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Instruments / Technical Area	Publication Details	Published
I14-Hard X-ray Nanoprobe	Identifying the origins of microstructural defects such as cracking within Ni‐rich NMC811 cathode particles for lithium‐ion batteries Thomas M. M. Heenan , Aaron Wade , Chun Tan , Julia E. Parker , Dorota Matras , Andrew S. Leach , James B. Robinson , Alice Llewellyn , Alexander Dimitrijevic , Rhodri Jervis , Paul D. Quinn , Dan J. L. Brett , Paul R. Shearing Advanced Energy Materials 1 DOI: 10.1002/aenm.202002655 Diamond Proposal Number(s): [20841, 23858] Open Access Show Abstract ▼ Abstract: The next generation of automotive lithium‐ion batteries may employ NMC811 materials; however, defective particles are of significant interest due to their links to performance loss. Here, it is demonstrated that even before operation, on average, one‐third of NMC811 particles experience some form of defect, increasing in severity near the separator interface. It is determined that defective particles can be detected and quantified using low resolution imaging, presenting a significant improvement for material statistics. Fluorescence and diffraction data reveal that the variation of Mn content within the NMC particles may correlate to crystallographic disordering, indicating that the mobility and dissolution of Mn may be a key aspect of degradation during initial cycling. This, however, does not appear to correlate with the severity of particle cracking, which when analyzed at high spatial resolutions, reveals cracking structures similar to lower Ni content NMC, suggesting that the disconnection and separation of neighboring primary particles may be due to electrochemical expansion/contraction, exacerbated by other factors such as grain orientation that are inherent in such polycrystalline materials. These findings can guide research directions toward mitigating degradation at each respective length‐scale: electrode sheets, secondary and primary particles, and individual crystals, ultimately leading to improved automotive ranges and lifetimes.	Nov 2020
I11-High Resolution Powder Diffraction	Using in-situ laboratory and synchrotron-based X-ray diffraction for lithium-ion batteries characterization: a review on recent developments Alice Llewellyn , Alessia Matruglio , Dan J. L. Brett , Rhodri Jervis , Paul R. Shearing Condensed Matter 5 DOI: 10.3390/condmat5040075 Open Access Show Abstract ▼ Abstract: Renewable technologies, and in particular the electric vehicle revolution, have generated tremendous pressure for the improvement of lithium ion battery performance. To meet the increasingly high market demand, challenges include improving the energy density, extending cycle life and enhancing safety. In order to address these issues, a deep understanding of both the physical and chemical changes of battery materials under working conditions is crucial for linking degradation processes to their origins in material properties and their electrochemical signatures. In situ and operando synchrotron-based X-ray techniques provide powerful tools for battery materials research, allowing a deep understanding of structural evolution, redox processes and transport properties during cycling. In this review, in situ synchrotron-based X-ray diffraction methods are discussed in detail with an emphasis on recent advancements in improving the spatial and temporal resolution. The experimental approaches reviewed here include cell designs and materials, as well as beamline experimental setup details. Finally, future challenges and opportunities for battery technologies are discussed.	Nov 2020
I12-JEEP: Joint Engineering, Environmental and Processing	Identifying the Cause of Rupture of Li-Ion Batteries during Thermal Runaway 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 Advanced Science 5 DOI: 10.1002/advs.201700369 Diamond Proposal Number(s): [13884] Open Access Show Abstract ▼ 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.	Oct 2017
I12-JEEP: Joint Engineering, Environmental and Processing	A novel molten-salt electrochemical cell for investigating the reduction of uranium dioxide to uranium metal by lithium using in situ synchrotron radiation Leon Brown , Rema Abdulaziz , Rhodri Jervis , Vidal Bharath , Thomas J. Mason , Robert C. Atwood , Christina Reinhard , Leigh Connor , Douglas Inman , Daniel J. L. Brett , Paul R. Shearing Journal Of Synchrotron Radiation 24 DOI: 10.1107/S1600577517000625 Diamond Proposal Number(s): [9690] Show Abstract ▼ Abstract: A novel electrochemical cell has been designed and built to allow for in situ energy-dispersive X-ray diffraction measurements to be made during reduction of UO2 to U metal in LiCl–KCl at 500°C. The electrochemical cell contains a recessed well at the bottom of the cell into which the working electrode sits, reducing the beam path for the X-rays through the molten-salt and maximizing the signal-to-noise ratio from the sample. Lithium metal was electrodeposited onto the UO2 working electrode by exposing the working electrode to more negative potentials than the Li deposition potential of the LiCl–KCl eutectic electrolyte. The Li metal acts as a reducing agent for the chemical reduction of UO2 to U, which appears to proceed to completion. All phases were fitted using Le Bail refinement. The cell is expected to be widely applicable to many studies involving molten-salt systems.	Mar 2017
I12-JEEP: Joint Engineering, Environmental and Processing	Characterising thermal runaway within lithium-ion cells by inducing and monitoring internal short circuits 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 Energy Environ. Sci. 5 DOI: 10.1039/C7EE00385D Diamond Proposal Number(s): [13884] Show Abstract ▼ 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.	Mar 2017
