I12-JEEP: Joint Engineering, Environmental and Processing
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Abstract: X-ray in-line phase contrasttomography holds great promise for the quantitative analysis of soft materials. However, its applications have been limited, so far, by the fact that direct methods based on the transport-of-intensity equation and the contrast transfer function are sensitive to noise and applicable only to limited types of samples. Here, we propose an iterative method based on the Gerchberg-Saxton algorithm (R. W. Gerchberg and W. O. Saxton, Optik 35, 237 (1972)), but overcoming its slow convergence by an acceleration technique, named random signed feedback, which shows an excellent performance, both in numerical simulation and tomographic experiment, of discriminating various polymers even when using 53 keV synchrotron X-rays.
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Dec 2012
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[9244]
Open Access
Abstract: Spiders are an important animal group, with a long history. Details of their origins remain limited, with little knowledge of their stem group, and no insights into the sequence of character acquisition during spider evolution. We describe a new fossil arachnid, Idmonarachne brasieri gen. et sp. nov. from the Late Carboniferous (Stephanian, ca 305–299 Ma) of Montceau-les-Mines, France. It is three-dimensionally preserved within a siderite concretion, allowing both laboratory- and synchrotron-based phase-contrast computed tomography reconstruction. The latter is a first for siderite-hosted fossils and has allowed us to investigate fine anatomical details. Although distinctly spider-like in habitus, this remarkable fossil lacks a key diagnostic character of Araneae: spinnerets on the underside of the opisthosoma. It also lacks a flagelliform telson found in the recently recognized, spider-related, Devonian–Permian Uraraneida. Cladistic analysis resolves our new fossil as sister group to the spiders: the spider stem-group comprises the uraraneids and I. brasieri. While we are unable to demonstrate the presence of spigots in this fossil, the recovered phylogeny suggests the earliest character to evolve on the spider stem-group is the secretion of silk. This would have been followed by the loss of a flagelliform telson, and then the ability to spin silk using spinnerets. This last innovation defines the true spiders, significantly post-dates the origins of silk, and may be a key to the group's success. The Montceau-les-Mines locality has previously yielded a mesothele spider (with spinnerets). Evidently, Late Palaeozoic spiders lived alongside Palaeozoic arachnid grades which approached the spider condition, but did not express the full suite of crown-group autapomorphies.
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Mar 2016
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I12-JEEP: Joint Engineering, Environmental and Processing
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Donal P.
Finegan
,
Eric
Darcy
,
Matthew
Keyser
,
Bernhard
Tjaden
,
Thomas M. M.
Heenan
,
Rhodri
Jervis
,
Josh J.
Bailey
,
Romeo
Malik
,
Nghia T.
Vo
,
Oxana V.
Magdysyuk
,
Robert
Atwood
,
Michael
Drakopoulos
,
Marco
Dimichiel
,
Alexander
Rack
,
Gareth
Hinds
,
Dan J. L.
Brett
,
Paul R.
Shearing
Diamond Proposal Number(s):
[13884]
Abstract: Lithium-ion batteries are being used in increasingly demanding applications where safety and reliability are of utmost importance. Thermal runaway presents the greatest safety hazard, and needs to be fully understood in order to progress towards safer cell and battery designs. Here, we demonstrate the application of an internal short circuiting device for controlled, on-demand, initiation of thermal runaway. Through its use, the location and timing of thermal runaway initiation is pre-determined, allowing analysis of the nucleation and propagation of failure within 18[thin space (1/6-em)]650 cells through the use of high-speed X-ray imaging at 2000 frames per second. The cause of unfavourable occurrences such as sidewall rupture, cell bursting, and cell-to-cell propagation within modules is elucidated, and steps towards improved safety of 18[thin space (1/6-em)]650 cells and batteries are discussed.
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Mar 2017
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B18-Core EXAFS
I18-Microfocus Spectroscopy
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Diamond Proposal Number(s):
[4939]
Open Access
Abstract: The physicochemical state of a catalyst is a key factor in determining both activity and selectivity; however these materials are often not structurally or compositionally homogeneous. Here we report on the 3-dimensional imaging of an industrial catalyst, Mo- promoted colloidal Pt supported on carbon. The distribution of both the active Pt species and Mo promoter have been mapped over a single particle of catalyst using microfocus X-ray Fluorescence computed tomography. X-ray absorption near edge spectroscopy (XANES) and extended X-ray absorption fine structure revealed a mixed local coordination environment, including the presence of both metallic Pt clusters and Pt chloride species, but also no direct interaction between the catalyst and Mo promoter. We also report on the benefits of scanning μ-XANES computed tomography for chemical imaging, allowing for 2- and 3-dimensional mapping of the local electronic and geometric environment, in this instance for both the Pt catalyst and Mo promoter throughout the catalyst particle.
