I13-2-Diamond Manchester Imaging
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Jishizhan
Chen
,
Alissa
Parmenter
,
Aikta
Sharma
,
Elis
Newham
,
Eral
Bele
,
Sebastian
Marussi
,
Andrew A.
Pitsillides
,
Nick J.
Terrill
,
Christopher
Mitchell
,
Himadri S.
Gupta
,
Peter
Lee
Diamond Proposal Number(s):
[29784]
Open Access
Abstract: Lower back pain is linked to vertebral biomechanics, with vertebral endplates (VEPs) playing a key role. Finite element modelling (FEM) is a powerful tool for studying VEP biomechanics but relies on accurate material property inputs, which remain difficult to obtain. Synchrotron computed tomography (sCT) enables detailed visualisation of intact VEP microstructure under near-physiological loads in situ, with three-dimensional strain fields obtained by digital volume correlation (DVC) providing experimental reference data for FEM validation. We applied inverse finite element methodologies to estimate of the elastic properties of rat VEPs by integrating DVC data into an image-based FE model. Our pipeline estimated an elastic modulus of 129 MPa and a Poisson’s ratio of 0.24 in a rat lumbar segment. The first-order Wasserstein distance between FEM and DVC strain distributions ranged from 0.08% to 0.28%, with Bland–Altman analysis revealing <95% spatial agreement between FEM-predicted and DVC-derived strains across multiple loading steps. Pipeline measurement consistency was evaluated across multiple rat lumbar FE models (n = 3), yielding an estimated VEP elastic modulus = 153 ± 21 MPa and a Poisson’s ratio = 0.28 ± 0.03. Regional variations of strain distribution in VEP bodies and protrusions were also identified (strain Wasserstein distance of 0.10%–0.48%). Our work demonstrates the efficacy of the established pipeline in estimating the isotropic elastic modulus and Poisson’s ratio of VEPs using FEMs in a physiologically relevant, complex load transfer system. As sCT data becomes available, our pipeline lays the foundations for estimating VEP properties in larger animals and humans.
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Mar 2026
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I22-Small angle scattering & Diffraction
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Tayyaba
Rabnawaz
,
Nathanael
Leung
,
Leonard C.
Nielsen
,
Robert A.
Harper
,
Richard M.
Shelton
,
Gabriel
Landini
,
Tim
Snow
,
Andy
Smith
,
Nick
Terrill
,
Marianne
Liebi
,
Tan
Sui
Diamond Proposal Number(s):
[20285]
Abstract: Dental caries, one of the most prevalent non-communicable diseases worldwide, is characterised by the progressive deterioration of the structure and mechanical properties of dental hard tissues. In human teeth, dentine is the most abundant mineralised tissue, forming the primary support material. To assess changes in the mechanical properties of dentine caused by dental caries and acid erosion, it is crucial to understand the relationship between organic and inorganic dentine components and their organisation into a 3D anisotropic structure at the nanoscale. Over the past 20 years, alterations in dentine structure caused by caries and artificial demineralisation have been reported using conventional microscopy techniques. However, due to the limited spatial resolution of these techniques, the 3D structural organisation including orientation and degree of alignment of mineralised collagen fibrils at the nanoscale, has not been fully explored. This study investigated alterations in the 3D structure of normal, carious and artificially demineralised dentine using SAXS tensor tomography (SASTT). This technique enabled the observation of differences in the local orientation of organic and inorganic components, as well as variations in local scattering intensity, resulting from natural caries and artificial demineralisation. In comparison to normal dentine, caries caused minor orientational differences of both components but had a major impact on the local X-ray scattering intensity. After artificial demineralisation of the dentine, most of the mineral was lost in the outer layers, resulting in a greater reduction in scattering intensity than that caused by caries.
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Mar 2026
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I22-Small angle scattering & Diffraction
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Kiranjit K.
Bains
,
James
Bell
,
Robert D.
