Using 4D synchrotron X-ray microtomography rigs for time-resolved X-ray diffraction experiments: applications with the Mjölnir suite
Abstract
Synchrotron 4D X-ray microtomography provides unique insights into evolving microstructures during deformation, fluid flow and mineral transformations, but offers limited access to crystallographic information such as phase composition, lattice strain, and stress. Conversely, synchrotron X-ray diffraction (XRD) provides direct crystallographic measurements but is commonly restricted to small sample volumes and specialised sample environments. Here, we demonstrate the use of the Mjölnir and Heitt Mjölnir miniature triaxial deformation rigs, originally developed for 4D synchrotron microtomography, as platforms for time-resolved high-energy XRD experiments. Using experiments performed at beamline I15 (Diamond Light Source) supported by theoretical analysis, we evaluate diffraction contributions from pressure vessels and ancillary components, establish practical beamline setup and acquisition procedures, and assess controls on diffraction quality. We show that high-quality diffraction data can be acquired through X-ray-transparent pressure vessels, enabling phase identification, reaction tracking and lattice-strain measurements in representative sample volumes of geological materials. The rotational symmetry of the rigs further enables rocking, sweeping and mapping acquisition strategies, improving powder statistics while preserving realistic sample geometries and boundary conditions. These results provide a practical framework for integrating XRD with synchrotron microtomography and open new opportunities for linking crystallographic evolution to four-dimensional microstructural evolution during in situ experiments.
Related
- Mineralogical Compositions of Mining Resources by Rietveld Simulation of High-Resolution Synchrotron X-Ray Diffraction
- Operando Synchrotron X-ray Diffraction Study of Reference Electrode: Impact, Accuracy and Stability in Lithium-ion Pouch Cells
- High-resolution in situ analysis of biomass pyrolysis by combining quantitative synchrotron μCT and 3D particle-resolved simulations
- Integrating Ion Mobility–Resolved Tandem Mass Spectrometry and Microcrystal Electron Diffraction for Structural Elucidation
- Frequency-resolved ultrafast electron diffraction: visualizing vibrational dynamics in frequency- and real-space
BibTeX
@misc{freitas2026using,
title = {{Using 4D synchrotron X-ray microtomography rigs for time-resolved X-ray diffraction experiments: applications with the Mjölnir suite}},
author = {Damien Freitas and Dominik Daisenberger and Simon Hunt and Ian Butler and Danielle Duggins and James Gilgannon and Christina Reinhard and Zhixin Liang and Neil Bourne},
howpublished = {EarthArXiv},
year = {2026},
month = oct,
doi = {10.31223/x5jz35},
url = {https://eartharxiv.org/repository/view/15478/},
note = {CC BY 4.0},
}
RIS
TY - UNPB
TI - Using 4D synchrotron X-ray microtomography rigs for time-resolved X-ray diffraction experiments: applications with the Mjölnir suite
AU - Damien Freitas
AU - Dominik Daisenberger
AU - Simon Hunt
AU - Ian Butler
AU - Danielle Duggins
AU - James Gilgannon
AU - Christina Reinhard
AU - Zhixin Liang
AU - Neil Bourne
PY - 2026
DA - 2026/10/12
PB - EarthArXiv
DO - 10.31223/x5jz35
UR - https://eartharxiv.org/repository/view/15478/
AB - Synchrotron 4D X-ray microtomography provides unique insights into evolving microstructures during deformation, fluid flow and mineral transformations, but offers limited access to crystallographic information such as phase composition, lattice strain, and stress. Conversely, synchrotron X-ray diffraction (XRD) provides direct crystallographic measurements but is commonly restricted to small sample volumes and specialised sample environments. Here, we demonstrate the use of the Mjölnir and Heitt Mjölnir miniature triaxial deformation rigs, originally developed for 4D synchrotron microtomography, as platforms for time-resolved high-energy XRD experiments. Using experiments performed at beamline I15 (Diamond Light Source) supported by theoretical analysis, we evaluate diffraction contributions from pressure vessels and ancillary components, establish practical beamline setup and acquisition procedures, and assess controls on diffraction quality. We show that high-quality diffraction data can be acquired through X-ray-transparent pressure vessels, enabling phase identification, reaction tracking and lattice-strain measurements in representative sample volumes of geological materials. The rotational symmetry of the rigs further enables rocking, sweeping and mapping acquisition strategies, improving powder statistics while preserving realistic sample geometries and boundary conditions. These results provide a practical framework for integrating XRD with synchrotron microtomography and open new opportunities for linking crystallographic evolution to four-dimensional microstructural evolution during in situ experiments.
ER -