I09-Surface and Interface Structural Analysis
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Diamond Proposal Number(s):
[36180]
Abstract: Cr2GaC/C and V2PC/C MAX phase composites were synthesized via a free-radical polymerization–pyrolysis route, achieving > 87 wt% crystalline MAX phase content. SEM/EDS confirms the expected 2:1 atomic ratios of Cr:Ga and V:P, while BET analysis reveals structures with specific surface areas of 344 and 282 m2 g−1 for the Cr2GaC/C and V2PC/C composites, respectively, which are attributed to the porous carbonaceous network. HAXPES verifies core-level signatures consistent with the targeted MAX phases. This approach demonstrates the versatility of sol–gel-derived free-radical polymer networks as reactive precursors for MAX phase formation. The method further provides a foundation for advanced processing strategies, including vat photopolymerization-based additive manufacturing of high-surface-area and complex MAX phase architectures.
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Sep 2026
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[37837, 33810]
Open Access
Abstract: Multilayer braided composite tubes are widely used in torsion-critical structures, yet their damage behaviour remains insufficiently understood. Here, we investigate vacuum-infused single-, double- and triple-layer ±45° diamond-braided carbon fibre/epoxy tubes under torsion using in-situ, time-resolved synchrotron X-ray computed tomography. Increasing the number of layers promotes inter-layer nesting and modifies the mesoscale architecture, producing a through-thickness variation in fibre volume fraction and a reduction in tow crimp from the inner to the outer layers. Although the effective shear modulus changes only marginally (∼8.2–8.5 GPa), the shear strain at damage initiation increases from ∼0.5% in single-layer tubes to ∼0.75% and ∼1.0% in double- and triple-layer tubes, respectively. Damage in the double- and triple-layer tubes is dominated by inter-layer and inter-tow debonding, whereas single-layer tubes show predominantly intra-tow cracking. Microscale fibre buckling/kinking is also delayed in the multilayer tubes, consistent with the through-thickness tow-crimp gradient and additional lateral confinement. The multilayer tubes further exhibit a more stable post-peak response, with no pronounced load drops in the load–displacement curves. Overall, these observations show that changing the number of braided layers substantially alters the mesoscale tow architecture and, in turn, governs the torsional damage response of braided composite tubes.
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Aug 2026
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[34540]
Open Access
Abstract: Fibrous plaster (FP) is a fabric-reinforced composite (FRC) comprising plaster of Paris (POP) and woven jute fabric (‘hessian’), historically used in decorative ceilings across the UK since the late 19th century. Despite its architectural significance, FP remains under-researched, limiting the development of reliable structural assessment methods. Recent ceiling failures have been linked to the tensile failure of the supporting component known as the ‘wad’. Acoustic emission (AE) provides a non-destructive means of remotely sensing and locating such failures from the underside of ceilings, yet its potential for extracting detailed information on FP wad failure processes remains unexplored. This study comprises two parts. First, an AE-based failure classification model was developed using unsupervised spherical k-means clustering to distinguish matrix cracking and fabric–matrix debonding based on the RA-AF method. Second, the first in-situ direct tensile tests on FP wad-analogue specimens conducted under synchrotron X-ray imaging were conducted at the I12 beamline of Diamond Light Source (DLS), UK, integrating AE monitoring with digital image correlation (DIC) and synchrotron X-ray computed tomography (sCT). This multi-modal dataset enabled examination of the AE model and internal failure analysis through digital volume correlation (DVC), while complementary crack analysis and the Kabsch algorithm provided new insight into the failure mechanisms of FP wads and revealed the reinforcement-bridging role of the hessian during progressive fracture. By linking remote AE monitoring with multi-scale observations, this study advances understanding of FP failure processes, offering a pathway for assessing historic ceilings and informing the design of more resilient FP components.
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Jun 2026
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I13-2-Diamond Manchester Imaging
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Dongze
He
,
Yuan
Chai
,
Jiduo
Zhang
,
Mohammad
Islam
,
Leonard
Turpin
,
Kaz
Wanelik
,
Valeriy
Titarenko
,
Elizabeth E.
Evans
,
Zihan
Song
,
Timothy L.
Burnett
,
Kali Babu
Katnam
,
Prasad
Potluri
,
Philip J.
Withers
Diamond Proposal Number(s):
[37837, 33810]
Open Access
Abstract: The aim of this study was to examine the extent to which different resin infiltration processes can lead to different architectures and hence different mechanical properties in braided composites based on the same textile preforms (i.e. having the same fibre content). To this end single-layer carbon/epoxy (±45°) braided tubes have been manufactured vacuum assisted resin infusion using: (a) resin transfer moulding (RTM) with rigid inner and outer moulds, and (b) vacuum infusion (VI) with a rigid inner mould, but with a flexible outer mould. Their 3D architecture and the resulting torsional behaviour has then been investigated by in-situ synchrotron X-ray CT and image-based finite element modelling. The VI process gave a significantly reduced the tube wall thickness (∼35%) relative to RTM, higher effective fibre volume fraction (∼55% VI vs ∼33% RTM) and flatter (half-lenticular) tow geometries with greater in- and out-of-plane crimp and higher crossover density. Taken together these differences in mesoscale architecture led to the VI braided tube exhibiting ∼16% higher shear modulus yet ∼30% lower torsional rigidity compared to the RTM specimens. Image-based modelling showed that the flattened tows and increased crimp angles in the VI braided tubes amplified the local stresses, leading to earlier damage initiation (∼0.5% shear strain) and intra-tow cracking. More widely this study exemplifies how different resin infiltration processes can lead to different post-cure fibre architectures and mechanical performance, even when based on the same textile preform.
