Lithium-Rich Rock Salt Type Sulfides-Selenides

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Lithium-Rich Rock Salt Type Sulfides-Selenides ( lithium-rich-rock-salt-type-sulfides-selenides )

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M the cubic rocksalt structure of Li TiSe S, and the theoretical composition became equiva- Materials 2022, 15, 3037 22 lent to Li4.17TiSe2S. We again detected extra discharge capacity, and this was even greater than the theoretical capacity of Li2TiSe2S (213 mAh·g−1 based on two electron exchange processes). Now, we cannot explain more than a three Li+ uptake with the same hypothe- sis; a combination of anionic and Ti3+/Ti4+ redox processes. In the cycling curve of Li2TiSe2S 7 of 11 cells, we observed that the second and third cycles were reversible; however, smaller charge and discharge capacities, as well as a rapid capacity fading, were detected. 8 of 12 aterials 2022, 15, x FOR PEER REVIEW To describe the possible redox processes taking place in Li2TiSexS3−x cells, we con- Se in the Li2TiSexS3−x materials leads to the activation of a new redox process, which is the ducted cyclic voltammetry measurements (Figure 5). origin of the extra capacity. only for the Se-substituted materials. This peak is reversible and can be observed in the second cycle of Li2TiSexS3−x cells. Therefore, we can assume that the substitution of S by Se in theFiLgui2rTeiS5.exRSe3d−xomx paoteterniatilaslslecaodmsptaoritshone oafctLivi2aTtiiSo3,nLoi2fTiaSenSe2,wanrdedLoi2xTipSreo2Sceslesc,trwodheicshatisthtehfeirst (5 Figure 5. Redox potentials comparison of Li2TiS3, Li2TiSeS2, and Li2TiSe2S electrodes at the first −1 −1 + originμVofsth)e(ae)x,at−rna1dcsaepcoancdity(1.0μVs )(b)cy−cl1esbetween3and1.5Vvs.Li/Li. + (5 μV·s ) (a), and second (10 μV·s ) (b) cycles between 3 and 1.5 V vs. Li /Li. To investigate the effect of this supplementary process on the cycling stability of the materials,Lwi2Te iTcSao3rcirneielvldsesothiugotawgteaedltvhaoeneoefsfoetaxctiidcoafcttyivhceilsinasngudspwpolnietemhretewndtuoacrdtyivfpferorpeceneastkslotohwnatvhroelstcuayglctelidncugfrts-ootmaffbsi:luitlyfuorf the 2−/ 2− 2−/ 2− one wreitdhomax craueteat-rcoitaifolfsna, tw(1Se.5cSaV2r,raiealdlnodowuSitn2 gaStlhv)eanactoy2sctl.a6int9igcVocynacntldhine2gs.s2u8wpVipthl.eMmtwoeornedtoaivrffyerp,er2no.t5cl1eosVws;cvahonaldtragogeneeacnaudt-2o.f2fs0: one 2 V, tVo daivswocihdtahrtaghecupmto-aotjefonfrtaiptaal1sr.5twoVef,ratehlldiosewtpeircnotgceedtshsien. cTLyhic2eTlirinSegesuSo2lntcstehpllerse,ssauenpndptel2ed.m4i3neVnFtiacgrhuyarrpegr6eocasehnsodsw;2a.1nth2daVtondeisa-t 2 V, the twchoasrugtobe saptviotoutiedtnedthiaselasmwapjeolersepcdaleretateorclfyttehbdiesninperfLoitcie2edTsisfS.reoT2mShecthreelelssur,eltdisnupcarecedcsoevrnodtleatdangcien wFwiigintuhdroepwr6e.svThihoeuwsimthre-astutlhtes two proveshmoewnsutinibsgsmtaitourertededuimcseapdmorwptlaoenrstkcfilnoergarLpliyo2TtbeieSnetei2aSfil,tfefodrfwSroehm-sicuhtbhtsehtireteuldotuewdcepmdoavtetoenlrtiaiaglesp.wrDoiuncerdisonswgr.edpTirshecehseiamnrgtpser,otvheement a bigagperppairsairmttionrfetohifmeaprseoedrctoaxndpt frroercdeLusis2ceTtisioS,new2pSite,hafokthrcewocuhalipdchabcteihtyeoblrosewetervnpetoidtoenanstaiataltshphero1uc4ledtshesrcryeopcflrtehsiemnmptsaroianvb-pigegaekr, part of the redox processes, with the capacity retention at the 14th cycle improving from 12% to ing from 12% to 76%. It is, thus, reasonable to assume that the supplementary process is a 76%. It is, thus, reasonable to assume that the supplementary process is a major factor in the major factor in the performance degradation of these materials. The stability of the non- performance degradation of these materials. The stability of the non-substituted material substituted material was not significantly modified; this was expected, as no major redox was not significantly modified; this was expected, as no major redox process occurs in the process occurs in the 1.5–2 V region for this material. 1.5–2 V region for this material. Figure 6. CFaigpuacreity6.rCetaepnaticoitny (r%et)eonftiLoni2T(%iS)3,oLf iL2Ti iSTeiS2, Lani dTiLSie2STi,Saen2SdcLeillsTicSyeclSedcealtlsacryactledofatCa/1r0atienof C/10 in 232222 different cycling windows: (a) 3–1.5 V and (b) 3–2.0 V vs. Li+/Li. + different cycling windows: (a) 3–1.5 V and (b) 3–2.0 V vs. Li /Li. ToinvestiTgoatinevwehstyigSaet-ecownhtyainSein-cgomntatienriinaglcmelalstefraiiallecdeullpsofanilceydcluinpgo,nacnydcltiong,eatnsodmtoegetsome hint of thheinat toufrtehoefntahteurleowof-pthoetelnowtia-lppotreoncteisasl,pwroecceossn,dwuectceodndexucstietud setxrusicttursatrluacntualryasleasnalyses of the electrodes at different states of charge. The results of Li TiS , Li TiSeS , and Li TiSe S of the electrodes at different states of charge. The results of Li2TiS3, Li2TiSe3S2, a2nd Li22TiSe2S 2 2 are shown in Figure 7. For both samples, we observed a reversible structural change in the are shown in Figure 7. For both samples, we observed a reversible structural change in diffraction patterns of the electrodes: the cubic structure became amorphous at the end of the diffraction patterns of the electrodes: the cubic structure became amorphous at the end the charge, then it recrystallized to a disordered rocksalt form at the end of the discharge. of the charge, then it recrystallized to a disordered rocksalt form at the end of the dis- Such flexible structural change in electrodes was previously reported for Li TiS [19]. charge. Such flexible structural change in electrodes was previously reported for Li2TiS32 3 Differently from Li TiS , metallic selenium was detected in selenium substituted electrodes [19].DifferentlyfromLi2TiS32,me3tallicseleniumwasdetectedinseleniumsubstitutedelec- at the end of the charge, and disappeared at the end of the discharge (Figure 7). trodes at the end of the charge, and disappeared at the end of the discharge (Figure 7).

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