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Condens. Matter 2021, 6, 28 3 of 11 and dislocation. Table 1 shows that the rolled material has an average lifetime of 208 ps, Condens. Matter 2021, 6, x FOR PEER REVIEW 3 of 12 near 30% higher than the undeformed Al (162 ps). Both Al samples well follow the trapping model with a bulk component of about 161 ps, according to the literature [41]. Figure 1. (a) Powder wide-angle X-ray diffractogram of pristine LCO material. hkl indices are reported into the figure on Figure 1. (a) Powder wide-angle X-ray diffractogram of pristine LCO material. hkl indices are reported into the figure on the top of the corresponding peaks. (b,c) HR-TEM images and (d) SAD pattern of the LCO material. The particle size the top of the corresponding peaks. (b,c) HR-TEM images and (d) SAD pattern of the LCO material. The particle size distribution obtained from TEM images for this material is reported in the inset of Figure 1b. distribution obtained from TEM images for this material is reported in the inset of Figure 1b. Further details on the high crystallinity of LCO are given by high-resolution Table 1. Reference materials especially relevant for the lifetime analysis. The cathodes were deposited transmission electron microscopy (HR-TEM) images (Figure 1b,c) and the selected area on the Al foil. The Al foil results are compared with an Al polycrystal sample of high purity (99.999%) diffraction (SAD) pattern (Figure 1d). The LCO material investigated in this work consists after a thermal treatment. The graphite powder used in the cathode preparation was sintered and of single-crystal particles of ca. 2 μm diameter. Well-defined lattice fringes are observed measured. in HR-TEM images (Figure 1c), thus revealing a high crystallinity. In particular, a d-spacing of ca. 2.46 Å is determined, which is consistent with the 100 (hkl) reflection also detected References τ1 (ps) τ2 (ps) I1 (%) I2 (%) τbulk (ps) τav (ps) in WAXD studies. The SAD pattern (Figure 1d) is coincident with that expected for a Al foil (rolled) 60 (5) 228 (3) 15 (2) 85 (2) 162 (4) 208 (3) LiCoO2 cathode material, since the d-spacings resulting from this investigation are Al (polycrystallyne) 158 (1) 234 (3) 96 (1) 4 (2) 161 (2) 162 (2) coincident with the 101, 012, 110, and 113 (hkl) reflections observed in the WAXD Graphite (C) 107 (4) 400 (5) 13 (3) 87 (2) - 362 (5) diffractogram. The graphite powder was sintered in two tablets (4 mm thick and 1.5 cm2 area) to 2.2. Positron Annihilation Lifetime Spectroscopy perform the PALS measurement. This sample possesses two lifetime components: (i) 2.2.1. Reference Samples the long lifetime component (~400 ps), the dominant one (87%), is associated to ”free For a better understanding of the thin cathodes results of positron annihilation volume” where ortho-positronium is formed which annihilates by pick-off in two gamma- lifetime spectroscopy (PALS), two reference materials were measured. One of them is the rays; and (ii) the shorter component in part is due to the graphite microstructure and aluminum foil used as the substrate of the cathodes and the other is the graphite powder para-positronium contribution. The average lifetime of the graphite sample is 362 ps. used in the mixture of cathode grains. To perform the measurement, the aluminum foil was folded on itself many times and then it was slightly pressed to prevent air remaining between the Al foils. Thus, a 1.5 mm thick sample with a surface of about 1 cm2 was obtained. The PALS measurement of the Al foils was compared to that of a high purity polycrystalline Al sample (99.999%) annealed. A long lifetime component (228–235 ps, in Table 1) appears in both samples, associated to vacancies or vacancy-like defects [41]. ThePDF Image | Positron Annihilation Spectroscopy LiCoO2 Cathode of Lithium-Ion Batteries
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