B18-Core EXAFS
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Diamond Proposal Number(s):
[36104]
Abstract: Seawater splitting has been considered an environmentally friendly and cost-effective method for hydrogen production. However, developing efficient electrocatalysts capable of enduring the severe corrosive conditions of natural seawaters for extended durations remains a notable technical challenge. Herein, the Ni3S2 supported NiFe oxalate ((NiFe)C2O4/Ni3S2) nanorod arrays were synthesised through hydrothermal and impregnation precipitation methods. Structural and spectroscopic analyses revealed that the (NiFe)C2O4/Ni3S2 catalyst formed an integrated oxide-sulfide interface with coexisting Ni–O/Ni–S coordination. This dual coordination environment, coupled with the presence of Fe in a higher oxidation state, confirmed interfacial electronic reorganization characterized by directional electron transfer from Ni to Fe. The resulting charge transfer pathway enhanced the electron delocalisation between active centers, thereby improving active site utilization. The obtained (NiFe)C2O4/Ni3S2 demonstrated remarkable catalytic activity for hydrogen evolution reaction (HER) and oxygen evolution reaction (OER) in a simulated alkaline seawater solution (NaCl + KOH), with overpotentials of 363 mV (HER) and 295 mV (OER) at a current density of 500 mA cm−2 for industrial electrolysis requirements and remarkable stability over 100 h of durability testing. Additionally, the (NiFe)C2O4/Ni3S2 electrode pairs only required a cell voltage of 1.81 V to achieve 100 mA cm−2 with Faradaic efficiency of 98 % in 1.0 M KOH + seawater. This study presents a novel approach for fabricating multifunctional electrocatalysts, providing a promising pathway for advancing seawater electrolysis and supporting the development of cost-effective green hydrogen production technologies.
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Nov 2025
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B16-Test Beamline
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Diamond Proposal Number(s):
[33032]
Open Access
Abstract: This study presents the first demonstration of the use of X-ray diffraction (XRD) to quantify the radial or transverse deformation in Hexcel IM7 PolyAcryloNitrile (PAN)-based carbon fibres at temperatures as low as 200 K (-70 °C). The Coefficient of Thermal Expansion (CTE) is a critical design parameter that needs to be precisely quantified for the next generation of carbon fibre-based Liquid Hydrogen (
) storage tanks for net-zero aviation. This variable quantitatively describes the thermal mismatch between the fibre and the resin that is the driver for microcracking and tank leakage. However, quantification of the CTE of the fibres is experimentally challenging. The results provide unique insights, indicating that the microscopic transverse CTE of the fibre (
) is equal to 26.2 × 10-6 K-1 and is governed by van der Waals forces, similar to those in the basal c-axis (out-of-plane) direction of graphite and the radial direction of multi-wall carbon nanotubes. Taking into account the microcrack-induced relaxation effect reported in polycrystalline graphite, the macroscopic fibre transverse CTE was determined to be 7.86 × 10-6 K-1. XRD data were also collected on Hexcel IM7/8552 Uni-directional (UD) and Quasi-isotropic (QI) composite laminates to investigate the influence of the interaction of the resin matrix with the fibre lattice and the stacking sequence on the development of thermal fibre lattice strain. In the UD laminate, the presence of resin induces an additional transverse strain in the fibres as a result of resin contraction during cooling, leading to the development of a compressive strain in the fibre direction. This behaviour was found to be in good agreement with numerical simulations, with a 13 % error at the lowest measured temperature. In contrast, the fibres in the QI configuration were reinforced in the transverse direction, effectively mitigating the influence of resin contraction. These CTE values, insights, and resulting models are essential for multi-scale modelling, design and certification of carbon fibre composite
tanks that are required to achieve net-zero aviation.
