I10-Beamline for Advanced Dichroism
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Open Access
Abstract: Element-specific spectroscopies using synchrotron-radiation can provide unique insights into materials properties. The recently developed technique of X-ray detected ferromagnetic resonance (XFMR) allows studying the magnetization dynamics of magnetic spin structures. Magnetic sensitivity in XFMR is obtained from the X-ray magnetic circular dichroism (XMCD) effect, where the phase of the magnetization precession of each magnetic layer with respect to the exciting radio frequency is obtained using stroboscopic probing of the spin precession. Measurement of both amplitude and phase response in the magnetic layers as a function of bias field can give a clear signature of spin-transfer torque (STT) coupling between ferromagnetic layers due to spin pumping. In the last few years, there have been new developments utilizing X-ray scattering techniques to reveal the precessional magnetization dynamics of ordered spin structures in the GHz frequency range. The techniques of diffraction and reflectometry ferromagnetic resonance (DFMR and RFMR) provide novel ways for the probing of the dynamics of chiral and multilayered magnetic materials, thereby accessing key information relevant to the engineering and development of high-density and low-energy consumption data processing solutions.
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Jul 2023
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I10-Beamline for Advanced Dichroism
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Diamond Proposal Number(s):
[16141]
Open Access
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.
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Mar 2023
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B21-High Throughput SAXS
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Open Access
Abstract: The current SARS-Covid-2 (SARS-CoV-2) pandemic has led to an acceleration of messenger ribonucleic acid (mRNA) vaccine technology. The development of production processes for these large mRNA molecules, especially self-amplifying mRNA (saRNA), has required concomitant development of analytical characterization techniques. Characterizing the purity, shape and structure of these biomolecules is key to their successful performance as drug products. This article describes the biophysical characterization of the Imperial College London Self-amplifying viral RNA vaccine (IMP-1) developed for SARS-CoV-2. A variety of analytical techniques have been used to characterize the IMP-1 RNA molecule. In this article, we use ultraviolet spectroscopy, dynamic light scattering, size-exclusion chromatography small-angle X-ray scattering and circular dichroism to determine key biophysical attributes of IMP-1. Each technique provides important information about the concentration, size, shape, structure and purity of the molecule.
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Jan 2023
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Detectors
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L.
Manzanillas
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S.
Aplin
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A.
Balerna
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P.
Bell
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J.
Casas
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M.
Cascella
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S.
Chatterji
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C.
Cohen
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G.
Dennis
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P.
Fajardo
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H.
Graafsma
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H.
Hirsemann
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F. J.
Iguaz
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K.
Klementiev
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T.
Kołodziej
,
T.
Martin
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R.
Menk
,
F.
Orsini
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M.
Porro
,
M.
Quispe
,
B.
Schmitt
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N.
Tartoni
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M.
Turcato
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C.
Ward
,
E.
Welter
Abstract: In past years efforts have concentrated on the development of arrays of Silicon Drift Detectors for X-ray spectroscopy. This is in stark contrast to the little effort that has been devoted to the improvement of germanium detectors, in particular for synchrotron applications. Germanium detectors have better energy resolution and are more efficient in detecting high energy photons than silicon detectors. In this context, the detector consortium of the European project LEAPS-INNOV has set an ambitious R&D program devoted to the development of a new generation of multi-element monolithic germanium detectors for X-ray detection. In order to improve the performance of the detector under development, simulations of the different detector design options have been performed. In this contribution, the efforts in terms of R&D are outlined with a focus on the modelization of the detector geometry and first performance results. These performance results show that a signal-to-background ratio larger than 1000 can be achieved in the energy range of interest from 5 keV to 100 keV.
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Dec 2022
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Detectors
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F.
Orsini
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S.
Aplin
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A.
Balerna
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P.
Bell
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J.
Casas
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M.
Cascella
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S.
Chatterji
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C.
Cohen
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G.
Dennis
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P.
Fajardo
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H.
Graafsma
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H.
Hirsemann
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F. J.
Iguaz
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K.
Klementiev
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T.
Kołodziej
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L.
Manzanillas
,
T.
Martin
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R.
Menk
,
M.
Porro
,
M.
Quispe
,
B.
Schmitt
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N.
Tartoni
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M.
Turcato
,
C.
Ward
,
E.
Welter
Abstract: The high brilliance and coherent beams resulting from recent upgraded synchrotron radiation facilities open the way for a large range of experiments, where detectors play a key role in the techniques and methods developed to fully exploit the upgraded synchrotron. For instance, one of the major limitations of XAFS experiment is the performance of the detectors. In order to be able to measure more challenging samples and to cope with the very high photon flux of the current and future (diffraction limited) sources, technological developments of detectors are necessary. In this framework, the germanium detector developed in the European project LEAPS-INNOV aims at improving several technological aspects. This type of detector represents a very important class of instruments for X-ray spectroscopy due to the fact that they enable to detect efficiently photons of considerable higher energy with respect to silicon detectors. The objective of this project consists in pushing the detector performance beyond the state-of-the-art. Preliminary layout and main choices for the design studies of this new detector are presented in this paper.
