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Materials 2022, 15, x FOR PEER REVIEW Materials 2022, 15, x FOR PEER REVIEW Materials 2022, 15, 3037 10 of 12 10 of 12 9 of 11 h. Figure 9. (a) SEM images and (b) EDX images of Li2TiSe2S electrodes charged to 3 V and kept for 24 Figure 9. (a) SEM images and (b) EDX images of Li TiSe S electrodes charged to 3 V and kept for 22 Fihg.ure 9. (a) SEM images and (b) EDX images of Li2TiSe2S electrodes charged to 3 V and kept for 24 24 h. To rule out the possible presence of Se in the pristine material, which would have To rule out the possible presence of Se in the pristine material, which would have stayTeodruunlneootuictedthdeupeotsositbhlenparneose-sniczeofrStoeainathmeoprprihsotiunsenmatautereri,aln, dwwhiochuldwtohuelndfhoallvoew stayed unnoticed due to the nano-size or to an amorphous nature, and would then follow stanyeOdsutwnanlodtirciepdendiunegtoprtohceenssanoor-sainzeaogrgltomaneramtionrpohfopuasrntiactluesrei,nanthdeweoleucltdrotlhyetne tfollfowrm an Ostwald ripening process or an agglomeration of particles in the electrolyte to form anbigOgsetwr apladrtriicplesni[n3g3]p, rwoceespserofroramneadgghliogmh-ereastoioluntiofnpXar-triacylesphinotohelecltercotrnolsyptectorofsocrompy bigger particles [33], we performed high-resolution X-ray photoelectron spectroscopy (XPS) b(igXgPeSr) opnarthicelepsri[s3ti3n],e wpoewpdeerrfso.rmed high-resolution X-ray photoelectron spectroscopy on the pristine powders. (XPS) Foinguthre p10risthinowe ps othwedSeer3s.d core peak of Li2TiS3, Li2TiSeS2, and Li2TiSe2S powders and Figure 10 shows the Se3d core peak of Li2TiS3, Li2TiSeS2, and Li2TiSe2S powders and seleFniguumrep1r0ecsuhroswors. TtheSfeo3udr scpoerectpraeawkeoref Lcai2lTibiSra3,teLdi2TbaiSseSd2,oannCd 1Lsi2cToirSe2pSepakowatd2e8r4s.a8nedV. selenium precursor. The four spectra were calibrated based on C 1s core peak at 284.8 eV. selenium precursor. The four spectra were calibrated based on C 1s core peak at 284.8 eV. FFigiguurere1100. . XPS spectra of powderrss::LLi2iTTiSi3S, L, iL2Ti iSTeiSe2,San, danLdi2TLiSTe2iSeanSdasnedlesneiulemniupmrecpurescourrastoSrea3td 232222 Ficgourere. 10. XPS spectra of powders: Li2TiS3, Li2TiSeS2, and Li2TiSe2S and selenium precursor at Se3d Se3d core. core. wvearkyF.iwrWsete,akistu. igWsgpeosstsustgihbgelehsytopthonetohtheicyseipsotththaatetsttihsheitshTpai3thsethnsiosgmnpaehlnseoninomitshedenuoSene-tsiosutbdhsueteiStueto3teddthcesraoSmsesp3-sdlecsctriaorsnes,- vwsehercyictihwonies,ahkwi.ghWhiceehr stihsuaghngigethstertThtieh3aShnoynptheoet(hrTeis3piSsectohtniavete(tlryhe,is0p.p9e3hc4teinveosl.my0,e.40n7.o93n3)4.iAsvsd.us0e.e4tn7o3in)t.htAehesSefis3egdeunrcerin,otshtshe-e FFirisrts,t,ititisispopsossibsilbe lteo tnoontiocetictheathtahtetThie3sTsi3igsnsailgsninalsthienSteh-esuSbes-tsiutubtsetditusatemdpsleasmaprelevsearyre 2− 0 2− 0 sbefiicngtdiuoirneg,wtehnheeicbrhginyidsoihnfigSgehe3nedrert(ghSyeanoft)hSwe3aTdsi3r(SaSteohne)erwl(oraewsperraetcththievarneloySw,e0e,.r9a3tn4hdav,nsu.Sn0ef.o4,r7at3un)d.nAa,tusenlsyfe,oerLntiu1insnaatnheldey, 2− 0 fSiLgei3u1drseb,aintnhdeiSnbegi3ndednibneirgngdeieinsegwrgeynreorfqguSieits3edwcle(oSrseeqt)uowietaeaschrloaosttheheterorl(eodawectehercotthehdaenrbeS(dtewe,teaecntde5d,2ubeneVftowartenuedna55t5e2elyeV,V, Lreai1snpsdea5cnt5idveeVSley, 3r).desEpbviencndtiivfnetglhye)n.LEeir1vgseinpeseifawktheoerveLeqir1luasiptesewackloitoshevtehtroalatepoasfchSweoi3tthdh,tethrhae(tdcoerftoeSscest3esde,ctbthieoetnwc(resoesnsss5ite2icvteiVtoyn afan(scdeton5rs5)iteoiVvfi,Stryee3sfdapce(t0cot.r8i)v2eo1lf)ySi)s.eE3mdvue(cn0h.i8fh2ti1hg)ehiseLrim1tshuapcnheaLhki1goshve(e0r.lt0ah2pa8sn)w. LTiith1hestr(he0fa.o0tr2oe8f,)Se. evT3ehdne,ritefhfioetrciesr,odesivsffiesnceucitflitoitnois (asdtetinrfifsbiicutuitvleitttythoefaLcttir1oiSrb)/uoStfe3Stdeh3epdLe(ai01k.Ss8/,2Sd1e)u3iedstmpoeupacokhss,hidbigulehepetrotlahpraoinzssaLitbio1lesnp(w0o.h0la2ern8i)zS.aTtaihtooenmrewsfoharereen, seSuvabetnsotimtfuisteaidsre by Se atoms (environment modification), the peak is mainly related to Se3d. dsifufbicsutiltuttoedatbtryibSueteattohme sL(ie1nSv/Sireo3ndmpenatkms, odduiefictoatpions)s,ibthle poealakrizsamtioainnlwyhrenlatSedattoomSse3adre. The core peak of Se0 was detected at 56 eV. A similar binding energy of Se0 was substituted by Se atoms (environment modification), the peak is mainly related to Se3d. reported previously [34]. Overall, no signature of selenium precursors was detected in thePDF Image | Lithium-Rich Rock Salt Type Sulfides-Selenides
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