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Materials 2022, 15, 3037 10 of 11 References XPS spectra, and, consequently, we conclude that there was no metallic selenium remaining in the powders after the synthesis. The origin of metallic selenium seen at the end of the charge could result from the selenium redox activity; therefore, further XPS analyses on selenium-sulfide electrodes at different states of charge are required to investigate this fact. 4. Conclusions In summary, selenium-substituted samples (Li2TiSeS2 and Li2TiSe2S) were synthesized in disordered rocksalt phase, with a flexible and versatile synthesis process. Unlike Li2TiS3 cells, Li2TiSeS2 and Li2TiSe2S provided larger discharge capacities than the theoretical capacities. In cyclic voltammetry tests, Li2TiSeS2 and Li2TiSe2S showed different oxidative and reductive potentials from Li2TiS3, indicating a different redox activity. We also detected a second phenomenon that leads to extra discharge capacities. XPS and SEM and XRD ex situ studies showed that this extra capacity was coming from the activity of metallic Se that was formed during the first charge in these substituted samples and led to the formation of soluble polyselenides during the next discharge. The possible shuttle mechanism known for these species can be the origin of the low cycle life of these samples when cycled at low potential. Further structural studies are needed to elucidate the redox activities of Li2TiSexS3−x. Author Contributions: Investigation, Y.C., J.-F.C., S.M., A.B. and D.P.; Writing—original draft, Y.C.; Writing—review & editing, J.-F.C., S.M., A.B. and D.P. All authors have read and agreed to the published version of the manuscript. Funding: This work was entirely supported by the CEA-LITEN. Institutional Review Board Statement: Not applicable. Data Availability Statement: No Supporting Information. Figures and tables are taken from the dissertation of the author, Yagmur Celasun. Conflicts of Interest: The authors declare no conflict of interest. 1. Larcher, D.; Tarascon, J.-M. Towards greener and more sustainable batteries for electrical energy storage. Nat. Chem. 2015, 7, 19–29. [CrossRef] [PubMed] 2. Rozier, P.; Tarascon, J.M. Review—Li-rich layered oxide cathodes for next-generation li-ion batteries: Chances and challenges. J. Electrochem. Soc. 2015, 162, A2490–A2499. [CrossRef] 3. Schmuch, R.; Wagner, R.; Hörpel, G.; Placke, T.; Winter, M. Performance and cost of materials for lithium-based rechargeable automotive batteries. Nat. Energy 2018, 3, 267–278. [CrossRef] 4. Wang, J.; Liu, C.; Xu, G.; Miao, C.; Wen, M.; Xu, M.; Wang, C.; Xiao, W. Strengthened the structural stability of in-situ F− doping Ni-rich LiNi0.8Co0.15Al0.05O2 cathode materials for lithium-ion batteries. Chem. Eng. J. 2022, 438, 135537. [CrossRef] 5. Yabuuchi, N. Material design concept of lithium-excess electrode materials with rocksalt-related structures for rechargeable non-aqueous batteries. Chem. Rec. 2018, 19, 690–707. [CrossRef] 6. Li, W.; Lee, S.; Manthiram, A. High-nickel NMA: A cobalt-free alternative to NMC and NCA cathodes for lithium-ion batteries. Adv. Mater. 2020, 32, 2002718. [CrossRef] 7. Zhang, L.; Wu, B.; Ning, L.; Feng, W. Hierarchically porous micro-rod lithium-rich cathode material Li1.2 Ni0.13 Mn0.54 Co0.13 O2 for high performance lithium-ion batteries. Electrochim. Acta 2014, 118, 67–74. [CrossRef] 8. He, X.; Wang, J.; Kloepsch, R.; Krueger, S.; Jia, H.; Liu, H.; Vortmann, B.; Li, J. Enhanced electrochemical performance in lithium ion batteries of a hollow spherical lithium-rich cathode material synthesized by a molten salt method. Nano Res. 2014, 7, 110–118. [CrossRef] 9. Song, B.; Liu, Z.; On Lai, M.; Lu, L. Structural evolution and the capacity fade mechanism upon long-term cycling in li-rich cathode material. Phys. Chem. Chem. Phys. 2012, 14, 12875–12883. [CrossRef] 10. Muralidharan, N.; Essehli, R.; Hermann, R.P.; Parejiya, A.; Amin, R.; Bai, Y.; Du, Z.; Belharouak, I. LiNix Fey Alz O2 , a new cobalt-free layered cathode material for advanced Li-ion batteries. J. Power Sour. 2020, 471, 228389. [CrossRef] 11. Xiao, J.; Chen, X.; Sushko, P.V.; Sushko, M.L.; Kovarik, L.; Feng, J.; Deng, Z.; Zheng, J.; Graff, G.L.; Nie, Z.; et al. High-Performance LiNi0.5Mn1.5O4 spinel controlled by Mn3+ concentration and site disorder. Adv. Mater. 2012, 24, 2109–2116. [CrossRef] [PubMed] 12. Kim, J.-H.; Myung, S.-T.; Yoon, C.S.; Kang, S.G.; Sun, Y.-K. Comparative study of LiNi0.5 Mn1.5 O4−δ and LiNi0.5 Mn1.5 O4 cathodes having two crystallographic structures: Fd3-m and P4332. Chem. Mater. 2004, 16, 906–914. [CrossRef]PDF Image | Lithium-Rich Rock Salt Type Sulfides-Selenides
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