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fixed with a polyethylene foil heated at high temperature (453 K) [47], allowing a more uniform stack pressure with respect to polymer films [48]. Standard pouch cells without modification can also be used in combination with synchrotron-based high-energy X-rays in transmission geometry: high- energy photons are able to fully penetrate the cell, obtaining a 2D diffraction patterns under more realistic conditions with respect to those obtained using a custom cell [49,50]. An alternative Condens. Matter 2020, 5, 75 6 of 28 configuration is given by Argonne’s multipurpose in situ X-ray (AMPIX) cell, shown in Figure 3c and characterized by a cup-shaped body, two X-ray transparent windows and a flat annular gasket which is sandwiched between the electrodes to contain the battery stack [51]. SwagelokTM tyTpMe cells are also is sandwiched between the electrodes to contain the battery stack [51]. Swagelok type cells are widely used, which are commercially available and composed of stainless steel caps and a Teflon also widely used, which are commercially available and composed of stainless steel caps and a Teflon body [52]. An example of one SwagelokTM type cell is shown in Figure 3d. Also, largely used are cells body [52]. An example of one SwagelokTM type cell is shown in Figure 3d. Also, largely used are cells inspired by SwagelokTM characterized by the positive electrode, separator (soaked with electrolyte), inspired by SwagelokTM characterized by the positive electrode, separator (soaked with electrolyte), and the negative electrode stacked layer by layer in between two Be windows and a stainless steel and the negative electrode stacked layer by layer in between two Be windows and a stainless steel cylindrical plunger [53]. This configuration allows both transmission and reflection analysis, and an cylindrical plunger [53]. This configuration allows both transmission and reflection analysis, and an example can be observed in Figure 3e. Finally, a radially accessible tubular in-situ X-ray (RATIX) cell example can be observed in Figure 3e. Finally, a radially accessible tubular in-situ X-ray (RATIX) cell is is commonly used for transmission XRD and is composed of the electrode stack, a containment tube, commonly used for transmission XRD and is composed of the electrode stack, a containment tube, two electrode pins, a tensioning screw, a base and a top assembly, and alignment pins [54]. An two electrode pins, a tensioning screw, a base and a top assembly, and alignment pins [54]. An example example is shown in Figure 3f. is shown in Figure 3f. Figure 3. Designs of the most common used types of in-situ XRD cells: (a) modified coin cell, with photo Figure 3. designs of the most common used types of in-situ XRD cells: (a) modified coin cell, with (on the left) of the cell mounted on the sample holder on the powder diffraction beamline at the Australian photo (on the left) of the cell mounted on the sample holder on the powder diffraction beamline at Synchrotron [13]; (b) modified pouch cell with a Kapton film window [46]; (c) example of AMPIX the Australian Synchrotron [13]; (b) modified pouch cell with a Kapton film window [46]; (c) example cell from reference [51], reproduced with permission of the International Union of Crystallography; of AMPIX cell from reference [51], reproduced with permission of the International Union of (d) schematic of a SwagelokTM type cells [55]; (e) photo (left) and design (right) of the SwagelokTM type Crystallography; (d) schematic of a SwagelokTM type cells [55]; (e) photo (left) and design (right) of cell described in [53]. The parts A, B and C compose the cylindrical plunger; (f) Schematic diagrams of the SwagelokTM type cell described in [53]. The parts A, B and C compose the cylindrical plunger; (f) a RATIX cell (left and middle images), with a cross section view (right image) [54], reproduced with Schematic diagrams of a RATIX cell (left and middle images), with a cross section view (right image) permission of the International Union of Crystallography. [54], reproduced with permission of the International Union of Crystallography. 3. Laboratory Diffractometer vs. Synchrotron XRD 3. Laboratory Diffractometer vs. Synchrotron XRD Laboratory diffractometers are largely used for in situ XRD battery analysis because of their Laboratory diffractometers are largely used for in situ XRD battery analysis because of their availability, ease of access and affordability. They typically make use of a copper X-ray source, which is availability, ease of access and affordability. They typically make use of a copper X-ray source, which generally not penetrative enough for in situ studies [56]. Harder X-rays are therefore favorable, which led to the adoption of molybdenum or silver sources for their better penetrative powers. Reeves-McLaren et al. used a laboratory diffractometer to confirm the existence of the solid solution mechanism in LiFePO4 [56]. A silver source was used, coupled with a PANalytical Empyrean GaliPIX detector suitable for hard radiation. Each diffraction pattern took 8 min to acquire, which, whilst much slower than synchrotron equivalents (ca. 10 s acquisition time) showed the improvements in performing lab-based operando studies in close to real time. Patterns were obtained continuously whilst the battery was charged at a C-rate of C/10. Variables such as the C-rate can be chosen to allow for data acquisition to be performed at multiple points throughout the cycle, at a time scale appropriate for the acquisition. For example, with an acquisition time of 8 min, a C-rate of C/2 would give 15 data points along the charge curve. The cell used in this study was a modified coin cell with a 10 mm Kapton window.PDF Image | Synchrotron-Based X-ray Diffraction for Lithium-Ion Batteries
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