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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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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I04-Macromolecular Crystallography
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Rachel L.
Palte
,
Mihir
Mandal
,
Justyna
Sikorska
,
Artjohn B.
Villafania
,
Meredith M.
Rickard
,
Robert J.
Bauer
,
Alexei V.
Buevich
,
Xiaomei
Chai
,
Jiafang
He
,
Zahid
Hussain
,
Markus
Koglin
,
Hannah B.
Macdonald
,
My S.
Mansueto
,
Klaus
Maskos
,
Joey L.
Methot
,
Jaclyn
Robustelli
,
Aileen
Soriano
,
Marcel J.
Tauchert
,
Sriram
Tyagarajan
,
Minjia
Zhang
,
Daniel J.
Klein
,
Jacqueline D.
Hicks
,
David G.
Mclaren
,
Sandra B.
Gabelli
,
Daniel F.
Wyss
Diamond Proposal Number(s):
[35460]
Open Access
Abstract: WRN helicase is an established synthetic lethal target for inhibition in the treatment of microsatellite instability-high (MSI-H) and mismatch repair deficient (MMRd) cancers. The identification of helicase inhibitors is challenging as high-throughput biochemical screening campaigns typically return few validated hits that are often inactive in cell-based assays. Herein, we highlight the power of non-covalent fragment-based lead discovery in locating new druggable allosteric sites on WRN, enabling us to bypass the challenging behavior of WRN during high-throughput screening hampering hit identification. During the fragment optimization process, structures of WRN with key prioritized fragments reveal multiple conformations of WRN with significant domain rotations up to 180°, including a WRN conformation not previously described. Rooted in a combination of biochemical, biophysical, and structural approaches, we present the detailed analyses of optimized chemical matter evolved from screening hits and the unique ability of WRN to accommodate diverse conformations as detailed by structural characterization.
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Jan 2026
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I12-JEEP: Joint Engineering, Environmental and Processing
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Da
Guo
,
Chengbo
Zhu
,
Harry E.
Chapman
,
Kai
Zhang
,
Wei
Li
,
Shishira
Bhagavath
,
Robert
Atwood
,
Stefan
Michalik
,
Dmitry G.
Eskin
,
Iakovos
Tzanakis
,
Chu Lun Alex
Leung
,
Peter D.
Lee
Diamond Proposal Number(s):
[34549]
Open Access
Abstract: Directed energy deposition (DED) additive manufacturing (AM) can fabricate, repair, and join near-net-shaped components for high-performance engineering applications, including biomedical, energy, and transport sectors. The broader adoption of DED remains constrained by the limited number of alloys available that can be reliably manufactured without imperfections, hence limiting mechanical properties. Here, we designed an Al-Ni-Ce-Mn-Fe AM alloy that can achieve an ultra-fine microstructure (<5 μm), uniform distribution of intermetallics, low residual stress (<32 MPa), and superior mechanical properties in as-built DED components. Compared to DED AlSi10Mg in the as-build state using the same conditions, the yield increased by 70%, and the ultimate tensile strength by 50%. DED-AM involves rapid cooling and complex thermal conditions, which largely influence the property of the final components. Post-characterization cannot capture the time resolved thermal behavior, hence offer limited mechanism-based guide for alloy design. In this study, we develop a novel multimodal characterization methodology for correlative in situ X-ray imaging, X-ray diffraction, and infrared imaging, enabling quantification of the in situ thermal-related behavior, including phase evolution, temperature distribution and stress accumulation during DED. We elucidated key mechanisms driving the structure refinement and stress development in this alloy. The insights gained into the interplay between alloy composition, thermal-related behavior, and performance under specific AM conditions informs next-generation material design tailored for AM technologies.
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Jan 2026
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E01-JEM ARM 200CF
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Naomi
Lawes
,
Igor
Kowalec
,
Sofia
Mediavilla-Madrigal
,
Kieran J.
Aggett
,
Louise R.
Smith
,
Malcolm
Dearg
,
Thomas J. A.
Slater
,
Eimear
Mccarthy
,
Herzain I.
Rivera-Arrieta
,
Matthias
Scheffler
,
David J.
Morgan
,
David J.
Willock
,
Andrew M.
Beale
,
Andrew J.
Logsdail
,
Nicholas F.
Dummer
,
Michael
Bowker
,
C. Richard A.
Catlow
,
Stuart H.
Taylor
,
Graham J.
Hutchings
Diamond Proposal Number(s):
[3104]
Open Access
Abstract: A series of PdZn/TiO2 catalysts prepared by chemical vapor impregnation (CVI) were tested for CO2 hydrogenation at 20 bar pressure and at temperatures of 230–270 °C. Changing the Pd and Zn molar ratio (Zn:Pd = 0–20) in a PdZn/TiO2 catalyst has a dramatic effect on selectivity for the CO2 hydrogenation reaction. Pd alone shows three main products: methanol, CO, and methane. Addition of small quantities of Zn results in the formation of a PdZn alloy, preventing methanation. At equimolar ratios of Pd and Zn, a 1:1 β-PdZn alloy is formed and a reverse water gas shift catalyst is produced. Adding Zn in excess relative to the Pd loading results in the formation of ZnO on the TiO2 surface in addition to the PdZn alloy, dramatically increasing methanol selectivity from 5% at Zn:Pd = 1 to 55% for Zn:Pd = 2. Through a combination of theory and experiment, the active site for methanol synthesis is concluded to be the interface between PdZn nanoparticles and the ZnO overlayer on the TiO2, where interfacial formate can react with hydrogen dissociated by the metal nanoparticle.
