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

Instruments / Technical Area	Publication Details	Published
B18-Core EXAFS	Extended X-ray absorption spectroscopy using an ultrashort pulse laboratory-scale laser-plasma accelerator Brendan Kettle , Cary Colgan , Eva E. Los , Elias Gerstmayr , Matthew J. V. Streeter , Felicie Albert , Sam Astbury , Rory A. Baggott , Niall Cavanagh , Kateřina Falk , Tim Hyde , Olle Lundh , P. Pattathil Rajeev , Dave Riley , Steven J. Rose , Gianluca Sarri , Chris Spindloe , Kristoffer Svendsen , Dan R. Symes , Michal Šmíd , Alec G. R. Thomas , Chris Thornton , Robbie Watt , Stuart P. D. Mangles Communications Physics 7 DOI: 10.1038/s42005-024-01735-1 Open Access Show Abstract ▼ Abstract: Laser-driven compact particle accelerators can provide ultrashort pulses of broadband X-rays, well suited for undertaking X-ray absorption spectroscopy measurements on a femtosecond timescale. Here the Extended X-ray Absorption Fine Structure (EXAFS) features of the K-edge of a copper sample have been observed over a 250 eV window in a single shot using a laser wakefield accelerator, providing information on both the electronic and ionic structure simultaneously. This capability will allow the investigation of ultrafast processes, and in particular, probing high-energy-density matter and physics far-from-equilibrium where the sample refresh rate is slow and shot number is limited. For example, states that replicate the tremendous pressures and temperatures of planetary bodies or the conditions inside nuclear fusion reactions. Using high-power lasers to pump these samples also has the advantage of being inherently synchronised to the laser-driven X-ray probe. A perspective on the additional strengths of a laboratory-based ultrafast X-ray absorption source is presented.	Jul 2024
B18-Core EXAFS	A new application of the commercial high temperature water gas shift catalyst for reduction of CO2 emissions in the iron and steel industry: Lab-scale catalyst evaluation Liliana Lukashuk , Leon G. A. Van De Water , H. A. J. Van Dijk , Paul D. Cobden , Deborah L. Dodds , Timothy I. Hyde , Michael J. Watson International Journal Of Hydrogen Energy 114 DOI: 10.1016/j.ijhydene.2021.09.203 Diamond Proposal Number(s): [15958] Show Abstract ▼ Abstract: In this study, we present a detailed investigation of a commercial iron-based high temperature water gas shift (HTWGS) catalyst (Johnson Matthey KATALCOTM 71-6) in a new application: the production of hydrogen from blast furnace gas (BFG), which originates from iron and steel manufacturing. During the lab-scale catalytic testing under BFG conditions the catalyst demonstrated: 1) high water gas shift activity and stability; 2) minimal methanation at reduced steam to CO ratios; 3) high resistance towards H2S impurities present in the feed. The results of post-characterization of the discharged samples confirm the robustness of KATALCO 71-6 towards BFG process conditions: no over-reduction of the catalytically active Fe3O4 phase and no formation of a less active FeS phase. An in situ X-ray absorption spectroscopy study revealed no over-reduction of the iron phase under BFG conditions and the stabilization of the iron phase by diffusion of chromium into the iron oxide matrix. The findings of this study demonstrate the suitability of the iron-based HTWGS catalyst KATALCO 71-6 for the production of hydrogen from BFG streams. Knowledge gained in this study is an essential step in the development and scale up of carbon capture and storage as well as carbon capture and utilization technologies, such as the sorption enhanced water gas shift (SEWGS) technology, aimed at reducing the CO2 footprint during steel manufacturing.	Oct 2021
B18-Core EXAFS	Operando XAFS investigation on the effect of ash deposition on three-way catalyst used in Gasoline Particulate Filters and the effect of the manufacturing process on the catalytic activity Monik Panchal , June Callison , Vainius Skukauskas , Diego Gianolio , Giannantonio Cibin , Andrew P. E. York , Manfred Erwin Schuster , Timothy I. Hyde , Paul Collier , C. Richard A. Catlow , Emma K. Gibson Journal Of Physics: Condensed Matter DOI: 10.1088/1361-648X/abfe16 Diamond Proposal Number(s): [24156] Open Access Show Abstract ▼ Abstract: Platinum group metals (PGM) such as palladium and rhodium based catalysts are currently being implemented in Gasoline Particulate Filter (GPF) autoexhaust aftertreatment systems. However, little is known about how the trapped particulate matter, such as the incombustible ash, interacts with the catalyst and so may affect its performance. This operando study follows the evolution of the Pd found in two different model GPF systems: one containing ash components extracted from a GPF and another from a catalyst washcoat prior to adhesion onto the GPF. We show that the catalytic activity of the two systems vary when compared with a 0 g ash containing GPF. Compared