Young
,
Qian
Ma
,
Sally
Hayes
,
Laura
Howard
,
Olga
Shebanova
,
Nick J.
Terrill
,
Keith M.
Meek
,
Justyn W.
Regini
,
Andrew J.
Quantock
Diamond Proposal Number(s):
[34903, 40168]
Open Access
Abstract: Purpose: To study the structural arrangement of crystallin proteins in the human lens during development.
Methods: Fetal human lenses were acquired from the UK Human Developmental Biology Resource and examined at four developmental stages; postconception weeks (pcw) 8 to 9 (n = 5), 12 to 13 (n = 3), 16 to 17 (n = 6), and 20 to 21 (n = 3). Small-angle X-ray scattering patterns were obtained as raster scans across the entirety of each lens using a 0.1 nm-wavelength, synchrotron X-ray beam measuring 200 × 150 µm at the specimen. Analysis of each small-angle X-ray scattering pattern provided a measure of the average nearest neighbor spacing and the extent of spatial order in the crystallin protein array.
Results: Crystallins in the lens center became compacted as development progressed, with the average spacing measuring 19.9 nm at 8 to 9 pcw, 19.6 nm at 12 to 13 pcw, 18.7 nm at 16 to 17 pcw, and 17.7 nm at 20 to 21 pcw. The spatial order of the crystallin proteins in the lens center also decreased with time as indicated by a parameter called the coherence distance, which measured 26.9 nm at 8 to 9 pcw, 24.7 nm at 12 to 13 pcw, 24.6 nm at 16 to 17 pcw, and 24.9 nm at 20 to 21 pcw. Spacing and spatial order were consistently higher at the lens periphery, compared with the center, at all developmental stages studied.
Conclusions: Spatiotemporal modifications in the array of crystallin proteins occur as the human lens develops. These are perhaps reflective of a shift in the relative proportions of crystallin subtypes present and have potential implications for the lens's developing refractive index.
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Jan 2026
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I22-Small angle scattering & Diffraction
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Diamond Proposal Number(s):
[15320]
Open Access
Abstract: Understanding the structure–function relationships in anisotropic fibre-symmetric materials is critical for both biological insight and bioinspired design. We present a generalized analytical model for X-ray diffraction intensity from nanofibrillar materials with fibre symmetry, accommodating arbitrary diffraction rings beyond prior axial and equatorial limits. This model integrates 3D orientation, strain heterogeneity and angular misalignment effects, and is validated using wide-angle X-ray diffraction (WAXD) from the Bouligand-structured cuticle of the mantis shrimp (Odontodactylus scyllarus). Using scanning synchrotron WAXD, we extract depth-averaged and sub-lamellar information on 3D fibre orientation and crystalline parameters from 2D scans. Model simulations and experimental fits show accurate reconstruction of the Bouligand texture and reveal spatial gradients in orientation, strain and angular dispersion. By fitting multiple reflections – axial (002), equatorial (110) and intermediate (013) – we improve the robustness in parameter extraction, especially in regions where the Ewald condition is partially satisfied. Our framework enhances the interpretation of WAXD in heterogeneous fibre-based materials and can be embedded into advanced tomographic or machine-learning workflows. This approach is applicable to a broad class of biological and synthetic composites, facilitating high-throughput structural characterization in scenarios where rotation is impractical or impossible.
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Dec 2025
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I22-Small angle scattering & Diffraction
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M.
Hassan Sk
,
S. M.
Clarke
,
M.
Woolley
,
A.
Osudare
,
S.
Agrawal
,
N.
Sharifi
,
D.
Eberl-Craske
,
R.
Lindsay
,
M. T. L.
Casford
,
A.
Smith
,
N.
