Very large-scale diffraction investigations enabled by a matrix-multiplication facilitated radial and azimuthal integration algorithm: <i>MatFRAIA</i>

Jensen, Alexander Bernthz; Christensen, Thorbjørn Erik Køppen; Weninger, Clemens; Birkedal, Henrik

doi:10.1107/s1600577522008232

Cited by 16 publications

(12 citation statements)

References 24 publications

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“…The collected detector images were azimuthally integrated with the MatFRAIA software (Jensen et al, 2022) to obtain one-dimensional intensity versus scattering angle datasets. A Rietveld model was refined against each PXRD dataset in batch mode using the TOPAS academic software (Coelho, 2018).…”

Section: Discussionmentioning

confidence: 99%

Beam damage in operando X-ray diffraction studies of Li-ion batteries

Christensen¹,

Karlsen²,

Drejer³

et al. 2023

J Synchrotron Rad

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Operando powder X-ray diffraction (PXRD) is a widely employed method for the investigation of structural evolution and phase transitions in electrodes for rechargeable batteries. Due to the advantages of high brilliance and high X-ray energies, the experiments are often carried out at synchrotron facilities. It is known that the X-ray exposure can cause beam damage in the battery cell, resulting in hindrance of the electrochemical reaction. This study investigates the extent of X-ray beam damage during operando PXRD synchrotron experiments on battery materials with varying X-ray energies, amount of X-ray exposure and battery cell chemistries. Battery cells were exposed to 15, 25 or 35 keV X-rays (with varying dose) during charge or discharge in a battery test cell specially designed for operando experiments. The observed beam damage was probed by µPXRD mapping of the electrodes recovered from the operando battery cell after charge/discharge. The investigation reveals that the beam damage depends strongly on both the X-ray energy and the amount of exposure, and that it also depends strongly on the cell chemistry, i.e. the chemical composition of the electrode.

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Section: Discussionmentioning

confidence: 99%

Beam damage in operando X-ray diffraction studies of Li-ion batteries

Christensen¹,

Karlsen²,

Drejer³

et al. 2023

J Synchrotron Rad

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show abstract

“…The collected detector images were azimuthally integrated with the MatFRAIA software (Jensen et al, 2022) to obtain one dimensional intensity vs. scattering angle datasets. A Rietveld model was refined against each PXRD dataset in batch mode using TOPAS academic software.…”

Section: Discussionmentioning

confidence: 99%

Beam damage in operando X-ray diffraction studies of Li-ion batteries

Christensen

Karlsen

Drejer

et al. 2022

Preprint

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Operando powder X-ray diffraction (PXRD) is a widely employed method for investigation of structural evolution and phase transitions in electrodes for rechargeable batteries. Due to the advantages of high brilliance and high X-ray energies, the experiments are often carried out at synchrotron facilities. It is known that the X-ray exposure can cause beam damage in the battery cell resulting in hindrance of the electrochemical reaction. In this study, we investigate the extent of X-ray beam damage during operando powder X-ray diffraction synchrotron experiments of battery materials with varying X-ray energies, amount of X-ray exposure and battery cell chemistries. Battery cells were exposed to 15, 25, or 35 keV X-rays (with varying dose) during charge or discharge in a battery tests cell specially designed for operando experiments. The observed beam damage was probed by µPXRD mapping of the electrodes recovered from the operando battery cell after charge/discharge. Our investigation reveals that beam damage depends strongly both on X-ray energy, amount of exposure and that it depends strongly on the cell chemistry, i.e. the chemical composition of the electrode.

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“…The XRD data were integrated using the MatFRAIA algorithm (Jensen et al, 2022) implemented at several beamlines at MAX IV including NanoMAX (Bjorling et al, 2021) and DanMAX (Jensen et al, 2022). This resulted in 1D diffraction patterns usable for phase composition analysis.…”

Section: Data Treatmentmentioning

confidence: 99%

“…The P06 data were also integrated to azimuthally resolved diffraction data (360 azimuthal angular bins) for orientation analysis. The orientations of mineral crystallites and chitin were analysed using the angular Gaussian fitting (AGUF) method (Jensen et al, 2022) that fits the azimuthal intensity distribution of a Bragg peak in a variation of the methods previously used for small-angle X-ray scattering (SAXS) data (To ¨rnquist et al, 2020;Bu ¨nger et al, 2010;Rinnerthaler et al, 1999;Fratzl et al, 1996). The AGUF analysis was performed on the calcite (104) and (110) peaks as well as the chitin (013) peak.…”

Section: Data Treatmentmentioning

confidence: 99%

“…This made it possible to carry out a positionally resolved orientation analysis on the two regions scanned. This was performed on a peak-by-peak basis using the AGUF method (Jensen et al, 2022) that fits the azimuthal intensity distribution. We note that a different technique for orientation analysis, also based on the azimuthal scattering angle, has previously been used on the tail armour of the stomatopod (Zhang et al, 2016); this method is visualized in full 3D, which is not possible for scans of the size used in the present work.…”

Section: Data Treatmentmentioning

confidence: 99%

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Flexible design in the stomatopod dactyl club

Christensen¹,

Chua²,

Wittig³

et al. 2023

Int Union Crystallogr J

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The stomatopod is a fascinating animal that uses its weaponized appendage dactyl clubs for breaking mollusc shells. Dactyl clubs are a well studied example of biomineralized hierarchical structures. Most research has focused on the regions close to the action, namely the impact region and surface composed of chitin and apatite crystallites. Further away from the site of impact, the club has lower mineralization and more amorphous phases; these areas have not been as actively studied as their highly mineralized counterparts. This work focuses on the side of the club, in what is known as the periodic and striated regions. A combination of laboratory micro-computed tomography, synchrotron X-ray diffraction mapping and synchrotron X-ray fluorescence mapping has shown that the mineral in this region undergoes the transition from an amorphous to a crystalline phase in some, but not all, clubs. This means that this side region can be mineralized by either an amorphous phase, calcite crystallites or a mixture of both. It was found that when larger calcite crystallites form, they are organized (textured) with respect to the chitin present in this biocomposite. This suggests that chitin may serve as a template for crystallization when the side of the club is fully mineralized. Further, calcite crystallites were found to form as early as 1 week after moulting of the club. This suggests that the side of the club is designed with a significant safety margin that allows for a variety of phases, i.e. the club can function independently of whether the side region has a crystalline or amorphous mineral phase.

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Very large-scale diffraction investigations enabled by a matrix-multiplication facilitated radial and azimuthal integration algorithm: MatFRAIA

Cited by 16 publications

References 24 publications

Beam damage in operando X-ray diffraction studies of Li-ion batteries

Beam damage in operando X-ray diffraction studies of Li-ion batteries

Beam damage in operando X-ray diffraction studies of Li-ion batteries

Flexible design in the stomatopod dactyl club

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