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23 items found (0 items not approved), displaying 1 to 10.[First/Prev] 1, 2, 3 [Next/Last]

Instruments / Technical Area	Publication Details	Published
B16-Test Beamline	Synchrotron X-ray diffraction and radiography - Lattice strain characterization in thin-walled carbon fibre channel structures subjected to buckling Pawel Czapski , Jiraphant Srisuriyachot , Filip Kazmierczyk , Tomasz Waś , Patryk Jakubczak , Igor P. Dolbnya , Jarosław Bieniaś , Alexander J. G. Lunt Carbon 215 DOI: 10.1016/j.carbon.2023.118429 Diamond Proposal Number(s): [28395] Open Access Show Abstract ▼ Abstract: Carbon fibre composites are widely used in low specific stiffness and high strength structures such as airframes. Compressive loading of these assemblies can lead to buckling and localised deformation around defects and imperfections that can hinder performance and lead to overengineering via excessive safety factors. Synchrotron X-Ray Diffraction (SXRD) has recently been shown to be capable of performing lattice strain mapping within carbon fibre composites at the microscale, a previously unprecedented resolution. In this study SXRD and radiography was performed on carbon fibre composite columns produced via two different methods (standard lamination and half square) at a range of different load states: unbuckled, one-third of the buckling load and post buckling. The results provide quantitative insights into the impact of these different production methods on lattice strain and fibre orientation, as well as the influence these factors have on reducing buckling load (by up to 22%). As well as being the first use of SXRD on industrially representative full-size carbon fibre samples, these insights provide invaluable detail into the factors which limit performance and the origins of column failure; crucial factors required to optimise structural design, production and loading capability.	Nov 2023
	In situ observation of crystal reorientation in polygranular graphite by synchrotron X-ray diffraction and neutron imaging Thomas Zillhardt , Genoveva Burca , Wolfgang Ludwig , Dong Liu , T. James Marrow Carbon 966 DOI: 10.1016/j.carbon.2023.118378 Open Access Show Abstract ▼ Abstract: The capacity of polygranular graphite to accommodate strain is important to its use within structural components. This study has used in situ neutron and synchrotron X-ray experiments to demonstrate that reorientation of crystal domains accompanies the accommodation of applied mechanical strain in unirradiated Gilsocarbon (GCMB/IM24) graphite. Orientation changes were observed using 3D X-ray Diffraction, and local changes in neutron scattering were also observed with energy-resolved Bragg-edge neutron imaging. In both cases, this behaviour at the crystal level was partially recovered when the load was removed. This study provides new evidence for crystal deformation mechanisms that contribute to polycrystalline graphite's elastic non-linearity and the development of permanent set, which may also explain the effects of fast neutron irradiation on graphite elastic behaviour.	Aug 2023
B18-Core EXAFS	Single‐atom Pt on carbon nanotubes for selective electrocatalysis Samuel S. Hardisty , Xiaoqian Lin , Anthony R. J. Kucernak , David Zitoun Carbon Energy 12 DOI: 10.1002/cey2.409 Open Access Show Abstract ▼ Abstract: Utilizing supported single atoms as catalysts presents an opportunity to reduce the usage of critical raw materials such as platinum, which are essential for electrochemical reactions such as hydrogen oxidation reaction (HOR). Herein, we describe the synthesis of a Pt single electrocatalyst inside single-walled carbon nanotubes (SWCNTs) via a redox reaction. Characterizations via electron microscopy, X-ray photoelectron microscopy, and X-ray absorption spectroscopy show the single-atom nature of the Pt. The electrochemical behavior of the sample to hydrogen and oxygen was investigated using the advanced floating electrode technique, which minimizes mass transport limitations and gives a thorough insight into the activity of the electrocatalyst. The single-atom samples showed higher HOR activity than state-of-the-art 30% Pt/C while almost no oxygen reduction reaction activity in the proton exchange membrane fuel cell operating range. The selective activity toward HOR arose as the main fingerprint of the catalyst confinement in the SWCNTs.	Aug 2023
