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  4. Beware of beam damage under reaction conditions: X-ray induced photochemical reduction of supported VOx catalysts during in situ XAS experiments
 
research article

Beware of beam damage under reaction conditions: X-ray induced photochemical reduction of supported VOx catalysts during in situ XAS experiments

Zabilska, Anna
•
Clark, Adam H.
•
Ferri, Davide
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August 25, 2022
Physical Chemistry Chemical Physics

In situ X-ray absorption spectroscopy (XAS) is a powerful technique for the investigation of heterogeneous catalysts and electrocatalysts. The obtained XAS spectra are usually interpreted from the point of view of the investigated chemical processes, thereby sometimes omitting the fact that intense X-ray irradiation may induce additional transformations in metal speciation and, thus, in the corresponding XAS spectra. In this work, we report on X-ray induced photochemical reduction of vanadium in supported vanadia (VOx) catalysts under reaction conditions, detected at a synchrotron beamline. While this process was not observed in an inert atmosphere and in the presence of water vapor, it occurred at room temperature in the presence of a reducing agent (ethanol or hydrogen) alone or mixed with oxygen. Temperature programmed experiments have shown that X-ray induced reduction of VOx species appeared very clear at 30-100 degrees C but was not detected at higher temperatures, where the thermocatalytic ethanol oxidative hydrogenation (ODH) takes place. Similar to other studies on X-ray induced effects, we suggest approaches, which can help to mitigate vanadium photoreduction, including defocusing of the X-ray beam and attenuation of the X-ray beam intensity by filters. To recognize beam damage under in situ/operando conditions, we suggest performing X-ray beam switching (on and off) tests at different beam intensities under in situ conditions.

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Type
research article
DOI
10.1039/d2cp02721f
Web of Science ID

WOS:000850442600001

Author(s)
Zabilska, Anna
Clark, Adam H.
Ferri, Davide
Nachtegaal, Maarten
Kroecher, Oliver  
Safonova, Olga, V
Date Issued

2022-08-25

Publisher

ROYAL SOC CHEMISTRY

Published in
Physical Chemistry Chemical Physics
Volume

24

Issue

36

Start page

21916

End page

21926

Subjects

Chemistry, Physical

•

Physics, Atomic, Molecular & Chemical

•

Chemistry

•

Physics

•

vanadium-oxide catalysts

•

uv-vis drs

•

selective oxidation

•

methanol oxidation

•

absorption spectroscopy

•

radiation-damage

•

v2o5

•

time

•

ethanol

•

raman

Editorial or Peer reviewed

REVIEWED

Written at

EPFL

EPFL units
GR-KRO  
Available on Infoscience
September 26, 2022
Use this identifier to reference this record
https://infoscience.epfl.ch/handle/20.500.14299/190960
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