A compact von Hámos spectrometer for parallel X-ray Raman scattering and X-ray emission spectroscopy at ID20 of the European Synchrotron Radiation Facility

Sahle, Christoph J.; Florent, Gerbon,; Henriquet, C.; Verbeni, R.; Detlefs, Blanka; Longo, Alessandro; Mirone, Alessandro; Lagier, Michel; Otte, Florian; Spiekermann, Georg; Petitgirard, Sylvain

doi:10.1107/s1600577522011171

Cited by 10 publications

(8 citation statements)

References 46 publications

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“…The XRS-XES experiment was performed at beamline ID20 , (Figure A) of the 6 GeV ESRF synchrotron (Grenoble, France, proposal CH6020). The pink beam produced from three U26 undulators was monochromatized, using a cryogenically cooled Si (111) and Si (311) crystal monochromator, and focused to a spot size of approximately 40 μm × 80 μm (V × H) at the sample position via a mirror system in Kirkpatrick–Baez geometry .…”

Section: Experimental Methodsmentioning

confidence: 99%

“…Figure B shows the full scan of XRS taken on the fresh Ni/MgFeAlO 4 sample. In parallel with the XRS measurement, XES data were collected for the transition metals Ni and Fe by means of a von Hamos detector . The detector comprises three cylindrically bent crystal analyzers, one Si (220) for Ni and two Si (111) for Fe, with a bending radius of 250 mm.…”

Section: Experimental Methodsmentioning

confidence: 99%

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Evolution of Low Z-Elements in a Ni/MgFeAlO₄ Catalyst during Reaction: Insight from In Situ XRS

Kumar Das,

D’ooghe,

Srinath

et al. 2024

ACS Catal.

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Ni/MgFeAlO 4 displays promising activity and stability in the dry reforming of methane. In order to establish a correlation between its performance and structural changes, an in-depth analysis of the Ni/ MgFeAlO 4 catalyst's constituent elements is conducted using in situ techniques, specifically combined X-ray emission spectroscopy (XES) and X-ray Raman scattering (XRS) spectroscopy. This investigation spans sequential treatments involving H 2 reduction, CO 2 reoxidation, and methane dry reforming. XES valence-to-core signals for Fe and Ni retrace the applied treatments. After the reaction, Ni is fully metallic, while Fe shows a mixed metal-oxide state. Comparing these XES spectroscopic data with ab initio simulations indicates that dry reforming of methane does not form metal carbide. C K-edge XRS data recorded after the reaction do not protrude above the noise, proving the capability of the Ni/MgFeAlO 4 catalyst to mitigate carbon deposition. O K-edge spectra exhibit variations corresponding to each treatment, effectively replicated through simulations with semiempirical screening parameters. These parameters represent electron transfer between oxygen and neighboring 3d transition metal elements and offer insights into the acid−base properties of the material. Furthermore, the Al L 2,3 -edge spectra provide valuable information about the impact of treatments on the spinel arrangement, indicating an increasing tetrahedral occupancy of Al 3+ in the support. By employing a comprehensive approach that combines XRS with XES, this study provides a holistic understanding of the evolution of low Z-elements, O and Al, alongside Fe and Ni, in the Ni/MgFeAlO 4 catalyst throughout the reduction, reoxidation, and methane dry reforming processes.

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Section: Experimental Methodsmentioning

confidence: 99%

Section: Experimental Methodsmentioning

confidence: 99%

Evolution of Low Z-Elements in a Ni/MgFeAlO₄ Catalyst during Reaction: Insight from In Situ XRS

Kumar Das,

D’ooghe,

Srinath

et al. 2024

ACS Catal.

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“…1(a). According to a target fluorescence energy and selected analyzer crystal planes, a two-dimensional (2D) detector on a robot arm is positioned on the Rowland circle in a vertical diffraction plane, and collects the X-ray emission spectrum dispersed by the analyzer crystals on the von Hamos spectrometer (Galler et al, 2019;Khakhulin et al, 2020;Sahle et al, 2023).…”

Section: Experimental Setup At the Xss Hutchmentioning

confidence: 99%

Resonant X-ray emission spectroscopy using self-seeded hard X-ray pulses at PAL-XFEL

