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Condens. Matter 2020, 5, 75 18 of 28 Again on the ID15A beamline at the European Synchrotron (ESRF, Grenoble, France), Liu and co-authors resolved and quantified the reaction heterogeneity within a whole LiFePO4 (LFP) electrode using the XRD-CT technique [108]. Figure 13 shows the dominant reaction heterogeneity as a function of depth within the electrode (upper part); the bottom part shows the maximum heterogeneity, Condens. Matter 2020, 5, x 19 of 30 as characterized by the standard deviation at any time during charge. Figure 13. XRD-CT voltage profile of a whole LFP electrode cycled at C/10 during operando XRD-CT Figure 13. XRD-CT voltage profile of a whole LFP electrode cycled at C/10 during operando XRD-CT (red curve); the bottom image shows the LFP phase fraction, i.e., the Li composition, map of different (red curve); the bottom image shows the LFP phase fraction, i.e., the Li composition, map of different horizontal layers across the electrode during cycling [108]. horizontal layers across the electrode during cycling [108]. An important contribution in the field was given by Roué’s group, who used synchrotron XRD-CT An important contribution in the field was given by Roué’s group, who used synchrotron XRD- on the Psiché beamline at Soleil Synchrotron (Gif-sur-Yvette, France) to study the morphological CT on the Psiché beamline at Soleil Synchrotron (Gif-sur-Yvette, France) to study the morphological changes in Si-based anodes induced by cycling at different stages of the 1st and the 10th cycles [109]. changes in Si-based anodes induced by cycling at different stages of the 1st and the 10th cycles [109]. The analysed electrode was composed of nanocrystalline/amorphous Si particles and a porous carbon The analysed electrode was composed of nanocrystalline/amorphous Si particles and a porous carbon paper as current collector and graphene nanoplatelets as conductive additive. They used a SwagelokTM paper as current collector and graphene nanoplatelets as conductive additive. They used a cell made of PFA polymer with a thin wall (2.5 mm-thick) near the electrode to obtain low X-ray SwagelokTM cell made of PFA polymer with a thin wall (2.5 mm-thick) near the electrode to obtain attenuation. Figure 14a shows the evolution of the electrode potential along the 1st and 10th cycles low X-ray attenuation. Figure 14a shows the evolution of the electrode potential along the 1st and performed during the in-situ XRD-CT experiments (left) and the corresponding colour map XRD 10th cycles performed during the in-situ XRD-CT experiments (left) and the corresponding colour peak intensity upon charging (right). The CT images at different stages of cycling were obtained on map XRD peak intensity upon charging (right). The CT images at different stages of cycling were representativeareasof280×280μM2andareshow2ninFigure14b.TheSiparticles,visibleinwhite obtained on representative areas of 280 × 280 μM and are shown in Figure 14b. The Si particles, at the pristine state, are traced in order to track their lithiation/delithiation upon cycling. The same visible in white at the pristine state, are traced in order to track their lithiation/delithiation upon cell configuration used in this study was adopted by the same group to analyse the microstructure cycling. The same cell configuration used in this study was adopted by the same group to analyse the evolution of a sulfur-based cathodes in Li-S batteries with the same techniques. A schematic diagram microstructure evolution of a sulfur-based cathodes in Li-S batteries with the same techniques. A of the used SwagelokTM cell is shown in FiTgMure 14c, with an inset showing the zoom of the central part schematic diagram of the used Swagelok cell is shown in Figure 14c, with an inset showing the czonotmainoifntghethcenetleracltrpoadretsco[1n1t0a]i.ning the electrodes [110].PDF Image | Synchrotron-Based X-ray Diffraction for Lithium-Ion Batteries
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