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@ARTICLE{Speer:1037258,
author = {Speer, Sebastian and Jovanovic, Sven and Merlen, Alexandre
and Bartoli, Francesco and Kiran, Kiran and Wolf, Niklas and
Karl, André and Jodat, Eva and Eichel, Rüdiger-A.},
title = {{L}aser induced oxidation {R}aman spectroscopy as an
analysis tool for iridium-based oxygen evolution catalysts},
journal = {Physical chemistry, chemical physics},
volume = {0},
issn = {1463-9076},
address = {Cambridge},
publisher = {RSC Publ.},
reportid = {FZJ-2025-00591},
pages = {0},
year = {2025},
abstract = {The study of degradation behavior of electrocatalysts in an
industrial context calls for rapid and efficient analysis
methods. Optical methods like Raman spectroscopy fulfil
these requirements and are thus predestined for this
purpose. However, the iridium utilized in proton exchange
membrane electrolysis (PEMEL) is Raman inactive in its
metallic state. This work demonstrates the high oxidation
sensitivity of iridium and its utilization in analysis of
catalyst materials. Laser induced oxidation Raman
spectroscopy (LIORS) is established as a novel method for
qualitative, chemical and structural analysis of iridium
catalysts. Differences in particle sizes of iridium powders
drastically change oxidation sensitivity. Oxidation of the
iridium powders to IrO2 occurred at a laser power density of
0.47 ± 0.06 mW μm−2 for the 850 μm powder and at 0.12
± 0.06 mW μm−2 and 0.019 ± 0.015 mW μm−2 for the 50
μm and 0.7–0.9 μm powders respectively. LIORS was
utilized to assess possible deterioration of an iridium
electrocatalyst due to operation under electrolysis. The
operating electrocatalyst exhibited higher oxidation
sensitivity, suggesting smaller iridium particle size due to
catalyst dissolution. Peak shifts of the IrO2 signal were
utilized to assess differences in transformation
temperatures. The operated electrocatalyst transformed to
IrO2 at lower temperature (8 cm−1 redshift) relative to
the pristine catalyst (10 cm−1 redshift), demonstrating
that pre-oxidation of the iridium to amorphous IrOx during
electrolysis diminishes the energy barrier needed for IrO2
formation. Thus, LIORS can be utilized as a straightforward
screening method for the analysis of iridium
electrocatalysts in the industrial application of PEMEL.},
cin = {IET-1},
ddc = {540},
cid = {I:(DE-Juel1)IET-1-20110218},
pnm = {1231 - Electrochemistry for Hydrogen (POF4-123) / SEGIWA -
Verbundvorhabenn $H2Giga_TP1a_SEGIWA:$ Online Analytik für
die Serienproduktion von Elektrolyseuren im Gigawatt-Bereich
(BMBF-03HY121B)},
pid = {G:(DE-HGF)POF4-1231 / G:(DE-Juel1)BMBF-03HY121B},
typ = {PUB:(DE-HGF)16},
pubmed = {39807029},
UT = {WOS:001395874600001},
doi = {10.1039/D4CP03592E},
url = {https://juser.fz-juelich.de/record/1037258},
}