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17 items found (0 items not approved), displaying 1 to 10.[First/Prev] 1, 2 [Next/Last]

Instruments / Technical Area	Publication Details	Published
I22-Small angle scattering & Diffraction	High resolution membrane structures within hybrid lipid-polymer vesicles revealed by combining X-ray scattering and electron microscopy Rashmi Seneviratne , Georgina Coates , Zexi Xu , Caitlin E. Cornell , Rebecca F. Thompson , Amin Sadeghpour , Daniel P. Maskell , Lars J. C. Jeuken , Michael Rappolt , Paul A. Beales Small 1863 DOI: 10.1002/smll.202206267 Diamond Proposal Number(s): [19127, 18027] Open Access Show Abstract ▼ Abstract: Hybrid vesicles consisting of phospholipids and block-copolymers are increasingly finding applications in science and technology. Herein, small angle X-ray scattering (SAXS) and cryo-electron tomography (cryo-ET) are used to obtain detailed structural information about hybrid vesicles with different ratios of 1-palmitoyl-2-oleoyl-sn-glycero-3-phosphocholine (POPC) and poly(1,2-butadiene-block-ethylene oxide) (PBd22-PEO14, Ms = 1800 g mol−1). Using single particle analysis (SPA) the authors are able to further interpret the information gained from SAXS and cryo-ET experiments, showing that increasing PBd22-PEO14 mole fraction increases the membrane thickness from 52 Å for a pure lipid system to 97 Å for pure PBd22-PEO14 vesicles. Two vesicle populations with different membrane thicknesses in hybrid vesicle samples are found. As these lipids and polymers are reported to homogeneously mix, bistability is inferred between weak and strong interdigitation regimes of PBd22-PEO14 within the hybrid membranes. It is hypothesized that membranes of intermediate structure are not energetically favorable. Therefore, each vesicle exists in one of these two membrane structures, which are assumed to have comparable free energies. The authors conclude that, by combining biophysical methods, accurate determination of the influence of composition on the structural properties of hybrid membranes is achieved, revealing that two distinct membranes structures can coexist in homogeneously mixed lipid-polymer hybrid vesicles.	Mar 2023
I10-Beamline for Advanced Dichroism	Probing the local electronic structure in metal halide perovskites through cobalt substitution Amir A. Haghighirad , Matthew T. Klug , L. B. Duffy , Junjie Liu , Arzhang Ardavan , Gerrit Van Der Laan , Thorsten Hesjedal , Henry J. Snaith Small Methods 642 DOI: 10.1002/smtd.202300095 Diamond Proposal Number(s): [16141] Open Access Show Abstract ▼ Abstract: Owing to the unique chemical and electronic properties arising from 3d-electrons, substitution with transition metal ions is one of the key routes for engineering new functionalities into materials. While this approach has been used extensively in complex metal oxide perovskites, metal halide perovskites have largely resisted facile isovalent substitution. In this work, it is demonstrated that the substitution of Co2+ into the lattice of methylammonium lead triiodide imparts magnetic behavior to the material while maintaining photovoltaic performance at low concentrations. In addition to comprehensively characterizing its magnetic properties, the Co2+ ions themselves are utilized as probes to sense the local electronic environment of Pb in the perovskite, thereby revealing the nature of their incorporation into the material. A comprehensive understanding of the effect of transition metal incorporation is provided, thereby opening the substitution gateway for developing novel functional perovskite materials and devices for future technologies.	Mar 2023
B18-Core EXAFS	High sodium-ion battery capacity in sulfur-deficient tin(II) sulfide thin films with a microrod morphology Zening Zhu , Geoffrey Hyett , Gillian Reid , Fred Robinson , Giannantonio Cibin , Andrew L. Hector Small Structures 7 DOI: 10.1002/sstr.202200396 Diamond Proposal Number(s): [14239] Open Access Show Abstract ▼ Abstract: Sulfur-deficient SnS thin films for sodium-ion battery anode application are prepared using aerosol-assisted chemical vapor deposition. Growth directly onto the metal foil current collector forms sulfur-deficient SnS microrod structures via a vapor–liquid–solid growth mechanism, with 92 nm average SnS crystallite size and an 800 nm film thickness. The sulfur deficiency is demonstrated with energy-dispersive X-ray analysis, powder X-ray diffraction, and X-ray absorption near-edge structure analyses. This sulfur-deficient SnS material demonstrates a very high capacity in sodium half cells. The first reduction scan at a specific current of 150 mA g−1 shows a capacity of 1084 mAh g−1. At the 50th cycle the specific capacity is 638 mAh g−1 for reduction and 593 mAh g−1 for oxidation. This capacity is demonstrated for tin sulfide itself without the need for a nanostructured carbon support, unlike previous high capacity SnS anodes in the literature. Both the capacity and ex situ characterization experiments indicate a conversion reaction producing tin, followed by alloying with sodium during reduction, and that both of these processes are reversible during oxidation.	Feb 2023
