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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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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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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I24-Microfocus Macromolecular Crystallography
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Open Access
Abstract: Serial synchrotron crystallography (SSX) enables structure determination from microcrystals under near-physiological, room-temperature conditions but is limited in part due to the inevitable onset of radiation damage. The ability to reduce the absorbed dose while retaining, or even improving, data quality is an attractive means of mitigating this limitation. Advances in detector technology have made the use of high-energy X-rays a routine approach in MX, improving diffraction efficiency and enhancing overall data quality. Here, we systematically evaluate low-dose SSX data collected at five different X-ray energies from 12.4 to 25 keV using a CdTe Eiger2 detector while maintaining a constant dose. Higher photon energies increased the mean diffracted intensity and signal-to-noise ratio per unit dose, and facilitated higher-resolution structure determination, even with limited crystal numbers. These findings highlight the advantages of high-energy X-rays and provide practical guidance for optimizing SSX experiments in probing protein dynamics.
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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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B21-High Throughput SAXS
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Diamond Proposal Number(s):
[29895]
Open Access
Abstract: A lipopeptide is designed that contains an epitope from simian virus T-antigen (SV40T, PKKKRKV) conjugated to an N-terminal palmitoyl (C16-) moiety, with the aim to act as an effective cell-penetrating lipopeptide, with additional aggregation propensity conferred by the lipid chain. A combination of cryo-TEM and small-angle X-ray scattering (SAXS) is used to show that the lipopeptide forms micelles, but mixtures with DNA lead to formation of fractal cluster-like co-assemblies due to intercalation of the DNA and peptide. Spectroscopic studies using fluorescence and circular dichroism (along with fiber X-ray diffraction) show that the peptide interacts with DNA and inserts into the groove. Confocal microscopy along with flow cytometry confirms delivery of DNA into both HeLa and mouse embryonic stem cells (mESCs) in pluripotent state, and the system shows excellent cytocompatibility as confirmed by MTT assays. Our data indicate that the lipopeptide may outperform the DNA transfection agent lipofectamine in DNA delivery into these stem cells and it enables DNA delivery into the cytoplasm and nucleus.
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Mar 2026
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Open Access
Abstract: Serial crystallography relies on the reproducible production of high-density suspensions of microcrystals, yet sample optimization remains a resource-intensive bottleneck. While phase diagrams provide a theoretical framework for controlling crystal size and number, experimental mapping is traditionally hindered by relatively high sample consumption. We present an automated microbatch-under-oil crystallization approach that rapidly maps phase boundaries using only 15–60 µl (∼0.15–3.8 mg) of protein. While this workflow is ideally suited for refining existing hits, it serves as a standalone platform for characterizing the crystallization landscape of new protein targets. The power of this approach lies in the integration of three distinct strategies that exploit the stable chemical environment of microbatch-under-oil. Firstly, we utilize an ingenious diagonal sampling strategy that traverses the phase boundary parallel to the solubility curve by systematically varying protein-to-precipitant ratios, identifying primary nucleation zones with far greater efficiency than traditional orthogonal grids. Secondly, we employ a linked variation of multiple precipitants to reveal morphology-specific regions, such as the rod versus plate transitions crucial for time-resolved experiments. Finally, we incorporate automated seed-stock titration to precisely define the metastable zone, enabling the predictive rescue of nucleation-limited systems. The synergy of these three strategies enables the systematic decoupling of nucleation from growth, providing a rational route to optimize microcrystal density, size and lattice order. Crucially, by eliminating the evaporation-related variables inherent in vapor diffusion, this method ensures that the chemical coordinates identified during screening remain constant during scale-up to larger volumes. This workflow transforms empirical serial crystallography sample preparation into a rational, reproducible and highly efficient process applicable to both the optimization of known conditions and the de novo development of microcrystal suspensions, tailored to the rigorous demands of modern serial diffraction experiments.
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Mar 2026
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VMXi-Versatile Macromolecular Crystallography in situ
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Diamond Proposal Number(s):
[28534, 34263]
Open Access
Abstract: Schistosoma mansoni cathepsin D1 (SmCD1) has been shown to be an essential enzyme for helminth metabolism due to its role in haemoglobin degradation: a key amino-acid source for the developing parasite. Therefore, the enzyme is a potential target for the development of antischistosomal inhibitors. SmCD1 has significant sequence identity to cathepsin D-like proteases found in other schistosome species and homology to mammalian aspartic proteases. Here, we report the first crystal structures of a helminth cathepsin D, SmCD1, and have identified a single-domain antibody (nanobody) that specifically binds to SmCD1 with nanomolar affinity but does not recognize human cathepsin D. We have mapped the epitope of the nanobody by determining the crystal structure of the enzyme–nanobody complex, revealing the conformation of SmCD1 in the propeptide-bound state.
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Feb 2026
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Alessia
Pepe
,
Ronald
Rios-Santacruz
,
Sara
Schianchi
,
Jovana
Vitas
,
Elena
Andreeva
,
Jacques-Philippe
Colletier
,
Nicolas
Coquelle
,
Elke
De Zitter
,
Shibom
Basu
,
Daniele
De Sanctis
,
Julien
Orlans
,
Ninon
Zala
,
Kyprianos
Hadjidemetriou
,
Kensuke
Tono
,
Takehiko
Tosha
,
Bruce
Doak
,
Robert
Shoeman
,
Martin
Weik
,
Paolo
Mariani
,
Giorgio
Schirò
Abstract: Serial X-ray crystallography is the method of choice for protein structural studies at X-ray free-electron lasers and is increasingly widely used at third- and fourth-generation synchrotron facilities. Sample delivery is a critical step in serial crystallography experiments, and the definition and control of delivery methods is especially important for time-resolved studies. Extruding protein crystals embedded in viscous matrices as a thin, stable jet is a delivery method that ensures low sample consumption. However, it requires specific characteristics, such as a constant speed, chemical compatibility and, for laser-triggered dynamic studies, optical transparency. Here, we present a new transparent carrier matrix for protein serial crystallography, based on a guanosine hydrogel. Crystal stability in the hydrogel, in terms of morphology, size and diffraction quality, along with optical properties, injection characteristics and X-ray background were tested at the ESRF synchrotron and compared with other commonly used matrices. Additionally, we present a high-quality serial femtosecond crystallography dataset collected at the Spring-8 Angstrom Compact Free-Electron Laser (Japan) using hen egg-white lysozyme microcrystals embedded in the hydrogel. The results establish that this new injection matrix is a suitable alternative to existing carriers. The main advantage is its stability, so that the composition of the aqueous phase inside the hydrogel can be easily modified and adapted to the crystallization conditions of the embedded crystals.
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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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