I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[28141]
Open Access
Abstract: This manuscript describes a workflow for automated data collection that uses a robotic arm for sample exchange, significantly improving data collection efficiency. The setup, implemented for synchrotron X-ray imaging at the Diamond Light Source (DLS) I13-2, Imaging beamline, utilizes a robot to achieve high-throughput serial tomography (3D) or imaging (2D). At present, for many experiments, the time required for manual sample exchange and alignment is comparable to, or even exceeds, the duration of the tomography scan itself. To maximize the efficient use of available beam time and increase experimental throughput, automating sample exchange and alignment is essential. Using the robot as a sample changer can increase throughput by at least 4-10 times compared to manual procedures, depending on which pixel size is chosen. With the Diamond II machine and the I13L beamlines Operando Coherent TOmography and Ptychographic Imaging (OCTOPI) upgrades, the increased X-ray flux will further reduce the experimental scan times, making the system even more efficient. Furthermore, the automation enables remote data collection, including an optional mail-in service for users. Automated sample centering allows fully unattended scanning, which can be performed remotely. This represents a unique and innovative feature of the system. This manuscript describes the complete procedure, including sample preparation, mounting on specialized holders, transport to the beamline, and placement on the dedicated trays for robotic sample exchange. The procedure for automated sample centering and the subsequent tomography reconstruction pipeline are presented.
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Jul 2026
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I13-2-Diamond Manchester Imaging
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Louis
Verschuren
,
Vladimir
Matskovsky
,
Matthieu N
Boone
,
Pieter
De Frenne
,
Tom
De Mil
,
Kristof
Haneca
,
Shashidhara
Marathe
,
Charlotte
Pearson
,
Christoph
Rau
,
Ute
Sass-Klaassen
,
Joris
Van Acker
,
Kris
Vandekerkhove
,
Kaz
Wanelik
,
Julia
Weidemüller
,
Valerie
Trouet
,
Jan
Van Den Bulcke
Diamond Proposal Number(s):
[36278]
Open Access
Abstract: Maximum latewood density of conifers is the most widely used annual-resolution summer temperature proxy. Regions with few conifers, however, remain underrepresented in global paleoclimate records. Here, we use x-ray micro–computed tomography (micro-CT) to show that latewood density measurements of European beech (Fagus sylvatica L.) in a temperate lowland forest exhibit a strong summer (May to September) temperature signal (r = 0.73; 1833 to 2022 CE). Complementary wood anatomical analyses using deep learning segmentation reveal that both vessel and fiber anatomy are key drivers of latewood density variability and its temperature sensitivity. By integrating these anatomical responses, x-ray micro-CT–based latewood density measurements generate a robust and temporally stable summer temperature signal. Our results highlight the untapped potential of broad-leaved tree species for density-based climate reconstructions in temperate regions and open previously unidentified avenues for high-resolution paleoclimatology beyond the use of conifers.
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Jul 2026
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DIAD-Dual Imaging and Diffraction Beamline
I13-2-Diamond Manchester Imaging
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Sarah
Davidson
,
Davide
Simone
,
Kathrin
Jansen
,
Max
Cowan
,
Caio
Machado
,
Ian
Reekie
,
Ananya
Bhalla
,
Rowie
Borst
,
Cesar
Prada Medina
,
Joshua
Bull
,
Zhi Yi
Wong
,
Sarah
Hill
,
Micon
Garvilles
,
Sam
Pledger
,
Patricia Reis
Nisa
,
Nora Rebecca
Schwingen
,
Dylan
Windell
,
Moustafa
Attar
,
Catherine
Disney
,
Andrew J.
Bodey
,
Alissa
Parmenter
,
Helen
Byrne
,
Sharif
Ahmed
,
Shashidhara
Marathe
,
Peter
Lee
,
Chris
Mahony
,
Adam P.
Croft
,
Stephen
Sansom
,
Mark C.
Coles
,
Christopher D.
Buckley
Diamond Proposal Number(s):
[30542, 34348]
Open Access
Abstract: The cellular basis for site-specific inflammation remains unclear. In human fingers, proximal interphalangeal (PIP) joints are preferentially affected by inflammatory arthritis, whereas distal interphalangeal joints are spared, providing a model to investigate the predilection of inflammation to distinct sites. Here we combine single-cell RNA sequencing, imaging and X-ray tomography to examine cellular composition, spatial organization and structure of finger joints during fetal development. PIP joints had a larger synovial volume and were enriched for PI16+ ‘universal’ fibroblasts. These cells were located in perivascular regions and at developing tendon–ligament interfaces. PI16+ fibroblasts exhibited both a shared inflammatory and cell-type-specific response to cytokine stimulation, suggesting that the combination of their spatial location and transcriptional responses promote inflammation. We suggest that differences in the stoichiometry of mesenchymal cells established in utero, including the key role of PI16+ fibroblasts, is a general principle that drives inflammation susceptibility across tissues.