B07-B-Versatile Soft X-ray beamline: High Throughput	Nanostructured silicon matrix for materials engineering Poting Liu , Alexander Schleusener , Gabriel Zieger , Arne Bochmann , Matthijs A. Van Spronsen , Vladimir Sivakov Small 4 DOI: 10.1002/smll.202206318 Diamond Proposal Number(s): [31119] Open Access Show Abstract ▼ Abstract: Tin-containing layers with different degrees of oxidation are uniformly distributed along the length of silicon nanowires formed by a top-down method by applying metalorganic chemical vapor deposition. The electronic and atomic structure of the obtained layers is investigated by applying nondestructive surface-sensitive X-ray absorption near edge spectroscopy using synchrotron radiation. The results demonstrated, for the first time, a distribution effect of the tin-containing phases in the nanostructured silicon matrix compared to the results obtained for planar structures at the same deposition temperatures. The amount and distribution of tin-containing phases can be effectively varied and controlled by adjusting the geometric parameters (pore diameter and length) of the initial matrix of nanostructured silicon. Due to the occurrence of intense interactions between precursor molecules and decomposition by-products in the nanocapillary, as a consequence of random thermal motion of molecules in the nanocapillary, which leads to additional kinetic energy and formation of reducing agents, resulting in effective reduction of tin-based compounds to a metallic tin state for molecules with the highest penetration depth in the nanostructured silicon matrix. This effect will enable clear control of the phase distributions of functional materials in 3D matrices for a wide range of applications.	Jan 2023
I15-1-X-ray Pair Distribution Function (XPDF)	Breaking with the principles of coreduction to form stoichiometric intermetallic PdCu nanoparticles Jette K. Mathiesen , Espen D. Bøjesen , Jack K. Pedersen , Emil T. S. Kjær , Mikkel Juelsholt , Susan Cooper , Jonathan Quinson , Andy S. Anker , Geoff Cutts , Dean S. Keeble , Maria S. Thomsen , Jan Rossmeisl , Kirsten M. Ø. Jensen Small Methods 68 DOI: 10.1002/smtd.202200420 Diamond Proposal Number(s): [20187] Open Access Show Abstract ▼ Abstract: Intermetallic nanoparticles (NPs) have shown enhanced catalytic properties as compared to their disordered alloy counterparts. To advance their use in green energy, it is crucial to understand what controls the formation of intermetallic NPs over alloy structures. By carefully selecting the additives used in NP synthesis, it is here shown that monodisperse, intermetallic PdCu NPs can be synthesized in a controllable manner. Introducing the additives iron(III) chloride and ascorbic acid, both morphological and structural control can be achieved. Combined, these additives provide a synergetic effect resulting in precursor reduction and defect-free growth; ultimately leading to monodisperse, single-crystalline, intermetallic PdCu NPs. Using in situ X-ray total scattering, a hitherto unknown transformation pathway is reported that diverges from the commonly reported coreduction disorder–order transformation. A Cu-rich structure initially forms, which upon the incorporation of Pd(0) and atomic ordering forms intermetallic PdCu NPs. These findings underpin that formation of stoichiometric intermetallic NPs is not limited by standard reduction potential matching and coreduction mechanisms, but is instead driven by changes in the local chemistry. Ultimately, using the local chemistry as a handle to tune the NP structure might open new opportunities to expand the library of intermetallic NPs by exploiting synthesis by design.	Apr 2022
I14-Hard X-ray Nanoprobe	Synchrotron-based nano-X-ray absorption near-edge structure revealing intracellular heterogeneity of iron species in magnetotactic bacteria Daniel M. Chevrier , Elisa Cerda-Donate , Yeseul Park , Fernando Cacho-Nerin , Miguel Gomez-Gonzalez , René Uebe , Damien Faivre Small Science DOI: 10.1002/smsc.202100089 Diamond Proposal Number(s): [23693, 23602] Open Access Show Abstract ▼ Abstract: Magnetotactic bacteria (MTB) sequester iron from the environment to biomineralize magnetite or greigite nanoparticles in magnetosome organelles, though the necessity of intracellular iron storage for the formation process is still in question. Understanding the role of iron storage would make clear the contribution of MTB in geochemical iron cycling and its potential importance during the biosynthesis of application-relevant magnetic nanoparticles. Herein, how scanning X-ray fluorescence microscopy (SXFM) and nanoscale X-ray absorption near-edge structure (nano-XANES) mapping can spatially and chemically identify intracellular iron species is reported, creating an opportunity to examine the role of iron storage in magnetite biomineralization at the single-cell level. Fe K-edge nano-XANES measurements of Magnetospirillum gryphiswaldense in varied iron media conditions and iron storage capacity reveal a significant quantity of intracellular iron heterogeneities through a distinction between formed magnetosomes and intracellular iron material. This intracellular iron component is found in both early and late stages of biomineralization. The capabilities of nano-XANES in providing an experimental advantage in the multidisciplinary field of biomineralization are highlighted.	Dec 2021