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Oct 2022
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B07-C-Versatile Soft X-ray beamline: Ambient Pressure XPS and NEXAFS
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Open Access
Abstract: Understanding how the microstructure of the active Cu0 component in the commercially applicable Cu/ZnO/Al2O3(−Cs2O) low-temperature water-gas shift catalyst evolves under various H2 partial pressures in the presence/absence of a Cs promoter during thermal activation has been investigated. Time-resolved XRD and spatially-resolved XRD-CT data were measured as a function of H2 concentration along a packed bed reactor to elucidate the importance of the zincite support and the effect of the promoter on Cu sintering mechanisms, dislocation character and stacking fault probability. The rate of Cu reduction showed a dependency on [Cs], [H2] and bed height; lower [Cs] and higher [H2] led to a greater rate of metallic copper nanoparticle formation. A deeper analysis of the XRD line profiles allowed for determining a greater edge character to the dislocations and subsequent stacking fault probability was also observed to depend on higher [H2], smaller Cu0 (and ZnO) crystallite sizes, increased [ZnO] (30 wt.%, sCZA) and lower temperature. The intrinsic activity of Cu/ZnO/Al2O3 methanol synthesis catalysts has been intimately linked to the anisotropic behaviour of copper, and thus the presence of lattice defects; to the best knowledge of the authors, this study is the first instance in which this type of analysis has been applied to LT-WGS catalysts.
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Aug 2022
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I15-1-X-ray Pair Distribution Function (XPDF)
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Jette K.
Mathiesen
,
Espen D.
Bøjesen
,
Jack K.
Pedersen
,
Emil T. S.
Kjær
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Mikkel
Juelsholt
,
Susan
Cooper
,
Jonathan
Quinson
,
Andy S.
Anker
,
Geoff
Cutts
,
Dean S.
Keeble
,
Maria S.
Thomsen
,
Jan
Rossmeisl
,
Kirsten M. Ø.
Jensen
Diamond Proposal Number(s):
[20187]
Open Access
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.
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Apr 2022
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I13-2-Diamond Manchester Imaging
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Fengcheng
Tang
,
Zhibin
Wu
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Chao
Yang
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Markus
Osenberg
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Andre
Hilger
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Kang
Dong
,
Henning
Markötter
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Ingo
Manke
,
Fu
Sun
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Libao
Chen
,
Guanglei
Cui
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.
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Aug 2021
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I12-JEEP: Joint Engineering, Environmental and Processing
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Antonios
Vamvakeros
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Dorota
Matras
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Thomas E.
Ashton
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Alan A.
Coelho
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Hongyang
Dong
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Dustin
Bauer
,
Yaroslav
Odarchenko
,
Stephen W. T.
Price
,
Keith T.
Butler
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Olof
Gutowski
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Ann-Christin
Dippel
,
Martin Von
Zimmerman
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Jawwad
Darr
,
Simon D. M.
Jacques
,
Andrew M.
Beale
Open Access
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.
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Aug 2021
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Ugis
Sarkans
,
Wah
Chiu
,
Lucy M.
Collinson
,
Michele C.
Darrow
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Jan
Ellenberg
,
David
Grunwald
,
Jean-Karim
Hériché
,
Andrii
Iudin
,
Gabriel G.
Martins
,
Terry
Meehan
,
Kedar
Narayan
,
Ardan
Patwardhan
,
Matthew Robert Geoffrey
Russell
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Helen R.
Saibil
,
Caterina
Strambio-De-Castillia
,
Jason R.
Swedlow
,
Christian
Tischer
,
Virginie
Uhlmann
,
Paul
Verkade
,
Mary
Barlow
,
Omer
Bayraktar
,
Ewan
Birney
,
Cesare
Catavitello
,
Christopher
Cawthorne
,
Stephan
Wagner-Conrad
,
Elizabeth
Duke
,
Perrine
Paul-Gilloteaux
,
Emmanuel
Gustin
,
Maria
Harkiolaki
,
Pasi
Kankaanpää
,
Thomas
Lemberger
,
Jo
Mcentyre
,
Josh
Moore
,
Andrew W.
Nicholls
,
Shuichi
Onami
,
Helen
Parkinson
,
Maddy
Parsons
,
Marina
Romanchikova
,
Nicholas
Sofroniew
,
Jim
Swoger
,
Nadine
Utz
,
Lenard M.
Voortman
,
Frances
Wong
,
Peijun
Zhang
,
Gerard J.
Kleywegt
,
Alvis
Brazma
Abstract: Bioimaging data have significant potential for reuse, but unlocking this potential requires systematic archiving of data and metadata in public databases. We propose draft metadata guidelines to begin addressing the needs of diverse communities within light and electron microscopy. We hope this publication and the proposed Recommended Metadata for Biological Images (REMBI) will stimulate discussions about their implementation and future extension.
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May 2021
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