I12-JEEP: Joint Engineering, Environmental and Processing
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Martin T. M.
Pham
,
John J.
Darst
,
Donal P.
Finegan
,
James B.
Robinson
,
Thomas M. M.
Heenan
,
Matt D. R.
Kok
,
Francesco
Iacoviello
,
Rhodri
Owen
,
William Q.
Walker
,
Oxana
Magdysyuk
,
Thomas
Connolley
,
Eric
Darcy
,
Gareth
Hinds
,
Dan J. L.
Brett
,
Paul
Shearing
Diamond Proposal Number(s):
[20903]
Abstract: It remains difficult to detect internal mechanical deformation and gas-induced degradation in lithium-ion batteries, especially outside specialized diagnostics laboratories. In this work, we demonstrate that electrochemical acoustic time-of-flight (EA-ToF) spectroscopy can be used as an insightful and field-deployable diagnostic/prognostic technique to sense the onset of failure. A 210 mAh commercial lithium-ion cell undergoing thermal abuse testing is probed with in situ and operando EA-ToF spectroscopy, together with simultaneous fractional thermal runaway calorimetry (FTRC) and synchrotron X-ray imaging. The combination of X-ray imaging and EA-ToF analysis provides new understanding into the through-plane mechanical deformation in lithium-ion batteries through direct visualisation and the acoustic ToF response. Internal structural changes, such as gas-induced delamination, are identified using EA-ToF spectroscopy due to variations in the attenuation and signal peak shifts. This is corroborated using X-ray imaging, demonstrating EA-ToF spectroscopy as a promising technique for detecting onset of battery failure.
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Jun 2020
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[12631, 13764, 19216]
Abstract: A key technique for controlling solidification microstructures is magneto-hydrodynamics (MHD), resulting from imposing a magnetic field to solidifying metals and alloys. Applications range from bulk stirring to flow control and turbulence damping via the induced Lorentz force. Over the past two decades the Lorentz force caused by the interaction of thermoelectric currents and the magnetic field, a MHD phenomenon known as Thermoelectric Magnetohydrodynamics (TEMHD), was also shown to drive inter-dendritic flow altering microstructural evolution. In this contribution, high-speed synchrotron X-ray tomography and computational simulation are coupled to reveal the evolution, dynamics and mechanisms of solidification within a magnetic field, resolving the complex interplay and competing flow effects arising from Lorentz forces of different origins. The study enabled us to reveal the mechanisms disrupting the traditional columnar dendritic solidification microstructure, ranging from an Archimedes screw-like structure, to one with a highly refined dendritic primary array. We also demonstrate that alloy composition can be tailored to increase or decrease the influence of MHD depending on the Seebeck coefficient and relative density of the primary phase and interdendritic liquid. This work paves the way towards novel computational and experimental methods of exploiting and optimising the application of MHD in solidification processes, together with the calculated design of novel alloys that utilise these forces.
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Jun 2020
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Abstract: The effect of gravity on thermo-solutal convection and its impact on solidification dynamics of an Al-15 wt%Cu alloy were studied using high speed synchrotron tomography. A method for mapping the composition of the solidifying samples was developed, enabling three-dimensional quantification of the time evolved solute concentration and dendrite morphology. Differences in solute segregation, dendrite morphology and fragmentation between upwards and downwards solidification were identified, which were attributed to buoyancy-modulated thermal-solutal convection.
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Apr 2020
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[18468]
Open Access
Abstract: There are several mechanisms contributing towards detrimental damage in wind turbine gearbox bearings, with sudden overload events believed to reduce their expected operational life. The generation of subsurface plasticity, followed by rolling contact fatigue, may lead to the initiation of either surface or subsurface cracking. This study presents a novel technique capable of measuring subsurface strain evolution in a rotating roller bearing, using energy dispersive X-ray diffraction. A pre-overloaded bearing was tested dynamically and consequently failed prematurely, supporting the hypothesis that overloads accelerate bearing failure. Throughout the test, an increase in compressive radial strain was observed, indicative of material softening, generally associated with the unstable stage of rolling contact fatigue, which occurs prior to definitive bearing failure.