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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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E03-EM03E ePSIC Microscope (JEOL FIB)
I13-1-Coherence
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Diamond Proposal Number(s):
[39271]
Open Access
Abstract: Multi-material structures have shown great versatility in wide applications. However, additive manufacturing of multi-metal mechanical composite structures is challenging. Beyond this, a comprehensive and multi-scale understanding of the fracture mechanisms in such structures has not been sufficiently elucidated. In this study, we exploited synchrotron phase contrast X-ray computed tomography and synchrotron X-ray ptychographic tomography to achieve in situ, continuous observation of the fracturing process in large-scale brick-and-mortar multi-metal composite structures, resolving phenomena spanning from the micro- to nano- scale. Findings suggest that nano-pores prevailingly exist in additively manufactured metals, and interfacial porosity as a transitional geometry between different materials can retard the crack growth and improve fracture toughness. This multi-scale study directly informs the designing, manufacturing, and testing of multi-metal composite structures.
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May 2026
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B22-Multimode InfraRed imaging And Microspectroscopy
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Diamond Proposal Number(s):
[40142]
Open Access
Abstract: Triboelectric nanogenerators (TENGs), which convert mechanical energy into electrical signals, have emerged as apromising platform for self-powered motion sensing. However, the development of high-sensitivity TENG sensors remains limited by the availability of tunable and efficient tribo-positive materials, which are electron donors. In this work, we present a material design strategy based on the incorporation of electron-donating functionalized metal–organic framework (MOF) fillers into a polyurethane (PU) polymer matrix. Three functional groups (−CH3, −NH2, and −OH) were systematically studied to investigate their influence on triboelectric performance. The resulting composite membranes demonstrated tunable charge-donating behavior and improved electrical output, with the −OH-modified MOF yielding the highest electrical output of 197.6 ± 1.3 V and 0.47 ± 0.08 μA/cm2, which are 2.3 and 3.2 times higher than that of the pristine PU. The enhanced charge-donating mechanism was elucidated through a combination of advanced micro- and nanoscale chemical and mechanical analysis. Theoretical calculations employing ab initio density functional theory (DFT) were performed to reveal the electron distribution within the periodic MOF structure. Furthermore, the practical application of the optimized TENG device was demonstrated in a single-electrode shear sensor configuration, exhibiting high sensitivity in sliding motion detection. This study highlights a scalable and biocompatible strategy for improving tribo-positive materials and advancing the performance of tunable TENG-based sensors to enable shear force monitoring.
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Mar 2026
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I13-2-Diamond Manchester Imaging
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Abstract: The volumetric additive manufacturing (VAM) of multifunctional polymer composites presents transformative potential for industries seeking sustainable, efficient, and precise production of complex geometries. However, challenges persist in controlling material properties, scaling for multifunctionality, and achieving cost-effective, eco-friendly manufacturing. This review explores state-of-the-art advancements in VAM technologies, including magnetic field-assisted reshaping, which decouples geometric complexity from initial fabrication. By utilizing external fields to reconfigure simple 3D-printed geometries into intricate structures, this approach drastically reduces production times, energy consumption, and interlayer defects. The study highlights the urgent need for process-serving composite materials with self-tuning properties, capable of responding to electromagnetic fields for geometric reshaping, enhanced reinforcement distribution, and polymerization control. Applications across aerospace, biomedical, and automotive industries currently underscore the versatility and sustainability of these methods. Furthermore, this chapter advocates for integrating circular manufacturing principles, emphasizing reusability and recyclability, to extend the lifecycle of components and minimize environmental impact. Emerging techniques in field-assisted VAM offer profound opportunities for scaling up complex, multifunctional composite production, fostering a paradigm shift toward green and adaptive manufacturing practices.
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Mar 2026
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I13-2-Diamond Manchester Imaging
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Mahendra P.
Raut
,
Andrea
Mele
,
Nicholas T. H.
Farr
,
Caroline S.
Taylor
,
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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E03-EM03E ePSIC Microscope (JEOL FIB)
I13-1-Coherence
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Diamond Proposal Number(s):
[39271, 42138]
Open Access
Abstract: Modern electroconductive materials involve copper-based carbon-enhanced composites featuring convenient mechanical properties and, simultaneously, favorable electric conductivity. Such composites can be processed by deformation/thermomechanical treatments to introduce advantageous microstructures, further enhancing their performance. The study features powder-based copper–carbon (Cu/C) composites, fabricated from chemical vapor deposition-prepared powder mixture by a direct consolidation using the rotary swaging method, which enables to eliminate the typical (costly and time consuming) preparation steps of consolidation and sintering. The directly consolidated Cu/C composites were further processed by the severe plastic deformation method of high-pressure torsion (HPT), introducing severe shear strain and high pressure and thus providing fine-grained microstructures. The consolidated composites were processed with two HPT revolutions. The results showed that the final microstructures and properties were primarily influenced by the carbon content within the prepared powder mixture; although the HPT-processed composites featured homogeneous fine-grained microstructures with the average grain sizes of 2–3 µm, the sizes of the graphene particles varied. The Vickers microhardness exceeded 100 HV0.1 for all the samples, and the electric conductivity varied between 98.8% and 102.1% IACS (International Annealed Copper Standard).
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Mar 2026
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