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US 10,991,944B2 9 10 FIG.13GshowshighresolutionS2pXPSspectraof chargedgammasulfurdepositedCNFsshowingthepres- enceofasulfurpeak. paternstomatchtheXRDpaternforthisphaseofsulfur. Themonoclinicgammaphasesulfurcanalsobeidentified byabestmatchtomonoclinicgammaphasesulfurusingthe FIGS.13Hand131showXPSspectraofdischargedand PDXLVersion2.8.4.0(IntegratedPowderDifractionSoft chargedsamplesoffluorine,respectively.Theformationof 5 warebyRigaku)databaseofXRD paternstomatchthe LiFlayersonthesurfaceandsomesaltspeciesindexedwere observedat-685.5eVad68eV,respectively.Theforma tionofLiFwasnotconsistentonthesurfaceasobservedin cycledSEMimages. XRDpaternforthisphaseofsulfur. TheXRDpaternsofFIGS.20A-20Bshowcomparisons of: 1.purealphaorthorhombicsulfur, FIG.14Ashowscyclicvoltametry(CV)curvesofa10 2.monoclinicgammaphasesulfuroftheinvention,an gammasulfurdepositedCNFscathodeatvariouscanrates. 3.thegammasulfur.ciffilefromtheNationalInstitutefor FIG.14Bshowstherateperformanceofagammasulfur MaterialsScience(NIMS)MaterialsDatabasediscusedin depositedCNFscathodeatvariouscurentdensities. Watanabe,Yasunari,“TheCrystalStructureofMonoclinic FIG.14Cshowsthecyclingstabilityofcathodesata0.1 15 Y-Sulphur,"Acta Cryst.(1974),B30,1396,The NIMS C rate. MaterialDatabasecanbefoundathtps:/mits.nims.go.jp/ FIG.14DshowsthepostmortemXRDpaternsofa index_en.html).InFIGS.20A-20Bpeaksofmonoclinic gammasulfurdepositedCNFscathode. gammaphasesulfursenat13.59+/-0.02matchexactly FIG.15AshowsCVcurvesofagammasulfurdeposited CNFscathodeat0.1mVs-1scanrates. with020(hkl)peaksofmonoclinicgammaphasesulfur FIG.15Bshowstherateperformanceofagammasulfur20fromthedatabase.Alphaphasesulfurhasnopeaksinthis depositedCNFscathode a0.5C te. sulfur,furthersugestingpreferentialorientationofthe FIG.16isaschematicofasulfurbateryofthepresent monoclinicgammaphasesulfurinthekdirection. inventionincludinganodeandcathodecurentcolectors25 Inadition,noneofthevapordepositedmonoclinic andaporousseparator. gammaphasesulfurpeaksmatchwiththealphaorthorhom FIG.17showsasurveyspectraofgammasulfurdepos- bicphase.Also,inthedatabase,themonoclinicgamma itedCNFs,whichshowstheexistenceofCls,S2p,andOls phasesulfurpeaksdonotoverlapwithanyalphaortho peaksinthecomposite. rhombicphase.Thissuportsaconclusionthatthepeaksof FIG.18Ashowsthecyclingstabilityofacarbonate30gammasulfurareuniqueinthehkldirection(010),(020), electrolyteat0.1Crate. (030),(040).(090)whencomparedtothecrystalstructure FIG.18Bshowsthecyclingstabilityofacarbonate database. electrolyteat0.5Crate. Furtherwhenthedatabasegammamonoclinicphaseis FIG.19showsthecyclingstabilityofanetherelectrolyte. comparedwiththebetamonoclinicphasenoneofthepeaks FIGS.20A-20Bshowcomparisonsof: 35andtheircorespondingintensitiesmatchwitheachother. 