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Jun 2026
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I13-2-Diamond Manchester Imaging
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Xuekun
Lu
,
Rhodri
Owen
,
Wenjia
Du
,
Zhenyu
Zhang
,
Antonio
Bertei
,
Roby
Soni
,
Xun
Zhang
,
Francesco
Iacoviello
,
Daqing
Li
,
Alice
Llewellyn
,
Jianuo
Chen
,
Han
Zhang
,
Xuhui
Yao
,
Qi
Li
,
Yunlong
Zhao
,
Shashidhara
Marathe
,
Christoph
Rau
,
Paul R.
Shearing
Diamond Proposal Number(s):
[29068]
Open Access
Abstract: Silicon is a promising negative electrode material for high-energy batteries, but its volume changes during cell cycling cause rapid degradation, limiting its loading to about 10 wt.% in conventional graphite/Si composite electrodes. Overcoming this threshold requires evidence-based design for the formulation of advanced electrodes. Here we combine multimodal operando imaging techniques, assisted by structural and electrochemical characterizations, to elucidate the multiscale electro-chemo-mechanical processes in graphite/Si composite negative electrodes. We demonstrate that the electrochemical cycling stability of Si particles strongly depends on the design of intraparticle nanoscale porous structures, and the encapsulation and loss of active Si particles result in excessive charging current being directed to the graphite particles, increasing the risk of lithium plating. We also show that heterogeneous strains are present between graphite and Si particles, in the carbon-binder domain and the electrode’s porous structures. Focusing on the volume expansion of the electrode during electrochemical cycling, we prove that the rate performance and Si utilization are heavily influenced by the expansion of the carbon-binder domain and the decrease in porosity. Based on this acquired knowledge, we propose a tailored double-layer graphite/Si composite electrode design that exhibits lower polarization and capacity decay compared with conventional graphite/Si electrode formulations.
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Oct 2025
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[31134]
Open Access
Abstract: Growth kinetics and orientation selection play a significant role in microstructure evolution during metal solidification, while gravity-induced convection adds significant complexity to the process. In-situ, time-resolved X-ray imaging of solidifying grain-refined Al–20 wt.% Cu alloy onboard the MASER-13 sounding rocket enabled the study of equiaxed dendrite growth under diffusion-controlled conditions, eliminating the influence of gravity. A machine learning-enabled analytical pipeline was developed to extract and evaluate the spatiotemporal behaviour of a large number of individual dendrites, including their growth characteristics, rotations and interactions. Post-flight synchrotron X-ray computed tomography and electron backscatter diffraction were used to reconstruct the three-dimensional dendrite structure with embedded details of crystallographic orientations. Correlated data analysis confirmed that most dendrites grew along directions parallel to the {100} plane under highly isothermal, diffusion-controlled conditions. However, growth along atypical directions was also observed, even in this simplified regime. The benchmark data revealed variation in dendrite arm evolution, influenced by local grain interactions and crystallographic orientation selection. It is shown that the equiaxed grains have random crystallographic orientations and evidence suggests that these survive from shortly after nucleation in the bulk liquid under microgravity conditions. The data processing protocols demonstrated here highlight the potential of integrating advanced experimental techniques with modern data science approaches to analyse solidification microstructure formation in metallic alloys under terrestrial and microgravity conditions.
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Oct 2025
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[35733]
Open Access
Abstract: This research examines the dynamics of reactive CO2 transport in carbonate rock, focusing on the impact of carbonic acid-induced formation damage. We provide real-time visualization of these processes by employing four-dimensional (4D) high-resolution synchrotron imaging at the I13 beamline hosted at the Diamond Light Source. We visualize and quantify the temporal effects of reactive CO2 transport at the pore scale in carbonate rock. The experiment involved injecting CO2-saturated brine through the sample with in situ scanning to track the different stages of chemical dissolution. Analysis of the images shows a channelled dissolution pattern which corresponds with a gradual increase in porosity due to pore structure changes. Pore network models were generated from the segmented images to carry out a sequence of drainage and imbibition simulations. The result demonstrated that reduced capillary entry pressure with increased pore connectivity after dissolution. Furthermore, the trapping efficiency was quantified to predict a slight decrease in dissolution as the pores become broader and better connected.
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Oct 2025
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I13-2-Diamond Manchester Imaging
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Dominic L. R.
Melvin
,
Marco
Siniscalchi
,
Dominic
Spencer-Jolly
,
Bingkun
Hu
,
Ziyang
Ning
,
Shengming
Zhang
,
Junfu
Bu
,
Shashidhara
Marathe
,
Anne
Bonnin
,
Johannes
Ihli
,
Gregory J.
Rees
,
Patrick S.
Grant
,
Charles W.
Monroe
,
T. James
Marrow
,
Guanchen
Li
,
Peter G.
Bruce
Diamond Proposal Number(s):
[30683]
Open Access
Abstract: Avoiding lithium dendrites at the lithium/ceramic electrolyte interface and, as a result, avoiding cell short circuit when plating at practical current densities remains a significant challenge for all-solid-state batteries. Typically, values are limited to around 1 mA cm−2, even, for example, for garnets with a relative density of >99%. It is not obvious that simply densifying ceramic electrolytes will deliver high plating currents. Here we show that plating currents of 9 mA cm−2 can be achieved without dendrite formation, by densifying argyrodite, Li6PS5Cl, to 99%. Changes in the microstructure of Li6PS5Cl on densification from 83 to 99% were determined by focused ion beam-scanning electron microscopy tomography and used to calculate their effect on the critical current density (CCD). Modelling shows that not all changes in microstructure with densification act to increase CCD. Whereas smaller pores and shorter cracks increase CCD, lower pore population and narrower cracks act to decrease CCD. Calculations show that the former changes dominate over the latter, predicating an overall increase in CCD, as observed experimentally.
