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imagesofthevapordepositedgammasulfurphaseonCNFs FIG.4AshowstheX-raydifractionpaternofvapordepos itedsulfuronCNFs. FIG.4Bshowsathermogravimetricanalysis(TGA)curve ofgammamonoclinicphasesulfurinaN,environment. 20 andacarbonateelectrolyte(EC:DEC). FIG.10Cshowsthecyclingstabilityofgammasulfur depositedCNFsinanEC:DECelectrolyteatacurentrate of0.5C. US 10,991,944B2 8 meansoftheelementsandcombinationsparticularlypointed FIGS.9B-9CshowSEMimagesofgammasulfurdepos outintheapendedclaims.Itistobeunderstodthatboth itedCNFsshowingwel-distributedgammasulfurdeposi theforegoinggeneraldescriptionandthefolowingdetailed tionandEDSelementalmaping. descriptionareexemplaryandexplanatoryonlyandarenot FIGS.9D-9FshowtheX-rayphotoelectronspectroscopy restrictiveofthedisclosure,asclaimed. 5 (XPS)spectraofS,O,andConthegammasulfurdeposited CNFs(afterdepositionofSulfur). BRIEF DESCRIPTION OF THE DRAWINGS thoxyethane:1,3-dioxolane(DME:DOL)andacarbonate electrolyte,ethylenecarbonate:diethylcarbonate(EC:DEC). FIG.1showsaschematicofthefabricationprocedurefor makingcarbonnanofibers(CNFs)andvapordepositionof10sulfurdepositedCNFsinandetherelectrolyte,1,2-dime gammamonoclinicphasesulfurontheCNFs. FIG.2showsavapordepositionasemblyanditsrespec tivepartssuitableforuseinthemethodofthepresent invention. FIG.10Bshowscyclicvoltametrycurvesofgamma FIGS.3A-3Dshowscaningelectronmicroscope(SEM)15sulfurdepositedCNFsinanetherelectrolyte(DME:DOL) FIG.10Dshowsthedischargecapacityofgammasulfur FIG.5AshowsCharge-DischargecurvesatC/50cycling depositedCNFsatvariousnumbersofcycles. ofanLi– Scel. FIG.10Eshowsadiferentialcapacityanalysisplotof FIG.5BshowsCharge-DischargecurvesatC/2,C/5and gammasulfurdepositedCNFsdisplayingasinglepeakin C/10cyclingratesoftheLi Scel. thecharge-dischargecycle. FIG.5CshowsCharge-DischargecurvesatC/2atvarious25 FIG.10FshowsaNyquistplotofgammasulfurdeposited numbersofcyclesoftheLi Scel. FIG.5Dshowscyclicvoltametrycurvesforthefirst, dischargecycle. secondandthirdcyclesat0.05mV/softheLi Scel. FIGS.11A-11Dshowtherateperformanceandhigh FIG.5EshowstheratecapabilityoftheLi-Scel. loadinganalysisofgammasulfurdepositedCNFs. FIG.5FshowsC/2cyclingofanLi–Scelwithvapor30 FIG.11Ashowstherateperformanceofgammasulfur depositedgammamonoclinicphasesulfuronCNFs. depositedCNFsincarbonateelectrolyte. FIGS.6A-6Cshowdiagramsofthevapordeposition FIG.11Bshowsthedischargeprofilesofgammasulfur assembly. depositedCNFsatvariousCrates. FIG.6Aisaperspectiveviewofthevapordeposition FIG.11Cshowslongcyclingofgammasulfurdeposited asembly,includingtheautoclavelidandautoclavecham-35CNFsatlowcurentrate0.1Cat1.2mg/cm2loading. ber. FIG.6Bisacros-sectionalviewofthevapordeposition FIG.11Dshowslongcyclingofgammasulfurdeposited CNFsasafunctionofhighloading. asemblyofFIG.6A,takenalonglineA-AofFIG.6A. FIG.6Ciscros-sectionalviewofthevapordeposition FIGS.12A-12Bshowpost-mortemSEMandTEManaly asemblyofFIG.6A,takenalonglineB-BofFIG.6A. 40 sisofgammasulfurdepositedCNFsafter20Charge FIG.7isaschematicofalithium-sulfurbaterydischarge DischargeCycles. inthecarbonate-basedelectrolyte.Atleastsomeofthe FIG.12AshowsaSEMimageofgammasulfurdeposited gamma-monoclinicsulfurisdepositedontheexternalsur- CNFsafter20dischargecycles. faceofthecarbonnanofibers.The medium sizedbals FIG.12BshowsaSEMimageofgammasulfurdeposited signifysurfacedepositedgamma-monoclinicsulfur,andthe45CNFsafter20chargecycles. smalbalssignifylithiumsulfide,theproductformedafter FIG.12CshowsaSEMimagetakenafterlithiationina reductionofsulfur. completelydischargedsamplepost1000cycles,showing FIGS.8A-8FshowthematerialcharacterizationofCNFs theadherenceofsulfurtocarbonnanofibers. deposition. dischargecycles,atC/10. FIG.8BshowsSEMimagesofCNFsaftergammasulfur FIG.13AshowsanXRDpaternofpristinegammasulfur deposition.Theinsetisanenlargedimageofwel-deposited depositedCNFs. gammasulfurparticlesofCNFs. FIG.13BshowsanXRDpaternofdischargedgamma FIG.8Cshowsacros-sectionalSEMimageofCNFs 5sulfurdepositedCNFsshowingconversiontoLi2S. aftersulfurdepositionshowinggammasulfurdeposited FIG.13Cshowsachargedspectrumofabaterythatwas throughoutthecathode. chargedandsubsequentlytheelectrodewasremovedfrom FIG.8DshowstheporesizedistributionofCNFsbefore thebatery,showingconversiontomonocliniccyclo-hexa andaftergammasulfurdeposition. cyclo-decasulfur. FIG.SEshowsisothermsobtainedbeforeandafter60 FIG.13Dshowsatypicalcharge-dischargevoltageprofile gammasulfurdepositiononCNFs. obtainedinthesamplesandthespecificpointswhere FIG.8FshowsaTGAcurveofgammasulfurdeposited spectroscopydatawascolected. CNFs in an argon environment. FIG. 13E shows high resolution S2p XPS spectra of FIGS.9A-9Fshowthephaseandsurfacecharacterization pristinegammasulfurdepositedCNFs. ofCNFs andgamma sulfurdepositedCNFs. 65 FIG.13F shows high resolution S2p XPS spectra of FIG.9AshowsanX-raydifraction(XRD)paternof dischargedgammasulfurdepositedCNFsdisplayingan CNFsandgammasulfurdepositedCNFs. Li2Speak. andy-sulfurdepositedCNFs. FIGS.13A-13Gshowpost-mortemXRDandXPSanaly FIG.8A shows SEM images of CNFs before sulfur 50 ses of gamma sulfur deposited CNFs after five charge FIGS.10A-10Fshowtheelectrochemicalcharacteriza tionofgammasulfurdepositedCNFs. FIG.10Ashowscharge-dischargepaternsofgamma CNFscathodeasafunctionofvoltageduringthechargePDF Image | SYNTHESIS OF GAMMA MONOCLINIC SULFUR
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