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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Atal
Pande
,
Lucille
Rose
,
Sam J.
England
,
Imran
Rahman
,
Ricardo
Pérez-De La Fuente
,
Andrew J.
Bodey
,
Kaz
Wanelik
,
Christian M.
Schlepütz
,
Jonathan
Günther
,
Christoph
Rau
,
Alexander
Blanke
,
Lauren
Sumner-Rooney
Diamond Proposal Number(s):
[20721, 32952, 17205]
Open Access
Abstract: Vision is one of the most important senses used by animals and contributes to fundamental behaviors, including foraging, navigation, and mate detection and selection.1 Although much is known about how eye position and orientation correlate to ecology in the context of binocularity,2 animals with multipartite visual systems (more than two eyes) remain comparatively neglected. Spiders are highly successful predators that occupy a range of ecological niches and usually possess eight eyes. Here, we use three-dimensional geometric morphometrics and evolutionary modeling to test whether eye positions, orientations, and interocular angles correlate with hunting strategies in 52 species across the spider phylogeny. We demonstrate that eye configurations diversified from an ancestral medial cluster, as seen in modern trapdoor spiders, to a halo-like configuration in orb-weavers, and to the frontal clustering of eyes in several members of derived spider lineages. We show that visual hunters have the highest disparity and evolutionary rates in the configuration of their eyes but display a distinct morphological signature with multiple eye pairs concentrated at the front of the carapace. Moreover, we quantify the extent to which eye configuration is modular and show that the position and orientation of the eye pairs evolve semi-independently of each other. Our findings demonstrate that modularity in the spider visual system facilitates not only the specialization of individual eyes but also the whole architecture of the visual system, in line with different hunting strategies, body plans, and ecological niches.
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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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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[38900, 36899]
Open Access
Abstract: The middle ear endures significant pressure variations during activities such as flying or diving, which can cause large displacements of the tympanic membrane and ossicles. While the middle ear of the general population usually withstands such displacements without impairing hearing function, little is known about the effects of sudden pressure changes in the middle ears of populations with connective tissue disorders, like osteogenesis imperfecta (OI or brittle bone disease). Similar to OI long bones, which fracture under minimal impact, we hypothesized that a sudden pressure change in the OI ear canal alters the ossicular chain integrity and impairs hearing function. Using the B6C3Fe a/a-Col1a1oim/oim (oim/oim) mouse model of severe OI, this study determines the impact of sudden pressure changes in the ear canal on hearing function by testing auditory brainstem response (ABR) and verifying ossicular structural integrity using synchrotron microtomography. No differences in baseline thresholds were observed between oim/oim mice and wild-type (WT) controls, as well as no changes in hearing function after pressure exposure, measured as (i) the change in the neural response amplitude at the highest sound level (ΔRMS90dB SPL), (ii) the change in ABR threshold (ΔThreshold), and (iii) the change in latency of the first positive peak of the neural response at the highest sound level (ΔLatency90dB SPL). However, post-pressure, the middle ear ossicles of oim/oim mice showed twice the incidence of incudomalleal joint abnormalities compared to healthy wild-type ears (27% vs. 13%), with incudomalleal joint narrowing, fractures, and particularly fusions.
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Feb 2026
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[24142, 30661, 36899]
Abstract: Hearing loss is common in people with osteogenesis imperfecta (OI or brittle bone disease). Bisphosphonates are widely used to treat long bone fragility in children with OI. However, its impact on the bone quality of the middle ear ossicles and hearing remains unknown. This study determines whether bisphosphonates treatment itself may contribute to hearing loss in OI by evaluating its effects in the oim/oim mouse model of severe OI having normal auditory function. Specifically, this study reports the effects of alendronate (ALN), a nitrogen-containing bisphosphonate, on ossicle morphology, porosity, and elemental composition in 14-week-old oim/oim mice treated weekly, starting at 2 weeks of age. The ossicles were examined using synchrotron microtomography and X-ray fluorescence microscopy (XFM). Hearing was assessed longitudinally until 26 weeks of age by determining auditory brainstem response (ABR) thresholds in another group of mice also treated weekly starting at 2 weeks of age. ALN treatment further reduces in size the already small oim/oim ossicles, specifically in female mice. Porosity, bone composition, and hearing function, however, were generally not affected by the ALN treatment. Furthermore, ALN does not prevent joint fusions, excessive bone formations, or enlarged joint spaces in WT or oim/oim experimental groups. One ALN-treated oim/oim mouse with a bone formation in the interior of the footplate, and one ALN-treated WT mouse with a fixed footplate had frequency-specific hearing loss. Since footplate abnormalities are not observed in PBS-treated mice in this study, it remains unclear whether ALN fails to prevent these changes or contributes to their development. Future studies should investigate the mechanisms of ossicular abnormalities and bisphosphonates modulatory role in the ossicles.
