B16-Test Beamline
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Diamond Proposal Number(s):
[28395]
Open Access
Abstract: Carbon fibre composites are widely used in low specific stiffness and high strength structures such as airframes. Compressive loading of these assemblies can lead to buckling and localised deformation around defects and imperfections that can hinder performance and lead to overengineering via excessive safety factors. Synchrotron X-Ray Diffraction (SXRD) has recently been shown to be capable of performing lattice strain mapping within carbon fibre composites at the microscale, a previously unprecedented resolution. In this study SXRD and radiography was performed on carbon fibre composite columns produced via two different methods (standard lamination and half square) at a range of different load states: unbuckled, one-third of the buckling load and post buckling. The results provide quantitative insights into the impact of these different production methods on lattice strain and fibre orientation, as well as the influence these factors have on reducing buckling load (by up to 22%). As well as being the first use of SXRD on industrially representative full-size carbon fibre samples, these insights provide invaluable detail into the factors which limit performance and the origins of column failure; crucial factors required to optimise structural design, production and loading capability.
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Nov 2023
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Sarlota
Birnsteinova
,
Danilo E.
Ferreira De Lima
,
Egor
Sobolev
,
Henry J.
Kirkwood
,
Valerio
Bellucci
,
Richard J.
Bean
,
Chan
Kim
,
Jayanath C. P.
Koliyadu
,
Tokushi
Sato
,
Fabio
Dall'Antonia
,
Eleni Myrto
Asimakopoulou
,
Zisheng
Yao
,
Khachiwan
Buakor
,
Yuhe
Zhang
,
Alke
Meents
,
Henry N.
Chapman
,
Adrian P.
Mancuso
,
Pablo
Villanueva-Perez
,
Patrik
Vagovic
Open Access
Abstract: The high pulse intensity and repetition rate of the European X-ray Free-Electron Laser (EuXFEL) provide superior temporal resolution compared with other X-ray sources. In combination with MHz X-ray microscopy techniques, it offers a unique opportunity to achieve superior contrast and spatial resolution in applications demanding high temporal resolution. In both live visualization and offline data analysis for microscopy experiments, baseline normalization is essential for further processing steps such as phase retrieval and modal decomposition. In addition, access to normalized projections during data acquisition can play an important role in decision-making and improve the quality of the data. However, the stochastic nature of X-ray free-electron laser sources hinders the use of standard flat-field normalization methods during MHz X-ray microscopy experiments. Here, an online (i.e. near real-time) dynamic flat-field correction method based on principal component analysis of dynamically evolving flat-field images is presented. The method is used for the normalization of individual X-ray projections and has been implemented as a near real-time analysis tool at the Single Particles, Clusters, and Biomolecules and Serial Femtosecond Crystallography (SPB/SFX) instrument of EuXFEL.
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Nov 2023
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I24-Microfocus Macromolecular Crystallography
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James
Birch
,
Tristan O. C.
Kwan
,
Peter J.
Judge
,
Danny
Axford
,
Pierre
Aller
,
Agata
Butryn
,
Rosana
Reis
,
Juan F.
Bada Juarez
,
Javier
Vinals
,
Robin L.
Owen
,
Eriko
Nango
,
Rie
Tanaka
,
Kensuke
Tono
,
Yasumasa
Joti
,
Tomoyuki
Tanaka
,
Shigeki
Owada
,
Michihiro
Sugahara
,
So
Iwata
,
Allen M.
Orville
,
Anthony
Watts
,
Isabel
Moraes
Diamond Proposal Number(s):
[19152]
Open Access
Abstract: Serial crystallography has emerged as an important tool for structural studies of integral membrane proteins. The ability to collect data from micrometre-sized weakly diffracting crystals at room temperature with minimal radiation damage has opened many new opportunities in time-resolved studies and drug discovery. However, the production of integral membrane protein microcrystals in lipidic cubic phase at the desired crystal density and quantity is challenging. This paper introduces VIALS (versatile approach to high-density microcrystals in lipidic cubic phase for serial crystallography), a simple, fast and efficient method for preparing hundreds of microlitres of high-density microcrystals suitable for serial X-ray diffraction experiments at both synchrotron and free-electron laser sources. The method is also of great benefit for rational structure-based drug design as it facilitates in situ crystal soaking and rapid determination of many co-crystal structures. Using the VIALS approach, room-temperature structures are reported of (i) the archaerhodopsin-3 protein in its dark-adapted state and 110 ns photocycle intermediate, determined to 2.2 and 1.7 Å, respectively, and (ii) the human A2A adenosine receptor in complex with two different ligands determined to a resolution of 3.5 Å.
