Planning, performing and analyzing X-ray Raman scattering experiments

Sahle, Christoph J.; Mirone, Alessandro; Niskanen, Johannes; Inkinen, Juho; Krisch, M.; Huotari, Simo

doi:10.1107/s1600577514027581

Cited by 90 publications

(116 citation statements)

References 64 publications

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“…XRS studies were carried out at beamlines ID20/ESRF (Sahle, Mirone et al, 2015;Huotari et al, 2017) and P01/ PETRAIII (Fig. 1).…”

Section: Methodsmentioning

confidence: 99%

“…We remedied this cross-compatibility issue by applying a 0.2 eV shift towards the higher energy transfer region for all the O K-edge spectra and applying a 0.08 eV shift towards the lower energy transfer region for the C Kedge spectra of the samples which were measured at P01. For data treatment, the same software was used (Sahle, Mirone et al, 2015;Sahle et al, 2017).…”

Section: Methodsmentioning

confidence: 99%

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X-ray Raman spectroscopy of lithium-ion battery electrolyte solutions in a flow cell

Ketenoğlu

Spiekermann

Harder

et al. 2018

J Synchrotron Radiat

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The effects of varying LiPF salt concentration and the presence of lithium bis(oxalate)borate additive on the electronic structure of commonly used lithium-ion battery electrolyte solvents (ethylene carbonate-dimethyl carbonate and propylene carbonate) have been investigated. X-ray Raman scattering spectroscopy (a non-resonant inelastic X-ray scattering method) was utilized together with a closed-circle flow cell. Carbon and oxygen K-edges provide characteristic information on the electronic structure of the electrolyte solutions, which are sensitive to local chemistry. Higher Li ion concentration in the solvent manifests itself as a blue-shift of both the π* feature in the carbon edge and the carbonyl π* feature in the oxygen edge. While these oxygen K-edge results agree with previous soft X-ray absorption studies on LiBF salt concentration in propylene carbonate, carbon K-edge spectra reveal a shift in energy, which can be explained with differing ionic conductivities of the electrolyte solutions.

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“…XRS studies were carried out at beamlines ID20/ESRF (Sahle, Mirone et al, 2015;Huotari et al, 2017) and P01/ PETRAIII (Fig. 1).…”

Section: Methodsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

X-ray Raman spectroscopy of lithium-ion battery electrolyte solutions in a flow cell

Ketenoğlu

Spiekermann

Harder

et al. 2018

J Synchrotron Radiat

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“…Details of the experimental data processing can be found in ref. 37. After background subtraction, we normalized the B K-edge XRS spectra to their integrated intensity between 183 and 223 eV energy loss and the Ca L 2,3 -edge spectra to their integrated intensity between 345 and 373 eV energy loss.…”

Section: Methodsmentioning

confidence: 99%

Formation of CaB₆in the thermal decomposition of the hydrogen storage material Ca(BH₄)₂

Sahle

Sternemann

Giacobbe

et al. 2016

Phys. Chem. Chem. Phys.

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Using a combination of high resolution X-ray powder diffraction and X-ray Raman scattering spectroscopy at the B K- and Ca L2,3-edges, we analyzed the reaction products of Ca(BH4)2 after annealing at 350 °C and 400 °C under vacuum conditions. We observed the formation of nanocrystalline/amorphous CaB6 mainly and found only small contributions from amorphous B for annealing times larger than 2 h. For short annealing times of 0.5 h at 400 °C we observed neither CaB12H12 nor CaB6. The results indicate a reaction pathway in which Ca(BH4)2 decomposes to B and CaH2 and finally reacts to form CaB6. These findings confirm the potential of using Ca(BH4)2 as a hydrogen storage medium and imply the desired cycling capabilities for achieving high-density hydrogen storage materials.

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“…The large-solid-angle x-ray scattering spectrometer (Huotari et al, 2017) was set up with 24 Si(660) analyzer crystals for an average momentum transfer of 7.3 ± 0.2 Å −1 and an overall energy resolution of 0.7 eV. All experimental data were analyzed using the XRStools software package (Sahle et al, 2015). The integrated intensity of each spectrum was normalized over a 35 eV energy range.…”

Section: X-ray Raman and Raman Methodsmentioning

confidence: 99%

Polymerized 4-Fold Coordinated Carbonate Melts in the Deep Mantle

et al. 2019

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Our understanding of the deep carbon cycle has witnessed amazing advances in the last decade, including the discovery of tetrahedrally coordinated high pressure (P) carbonate phases. However, little is known about the physical properties of their molten counterpart at moderate depths, while their properties at lower mantle conditions remain unexplored. Here, we report the structure and density of FeCO 3 melts and glasses from 44 to 110 GPa by means of in situ x-ray synchrotron diffraction, and ex situ Raman and x-ray Raman spectroscopies. Carbon is fully transformed to 4-fold coordination, a bond change recoverable at ambient P. While low P melts react with silica, resulting in the formation of silico-carbonate glasses, high P melts are not contaminated but still quench as glasses. Carbonate melts are therefore polymerized, highly viscous and poorly reacting with silicates in the lower mantle, in stark opposition with their low P properties.

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Planning, performing and analyzing X-ray Raman scattering experiments

Abstract: A summarising review of data treatment for non-resonant inelastic X-ray scattering data from modern synchrotron-based multi-analyzer spectrometers.

Cited by 90 publications

References 64 publications

X-ray Raman spectroscopy of lithium-ion battery electrolyte solutions in a flow cell

X-ray Raman spectroscopy of lithium-ion battery electrolyte solutions in a flow cell

Formation of CaB₆in the thermal decomposition of the hydrogen storage material Ca(BH₄)₂

Polymerized 4-Fold Coordinated Carbonate Melts in the Deep Mantle

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Planning, performing and analyzing X-ray Raman scattering experiments

Abstract: A summarising review of data treatment for non-resonant inelastic X-ray scattering data from modern synchrotron-based multi-analyzer spectrometers.

Cited by 90 publications

References 64 publications

X-ray Raman spectroscopy of lithium-ion battery electrolyte solutions in a flow cell

X-ray Raman spectroscopy of lithium-ion battery electrolyte solutions in a flow cell

Formation of CaB6in the thermal decomposition of the hydrogen storage material Ca(BH4)2

Polymerized 4-Fold Coordinated Carbonate Melts in the Deep Mantle

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Product

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Formation of CaB₆in the thermal decomposition of the hydrogen storage material Ca(BH₄)₂