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Nov 2014
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I12-JEEP: Joint Engineering, Environmental and Processing
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Hamish
Yeung
,
Adam F.
Sapnik
,
Felicity
Massingberd-mundy
,
Michael W.
Gaultois
,
Yue
Wu
,
Duncan X.
Fraser
,
Sebastian
Henke
,
Roman
Pallach
,
Niclas
Heidenreich
,
Oxana
Magdysyuk
,
Nghia T.
Vo
,
Andrew L.
Goodwin
Diamond Proposal Number(s):
[16354, 16450]
Abstract: There is an increasingly large amount of interest in metal‐organic frameworks (MOFs) for a variety of applications, from gas sensing and separations to electronics and catalysis. Their exciting properties arise from their modular architectures, which self‐assemble from different combinations of metal‐based and organic building units. However, the exact mechanisms by which they crystallize remain poorly understood, thus limiting any realisation of real “structure by design”. We report important new insight into MOF formation, gained using in situ X‐ray diffraction, pH and turbidity measurements to uncover for the first time the evolution of metastable intermediate species in the canonical zeolitic imidazolate framework system, ZIF‐8. We reveal that the intermediate species exist in a dynamic pre‐equilibrium prior to network assembly and, depending on the reactant concentrations and the progress of reaction, the pre‐equilibrium can be made to favour under‐ or over‐coordinated Zn‐imidazolate species, thus accelerating or inhibiting crystallization, respectively. We thereby find that concentration can be effectively used as a synthetic handle to directly control particle size, with great implications for industrial scale‐up and gas sorption applications. These finding enables us to rationalise the apparent contradictions between previous studies of ZIF‐8 and, importantly, opens up new opportunities for the control of crystallization in network solids more generally, from the design of local structure to assembly of particles with precise dimensions.
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Nov 2018
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I12-JEEP: Joint Engineering, Environmental and Processing
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M.
Polacci
,
F.
Arzilli
,
G.
La Spina
,
N.
Le Gall
,
B.
Cai
,
M. E.
Hartley
,
D.
Di Genova
,
Nghia
Vo
,
S.
Nonni
,
R. C.
Atwood
,
E. W.
Llewellin
,
P. D.
Lee
,
M. R.
Burton
Diamond Proposal Number(s):
[12392, 16188]
Open Access
Abstract: Magma crystallisation is a fundamental process driving eruptions and controlling the style of volcanic activity. Crystal nucleation delay, heterogeneous and homogeneous nucleation and crystal growth are all time-dependent processes, however, there is a paucity of real-time experimental data on crystal nucleation and growth kinetics, particularly at the beginning of crystallisation when conditions are far from equilibrium. Here, we reveal the first in situ 3D time-dependent observations of crystal nucleation and growth kinetics in a natural magma, reproducing the crystallisation occurring in real-time during a lava flow, by combining a bespoke high-temperature environmental cell with fast synchrotron X-ray microtomography. We find that both crystal nucleation and growth occur in pulses, with the first crystallisation wave producing a relatively low volume fraction of crystals and hence negligible influence on magma viscosity. This result explains why some lava flows cover kilometres in a few hours from eruption inception, highlighting the hazard posed by fast-moving lava flows. We use our observations to quantify disequilibrium crystallisation in basaltic magmas using an empirical model. Our results demonstrate the potential of in situ 3D time-dependent experiments and have fundamental implications for the rheological evolution of basaltic lava flows, aiding flow modelling, eruption forecasting and hazard management.
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May 2018
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[13704, 18197]
Abstract: Here we present the first real-time three dimension (3D) observations of damage evolution in a composite tube under torsion. An in-situ torsion test of 1/1 45° (diamond) braided carbon fibre-epoxy circular composite tube was performed on a loading rig and the damage process was characterised by synchrotron X-ray computed tomography (CT). A number of damage modes and their damage sequence has been identified and monitored globally and in more detail within a representative region of interest. In particular, intra-tow cracks and inter-tow debonding have been found to occur almost simultaneously at low shear strains (1.5%). It is noteworthy that inter-tow debonding was initially trapped/limited within repeated braid units before propagating and connecting with other damage modes in 3D. The area fraction of inter-tow debonds was quantified at different stages and it was found to dramatically increase with increasing shear strain beyond 1.5%. The total volume fraction of the observed intra-tow cracks of various forms was seen to grow rapidly beyond shear strain of 2.0%. Beyond the peak shear stress (at shear strain of 2.5%), fibre micro-buckling and kink bands occur in the tows subjected to torsion induced axial compression at crimped regions close to tow crossovers. Tow crossovers control many aspects of damage propagation under torsion, positively by localising inter-tow debonds and negatively by initiating fibre micro-buckling.