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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):
[187201]
Abstract: In this study, the polymorphic transitions of mefenamic acid (MA) were studied by synchrotron X-ray powder diffraction combined with differential scanning calorimetry (XRD-DSC). The initial material was found to be phase-pure form I which, when heated, produces two endotherms that can be observed by DSC at 162.72 and 219.55°C. The former was found to correspond to a solid–solid enantiotropic transition from form I to a mixture of forms II and III. The latter is the melting point of form II. As form I is heated, significantly greater unit-cell expansion is seen in the a direction than in b and c, which can be explained by the stronger intermolecular interactions in the bc plane. Refinements of the reported MA structures against the patterns collected during heating revealed that at 175°C there exists a mixture of forms I, II and III, whereas only forms II and III remain at 205°C. However, reflections are observed at both temperatures which cannot be fitted with the known forms of MA. It is hypothesized that a new form of MA is produced upon heating. The stability of MA after the enantiotropic transition temperature is II > III > I, which differs from the previously reported II > I > III.
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Dec 2019
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B22-Multimode InfraRed imaging And Microspectroscopy
I11-High Resolution Powder Diffraction
I12-JEEP: Joint Engineering, Environmental and Processing
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Harry G. W.
Godfrey
,
Lydia
Briggs
,
Xue
Han
,
William J. F.
Trenholme
,
Christopher
Morris
,
Mathew
Savage
,
Louis
Kimberley
,
Oxana
Magdysyuk
,
Michael
Drakopoulos
,
Claire A.
Murray
,
Chiu C.
Tang
,
Mark D.
Frogley
,
Gianfelice
Cinque
,
Sihai
Yang
,
Martin
Schroeder
Diamond Proposal Number(s):
[11278]
Open Access
Abstract: Understanding the mechanism of assembly and function of metal-organic frameworks (MOFs) is important for the development of practical materials. Herein, we report a time-resolved diffraction analysis of the kinetics of formation of a robust MOF, MFM-300(Fe), which shows high adsorption capacity for CO2 (9.55 mmol g−1 at 293 K and 20 bar). Applying the Avrami-Erofe’ev and the two-step kinetic Finke-Watzky models to in situ high-energy synchrotron X-ray powder diffraction data obtained during the synthesis of MFM-300(Fe) enables determination of the overall activation energy of formation (50.9 kJ mol−1), the average energy of nucleation (56.7 kJ mol−1), and the average energy of autocatalytic growth (50.7 kJ mol−1). The synthesis of MFM-300(Fe) has been scaled up 1000-fold, enabling the successful breakthrough separations of the CO2/N2 mixture in a packed-bed with a selectivity for CO2/N2 of 21.6. This study gives an overall understanding for the intrinsic behaviors of this MOF system, and we have determined directly the binding domains and dynamics for adsorbed CO2 molecules within the pores of MFM-300(Fe).
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Nov 2019
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I12-JEEP: Joint Engineering, Environmental and Processing
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Shenghang
Xu
,
Meng
Du
,
Jia
Li
,
Kun
Yan
,
Biao
Cai
,
Quanfeng
He
,
Qihong
Fang
,
Oxana
Magdysyuk
,
Bin
Liu
,
Yong
Yang
,
Yong
Liu
Diamond Proposal Number(s):
[18192]
Abstract: Nature materials, such as bones and nacre, achieve excellent balance of toughness and strength via a hierarchical “brick-and-mortar” microstructure, which is an attractive model for engineering materials design. Here, we produced nacre-like Ti-Ta metallic composites via a powder metallurgy process, during which mixed powders were sintered by spark plasma sintering, followed by hot and cold rolling and then annealing. The structure consists of soft Ta-enriched regions and hard Ti-enriched regions in a hierarchical and laminated fashion. The microstructural heterogeneity spans several scales due to the diffusion between Ti and Ta. This yields a novel metal-metal composite with a balanced combination of strength and ductility (1226 MPa ultimate tensile strength and 20.8% elongation), outperforming most of conventional Ti based alloys and composites. Via the complementary in situ synchrotron X-ray diffraction and electron microscopies, it is found out that multiple micromechanisms are active, including nano-particle and dislocation localized strengthening as well as phase transformation induced plasticity. The manufacturing route developed here is versatile, capable of making high performance bio-mimic metallic composites.
