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

Instruments / Technical Area	Publication Details	Published
I13-1-Coherence	Quantitative phase measurements of human cell nuclei using X-ray ptychography Jorg Schwenke , Mohammed Yusuf , Laura A. Shemilt , Ulrich Wagner , Atiqa Sajid , Graeme R. Morrison , Fucai Zhang , Aaron Parsons , Christoph Rau , Ian K. Robinson Journal Of Synchrotron Radiation 28 DOI: 10.1107/S1600577521004586 Show Abstract ▼ Abstract: The human cell nucleus serves as an important organelle holding the genetic blueprint for life. In this work, X-ray ptychography was applied to assess the masses of human cell nuclei using its unique phase shift information. Measurements were carried out at the I13-1 beamline at the Diamond Light Source that has extremely large transverse coherence properties. The ptychographic diffractive imaging approach allowed imaging of large structures that gave quantitative measurements of the phase shift in 2D projections. In this paper a modified ptychography algorithm that improves the quality of the reconstruction for weak scattering samples is presented. The application of this approach to calculate the mass of several human nuclei is also demonstrated.	Jul 2021
I13-1-Coherence	Imaging defects in vanadium( iii ) oxide nanocrystals using Bragg coherent diffractive imaging Zachary Barringer , Jie Jiang , Xiaowen Shi , Elijah Schold , Anastasios Pateras , Silvia Cipiccia , Christoph Rau , Jian Shi , Edwin Fohtung Crystengcomm 54 DOI: 10.1039/D1CE00736J Diamond Proposal Number(s): [20381] Show Abstract ▼ Abstract: Defects in strongly correlated materials such as V2O3 play influential roles on their electrical properties. Understanding the defects' structure is of paramount importance. In this project, we investigate defect structures in V2O3 grown via a flux method. We use AFM to see surface features in several large flake-like particles that exhibit characteristics of spiral growth. We also use Bragg coherent diffractive imaging (BCDI) to probe in 3 dimensions a smaller particle without flake-like morphology and note an absence of the pure screw dislocation characteristic of spiral growth. We identified and measured several defects by comparing the observed local displacement of the crystal, measured via BCDI to well-known models of the displacement around defects in the crystal. We identified two image file: d1ce00736j-t1.tif partial dislocations in the crystal. We discuss how defects of different types influence the morphology of V2O3 crystals grown via a flux method.	Jul 2021
I13-1-Coherence	X-ray ptychography with a laboratory source Darren Batey , Frederic Van Assche , Sander Vanheule , Matthieu N. Boone , Andrew J. Parnell , Oleksandr O. Mykhaylyk , Christoph Rau , Silvia Cipiccia Physical Review Letters 126 DOI: 10.1103/PhysRevLett.126.193902 Open Access Show Abstract ▼ Abstract: X-ray ptychography has revolutionized nanoscale phase contrast imaging at large-scale synchrotron sources in recent years. We present here the first successful demonstration of the technique in a small-scale laboratory setting. An experiment was conducted with a liquid metal-jet x-ray source and a single photon-counting detector with a high spectral resolution. The experiment used a spot size of 5 μ m to produce a ptychographic phase image of a Siemens star test pattern with a submicron spatial resolution. The result and methodology presented show how high-resolution phase contrast imaging can now be performed at small-scale laboratory sources worldwide.	May 2021
I13-2-Diamond Manchester Imaging	Tracking lithium penetration in solid electrolytes in 3D by in-situ synchrotron X-ray computed tomography Shuai Hao , Sohrab R. Daemi , Thomas M. M. Heenan , Wenjia Du , Chun Tan , Malte Storm , Christoph Rau , Dan J. I. Brett , Paul R. Shearing Nano Energy 82 DOI: 10.1016/j.nanoen.2021.105744 Diamond Proposal Number(s): [22198] Show Abstract ▼ Abstract: Solid state batteries have attracted extensive attention, but the lithium penetration through the solid electrolyte remains a critical barrier to commercialisation and is not yet fully understood. In this study, the 3D morphological evolution of cracks with deposited lithium were tracked as they penetrated through the solid electrolyte during repetitive plating. This is achieved by utilising in-situ synchrotron X-ray computed tomography with high spatial and temporal resolutions. Thin-sheet cracks were observed to penetrate the solid electrolyte without immediate short-circuiting of the cell. Changes in their width and volume were quantified. By calculating the volume of deposited lithium, it was found that the lithium was only partially filled in cracks, and its filling ratio quickly dropped from 94.95% after the 1st plating to ca. 20% after the 4th plating. The filling process was revealed through tracking the line profile of grayscale along cracks. It was found that lithium grew much more slowly than cracks, so that the cracks near the cathode side were largely hollow and the cell could continue to operate. The deposited lithium after short circuit was segmented and its distribution was visualised. DVC analysis was applied to map local high stress and strain, which aggregated along cracks and significantly increased at areas where new cracks formed.	Apr 2021
