I22-Small angle scattering & Diffraction
|
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.
|
Mar 2026
|
|
I22-Small angle scattering & Diffraction
|
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.
|
Dec 2025
|
|
I18-Microfocus Spectroscopy
|
Sarah B.
Gosling
,
Emily L.
Arnold
,
Lois
Adams
,
Paul
Cool
,
Kalotina
Geraki
,
Mark O.
Kitchen
,
Iain D.
Lyburn
,
Keith D.
Rogers
,
Tim
Snow
,
Nick
Stone
,
Charlene E.
Greenwood
Diamond Proposal Number(s):
[31847]
Open Access
Abstract: Calcifications across the body offer snapshots of the surrounding ionic environment at the time of their formation. Links between prostate calcification chemistry and cancer are becoming of increasing interest, particularly in identifying biomarkers for disease. This study utilizes X-ray fluorescence mapping of 72 human prostate calcifications, measured at the I18 beamline at the Diamond Light Source, to determine the links between calcifications and their environment. This paper offers the first investigation of the elemental heterogeneity of prostate calcifications, demonstrating lower relative levels of minor elements at the calcification center compared to the edge but higher levels of zinc. Importantly, this study uniquely presents links between average Fe, Cr, Mn, Cu, and Ni ratios and grade Group (a classification system for urological tumors, specifically for prostate cancer), highlighting a potential avenue of exploration for biomarkers in prostate calcifications.
|
Jul 2025
|
|
I22-Small angle scattering & Diffraction
|
Open Access
Abstract: Carbon materials are essential for emerging energy applications and there is a pressing need to be able to produce carbons with controlled properties from sustainable precursors. Iron-catalysed graphitization of biomass is an attractive approach, where simple iron salts are used to convert organic matter to graphitic carbons at relatively low temperature. The choice of iron salt can have a significant impact on the chemical and structural properties of carbons derived from biomass. In this paper, we report a detailed mechanistic investigation of iron catalysed graphitization of cellulose by Fe(NO3)3 and FeCl3. In situ small and wide angle X-ray scattering and electron microscopy show that the evolution of catalyst particles from the two salts follows very different pathways. Remarkably, graphitization by FeCl3 is an order of magnitude faster than by Fe(NO3)3.
|
Jul 2025
|
|
I07-Surface & interface diffraction
|
Diamond Proposal Number(s):
[13962]
Open Access
Abstract: Mechanisms for surface pattern formation from evaporation of a reactive nanofluid sessile drop are not well understood. In contrast to the coffee-ring effect from inert particles, rapid chemical and morphological transformation of reactive nanoparticles upon rapid evaporative drying are challenging to probe experimentally. Here, using grazing-incidence X-ray surface scattering, the nanostructure of nascent surface patterns has been probed as a ZnO nanofluid sessile drop rapidly dries. The high temporal resolution enabled by the high flux of synchrotron X-rays allows the observation of the emergence of Zn(OH)2 surface crystals from the onset of evaporation and their rapid evolution into the final residual surface pattern, via transient layered complexes evident from the temporary appearance of X-ray diffraction peaks preceding Zn(OH)2 formation. The results offer mechanistic insights of morphogenesis of surface patterns from evaporation-induced self-assembly and self-organization of reactive nanofluids, previously untenable using other experimental methods.
|
Jul 2025
|
|
I18-Microfocus Spectroscopy
|
Sarah B.
Gosling
,
Emily L.
Arnold
,
Lois
Adams
,
Paul
Cool
,
Kalotina
Geraki
,
Mark O.
Kitchen
,
Iain D.
Lyburn
,
Keith D.
Rogers
,
Tim
Snow
,
Nick
Stone
,
Charlene E.
Greenwood
Diamond Proposal Number(s):
[31847]
Open Access
Abstract: Prostate cancer remains the most common male cancer; however, treatment regimens remain unclear in some cases due to a lack of agreement in current testing methods. Therefore, there is an increasing need to identify novel biomarkers to better counsel patients about their treatment options. Microcalcifications offer one such avenue of exploration. Microfocus spectroscopy at the i18 beamline at Diamond Light Source was utilised to measure X-ray diffraction and fluorescence maps of calcifications in 10 µm thick formalin fixed paraffin embedded prostate sections. Calcifications predominantly consisted of hydroxyapatite (HAP) and whitlockite (WH). Kendall’s Tau statistics showed weak correlations of ‘a’ and ‘c’ lattice parameters in HAP with GG (rτ = − 0.323, p = 3.43 × 10–4 and rτ = 0.227, p = 0.011 respectively), and a negative correlation of relative zinc levels in soft tissue (rτ = − 0.240, p = 0.022) with GG. Negative correlations of the HAP ‘a’ axis (rτ = − 0.284, p = 2.17 × 10–3) and WH ‘c’ axis (rτ = − 0.543, p = 2.83 × 10–4) with pathological stage were also demonstrated. Prostate calcification chemistry has been revealed for the first time to correlate with clinical markers, highlighting the potential of calcifications as biomarkers of prostate cancer.
