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3. Results and Discussion In order to observe the inner structure of the fresh and aged cells, Compton scattered X-ray intensities were measured by scanning incident X-rays from the outer casing to the center of the cell Condens. Matter 2019, 4, 66 4 of 8 following a procedure similar to that described by Suzuki et al. [9]. Figure 2 shows the corresponding results. Figure 2a,b shows the results of the fresh and aged cells, respectively. The open circuit voltage (OCV) of the discharged and charged states of the fresh and aged cells was 2.628 V, 4.193 V, 2.677 V, (OCV) of the discharged and charged states of the fresh and aged cells was 2.628 V, 4.193 V, 2.677 V, and 4.125 V, respectively. The measurement of the discharged state was performed for 2 s per point, and 4.125 V, respectively. The measurement of the discharged state was performed for 2 s per point, while that for the charged state was done for 1 s per point. The total number of points measured was while that for the charged state was done for 1 s per point. The total number of points measured was 411 in each case. 411 in each case. Figure 2. Structure of the fresh cell (a) and the aged cell (b) observed by Compton scattered X-ray Figure 2. Structure of the fresh cell (a) and the aged cell (b) observed by Compton scattered X-ray intensities. Blue and red lines refer to discharged and charged states, respectively. The results were intensities. Blue and red lines refer to discharged and charged states, respectively. The results were obtained by scanning incident X-rays at the region shown in the inset to (a). obtained by scanning incident X-rays at the region shown in the inset to (a). This measurement was performed using a spatial resolution of 20 μm in height, 750 μm in width, This measurement was performed using a spatial resolution of 20 m in height, 750 m in width, and 500 μm in depth (note that a 20-μm height is small compared to the thickness of either electrode and 500 m in depth (note that a 20-m height is small compared to the thickness of either electrode (0.19 mm for the anode and 0.15 mm for the cathode). Therefore, the layered structure can be clearly (0.19 mm for the anode and 0.15 mm for the cathode). Therefore, the layered structure can be clearly resolved as seen in Figure 2a,b in the fresh as well as the aged cells. In these graphs, the largest peaks resolved as seen in Figure 2a,b in the fresh as well as the aged cells. In these graphs, the largest peaks around the vertical position of z = 0 mm correspond to the outer casing of the cell, the broad peaks around the vertical position of z = 0 mm correspond to the outer casing of the cell, the broad peaks correspond to the cathode and the Al collector, and the anode is located around the sharp peaks of correspond to the cathode and the Al collector, and the anode is located around the sharp peaks of the Cu collector. The decay of intensity in the inner layer reflects the absorption of X-rays in the the Cu collector. The decay of intensity in the inner layer reflects the absorption of X-rays in the matter. In order to focus on different lithiation states of the cells, the Compton scattered spectrum matter. In order to focus on different lithiation states of the cells, the Compton scattered spectrum was measured in two selected regions: 0.35 < z < 1.3 mm, which corresponds to the outer layer, and was measured in two selected regions: 0.35 < z < 1.3 mm, which corresponds to the outer layer, and 5.6 < z < 6.6 mm, which corresponds to the inner layer. 5.6 < z < 6.6 mm, which corresponds to the inner layer. Figure 3 shows the values of the S-parameter extracted from two different regions of the fresh and Figure 3 shows the values of the S-parameter extracted from two different regions of the fresh aged cells by applying Equation 3 to the Compton scattered spectrum measured by scanning incident and aged cells by applying Equation 3 to the Compton scattered spectrum measured by scanning X-rays along the z-direction of the cell. Figure 3a,b shows the results for two different states of charging incident X-rays along the z-direction of the cell. Figure 3a,b shows the results for two different states at the outer and inner layers of the fresh cell, while Figure 3c,d provides similar results for the aged of charging at the outer and inner layers of the fresh cell, while Figure 3c,d provides similar results cell. The background colors in Figure 3 identify the regions of the graphite anode (yellow), the NMC for the aged cell. The background colors in Figure 3 identify the regions of the graphite anode cathode (green), and the Cu/Al current collectors (gray). Notably, there is a separator between the (yellow), the NMC cathode (green), and the Cu/Al current collectors (gray). Notably, there is a cathode and the anode in our cell. However, we could not observe this separator because it is too separator between the cathode and the anode in our cell. However, we could not observe this thin compared with the incident X-ray beam size. The results in Figure 3a,b show that when the separator because it is too thin compared with the incident X-ray beam size. The results in Figure 3a,b battery is charged, the S-parameter increases at the anode while it decreases at the cathode. This show that when the battery is charged, the S-parameter increases at the anode while it decreases at implies that lithium moves from the cathode to the anode when the cell is charged. The variation in the cathode. This implies that lithium moves from the cathode to the anode when the cell is charged. the S-parameter between the charge and discharge in the aged cell is smaller than that in the fresh cell The variation in the S-parameter between the charge and discharge in the aged cell is smaller than (Table 1). Here, the error bar for the S-parameter was estimated from the error in Compton scattered that in the fresh cell (Table 1). Here, the error bar for the S-parameter was estimated from the error in X-ray intensity in the low- and high-momentum regions based on Equation (3). The error bar for the Compton scattered X-ray intensity in the low- and high-momentum regions based on Equation (3). averaged S-parameter was then determined by applying error propagation rules to the error bar of the The error bar for the averaged S-parameter was then determined by applying error propagation rules S-parameter in each position. In the fresh cell, the average S-parameter of the outer layer decreases to the error bar of the S-parameter in each position. In the fresh cell, the average S-parameter of the by about 1.9% at the cathode and increases by about 3.0% at the anode on charging. The average S-parameter of the inner layer decreases by about 3.3% at the cathode and increases by about 5.9% at the anode on charging. Thus, in the fresh cell, the values of the S-parameter show that a larger level of lithiation occurs in the inner layer. In contrast, in the aged cell, the average S-parameter of the outerPDF Image | High-Energy X-Ray Compton Scattering Imaging of 18650-Type Lithium-Ion Battery
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