to the 0 g ash sample the 20 g ash containing sample had a higher CO light off temperature, in addition, an oscillation profile for CO, CO2 and O2 was observed, which is speculated to be a combination of CO oxidation, C deposition via a Boudouard Reaction and further partial oxidation of the deposited species to CO. During the ageing procedure the washcoat sample reduces NO at a lower temperature than the 0 g ash sample. However, post ageing the 0 g ash sample recovers and both samples reduce NO at 310 circleC. In comparison, the 20 g ash GPF sample maintains a higher NO reduction temperature of 410 circleC post ageing, implying that the combination of high temperature ageing and presence of ash has an irreversible negative effect on catalyst performance.	May 2021
B18-Core EXAFS	Monitoring the process of formation of ZnO from ZnO2 using in situ combined XRD/XAS technique Thomas Daley , Kwasi Opuni , Edwin Raj , Andrew J. Dent , Giannantonio Cibin , Timothy I Hyde , Gopinathan Sankar Journal Of Physics: Condensed Matter DOI: 10.1088/1361-648X/abfb91 Diamond Proposal Number(s): [6966] Open Access Show Abstract ▼ Abstract: Use of in situ combined X-ray diffraction and X-ray absorption spectroscopy for the study of the thermal decomposition of zinc peroxide to zinc oxide is reported here. Comparison of data extracted from both X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) with thermo gravimetric analysis (TGA) enabled us to follow the nature of the conversion of ZnO2 to ZnO. A temperature range between 230 and 350oC appears to show a very poorly crystalline ZnO is formed prior to the formation of ordered ZnO material. Both the decrease in white line intensity in the Zn K-edge XANES and resulting lower coordination numbers estimated from analysis of Zn K-edge data of ZnO heated at 500oC, in comparison to bulk ZnO, suggest that that the ZnO produced by this method has significant defects in the system.	Apr 2021
I20-Scanning-X-ray spectroscopy (XAS/XES)	Elucidation of copper environment in a Cu-Cr-Fe oxide catalyst through in situ high-resolution XANES investigation Tahmin Lais , Liliana Lukashuk , Leon Van De Water , Tim Hyde , Matteo Aramini , Gopinathan Sankar Physical Chemistry Chemical Physics DOI: 10.1039/D0CP06468H Diamond Proposal Number(s): [18039] Open Access Show Abstract ▼ Abstract: Copper containing oxides are widely used in a range of catalytic applications. Here, we report the use of Cu K-edge high resolution XANES to determine the local site symmetry of copper ions during the thermal treatment of a Cu-Cr-Fe oxide catalyst. We exploited the Cu K-edge XANES spectral features, in particular the correlation between area under the pre-edge peak and its position to determine the local environment of Cu2+ ions. The information gained from this investigation rules out the presence of Cu2+ ions in a tetrahedral, square planar geometry, a mixture of these sites or in a reduced oxidation state. Evidence is presented that the Cu2+ ions in the Cu-Cr-Fe oxide system are present in a distorted octahedral environment.	Feb 2021
I13-2-Diamond Manchester Imaging	4D in-situ microscopy of aerosol filtration in a wall flow filter Matthew P. Jones , Malte Storm , Andrew P. E. York , Timothy I. Hyde , Gareth Hatton , Alex G. Greenaway , Sarah J. Haigh , David S. Eastwood Materials 13 DOI: 10.3390/ma13245676 Diamond Proposal Number(s): [23490] Open Access Show Abstract ▼ Abstract: The transient nature of the internal pore structure of particulate wall flow filters, caused by the continuous deposition of particulate matter, makes studying their flow and filtration characteristics challenging. In this article we present a new methodology and first experimental demonstration of time resolved in-situ synchrotron micro X-ray computed tomography (micro-CT) to study aerosol filtration. We directly imaged in 4D (3D plus time) pore scale deposits of TiO2 nanoparticles (nominal mean primary diameter of 25 nm) with a pixel resolution of 1.6 μ m. We obtained 3D tomograms at a rate of ∼1 per minute. The combined spatial and temporal resolution allows us to observe pore blocking and filling phenomena as they occur in the filter’s pore space. We quantified the reduction in filter porosity over time, from an initial porosity of 0.60 to a final porosity of 0.56 after 20 min. Furthermore, the penetration depth of particulate deposits and filtration rate was quantified. This novel image-based method offers valuable and statistically relevant insights into how the pore structure and function evolves during particulate filtration. Our data set will allow validation of simulations of automotive wall flow filters. Evolutions of this experimental design have potential for the study of a wide range of dry aerosol filters and could be directly applied to catalysed automotive wall flow filters.	Dec 2020