	Do specific ion effects influence the physical chemistry of aqueous graphene-based supercapacitors? Perspectives from multiscale QMMD simulations Joshua D. Elliott , Mara Chiricotto , Alessandro Troisi , Paola Carbone Carbon 113 DOI: 10.1016/j.carbon.2023.03.019 Open Access Show Abstract ▼ Abstract: Whether or not specific ion effects determine the charge storage properties of aqueous graphene and graphite-based supercapacitors remains a highly debated topic. In this work we present a multiscale quantum mechanics – classical molecular dynamics (QMMD) investigation of aqueous mono- and divalent salt electrolytes in contact with fully polarizable charged graphene sheets. By computing both the electrochemical double layer (EDL) and quantum capacitance we observe a constant electrode specific capacitance with cationic radii and charge. Counterintuitively, we determine that a switch in the cation adsorption mechanism from inner to outer Helmholtz layers leads to negligible changes to the EDL capacitance, this appears to be due to the robust electronic structure of the graphene electrodes. However, the ability of ions (such as K+) with a relatively low hydration free energy to penetrate the inner Helmholtz plane and adsorb directly on the electrode surface is found to slow their diffusion parallel to the interface. Ions in the outer Helmholtz layer are found to have higher diffusivity at the surface due to their position in ion channels between water layers. Our results show that surface effects such as the surface polarization and the partial dehydration and local structuring of ions on the surface underpin the behaviour of cations at the interface and add a vital new perspective on trends in ion mobilities seen under confinement.	Mar 2023
I20-Scanning-X-ray spectroscopy (XAS/XES)	Use of copper carbonate as corrosion inhibitor for carbon steel in post combustion carbon capture Epameinondas Skountzos , Cameron A. Price , Mustafa M. Alsalem , Samuel G. Booth , Simone Polastri , Serena A. Cussen , Christopher Parlett , Kyra Sedransk Campbell Carbon Capture Science & Technology 31 DOI: 10.1016/j.ccst.2022.100095 Diamond Proposal Number(s): [25542] Open Access Show Abstract ▼ Abstract: The realisation of post-combustion CO2 capture (PCCC) at industrial scale remains limited; one challenge is the concerns around capital costs and another concern is corrosion of the system itself. Corrosion resistance and mitigation against the amine solvent monoethanolamine (MEA) was studied, using the inhibitor copper (II) carbonate basic (CC). Carbon steel (C1018) was tested in CO2 loaded, 5M aqueous MEA solution, alone and in the presence of CC, to assess the corrosivity of the solution. Immersion testing used mass loss, Fe and Cu ion concentration in solution via ICP-MS, imaging (SEM) and analytical techniques (XRD and EDX) to investigate the effect of corrosion. Generally, the use of CC improved C1018 corrosion resistance relative to C1018 alone. Even at low concentrations (0.9 mM), CC was effective in inhibiting corrosion against CO2 loaded MEA, as the observed corrosion rate was effectively zero and no dissolved Fe was detected in solution. There was no evidence of copper surface adsorption. To clarify the solution chemistry resulting in corrosion inhibition, the local chemical environment of Fe and Cu were probed by Cu and Fe K-edge X-ray Absorption Spectroscopy, respectively. The Cu K- edge HERFD-XANES spectra reveal that a Cu2+ amine complex forms, critical to understanding the structure which is promoting significant corrosion inhibition.	Dec 2022
