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16,292 items found (0 items not approved), displaying 71 to 80.[First/Prev] 4, 5, 6, 7, 8, 9, 10, 11 [Next/Last]

Instruments / Technical Area	Publication Details	Published
I20-Scanning-X-ray spectroscopy (XAS/XES)	3D atomic-scale imaging of mixed Co-Fe spinel oxide nanoparticles during oxygen evolution reaction Weikai Xiang , Nating Yang , Xiaopeng Li , Julia Linnemann , Ulrich Hagemann , Olaf Ruediger , Markus Heidelmann , Tobias Falk , Matteo Aramini , Serena Debeer , Martin Muhler , Kristina Tschulik , Tong Li Nature Communications 13 DOI: 10.1038/s41467-021-27788-2 Diamond Proposal Number(s): [25636] Open Access Show Abstract ▼ Abstract: The three-dimensional (3D) distribution of individual atoms on the surface of catalyst nanoparticles plays a vital role in their activity and stability. Optimising the performance of electrocatalysts requires atomic-scale information, but it is difficult to obtain. Here, we use atom probe tomography to elucidate the 3D structure of 10 nm sized Co2FeO4 and CoFe2O4 nanoparticles during oxygen evolution reaction (OER). We reveal nanoscale spinodal decomposition in pristine Co2FeO4. The interfaces of Co-rich and Fe-rich nanodomains of Co2FeO4 become trapping sites for hydroxyl groups, contributing to a higher OER activity compared to that of CoFe2O4. However, the activity of Co2FeO4 drops considerably due to concurrent irreversible transformation towards CoIVO2 and pronounced Fe dissolution. In contrast, there is negligible elemental redistribution for CoFe2O4 after OER, except for surface structural transformation towards (FeIII, CoIII)2O3. Overall, our study provides a unique 3D compositional distribution of mixed Co-Fe spinel oxides, which gives atomic-scale insights into active sites and the deactivation of electrocatalysts during OER.	Jan 2022
I11-High Resolution Powder Diffraction I19-Small Molecule Single Crystal Diffraction	3D cage COFs: A dynamic three-dimensional covalent organic framework with high-connectivity organic cage nodes Qiang Zhu , Xue Wang , Rob Clowes , Peng Cui , Linjiang Chen , Marc Little , Andrew I. Cooper Journal Of The American Chemical Society DOI: 10.1021/jacs.0c07732 Diamond Proposal Number(s): [21726, 23666] Open Access Show Abstract ▼ Abstract: Three-dimensional (3D) covalent organic frameworks (COFs) are rare because there is a limited choice of organic building blocks that offer multiple reactive sites in a polyhedral geometry. Here, we synthesized an organic cage molecule (cage-6-NH2), which was used as a triangular prism node to yield the first cage-based 3D COF, 3D-CageCOF-1. This COF adopts an unreported twofold interpenetrated acs topology and exhibits reversible dynamic behavior, switching between a small-pore (sp) structure and a large-pore (lp) structure. It also shows high CO2 uptake and captures water at low humidity (<40%). This demonstrates the potential for expanding the structural complexity of 3D COFs by using organic cages as the building units.	Sep 2020
I12-JEEP: Joint Engineering, Environmental and Processing	3D cellular automata finite element (CAFE) modelling and experimental observation of damage in quasi-brittle nuclear materials: Indentation of a SiC-SiC fibre ceramic matrix composite Luis Saucedo Mora , Mahmoud Mostafavi , Danial Khoshkhou , Christina Reinhard , Robert Atwood , Shuang Zhao , Brian Connolly , James Marrow OECD Nuclear Energy Agency International Workshop on Structural Materials for Innovative Nuclear Systems 2013 Diamond Proposal Number(s): [7730] Show Abstract ▼ Abstract: Cellular Automata integrated with Finite Elements (CAFE) have been used to develop a method to account for the effect of microstructure on quasi-brittle damage development. The microstructure is simulated explicitly by subdividing a finite element into smaller cells. A heterogeneous structure is created from key cells (seeds) using defined characteristics; the influence of the initial finite element mesh is effectively removed during the development of the microstructure. Graded microstructures, textures, particle anisotropy and multiple phases can be readily simulated, such as those in composites and porous materials. A mesh-free framework has been developed to compute the damage development through the microstructure, using cellular automata. With this method, we can study the development of discontinuous cracking and damage coalescence, and its sensitivity to microstructure. Experiments have been carried out to observe the three-dimensional development of damage, using high-resolution synchrotron X-ray computed tomography and digital volume correlation to observe Hertzian indentation of a SiC-SiC fibre composite, quantifying damage by measurement of the displacement fields within the material. The results demonstrate the applicability of the modelling strategy to damage development, and show how model input data may be obtained from small specimen tests, which could be performed at elevated temperatures with irradiated materials.	Oct 2013
	3D characterisation of the Fe-rich intermetallic phases in recycled Al alloys by synchrotron X-ray microtomography and skeletonisation Y. Zhao , W. Du , B. Koe , T. Connolley , S. Irvine , P. K. Allan , C. M. Schlepütz , W. Zhang , F. Wang , D. G. Eskin , J. Mi Scripta Materialia 146, 321 - 326 DOI: 10.1016/j.scriptamat.2017.12.010 Show Abstract ▼ Abstract: Synchrotron X-ray microtomography and skeletonisation method were used to study the true 3D network structures and morphologies of the Fe-rich intermetallic phases in recycled Al-5.0%Cu-0.6%Mn alloys with 0.5% and 1.0% Fe. It was found that, the Fe-phases in the 1.0%Fe alloy have node lengths of 5–25 μm; while those in the 0.5%Fe alloy are of 3–17 μm. The Fe-phases in the 1.0%Fe alloy also developed sharper mean curvature with wider distribution than those in the 0.5%Fe alloy. Combining SEM studies of the deeply-etched samples, the true 3D structures of 4 different type Fe phases in both alloys are also revealed and demonstrated.	Mar 2018
