DIAD-Dual Imaging and Diffraction Beamline
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James
Le Houx
,
Daniel
Mckay Fletcher
,
Alberto
Leonardi
,
Katherine A.
Williams
,
Nancy
Walker
,
Fernando
Alvarez-Borges
,
Ebrahim
Afsar Dizaj
,
Madhu
Murthy
,
Ronan
Smith
,
Liam
Perera
,
Navid
Aslani
,
Andrew
James
,
Sharif
Ahmed
,
Tiina
Roose
,
Siul
Ruiz
Diamond Proposal Number(s):
[30961, 32138, 33343]
Open Access
Abstract: Soil compaction and escalating global drought increase soil strength and stiffness. It remains unclear which plant root biomechanical mechanisms/traits enable growth in these harsh conditions. Here, we combine synchrotron X-ray computed tomography with spatially resolved X-ray diffraction to characterize the biomechanics of a replica root-soil system. We map the strain field around the root tip analog, finding strong agreement with finite element simulations, thereby demonstrating a promising new in vivo measurement protocol.
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Jul 2025
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Open Access
Abstract: Natural marine sediments are heterogeneous with respect to sediment-physical properties, and have a wide range in composition and structures. For many years, sediment-physical characterization has relied primarily on laboratory experiments. However, the investigation of small-(grain-)scale sedimentary structures, which appear to control many sediment (re-)depositional and emplacement mechanisms, requires new analytical methods. Here, we test high-resolution X-ray synchrotron micro-tomography (μCT) to qualitatively and quantitatively investigate structural differences, in 3D, between two lithological end-member types of marine sediments: a coarse-grained, sandy sediment and a fine-grained, silty-clay sediment. Our results show clear compositional and structural differences between the two end-members, as well as between samples taken from the same lithological unit. These differences can be attributed partly to different sediment types, that is, coarse-versus fine-grained sediments, but also reveal a dependency on the sedimentation regime. We find that pore space distribution is highly spatially variable, even down to a sub-millimeter scale. Such high variability in porosity would be missed by standard geotechnical experiments, which only provide information averaged over far larger sediment samples. The identification of small-(grain-)scale changes in pore space, however, directly impacts sediment properties such as permeability, which in turn is crucial for the understanding of geological processes such as fluid flow and storage capacity of sediments and assessing hazards such as the preconditioning of submerged slopes to collapse. Our results therefore demonstrate the potential of μCT to investigate the internal structure of natural sediments, obtaining information that is not resolved or lost in data acquired through other analytical methods.
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Apr 2025
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DIAD-Dual Imaging and Diffraction Beamline
I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[32980]
Open Access
Abstract: Machine learning techniques are being increasingly applied in medical and physical sciences across a variety of imaging modalities; however, an important issue when developing these tools is the availability of good quality training data. Here we present a unique, multimodal synchrotron dataset of a bespoke zinc-doped Zeolite 13X sample that can be used to develop advanced deep learning and data fusion pipelines. Multi-resolution micro X-ray computed tomography was performed on a zinc-doped Zeolite 13X fragment to characterise its pores and features before spatially resolved X-ray diffraction computed tomography was carried out to characterise the topographical distribution of sodium and zinc phases. Zinc absorption was controlled to create a simple, spatially isolated, two-phase material. Both raw and processed data are available as a series of Zenodo entries. Altogether we present a spatially resolved, three-dimensional, multimodal, multi-resolution dataset that can be used to develop machine learning techniques. Such techniques include the development of super-resolution, multimodal data fusion, and 3D reconstruction algorithms.
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Feb 2025
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DIAD-Dual Imaging and Diffraction Beamline
I12-JEEP: Joint Engineering, Environmental and Processing
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Franck P.
