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Processes 2018, 6, 59 Processes 2018, 6, x FOR PEER REVIEW Processes 2018, 6, x FOR PEER REVIEW 6 of 14 6 of 14 6 of 14 FigFuigreur3e.3S.ySnythnethtiectimcemchecahnaisnmissm:s(:a,(ba),bs)ysnythnethsiessiosfoLfMLOM;O(c;)(ca)bsaobrspotripotnio-dne-dsoerspotripotniomnemcheachnaisnmismofof Figure 3. Synthetic mechanisms: (a,b) synthesis of LMO; (c) absorption-desorption mechanism of λ-Mλ-nMOnO(H2M(HOM) aOnd) aLnMdOL.MO. 2 λ-MnO2 (HMO) and LMO. 3.23..2Io.nIo-Sni-eSviesveCshCahracrtaecrtiezraitziaotnion 3.2. Ion-Sieves Characterization FigFuigruer4es4hsohwoswtshethXeRXDRDpapttaetrtnersnosfotfhethLeMLOM,OH,MHOMOanadntdhethseamsapmleplaeftaefrteardasdosroprtpiotniopnrporcoecssess Figure 4 shows the XRD patterns of the LMO, HMO and the sample after adsorption process (no(nteodteadsaLsMLOM-O1)-.1T).hTehdeidffirfafcraticotniopnepaekaokfoLfMLMOOcocrorersrpesopnodnsdtsotaocaucbuicbiscpsinpeinleHlMHMOOstrsutrcutucrtuer[esp[sapceace (noted as LMO-1). The diffraction peak of LMO corresponds to a cubic spinel HMO structure [space grgoruopu:pF:dF3dm3m(JC(JPCDPSD3S53-057-08728)2],)]w,iwthiththtehleatltaitcteicceocnosntastnatnstisi8s.283.2Å3.ÅI.tIsthsohuoludldbebneonteodtetdhtahtatthtehXeRXDRD group: Fd3m (JCPDS 35-0782)], with the lattice constants is 8.23 Å. It should be noted that the XRD papttaetrtnersnosfoHfMHOMOanadnLdMLMO-O1-a1rearseimsiimlairlawriwthitthethdeifdfrifafcrtaicotniopnapttaetrtnersnosfoLfMLOM,Ow,iwthitlhatltaitcteicceocnosntasntatsnts patterns of HMO and LMO-1 are similar with the diffraction patterns of LMO, with lattice constants ++ ofo8f.081.0Å1Åanadn8d.283.2Å3,Åre,srpesepcteicvteivlye,liyn,dinicdaitciantgintghatthtahtethLeiLisifsrefereteotaocaceccssestshethsetrsutrcutuctrueraenadntdhethMeMn-On-O of 8.01 Å and 8.23 Å, respectively, indicating that the Li+ is free to access the structure and the Mn-O latltaitcteicremreaminasinsstasbtalebldeudruinrgintghethaedasdosroprtpiotnioannadndedsoesroprtpiotniopnrporcoecsse.ssI.t Iits ifsoufonudntdhtahtatthethdeifdfirfafcraticotnion lattice remains stable during the adsorption and desorption process. It is found that the diffraction pepaekaokfoHfMHMOOshsifhtisftsotaohaighhigehredrifdfrifafcrtaicotnioannagnlegltehathnatnhathtaotfoLfMLMO,Ow,hwichhicchacnabnebexepxlapilnaeindedbybtyhtehe peak of HMO shifts to a higher diffraction angle than that of LMO, which can be explained by the ++ ++ memcehcahnaisnmismshsohwoewdeidniFnigFuigruer3ec.3Dc.uDriunrgintghethLeiLdiedsoesroprtpiotniopnrpocroescse,sHs,Hininthtehseosluoltuiotniorneprelapclaecsetshethe mechanism showed in Figure 3c. During the Li+ desorption process, H+ in the solution replaces the ++++++ oriogringainlaplopsiotisoitnioonfoLfiLinitnhtehLeMLMOOthtehieonioicnircadraiudsiuosfoHfHisismsmallaelrletrhtahnaLniL,il,elaedaidnigngtotoceclellslhsrhinriknakgaeg,e, original position of Li+ in the LMO the ionic radius of H+ is smaller than Li+, leading to cell shrinkage, whwichhicihs aislsaolsroepreoprtoerdteidnilnitelirtaetruartuer[e26[]2.6T].hTehcehcahracratecrtiesrtisctidcifdfirfafcraticotniopnepaekaskosfoLfMLMO-O1-a1rearsetislltisllhsahrparp which is also reported in literature [26]. The characteristic diffraction peaks of LMO-1 are still sharp anadnodnolynltyhethientienntesnitsieitsiedsedcreecareseadsecdocmopmapreadrewdiwthitthethLeMLOM,Oin,dinicdaitciantgintghathtathtethHeMHMOOcacnabnebuesuesdefdofror