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Condens. Matter 2020, 5, 75 17 of 28 Taking advantage of XRD-CT’s ability to spatially resolve phenomena is the work performed by Daemi et al. which analyzed the change in unit cell parameters upon cycling, allowing for heterogeneities within the cell to be studied at multiple scale lengths, from particle to electrode [106]. A multiscale approach is necessary in order to understand the phenomena at all levels and how they materialize into full-cell degradation. The pencil beam used for XRD-CT also leads to high spatial resolution in point diffraction experiments when rastering through the thickness of the electrode. Recently, Finegan et al. performed Condens. Matter 2020, 5, x 18 of 30 the first high-speed XRD-CT to probe, in 3D, crystallographic heterogeneities within a graphite-Si composite electrode with a spatial resolution of 1 μM. The experiment was performed on the ID15A beamline at the European Synchrotron (ESRF, Grenoble, France) [107]. They proposed an in-house beamline at the European Synchrotron (ESRF, Grenoble, France) [107]. They proposed an in-house design design microcell consisting of a perfluoroalkoxy alkane (PFA) Swagelok union fitting and a bespoke microcell consisting of a perfluoroalkoxy alkane (PFA) Swagelok union fitting and a bespoke polyether polyether ether ketone body which housed the battery. They were able to analyse the local charge- ether ketone body which housed the battery. They were able to analyse the local charge-transfer transfer mechanism within and between individual particles, observing charge balancing kinetics mechanism within and between individual particles, observing charge balancing kinetics between the between the graphite and Si during the minutes following the transition from operation to open graphite and Si during the minutes following the transition from operation to open circuit. Moreover, circuit. Moreover, subparticle lithiation heterogeneities in both Si and graphite with their respective subparticle lithiation heterogeneities in both Si and graphite with their respective diffraction patterns diffraction patterns have been characterized with spatial resolution. Figure 12 presents a XRD-CT have been characterized with spatial resolution. Figure 12 presents a XRD-CT slice taken at the slice taken at the beginning of the charge step, with magnified regions of interest (left images); the beginning of the charge step, with magnified regions of interest (left images); the XRD patterns from XRD patterns from segmented lithium silicide shells and Si cores are shown on the right. The inset segmented lithium silicide shells and Si cores are shown on the right. The inset shows a picture of shows a picture of the used cell. Using the same cell type, techniques, and beamline, the group was the used cell. Using the same cell type, techniques, and beamline, the group was able to obtain the able to obtain the spatial and temporal quantification of crystallographic heterogeneities within and spatial and temporal quantification of crystallographic heterogeneities within and between particles between particles throughout both fresh and degraded LixMn2O4 electrodes during cycling [104]. A throughoutbothfreshanddegradedLixMnO electrodesduringcycling[104].Asimilardesignwas 24 similar design was previously adopted by Tan and co-workers for in-situ and operando micro-CT previously adopted by Tan and co-workers for in-situ and operando micro-CT studies to quantify studies to quantify microstructure evolution of NMC and Li-sulfur electrode and analyse the microstructure evolution of NMC and Li-sulfur electrode and analyse the degradation [35]. degradation [35]. Figure 12. XRD-CT of graphite-silicon composite electrode with phase-distribution map (upper-left Figure 12. XRD-CT of graphite-silicon composite electrode with phase-distribution map (upper-left image), with magnified regions of interests (bottom-left). On the right, the XRD pattern from segmented image), with magnified regions of interests (bottom-left). On the right, the XRD pattern from lithium silicide shells and Si cores. Adapted with permission from [107], copyright 2019 American segmented lithium silicide shells and Si cores. Adapted with permission from [107], copyright 2019 Chemical Society. American Chemical Society. 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, as characterized by the standard deviation at any time during charge.PDF Image | Synchrotron-Based X-ray Diffraction for Lithium-Ion Batteries
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