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):
[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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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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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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I22-Small angle scattering & Diffraction
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Diamond Proposal Number(s):
[15320]
Open Access
Abstract: Determining the mechano-structural relations in biological materials with hierarchical structure is crucial to understanding natural optimization strategies and designing functional bioinspired composites. However, measuring the nanoscale mechanics and dynamic response is challenging when the specimen geometry and loading environment are physiologically complex. To overcome this challenge, we develop a combination of synchrotron X-ray diffraction testing and analytical modelling to explore the mechano-structural changes during bending loads on stomatopod cuticle. Stomatopod cuticle is an example of a hierarchical biomaterial optimized for high impact and bending resistance. Using models for large deformations of elastic continua, we measure cuticle strains from macroscopic deformations and combine diffraction-based fibril strains with stresses to quantify the local elastic moduli and nanoscale strain concentration factors, which are found to vary across cuticle sub-regions and under different flexion loading modes. This approach has the advantage of identifying constituent biomaterial properties and mechanisms in situ and is also suitable for studying time-dependent changes, such as concurrent strains of the nanofibrous phase that occur during physiological loading.
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Mar 2025
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Open Access
Abstract: Mimicking the fibrous structures of meat is a significant challenge as natural plant protein assemblies lack the fibrous organisation ubiquitous in mammalian muscle tissues. In this work, wet-spun hydrogel fibres resembling the anisotropic fibrous microstructure of meat are fabricated using carboxymethyl cellulose as a model polysaccharide and sodium caseinate as a model protein which are crosslinked using 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide (EDC). Hydrogels and spun fibres were characterised using a combination of rheology (shear, oscillatory, and extensional), microscopy (light, polarised, and fluorescence), rheo-NMR, and X-ray diffraction. Examination of structuring behaviour under shear uncovered a relationship between enhanced biopolymer orientation along the fibre axis and a viscoelastic time-dependent ageing window for optimal hydrogel spinnability. This study provides novel rheological and structural insights into mechanisms of protein-polysaccharide assembly that may prove instrumental for development of tuneable fibres for applications in plant-based foods, tissue engineering, and biomaterials.
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Feb 2025
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I22-Small angle scattering & Diffraction
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Qian
Ma
,
Andri K.
Riau
,
Robert D.
Young
,
James S.
Bell
,
Olga
Shebanova
,
Nicholas J.
Terrill
,
Gary H. F.
Yam
,
Evelina
Han
,
Keith M.
Meek
,
Jodhbir S.
Mehta
,
Craig
Boote
Diamond Proposal Number(s):
[23514, 28285, 29862, 34903]
Open Access
Abstract: Purpose: Donor tissue shortfalls and postsurgical complications are driving novel corneal tissue regeneration approaches. Corneal stromal keratocytes (CSKs) have shown promise in promoting corneal repair and restoring transparency. We investigated the impact of intrastromal CSK injection on corneal ultrastructure and proteoglycan (PG) distribution in a rat injury model.
Methods: Rats were divided into four groups: normal (n = 12), injured (irregular phototherapeutic keratectomy centrally; n = 6), CSK (injured + human CSK intrastromal injection; n = 6), and PBS (injured + PBS injection; n = 6). Three weeks after treatment, corneas were examined by slit-lamp and optical coherence tomography. Corneal ultrastructure was analysed via small-angle x-ray scattering (collagen fibril diameter, interfibrillar spacing and matrix order), transmission electron microscopy with cuprolinic blue before and after chondroitinase digestion (CS/DS and KS PGs), and immunofluorescence staining (lumican and decorin).
Results: Irregular phototherapeutic keratectomy caused corneal opacity and significantly disrupted stromal ultrastructure, characterized by increased haze density (P < 0.0001), change in central corneal thickness (P = 0.0005), and interfibrillar spacing (P < 0.0001), along with decreased fibril diameter (P < 0.0001), matrix order (P < 0.0001), CS/DS (P < 0.0001) and KS (P < 0.0001) PGs, lumican, and decorin. CSK injection recovered corneal clarity and native stromal ultrastructure, with haze density (P = 0.8086), change in central corneal thickness (P = 0.9503), fibril diameter (P = 0.1139), interfibrillar spacing (P = 0.5879), matrix order (P = 0.9999), CS/DS (P = 0.9969) and KS (P = 0.2877) PGs, lumican, and decorin returning to normal. In contrast, the PBS group exhibited similar corneal injury responses to the injured group.
Conclusions: CSK injection resolved early stage corneal scarring by restoring stromal collagen arrangement and PG distribution, further endorsing its potential for treating corneal opacities.
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Feb 2025
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I22-Small angle scattering & Diffraction
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Diamond Proposal Number(s):
[33748, 35376]
Open Access
Abstract: We report that self-supporting mesoporous platinum 3D nanowires with a single diamond (SD) morphology and a high specific surface area of 40.4 m2 g–1 demonstrated enhanced stability toward the oxygen reduction reaction (ORR). These were found to be superior to commercially available carbon-supported Pt nanoparticles (Pt/C). After 1000 potential cycles, there was a 21% loss in surface area for SD-Pt, as compared with a 40.3% loss for Pt/C with no reduction in their half-wave potential (measured at J = 3.0 mA cm–2), whereas the Pt/C catalyst showed a 11.9 mV decrease. Our findings revealed that our SD-Pt thin films also exhibited excellent ORR activity, which offers significant potential for their application as high-performance cathode materials in alkaline fuel cells.
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Feb 2025
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I22-Small angle scattering & Diffraction
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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.
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Nov 2024
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