and only the intensities decreased compared with the LMO, indicating that the HMO can be used for ++ effiecffiiecnietnatdasdorspotripotnioonfoLfiL.i . efficient adsorption of Li+. LMO LMO −nO Intensity (a.u) Intensity (a.u) (311) (222) (311) (222) (400) (331) (400) (331) (511) (511) (440) (531) (440) (531) (111) (111) 1010 2020 3030 4040 5050 6060 7070 8080 2Theta (°) 2Theta (° ) Figure 4. XRD patterns of optimized LMO, HMO and LMO-1. Figure 4. XRD patterns of optimized LMO, HMO and LMO-1. Figure 4. XRD patterns of optimized LMO, HMO and LMO-1. Figure 5 describes the XPS spectra of LMO and HMO. As showed in Figure 5a, the spectra of the Figure 5 describes the XPS spectra of LMO and HMO. As showed in Figure 5a, the spectra of the MnF3isguorreb5itdsehsocwrisbetshethebiXndPiSnsgpencterragoyfdLiMffeOreanncdeHofMthOe.AtwsoshpoewakesdwinaFsig5u.1r5ee5Va,t(hΔeEs=pe5c.t1r5aoeVf), Mn3s orbit shows the binding energy difference of the two peaks was 5.15 eV (ΔE = 5.15 eV), 3+ theinMdinca3tsinogrbtihtasthtohwesvtahlenbciensdoinfgMeneinrgLyMdiOffearreenc+e3oafntdhe+4t.wTohpeebaiknsdwinagse5n.1e5rgeyVo(f∆MEn= 5p.1e5akeVw),as indicating that the valences of Mn in LMO are +3 and +4. The binding energy of Mn3+ peak was 4+ 3+ ind64ic1a.3ti3ngeVthatndtheMvnalepnecaekssofwMerne i6n43L.7M6OeVaraen+d36a4n2d.66+4e.V,Twhehibcihndwinegreeonbetragiyneodf Mbynmepaenaskof 641.33 eV and Mn4+ peaks were 643.76 eV and 642.66 eV, which were obtained by means of 4+ wapsea6k4-1d.3if3ferVenatinadtioMn-nimitpaetainkgsawnearlyes6is43a.t7t6heVMann2pd36/242o.r6b6ite(VF,igwuhriec5hbw).eTrheeorbetsauilntsedarbeyinmlienaenwsiothf a peak-differentiation-imitating analysis at the Mn2p3/2 orbit (Figure 5b). The results are in line with a pepakre-dvioffuesrernetpiaotrito[n2-7im]. iTtahteinagvearnaglyesvisalaetntcheoMf Mn2np3in/2LMorObit(+(F3i.g65u)reco5ubl)d. Tbheecarelcsulatsteadre(Tinablilnee2w), iwthhaich previous report [27]. The average valence of Mn in LMO (+3.65) could be calculated (Table 2), which 3+ preisvhioiughsererpthoartn[2th7e].tThheeoraevteicralgveavleanlecnec(e+o3f.5M),ninidniLcaMtiOng(+th3a.6t5p)rcopuoldrtiboencoaflcMulnatedin(TLaMblOe 2is),lwowhiecrhthisan is higher than the theoretical valence (+3.5), indicating that proportion of Mn3+ in LMO is lower than 3+ higtheorrtehtiacnalt.hTehtuhse,oirtectiacnalbvealdeendcuec(e+d3.t5h)a, tinLdMicOatihnagsthaamt poreopsotarbtiloencroyfsMtanl striuncLtuMreO. Fisigluorwee5rcthisanthe theoretical. Thus, it can be deduced that LMO has a more stable crystal structure. Figure 5c is the theXoPrSetsipcaelc.trTahoufsH, iMt cOaninbtehdeeMdnu3csedortbhiattaLndMtOhehbaisnadimngoreenesrtagbyledicfrfeyrsetanlcestoruf tchtuertew. oFipgeuarkes5isc 4is.7t8heV, XPS spectra of HMO in the Mn3s orbit and the binding energy difference of the two peaks is 4.78 eV, XPinSdsipceacttinragothf aHtMthOe minatnhgeaMnens3esvoarlbenitcaenidn tHhMe bOinidsi+n4g. Fenuertrhgeyrmdioffreer,etnhcies oisfathlseotpwrovpeenakbsyitsh4e.7p8eaekV,of indicating that the manganese valence in HMO is +4. Furthermore, this is also proven by the peak of HMO in the Mn2p3/2 orbital (Figure 5d). HMO in the Mn2p3/2 orbital (Figure 5d). λ−ΜnO LMO-1 2 2 L M O -1 JCPDS 35-0782 JCPDS 35-0782PDF Image | Sieves for Highly Selective Li Adsorption
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