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Oct 2025
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I11-High Resolution Powder Diffraction
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Diamond Proposal Number(s):
[32708]
Open Access
Abstract: BCC superalloys are a promising class of high-temperature materials with a wide range of lattice misfit values, ranging from near-zero to ∼8 %. Analogous to nickel superalloys, lattice misfit combined with elastic anisotropy dictates precipitate morphology (spherical, cuboidal, plate/needle-like), coarsening kinetics, strengthening mechanisms, and microstructure evolution, making misfit control critical for tailoring microstructural stability and creep resistance. However, misfit characterisation, especially at high temperatures, is still in its infancy to establish its links with mechanical properties. This perspective emphasises three aspects of BCC superalloys: representative misfit-driven microstructures and temperature-dependent misfit evolution, state-of-the-art diffraction techniques for high-temperature misfit quantification, and machine learning frameworks to accelerate alloy design involving misfit. By consolidating diverse misfit data and advanced characterisation/modelling strategies, we outline strategies to bridge computational and experimental gaps, advocating for physics-informed models and high-throughput techniques to design next-generation BCC superalloys and motivate systematic studies on the misfit-property relationship in this nascent material class.
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Oct 2025
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B16-Test Beamline
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Diamond Proposal Number(s):
[30528]
Open Access
Abstract: This paper demonstrates a new approach that exploits both lattice strain mapping via Wide Angle X-ray Scattering (WAXS) and Digital Volume Correlation (DVC) of Computed Tomography (CT) to understand the material response at different length scales in Carbon Fibre Reinforced Polymers (CFRPs) under in-situ loading, a phenomenon of substantial importance for the modelling, design, and certification of composite structures. WAXS gives insight into fibre lattice strain, while DVC provides sub-laminate response in the CFRP. A detailed numerical simulation was also developed to compare with these novel experimental methods. This approach is the first demonstration that the strain within the crystalline regions of the fibre is distinct from the sub-laminate behaviour, with up to 80 % and 36 % differences in the longitudinal and transverse directions, respectively, as a result of the complex microstructure of the fibres. An improved understanding of composite behaviour is fundamental to understanding how strain accommodation leads to structural failure, providing routes to refine part rejection criteria and reduce the environmental impact of this increasingly widespread material class.
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Oct 2025
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B18-Core EXAFS
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Aysun Ipek
Paksoy
,
Luis Francisco
Bobadilla
,
Rubén
Blay-Roger
,
Loukia-Pantzechroula
Merkouri
,
Victor
López-Flores
,
Claude
Coppex
,
Jelena
Jelic
,
Felix
Studt
,
Tomas
Ramirez Reina
,
José Antonio
Odriozola
,
Melis Seher
Duyar
Diamond Proposal Number(s):
[29271]
Abstract: This study reports a dual function material (DFM) composed entirely of non-precious metals for methanol production (13.8 μmol/g material) at ambient pressure from passively captured CO2 from the air. While state of the art carbon capture and utilisation (CCU) processes rely on expensive CO2 capture systems and a high-pressure catalytic reactor for methanol synthesis, this Ni-Ga-Ca DFM can be an enabler for significant energy efficiency gains in methanol synthesis from CO2 through the direct utilisation of dilute emissions and substantially lower operating pressures. Using operando DRIFT spectroscopy coupled with density functional theory, XAFS, XRD, and TEM-HAADF, a combination of Ni-Ga intermetallic species and their oxides are identified as the active sites. During cyclic operation a shift in selectivity towards methane is observed, which is associated with dynamic restructuring of the DFM. Guided by mechanistic and structural understanding, a synthesis strategy is developed to enhance cyclic stability by mitigating dealloying and Ni particle agglomeration. It is indicated that cyclic stability can be achieved by strengthening the Ni-Ga-Ca interaction, however, there remains a gradual shift in selectivity towards methane which highlights the need for further material optimisation.