Terrill
Diamond Proposal Number(s):
[23699, 28693, 32669]
Open Access
Abstract: In this study we have investigated the nucleation mechanism of ‘sweet’, CO2 corrosion scale in situ using synchrotron scattering under industrially relevant conditions (CO2 saturated brine, ultra-low oxygen (8–32 ppb), 80 °C, pH 6.8, open-circuit-potential (OCP)). Simultaneous small and wide-angle X-Ray Scattering (SAXS-WAXS) measurement allows the phase and state of the nucleating corrosion scale to be characterised as a function of both immersion time and location with respect to the metal/solution interface. The results indicate that a precursor amorphous phase is formed prior to the emergence of a crystalline iron carbonate scale.
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Dec 2025
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I22-Small angle scattering & Diffraction
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Diamond Proposal Number(s):
[33748, 35376, 35348]
Open Access
Abstract: Pulsed potential (PP) electrodeposition was utilized for the first time to fabricate three-dimensional (3D) platinum (Pt) nanostructures within phytantriol-based double diamond cubic templates, both with or without 20 % w/w Brij-56 as a pore swelling agent. Unlike conventional direct potential (DP) deposition, the PP approach yielded Pt nanostructures with markedly enhanced uniformity and superior lattice ordering. Small Angle X-ray Scattering (SAXS) revealed that PP-grown structures exhibited sharp, well-defined Bragg peaks corresponding to lattice parameters of 134.2 ± 2.1 Å without Brij-56 and 236.7 ± 2.5 Å with 20 % w/w Brij-56, whereas DP-grown structures showed broader, less distinct peaks with smaller lattice parameter (130.7 ± 1.9 Å and 197.1 ± 2.8 Å, respectively). Notably, In-situ SAXS measurements provided real-time insights into the evolution of 3D Pt nanostructures, enabling direct monitoring of orientational and lateral ordering within the templated phases. High resolution SEM further confirmed the superior quality of PP-grown structures, revealing highly ordered 3D nanowire network with uniform pore sizes of 89.5 ± 1.3 (without Brij-56) and 102.0 ± 0.7 Å (with 20 % w/w Brij-56). Overall, these findings highlight the effectiveness of PP electrodeposition in mitigating structural inhomogeneities, establishing it as a powerful strategy for fabricating well-ordered 3D Pt nanostructures.
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Nov 2025
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I22-Small angle scattering & Diffraction
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Diamond Proposal Number(s):
[34903]
Open Access
Abstract: Introduction: The mechanisms underpinning the stiffening and stabilising effect of riboflavin/UVA crosslinking on the corneal stroma are not well understood. We report the findings of a biomechanics and synchrotron X-ray scattering study aimed at quantifying hierarchical strain mechanisms in treated and untreated porcine corneas. We applied the same approach to specimens treated with human recombinant decorin core protein, in isolation and in conjunction with riboflavin/UVA.
Methods: Tensile testing was carried out in conjunction with simultaneous synchrotron X-ray scattering. Diffraction peaks associated with the interfibrillar spacing and D-period of collagen were fit to bespoke models to quantify fibril elongation and reorientation under load.
Results: Riboflavin/UVA crosslinking stiffened corneas by approximately 60% while decorin treatment did not significantly affect the mechanical properties. Correlations between fibril elongation caused by applied tensile strain and bulk stiffness were used to approximate fibril stiffness, values for which were relatively similar for control and treatment groups, compared with the magnitude of difference in the bulk stiffness alone.
Discussion: The results imply the bulk stiffening caused by crosslinking was not primarily due to increases in fibril stiffness. Instead, trends in bulk fibril reorientation and straightening/uncrimping imply the stiffening is attributable to enhanced interconnectivity of the fibrillar stroma, leading to greater fibril recruitment fraction. The techniques reported here are applicable to a wide range of tissues for the evaluation of new, existing and adjuvant therapies.