I12-JEEP: Joint Engineering, Environmental and Processing	Following the electroreduction of uranium dioxide to uranium in LiClKCl eutectic in situ using synchrotron radiation L D Brown , Rema Abdulaziz , Rhodri Jervis , Vidal Bharath , R C Attwood , Christina Reinhard , Leigh Connor , S J R Simons , D. Inman , D J L Brett , Paul Shearing Journal Of Nuclear Materials 464, 256 - 262 DOI: 10.1016/j.jnucmat.2015.04.037 Diamond Proposal Number(s): [9690] Open Access Show Abstract ▼ Abstract: The electrochemical reduction of uranium dioxide to metallic uranium has been investigated in lithium chloridepotassium chloride eutectic molten salt. Laboratory based electrochemical studies have been coupled with in situ energy dispersive X-ray diffraction, for the first time, to deduce the reduction pathway. No intermediate phases were identified using the X-ray diffraction before, during or after electroreduction to form α-uranium. This suggests that the electrochemical reduction occurs via a single, 4-electron-step, process. The rate of formation of α-uranium is seen to decrease during electrolysis and could be a result of a build-up of oxygen anions in the molten salt. Slow transport of O2− ions away from the UO2 working electrode could impede the electrochemical reduction.	Sep 2015
I12-JEEP: Joint Engineering, Environmental and Processing	Investigating the effect of thermal gradients on stress in solid oxide fuel cell anodes using combined synchrotron radiation and thermal imaging James Robinson , Leon D. Brown , Rhodri Jervis , Oluwadamilola Taiwo , Thomas M.m. Heenan , Jason Millichamp , Thomas J. Mason , Tobias P. Neville , Ralph Clague , David Eastwood , Christina Reinhard , P.d Lee , Daniel J.l. Brett , Paul R. Shearing Journal Of Power Sources 288, 473 - 481 DOI: 10.1016/j.jpowsour.2015.04.104 Diamond Proposal Number(s): [8612] Open Access Show Abstract ▼ Abstract: Thermal gradients can arise within solid oxide fuel cells (SOFCs) due to start-up and shut-down, non-uniform gas distribution, fast cycling and operation under internal reforming conditions. Here, the effects of operationally relevant thermal gradients on Ni/YSZ SOFC anode half cells are investigated using combined synchrotron X-ray diffraction and thermal imaging. The combination of these techniques has identified significant deviation from linear thermal expansion behaviour in a sample exposed to a one dimensional thermal gradient. Stress gradients are identified along isothermal regions due to the presence of a proximate thermal gradient, with tensile stress deviations of up to 75 MPa being observed across the sample at a constant temperature. Significant strain is also observed due to the presence of thermal gradients when compared to work carried out at isothermal conditions.	Aug 2015
I12-JEEP: Joint Engineering, Environmental and Processing	A novel high-temperature furnace for combined in situ synchrotron X-ray diffraction and infrared thermal imaging to investigate the effects of thermal gradients upon the structure of ceramic materials James Robinson , Leon Brown , Rhodri Jervis , Oluwadamilola Taiwo , Jason Millichamp , Thomas J. Mason , Tobias P. Neville , David S. Eastwood , Christina Reinhard , Peter Lee , Daniel J. L. Brett , Paul Shearing Journal Of Synchrotron Radiation 21, 1134 - 1139 DOI: 10.1107/S1600577514014209 PMID: 25178003 Diamond Proposal Number(s): [8612] Open Access Show Abstract ▼ Abstract: A new technique combining in situ X-ray diffraction using synchrotron radiation and infrared thermal imaging is reported. The technique enables the application, generation and measurement of significant thermal gradients, and furthermore allows the direct spatial correlation of thermal and crystallographic measurements. The design and implementation of a novel furnace enabling the simultaneous thermal and X-ray measurements is described. The technique is expected to have wide applicability in material science and engineering; here it has been applied to the study of solid oxide fuel cells at high temperature.	Sep 2014
I11-High Resolution Powder Diffraction	Hydrogen Oxidation on PdIr/C Catalysts in Alkaline Media Rhodri Jervis , Noramalina Mansor , Christopher Gibbs , Claire Murray , Chiu Tang , Paul Shearing , Dan J.l. Brett Journal Of The Electrochemical Society 161 (4), F458 - F463 DOI: 10.1149/2.037404jes Show Abstract ▼ Abstract: A novel PdIr/C supported alloy nanoparticle catalyst has been developed for use in the hydrogen oxidation reaction (HOR) at the anode of an Alkaline Anion Exchange Membrane (AAEM) fuel cell. The catalyst has been characterized using Transmission Electron Microscopy (TEM), Energy Dispersive X-ray Spectroscopy (EDX) and Synchrotron X-ray Powder Diffraction (SXPD). Electrochemical testing suggests it has a comparable activity for HOR as Pt/C and is a good candidate for use on the anode of an AAEM fuel cell.	Jan 2014
I11-High Resolution Powder Diffraction	Novel PdIr/C Catalysts for the Hydrogen Oxidation Reaction in Alkaline Media Rhodri Jervis , N. Mansor , C. Gibbs , Claire Murray , Chiu Tang , D. J. L. Brett Ecs Transactions 58 (1), 637 - 650 DOI: 10.1149/05801.0637ecst Show Abstract ▼ Abstract: A novel PdIr/C supported alloy nanoparticle catalyst has been developed for use in the hydrogen oxidation reaction (HOR) at the anode of an Alkaline Anion Exchange Membrane (AAEM) fuel cell. The catalyst has been characterised using Transmission Electron Microscopy (TEM), Energy Dispersive X-ray Spectroscopy (EDX) and Synchrotron X-ray Powder Diffraction (SXPD). Electrochemical testing suggests it has a comparable activity for HOR as Pt/C and is a good candidate for use on the anode of an AAEM fuel cell.	Oct 2013

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