I22-Small angle scattering & Diffraction
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Diamond Proposal Number(s):
[34844, 37870]
Open Access
Abstract: Fats are essential ingredients widely used in the food industry, as well as in cosmetic and pharmaceutical formulations. Solid fats are complex multicomponent systems primarily composed of triacylglycerols (TAGs), which determine the types and properties of the crystalline structures formed. TAGs crystallize in different polymorphs and stacking configurations, with distinct thermal and mechanical properties that influence the macroscopic structure and sensory profile of fat-based products. In this study, a comprehensive multi-technique analysis of animal-derived fats, specifically chicken and beef fats, was conducted. Chemical characterization was performed and solid fat content (SFC) was determined. Thermal behaviour was investigated using differential scanning calorimetry (DSC), whereas crystallization experiments were conducted using in situ turbidity measurements and synchrotron small-angle and wide-angle x-ray scattering (SAXS/WAXS) for structural characterization. Three different synchrotron experimental setups were used for crystallization experiments, including static and sheared conditions. The results demonstrate that the crystallization behaviour of beef and chicken fat samples closely correlate with their TAGs composition. Synchrotron x-ray scattering provided structural insights, highlighting how the polymorphic behaviour is influenced by fat origin and crystallization conditions. For both animal fat types, all three main polymorphs and possible transitions were detected. Moreover, the presence of shear promoted crystallization of stable polymorphs.
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May 2026
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I22-Small angle scattering & Diffraction
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Diamond Proposal Number(s):
[29929]
Abstract: Objectives: Biomimetic hydroxyapatite (HAp)-based composites are promising materials for dental restorations due to their hierarchical structure and similarity to natural dental tissues. This study aims to investigate the three-dimensional crystallographic organization of HAp within nacre-inspired composites and to evaluate how different polymers infiltrations influence the structural orientation.
Methods: Nacre-inspired HAp ceramic scaffolds were fabricated via bidirectional freeze-casting and subsequently infiltrated with different polymers, including Polyurethane (PU), Poly(methyl methacrylate) (PMMA), Epoxy, and Urethane dimethacrylate (UDMA). The three-dimensional structural organization and crystallite orientation of these composites were investigated using synchrotron-based 3D SAXS tensor tomography (3D SASTT), complemented by scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX).
Results: The results reveal distinct differences in crystallite alignment among the composites. HAp/PU exhibits the highest degree of preferred orientation (∼0.7–0.8), whereas HAp/PMMA and HAp/Epoxy show lower alignment values (∼0.2–0.4). The HAp/UDMA composite displays heterogeneous orientation with localized regions of moderate alignment. SEM and EDX analyses confirm variations in lamellar morphology, polymer infiltration, and porosity distribution across the composites.
Significance: These findings demonstrate that 3D SASTT enables quantitative mapping of nanoscale crystallite orientation within bulk biomimetic scaffolds and provides new insights into the hierarchical structure of composites, supporting structural design of advanced dental restorative materials.
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May 2026
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I22-Small angle scattering & Diffraction
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Diamond Proposal Number(s):
[36753]
Open Access
Abstract: Slow skeletal muscles maintain posture and produce graded movement at low metabolic cost. ATP utilization during fixed-end contractions is typically five times slower in slow muscles than in fast muscles from the same species. Mechanical measurements previously suggested that more myosin motors are attached to thin filaments during contraction of slow muscle, which seems incompatible with its high efficiency. We therefore used small-angle X-ray diffraction to provide a structural estimate of the fraction of myosin motors attached to thin filaments in slow muscle. The X-ray signals associated with myosin binding to actin indicate that only ∼10% of myosin motors are actin bound during fixed-end tetani of rat soleus slow muscles, compared with ∼25% in mouse extensor digitorum longus fast muscle. Moreover, X-ray signals associated with the helical organization of OFF myosin motors in the thick filaments show that ∼70% of myosin motors remain in the OFF conformation during tetanic contraction of rat soleus muscle, compared with only 30% in mouse extensor digitorum longus muscle. The much slower force development in soleus muscle also allowed clear separation of early structural changes in thick filaments on activation, some of which are distinct from those reported previously in fast muscles. Moreover, the early structural changes in soleus muscle have about the same amplitude in a twitch and a tetanus, suggesting that they are triggered by thin filament activation rather than thick filament stress and implying a fast signalling pathway between thin and thick filaments.
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Apr 2026
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I22-Small angle scattering & Diffraction
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Diamond Proposal Number(s):
[37847]
Open Access
Abstract: We report a simple design strategy to introduce lithium-responsiveness into N-capped peptide low-molecular-weight gelators by incorporating the FFD tripeptide motif (FF extended with Asp). Asp adds an oxygen-rich carboxylate residue that enables cation-mediated assembly. In high pH aqueous solutions, 2NapFFD shows a pronounced cation selectivity. Li+ generates highly viscous, shear-thinning solutions with birefringent textures, while other Group 1 metals and bulky organic counterions result in low-viscosity and weakly ordered solutions. SAXS and SANS reveal that the addition of Li+ produces substantially extended micellar structures consistent with long cylindrical assemblies, whereas other monovalent cations lead to the formation of short cylindrical objects. The Li+ selectivity is intrinsic to the FFD sequence, with other aromatic caps tuning packing and mesoscale order. Finally, dialysis-driven Li+ exchange induces gelation and enables us to quantify the Li+ uptake by ICP-OES, illustrating potential for selective lithium capture.