Vidal
,
Shaghayegh
Afshari
,
Sharif
Ahmed
,
Carolyn
Atkins
,
Eric
Béchet
,
Alberto
Corbi Bellot
,
Stefan
Bosse
,
Younes
Chahid
,
Cheng-Ying
Chou
,
Robert
Culver
,
Lewis
Dixon
,
Johan
Friemann
,
Amin
Garbout
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Clémentine
Hatton
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Audrey
Henry
,
Christophe
Leblanc
,
Alberto
Leonardi
,
Jean Michel
Létang
,
Harry
Lipscom
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Tristan
Manchester
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Bas
Meere
,
Simon
Middleburgh
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Iwan
Mitchell
,
Liam
Perera
,
Marti
Puig Fantauzzi
,
Jenna
Tugwell-Allsup
Diamond Proposal Number(s):
[29820]
Abstract: gVirtualXray (gVXR) is an open-source framework that relies on the Beer-Lambert law to simulate x-ray images in real time on a graphics processor unit (GPU) using triangular meshes. A wide range of programming languages is supported (C/C++, Python, R, Ruby, Tcl, C#, Java, and GNU Octave). Simulations generated with gVXR have been benchmarked with clinically realistic phantoms (i.e. complex structures and materials) using Monte Carlo (MC) simulations, real radiographs and real digitally reconstructed radiographs (DRRs), and x-ray computed tomography (CT). It has been used in a wide range of applications, including real-time medical simulators, proposing a new densitometric radiographic modality in clinical imaging, studying noise removal techniques in fluoroscopy, teaching particle physics and x-ray imaging to undergraduate students in engineering, and XCT to masters students, predicting image quality and artifacts in material science, etc. gVXR has also been used to produce a high number of realistic simulated images in optimization problems and to train machine learning algorithms. This paper presents applications of gVXR related to XCT.
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Oct 2024
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DIAD-Dual Imaging and Diffraction Beamline
I11-High Resolution Powder Diffraction
I12-JEEP: Joint Engineering, Environmental and Processing
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Open Access
Abstract: The plumes of Enceladus contain a non-ice component that originates from aqueous processes occurring within the interior 1,2. The ocean of Enceladus is thought to be connected to the surface across a range of time scales. These processes range from the rapid eruption of cryovolcanic plumes to slow crustal convection on geological timescales3,4. In every case, the system will have a temperature and geochemical evolution as it freezes, with the history of evolution recorded in the sequence of mineral precipitation. Analogously to igneous and metamorphic petrology, we can explore the mineralogy and its context to reconstruct the history of that sample. Most importantly, for astrobiological investigations, the formation and cryo-petrological study of inorganic salts can be used to identify sites of recent exposure on the surface.
Synchrotron X-ray techniques allow fast, high-resolution probing of these systems with X-ray light. By exploring large, multi-component samples with multiple techniques, with variable temperature over time we can reveal many emergent processes that may not be predictable with simple phase diagrams.
We use a combination of synchrotron powder X-ray diffraction (PXRD) and X-ray microtomography (µCT) across multiple beamlines at Diamond Light Source (I11, I12 and DIAD). Using a multi-modal approach, we present an in-situ study of the low-temperature phase behaviour of Na-Cl-HCO3 fluids. We employ K11-DIAD (Dual Imaging and Diffraction) to carry out ‘image-guided diffraction’ on an Enceladus-type sample frozen in real-time. DIAD’s unique capabilities allow us not only to study microstructure down to 1 µm but also to carry out spatially resolved XRD and identify solid phases present.
We present, for the first time, the use of dual imaging and diffraction of a Na-Cl-CO₃ solution frozen in real time in 3 dimensions [Figure 1]. DIAD’s imaged guided diffraction provides spatially-resolved XRD, allowing us to probe different regions of our sample and identify the formation of Na2CO₃ hydrates. We show the influence of carbonate chemistry on the sequence of cryogenic precipitation and the development of complex microstructures. These results provide insights into crustal transport processes and will help with interpreting observational data from upcoming Galilean missions.
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Sep 2024
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Abstract: The aqueous Al-ion battery potentially has improved safety and environmental advantages over the incumbent lithium-ion technology [1,2]. Using 3D carbon-felt matrix electrodes, the performance of these batteries can be optimised. Typically, the electrodes are compressed to improve electrical conductivity by improving contact between adjacent fibres, which also closes the electrolyte pores, reducing the ionic diffusivity [3]. In this work, we set out to understand the role of electrode compression on the interplay between these key performance parameters for the aq. Al-ion battery.