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Oct 2023
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DIAD-Dual Imaging and Diffraction Beamline
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Abstract: Purpose / Aim: Dentine hypersensitivity (DH) is a commonly occurring dental condition where sharp pain derived from exposed dentine in response to stimuli that cannot be ascribed to any other dental diseases. It is highly prevalent affecting up to 69% of the UK population and has a significant impact on the quality of life. Bioactive glasses that degrade in oral environment and form apatite are thought to be beneficial in occluding the exposed open dentine tubules and have been introduced to toothpastes, e.g. Novamin® (45S5 Bioglass) for Sensodyne by GSK, fluoride containing bioactive glass for BioMin® F by BioMin Technologies Ltd. Post-mortem characterisations evidenced tubule occlusion (Fig.1) but failed in providing dynamic history. Therefore, this study aimed to monitor dentine tubule occlusion with bioactive glasses using an operando time-lapse X-ray diffraction tomography experiment. Materials & Methods: Disinfected Teeth (collected under REC reference 16/SW/0220) were sectioned mesio-distally into discs approximately 500 μm thick using a precision diamond saw, polished down to 300 μm manually. Matchstick specimens (5 mm length x 3 mm width) prepared were brushed for 2 mins with bioactive glasses pastes, housed in a modified Eppendorf tube and positioned on the tomography stage of the Dual Imaging and Diffraction (DIAD) beamline at Diamond Light Source (UK’s national synchrotron). A baseline X-ray tomography (pink beam, 0-180°, detector exposure of 0.01 and 5,000 projections) and X-ray diffraction mapping (matrix scan with 10x10 points, 20 s exposure) were collected before artificial saliva was introduced. Time-lapse X-ray tomography and X-ray diffraction mapping using the same parameters as baseline scan were carried out consecutively for 8 h allowing the visualisation of tubule occlusion and changes of mineral density as well as monitor the phase evolution from glass to apatite. Artificial saliva was manually replenished. Monochromatic beam with an energy of 20 keV was used and calibrations were performed. Results: The collected tomography data allow visualisation of dentine tubule occlusion showing improved occlusion with time. 2D XRD data provide qualitative and quantitative information relates to glass dissolution and apatite formation as a function of time. Conclusions: The Dual Imaging and Diffraction (DIAD) beamline correlates X-ray tomography and X-ray diffraction mapping offers the opportunity to study dentine occlusion by bioactive glasses in a time evolving manner that is not available via other techniques. Although in vitro but clinically relevant. The results will potentially provide a guidance for optimising and designing products for dentine tubule occlusion/treating dentine hypersensitivity – one of the most prevalent global diseases with healthy ageing.
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Oct 2023
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B18-Core EXAFS
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Diamond Proposal Number(s):
[24523]
Abstract: Aggregation modulates the photochemical and photophysical properties of methylene blue (MB+). MB+ adsorbed by the anionic polymer Chelex® 100 was characterized by UV–visible absorption spectroscopy and sulfur K-edge X-ray absorption near edge structure (XANES) as H- and J-aggregates. Nuclear magnetic resonance (NMR) indicates that dye molecules bind to the unprotonated carboxylic groups of the polymer via electrostatic interactions and are bridged by water molecules. MB+ also stacks with phenyl rings appended in the Chelex® 100 chain, leading to a gain in the mobility of ordered water displaced around the aromatic rings. Like the blue bottle experiment, MB+ in Chelex® 100 was entirely photoconverted for the leuco form (LMB) by visible and red light and reoxidized by molecular oxygen. Electron paramagnetic resonance (EPR) of MB+ in Chelex® 100 demonstrated the formation of a sulfur-centered free radical during photobleaching. The free radical involvement in MB+ photobleaching is consistent with a type I mechanism in which the stabilization of the products MB2+• and MB• in dye aggregates allows the formation of LMB by MB• dismutation or a second electron abstraction. Chelex® 100 beds loaded with MB+ solutions prepared in H2O and D2O produce H2O2 and D2O2, respectively, after successive cycles of photobleaching and recycling by O2 dissolved in the liquid phase. The formation of hydrogen peroxide is attributed to spontaneous superoxide ion disproportionation in the microenvironment of the polymer lattice. The LMB produced in Chelex® 100 was also able to act as a reducing agent for the synthesis of anisotropic iridescent gold nanoparticles (GNPs). The LMB/Chelex system allows the modulation of the shape and size of GNPs using different dye/Au3+ ratios. GNPs produced using LMB as a reducing agent are also efficient cell delivery systems. The specific properties of LMB confined in solid hosts LMB/Chelex also have potential applications in new solid-state optoelectronic devices such as sensing and imaging.
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Oct 2023
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I22-Small angle scattering & Diffraction
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Abstract: In situations where the stereoregularity of the polymer chains permits, crystals can form in synthetic or natural polymers. These crystals have an immense impact on the properties of the polymeric material. Typically polymers crystallized from a quiescent melt form spherulites, but where the melt exhibits a level of anisotropy, the crystalline morphology, is quite different to the spherulitic structure, although it may well contain chain-folded lamellar crystals. We consider a number of different systems in which the anisotropy has developed in different ways. Despite these differences, there are strong features in common within the semi-crystalline polymer morphology. We consider the strain-induced crystallization in deformed natural rubber, in sheared melts containing both self-assembling nanoparticles and engineered nanoparticles, and during extrusion as part of fused granular deposition-based 3D printing.