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Dec 2019
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[8491, 9825, 11407]
Open Access
Abstract: Purpose: Cerebrospinal fluid pressure (CSFp) changes are involved or implicated in various ocular conditions including glaucoma, idiopathic intracranial hypertension, and visual impairment and intracranial pressure syndrome. However, little is known about the effects of CSFp on lamina cribrosa and retrolaminar neural tissue (RLNT) biomechanics, potentially important in these conditions. Our goal was to use an experimental approach to visualize and quantify the deformation of these tissues as CSFp increased.
Methods: The posterior eye and RLNT of porcine eyes (n = 3) were imaged using synchrotron radiation phase-contrast micro-computed tomography (PC μCT) at an intraocular pressure of 15 mm Hg and CSFps of 4, 10, 20, and 30 mm Hg. Scans of each tissue region were acquired at each CSFp step and analyzed using digital volume correlation to determine 3-dimensional tissue deformations.
Results: Elevating CSFp increased the strain in the lamina cribrosa and RLNT of all three specimens, with the largest strains occurring in the RLNT. Relative to the baseline CSFp of 4 mm Hg, at 30 mm Hg, the lamina cribrosa experienced a mean first and third principal strain of 4.4% and −3.5%, respectively. The corresponding values for the RLNT were 9.5% and −9.1%.
Conclusions: CSFp has a significant impact on the strain distributions within the lamina cribrosa and, more prominently, within the RLNT. Elevations in CSFp were positively correlated with increasing deformations in each region and may play a role in ocular pathologies linked to changes in CSFp.
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Apr 2017
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[16676]
Open Access
Abstract: Solute transport in unsaturated porous materials is a complex process, which exhibits some distinct features differentiating it from transport under saturated conditions. These features emerge mostly due to the different transport time scales at different regions of the flow network, which can be classified into flowing and stagnant regions, predominantly controlled by advection and diffusion, respectively. Under unsaturated conditions, the solute breakthrough curves show early arrivals and very long tails, and this type of transport is usually referred to as non-Fickian. This study directly characterizes transport through an unsaturated porous medium in three spatial dimensions at the resolution of 3.25 μm and the time resolution of 6 s. Using advanced high-speed, high-spatial resolution, synchrotron-based X-ray computed microtomography (sCT) we obtained detailed information on solute transport through a glass bead packing at different saturations. A large experimental dataset (>50 TB) was produced, while imaging the evolution of the solute concentration with time at any given point within the field of view. We show that the fluids’ topology has a critical signature on the non-Fickian transport, which yet needs to be included in the Darcy-scale solute transport models. The three-dimensional (3D) results show that the fully mixing assumption at the pore scale is not valid, and even after injection of several pore volumes the concentration field at the pore scale is not uniform. Additionally, results demonstrate that dispersivity is changing with saturation, being twofold larger at the saturation of 0.52 compared to that at the fully saturated domain.
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Sep 2020
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[8491]
Open Access
Abstract: Purpose: Scleral stiffening has been proposed as a treatment for glaucoma to protect the lamina cribrosa (LC) from excessive intraocular pressure–induced deformation. Here we experimentally evaluated the effects of moderate stiffening of the peripapillary sclera on the deformation of the LC.
Methods: An annular sponge, saturated with 1.25% glutaraldehyde, was applied to the external surface of the peripapillary sclera for 5 minutes to stiffen the sclera. Tissue deformation was quantified in two groups of porcine eyes, using digital image correlation (DIC) or computed tomography imaging and digital volume correlation (DVC). In group A (n = 14), eyes were subjected to inflation testing before and after scleral stiffening. Digital image correlation was used to measure scleral deformation and quantify the magnitude of scleral stiffening. In group B (n = 5), the optic nerve head region was imaged using synchrotron radiation phase-contrast microcomputed tomography (PC μCT) at an isotropic spatial resolution of 3.2 μm. Digital volume correlation was used to compute the full-field three-dimensional deformation within the LC and evaluate the effects of peripapillary scleral cross-linking on LC biomechanics.
Results: On average, scleral treatment with glutaraldehyde caused a 34 ± 14% stiffening of the peripapillary sclera measured at 17 mm Hg and a 47 ± 12% decrease in the maximum tensile strain in the LC measured at 15 mm Hg. The reduction in LC strains was not due to cross-linking of the LC.
Conclusions: Peripapillary scleral stiffening is effective at reducing the magnitude of biomechanical strains within the LC. Its potential and future utilization in glaucoma axonal neuroprotection requires further investigation.
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May 2016
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