DIAD-Dual Imaging and Diffraction Beamline
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Diamond Proposal Number(s):
[39247]
Open Access
Abstract: This work presents the design and development of a 3D printed flow cell tailored for X-ray computed microtomography of liquid–solid systems. The flow cell is manufactured using stereolithographic printing and utilizes a novel pillarless pull-through geometry. The use of the flow cell developed for K-11 DIAD (Dual Imaging and Diffraction beamline, Diamond Light Source, UK) is demonstrated with the in situ flow and selective recovery of an Sn precipitate from solution using an organic ligand. The 3D designs and components are made freely available with this publication.
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Mar 2026
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I14-Hard X-ray Nanoprobe
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Diamond Proposal Number(s):
[36126]
Open Access
Abstract: Coal fly ash (CFA), a metal-rich byproduct of coal combustion is produced in vast quantities and poses significant ecological risks. CFA also contains abundant technologically relevant metal oxides and trace metals, including rare earth elements (REE), often at higher concentrations than in primary ores. This makes sustainable recovery strategies a major industrial opportunity. Here, green solvent systems were applied to leach metals from CFA, and the resulting leachates were added to cultures of Magnetospirillum gryphiswaldense (MSR1), a model magnetotactic bacterium that biomineralizes iron into membrane-bound magnetic nanoparticles (magnetosomes) and is capable of interacting with non-iron metals through adsorption and biomineralization. Eleven green solvents, including deep eutectic solvents (DES), were tested for extraction efficiency, with six showing performance comparable to a mineral acid control. Copper (Cu) emerged as the primary toxicant to MSR1, prompting selective precipitation with potassium ferrocyanide trihydrate (PFCT) to reduce its concentration. Cu-depleted lactic acid-based leachates supported MSR1 growth and magnetosome formation even without supplemented iron. Nano-XRF and ICP-MS analysis revealed MSR1 interacts with CFA-derived metals, most significantly showing that produced CFA magnetosomes contained a 5.3–6.1-fold increase in Cu compared to controls. As Cu is both a growth inhibitor and a target pollutant, these findings suggest MSR1 may bioaccumulate Cu within magnetosomes as a detoxification strategy. Overall, this study demonstrates a combined chemical–biological route for CFA valorisation, enabling recovery of diverse metals from waste while producing magnetosomes with distinct compositions.
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Mar 2026
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I13-2-Diamond Manchester Imaging
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Mahendra P.
Raut
,
Andrea
Mele
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Nicholas T. H.
Farr
,
Caroline S.
Taylor
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David A.
Gregory
,
Jingqiong
Zhang
,
Yufeng
Lai
,
Annabelle
Fricker
,
Jon
Willmott
,
Candice
Majewski
,
Lyudmila
Mihaylova
,
Cornelia
Rodenburg
,
Ipsita
Roy
Diamond Proposal Number(s):
[33034]
Open Access
Abstract: Bone tissue engineering (BTE) aims to address the challenge of repairing critical size bone defects, but effective substitutes with suitable mechanical properties and bioactivity are still needed. Poly(3-hydroxybutyrate), P(3HB)is a sustainable polymer with promising potential but suffers from poor mechanical properties and thermal instability. In this study, P(3HB) was reinforced with various carbon-based materials (CBMs) to evaluate thermomechanical and structural properties as well as biological responses, in composites before and after aging. CBMs with P(3HB) interactions and their spatial distribution were examined using advanced imaging, including Atomic Force Microscopy (AFM), Secondary Electron Hyperspectral Imaging (SEHI), and Short-Wave Infrared (SWIR) analysis. Biological responses were assessed using various biocompatibility assays; cytotoxicity and osteogenicity with primary human osteoblasts (ECACC, 406-05a) and MG63 cells. Aged P(3HB)/inkjet composites showed a 140 % increase in Young's modulus (1.2 GPa), matching trabecular bone stiffness, with a 3 % lower processing temperature than neat P(3HB), enhancing suitability for 3D printing. SEHI revealed elevated OH (4.8 eV) and CO (5.7 eV) functional groups, resulting in increased surface hydrophilicity and promoted cellular responses. P(3HB)/inkjet demonstrated the highest cell attachment (267.5 ± 43.3 cells) and ALP activity (6.3 ± 0.7 nmol PNP/min), outperforming composites with Starbon (150.1 ± 38.3 cells, 6.1 ± 0.8 ALP) and activated carbon (103.4 ± 24.5 cells, 5.7 ± 0.5 ALP). All aged composites showed improved performance over their fresh counterparts. In contrast, TCP and neat P(3HB) exhibited the lowest levels of mineralization. 3D printing offers further potential for enhancing P(3HB)/inkjet composites through precise and bespoke scaffold design and clinical feasibility.