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Sep 2025
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I11-High Resolution Powder Diffraction
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Diamond Proposal Number(s):
[33667]
Open Access
Abstract: Refractory high entropy alloys have gained significant interest over the past decade as promising candidates for high-strength applications, particularly at high temperatures. However, achieving ductility and workability at room temperature remains a challenge for large-scale manufacturing and applications. This study explores the design and characterisation of a novel RHEA with low density, high ductility, and high strength at room temperature. High-throughput screening and experimental validation identified a non-equiatomic composition, Zr35Ti35Nb20V5Al5 (at%), which exhibits a room-temperature yield strength of 1030 MPa, 11% tensile strain to failure, and a low density of 6 g/cm3. The alloy's grain size was refined to <20 μm through rolling and recrystallisation, bypassing traditional high-temperature homogenisation while avoiding microsegregation. The tailored Zr35Ti35Nb20V5Al5 RHEA demonstrates a new design approach and processing route, opening applications in next-generation nuclear and aerospace technologies.
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Aug 2025
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Accelerator Physics
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Younes
Chahid
,
Carolyn
Atkins
,
Stephen
Hodbod
,
John
Robinson
,
Xia
Liu
,
Stephen
Watson
,
Maia
Jones
,
Mark
Cliffe
,
Dayo
Ogunkanmi
,
Richard
Kotlewski
,
Lee
Chapman
,
Scott
Beamish
,
Jorge
Linde Cerezo
,
Thomas
Wearing
,
Ahmad
Baroutaji
,
Arun
Arjunan
,
Chantal
Fowler
,
Paul
Vivian
Open Access
Abstract: Many of the 70 synchrotron facilities worldwide are undergoing upgrades to their infrastructure to meet a growing demand for increased beam brightness with nanometre-level stability. These upgrades increase the mechanical and thermal challenges faced by beamline components, creating opportunities to apply novel methodologies and manufacturing processes to optimize hardware performance and beam accuracy. Absorbers are important beamline components that rely on water-cooled channels to absorb thermal energy from excess light caused by synchrotron radiation or photon beams created by insertion devices, all within a limited volume, to protect downstream equipment and ensure safe, reliable operation. Additive manufacturing (AM) has been shown to meet criteria relevant to synchrotron environments like leak tightness and vacuum compatibility. However, there is a research gap on the heat transfer and pressure drop impact of different AM conformal cooling channel geometries, as well as the print quality of AM copper parts using low-power infrared lasers and their compliance with absorber requirements. In this study, an intermediate model of a Diamond Light Source photon absorber was optimized to incorporate AM conformal cooling channels, leading to two concept designs named `Horizontal' and `Coil'. When compared with the baseline design, the lightweight Horizontal concept performed the best in this study, with simulations showing a maximum temperature drop of 11%, a calculated pressure drop reduction of 82%, a mass reduction of 86%, and the consolidation of 21 individually brazed pipes into a single manifold. The AM print quality and compliance with the synchrotron environment was examined by producing custom benchmark artefacts and measuring their surface roughness, dimensional accuracy and porosity levels, which are characteristics that can affect heat absorption, structural integrity, thermal conductivity and vacuum performance. The study demonstrates the benefits and addresses outstanding challenges in reducing thermal fatigue, as well as the size, vibrations and energy consumption of AM absorbers.
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Jul 2025
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I20-EDE-Energy Dispersive EXAFS (EDE)
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Diamond Proposal Number(s):
[30680]
Open Access
Abstract: The increasing demand for environmentally friendly and sustainable approaches to materials synthesis calls, inter alia, for the development of biogenic methods to produce inorganic compounds by exploiting biological macromolecules and organisms. This study focuses on the optimization of a one-pot green synthesis of zinc oxide (ZnO) particles using microalgae extracts as a biogenic agent. Microalgae serve as an environmentally friendly platform for biotechnological applications due to their ability to promote the synthesis of valuable chemicals, thanks to their active components, such as enzymes. A systematic investigation of the experimental parameters revealed that both the reaction temperature and the concentration of microalgae extract significantly influenced the crystallite size of ZnO nanoparticles. In addition, the role of sodium hydroxide as a precipitating agent when used in combination with microalgae extract was addressed and compared with existing literature. The results indicate that microalgae extract can act as a scaffold to promote the controlled growth of ZnO particles. Antimicrobial tests also showed that ZnO particles synthesized with microalgae exhibited comparable antimicrobial activity with respect to ZnO produced by conventional methods. These results highlight the potential of microalgae as biogenic agents for the green synthesis of ZnO particles with tunable structural and antimicrobial properties.
