ray absorption voltammetry. In the conclusions, we will analyze possible future perspectives for these techniques.

scholarly journals Operando tracking of oxidation-state changes by coupling electrochemistry with time-resolved X-ray absorption spectroscopy demonstrated for water oxidation by a cobalt-based catalyst film

2021 ◽  
Author(s):  
Chiara Pasquini ◽  
Si Liu ◽  
Petko Chernev ◽  
Diego Gonzalez-Flores ◽  
Mohammad Reza Mohammadi ◽  
...  
Keyword(s):  
Oxidation State ◽  
Absorption Spectroscopy ◽  
Performance Optimization ◽  
Water Oxidation ◽  
Electrochemical Techniques ◽  
Time Resolved ◽  
Catalytic Current ◽  
X Ray ◽  
State Changes ◽  
X Ray Absorption

AbstractTransition metal oxides are promising electrocatalysts for water oxidation, i.e., the oxygen evolution reaction (OER), which is critical in electrochemical production of non-fossil fuels. The involvement of oxidation state changes of the metal in OER electrocatalysis is increasingly recognized in the literature. Tracing these oxidation states under operation conditions could provide relevant information for performance optimization and development of durable catalysts, but further methodical developments are needed. Here, we propose a strategy to use single-energy X-ray absorption spectroscopy for monitoring metal oxidation-state changes during OER operation with millisecond time resolution. The procedure to obtain time-resolved oxidation state values, using two calibration curves, is explained in detail. We demonstrate the significance of this approach as well as possible sources of data misinterpretation. We conclude that the combination of X-ray absorption spectroscopy with electrochemical techniques allows us to investigate the kinetics of redox transitions and to distinguish the catalytic current from the redox current. Tracking of the oxidation state changes of Co ions in electrodeposited oxide films during cyclic voltammetry in neutral pH electrolyte serves as a proof of principle. Graphical abstract

scholarly journals Fluorescence-detected quick-scanning X-ray absorption spectroscopy

2020 ◽  
Vol 27 (3) ◽  
pp. 681-688 ◽  
Author(s):  
Adam H. Clark ◽  
Patrick Steiger ◽  
Benjamin Bornmann ◽  
Stephan Hitz ◽  
Ronald Frahm ◽  
...  
Keyword(s):  
Absorption Spectroscopy ◽  
Time Resolution ◽  
The State ◽  
Complex Materials ◽  
Time Resolved ◽  
Temperature Oxidation ◽  
X Ray ◽  
Signal Collection ◽  
Transmission Measurements ◽  
X Ray Absorption

Time-resolved X-ray absorption spectroscopy (XAS) offers the possibility to monitor the state of materials during chemical reactions. While this technique has been established for transmission measurements for a number of years, XAS measurements in fluorescence mode are challenging because of limitations in signal collection as well as detectors. Nevertheless, measurements in fluorescence mode are often the only option to study complex materials containing heavy matrices or in samples where the element of interest is in low concentration. Here, it has been demonstrated that high-quality quick-scanning full extended X-ray absorption fine-structure data can be readily obtained with sub-second time resolution in fluorescence mode, even for highly diluted samples. It has also been demonstrated that in challenging samples, where transmission measurements are not feasible, quick fluorescence can yield significant insight in reaction kinetics. By studying the fast high-temperature oxidation of a reduced LaFe0.8Ni0.8O3 perovskite type, an example where the perovskite matrix elements prevent measurements in fluorescence, it is shown that it is now possible to follow the state of Ni in situ at a 3 s time resolution.

Application of In Situ X-ray Absorption Spectroscopy to Study Dilute Chromium Ions in a Molten Chloride Salt

2019 ◽  
Author(s):  
Jisue Moon ◽  
Carter Abney ◽  
Dmitriy Dolzhnikov ◽  
James M. Kurley ◽  
Kevin A. Beyer ◽  
...  
Keyword(s):  
Absorption Spectroscopy ◽  
Local Structure ◽  
Chloride Salt ◽  
X Ray ◽  
Molten Chloride ◽  
Stable Species ◽  
Higher Temperature ◽  
Cr Concentration ◽  
X Ray Absorption

The local structure of dilute CrCl<sub>3</sub> in a molten MgCl<sub>2</sub>:KCl salt was investigated by <i>in situ</i> x-ray absorption spectroscopy (XAS) at temperatures from room temperature to 800<sup>o</sup>C. This constitutes the first experiment where dilute Cr speciation is explored in a molten chloride salt, ostensibly due to the compounding challenges arising from a low Cr concentration in a matrix of heavy absorbers at extreme temperatures. CrCl<sub>3</sub> was confirmed to be the stable species between 200 and 500<sup>o</sup>C, while mobility of metal ions at higher temperature (>700<sup>o</sup>C) prevented confirmation of the local structure.

Chemical State and Local Structure around Titanium Atoms in NaAlH4Doped with TiCl3Using X-ray Absorption Spectroscopy

2004 ◽  
Vol 108 (42) ◽  
pp. 16372-16376 ◽  
Author(s):  
Aline Léon ◽  
Oliver Kircher ◽  
Jörg Rothe ◽  
Maximilian Fichtner
Keyword(s):  
Absorption Spectroscopy ◽  
Local Structure ◽  
Chemical State ◽  
X Ray ◽  
State And Local ◽  
X Ray Absorption

Local structure of Fe in Fe-doped misfit-layered calcium cobaltite: An X-ray absorption spectroscopy study

2013 ◽  
Vol 204 ◽  
pp. 257-265 ◽  
Author(s):  
Natkrita Prasoetsopha ◽  
Supree Pinitsoontorn ◽  
Atipong Bootchanont ◽  
Pinit Kidkhunthod ◽  
Pornjuk Srepusharawoot ◽  
...  
Keyword(s):  
Absorption Spectroscopy ◽  
Local Structure ◽  
Spectroscopy Study ◽  
X Ray ◽  
X Ray Absorption

Local structure ofBaBixPb1−xO3determined by x-ray-absorption spectroscopy

1991 ◽  
Vol 44 (13) ◽  
pp. 6961-6972 ◽  
Author(s):  
J. B. Boyce ◽  
F. G. Bridges ◽  
T. Claeson ◽  
T. H. Geballe ◽  
G. G. Li ◽  
...  
Keyword(s):  
Absorption Spectroscopy ◽  
Local Structure ◽  
X Ray ◽  
X Ray Absorption

scholarly journals A setup for ultrafast time-resolved x-ray absorption spectroscopy

2004 ◽  
Vol 75 (1) ◽  
pp. 24-30 ◽  
Author(s):  
Melanie Saes ◽  
Frank van Mourik ◽  
Wojciech Gawelda ◽  
Maik Kaiser ◽  
Majed Chergui ◽  
...  
Keyword(s):  
Absorption Spectroscopy ◽  
Time Resolved ◽  
X Ray ◽  
X Ray Absorption
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