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25 26 US 10,991,944B2 thecycledClsandOlsspectra.Also,atlowerscanratesno at50mAh/gand325mAh/g,respectively.Theseexperi curentresponsewasrecordedcorrespondingtoposiblesalt mentswerecariedoutatabout18-25°C. decomposition. PotassiumSulfurCells backtosulfurinthechargecycle.Thepresenceofsome reductionpeak,3distinctpeaksareatributedtothecon Li2Sevenafterchargemaybeasociatedwithincomplete versionofsulfurtoKSztoK2S,andfinalytoKS. Aftercompletecharge,S2pspectrashowsadiminished FIG.15Adisplaysacyclicvoltametrycurveofagamma Li2Speakat161.8eVandsulfurdoubletpeaksdominatethe5sulfurdeposited-CNFscathodewithapotasiumanodein1 overalspectrumindicatingreversibleconversionofLi2S MKPFinEC:DECatvariouscyclesat0.1mV/s.Inthe conversionduetothefastchargerate.TheF1sspectra However,duringthechargestep,asingleoxidationpeakis continuestoshowthepresenceofLiFandLiFxNypeaks10observed,whichisatributedtodirectconversiontosulfur fromsaltdecompositionandsaltspeciesat685.5and68 withoutintermediateconversion.Agammasulfurdeposited eV,respectively,inchargedsamples,whichisexpectedas CNFscathodeperformssubstantialybeterthananycath LiFisknowntobeastableSEIcomponentinLi-ion odesreportedintheliteratureupto5C.Thecathoderetains bateries. FIGS.13A-13CshowtheXRDpaternsofthepristine15alofitscapacitywhencycledbackat0.1C,displaying superiorcathodearchitectureandcompleteutilizationofthe chargedcathodes.Thedifractogramofthepristinecathode activematerial.Cyclingstabilitywasstudiedat0.5Crate, asdiscusedearliershowspeaksofgammamonoclinic andthecathodedisplayedacapacityof870mAh/gafter120 phasesulfur.Duringinitialdischarge,weobserveaplateau cyclesshowingitspotentialtobeusedasacathodematerial at2.0V.Theplateaucontinuestoprogrestowardscomplete20inapotasium-sulfursystem.Theseexperimentswerecar sulfurreductionat1.0Vatarateof0.1C.Aftercomplete riedoutatabout18-25°C. reductionofcathodes,thedifractionpaternshowsthe Otherembodimentsofthepresentdisclosurewilbe presenceofLi2Speaks(00-023-0369)at1.61,13.41, aparenttothoseskiledintheartfromconsiderationofthe 19.01,2.31,whichcorespondtoreflections(1),(200), specificationandpracticeoftheembodimentsdisclosed (20)and(31),respectively.Itconfirmsthefindingfrom25herein.Asusedthroughoutthespecificationandclaims,“a” XPSandTEMthatthesingleplateauobservedinthe and/or“an"mayrefertooneormorethanone.Unles dischargecycleisasociatedwiththereductionofgamma otherwiseindicated,alnumbersexpresingquantitiesof monoclinicphasesulfurtolithiumsulfide(Li2S).After ingredients,propertiessuchasmolecularweight,percent, charge,interestingly,acompletelydiferentsulfurXRD ratio,reactionconditions,andsoforthusedinthespecifi paternisobserved.Suchpaternhasnotbenreportedyet30cationandclaimsaretobeunderstodasbeingmodifiedin intheLi–Sliterature.Thesepeaksareatributedtocyclo- alinstancesbytheterm“about,”whetherornottheterm deca-cyclo-hexasulfur,alsobelongingtoamonoclinic “about”ispresent.Acordingly,unlesindicatedtothe crystalstructurefamily.Nooverlapinggammamonoclinic contrary,thenumericalparameterssetforthinthespecifi sulfurpeakswereobserved.Thispostmortemstudydem- cationandclaimsareaproximationsthatmayvarydepend onstratescompleteconversionofß-monoclinicsulfurto35inguponthedesiredpropertiessoughttobeobtainedbythe