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Operando X-ray Spectroscopy

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Operando X-ray Spectroscopy

The Operando X-ray Spectroscopy belongs to Environment Division (ENE) of PSI and is within a matrix organization responsible for the operation of the SuperXAS and Debye beamlines to LSF.

Scientific Highlights

1. März 2023
Zabilska_Angewandte

Activity Trend Origin of Ethanol Oxidative Dehydrogenation over VOx/CeO2

Using operando time-resolved X-ray absorption spectroscopy, we investigated the origin of volcano-shaped ethanol oxidative dehydrogenation activity trend of VOx/CeO2 catalysts as a function of VOx surface coverage. Vanadium and cerium synergistically change their oxidation states during the catalytic cycle. The catalytic activity correlates with the concentration of reversible Ce4+/3+species.

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9. November 2022
PROX

Platinum-Iron(II) Oxide Sites Directly Responsible for Preferential Carbon Monoxide Oxidation at Ambient Temperature: An Operando X-ray Absorption Spectroscopy Study

Operando X-ray absorption spectroscopy revealed a linear correlation between the amount of oxidic Fe2+ and the ambient temperature activity of Pt−FeOx preferential carbon monoxide oxidation catalysts. The hydrogen prereduction temperature and pressure determines the amount of active Fe2+ sites for alumina- and silica-supported Pt−Fe catalysts. Catalyst deactivation is linked with the oxidation of these sites.

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21. April 2022
CsPbBr3

Quantifying Photoinduced Polaronic and Thermal Distortions in Inorganic Lead Halide Perovskite Nanocrystals

The development of next-generation perovskite-based optoelectronic devices relies critically on the understanding of the interaction between charge carriers and the polar lattice in out-of-equilibrium conditions. While it has become increasingly evident for CsPbBr3 perovskites that the Pb–Br framework flexibility plays a key role in their light-activated functionality, the corresponding local structural rearrangement has not yet been unambiguously identified. In this work the photoinduced lattice changes were investigated using combination of time-resolved and temperature-dependent studies at Br K and Pb L3 X-ray absorption edges and ab initio simulations.

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14. März 2022
Zabilska_JACSAu

Redox Dynamics of Active VOx Sites Promoted by TiOx during Oxidative Dehydrogenation of Ethanol Detected by Operando Quick XAS

Operando time-resolved V and Ti K-edge X-ray absorption near-edge spectroscopy, coupled with a transient experimental strategy, quantitatively showed that the formation of acetaldehyde over 5% V2O5/15% TiO2/SiO2 is kinetically coupled to the formation of a V4+ intermediate, while the formation of V3+ is delayed and 10–70 times slower. The low-coordinated nature of various redox states of VOx species (V5+, V4+, and V3+) in the 5% V2O5/15% TiO2/SiO2 catalyst is confirmed using the extensive database of V K-edge XANES spectra of standards and specially synthesized molecular crystals.

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1. Februar 2022
4 and 5 coordinated Cu complexes

Exploring the role of structural distortions to obtain Cu photosensitizer with thousand times longer excited state lifetime

Cu diimine complexes present a noble metal free alternative to classical Ru, Re, Ir and Pt based photosensitizers in solution photochemistry, photoelectrochemical or dye-sensitized solar cells. Optimization of these dyes requires an understanding of factors governing the key photochemical properties: excited state lifetime and emission quantum yield. Using pump-probe XAS and DFT calculations we have explored the involvement of exciplex formation in the deactivation of the photoexcited state.

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18. Februar 2021
Platinum chloride in aqueous solution promotes the dispersion of large gold nanoparticles (>70 nm) on carbon

Sustainable Synthesis of Bimetallic Single Atom Gold-Based Catalysts with Enhanced Durability in Acetylene Hydrochlorination

Platinum chloride in aqueous solution promotes the dispersion of large gold nanoparticles (>70 nm) on carbon carriers into single atoms, forming bimetallic single-atom catalysts with improved resistance against sintering at temperatures up to 800 K and under the harsh reductive reaction conditions of acetylene hydrochlorination, leading to improved lifetime in this reaction. To rationalize these observations, this study, led by ETH Zurich, utilized X-ray adsorption spectroscopy conducted at the SuperXAS beamline of the SLS to provide insights into the degree of gold dispersion and the structure of the isolated metal sites in the bimetallic catalysts.

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2. Dezember 2020
goerlin_2020.png

Key activity descriptors of nickel-iron oxygen evolution electrocatalysts in the presence of alkali metal cations

Ni-Fe oxyhydroxide is among the most active oxygen evolution electrocatalysts. Electrolyte alkali metal cations modify the activity and reaction intermediates, however, the exact mechanism is at question due to unexplained deviations from the cation size trend. Our X-ray absorption spectroelectrochemical results show that the OER activity follows the variations in .electrolyte pH rather than a specific cation. Our DFT-based reactivity descriptors confirm the conclusions of an indirect pH effect.

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31. August 2020
Smolentsev_2020

The structure of active sites of CoMo/Al2O3 catalysts determined by RIXS spectroscopy.

A fundamental understanding of the active sites in technical CoMo/ Al2O3 catalysts is crucial to improve the production of clean transportation fuels by hydrodesulfurization (HDS), which removes sulfur from fossil fuels. Sulfur dioxide, resulting from fossil fuel combustion, is one of the main causes for acid rain. In situ X-ray spectroscopic experiments at the SuperXAS beamline of the SLS provided insight in the structure and number of active sites (“Co−Mo−S”) in sulfided CoMo/ Al2O3 catalysts. When the Co to Mo ratio is less than 0.1, cobalt forms isolated sites on the MoS2 phase, where the cobalt promoter atoms are in centrosymmetric octahedral coordination with six-sulfur ligands.

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1. Mai 2020
smolentsev_nature_comm_2020.jpg

Taking a snapshot of the triplet excited state of an OLED organometallic luminophore using X-rays

In this work, the complementarity of pump-probe experiments at SwissFEL (ALVRA endstation) and at synchrotrons (SuperXAS beamline of SLS and ID09 of ESRF) is used to investigate the triplet excited state of Cu OLED materials. Details about the charge transfer and structural rearrangements in the excited state of this material are revealed and obtained data can be used to verify computational methods for rational development of new OLED materials.

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Dr. Maarten Nachtegaal
Paul Scherrer Institut
5232 Villigen-PSI
Switzerland
Telephone: +41 56 310 3056
E-mail: maarten.nachtegaal@psi.ch

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Laboratory for Synchrotron Radiation and Femtochemistry

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Synchrotron light large research facility.

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The new X-ray free electron laser facility.

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