B16-Test Beamline	Carbon fibre lattice strain mapping via microfocus synchrotron X-ray diffraction of a reinforced composite Jiraphant Srisuriyachot , Sophie A. M. Mcnair , Yang Chen , Thomas Barthelay , Rob Gray , Jean Bénézech , Igor P. Dolbnya , Richard Butler , Alexander J. G. Lunt Carbon 194 DOI: 10.1016/j.carbon.2022.08.041 Diamond Proposal Number(s): [23372] Open Access Show Abstract ▼ Abstract: Synchrotron X-ray diffraction (SXRD) strain analysis is well established for high crystalline materials such as metals and ceramics, however, previously it has not been used in Carbon Fibre Reinforced Polymer (CFRP) composites due to their complex turbostratic atomic structure. This paper will present the feasibility of using SXRD for fibre orientation and lattice strain mapping inside CFRPs. In particular, it is the first time that the radial and axial strains of carbon fibre crystal planes have been analysed and cross-validated via numerical multi-scale simulation in a two-scale manner. In order to simplify the analysis and provide comparable estimates, an UniDirectional (UD) CFRP formed into a well-established humpback bridge shape was used. The lattice strain estimates obtained from SXRD showed localised stress concentrations and effectively matched the numerical results obtained by modelling. The mean absolute percentage differences between the two were 25.80% and 28.50% in the radial and axial directions, respectively. Differences between the two measurements are believed to originate from the non-uniform thermal history, forming geometry and tool-part interaction which leads to localised residual strains in the laminate which are unable to be fully captured by the numerical simulation performed. The carbon fibre microstructures of the inner plies adjacent to the tool were found to be significantly influenced by these factors and therefore the largest errors were observed at these locations. The approach presented has significant promise and implications for research into the micromechanics of composite materials and areas for future improvement have been outlined.	Aug 2022
B07-C-Versatile Soft X-ray beamline: Ambient Pressure XPS and NEXAFS	Plasma jet printing induced high-capacity graphite anodes for sustainable recycling of lithium-ion batteries Madhushri Bhar , Avishek Dey , Sourav Ghosh , Matthijs A. Van Spronsen , Vimalnath Selvaraj , Yalamanchili Kaliprasad , Satheesh Krishnamurthy , Surendra K. Martha Carbon 183 DOI: 10.1016/j.carbon.2022.07.027 Diamond Proposal Number(s): [27982] Show Abstract ▼ Abstract: Graphite is an integral part of lithium-ion batteries (LIBs). However, due to limited resources and high production cost of the highly purified (battery grade) graphite are becoming a challenge to meet the ever-increasing demands for energy storage devices. One viable approach is to recycle the spent graphite anodes from end-of-life LIBs. Importantly, recycling of spent lithium-ion batteries (LIBs) is off utmost importance to address the global challenge of electronic waste management. Herein, we present an environment friendly technique of graphite recycling from the spent LIB by water leaching, followed by atmospheric plasma jet printing. The major advantage of this method is that it does not require any binders or conductive diluents. Plasma printed recycled graphite showed significantly enhanced specific capacity of 402 mAh g−1 at 500 mA g−1 at the end of the 1000th charge-discharge cycles, in comparison to with water-washed recycled graphite (112 mAh g−1) and a 23.35 times faster diffusivity of Li+. A detailed experimental investigation revealed the plasma activation of the graphitic structure resulted in the improved reversible Li+ storage. This work provides a new perspective on the recycling strategy of graphite anodes using the in-situ plasma functionalization strategy, a significant step towards the sustainable future of LIBs.	Jul 2022
I12-JEEP: Joint Engineering, Environmental and Processing	Unraveling compacted graphite evolution during solidification of cast iron using in-situ synchrotron X-ray tomography Chaoling Xu , Tim Wigger , Mohammed Azeem , Tito Andriollo , Søren Fæster , Samuel Clark , Zhixuan Gong , Robert Atwood , Jean-Claude Grivel , Jesper H. Hattel , Peter D. Lee , Niels S. Tiedje Carbon 141 DOI: 10.1016/j.carbon.2021.08.069 Diamond Proposal Number(s): [22627] Open Access Show Abstract ▼ Abstract: In spite of many years of research, the physical phenomena leading to the evolution of compacted graphite (CG) during solidification is still not fully understood. In particular, it is unknown how highly branched CG aggregates form and evolve in the semi-solid, and how local microstructural variations at micrometer length scale