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Oct 2023
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I05-ARPES
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Kevin P.
Kramer
,
Rina
Tazai
,
Karin
Von Arx
,
Masafumi
Horio
,
Julia
Küspert
,
Qisi
Wang
,
Yasmine
Sassa
,
Timur K.
Kim
,
Cephise
Cacho
,
Julien E.
Rault
,
Patrick
Le Fèvre
,
François
Bertran
,
Marc
Janoschek
,
Nicolas
Gauthier
,
Daniel
Mazzone
,
Ramzy
Daou
,
Johan
Chang
Open Access
Abstract: We present a resonant angle-resolved photoemission spectroscopy (ARPES) study of the electronic band structure and heavy fermion quasiparticles in CeRu2Si2. Using light polarization analysis, considerations of the crystal field environment and hybridization between conduction and f electronic states, we identify the d-electronic orbital character of conduction bands crossing the Fermi level. Resonant ARPES spectra suggest that the localized Ce f states hybridize with eg and t2g states around the zone center. In this fashion, we reveal the orbital structure of the heavy fermion quasiparticles in CeRu2Si2 and discuss its implications for metamagnetism and superconductivity in the related compound CeCu2Si2.
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Oct 2023
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I07-Surface & interface diffraction
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Diamond Proposal Number(s):
[25808]
Abstract: Among the functional materials suitable for the realization of solar cells and light emission diodes (LEDs), perovskites, especially fully inorganic perovskites, are considered among the most promising. CsPbBr3 is the most studied due to its favorable band gap value and stability under mild atmospheric conditions: moisture and UV visible radiation exposure. Using this material, highly efficient thin film solar cells have been produced at the lab scale, and researchers aim to scale the process up to the industrial level. Here, ultrathin films of CsPbBr3 were obtained by magnetron sputtering, and the texture and morphology of the deposited films were evaluated as a function of their thickness and the substrate's nature. The obtained films are composed of highly textured structures of submicrometric crystals homogeneously distributed all over the surface. Finally, the texture decreases as the deposit thickness increases.
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Oct 2023
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B21-High Throughput SAXS
I04-Macromolecular Crystallography
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Abstract: Septins are membrane-associated, GTP-binding proteins that are present in most eukaryotes. They polymerize to play important roles as scaffolds and/or diffusion barriers as part of the cytoskeleton. α-Helical coiled-coil domains are believed to contribute to septin assembly, and those observed in both human SEPT6 and SEPT8 form antiparallel homodimers. These are not compatible with their parallel heterodimeric organization expected from the current model for protofilament assembly, but they could explain the interfilament cross-bridges observed by microscopy. Here, the first structure of a heterodimeric septin coiled coil is presented, that between SEPT14 and SEPT7; the former is a SEPT6/SEPT8 homolog. This new structure is parallel, with two long helices that are axially shifted by a full helical turn with reference to their sequence alignment. The structure also has unusual knobs-into-holes packing of side chains. Both standard seven-residue (heptad) and the less common 11-residue (hendecad) repeats are present, creating two distinct regions with opposite supercoiling, which gives rise to an overall straight coiled coil. Part of the hendecad region is required for heterodimerization and therefore may be crucial for selective septin recognition. These unconventional sequences and structural features produce a metastable heterocomplex that nonetheless has enough specificity to promote correct protofilament assembly. For instance, the lack of supercoiling may facilitate unzipping and transitioning to the antiparallel homodimeric state.
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Oct 2023
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I24-Microfocus Macromolecular Crystallography
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Open Access
Abstract: The aTfaRel2/faRel2 operon from Coprobacillus sp. D7 encodes a bicistronic type II toxin–antitoxin (TA) module. The FaRel2 toxin is a toxic small alarmone synthetase (toxSAS) that inhibits translation through the pyrophosphorylation of uncharged tRNAs at the 3′-CCA end. The toxin is neutralized by the antitoxin ATfaRel2 through the formation of an inactive TA complex. Here, the production, biophysical analysis and crystallization of ATfaRel2 and FaRel2 as well as of the ATfaRel2–FaRel2 complex are reported. ATfaRel2 is monomeric in solution. The antitoxin crystallized in space group P21212 with unit-cell parameters a = 53.3, b = 34.2, c = 37.6 Å, and the best crystal diffracted to a resolution of 1.24 Å. Crystals of FaRel2 in complex with APCPP, a nonhydrolysable ATP analogue, belonged to space group P21, with unit-cell parameters a = 31.5, b = 60.6, c = 177.2 Å, β = 90.6°, and diffracted to 2.6 Å resolution. The ATfaRel2–FaRel2Y128F complex forms a heterotetramer in solution composed of two toxins and two antitoxins. This complex crystallized in two space groups: F4132, with unit-cell parameters a = b = c = 227.1 Å, and P212121, with unit-cell parameters a = 51.7, b = 106.2, c = 135.1 Å. The crystals diffracted to 1.98 and 2.1 Å resolution, respectively.
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Oct 2023
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