I12-JEEP: Joint Engineering, Environmental and Processing
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Matthew J.
Pankhurst
,
Nghia T.
Vo
,
Alan R.
Butcher
,
Haili
Long
,
Hongchang
Wang
,
Sara
Nonni
,
Jason
Harvey
,
Guđmundur
Guđfinnsson
,
Ronald
Fowler
,
Robert
Atwood
,
Richard
Walshaw
,
Peter D.
Lee
Diamond Proposal Number(s):
[14033]
Abstract: Olivine is a key constituent in the silicate Earth; its composition and texture informs petrogenetic understanding of numerous rock types. Here we develop a quantitative and reproducible method to measure olivine composition in three dimensions without destructive analysis, meaning full textural context is maintained. The olivine solid solution between forsterite and fayalite was measured using a combination of three-dimensional (3D) X-ray imaging techniques, 2D backscattered electron imaging, and spot-analyses using wavelength-dispersive electron probe microanalysis. The linear attenuation coefficient of natural crystals across a range of forsterite content from ∼73–91 mol% were confirmed to scale linearly with composition using 53, 60, and 70 kV monochromatic beams at I12-JEEP beamline, Diamond Light Source utilizing the helical fly-scan acquisition. A polychromatic X-ray source was used to scan the same crystals, which yielded image contrast equivalent to measuring the mol% of forsterite with an accuracy of <1.0%. X-ray tomography can now provide fully integrated textural and chemical analysis of natural samples containing olivine, which will support 3D and 3D+time petrologic modeling. The study has revealed >3 mm domains within a large crystal of San Carlos forsterite that varies by ∼2 Fo mol%. This offers a solution to an outstanding question of inter-laboratory standardization, and also demonstrates the utility of 3D, non-destructive, chemical measurement. To our knowledge, this study is the first to describe the application of XMT to quantitative chemical measurement across a mineral solid solution. Our approach may be expanded to calculate the chemistry of other mineral systems in 3D, depending upon the number, chemistry, and density of end-members.
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Nov 2018
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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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Open Access
Abstract: Synchrotron-based X-ray micro-tomography systems often suffer severe ring artifacts in reconstructed images. In sinograms the artifacts appear as straight lines or stripe artifacts. These artifacts are caused by the irregular response of a detecting system giving rise to a variety of observed types of stripes: full stripes, partial stripes, fluctuating stripes, and unresponsive stripes. The use of pre-processing techniques such as distortion correction or phase retrieval blurs and enlarges these stripes. It is impossible for a single approach to remove all types of stripe artifacts. Here, we propose three techniques for tackling all of them. The proposed techniques are easy to implement; do not generate extra stripe artifacts and void-center artifacts; and give superior quality on challenging data sets and in comparison with other techniques. Implementations in Python and a challenging data set are available for download.
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Oct 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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I12-JEEP: Joint Engineering, Environmental and Processing
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A.
Jin
,
J.
Cobb
,
U.
Hansen
,
R.
Bhattacharya
,
C.
Reinhard
,
N.
Vo
,
R.
Atwood
,
J.
Li
,
A.
Karunaratne
,
C.
Wiles
,
R.
Abel
Diamond Proposal Number(s):
[9811, 852]
Open Access
Abstract: Objectives Bisphosphonates (BP) are the first-line treatment for preventing fragility fractures. However, concern regarding their efficacy is growing because bisphosphonate is associated with over-suppression of remodelling and accumulation of microcracks. While dual-energy X-ray absorptiometry (DXA) scanning may show a gain in bone density, the impact of this class of drug on mechanical properties remains unclear. We therefore sought to quantify the mechanical strength of bone treated with BP (oral alendronate), and correlate data with the microarchitecture and density of microcracks in comparison with untreated controls.
Methods Trabecular bone from hip fracture patients treated with BP (n = 10) was compared with naïve fractured (n = 14) and non-fractured controls (n = 6). Trabecular cores were synchrotron scanned and micro-CT scanned for microstructural analysis, including quantification of bone volume fraction, microarchitecture and microcracks. The specimens were then mechanically tested in compression.
Results BP bone was 28% lower in strength than untreated hip fracture bone, and 48% lower in strength than non-fractured control bone (4.6 MPa vs 6.4 MPa vs 8.9 MPa). BP-treated bone had 24% more microcracks than naïve fractured bone and 51% more than non-fractured control (8.12/cm2 vs 6.55/cm2 vs 5.25/cm2). BP and naïve fracture bone exhibited similar trabecular microarchitecture, with significantly lower bone volume fraction and connectivity than non-fractured controls.
Conclusion BP therapy had no detectable mechanical benefit in the specimens examined. Instead, its use was associated with substantially reduced bone strength. This low strength may be due to the greater accumulation of microcracks and a lack of any discernible improvement in bone volume or microarchitecture. This preliminary study suggests that the clinical impact of BP-induced microcrack accumulation may be significant.
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Oct 2017
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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
,
Nghia T.
Vo
,
Oxana V.
Magdysyuk
,
Michael
Drakopoulos
,
Marco Di
Michiel
,
Alexander
Rack
,
Gareth
Hinds
,
Dan J. L.
Brett
,
Paul
Shearing
Diamond Proposal Number(s):
[13884]
Open Access
Abstract: As the energy density of lithium-ion cells and batteries increases, controlling the outcomes of thermal runaway becomes more challenging. If the high rate of gas generation during thermal runaway is not adequately vented, commercial cell designs can rupture and explode, presenting serious safety concerns. Here, ultra-high-speed synchrotron X-ray imaging is used at >20 000 frames per second to characterize the venting processes of six different 18650 cell designs undergoing thermal runaway. For the first time, the mechanisms that lead to the most catastrophic type of cell failure, rupture, and explosion are identified and elucidated in detail. The practical application of the technique is highlighted by evaluating a novel 18650 cell design with a second vent at the base, which is shown to avoid the critical stages that lead to rupture. The insights yielded in this study shed new light on battery failure and are expected to guide the development of safer commercial cell designs.
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Oct 2017
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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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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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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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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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