B24-Cryo Soft X-ray Tomography	3D correlative cryo-structured illumination fluorescence and soft X-ray microscopy elucidates reovirus intracellular release pathway Ilias Kounatidis , Megan L. Stanifer , Michael A. Phillips , Perrine Paul-Gilloteaux , Xavier Heiligenstein , Hongchang Wang , Chidinma Okolo , Thomas M. Fish , Matthew C. Spink , David I. Stuart , Ilan Davis , Steeveh Boulant , Jonathan M. Grimes , Ian M. Dobbie , Maria Harkiolaki Cell DOI: 10.1016/j.cell.2020.05.051 Diamond Proposal Number(s): [21046, 18314] Open Access Show Abstract ▼ Abstract: Imaging of biological matter across resolution scales entails the challenge of preserving the direct and unambiguous correlation of subject features from the macroscopic to the microscopic level. Here, we present a correlative imaging platform developed specifically for imaging cells in 3D under cryogenic conditions by using X-rays and visible light. Rapid cryo-preservation of biological specimens is the current gold standard in sample preparation for ultrastructural analysis in X-ray imaging. However, cryogenic fluorescence localization methods are, in their majority, diffraction-limited and fail to deliver matching resolution. We addressed this technological gap by developing an integrated, user-friendly platform for 3D correlative imaging of cells in vitreous ice by using super-resolution structured illumination microscopy in conjunction with soft X-ray tomography. The power of this approach is demonstrated by studying the process of reovirus release from intracellular vesicles during the early stages of infection and identifying intracellular virus-induced structures.	Jun 2020
I12-JEEP: Joint Engineering, Environmental and Processing	3D correlative imaging of lithium ion concentration in a vertically oriented electrode microstructure with a density gradient Chun Huang , Matthew Wilson , Kosuke Suzuki , Enzo Liotti , Thomas Connolley , Oxana Magdysyuk , Stephen Collins , Frederic Van Assche , Matthieu N Boone , Matthew C. Veale , Andrew Lui , Rhian-Mair Wheater , Chu Lun Alex Leung Advanced Science 92 DOI: 10.1002/advs.202105723 Diamond Proposal Number(s): [23400] Open Access Show Abstract ▼ Abstract: The performance of Li+ ion batteries (LIBs) is hindered by steep Li+ ion concentration gradients in the electrodes. Although thick electrodes (≥300 µm) have the potential for reducing the proportion of inactive components inside LIBs and increasing battery energy density, the Li+ ion concentration gradient problem is exacerbated. Most understanding of Li+ ion diffusion in the electrodes is based on computational modeling because of the low atomic number (Z) of Li. There are few experimental methods to visualize Li+ ion concentration distribution of the electrode within a battery of typical configurations, for example, coin cells with stainless steel casing. Here, for the first time, an interrupted in situ correlative imaging technique is developed, combining novel, full-field X-ray Compton scattering imaging with X-ray computed tomography that allows 3D pixel-by-pixel mapping of both Li+ stoichiometry and electrode microstructure of a LiNi0.8Mn0.1Co0.1O2 cathode to correlate the chemical and physical properties of the electrode inside a working coin cell battery. An electrode microstructure containing vertically oriented pore arrays and a density gradient is fabricated. It is shown how the designed electrode microstructure improves Li+ ion diffusivity, homogenizes Li+ ion concentration through the ultra-thick electrode (1 mm), and improves utilization of electrode active materials.	Apr 2022
I13-2-Diamond Manchester Imaging	3D cyclorama for digital unrolling and visualisation of deformed tubes Charalambos Rossides , Sylvia L. F. Pender , Philipp Schneider Scientific Reports 11 DOI: 10.1038/s41598-021-93184-x Diamond Proposal Number(s): [22588, 17241] Open Access Show Abstract ▼ Abstract: Colonic crypts are tubular glands that multiply through a symmetric branching process called crypt fission. During the early stages of colorectal cancer, the normal fission process is disturbed, leading to asymmetrical branching or budding. The challenging shapes of the budding crypts make it difficult to prepare paraffin sections for conventional histology, resulting in colonic cross sections with crypts that are only partially visible. To study crypt budding in situ and in three dimensions (3D), we employ X-ray micro-computed tomography to image intact colons, and a new method we developed (3D cyclorama) to digitally unroll them. Here, we present, verify and validate our ‘3D cyclorama’ method that digitally unrolls deformed tubes of non-uniform thickness. It employs principles from electrostatics to reform the tube into a series of onion-like surfaces, which are mapped onto planar panoramic views. This enables the study of features extending over several layers of the tube’s depth, demonstrated here by two case studies: (i) microvilli in the human placenta and (ii) 3D-printed adhesive films for drug delivery. Our 3D cyclorama method can provide novel insights into a wide spectrum of applications where digital unrolling or flattening is necessary, including long bones, teeth roots and ancient scrolls.	Jul 2021