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Mar 2026
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I14-Hard X-ray Nanoprobe
I18-Microfocus Spectroscopy
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Diamond Proposal Number(s):
[39618, 39938, 302085, 31588, 5116, 36811]
Open Access
Abstract: Correlative microscopy linking synchrotron X-ray fluorescence (SXRF) with optical imaging is valuable for contextualizing chemical element distributions in biology. The spatial correlation necessary to achieve this presents fundamental challenges and can be a significant constraint on accuracy and data interpretation. We present a technical solution based on a finder grid concept, optimized for SXRF correlative studies of metals in biological tissues, with scope for wider adaptation and application. A hierarchically patterned fiducial system was directly etched onto spectroscopically clean quartz substrates via femtosecond laser ablation. This design enables improved correlation among SXRF, optical imaging, and histological staining over a greater range of length scales than conventional registration methods such as the use of tissue architecture from serial sections and the use of electron-microscopy-resolution finder grids and applied fiduciary markers that can introduce XRF-signal-dominating levels of elements such as copper, nickel, gold, and titanium. We present two quartz finder grid formats: a microgrid and a nanogrid design. We demonstrate their utility for rapid ROI relocalization and same-section correlative workflows using human brain tissue. The etched quartz finder grid approach facilitates rapid and reproducible ROI relocalization and alignment across instruments, particularly where integral fiducial markers are sparse or ambiguous.
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Mar 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):
[17616]
Open Access
Abstract: Ermine moths produce bursts of ultrasonic clicks that protect them from their predators. The clicks are produced by a tymbal organ that features a series of corrugated striations in the membrane of the hindwings. In response to wing folding during the wingbeat cycle, individual stria snap-through sequentially to excite the natural frequencies of a scaleless patch adjacent to the striations. Based on morphological characterization of the aeroelastic tymbal of Yponomeuta moths, we propose an analogue origami-like creased shell model to reproduce the actuation and sequential click production of the biological structure. The origami-like model helps to explain the governing biomechanics of aeroelastic tymbals; namely, the burst of clicks occurs as a result of a series of snapping vertex folds, reminiscent of the origami waterbomb, that buckle and snap-through in sequence when actuated by a global stimulus (wing folding). Such sequential buckling behaviour often occurs in pattern formation events and in the structural failure of compressed cylindrical shells and sandwich panels. Interestingly, ermine moths instead use this instability phenomenon for functionality—namely, phased acoustic sound emission—creating opportunities for new engineering applications.
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Feb 2026
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I13-2-Diamond Manchester Imaging
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Will J.
Dawson
,
Andrew R. T.
Morrison
,
Simon M.
Tonge
,
Matthew P.
Jones
,
Myles Kofi
Coke
,
Isabel C.
Antony
,
Kaz
Wanelik
,
Vyacheslav
Kachkanov
,
Partha P.
Paul
,
Bratislav
Lukić
,
Robert S.
Young
,
Zifa
Zuhair
,
James
Parker
,
Inez
Kesuma
,
Gargi
Giri
,
Liam
Bird
,
Alexander J. E.
Rettie
,
Rhodri
Jervis
,
James B.
Robinson
,
Denis
Cumming
,
Thomas S.
Miller
,
Paul R.
Shearing
Diamond Proposal Number(s):
[33315]
Open Access
Abstract: Drying of slurry cast electrodes is amongst the most energy intensive unit operations in battery manufacture. In spite of this, the optimisation of drying processes has been highly empirical, and there remains limited understanding of the interplay between drying dynamics and resulting microstructure. In this work, we used synchrotron X-ray computed microtomography in order to study the formation of mud cracks during the drying process, and evaluate their impact on the electrode microstructure. This was achieved by applying a reduced drying rate, which proved to be an effective means of studying the drying mechanism with a greater resolution and image contrast than otherwise possible. The rate of crack growth is measured, and the differing crack morphology resultant from changes in thickness (between 300 and 800 µm doctor blade gaps) and the presence of air bubbles in the slurry is demonstrated. Digital volume correlation is utilised to identify the specific location of crack formation before these cracks were visible, suggesting image correlation methods as an appropriate tool for process feedback in order to control or eliminate mud cracking. This new approach which enables direct quantification of the evolving microstructure during dynamic drying, in 3D, is therefore transformative in our understanding of the underlying physical processes and will guide rational optimisation of this industrially significant process.