affect this growth process. We present here the first time-resolved synchrotron tomography combined with a bespoke high-temperature environmental cell that allows direct observation of the evolution of CG and relates this dynamic process to the local surrounding microstructures in a cast iron sample during repeated melting and solidification. Distinct processes are identified for the formation of CG involving the nucleation, growth, development of branches and interconnection of graphite particles, ultimately evolving into highly branched graphite aggregates with large sizes and low sphericities. CG is found to nucleate with a spheroidal or a plate-like shape, developing branches induced by high carbon concentration, e.g. thin melt channels. Additionally, CG grows much faster than spheroidal graphite during subsequent cooling in solid state. The direct visualization of the dynamic solidification process provides unprecedented new insights into formation mechanisms of CG and correlating factors such as local microstructural variations, and guides the development of CG iron solidification models.	Sep 2021
I22-Small angle scattering & Diffraction	Ordered mesoporous carbons with body centred cubic pore structure F. Sakina , R. T. Baker Carbon Trends 4 DOI: 10.1016/j.cartre.2021.100051 Open Access Show Abstract ▼ Abstract: The preparation of mesoporous carbons possessing a highly ordered body centred cubic (bcc) arrangement of pores by employing a halide- and metal-free synthesis method is reported. Products were characterised using gas physisorption, Small Angle X-ray Diffraction and X-ray Scattering, Raman spectroscopy and High Resolution Transmission Electron Microscopy (TEM). The materials produced in this work had Specific Surface Areas of between 422 and 988 m2g−1 and pore diameters of around 7 nm. From the TEM images, high quality Digital Diffraction Patterns, relating to the ordered mesopore structure, were obtained. On increasing calcination temperature from 350 to 1000°C the bcc structure was retained but its dimensions decreased progressively as the mesopore structure shrank. The effects on the structure and texture of the materials of the three key parameters of polymerisation time and the concentrations of the two catalysts employed, NH4OH and oxalic acid, were studied. Shorter polymerisation times and lower catalyst concentrations gave rise to the most well-ordered products whereas longer polymerisation times with higher concentrations of base and acid catalyst resulted in disordered pore structures.	Jul 2021
I13-2-Diamond Manchester Imaging	Assessment of the fracture toughness of neutron-irradiated nuclear graphite by 3D analysis of the crack displacement field Xiaochao Jin , James Wade-Zhu , Yang Chen , Paul M. Mummery , Xueling Fan , T. James Marrow Carbon 171, 882 - 893 DOI: 10.1016/j.carbon.2020.09.072 Diamond Proposal Number(s): [16668] Show Abstract ▼ Abstract: Digital volume correlation of in situ synchrotron X-ray computed tomographs has been used to measure the three-dimensional displacement fields around quasi-static propagating cracks in neutron irradiated and unirradiated graphite in specimens of the double cleavage drilled compression geometry. The crack tip location and crack opening were extracted from the displacement fields using a phase congruency edge detection method as cracks were propagated over ∼5 mm. The cracks propagated in mode I, maintaining a constant crack opening angle that was ∼50% smaller for the irradiated graphite. 3D finite element simulations, using the measured full field displacements as boundary conditions, obtained the critical elastic strain energy release rate for crack propagation by calculation of the domain contour J-integral. When the non-linear properties of unirradiated graphite were considered, the strain energy release rate for propagation was constant (180 ± 22 Jm-2) with increasing crack length. The irradiated graphite (fluence of 19.7 × 1020 neutrons cm−2 or 2.6 dpa, 4% weight loss by radiolytic oxidation) had linear elastic properties, and the strain energy release rate for propagation increased linearly from 118 ± 12Jm-2 to 485 ± 75 Jm-2 with crack length.	Oct 2020

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