B18-Core EXAFS
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Diamond Proposal Number(s):
[34632]
Abstract: Polychlorinated aromatic hydrocarbons (PCAHs) in flue gas seriously threaten the environment and human health, and Ru-based catalysts exhibit efficient oxidation property for PCAHs removal. However, the current Ru catalysts either have high Ru loading/non-stable structure or are developed empirically whilst lack of design mechanism. Herein, a robust Ru single atom catalyst (0.5 Ru1/TiO2) was designed based on metal-support interaction for o-DCB (o-dichlorobenzene, a typical PCAHs) degradation, and it revealed significantly better oxidation activity with T50 = 207.4 °C and T90 = 243.5 °C than its contrast with weak metal-support interaction (0.5 RuNP/TiO2, T50 = 247.4 °C, T90 > 300 °C). In addition, 0.5 Ru1/TiO2 exhibited much better chlorine resistance stability, maintaining >90% o-DCB conversion for 700 min versus∼70% on 0.5 RuNP/TiO2. The superior performance of 0.5 Ru1/TiO2 was attributed to its stronger metal-support interaction between Ru and TiO2, verified by H2-TPR, which offered higher active oxygen species (22.4%), more Lewis acid (0.675 mmol/g) and higher exposed Ru ratio (> 90.0%) than 0.5 RuNP/TiO2 (15.0%, 0.068 mmol/g, 28.6%, respectively). The above properties can not only enhance o-DCB adsorption/activation and weaken its Csingle bondCl bonds but also favor partial/deep oxidation and remove deposited chlorine on 0.5 Ru1/TiO2, proved by in situ FT-IR. Moreover, notable higher water resistance under different water vapor and applicability under varied pollutant concentration were observed on the robust Ru1/TiO2. This work reveals insightful function-property study on Ru single atom catalysts for PCAHs oxidative removal.
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May 2026
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I15-1-X-ray Pair Distribution Function (XPDF)
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Diamond Proposal Number(s):
[345501]
Open Access
Abstract: The Ga₂S₃–Sb₂S₃ quasi-binary system has been investigated for its potential to yield stable chalcogenide glasses with tailored thermal and structural properties. Using melt-quenching techniques, a series of (Ga₂S₃)ₓ(Sb₂S₃)₁₋ₓ compositions (0.0 ≤ x ≤ 0.5) were synthesized, and their glass-forming domain was mapped. The latter extends up to approximately x ≤ 0.40, as confirmed by X-ray diffraction and DSC analyses, with the x = 0.4 composition exhibiting a glass-ceramic character. Density measurements, combined with calculations of molar volume and packing density, revealed a continuous structural densification as Ga₂S₃ content increased. Differential scanning calorimetry showed an increase in glass transition temperature (Tg), with the best thermal stability observed for x = 0.2, as assessed by the Hruby criterion. Electrical conductivity measurements demonstrated thermally activated behaviour following the Arrhenius law, with maximum activation energy also centred at x = 0.2. Raman spectroscopy and DFT modelling were used to decipher the structural contributions of Sb–S and Ga–S bonding. The emergence of vibrational modes characteristic of Ga-based structural units, especially beyond x > 0.2, suggests a structural reorganization from Sb-centred pyramidal units to Ga-centred tetrahedral. This was corroborated by high-energy X-ray diffraction, which showed significant changes in intermediate-range order with increasing Ga content, particularly in the first sharp diffraction peak and partial coordination environments.