Choi,

Park,

Kim

et al. 2023

J Synchrotron Radiat

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Self-seeded hard X-ray pulses at PAL-XFEL were used to commission a resonant X-ray emission spectroscopy experiment with a von Hamos spectrometer. The self-seeded beam, generated through forward Bragg diffraction of the [202] peak in a 100 µm-thick diamond crystal, exhibited an average bandwidth of 0.54 eV at 11.223 keV. A coordinated scanning scheme of electron bunch energy, diamond crystal angle and silicon monochromator allowed us to map the Ir Lβ2 X-ray emission lines of IrO2 powder across the Ir L 3-absorption edge, from 11.212 to 11.242 keV with an energy step of 0.3 eV. This work provides a reference for hard X-ray emission spectroscopy experiments utilizing self-seeded pulses with a narrow bandwidth, eventually applicable for pump–probe studies in solid-state and diluted systems.

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“…The 500 mm working distance of the VHS at FXE was chosen to provide a good compromise between energy resolution and collection efficiency, while maintaining the possibility to collect multiple emission lines simultaneously by either using several different analyzers or by slightly changing the Bragg angles. Naturally, the final energy resolution of dispersive X-ray spectrometers is also a function of the beam size along the dispersive direction, the detector pixel size, the specific material of the analyzers and the Bragg angle of operation (Szlachetko et al, 2012;Alonso-Mori et al, 2012;Sahle et al, 2023).…”

Section: X-ray Emission Spectroscopymentioning

confidence: 99%

Experimental capabilities for liquid jet samples at sub-MHz rates at the FXE Instrument at European XFEL

Lima,

Otte,

Vakili

et al. 2023

J Synchrotron Rad

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The Femtosecond X-ray Experiments (FXE) instrument at the European X-ray Free-Electron Laser (EuXFEL) provides an optimized platform for investigations of ultrafast physical, chemical and biological processes. It operates in the energy range 4.7–20 keV accommodating flexible and versatile environments for a wide range of samples using diverse ultrafast X-ray spectroscopic, scattering and diffraction techniques. FXE is particularly suitable for experiments taking advantage of the sub-MHz repetition rates provided by the EuXFEL. In this paper a dedicated setup for studies on ultrafast biological and chemical dynamics in solution phase at sub-MHz rates at FXE is presented. Particular emphasis on the different liquid jet sample delivery options and their performance is given. Our portfolio of high-speed jets compatible with sub-MHz experiments includes cylindrical jets, gas dynamic virtual nozzles and flat jets. The capability to perform multi-color X-ray emission spectroscopy (XES) experiments is illustrated by a set of measurements using the dispersive X-ray spectrometer in von Hamos geometry. Static XES data collected using a multi-crystal scanning Johann-type spectrometer are also presented. A few examples of experimental results on ultrafast time-resolved X-ray emission spectroscopy and wide-angle X-ray scattering at sub-MHz pulse repetition rates are given.

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A compact von Hámos spectrometer for parallel X-ray Raman scattering and X-ray emission spectroscopy at ID20 of the European Synchrotron Radiation Facility

Cited by 10 publications

References 46 publications

Evolution of Low Z-Elements in a Ni/MgFeAlO₄ Catalyst during Reaction: Insight from In Situ XRS

Evolution of Low Z-Elements in a Ni/MgFeAlO₄ Catalyst during Reaction: Insight from In Situ XRS

Resonant X-ray emission spectroscopy using self-seeded hard X-ray pulses at PAL-XFEL

Experimental capabilities for liquid jet samples at sub-MHz rates at the FXE Instrument at European XFEL

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A compact von Hámos spectrometer for parallel X-ray Raman scattering and X-ray emission spectroscopy at ID20 of the European Synchrotron Radiation Facility

Cited by 10 publications

References 46 publications

Evolution of Low Z-Elements in a Ni/MgFeAlO4 Catalyst during Reaction: Insight from In Situ XRS

Evolution of Low Z-Elements in a Ni/MgFeAlO4 Catalyst during Reaction: Insight from In Situ XRS

Resonant X-ray emission spectroscopy using self-seeded hard X-ray pulses at PAL-XFEL

Experimental capabilities for liquid jet samples at sub-MHz rates at the FXE Instrument at European XFEL

Contact Info

Product

Resources

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Evolution of Low Z-Elements in a Ni/MgFeAlO₄ Catalyst during Reaction: Insight from In Situ XRS

Evolution of Low Z-Elements in a Ni/MgFeAlO₄ Catalyst during Reaction: Insight from In Situ XRS