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Sep 2025
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I13-2-Diamond Manchester Imaging
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Iain
Malone
,
Secil
Unsal
,
R. Scott
Young
,
Matthew P.
Jones
,
Francesco
Spanu
,
Shashidhara
Marathe
,
Rhodri
Jervis
,
Hugh G. C.
Hamilton
,
Christopher M.
Zalitis
,
Thomas S.
Miller
,
Alexander J. E.
Rettie
Diamond Proposal Number(s):
[35192]
Open Access
Abstract: Anion exchange membrane water electrolysers are held back by the low durability of the ionomer in the membrane and catalyst layers. Studying ionomer degradation in these systems is challenging because the main mechanisms - which result in catalyst detachment, membrane thinning, and loss of cationic functionality - have opposing effects on the cell potential. Electrochemical measurements alone are therefore insufficient for elucidating the underlying causes of degradation. To address this, a bespoke miniature-electrolyser-cell is developed for X-ray microtomography imaging of membrane electrode assemblies at 1.6 µm resolution. This setup enables the study of the entire active volume of the electrolyser under static and operando conditions and is validated against standard 5 cm2 laboratory cells. An operando investigation of degradation in Fumasep-based catalyst-coated membranes reveals both significant membrane thinning and loss of membrane ionic conductivity during stability testing, leading to increased ohmic resistance and cell potential. In contrast, a Selemion membrane shows minimal changes in thickness and conductivity and is significantly more stable compared to Fumasep when exposed to synchrotron radiation. This platform has relevance for operando studies of electrochemical materials and devices generally, including proton exchange membrane electrolysers, fuel cells, and CO2 electrolysers using both lab-based and synchrotron X-ray sources.
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Sep 2025
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I13-2-Diamond Manchester Imaging
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Abstract: Cell behaviour and tissue development are inherently sensitive to morphological features of tissue-engineered scaffolds. Traditionally, imaging techniques such as SEM, TEM, AFM, and CLSM provide high-resolution 2D images to characterise scaffold morphology. However, these techniques have poor penetration and low resolution transversely to the sliced planes. In contrast, synchrotron radiation X-ray micro-computed tomography (SR-µCT) enables 3-D imaging of large volumes with submicron isotropic resolution.
We used SR-µCT at beamline I13-2 (Diamond Light Source) to image jet-sprayed nonwoven fibrous scaffolds used in the Harefield Valve, both with and without human adipose-derived stem cells preserved in ethanol to maintain native wet conditions. Large-volume imaging was achieved by stitching 2x2 tiled datasets and reconstructing them into 1 mm³ volumes at 0.325 µm voxel size, enabling clear scaffold.
The scaffold exhibited a layered, transversely isotropic structure, with additional in-plane anisotropy observed when using high-speed drum fabrication. SR-µCT revealed significantly higher scaffold porosity compared to SEM analysis, which consistently underestimates porosity due to limited depth and connectivity information. Cell distribution and morphology showed that cells preferentially adhered and proliferated along in-plane structures at full scaffold colonisation. We hypothesise that the cells minimise energy expenditure by expanding in directions of least resistance.
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Sep 2025
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I13-2-Diamond Manchester Imaging
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Josh
Williams
,
Rudolf
Hellmuth
,
Yuan-Tsan
Tseng
,
Marta
Pena Fernandez
,
Oriol
Roche I Morgo
,
Yunpeng
Jia
,
Marco
Endrizzi
,
Kazimir
Wenelik
,
Leonard
Turpin
,
Shashidhara
Marathe
,
Magdi
Yacoub
Abstract: Micro-computational tomography (µCT) is a useful technique for acquiring 3-D imaging of tissue-engineered scaffolds for morphology characterisation and analysis of the mechanical interactions between scaffold and cells. We used synchrotron light µCT at Diamond Light Source (UK) to image jet-sprayed nonwoven fibrous scaffolds, with and without human adipose-derived stem cells.
Large-volume imaging was achieved by stitching 2×2 tiled datasets and reconstructing them into 1 mm³ volumes at sub-micron resolution, enabling clear scaffold segmentation from the background. However, cells and fibres produce the same X-ray attenuation, this provides challenges in segmentation between fibres and cells. A deep learning algorithm with morphological recognition was employed. It enabled rapid selective segmentation, which allowed the analysis of cell distribution and morphology, revealing that cells preferentially adhered and proliferated along in-plane structures at full scaffold colonisation. We hypothesise that the cells minimise energy expenditure by expanding in directions of least resistance.
This process for analysing tissue-engineered scaffold opens new avenues for rapid, non-destructive, high-resolution, large-volume characterisation to elucidate cell and structural interaction.
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Sep 2025
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