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Sep 2025
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I22-Small angle scattering & Diffraction
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Diamond Proposal Number(s):
[7249]
Abstract: Despite the potential of poly(2-methacryloyloxy ethyl phosphorylcholine)–poly(2-(diisopropylamino)ethyl methacrylate) (PMPC–PDPA) diblock copolymer nanoparticles for several biological applications, the exact mechanism of pH-induced self-assembly of the PMPC–PDPA chains into nanoparticles remains unclear, although it has been extensively studied by ex situ transmission electron microscopy. Here, we probe this process using time-resolved small-angle X-ray scattering (TR-SAXS) to gain an understanding of the phenomena that occur on the nanoscale. Modeling the TR-SAXS data indicated that spherical micelles and vesicles were formed at a pH as low as 3, and the spherical micelle and vesicle structures reformed at pH 5.5. At pH ∼5.5, insoluble PMPC25–PDPA70 diblock copolymer precipitation was also observed by SAXS. A huge soluble PMPC25–PDPA70 diblock copolymer reservoir might assist in PMPC25–PDPA70 vesicle construction. Additionally, a potential pathway of vesicle construction by spherical micelle fusion was supported by the SAXS evidence.
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Sep 2025
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DIAD-Dual Imaging and Diffraction Beamline
I13-2-Diamond Manchester Imaging
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Alissa
Parmenter
,
Elis
Newham
,
Aikta
Sharma
,
Catherine M.
Disney
,
Hans
Deyhle
,
Federico
Bosi
,
Nick J.
Terrill
,
Brian K.
Bay
,
Andrew A.
Pitsillides
,
Himadri S.
Gupta
,
Peter
Lee
Diamond Proposal Number(s):
[29633, 29784]
Open Access
Abstract: The function of all musculoskeletal joints depends on hierarchical structures spanning the molecular to whole-joint scales. Investigating biomechanics across length scales requires correlative multiscale experimental methods. This study applies multimodal in situ synchrotron imaging techniques to spinal joints—focusing on the vertebral endplates—to explore relationships between structure and mechanical strain across spatial scales. Strain mapping using digital volume correlation combined with microarchitectural analysis reveals that high tensile and shear strains play a role in the cartilage to bone transition. Correlative imaging and diffraction show that bone contains narrower mineral nanocrystallites under greater compressive prestrain compared with calcified cartilage. We hypothesize that this multiscale structural adaptation supports the mechanical function of the intervertebral disc. Future applications of the techniques presented here have potential to help unravel the biomechanical underpinnings of pathologies affecting mineralized tissue structure. The multiscale structure-function relationships uncovered here may inspire the design of biomaterials and orthopedic implants.
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Jul 2025
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B21-High Throughput SAXS
I22-Small angle scattering & Diffraction
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Ester
Serrano
,
Tianxiao
Zhao
,
David R.
Mark
,
Mostafa
Soroor
,
Iris
Floria
,
Nicholas J.
Terrill
,
Nikil
Kapur
,
Arwen I. I.
Tyler
,
Mathew H.
Horrocks
,
Andrew J.
Roe
,
Olwyn
Byron
Diamond Proposal Number(s):
[28516]
Open Access
Abstract: Enterohaemorrhagic Escherichia coli causes sporadic, and sometimes large-scale, food poisoning outbreaks, for which antibiotic treatment in humans is contraindicated. As an alternative form of therapy, previous studies developed the family of salicylidene acylhydrazide (SA) anti-virulence compounds. One target of the SA compounds is AdhE, an enzyme that converts acetyl-CoA to ethanol and vice versa. AdhE oligomerizes, forming helicoidal filaments, heterogeneous in length, called spirosomes. We show it is possible to only partially fractionate AdhE spirosomes because in vitro they oligomerize in the absence of stimuli, and that spirosome formation is necessary to regulate the direction of AdhE enzymatic reactions. We also show that the SA compound ME0054 binds and perturbs AdhE spirosomes, enhancing the conversion of ethanol to acetyl-CoA. This mechanistic understanding of how ME0054 impacts AdhE function will help in the development of SA compounds as novel anti-virulence inhibitors.
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Jun 2025
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