I13-2-Diamond Manchester Imaging	4D micro-scale, phase-contrast X-ray imaging and computed tomography of HMX-based polymer-bonded explosives during thermal runaway G. R. Parker , D. S. Eastwood , M. Storm , K. Vitharana , E. M. Heatwole , I. Lopez-Pulliam , R. M. Broilo , P. M. Dickson , A. Martinez , Christoph Rau , N. K. Bourne Combustion And Flame 226, 478 - 489 DOI: 10.1016/j.combustflame.2020.12.025 Diamond Proposal Number(s): [15068, 16650, 18198] Show Abstract ▼ Abstract: High-resolution synchrotron x-ray radiography with computed tomography is used to observe the evolution of porosity created by thermal exposure in two HMX-based polymer-bonded explosive compositions; LX-04 and BX-63. The measurements were made in situ, over an extended period of time, during which the samples were heated on a slow-rate thermal trajectory. The tests ended with thermal-runaway to ignition after which the samples were consumed by combustion. The primary means of damage appears to be from mechanical debonding of the HMX-binder interface with secondary contribution from chemical decomposition. Confinement and binder properties affect the amount of porosity and permeability that develops. Additionally, observations were made describing the emergence and structure of an internal ignition volume, the formation and transport of a pre-ignition melt layer, and how the early stages of combustion were affected by material morphology, mechanical confinement and melt. The contact angle between molten HMX and the fluoropolymer, Viton A, is also presented. For the first time we have time-resolved x-ray images of ignition in sufficient detail to verify the mechanism of cookoff in polymer-bonded explosive compositions.	Apr 2021
I13-1-Coherence	X-ray ptychography imaging of human chromosomes after low-dose irradiation Archana Bhartiya , Darren Batey , Silvia Cipiccia , Xiaowen Shi , Christoph Rau , Stanley Botchway , Mohammed Yusuf , Ian K. Robinson Chromosome Research 55 DOI: 10.1007/s10577-021-09660-7 Open Access Show Abstract ▼ Abstract: Studies of the structural and functional role of chromosomes in cytogenetics have spanned more than 10 decades. In this work, we take advantage of the coherent X-rays available at the latest synchrotron sources to extract the individual masses of all 46 chromosomes of metaphase human B and T cells using hard X-ray ptychography. We have produced ‘X-ray karyotypes’ of both heavy metal–stained and unstained spreads to determine the gain or loss of genetic material upon low-level X-ray irradiation doses due to radiation damage. The experiments were performed at the I-13 beamline, Diamond Light Source, Didcot, UK, using the phase-sensitive X-ray ptychography method.	Mar 2021
I13-2-Diamond Manchester Imaging	Increased cochlear otic capsule thickness and intracortical canal porosity in the oim mouse model of osteogenesis imperfecta Annalisa De Paolis , Brendyn James Miller , Michael Doube , Andrew John Bodey , Christoph Rau , Claus-Peter Richter , Luis Cardoso , Alessandra Carriero Journal Of Structural Biology DOI: 10.1016/j.jsb.2021.107708 Diamond Proposal Number(s): [9860] Show Abstract ▼ Abstract: Osteogenesis imperfecta (OI or brittle bone disease) is a group of genetic disorders of the connective tissues caused mainly by mutations in the genes encoding collagen type I. Clinical manifestations of OI include skeletal fragility, bone deformities, and severe functional disabilities, such as hearing loss. Progressive hearing loss, usually beginning in childhood, affects approximately 70% of people with OI with more than half of the cases involving the inner ear. There is no cure for OI nor a treatment to ameliorate its corresponding hearing loss, and very little is known about the properties of OI ears. In this study, we investigate the morphology of the otic capsule and the cochlea in the inner ear of the oim mouse model of OI. High-resolution 3D images of 8-week old oim and WT inner ears were acquired using synchrotron microtomography. Volumetric morphometric measurements were conducted for the otic capsule, its intracortical canal network and osteocyte lacunae, and for the cochlear spiral ducts. Our results show that the morphology of the cochlea is preserved in the oim ears at 8 weeks of age but the otic capsule has a greater cortical thickness and altered intracortical bone porosity, with a larger number and volume density of highly branched canals in the oim otic capsule. These results portray a state of compromised bone quality in the otic capsule of the oim mice that may contribute to their hearing loss.	Feb 2021