Synchrotron X-ray computed tomography was used to examine the 3D morphology of the carbon felt electrodes under 11 different compression ratios [4]. A bespoke in-situ tensile/compression rig was used to measure displacement and loading for three electrode types: raw carbon felt, positive electrodes loaded with a copper hexacyanoferrate ink and negative electrodes loaded with TiO2 anatase powder. Data was acquired using two voxel sizes (330nm, and 540nm) to compare the effects of spatial resolution and imaged volume size on subsequent image analysis. The tomograms were reconstructed using Paganin phase retrieval, to improve the contrast of the weakly attenuating carbon, and a filtered back projection algorithm. A U-net convolutional neural network was trained on uncompressed, fully compressed and partially compressed (three volumes) data, and then used to fully segment all tomograms.
A high-throughput, image-based model was then used to analyse how compression affects the porosity, tortuosity, volume-specific area, ionic diffusivity, and electrical conduction of the electrodes. A finite differences-based model was used to solve the equilibrium partial differential equations directly on the voxel datasets, with no additional regularisation [5]. The heterogeneity of the electrode samples is quantified by comparing the effect of representative elementary volume on the value of the computed parameters [6]. Finally, aq. Al-ion batteries are manufactured using the predicted optimal compression ratio and compared to the simulated results.
This is the first in-situ study of the compression effect on the aqueous aluminium-ion battery, and the largest XCT-based modelling study known to the authors (99 XCT tomograms). This work aims to improve the understanding of the effect of manufacturing parameters on the aqueous Al-ion battery and other similar batteries, and ultimately, its performance.
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Aug 2024
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DIAD-Dual Imaging and Diffraction Beamline
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Himanshu
Vashishtha
,
Parastoo
Jamshidi
,
Anastasia
Vrettou
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Anna
Kareer
,
Michael
Goode
,
Hans
Deyhle
,
Andrew
James
,
Sharif
Ahmed
,
Christina
Reinhard
,
Moataz M.
Attallah
,
David M.
Collins
Diamond Proposal Number(s):
[28029]
Open Access
Abstract: This study explores cardiovascular stents fabricated using laser powder bed fusion (LPBF) which is an emerging method to offer patient-specific customisable parts. Here, the shape memory alloy NiTi, in a near equiatomic composition, was investigated to deconvolve the material response from macroscopic component effects. Specifically, stress-geometry interactions were revealed, in-situ, for a minaturised cardiovascular stent subjected to an externally applied cylindrical stress whilst acquiring synchrotron X-ray imaging and diffraction data. The approach enabled the collection of spatially resolved micromechanical deformation data; the formation of stress-induced martensite and R-phase was evident, occurring in locations near junctions between stent ligaments where stress concentrations exist. In the as-fabricated condition, hardness maps were obtained through nanoindentation, demonstrating that the localised deformation and deformation patterning is further controlled by porosity and microstructural heterogeneity. Electron backscatter diffraction (EBSD) supported these observations, showing a finer grain structure near stent junctions with higher associated lattice curvature. These features, combined with stress concentrations when loaded will initiate localised phase transformations. If the stent was subjected to repeated loading, representing in-vivo conditions, these regions would be susceptible to cyclic damage through transformation memory loss, leading to premature component failure. This study highlights the challenges that must be addressed for the post-processing treatment of LPBF-processed stents for healthcare-related applications.
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Jul 2024
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Open Access
Abstract: Understanding when gravel moves in river beds is essential for a range of different applications but is still surprisingly hard to predict. Here we consider how our ability to predict critical shear stress (τc) is being improved by recent advances in two areas: (1) identifying the onset of bedload transport; and (2) quantifying grain-scale gravel bed structure. This paper addresses these areas through both an in-depth review and a comparison of new datasets of gravel structure collected using three different methods. We focus on advances in these two areas because of the need to understand how the conditions for sediment entrainment vary spatially and temporally, and because spatial and temporal changes in grain-scale structure are likely to be a major driver of changes in τc. We use data collected from a small gravel-bed stream using direct field-based measurements, terrestrial laser scanning (TLS) and computed tomography (CT) scanning, which is the first time that these methods have been directly compared. Using each method, we measure structure-relevant metrics including grain size distribution, grain protrusion and fine matrix content. We find that all three methods produce consistent measures of grain size, but that there is less agreement between measurements of grain protrusion and fine matrix content.