E02-JEM ARM 300CF	Atomistic mechanics of torn back folded edges of triangular voids in monolayer WS2 Gyeong Hee Ryu , Gang Seob Jung , Hyoju Park , Ren‐jie Chang , Jamie H. Warner Small 102 DOI: 10.1002/smll.202104238 Show Abstract ▼ Abstract: Triangular nanovoids in 2D materials transition metal dichalcogenides have vertex points that cause stress concentration and lead to sharp crack propagation and failure. Here, the atomistic mechanics of back folding around triangular nanovoids in monolayer WS2 sheets is examined. Combining atomic-resolution images from annular dark-field scanning transmission electron microscopy with reactive molecular modelling, it is revealed that the folding edge formation has statistical preferences under geometric conditions based on the orientation mismatch. It is further investigated how loading directions and strong interlayer friction, interplay with WS2 lattice's crack preference, govern the deformation and fracture pattern around folding edges. These results provide fundamental insights into the combination of fracture and folding in flexible monolayer crystals and the resultant Moiré lattices.	Oct 2021
I13-2-Diamond Manchester Imaging	Synchrotron x‐ray tomography for rechargeable battery research: Fundamentals, setups and applications Fengcheng Tang , Zhibin Wu , Chao Yang , Markus Osenberg , Andre Hilger , Kang Dong , Henning Markötter , Ingo Manke , Fu Sun , Libao Chen , Guanglei Cui Small Methods 34 DOI: 10.1002/smtd.202100557 Show Abstract ▼ Abstract: Understanding the complicated interplay of the continuously evolving electrode materials in their inherent 3D states during the battery operating condition is of great importance for advancing rechargeable battery research. In this regard, the synchrotron X-ray tomography technique, which enables non-destructive, multi-scale, and 3D imaging of a variety of electrode components before/during/after battery operation, becomes an essential tool to deepen this understanding. The past few years have witnessed an increasingly growing interest in applying this technique in battery research. Hence, it is time to not only summarize the already obtained battery-related knowledge by using this technique, but also to present a fundamental elucidation of this technique to boost future studies in battery research. To this end, this review firstly introduces the fundamental principles and experimental setups of the synchrotron X-ray tomography technique. After that, a user guide to its application in battery research and examples of its applications in research of various types of batteries are presented. The current review ends with a discussion of the future opportunities of this technique for next-generation rechargeable batteries research. It is expected that this review can enhance the reader's understanding of the synchrotron X-ray tomography technique and stimulate new ideas and opportunities in battery research.	Aug 2021
I12-JEEP: Joint Engineering, Environmental and Processing	Cycling rate-induced spatially-resolved heterogeneities in commercial cylindrical Li-ion batteries Antonios Vamvakeros , Dorota Matras , Thomas E. Ashton , Alan A. Coelho , Hongyang Dong , Dustin Bauer , Yaroslav Odarchenko , Stephen W. T. Price , Keith T. Butler , Olof Gutowski , Ann-Christin Dippel , Martin Von Zimmerman , Jawwad Darr , Simon D. M. Jacques , Andrew M. Beale Small Methods 33 DOI: 10.1002/smtd.202100512 Open Access Show Abstract ▼ Abstract: Synchrotron high-energy X-ray diffraction computed tomography has been employed to investigate, for the first time, commercial cylindrical Li-ion batteries electrochemically cycled over the two cycling rates of C/2 and C/20. This technique yields maps of the crystalline components and chemical species as a cross-section of the cell with high spatiotemporal resolution (550 × 550 images with 20 × 20 × 3 µm3 voxel size in ca. 1 h). The recently developed Direct Least-Squares Reconstruction algorithm is used to overcome the well-known parallax problem and led to accurate lattice parameter maps for the device cathode. Chemical heterogeneities are revealed at both electrodes and are attributed to uneven Li and current distributions in the cells. It is shown that this technique has the potential to become an invaluable diagnostic tool for real-world commercial batteries and for their characterization under operating conditions, leading to unique insights into “real” battery degradation mechanisms as they occur.	Aug 2021
B18-Core EXAFS	Enhancing hydrogen evolution electrocatalytic performance in neutral media via nitrogen and iron phosphide interactions Siyu Zhao , Ruikuan Xie , Liqun Kang , Manni Yang , Xingyu He , Wenyao Li , Ryan Wang , Dan J. L. Brett , Guanjie He , Guoliang Chai , Ivan P. Parkin Small Science 355 DOI: 10.1002/smsc.202100032 Diamond Proposal Number(s): [19850] Open Access Show Abstract ▼ Abstract: It remains a challenge to develop efficient electrocatalysts in neutral media for hydrogen evolution reaction (HER) due to the sluggish kinetics and switch of the rate determining step. Although metal phosphides are widely used HER catalysts, their structural stability is an issue due to oxidization, and the HER performance in neutral media requires improvement. Herein, a new material, i.e., grapevine‐shaped N‐doped iron phosphide on carbon nanotubes, as an efficient HER catalyst in neutral media is developed. The optimized catalyst shows an overpotential of 256 mV at a large current density of 65 mA cm−2, which is even 10 mV lower than that of the commercial 20% Pt/C catalyst. The excellent performance of the catalyst is further studied by combined computational and experimental techniques, which proves that the interaction between nitrogen and iron phosphides can provide more efficient active structures and stabilize the metal phosphide electrocatalysts for HER.	May 2021

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