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Jan 2026
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[33261]
Open Access
Abstract: Lithium metal (LM) and zero-excess lithium (ZE) anodes offer pathways to increase the energy density of all-solid-state batteries (ASSBs). We employ operando X-ray computed tomography combined with an image subtraction method to visualize lithium plating/stripping morphology, stack mechanical failure, and quantify the lithium reversibility in asymmetric Li6PS5Cl (LPSC)-based ASSBs. Lithium metal counter electrode (CE) and copper (Cu) working electrode (WE) emulate LM and ZE interface configurations, respectively. We compare bare Cu and silver-coated Cu (Ag/Cu) WEs under varying current densities. At 0.25 mA cm−2(WE), bare Cu shows edge-localized and non-uniform lithium deposition, while Ag/Cu facilitates more uniform lithium spreading, but results in higher first-cycle irreversibility and lower Coulombic efficiency. Above 0.5 mA cm−2(WE), failure in Li|LPSC|Cu cells initiate at the LPSC|Cu interface via spallation cracks. In contrast, Ag preserves interface integrity at the WE despite lithium initially plates at discrete nucleation spots. However, failure shifts to the Li|LPSC interface, where non-uniform lithium depletion at the CE exposes the underlying Cu, leading to spallation cracks upon subsequent plating. Mechanical finite element simulations support these observations and underscore the critical role of the nucleation layers in mitigating mechanical failure. This study highlights interface engineering as a key strategy to address electro-chemo-mechanical degradation in LM- and ZE-ASSBs.
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Jan 2026
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Krios I-Titan Krios I at Diamond
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Diamond Proposal Number(s):
[38262]
Open Access
Abstract: Pseudomonas putida is a plant-beneficial rhizobacterium that encodes multiple type-VI secretion systems (T6SS) to outcompete phytopathogens in the rhizosphere. Among its antibacterial effectors, Tke5 (a member of the BTH_I2691 protein family) is a potent pore-forming toxin that disrupts ion homeostasis without causing considerable membrane damage. Tke5 harbours an N-terminal MIX domain, which is required for T6SS-dependent secretion in other systems. Many MIX domain-containing effectors require T6SS adaptor proteins (Tap) for secretion, but their molecular mechanisms of adaptor-effector binding remain elusive. Here, we report the 2.8 Å cryo-EM structure of the Tap3-Tke5 complex of P. putida strain KT2440, providing structural and functional insights into how effector Tke5 is recruited by its cognate adaptor protein Tap3. Functional dissection shows that the α-helical region of Tke5 is sufficient to kill intoxicated bacteria, while its β-rich region likely contributes to target membrane specificity. These findings delineate a mechanism of BTH_I2691 proteins for Tap recruitment and toxin activity, contributing to our understanding of a widespread yet understudied toxin family.
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Jan 2026
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I22-Small angle scattering & Diffraction
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Diamond Proposal Number(s):
[33542]
Open Access
Abstract: Artificial cells assembled from materials such as hydrogels have emerged as platforms to replicate and understand biological functionalities, processes, and behaviors. However, hydrogels lack a lipid membrane, a vital property of cellular systems. Here we develop a process for the assembly of a fluid and stable lipid membrane which coats the hydrogel mesh network within the particle, through electostatically-mediated fusion of nanoscale lipid vesicles. This confers cell-mimetic and biotechnologically relevant properties upon microscale, cell sized, hydrogel artificial cells generated through microfluidics. We exploit the properties of the created membrane to augment existing hydrogel properties through permeability alteration and protection of the hydrogel from small molecule degraders. Furthermore, we show that the lipid membrane is compatible with organelle substructures within the hydrogels, which enables the exploitation of an enhanced material design space to build hydrogel artificial cells that increasingly mimic the organization of cells. This platform paves the way for producing next generation artificial cells and functional microdevices from interfaced hydrogel-lipid materials. Our technologies may underpin new opportunities for integrating membranes into hydrogel-based systems, inlcuding for drug delivery and tissue engineering.
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Jan 2026
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Optics
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Arindam
Majhi
,
Wadwan
Singhapong
,
Wai Jue
Tan
,
Andrey
Sokolov
,
Stefano
Agrestini
,
Mirian
Garcia-Fernandez
,
Ke-Jin
Zhou
,
Andrew C.
Walters
,
Chris
Bowen
,
Alexander J. G.
Lunt
,
Hongchang
Wang
,
Kawal J.
Sawhney
Open Access
Abstract: Laterally graded multilayer optics play an important role in advanced X-ray applications, enabling precise control of beam properties for spectroscopic and focusing techniques. The Multilayer Deposition System (MDS) at Diamond Light Source (DLS) has demonstrated its ability to fabricate highly precise laterally graded X-ray optics. Developing such optics is challenging due to stringent requirements for precise lateral thickness variations and sagittal uniformity, achieved through optimized substrate speed profiles and advanced mask design. This study presents a comprehensive investigation into the design, fabrication, and characterization of laterally graded multilayers. An adjustable mask design improves sagittal uniformity and reduces optimization times. The structural and optical performance of the multilayers is evaluated, confirming their suitability for synchrotron applications. Two types of laterally graded multilayers were developed: one with a constant lateral gradient (0.005 nm/mm) for O-K edge polarizers, achieving sagittal thickness variations of approximately 0.3–0.4% across an 80 mm substrate, and another featuring a strong variable gradient from 0.037 to 0.112 nm/mm, designed to match the elliptical periodicity profile. The constant gradient multilayer polarizer has been successfully implemented on the state-of-the-art I21 beamline at DLS, highlighting the MDS's role in producing next-generation X-ray optics that meet the stringent demands of synchrotron beamlines.
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Jan 2026
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