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US 10,991,944B2 34 Theaforementionedisuesofether-basedelectrolytescan 2Na+xS Na2Sx becircumventedbyusingacarbonate-basedelectrolyte. Similartoi-Sbateries,roomtemperaturesodium-bater Carbonate-basedelectrolytesystemsareusedinusedin iesfaceproblemsasociatedwithachievingchargecapacity comercialLi-ionbateries(LIBs)duetotheirsafeand closetotheoreticalandretainingchargewithrepeated stablepropertiesaswelastheirbroadoperatingtemperature5cycling.Assuch,comercialyavailableNa Sbateries window.Also,avarietyofhigh-temperaturesaltshaveben typicalyoperateattemperaturesof30-350°C.sothatthey investigatedanddesignedforcarbonate-basedelectrolytes mayemploymoltensodiumandsulfurphasesinconjunction forthecommercialLi-ionbaterymarkettofurtherenhance withasolid,ceramicelectrolyteinordertomitigatethe theirreliability. However,theuseofsulfur-basedcathodesincombination 10 shutle-effect. withcarbonate-basedelectrolytesresultsintheireversible Potasium-bateries,magnesium-bateries,andcalcium formationofundesirableby-productssuchasthiocarbonate bateriesposesimilarproblemsassodium-bateries.Specifi andethyleneglycol,whichrenderthebaterynon-func- caly,potasium-bateriesarelargerandthusexperience tional.Recentdevelopmentsinsulfurcathodeshave evenmoresignificantproblems. improvedsystemsemployingcarbonate-basedelectrolytes15 forLi-Sandothersulfur-basedbateriesusingalternate anodessuchasMgNa,andCa. Li-Sbaterieswithcarbonateelectrolyterequirecon- Inafirstaspect,thepresentinventionrelatestoamethod finementofthesulfurinnanopores.Asaresult,thecom- ofdepositingmonoclinicsulfuronasubstrate.Inthe plicatedarchitecturerequiredtoimplementthesesulfur20method,monoclinicphasesulfurthatisstableatatempera cathodeswiththesulfurconfinedinthenanoporesrestricts turebelow80oC.isdepositedviavapordepositionontoa theircomercialaplicationandreducesthesulfurloading substratewhichmaybeaporousmaterialinasealedvapor ofsuchbateries. depositionaparatusatatemperaturesuficienttovaporize GammaandBetaphasesofsulfuraredificulttosynthe- thesulfurandforatimesuficienttoprovidethemonoclinic sizeandaretypicalymetastableatroomtemperature.25phasesulfur,andthemonoclinicphasesulfurdepositedon Curentmethodsofsynthesizinggammaphasesulfurarenot thesubstrateiscoledtoatemperatureof0-50°C.or15-40° entirelyunderstoodwithonlyafewarticlespublishedinthe C.or18-25°C. past 150 years.When exposed to ambient air,gamma Inthemethod,acathodesuitableforuseinanelectrode monoclinicphasesulfurisexpectedtoconvertbacktoa ofacelorbaterymaybeproduced. stableorthorhombicstructure,themostcommonphaseof30 Ineachoftheforegoingembodiments,aloadingofthe sulfur. monoclinicphasesulfuronthesubstrateofatleast0.05 Theuseofcomercialyviablecarbonate-basedelectro- mg/cm2,oratleast0.5mg/cm2,canbeprovided. lytesforion-basedsulfurbateriesleadstotheformationof Intheforegoingembodiment,theheatingstepmaybe ireversibleproducts(thiocarbonateandethyleneglycol) cariedoutatatemperatureoffrom140°C.toabout350° duetothereactionbetwenpolysulfidespeciesandelectro-35C.,orfrom140°C.to250°C.,orfrom150°C.to210°C., lyte.Recently,strategiessuchasconfiningsmalersulfur orfrom160°C.to190°C.,oratabout175°C. molecules(S2-S4)inmicroporouscarbon(poresize<0.5 Ineachoftheforegoingembodiments,theheatingstep nm),croslinkingsulfurmoleculestopolymericmaterials maybecariedoutforaperiodofatleastabout1minute, andformationofSolidElectrolyteInterphase(SEI)haveled orfrom1minuteto10hours,or1minuteto48hours,or touseofcarbonate-basedelectrolytesresultinginasolidto40from10to30hours,orfrom20to28hours,orforabout24 solidconversion. hours. Ambienttemperature(about18-25°C.)sodium-sulfur Ineachoftheforegoingembodiments,thecolingstep bateries(Na—S)arealsoknownintheartandareof maybecariedoutbyexposingthevapordepositionappa interestduetotheirtheoreticalyhighenergydensityand ratusorthesampletoatemperatureofequaltoorlesthan lowcost.Moreover,ascomparedtolithiumbateries,Na-S4550°C.,orfromabout-20°C.toabout25°C.orfrom0°C. bateriesavoidtheuseofrelativelyexpensiveLiinfavorof toabout25°C.,orfromabout20°C.toabout25°C.,or Na. fromabout20°C.to22°C. Lithiumionbateriescomprisecathodesusualymade Ineachoftheforegoingembodiments,thevapordepo from LiFePO (LFP), LiMn04 (LMO), and sitionaparatusmaybecoledimediatelyuponcomple LiNi,Co,Mni2x1uxl202(NCM),andanodematerialsthatmay 50tionoftheheatingstep. includeLiTiz012(LTO)andgraphite(C).Totestindividual Ineachoftheforegoingembodiments,thesubstratemay capacitiesofthecathode(NCM)andanode(Graphite),they beaporousmaterialhavingaporevolumeof10-95%,after arecoupledwithlithiumandperformanceisevaluated. thestepofdepositingthemonoclinicphasesulfur. FurthercathodessuchasNCMandgraphitearecoupledto Ineachoftheforegoingembodiments,thesubstratemay formafulcel.ThevoltagewindowofLi|NCMis3-4V 5beconductiveornon-conductive.Ineachoftheforegoing andLilgraphiteis0.6-0.01Vandthecoupledvoltagewin- embodiments,thesubstratemayincludecarbonnanofibers dowis3-3.5V.Hence,whensulfurcathodesarecoupled suchasamatofcarbonnanofibersorfre-standingcarbon withdiferentmetaloxide/graphiteanodes,thevoltagewin- nanofibers. dowistypicalydiferent. Ineachoftheforegoingembodiments,thesubstratemay Ambienttemperaturesodium-bateries,potasium-bater-60belocatedinthevapordepositionaparatuswithagap ies,magnesium-bateries,andcalcium-bateriesmaycom- betwenthesurfaceofaliquidsulfurreservoirandthe priseacathodeincludingsulfur,ananodeincludingsodium, substratesuchthatthesubstratedoesnotcomeintocontact potasium,magnesium,orcalcium,andanelectrolyte.Gen- withliquidsulfurduringthevapordepositionstep. eraly,duringthebaterydischargecycle,polysulfidesare Ineachoftheforegoingembodimentsofthemethod,the reducedonthecathodesurfaceandduringthebatery65monoclinicphasesulfurmaycompriseaformofsulfur chargingcycle,polysulfidesareformedatthecathode.For selectedfromthegroupconsistingofmonoclinicgamma example: SUMMARY OF THE INVENTION phasesulfur;monoclinicsulfurthatbestmatchesmonoclinicPDF Image | SYNTHESIS OF GAMMA MONOCLINIC SULFUR
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