I15-1-X-ray Pair Distribution Function (XPDF) I20-Scanning-X-ray spectroscopy (XAS/XES)	Temperature reversible synergistic formation of cerium oxyhydride and Au hydride: a combined XAS and XPDF study Adam H. Clark , Nadia Acerbi , Philip A. Chater , Paul Collier , Shusaku Hayama , Timothy I. Hyde , Gopinathan Sankar Physical Chemistry Chemical Physics DOI: 10.1039/D0CP00455C Diamond Proposal Number(s): [15696, 16508] Open Access Show Abstract ▼ Abstract: In situ studies on the physical and chemical properties of Au in inverse ceria alumina supported catalysts have been conducted between 295 and 623 K using high energy resolved fluorescence detection X-ray absorption near edge spectroscopy and X-ray total scattering. Precise structural information is extracted on the metallic Au phase present in a 0.85 wt% Au containing inverse ceria alumina catalyst (ceria/Au/alumina). Herein evidence for the formation of an Au hydride species at elevated temperature is presented. Through modelling of total scattering data to extract the thermal properties of Au using Grüneisen theory of volumetric thermal expansion it proposed that the Au Hydride formation occurs synergistally with the formation of a cerium oxyhydride. The temperature reversible nature, whilst remaining in a reducing atmosphere, demonstatrates the activation of hydrogen without consumption of oxygen from the supporting ceria lattice.	Apr 2020
I20-Scanning-X-ray spectroscopy (XAS/XES)	The unusual redox behaviour of ceria and its interaction with hydrogen Adam H. Clark , Kevin A. Beyer , Shusaku Hayama , Timothy I. Hyde , Gopinathan Sankar Chemistry Of Materials DOI: 10.1021/acs.chemmater.9b02854 Diamond Proposal Number(s): [16508] Show Abstract ▼ Abstract: The reaction between ceria and hydrogen has been subject to numerous theoretical and experimental studies due to its importance as a catalytic material. Here we present dynamic and reversible evolution of the cerium oxidation states observed through X-ray Absorption Spectroscopy experiments in addition to the investigation of associated lattice expansion and contraction through X-ray diffraction and PDF methods. Employing a novel calculation of the temperature dependence of the Gibbs free energy through consideration of the relationship between the instantaneous thermal lattice expansion and the rate of change of the cerium oxidation state, the unusual redox chemistry is reported here. This unusual behaviour is interpreted as due to the formation of a metastable cerium oxyhydride as suggested.	Aug 2019
B18-Core EXAFS I22-Small angle scattering & Diffraction	Synthesis and characterization of platinum nanoparticle catalysts capped with isolated zinc species in SBA-15 channels: the wall effect Elizabeth Raine , Adam Clark , Glen Smales , Andrew Smith , Diego Gianolio , Tong Li , Jianwei Zheng , Benjamin Griffith , Timothy I. Hyde , Mark Feaviour , Paul Collier , John V. Hanna , Gopinathan Sankar , Shik Chi Edman Tsang Acs Applied Nano Materials DOI: 10.1021/acsanm.8b01357 Diamond Proposal Number(s): [16316, 16583] Show Abstract ▼ Abstract: The strong directing effects and difficulties in the removal of organic based surfactants makes the templated synthesis of nanoparticles in solid porous structures of defined molecular sizes such as SBA-15, without the use of surfactants, considerably attractive. However, the effects of their internal surface structures, adsorption affinities and lattice mis-match on the particle morphology grown therein have not been fully appreciated. Here, we report the internal surface of the silica preferentially hosts isolated tetrahedrally coordinated oxidic Zn species on the molecular walls of the SBA-15 channels from wet impregnated Zn2+ and Pt2+ species. This leads to less thermodynamic stable but kinetic controlled configuration of atomic zinc deposition on core platinum nanoparticles with unique confined lattice changes and surface properties to both host and guest structures at the interface upon reduction of the composite. This method for the formation templated nanoparticles may generate interests to form new tunable materials as dehydrogenation catalysts.	Nov 2018
	Reverse Monte Carlo studies of CeO2 using neutron and synchrotron radiation techniques Adam H. Clark , Huw R. Marchbank , Timothy I. Hyde , Helen Playford , Matthew G Tucker , Gopinathan Sankar Physica Scripta 92 DOI: 10.1088/1402-4896/aa547f Open Access Show Abstract ▼ Abstract: A reverse Monte Carlo analysis method was employed to extract the structure of CeO2 from Neutron total scattering (comprising both neutron diffraction (ND) and pair-distribution functions (PDF) and Ce L3- and K-edge EXAFS data. Here it is shown that there is a noticeable difference between using short ranged x-ray absorption spectroscopy data and using medium-long range PDF and ND data in regards to the disorder of the cerium atoms. This illustrates the importance of considering multiple length scales and radiation sources.	Mar 2017

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