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Condens. Matter 2020, 5, 75 19 of 28 Condens. Matter 2020, 5, x 20 of 30 FiguFreig1u4re. 1(a4). (dai)sdchisacrhgaerg/ceh/cahragregecucurvrveess((lleefft) and respeecctitviveecocloluorumr ampaXpRXDRrDelarteldatteodsteopste1p–2s41–24 (right); (b) lateral CT images at z ~5, 50 and 100 μM for different stages of cycling. The numbers 1−24 (right); (b) lateral CT images at z ~5, 50 and 100 μM for different stages of cycling. The numbers 1–24 correspond to those indicated on the discharge/charge curves in (a); (c) schematic diagram of the used correspond to those indicated on the discharge/charge curves in (a); (c) schematic diagram of the used in-situ cell. Reprinted (adapted) with permission from [110]. in-situ cell. Reprinted (adapted) with permission from [110]. The spatial sensitivity afforded to XRD when using a pencil beam makes it an excellent tool for The spatial sensitivity afforded to XRD when using a pencil beam makes it an excellent tool for studying heterogeneities within the material during cycling. Finegan et al. applied point XRD to studying heterogeneities within the material during cycling. Finegan et al. applied point XRD to study study lithium dynamics within a graphite electrode during cycling in order to quantify lithium lithium dynamics within a graphite electrode during cycling in order to quantify lithium plating [111]. plating [111]. The tendency for lithium plating to occur under stressful operating conditions (such as The tendency for lithium plating to occur under stressful operating conditions (such as accelerated accelerated C-rates and low temperatures) is hindering the application of fast charging of lithium ion C-rates and low temperatures) is hindering the application of fast charging of lithium ion batteries. batteries. This work was carried out at the ID15A beamline at ESRF and made use of the extremely This work was carried out at the ID15A beamline at ESRF and made use of the extremely quick high quick high resolution (0.5 s) which is essential for fast C-rates. A modified coin cell architecture was resolaudtoiopnte(d0.f5ors)thwisheixcpheirsimesesnetn(Ftiaglufroer1f5a),stneCg-artaitnegs.anAymcoondceifirnesdthcoatinbecsepllokaercohpieteracntudroecwelalsgaidveopritsed for thisetoxpuenruimsueanltre(Fsuigltusrdeu1e5)to,ntehgeacteinllgdaesniygnc.oSnicgenrifnicsatnhtaltitbheiuspmokcoenocpenetrantidonocgeralldsiegnivtsewriesreetfooundusual throughout the depth of the electrode during cycling, and a description of lithium plating was results due to the cell design. Significant lithium concentration gradients were found throughout the developed; results can be seen in Figure 15. depth of the electrode during cycling, and a description of lithium plating was developed; results can Condens. Matter 2020, 5, x 21 of 30 be seen in Figure 15. Figure 15. Modified coin cell used in the XRD-CT experiment (left); 3D plot showing LiC6 value as Figure 15. modified coin cell used in the XRD-CT experiment (left); 3D plot showing LiC6 value as a a function of time and depth during 6C charge and 2C charge [111], published by The Royal Society function of time and depth during 6C charge and 2C charge [111], published by The Royal Society of of Chemistry. Chemistry. 7. XRD and Pair Distribution Function While XRD covers only Bragg scattering and provides long-range average structural information, PDF analysis utilizes the total scattering (Bragg and diffuse scattering) to investigate materials with short-range ordering. PDF can provide local information on the atomic pair distribution relating to chemical, structural, and morphological transformations that occur duringPDF Image | Synchrotron-Based X-ray Diffraction for Lithium-Ion Batteries
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