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Sep 2019
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I12-JEEP: Joint Engineering, Environmental and Processing
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Abstract: In this work, three new cocrystals of the nonsteroidal anti-inflammatory drug flurbiprofen with salicylamide, benzamide and picolinamide have been discovered using thermodynamic analysis of solid-liquid binary phase diagrams, and their crystal structures have been determined from the high-resolution synchrotron powder diffraction data. Solid state DFT calculations have been carried out to gain additional insight into energy differences between the cocrystal structures. The pH-solubility behavior and solubility advantage of the cocrystals have been examined via eutectic concentrations of the components, and the thermodynamic stability relationships between different solid phases have been rationalized in terms of Gibbs energies of the formation reactions. In addition, a new model has been proposed for estimating the solubility product (Ksp) of a cocrystal, based on the experimental intrinsic solubility of the drug and coformer complemented by calculated physicochemical HYBOT descriptors. The applicability of the molecular volume of cocrystal formation as a reliable parameter for clarifying the relationship between the driving force of the cocrystallization process and the structural features of participating solids has been also discussed.
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Aug 2019
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[14465]
Abstract: Tb for Ca substituted hydroxyapatite ceramic samples with composition Ca10−xTbx(PO4)6(OH1−x/2−δ)2, where x = 0.1, 0.5, were synthesized by solid-state reaction at 1300 °C in air, and their crystal structure, vibrational spectra, luminescence, and magnetic properties were studied. Implanting Tb3+ into the calcium apatite crystal lattice results in formation of an effective TbO+ ion which displays a short terbium–oxygen bond of 2.15 Å and a stretching vibration at 534 cm−1. The Tb3+ electronic structure has been revealed by analyzing the luminescence spectra and dc/ac magnetization data. Accordingly, the ground state represents a pseudo doublet with MJ = ±6 and the first exited level is by 112 cm−1 higher in energy. The ion exhibits field induced magnetic bistability with the magnetization reversing over the first exited state. Three paths of magnetization relaxation with field-temperature controlled switching between the paths have been identified.
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Mar 2019
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I12-JEEP: Joint Engineering, Environmental and Processing
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Abstract: Controlling the final grain size in a uniform and controlled manner in powder metallurgy nickel-based superalloys is important since many mechanical properties are closely related to it. However, it has been widely documented that powder metallurgy superalloys are prone to suffer from growth of abnormally large grains (ALGs) during supersolvus heat treatment, which is harmful to in-service mechanical performance. The underlying mechanisms behind the formation of ALGs are not yet fully understood. In this research, ALGs were intentionally created using spherical indentation applied to a polycrystalline nickel-based superalloy at room temperature, establishing a deformation gradient underneath the indentation impression, which was quantitatively determined using finite element modelling, electron backscatter diffraction (EBSD) and synchrotron diffraction. Subsequent supersolvus heat treatment leads to the formation of ALGs in a narrow strain range, which also coincides with the contour of residual plastic strain in a range of about 2% to 10%. The formation mechanisms can be attributed to: (1) nucleation sites available for recrystallization are limited, (2) gradient distribution of stored energy across grain boundary. The proposed mechanisms were validated by the phase-field simulation. This research provides a deeper insight in understanding the formation of ALGs in polycrystalline nickel-based superalloy components during heat treatment, when subsurface plastic deformation caused by (mis)handling before super-solvus heat treatment occurs.
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Feb 2019
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