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Apr 2026
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I14-Hard X-ray Nanoprobe
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Diamond Proposal Number(s):
[36126]
Open Access
Abstract: Coal fly ash (CFA), a metal-rich byproduct of coal combustion is produced in vast quantities and poses significant ecological risks. CFA also contains abundant technologically relevant metal oxides and trace metals, including rare earth elements (REE), often at higher concentrations than in primary ores. This makes sustainable recovery strategies a major industrial opportunity. Here, green solvent systems were applied to leach metals from CFA, and the resulting leachates were added to cultures of Magnetospirillum gryphiswaldense (MSR1), a model magnetotactic bacterium that biomineralizes iron into membrane-bound magnetic nanoparticles (magnetosomes) and is capable of interacting with non-iron metals through adsorption and biomineralization. Eleven green solvents, including deep eutectic solvents (DES), were tested for extraction efficiency, with six showing performance comparable to a mineral acid control. Copper (Cu) emerged as the primary toxicant to MSR1, prompting selective precipitation with potassium ferrocyanide trihydrate (PFCT) to reduce its concentration. Cu-depleted lactic acid-based leachates supported MSR1 growth and magnetosome formation even without supplemented iron. Nano-XRF and ICP-MS analysis revealed MSR1 interacts with CFA-derived metals, most significantly showing that produced CFA magnetosomes contained a 5.3–6.1-fold increase in Cu compared to controls. As Cu is both a growth inhibitor and a target pollutant, these findings suggest MSR1 may bioaccumulate Cu within magnetosomes as a detoxification strategy. Overall, this study demonstrates a combined chemical–biological route for CFA valorisation, enabling recovery of diverse metals from waste while producing magnetosomes with distinct compositions.
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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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I11-High Resolution Powder Diffraction
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Diamond Proposal Number(s):
[33667]
Open Access
Abstract: The use of conventional zirconium alloys at temperatures above 400 °C is limited by high temperature strength and creep resistance. This has prevented the consideration of zirconium alloys for fusion and Generation IV fission plant designs operating at 500 °C–1000 °C. The physical metallurgy of zirconium is similar to titanium which has seen alloying advances allowing application temperatures up to 600 °C. Although the oxidation resistance of zirconium-based alloys is expected to be poor, in a water environment, new Generation-IV and fusion reactors are designed to operate using alternative coolants such as liquid metals and molten salts. Therefore, a new class of zirconium alloys in the Zr-Al-Sn-(Si,Cr,V) system, designed by analogy to near-
titanium alloys, were synthesised by arc melting and processed in a sequence of homogenisation, hot/cold rolling, recrystallisation, and ageing treatments. Microscopy and diffraction identified a refined fully lath grain structure reinforced by nanoscale lamellar or discrete coherent Zr3Al precipitates, with morphology and crystal structure differing with ageing times. Additionally alloying with Si, Cr, and V respectively leads to Zr2Si, ZrCr2, and ZrV2 incoherent precipitates. Tensile testing revealed a strengthening effect by Al, but with significant changes to ductility on ageing depending on the evolution of Zr3Al. Creep testing showed creep rates orders of magnitude better than conventional Zircaloy-4 and nuclear ferritic/martensitic steels, approaching near-
Ti alloys. The present work offers new insights and perspectives into how high-temperature zirconium alloys might be designed to meet the requirements for fusion and Gen-IV fission.
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Mar 2026
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B18-Core EXAFS
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Yingxiang
Zhao
,
Yingjie
Zhao
,
Xinyue
Zhou
,
Haiwei
Guo
,
Qiqi
Yin
,
Yutao
Jiang
,
Haiyan
He
,
Na
Liu
,
Gengbo
Ren
,
Christopher M. A.
