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11 12 US 10,991,944B2 thenthesulfurforwhichtheXRDpaternhasbenobtained minute,orfrom1minuteto10hours,or1minuteto48 isconsideredtobewithinthescopeofthepresentinvention. hours,orfrom10to30hours,orfrom20to28hours,orfor AssenfromtheSEMimages,FIGS.3A-3D,8B,9B-9C, about24hours. and12A-12Cshowthethatthegammamonoclinicphase Thevapordepositionstepisfolowedbyastepofcoling, sulfurisnon-confinedasitshowsblocksofsulfurin-5whichmaybecariedoutbyexposingthevapordeposition betweentheinterfibercarbon-nanofiberspacing.TheXRD aparatusorthesampletoatemperatureoflesthan50°C., datashowsthepresenceofcrystalinepeaksdenotingthe oranenvironmentaltemperatureoflesthan25°C.,orfrom presenceofgammamonoclinicphasesulfuronCNFs.See about-20°C.toabout25°C.orfrom0°C.toabout25°C., FIGS.9a,13A-13B,and14D.Thepresentinvention orfromabout20°C.toabout25°C.,orfromabout20°C. employsaporousmaterialthus,apartialdepositionofsulfur10to2°C.Insomeembodiments,thevapordeposition mighttakeplaceinthepores.Curentmethodsemploying aparatusiscoledimediatelyuponcompletionofthe carbonateelectrolyteareonlyefectivewhensulfuriscon- vapordepositionstep. fined,incontrast,theelectrodesofthepresentinventionare Theporousmaterialemployedforthesubstrateinthe capableofworkingdespitebeingnon-confined.Theinven- presentinventionmaybeconductiveornon-conductive,and torstheorizethatthisisduetogammamonoclinicgamma 15preferablyisselectedfromasubstratecomprisingcarbon phaseofsulfur. nanofibers,amatofcarbonnanofibers,fre-standingcarbon Inthepresentinvention,gammamonoclinicphasesulfur nanofibers,conductivecarbonpowders,carbonnanotubes, issynthesized/depositedonasuportforacathodeofa graphene,andcarbide-derivedcarbons.Afterthestepof sulfurcel.Despiteanexposedun-confineddepositionof depositingthegammamonoclinicphasesulfur,theporous this sulfur phase on a substrate,carbonate-based cels 20 materialmayhaveaporevolumeof10-95%.Furthermore, employingthissulfurphaseexhibitahighreversiblecapac- duringthemethodandparticularlythevapordeposition ityof,forexample,70mAh/gafter20cycles,or50 step,theporousmaterialispreferablylocatedinthevapor mAh/gafter4000cycles,bothatC/2rate,or50mAh/g depositionaparatussuchthattheporousmaterialdoesnot after80cyclesatC/10.LiSelectrodeswiththissulfur contactwiththeliquidsulfur. phasealsoexhibitahighrateperformanceuptoa40Crate25TheCathode andahigharealloadingofsulfurofupto5mg/cm2.The Thecathodeofthepresentinventionmaybepreparedby electrodemayconsistoffrestanding,binderandcurent themethodofdepositinggammamonoclinicphasesulfur colector-frecarbonnanofibers.Aftersulfurdepositionand viavapordepositionontoasubstrateasdescribedabove. slowcolingatroomtemperatureinanautoclave,thesulfur Thepristinecathodeincludesmonoclinicgammamono adoptstheuncommonmonoclinicgammaphasestructure30clinicphasesulfuronasubstrate.Thegammamonoclinic ratherthanthetypicalorthorhombicalphaphase,evenon phasesulfurloadingonthecathodemaybeinarangeof theexternalsurfaceofasubstratesuchascarbonnanofibers. fromabout1.0mg/cm2toabout150mg/cm2orfromabout Thismonoclinicgammaphaseremainsstableatroom 5mg/cm2toabout125mg/cm2orfromabout10mg/cm2to temperatureforoverayearwithnoaparentevidenceofa