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Apr 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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Diamond Proposal Number(s):
[36690]
Abstract: The online structure development during tenter-frame biaxial stretching of linear low-density (LLDPE), high-density polyethylene (HDPE), and their 50/50 blend was investigated using synchrotron Wide-Angle X-ray Scattering (WAXS). During stretching, crystallite reorientation, crystallographic slip phenomena activated at yielding, and lamellar fragmentation at higher strains are responsible for a decrease in crystallinity. These processes induce a morphological transformation from the initial semisolid spherulitic morphology into an oriented fibrillar network with lamellae in edge-on orientation, and the b- and c-axes constrained within the film plane, as confirmed by ex-situ WAXS and SAXS. These phenomena are more important for HDPE, which exhibits higher susceptibility to biaxial stretching. Upon cooling, the morphology developed during stretching is preserved, as newly crystallized material grows epitaxially on the preexisting structure. These findings highlight the higher structural sensitivity of HDPE during semisolid biaxial stretching compared with LLDPE, providing unique information to understand and control the biaxial processing of polyethylene.
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Mar 2026
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I22-Small angle scattering & Diffraction
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Diamond Proposal Number(s):
[39895]
Open Access
Abstract: Benchtop ultra-small-angle X-ray scattering (USAXS) offers a practical route to probing micron-scale structural features in soft-matter systems, provided that instrumental limitations are explicitly defined and respected. In this work, a Rigaku NANOPIX mini USAXS instrument is used to characterize hierarchical fat crystal networks, with emphasis on establishing a reliable analysis window and appropriate treatment of slit-geometry effects. Analyzer crystal rocking curves are employed to define a lower bound for quantitative analysis (qmin ≈ 3.4 × 10−4 Å−1), while counting-statistics considerations define an upper bound (qmax ≈ 1.4 × 10−2 Å−1). Data outside this window are shown to be strongly influenced by direct-beam and noise artifacts and are therefore excluded from interpretation. Within the valid q-range, slit-smearing effects inherent to Bonse–Hart geometries are addressed by smearing structural models using open-source SASView software rather than numerically desmearing experimental data. Using cocoa butter, commercial chocolate, and a reference triglyceride mixture as representative case studies, power-law scattering regimes are extracted and compared with synchrotron SAXS measurements over overlapping q-ranges. While absolute slope values vary between instruments and samples, benchtop USAXS captures consistent scattering trends, including stable power-law behavior in tempered systems and transient curvature in untempered samples that diminishes upon storage. These results demonstrate that benchtop USAXS, when interpreted within a rigorously defined q-window and with appropriate resolution treatment, provides a reproducible and accessible tool for comparative analysis of hierarchical fat systems. More broadly, this study outlines best practices and interpretive boundaries for laboratory-scale USAXS measurements in soft-matter research.
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Mar 2026
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I22-Small angle scattering & Diffraction
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Diamond Proposal Number(s):
[39895]
Abstract: A hierarchical additive framework is developed for the quantitative interpretation of X-ray scattering (SAXS) from lamellar crystalline materials. The formulation extends the classical decomposition I(q) = P(q)S(q), with I(q) the scattering intensity, P(q) the form factor, and S(q) the structure factor, by explicitly coupling the contributions of three structural regimes: low-q power-law (fractal-like) aggregation, intermediate-q Guinier curvature arising from finite nanocrystal dimensions, and high-q Bragg reflections associated with lamellar periodicity. Each regime is expressed analytically and linked through shared structural parameters, ensuring physical consistency across length scales. The scattering intensity is interpreted as the Fourier transform of the electron-density correlation function, following Debye’s original formulation (Debye, 1915), which naturally accommodates cross-correlations between internal morphology and interparticle organization. Simulated scattering profiles illustrate how parameter variations influence the overall signature, and the model is applied to synchrotron SAXS data from cocoa-butter triacylglycerols to demonstrate practical fitting performance. The resulting approach provides a compact and physically rigorous description of hierarchical lamellar systems and offers a generalizable framework for complex materials in which form and structure factors cannot be treated independently.
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Mar 2026
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I22-Small angle scattering & Diffraction
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Sasha
Murokh
,
Alexander
Alekseev
,
Viacheslav
Kubytskyi
,
Viacheslav
Shcherbakov
,
Oleksii
Avdieiev
,
Sergey A.
Denisov
,
Ashkan
Ajeer
,
Lois
Adams
,
Charlene
Greenwood
,
Keith
Rogers
,
Lev
Mourokh
,
Pavel
Lazarev
Diamond Proposal Number(s):
[24977]
Open Access
Abstract: Structural biomarkers determined by X-ray scattering of the tissues can complement conventional histopathology and facilitate a fast triage procedure of cancer biopsy samples. It has been shown previously that lipid reflexes can distinguish cancerous from benign samples, except for fibroadenomas. In the present study, we demonstrate that fibroadenoma samples can be recognized using X-ray scattering of collagen. Moreover, we show that modifications in collagen structure are manifested in the water reflexes. Examination of diffraction patterns from water using two-dimensional Fourier transformation and machine learning yields excellent classification metrics in both synchrotron images and laboratory diffractometer data.
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Feb 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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