Parlett
,
Changzhi
Li
Diamond Proposal Number(s):
[34632]
Abstract: M–N–C single-atom catalysts (SACs) represent promising candidates owing to their atomically dispersed active sites and tunable catalytic properties and have shown broad potential in various catalysis reactions. However, the mechanisms and true active sites involved in lignin conversion, particularly oxidative depolymerization, remain unclear. Herein, a Ru–N–C SAC with a well-defined configuration, including coordination environment and coordination number, was synthesized via a straightforward ball-milling method for lignin oxidation. The Ru–N–C SAC prepared with 12 h of ball milling demonstrated high catalytic performance in the oxidative depolymerization of various β-O-4 model compounds and diverse lignin feedstocks. Structural analysis via X-ray absorption spectroscopy demonstrated that the Ru–N4 motif constitutes the predominant coordination environment in Ru–N–C, which is regarded as the primary active site in activating O2 into superoxide radicals, as confirmed by free-radical quenching experiments and electron paramagnetic resonance analysis; meanwhile, it also served as a basic site in polarizing Cβ–H bonds in β-O-4 that favored C–O/C–C bond cleavage, which was disclosed by CO2 temperature-programmed desorption and electron localization function analysis. The critical role of Ru–N4 in the activation of O2 and C–O/C–C bond cleavage was further confirmed by density functional theory calculation, which indicated that the Ru–N4 center exhibits strong adsorption toward both the O2 and β-O-4 linkages. This work provides a deep understanding on the active sites within Ru–N–C SACs for lignin oxidative cleavage and offers great potential on the rational design of next-generation SACs in biomass valorization.
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Feb 2026
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DIAD-Dual Imaging and Diffraction Beamline
I14-Hard X-ray Nanoprobe
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Abstract: High-resolution characterisation of biomaterials across multiple length scales to investigate their effect on (re)mineralisation can inform the development of effective interventions for clinical conditions such as dental caries, a disease with an estimated global economic burden of approximately $245 billion. This thesis presents a multi-modal, synchrotron-based approach on novel instruments to study the role of self-assembling peptide P11-4 in dental enamel (re)mineralisation, with the aim of elucidating its mechanism of action for potential optimisation to treat early caries lesions non-invasively, and to use P11-4 as a model system for the development of a liquid flow cell that can be used to characterise biomimetic materials in situ using synchrotron X-ray diffraction (XRD) and X-ray microtomography (XMT).
X-ray fluorescence combined with differential phase contrast imaging on the I14 beamline, together with XRD and XMT on the Dual Imaging and Diffraction beamline at Diamond Light Source, along with complementary laboratory-based techniques, were employed to characterise P11-4.
P11-4 accelerated the initial kinetics of the mineralisation process compared to the control, via the provision of calcium-binding sites, and controlled the mineral deposition process, mimicking the role of enamel matrix proteins during biomineralisation. The chemical model used for artificial demineralisation to create caries-like lesions resulted in preferential demineralisation of the enamel prisms. Within the caries-like lesions, the developed flow cell demonstrated that P11-4 promoted deep remineralisation of the lesion via the gradual formation of organised apatite structures within one specific population of crystallites, likely corresponding to the prisms. The organisation of crystallites within the regenerated structure is comparable to healthy enamel, highlighting its role in restoring the organised structure lost due to caries, and its significance as a non-invasive clinical treatment.
The methodology presented in this thesis can be applied to analyse lesions and characterise other biomaterials/proteins, and the flow cell is available to other users.
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Feb 2026
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I12-JEEP: Joint Engineering, Environmental and Processing
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Imogen
Cowley
,
Harry E.
Chapman
,
Sebastian
Marussi
,
Xianqiang
Fan
,
David
Rees
,
Tristan
Fleming
,
Yunhui
Chen
,
Alexander
Rack
,
Robert C.
Atwood
,
Martyn A.
Jones
,
Samuel J.
Clark
,
Chu Lun Alex
Leung
,
Peter D.
Lee
Diamond Proposal Number(s):
[28804]
Open Access
Abstract: In situ synchrotron studies of Directed Energy Deposition (DED) additive manufacturing provide unique process insights, using high-resolution spatial and temporal observations to reveal melt pool dynamics, phase evolution, and defect formation mechanisms. However, capturing these phenomena under industrially relevant conditions remains a challenge. Here, a second-generation DED apparatus is presented that replicates industrially relevant process conditions whilst enabling multi-modal in situ monitoring, including synchrotron X-ray radiography and diffraction, infrared (IR) imaging, inline coherent imaging (ICI), and optical imaging. The equipment, termed the Blown-powder Additive Manufacturing Process Replicator-II (BAMPR-II), also facilitates a range of unique process adaptations including the application of heat, magnetic fields, and ultrasound. Two case studies are described demonstrating how BAMPR-II reveals the underlying phenomena controlling DED, including: (1) simultaneous X-ray and ICI imaging to capture cracking mechanisms during DED; and (2) X-ray imaging of DED illustrating how magnetic fields can control flow in the melt pool.
