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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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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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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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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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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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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Matthew P.
Jones
,
Huw C. W.
Parks
,
Alice V.
Llewellyn
,
Hamish T.
Reid
,
Chun
Tan
,
Aaron
Wade
,
Thomas M. M.
Heenan
,
Francesco
Iacoviello
,
Shashidhara
Marathe
,
Paul R.
Shearing
,
Rhodri
Jervis
Diamond Proposal Number(s):
[28650]
Open Access
Abstract: During battery operation, cracking occurs in Nickel Manganese Cobalt (NMC) oxide secondary particles. Cracked particles appear darker in micro-computed tomography (micro-CT) images due to the partial volume effect, where voxels containing both void and solid yield intermediate grey-levels. This work presents an automated method for tracking grey-level changes caused by this effect in large, statistically meaningful micro-CT datasets containing over 10 000 individual particles. It extends earlier work using the GREAT algorithm to analyze NMC particles in tomography images. The new GREAT2 algorithm increases processing speed, from around 1,400 particles per day with GREAT to over 10 000 particles in under a minute. Furthermore, this work introduces methods for automated tracking of grey-level intensity changes in individual particles through different states of charge in an operando experiment. This capability enables temporal analysis of particle degradation mechanisms. Additional data processing methods are presented that extract useful insights. Through this work we show that the large sample sizes, enabled by this method and GREAT2, allow for statistically robust analysis of particle populations. These advances significantly accelerate the tomographic study of cracking in battery electrodes. The GREAT2 algorithm and associated workflows have been made available as the GRAPES Python toolkit.
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Jun 2025
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I13-2-Diamond Manchester Imaging
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Huw C. W.
Parks
,
Matthew
Jones
,
Aaron
Wade
,
Alice
Llewellyn
,
Chun
Tan
,
Hamish
Reid
,
Ralf
Ziesche
,
Thomas M. M.
Heenan
,
Shashidhara
Marathe
,
Christoph
Rau
,
Paul R.
Shearing
,
Rhodri
Jervis
Diamond Proposal Number(s):
[28650]
Open Access
Abstract: To understand fracture behaviour in battery materials, X-ray computed tomography (X-ray CT) has become the primary technique for non-destructive particle and crack analysis. Cracking causes performance decline in polycrystalline NMC811 by exposing new surfaces for parasitic electrolyte reactions and disconnecting active material from the electrode matrix. First cycle crack formation has been documented, but definitive electrochemically induced particle fracture is challenging to assess due to complex sample preparation and high-resolution X-ray imaging requirements. Presented here is an operando X-ray CT technique that enables accurate observation of fracture behaviour during de-/lithiation. A non-linear relationship between fracture behaviour and cell voltage was uncovered, and evidence of particle reformation during re-lithiation. Using a grey level analysis algorithm for fracture detection, we expedite damage evaluation in several thousands of particles throughout the electrochemical process, understanding crack initiation, propagation, and closure on a large, statistical scale and give the ability to track any one of the thousands of particles through its individual electrochemical history. Additionally, we explore the effects of continued volumetric hysteresis on particle damage. For the first time, we demonstrate the complex plurality of fracture behaviour in commercial lithium-ion battery materials, aiding in designing mitigation strategies against particle fracture.
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Mar 2025
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[34473]
Open Access
Abstract: Molluscan brains are composed of morphologically consistent and functionally interrogable neurons, offering rich opportunities for understanding how neural circuits drive behavior. Nonetheless, detailed component-level CNS maps are often lacking, total neuron numbers are unknown, and organizational principles remain poorly defined, limiting a full and systematic characterization of circuit operation. Here, we establish an accessible, generalizable approach, harnessing synchrotron X-ray tomography, to rapidly determine the three-dimensional structure of the multimillimeter-scale CNS of Lymnaea. Focusing on the feeding ganglia, we generate a full neuron-level reconstruction, revealing key design principles and revising cell count estimates upward threefold. Our atlas uncovers the superficial but also nonsuperficial ganglionic architecture, reveals the cell organization in normally hidden regions—ganglionic “dark sides”—and details features of single-neuron morphology, together guiding targeted follow-up functional investigation based on intracellular recordings. Using this approach, we identify three pivotal neuron classes: a command-like food-signaling cell type, a feeding central pattern generator interneuron, and a unique behavior-specific motoneuron, together significantly advancing understanding of the function of this classical control circuit. Combining our morphological and electrophysiological data, we also establish a functional CNS atlas in Lymnaea as a shared and scalable resource for the research community. Our approach enables the rapid construction of cell atlases in large-scale nervous systems, with key relevance to functional circuit interrogation in a diverse range of model organisms.
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Mar 2025
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