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Dec 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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Diamond Proposal Number(s):
[33620, 38900, 36899]
Abstract: Hearing loss is a prevalent symptom of osteogenesis imperfecta (OI), a group of collagen type I-related skeletal disorders, commonly known as brittle bone disease. Clinical manifestation of hearing loss in OI often presents with stapes footplate fixation and hypodense foci in the otic capsule. However, the etiology and evolution of OI-hearing loss and its relation to bone abnormalities are still unknown. This study investigates the onset, severity, and progression of hearing loss in the homozygous oim mouse model of severe OI Type III, which is reported to exhibit hearing loss at 11-12 weeks of age (Chen et al., 2007), using auditory brainstem responses up to 26 weeks of age. We further examine the presence of deformities, microcracks, and fractures of the ossicular chain using synchrotron microtomography. Our results demonstrate that oim/oim mice have normal hearing, regardless of i) their parental lineage, ii) their husbandry in isolation or with other animals, iii) their mastication with powder or chow food, and iv) their anesthesia with single or multiple ketamine injections. Bone abnormalities like excessive formations, fusions, and fractures, were observed in up to 33% of wild-type and up to 43% of oim/oim mice in each group. Among these, joint and bone-tendon abnormalities were twice as frequent in the oim/oim mice compared to the wild-type mice. Notably, these abnormalities did not impact the hearing response in mice. Whether such bone abnormalities occur and alter auditory function in humans with OI remains uncertain.
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Jul 2025
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[22198]
Open Access
Abstract: Solid-state lithium batteries are developing rapidly as a promising next-generation battery, while challenges still persist in understanding their degradation processes during cycling due to the difficulties in characterization. In this study, the 3D morphological evolution of the Li3PS4 solid electrolyte was tracked during electrochemical cycles (plating and stripping) until short circuit by utilizing in situ synchrotron X-ray computed tomography with sufficient spatial and temporal resolution. During the degradation process, cracks in the electrolyte alternately generated from the two electrode/electrolyte interfaces and propagated until shorting. The lithium dendrites filled in the electrolyte cracks but had a greatly reduced filling ratio after the first plating stage; therefore, the cell could continue working for some time after the solid electrolyte was fully fractured by cracks. The compression of the two lithium electrodes mainly occurred in initial cycles where a ca. 4–7 μm reduction in thickness was observed. The mechanical force and electric potential fields were modeled to visualize their redistributions in different stages of cycling. The release of strain energy after the first penetration and thereafter the subsequent driving forces are discussed. These results reveal a fast degradation of solid electrolyte in the initial cycles, providing insights for further modifications and improvements in solid-state batteries.
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May 2025
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[20925, 24142]
Abstract: Hearing loss affects approximately 70 % of individuals with osteogenesis imperfecta (OI), a genetic connective tissue disorder characterized by bone fragility and deformities. No effective treatments exist for OI hearing loss, and its etiology is unknown limiting the development of new targeted therapies. This work investigates the impact of OI type I collagen mutations on the ossicle bone properties in the homozygous oim mouse model of severe OI, which is known to exhibit hearing loss. The morphology and porosity of the ossicles of 14-week-old oim and wild-type mice were analyzed using high-resolution synchrotron radiation microtomography. Additionally, the collagen fibers structure, bone tissue composition and mechanical properties were evaluated through second harmonic generation microscopy, Raman spectroscopy, and nanoindentation. The results demonstrated that oim ossicles are small, highly porous with an elevated lacunar number density, a flat stapes footplate and a small malleal processus brevis. One-in-two oim ossicles had incudomalleal joint abnormalities, exhibiting either a localized fracture in the incus head or a joint space widening. No differences were observed in collagen fibers structure, bone tissue composition and mechanical properties. These findings suggest that bone fractures observed in the oim incus may contribute to their reported hearing loss. However, the underlying mechanism for these fracture development remains to be investigated, as they do not appear to result from changes in bone tissue properties (collagen fibers organization, tissue composition or mechanical properties). Instead, they may be associated with joint space widening, and possibly altered ossicle chain kinematics.
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Apr 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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