about15mg/cm2,oratleastfromabout25mg/cm2. phasechangeevenbeyondthistimeframe.Extensiveelec-35 Thecathodemayhaveaninitialdischargecapacityina trochemicalcharacterizationandpostmortemspectroscopy/ rangeoffromabout30mAh/gtoabout2500mAh/g,or microscopystudiesoncycledcelsrevealanalteredredox fromabout350mAh/gtoabout2000mAh/g,orfromabout mechanismthatreversiblyconvertsmonoclinicsulfurto 375mAh/gtoabout1700mAh/g,orfromabout400mAh/g Li2Swithouttheformationofintermediatepolysulfidesover toabout130mAh/g,orfromabout600mAh/gtoabout uptoandbeyond2000cycles.Thedevelopmentofnon-4010mAh/g,orfromabout750mAh/gto90mAh/g,or confinedhighloadingsulfurcathodesforuseinbateries 80mAh/g,basedonatotalweightofthesulfurinthe employingcarbonate-basedelectrolytescanrevolutionize cathode. thefieldofhighenergydensitypracticalbateries. Thecathodeofthepresentinventionmayoptionaly Thepresentinventionemploysamonoclinicgamma includeacathodecurentcolectorthoughacurentcolector phasesulfurthatenablesasingleplateaulithium-sulfur45wilnottypicalyberequired. reactionin,forexample,acarbonateelectrolytesystem.This TheAnode systemavoidstheformationofpolysulfidesduringcharge- Theanodesofthepresentinventionareionreservoirs, discharge.Asaresult,itisexpectedthatthemonoclinic optionalyincludinganactivematerialselectedfromalkali gammaphasesulfurwilhavealongcyclelifeinabatery, metals,alkalinemetals,transitionmetals,graphite,aloys, evenifacarbonateelectrolytesystemisemployed. 50andcompositions. MethodforPreparingaCathodeViaVaporDeposition Suitableexamplesofactivematerialsmaybeselected Inoneembodiment,thegammamonoclinicphasesulfur fromlithium,sodium,potasium,magnesium,calcium,zinc, maybedepositedonasubstrateviavapordeposition.Vapor coper,titanium,nickel,cobalt,iron,aluminum,silicon, depositioniscariedoutinasealedvapordepositionapa- germanium,tin,lead,antimony,bismuth,manganese,and ratusatatemperaturesuficienttovaporizesulfurandfora5cadmium,andlithiatedversionsthereof.Theactivemateri timesuficienttoprovidegammamonoclinicphasesulfur. alsoftheanodesmayalsobealoysorintermetalicselected Oncethegammamonoclinicphasesulfurisdepositedonthe fromcompoundsoflithium,sodium,potasium,magne substrate,itiscoledtoambienttemperatureofabout sium,calcium,zinc,coper,titanium,nickel,cobalt,iron, 18-25°C.Preferably,thesulfurloadingonthesubstrateisat aluminum,silicon,germanium,tin,lead,antimony,bismuth, least0.05mg/cm2.Forthispurpose,itmaybedesirableto60manganese,andcadmium,andlithiatedversionsthereof, employaporoussubstrateinordertoincreasethesurface wherethealoysorcompoundsarestoichiometricornon areaofthesubstrateavailableforsulfurdeposition. stoichiometric. Suitabletemperaturesforcaryingoutthevapordeposi- Insomeembodimentstheactivematerialsoftheanode tionmayrangefromabout140°C.to350°C.,orfrom140° maybeoxides,carbides,nitrides,sulfides,phosphides, C.to250°C.,orfrom150°C.to210°C.,orfrom160°C.65selenides,andteluridesoflithium,sodium,potasium, to190°C.,oratabout175°C.Preferably,thevapor magnesium,calcium,zinc,coper,titanium,nickel,cobalt, depositioniscariedoutforaperiodofatleastabout1 iron,aluminum,silicon,germanium,tin,lead,antimony,PDF Image | SYNTHESIS OF GAMMA MONOCLINIC SULFUR
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