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Feb 2026
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DIAD-Dual Imaging and Diffraction Beamline
I14-Hard X-ray Nanoprobe
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Abstract: High-resolution characterisation of biomaterials across multiple length scales to investigate their effect on (re)mineralisation can inform the development of effective interventions for clinical conditions such as dental caries, a disease with an estimated global economic burden of approximately $245 billion. This thesis presents a multi-modal, synchrotron-based approach on novel instruments to study the role of self-assembling peptide P11-4 in dental enamel (re)mineralisation, with the aim of elucidating its mechanism of action for potential optimisation to treat early caries lesions non-invasively, and to use P11-4 as a model system for the development of a liquid flow cell that can be used to characterise biomimetic materials in situ using synchrotron X-ray diffraction (XRD) and X-ray microtomography (XMT).
X-ray fluorescence combined with differential phase contrast imaging on the I14 beamline, together with XRD and XMT on the Dual Imaging and Diffraction beamline at Diamond Light Source, along with complementary laboratory-based techniques, were employed to characterise P11-4.
P11-4 accelerated the initial kinetics of the mineralisation process compared to the control, via the provision of calcium-binding sites, and controlled the mineral deposition process, mimicking the role of enamel matrix proteins during biomineralisation. The chemical model used for artificial demineralisation to create caries-like lesions resulted in preferential demineralisation of the enamel prisms. Within the caries-like lesions, the developed flow cell demonstrated that P11-4 promoted deep remineralisation of the lesion via the gradual formation of organised apatite structures within one specific population of crystallites, likely corresponding to the prisms. The organisation of crystallites within the regenerated structure is comparable to healthy enamel, highlighting its role in restoring the organised structure lost due to caries, and its significance as a non-invasive clinical treatment.
The methodology presented in this thesis can be applied to analyse lesions and characterise other biomaterials/proteins, and the flow cell is available to other users.
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Feb 2026
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[33984]
Abstract: In situ tomography enables non-destructive, time-lapse imaging of biological tissues under load, offering insights into structural and mechanical changes. However, repeated scans can expose samples to high radiation doses, potentially altering tissue properties. This study evaluated the feasibility of low-dose synchrotron computed tomography (sCT) for high-resolution, in situ imaging of intact bovine intervertebral discs (IVDs), and assessed the effects of repeated x-ray exposure on mechanical, microstructural, and molecular integrity. Intact oxtail IVD segments were imaged using propagation-based phase contrast sCT at 54 keV. Scan parameters were optimised to achieve high image quality within 66 seconds per scan, resulting in a total absorbed dose of ∼30 kGy over six scans. Mechanical properties were assessed under cyclic loading, microstructural changes via digital volume correlation (DVC), and molecular alterations using Raman spectroscopy. High-resolution imaging of soft and calcified tissues was achieved. Changes in sample stiffness, hysteresis, or stress recovery between irradiated and control were not identified. DVC revealed no microstructural damage or strain accumulation in the calcified endplate. Raman spectroscopy indicated minimal changes in soft tissues, with bone showing slightly increased collagen crosslinking and reduced mineralisation. Overall, this study demonstrates that high-energy, low-dose sCT enables repeated imaging of musculoskeletal tissues without compromising integrity, supporting its application in dynamic, time-lapse imaging studies. Importantly, larger, intact samples, such as whole bovine IVDs, were imaged overcoming limitations of previous studies that relied on small animal models. This approach supports more physiologically relevant investigations of tissue mechanics and degeneration in complex systems.
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Feb 2026
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B16-Test Beamline
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S.-X.
Wang
,
Z.-Q.
Zhao
,
X.-Y.
Wang
,
T.-J.
Li
,
Y.
Su
,
Y.
Uemura
,
F.
Alves Lima
,
A.
Khadiev
,
B.-H.
Wang
,
J. M.
Ablett
,
J.-P.
Rueff
,
H.-C.
Wang
,
O. J. L.
Fox
,
Wenbin
Li
,
L.-F.
Zhu
,
X.-C.
Huang
Diamond Proposal Number(s):
[31397]
Open Access
Abstract: X-ray cavity quantum optics with inner-shell transitions has been limited by the spectral overlap between resonant and continuum states. Here, we report the first experimental demonstration of cavity-controlled core-to-core resonant inelastic x-ray scattering (RIXS). We suppress the absorption-edge effects by monitoring the RIXS profile, thereby resolving the resonant state from the overlapping continuum. We observe distinct cavity-induced energy shifts and cavity-enhanced decay rates in the 2𝑝3𝑑 RIXS spectra of WSi2. These effects, manifesting as stretched or shifted profiles in the RIXS planes, enable novel spectroscopic applications via cavity-controlled core-hole states. Our results establish core-to-core RIXS as a powerful tool to manipulate inner-shell dynamics in x-ray cavities, offering new avenues for integrating quantum optical effects with x-ray spectroscopy.
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Feb 2026
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