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Jul 2025
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I18-Microfocus Spectroscopy
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Xutong
Wang
,
Huwei
Li
,
Junxia
Wang
,
Wolfram
Buss
,
Anna
Bogush
,
Ondrej
Masek
,
Youjun
Zhang
,
Fan
Yu
,
Beibei
Yan
,
Zhanjun
Cheng
,
Xiaoqiang
Cui
,
Guanyi
Chen
,
Konstantin
Ignatyev
Diamond Proposal Number(s):
[32515]
Abstract: Recycling of sewage sludge and the endogenous phosphorus (P) is a promising strategy for sustainable development, while the disposal of heavy metals (HMs) in sewage sludge and the recovery of targeted P species remain challenges. An innovative method coupling electrokinetic treatment with pyrolysis was proposed in the present study to achieve the effective reclamation of available P and the separation of HMs from sewage sludge. The pristine and FeCl3-assisted electrokinetic treatment were employed for the removal of HMs from sewage sludge and to modify the P species, and the subsequent pyrolysis (300–700 °C) was conducted for the recovery of available P along with the production of biochar. The X-ray absorption near-edge spectroscopy (XANES), 31P liquid nuclear magnetic resonance (NMR) spectroscopy, and sequential chemical extraction were used to systematically determine the evolution of P during the combined treatment of sewage sludge. 19.69–24.80 % of Ni, Cu, and Zn were removed from sewage sludge after pristine electrokinetic treatment, and the HM removal efficiency was further elevated to 47.01–56.86 % with the assistance of FeCl3. Consequently, in comparison with the raw sewage sludge-derived biochars (SBs), the biochars derived from FeCl3-assisted electrokinetic treated sewage sludge (FESBs) contained much lower HM contents and showed higher stability of HMs. The FeCl3-assisted electrokinetic treatment converted alkaline biochars dominated by poorly soluble Ca-phosphates into neutral to slightly acidic biochars dominated by Al/Fe-associated phosphates. This transformation greatly improved the available P concentrations determined by diffusive gradients in thin film in FESBs by 0.6–1.3 folds compared to untreated SBs. Therefore, coupling FeCl3–assisted electrokinetic treatment with pyrolysis could be a promising strategy to achieve the reclamation of available P and the separation of HMs from sewage sludge.
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Jul 2025
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B21-High Throughput SAXS
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Diamond Proposal Number(s):
[23942]
Open Access
Abstract: Performance plastics, such as poly(methyl methacrylate), underpin the modern economy. Global manufacturing of plastic precursors relies on fossil carbon sources, and the urgently needed shift toward renewable carbon use through biofermentation is hindered by the low tolerance of producer strains to methacrylate esters. The principal mode of butyl methacrylate cellular toxicity is membrane disruption. To understand this process, the conditions for membrane stability, and recovery after solvent shock, we investigate the phase stability of hydrated lipid membranes at high levels of a key intermediate, butyl methacrylate. We assess the role of cis- vs trans-unsaturation in 18-carbon chain phospholipids on butyl methacrylate-induced phase conversion and polymorphism. Using ssNMR, SAXS and cryoEM, we demonstrate the formation of stable lipidic cubic phases in hydrated lipid/solvent (cis-chain phospholipid lipid/butyl methacrylate) systems at a 1:6 molar ratio entirely lacking monoolein. Transient lipidic cubic phases form in trans-chain phospholipid/butyl methacrylate systems, which slowly convert to bilayers through a spontaneous “membrane healing” process during recovery after solvent shock. The observed bicontinuous nanostructures with a cubic phase architecture coexist with a stable, monocontinuous hydrated phase of the same morphology but with simpler topological connectivity, which demonstrates that phase stability in cubic phases does not require topological complementarity. We propose trans-lipid substitutions in membranes of fermentative strains as a key step toward sustainable production of methacrylate esters.
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Jul 2025
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