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Crystals 2018, 8, 425 5 of 12 literature [14,33,34]. The Mn 2p3/2 XPS of the pristine LNCM centers at 641.7 eV, which indicates that the oxidation state of Mn of the pristine LNCM is a mixed oxidation state of Mn3+ and Mn4+. In the case of Cl and Br co-doped LNCM, the spectra of Ni2p3/2, Co2p3/2, and Mn2p3/2 shift to higher binding energy, indicating that the valences of the transition metals increase. The relative amounts of Ni2+ and Ni3+ are estimated to 70.06% and 29.94%, respectively. The binding energy for Mn2p3/2 of the Cl and Br co-doped LNCM is 642.24 eV, which agrees well with that of Mn4+ reported in the literature [34]. After being ion-etched for 30 s, the Ni, Mn, and Co XPS core level spectra of the Cl and Br co-doped LNCM shift back to almost the same binding energy of the pristine LNCM. This indicates that the doping mainly affected the surface oxidation state of LNCM, and only happened to the surface near the regions of the material. This is probably because the synthesized Ni1/3Co1/3Mn1/3(OH)2 precursors were used to prepare the LNCM compound, and it is hard for Cl and Br to diffuse into the bulk material uniformly. Figure 3. XPS spectra of (a) O 1s, (b) Ni 2p3/2, (c) Co 2 p3/2, (d) Mn 2p3/2 for Pristine LNCM; (e) O 1s, (f) Ni 2p3/2, (g) Co 2p3/2, (h) Mn 2p3/2 for Cl&Br co-doped LNCM; (i) O 1s, (j) Ni 2p3/2, (k) Co 2p3/2, (l) Mn 2p3/2 for Cl&Br co-doped LNCM being ion-etched for 30 s. The initial charge/discharge capacities and the cyclic performances of the synthesized LiNi1/3Co1/3Mn1/3O2 compounds were evaluated at different rates in 2.5~4.6 V at room temperature. Figure 4 shows the initial charge/discharge curves of the synthesized LiNi1/3Co1/3Mn1/3O2 compounds at 0.1C, 0.2C, 0.5C, 1C, and 3C respectively. The pristine LNCM delivers discharge capacities of 203.1 mAh g−1, 191.8 mAh g−1, 170.2 mAh g−1, 152.6 mAh g−1, and 135.8 mAh g−1, while the Cl and Br co-doped LNCM delivers 208.9 mAh g−1, 200.6 mAh g−1, 188.2 mAh g−1, 173.3 mAh g−1, and 157.1 mAh g−1 at the corresponding rates of 0.1C, 0.2C, 0.5C, 1C, and 3C, respectively. The initial discharge capacities of Cl and Br co-doped LNCM are 5.8 mAh g−1, 8.8 mAh g−1, 18 mAh g−1, 20.7 mAh g−1, and 21.3 mAh g−1 higher than the pristine one at the corresponding rates, respectively. It is indicated that the initial electrochemical capacity has been improved by Cl and Br co-doping. As shown in SEM analysis, the pores on the surface of co-doped LNCM can increase the contact area of the electrode/electrolyte, and also provide channels for the intercalation/deintercalation of lithium ions. More Ni2+ exists in the pristine LNCM, which can cause more cation disordering, as shown in XPS analysis, and a larger R(sei+ct) value, which is discussed inPDF Image | Enhanced High Voltage Performance of Chlorine Bromine
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