Li2Sandbacktoanewsulfurmonocliniccrystalphase.This presentdisclosure.Attheveryleast,andnotasanatempt isthefirsteverstudytoreportstabilityofsuchsulfurcrystal tolimittheaplicationofthedoctrineofequivalentstothe structuresinLi-Sbateriesandtheiroperationincarbonate scopeoftheclaims,eachnumericalparametershouldat electrolyte.Ithasbenpreviouslyreportedinether-based leastbeconstruedinlightofthenumberofreportedsig Li–Sbateriesthata-orthorhombicsulfuralotrope(the40nificantdigitsandbyaplyingordinaryroundingtech moststablesulfuralotropeatroomtemperature)inded niques.Notwithstandingthatthenumericalrangesand convertstotheB-monoclinicphaseandthatphasedominates parameterssetingforththebroadscopeofthedisclosureare afterthefirstchargecycle.Usingthisanalogy,wehypoth- aproximations,thenumericalvaluessetforthinthespecific esizethatthemonoclinicphaseisthermodynamicalymore examplesarereportedaspreciselyasposible.Anynumeri stableintheLi-Selectrolytemediumandistherefore45calvalue,however,inherentlycontainscertainerorsnec retainedinoursystemevenafterthechargingcycle.Nev- esarilyresultingfromthestandarddeviationfoundintheir ertheles,weobserveauniquemonoclinicphaseinthese respectivetestingmeasurements.Itisintendedthatthe chargedsamples,whichisdiferentfromtheB-monoclinic specificationandexamplesbeconsideredasexemplaryonly, phaseseninetherelectrolyteandthisposiblyplaysarole withatruescopeandspiritofthedisclosurebeingindicated inretainingsingleplateaubehaviorincharge-discharge50bythefolowingclaims. profilesforover2000cycles.AlexperimentswithLi-S Theforegoingembodimentsaresusceptibletoconsider celswerecariedoutatabout18-25°C.unlesotherwise ablevariationinpractice.Acordingly,theembodimentsare specified. notintendedtobelimitedtothespecificexemplificationsset SodiumSulfurCelsFIG.14Adisplaysacyclicvoltame- forthhereinabove.Rather,theforegoingembodimentsare trycurveofgammasulfurdeposited-CNFscathodewitha5withinthespiritandscopeoftheappendedclaims,including sodiumanodein1MNaC104inEC:DEC(1:1V/V)with5% theequivalentsthereofavailableasamateroflaw.Other FECatvariousscanrates.Inthereductioncurve,twopeaks suitablemodificationsandadaptationsofthevarietyof canbesenwhichareatributedtotheconversionofsulfur conditionsandparametersnormallyencounteredinthefield, toshortchainsodiumsulfidesNaS,andNaS,respectively. andwhichareobvioustothoseskiledintheart,arewithin Further,asimilartrendintheoxidationcurveissenwhere 60thescopeofthedisclosure. Na2SconvertstoNa2S2,andthenfinalytosulfur.FIG.14B Alpatentsandpublicationscitedhereinarefulyincor displaystherateperformanceofgammasulfurdeposited- poratedbyreferencehereinintheirentiretyoratleastforthe CNFsincarbonate-basedelectrolytes.Itdeliversahigh portionoftheirdescriptionforwhichtheyarespecificaly initialcapacityof780mAh/gata0.05Crate.Further citedorrelieduponinthepresentdescription. improvementintheCrateto0.1Cand0.2C,causesalos65 Thepatentesdonotintendtodedicateanydisclosed ofcapacityatributedtohighercurentdensitiesandlower embodimentstothepublic,andtotheextentanydisclosed timeforconversionandreaction,whichcapacitiesstabilized modificationsoralterationsmaynotliteralyfalwithinthe gammasulfurdeposited-CNFs,aswelasdischargedandPDF Image | SYNTHESIS OF GAMMA MONOCLINIC SULFUR
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