B16-Test Beamline Detectors	3D detectors for synchrotron applications David Pennicard Open Access Show Abstract ▼ Abstract: 3D detectors are a novel variety of photodiode radiation detector, invented by Parker, Kenney and Segal (1997). Instead of having n- and p-type contacts on the front and back surfaces of a silicon substrate, like a standard photodiode, they have columns of doped material passing through the thickness of the silicon. This structure means that the detector can combine a reasonable substrate thickness with a very small electrode spacing, resulting in a low depletion voltage, fast charge collection and low charge sharing. These detectors have a couple of promising applications. Their fast charge collection and low depletion voltage should make them very radiation-tolerant. So, they could be used for future particle physics experiments at the Super Large Hadron Collider (SLHC), where high levels of radiation damage are expected. Also, their low charge sharing means they could potentially improve X-ray diffraction measurements at synchrotrons such as Diamond Light Source. This would allow these experiments, for example, to determine the structures of biological molecules more accurately. However, before 3D devices can be used in practical experiments, their design and fabrication must be optimised to ensure that reliable, high-performance detectors can be produced on a reasonably large scale. The aim of this thesis is to evaluate and understand the behaviour of a variety of 3D detectors using a combination of lab tests and computer simulations. Using these results, future fabrication runs can then be re-designed to improve their performance.	Apr 2009
Detectors	3D electron diffraction of small molecules on the MerlinEM detector Pedro Nunes , Matus Krajnak , Adriana L. Klyszejko , Alistair C. Siebert Microscopy and Microanalysis 2023 DOI: 10.1093/micmic/ozad067.511 Show Abstract ▼ Abstract: The MerlinEM/Medipix3 is a versatile detector widely used for scanned electron diffraction, precession, dynamic transmission electron microscopy (TEM) and scanning transmission electron microscopy (4D STEM). It can be used to image direct probes (up to 300kV) while still retaining the ability to count single electrons for the weaker diffraction spots [1]. It contains two 12-bit counters, enabling zero dead time acquisitions and noiseless readout. This makes MerlinEM an attractive solution for low-dose techniques in many areas of electron microscopy. We are particularly interested in the application of micro electron diffraction (3DED, microED) techniques for structure determination of small molecules of biological and pharmaceutical importance [2]. 3DED has been growing in popularity in recent years thanks to the development of more sensitive detectors and stable automated diffraction setups. Electron diffraction has the essential advantage over X-ray crystallography when crystal size is concerned. It produced multiple medium to high resolution structures from nano crystals and from artificially thinned (by focused ion beam milling) crystals [3, 4]. Furthermore, electrons have an advantage over X-rays as they interact orders of magnitude more strongly with samples. This allows hydrogen atoms to be located within the structure to gain insights into the chemical properties of small compounds. This is essential in chemical research, pharmaceutical drug discovery and other industries [5]. Furthermore, performing electron diffraction tomography on multiple crystals in an automated manner enables efficient collection of large datasets. For this reason, we worked closely with the team at Quantum Detectors. A recently available plugin for MerlinEM to the academic SerialEM software environment [6] has enabled low-dose 3DED data collections on the MerlinEM Quad 4S installed on the FEI Tecnai F30 cryo electron microscope at the Rosalind Franklin institute. We present data obtained on small compounds of pharmaceutical interest by HeXI at Diamond Light Source using 3DED with MerlinEM.	Aug 2023
I12-JEEP: Joint Engineering, Environmental and Processing I13-2-Diamond Manchester Imaging I18-Microfocus Spectroscopy	3D imaging advances with Python Diamond Light Source Show Abstract ▼ Abstract: Tomography users at Diamond are set to get a boost with new open-source software that makes 3D reconstruction quicker, easier, and more customisable than ever before. Automated processing steps will allow users to get higher-quality 3D reconstructions faster by reducing manual intervention, and make the most of their beamtime by optimising experimental techniques as they go. Novice and experienced users will now have the opportunity to customise how their data are processed by adding Python plugins to their processing pipeline. Analysis and correction of experimental problems will be possible shortly after each data collection with the application of specific modules. This rapid feedback loop has not previously been available in synchrotron-based X-ray tomography at Diamond. Aptly named ‘Savu’, after a python subspecies that is incredibly adaptable in terms of habitat, this new modular processing pipeline is open licenced, facility independent, able to operate on any standard cluster infrastructure, and freely available on Github in alpha release. The Savu system has been developed to drive the high-throughput of high-quality tomographic reconstructions, as detailed in a recent Philosophical Transactions A publication.	Sep 2015

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