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Apr 2024
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Open Access
Abstract: Understanding when gravel moves in river beds is essential for a range of different applications, but is still surprisingly hard to predict. The critical shear stress at which a grain will move depends on its relative size and structure within the bed, and spatial and temporal changes in grain-scale structure are likely to be a major driver of changes in critical shear stress. Consequently grain-structure metrics such as protrusion, pivot angle and contact with any surrounding fine grained matrix are used as parameters in models to predict critical shear stress, and so there is an increasing demand for measurements of these parameters in order to improve our predictive ability. However, we do not have established methods for measuring these parameters, nor do we know whether different methods provide consistent results. Here we present and compare new datasets of sediment structure metrics collected from eight locations in a small gravel-bed stream using three different methods: direct field-based measurements, terrestrial laser scanning (TLS), and computed tomography (CT) scanning. Using each method, we measure metrics including grain size distribution, grain protrusion and fine matrix content. We find that distributions of grain size are consistent between field-based and TLS data, but smaller in CT data. All three methods produce similar distributions of protrusion relative to grain size. There is also some consistency between field and CT measures of fine-grained matrix. However, the identification of similarity also depends on the type of analysis, and an alternative analysis shows less similarity in protrusion and fine-grained matrix between the different methods. Of the three methods, TLS-based approaches have potential to be most easily applied, and our analysis suggests that for grain-size and protrusion they perform as well as the alternative methods. However, they cannot currently be used for measuring fine-grained matrix content.
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Mar 2024
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DIAD-Dual Imaging and Diffraction Beamline
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Cyril
Besnard
,
Ali
Marie
,
Sisini
Sasidharan
,
Hans
Deyhle
,
Andrew M.
James
,
Sharif I.
Ahmed
,
Christina
Reinhard
,
Robert A.
Harper
,
Richard M.
Shelton
,
Gabriel
Landini
,
Alexander M.
Korsunsky
Diamond Proposal Number(s):
[28054]
Open Access
Abstract: The Dual Imaging and Diffraction (DIAD) beamline at Diamond Light Source (Didcot, U.K.) implements a correlative approach to the dynamic study of materials based on concurrent analysis of identical sample locations using complementary X-ray modalities to reveal structural detail at various length scales. Namely, the underlying beamline principle and its practical implementation allow the collocation of chosen regions within the sample and their interrogation using real-space imaging (radiography and tomography) and reciprocal space scattering (diffraction). The switching between the two principal modes is made smooth and rapid by design, so that the data collected is interlaced to obtain near-simultaneous multimodal characterization. Different specific photon energies are used for each mode, and the interlacing of acquisition steps allows conducting static and dynamic experiments. Building on the demonstrated realization of this state-of-the-art approach requires further refining of the experimental practice, namely, the methods for gauge volume collocation under different modes of beam–sample interaction. To address this challenge, experiments were conducted at DIAD devoted to the study of human dental enamel, a hierarchical structure composed of hydroxyapatite mineral nanocrystals, as a static sample previously affected by dental caries (tooth decay) as well as under dynamic conditions simulating the process of acid demineralization. Collocation and correlation were achieved between WAXS (wide-angle X-ray scattering), 2D (radiographic), and 3D (tomographic) imaging. While X-ray imaging in 2D or 3D modes reveals real-space details of the sample microstructure, X-ray scattering data for each gauge volume provided statistical nanoscale and ultrastructural polycrystal reciprocal-space information such as phase and preferred orientation (texture). Careful registration of the gauge volume positions recorded during the scans allowed direct covisualization of the data from two modalities. Diffraction gauge volumes were identified and visualized within the tomographic data sets, revealing the underlying local information to support the interpretation of the diffraction patterns. The present implementation of the 4D microscopy paradigm allowed following the progression of demineralization and its correlation with time-dependent WAXS pattern evolution in an approach that is transferable to other material systems.
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Mar 2024
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