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Instruments / Technical Area	Publication Details	Published
I13-2-Diamond Manchester Imaging	Tracking lithium penetration in solid electrolytes in 3D by in-situ synchrotron X-ray computed tomography Shuai Hao , Sohrab R. Daemi , Thomas M. M. Heenan , Wenjia Du , Chun Tan , Malte Storm , Christoph Rau , Dan J. I. Brett , Paul R. Shearing Nano Energy 82 DOI: 10.1016/j.nanoen.2021.105744 Diamond Proposal Number(s): [22198] Show Abstract ▼ Abstract: Solid state batteries have attracted extensive attention, but the lithium penetration through the solid electrolyte remains a critical barrier to commercialisation and is not yet fully understood. In this study, the 3D morphological evolution of cracks with deposited lithium were tracked as they penetrated through the solid electrolyte during repetitive plating. This is achieved by utilising in-situ synchrotron X-ray computed tomography with high spatial and temporal resolutions. Thin-sheet cracks were observed to penetrate the solid electrolyte without immediate short-circuiting of the cell. Changes in their width and volume were quantified. By calculating the volume of deposited lithium, it was found that the lithium was only partially filled in cracks, and its filling ratio quickly dropped from 94.95% after the 1st plating to ca. 20% after the 4th plating. The filling process was revealed through tracking the line profile of grayscale along cracks. It was found that lithium grew much more slowly than cracks, so that the cracks near the cathode side were largely hollow and the cell could continue to operate. The deposited lithium after short circuit was segmented and its distribution was visualised. DVC analysis was applied to map local high stress and strain, which aggregated along cracks and significantly increased at areas where new cracks formed.	Apr 2021
I13-2-Diamond Manchester Imaging	Evolution of electrochemical cell designs for in-situ and operando 3D characterization Chun Tan , Sohrab R. Daemi , Oluwadamilola O. Taiwo , Thomas M. M. Heenan , Daniel J. L. Brett , Paul Shearing Materials 11 DOI: 10.3390/ma11112157 Diamond Proposal Number(s): [11539] Open Access Show Abstract ▼ Abstract: Lithium-based rechargeable batteries such as lithium-ion (Li-ion), lithium-sulfur (Li-S), and lithium-air (Li-air) cells typically consist of heterogenous porous electrodes. In recent years, there has been growing interest in the use of in-situ and operando micro-CT to capture their physical and chemical states in 3D. The development of in-situ electrochemical cells along with recent improvements in radiation sources have expanded the capabilities of micro-CT as a technique for longitudinal studies on operating mechanisms and degradation. In this paper, we present an overview of the capabilities of the current state of technology and demonstrate novel tomography cell designs we have developed to push the envelope of spatial and temporal resolution while maintaining good electrochemical performance. A bespoke PEEK in-situ cell was developed, which enabled imaging at a voxel resolution of ca. 230 nm and permitted the identification of sub-micron features within battery electrodes. To further improve the temporal resolution, future work will explore the use of iterative reconstruction algorithms, which require fewer angular projections for a comparable reconstruction.	Nov 2018
I13-2-Diamond Manchester Imaging	Four-dimensional studies of morphology evolution in lithium-sulfur batteries Chun Tan , Thomas M. M. Heenan , Ralf F. Ziesche , Sohrab R. Daemi , Jennifer Hack , Maximilian Maier , Shashidhara Marathe , Christoph Rau , Daniel J. L. Brett , Paul R. Shearing Acs Applied Energy Materials DOI: 10.1021/acsaem.8b01148 Diamond Proposal Number(s): [16110] Open Access Show Abstract ▼ Abstract: Lithium sulfur (Li-S) batteries have great potential as a successor to Li-ion batteries but their commercialization has been complicated by a multitude of issues stemming from their complex multi-phase chemistry. In-situ X-ray tomography investigations enable direct observations to be made about a battery, providing unprecedented insight into the microstructural evolution of the sulfur cathode and shedding light on the reaction kinetics of the sulfur phase. Here, for the first time, the morphology of a sulfur cathode was visualized in 3D as a function of state of charge at high temporal and spatial resolution. Whilst elemental sulfur was originally well dispersed throughout the uncycled cathode, subsequent charging resulted in the formation of sulfur clusters along preferred orthogonal orientations in the cathode. The electrical conductivity of the cathode was found not to be rate-limiting, suggesting the need to optimize the loading of conductive carbon additives. The carbon and binder domain, and surrounding bulk pore phase were visualized in the in-situ cell, and contrast changes within both phases were successfully extracted. The applications of this technique are not limited to microstructural and morphological characterization, and the volumetric data can serve as a valuable input for true 3D computational modelling of Li-S batteries.	Aug 2018

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