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Feb 2026
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I11-High Resolution Powder Diffraction
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Ziqin
Jiao
,
Tao
Zeng
,
Wenhai
Ji
,
Zheng
Liu
,
Wenguang
Zhao
,
Xiaoyu
Gao
,
Yongbiao
Mu
,
Xuansi
Jiang
,
Yubin
Li
,
Guojie
Chen
,
Wenqing
Yao
,
Jinqi
Li
,
Ze
He
,
Juping
Xu
,
Ping
Miao
,
Wen
Yin
,
Yuguang
Pu
,
Rui
Wang
,
Yinguo
Xiao
Diamond Proposal Number(s):
[34243]
Abstract: Lattice-oxygen redox (L-OR) has been widely considered a viable approach to attain high-capacity cathodes for next-generation batteries. However, achieving highly reversible L - OR remains challenging due to the intrinsic chemical instability of lattice oxygen. As such, stabilizing the lattice oxygen becomes necessary for improving the performance of cathode materials with oxygen redox chemistry. In this study, the distinct properties of both bulk and surface lattice oxygen are systematically studied in a model Li-rich layered oxide material (LRMO, i.e., Li1.2Ni0.2Mn0.6O2) by employing different techniques. We find that, in the bulk, distortions in octahedral coordination geometry are closely correlated with variations in the electronic structure, and the substitution of Li ions with protons in a subsurface layer enhances the stability of surface lattice oxygen by altering its coordination environment. By jointly regulating the local environments of both bulk and surface lattice oxygen, the initial Coulombic efficiency is remarkably improved from 73.88% to 91.72%. Moreover, the modified LRMO demonstrates an impressive cycle stability, which realizes a capacity retention of 95.9% after 500 cycles at 250 mA g−1. This work demonstrates that rationally-designed local environments of lattice oxygen can effectively stabilize the oxygen redox in Li-rich cathodes.
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Feb 2026
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I10-Beamline for Advanced Dichroism - scattering
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Diamond Proposal Number(s):
[35696]
Open Access
Abstract: Cobalt ferrite nanoparticles are a benchmark among low-to-medium energy alternatives to rare-earth permanent magnets, although their intrinsic behavior is often obscured by surface disorder, finite-size effects, and superparamagnetic relaxation. Here, we overcome these limitations by synthesizing large, highly crystalline cobalt-doped ferrite nanoparticles (≈ 25 nm), which remain blocked at room temperature and thus provide a clean platform to disentangle the fundamental role of cobalt in the spinel lattice. By systematically varying the cobalt content, we reveal a complex interplay between cation distribution, oxygen vacancy formation, and magnetic response. Structural and compositional analysis confirms predominant Co2+ occupancy at octahedral sites, accompanied by a redistribution of Fe2+/Fe3+ and non-linear oxygen vacancy generation. We find that while saturation magnetization is largely governed by defect chemistry, the coercivity and effective anisotropy are primarily controlled by cobalt incorporation and saturate at intermediate compositions. In contrast, thermomagnetic analysis reveals an anomalous evolution of magnetization at intermediate temperatures for specific cobalt contents. This behavior is consistent with a change in the anisotropy landscape, suggestive of a growing contribution from higher-order anisotropy terms, rather than a simple uniform increase in magnetocrystalline anisotropy. These results indicate that cobalt doping tunes the balance between different anisotropy contributions in a composition- and temperature-dependent manner. Overall, our findings highlight the subtle interplay between cation distribution, anisotropy landscape, and thermal stability in spinel ferrites, providing fundamental insight for the design of high-coercivity rare-earth-free nanomagnets.
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Feb 2026
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