|
Apr 2025
|
|
|
|
Ameni
Zaouali
,
David
Gloaguen
,
Eric
Le Bourhis
,
Pierre-Antoine
Dubos
,
Marie-José
Moya
,
Matthias
Schwartzkopf
,
Tim
Snow
,
Konrad
Schneider
,
Baobao
Chang
,
Fabienne
Jordana
,
Solène
Tessier
,
Pierre
Tournier
,
Arnaud
Pare
,
Pierre
Weiss
,
Valérie
Geoffroy
,
Baptiste
Girault
Abstract: Various cellular activities regulate bone healing, causing structural changes and evolving mechanical characteristics during the regeneration process. This pilot study aimed to correlate the time- and space-resolved mechanical behavior of regenerating and related biological processes. While the mechanical properties of bone are known to be based on a nanostructure organization, this study intends to highlight the evolution of the strain distribution induced by the reconstruction process, which is mainly driven by the mineral part (i.e., hydroxyapatite) of the bone architecture. Multiscale mechanical (tensile and nanoindentation tests) and biological (X-ray microtomography measurements and histological observations) characterization methods were applied to 3 mm rat cranial defects, one of the most reproducible animal models used to assess bone regeneration, filled with bone grafts, the gold standard for bone repair. The size and crystallographic orientation of the hydroxyapatite particles as well as their lattice (elastic) strain distribution under tensile loading were investigated through in situ synchrotron wide-angle and small-angle X-ray scattering measurements at various healing stages. Analyses were completed to quantify the elastic properties at the tissue-scale via nanoindentation measurements. The resulting mappings of lattice strain, mean particle thickness and crystallographic orientations revealed how tissue evolves during bone repair. At the early stages of the regeneration process, the microstructural changes consisted of a restored hydroxyapatite platelet shape and crystallographic orientation. At later stages, the hydroxyapatite crystallographic orientation reached that of native bone, and the mechanical function of the tissue in the defect zone was restored at the mineral particle scale. Nevertheless, even for the longest regeneration duration (20 weeks), mechanical properties at the tissue-scale remained ineffective, highlighting the importance of multiscale investigations to address this type of issue.
|
Apr 2025
|
|
I22-Small angle scattering & Diffraction
|
Diamond Proposal Number(s):
[25602]
Open Access
Abstract: By developing a 3D X-ray modeling and spatially correlative imaging method for fibrous collagenous tissues, this study provides a comprehensive mapping of nanoscale deformation in the collagen fibril network across the intact bone-cartilage unit (BCU), whose healthy functioning is critical for joint function and preventing degeneration. Extracting the 3D fibril structure from 2D small-angle X-ray scattering before and during physiological compression reveals of dominant deformation modes, including crystallinity transitions, lateral fibril compression, and reorientation, which vary in a coupled, nonlinear, and correlated manner across the cartilage-bone interface. A distinct intermolecular arrangement of collagen molecules, and enhanced molecular-level disorder, is found in the cartilage (sliding) surface region. Just below, fibrils accommodate tissue strain by reorientation, which transitions molecular-level kinking or loss of crystallinity in the deep zone. Crystalline fibrils laterally shrink far more (20×) than they contract, possibly by water loss from between tropocollagen molecules. With the calcified plate acting as an anchor for surrounding tissue, a qualitative switch occurs in fibrillar deformation between the articular cartilage and calcified regions. These findings significantly advance this understanding of the complex, nonlinear ultrastructural dynamics at this critical interface, and opens avenues for developing targeted diagnostic and therapeutic strategies for musculoskeletal disorders.
|
Nov 2024
|
|
I22-Small angle scattering & Diffraction
|
Diamond Proposal Number(s):
[20568]
Open Access
Abstract: Nanostructured materials can be utilised as potential catalysts for the production of platform chemicals and renewable biofuels from biomass derived molecules. The formation of hierarchical meso-microporous zeolites LTL and FAU via the surfactant assisted tandem acid-base post-synthesis treatment has been investigated by time-resolved in situ synchrotron SAXS and WAXS, providing a new insight into the mechanism of the mesostructuring treatment. Based on the results of TEM and in situ synchrotron measurements, a model for the formation of the core-shell structure of LTL zeolite crystals is proposed. Complementary evaluation using FTIR, NMR and nitrogen adsorption, in conjunction with reaction studies on mesostructured zeolites, demonstrated a potential for enhanced catalytic performance of these materials owing to the increased accessibility of the active sites and reduced transport limitations.
|
Oct 2024
|
|
I22-Small angle scattering & Diffraction
|
Adelaide
Lerebours
,
Justyn
Regini
,
Roy A.
Quinlan
,
Toshihiro
Wada
,
Barbara
Pierscionek
,
Martin
Devonshire
,
Alexia A.
Kalligeraki
,
Alice
Uwineza
,
Laura
Young
,
John M.
Girkin
,
Phil
Warwick
,
Kurt
Smith
,
Masato
Hoshino
,
Kentaro
Uesugi
,
Naoto
Yagi
,
Nick
Terrill
,
Olga
Shebanova
,
Tim
Snow
,
Jim T.
Smith
Diamond Proposal Number(s):
[17075]
Open Access
Abstract: Recent studies apparently finding deleterious effects of radiation exposure on cataract formation in birds and voles living near Chernobyl represent a major challenge to current radiation protection regulations. This study conducted an integrated assessment of radiation exposure on cataractogenesis using the most advanced technologies available to assess the cataract status of lenses extracted from fish caught at both Chernobyl in Ukraine and Fukushima in Japan. It was hypothesised that these novel data would reveal positive correlations between radiation dose and early indicators of cataract formation.
The structure, function and optical properties of lenses were analysed from atomic to millimetre length scales. We measured the short-range order of the lens crystallin proteins using Small Angle X-Ray Scattering (SAXS) at both the SPring-8 and DIAMOND synchrotrons, the profile of the graded refractive index generated by these proteins, the epithelial cell density and organisation and finally the focal length of each lens.
The results showed no evidence of a difference between the focal length, the epithelial cell densities, the refractive indices, the interference functions and the short-range order of crystallin proteins (X-ray diffraction patterns) in lens from fish exposed to different radiation doses. It could be argued that animals in the natural environment which developed cataract would be more likely, for example, to suffer predation leading to survivor bias. But the cross-length scale study presented here, by evaluating small scale molecular and cellular changes in the lens (pre-cataract formation) significantly mitigates against this issue.
|
Aug 2023
|
|