I13-1-Coherence	Operando Bragg coherent diffraction imaging of LiNi0.8Mn0.1Co0.1O2 primary particles within commercially printed NMC811 electrode sheets Ana Katrina C. Estandarte , Jiecheng Diao , Alice Llewellyn , Anmol Jnawali , Thomas M. M. Heenan , Sohrab R. Daemi , Josh J. Bailey , Silvia Cipiccia , Darren Batey , Xiaowen Shi , Christoph Rau , Dan J. L. Brett , Rhodri Jervis , Ian K. Robinson , Paul Shearing Acs Nano DOI: 10.1021/acsnano.0c08575 Diamond Proposal Number(s): [25852, 25440, 24129, 22373, 22309, 21652] Show Abstract ▼ Abstract: Due to complex degradation mechanisms, disparities between the theoretical and practical capacities of lithium-ion battery cathode materials persist. Specifically, Ni-rich chemistries such as LiNi0.8Mn0.1Co0.1O2 (or NMC811) are one of the most promising choices for automotive applications; however, they continue to suffer severe degradation during operation that is poorly understood, thus challenging to mitigate. Here we use operando Bragg coherent diffraction imaging for 4D analysis of these mechanisms by inspecting the individual crystals within primary particles at various states of charge (SoC). Although some crystals were relatively homogeneous, we consistently observed non-uniform distributions of inter- and intracrystal strain at all measured SoC. Pristine structures may already possess heterogeneities capable of triggering crystal splitting and subsequently particle cracking. During low-voltage charging (2.7–3.5 V), crystal splitting may still occur even during minimal bulk deintercalation activity; and during discharging, rotational effects within parallel domains appear to be the precursor for the nucleation of screw dislocations at the crystal core. Ultimately, this discovery of the central role of crystal grain splitting in the charge/discharge dynamics may have ramifications across length scales that affect macroscopic performance loss during real-world battery operation.	Dec 2020
I13-1-Coherence I18-Microfocus Spectroscopy	Structural and compositional characteristics of Fukushima release particulate material from Units 1 and 3 elucidates release mechanisms, accident chronology and future decommissioning strategy Peter Martin , Christopher P. Jones , Stuart Bartlett , Konstantin Ignatyev , Dave Megson-Smith , Yukihiko Sato , Silvia Cipiccia , Darren J. Batey , Christoph Rau , Keisuke Sueki , Tatsuya Ishii , Junya Igarashi , Kazuhiko Ninomiya , Atsushi Shinohara , Alison Rust , Thomas B. Scott Scientific Reports 10 DOI: 10.1038/s41598-020-79169-2 Diamond Proposal Number(s): [24769, 19881] Open Access Show Abstract ▼ Abstract: The structural form and elemental distribution of material originating from different Fukushima Daiichi Nuclear Power Plant reactors (Units 1 and 3) is hereby examined to elucidate their contrasting release dynamics and the current in-reactor conditions to influence future decommissioning challenges. Complimentary computed X-ray absorption tomography and X-ray fluorescence data show that the two suites of Si-based material sourced from the different reactor Units have contrasting internal structure and compositional distribution. The known event and condition chronology correlate with the observed internal and external structures of the particulates examined, which suggest that Unit 1 ejecta material sustained a greater degree of melting than that likely derived from reactor Unit 3. In particular, we attribute the near-spherical shape of Unit 1 ejecta and their internal voids to there being sufficient time for surface tension to round these objects before the hot (and so relatively low viscosity) silicate melt cooled to form glass. In contrast, a more complex internal form associated with the sub-mm particulates invoked to originate from Unit 3 suggest a lower peak temperature, over a longer duration. Using volcanic analogues, we consider the structural form of this material and how it relates to its environmental particulate stability and the bulk removal of residual materials from the damaged reactors. We conclude that the brittle and angular Unit 3 particulate are more susceptible to further fragmentation and particulate generation hazard than the round, higher-strength, more homogenous Unit 1 material.	Dec 2020
I13-1-Coherence I13-2-Diamond Manchester Imaging	Multiscale characterization of the 3D network structure of metal carbides in a Ni superalloy by synchrotron X-ray microtomography and ptychography Zhiguo Zhang , Jia Chuan Khong , Billy Koe , Shifeng Luo , Shi Huang , Ling Qin , Silvia Cipiccia , Darren Batey , Andrew J. Bodey , Christoph Rau , Yu Lung Chiu , Zhu Zhang , Jean-Christophe Gebelin , Nick Green , Jiawei Mi Scripta Materialia 193, 71 - 76 DOI: 10.1016/j.scriptamat.2020.10.032 Diamond Proposal Number(s): [9974, 13488, 22525] Open Access Show Abstract ▼ Abstract: Synchrotron X-ray microtomography and ptychography were used to characterize the 3D network structure, morphology and distribution of metal carbides in an as-cast IN713LC Ni superalloy. MC typed carbides were found to distribute mainly on the grain boundary between the matrix γ and γ' phase. The differences in solidification cooling rate had a minor influence on the volume fraction of the MC type carbides, but significantly affected the carbide size, distribution and network morphology. Depending on the local composition of the remaining liquid phase and geometric constraints, the carbides can form either spherical or strip or network morphologies. The research demonstrated clearly the advantage and technical potential of using the two complementary tomography techniques synergistically to characterize non-destructively complex multiple-phase structures in three dimensional space with a spatial resolution of ~30 nm.	Oct 2020

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