1.purealphaorthorhombicsulfur, PostmortemstudiesofcycledcelsusingXRD,XPSand 2.monoclinicgammaphasesulfuroftheinvention,and TEMfoundredoxproductsafterchargeanddischargecycles 3.thegammasulfur.ciffilefromtheNationalInstitutefor includingclearevidencefortheformationofLi2Sattheend MaterialsScience(NIMS)MaterialsDatabasediscusedin ofthedischargecycle.Inadition,thesestudiesindicatethat Watanabe,Yasunari,“TheCrystalStructureofMonoclinic40thesulfurrearangesitselftoyetanotheruncommon y-Sulphur,”ActaCryst.(1974),B30,1396,TheNIMS phasecyclo-deca-cyclo-hexasulfur,alsobelongingtothe MaterialDatabasecanbefoundathtps:/mits.nims.go.jp/ monocliniccrystalstructurefamily,afterthefirstcharge. depositedCNFscathodeatvariouscurentdensities. FIG.15Cshowsthecyclingstabilityofagammasulfur peakat040(hkl)whichdoesnotover-lapwithorthorhombic index_en.html). DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Nevertheles,noefectofsuchphaseshiftissenonthe electrochemicalredoxbehaviorasshownbygalvanostatic 45 charge-dischargetests.Thissemstobethefirstreportof thesetypesofstablesulfurcrystalstructuresinLi Scels orbateriesandtheiroperationincarbonateelectrolyte. Inthepresentinvention,ararephaseofsulfur—the Thecyclo-deca-cyclo-hexamonoclinicphasesulfurmay monoclinicgammaphasesulfur(Rosykite)isprovidedin beidentifiedbyabestmatchtoPDFCardNo.:01-072-4584 astableformonasuport.Thisenablessucesfuloperation50Quality:Sforcyclo-decasulfur-cyclo-hexasulfur,optionaly ofsulfurcelsandbateriesinacarbonateelectrolyteforup usingthePDXLVersion2.8.4.0(IntegratedPowderDifrac toormorethan4000cycles.Electrochemicalcharacteriza- tionSoftwarebyRigaku)databaseofXRDpaternstomatch tionsviagalvanostaticcharge-dischargetests,cyclicvolta- theXRDpaternforthisphaseofsulfur.Alternatively,the mmetry,diferentialcapacityandin-operandoEISmeasure- cyclo-deca-cyclo-hexamonoclinicphasesulfurmaybe ments sugest a redox mechanism that consistently5identifiedbyabestmatchtocyclo-decasulfur-cyclo-hexas eliminatesintermediatepolysulfidesovertheentire2000 ulfur,usingthePDXLVersion2.8.4.0(IntegratedPowder cycles,thuspreventingadversereactionswiththeelectro- DifractionSoftwarebyRigaku)databaseofXRDpaterns lyte. tomatchtheXRDpaternforthisphaseofsulfur. Thus,inoneembodiment,thepresentinventionrelatesto By“bestmatch”inthecontextofusingthesoftwareto acathodethatincludesmonoclinicgammaphasesulfurthat60matchaPDFcardismeantatypeofbestmatchalgorithm isstableattemperaturesupto80°C.,orattemperaturesof whichdeterminesthebestmatchofaparticularXRDpatent from0°C.to80°C.,orfrom15°C.to50°C.,orfrom18° tooneofthePDFcardsforformsofsulfur.Thus,as C.to40°C.,Themonoclinicgammaphasesulfurcanbe demonstratedbelow,notalpeaksoftheXRDpatentmust identifiedbyabestmatchtoPDFCardNo.:00-013-0141 matchthepaternonthePDFcardandnotalpeaksonthe Quality:BforRosickyite,monoclinicgammaphasesulfur,65PDFcaremustbepresentfortheretobeamatch.Rather,if optionalyusingthePDXLVersion2.8.4.0(IntegratedPow- thespecifiedsoftwaredeterminesthattheXRDpaternofa derDifractionSoftwarebyRigaku)databaseofXRD particularmaterialisabestmatchtothespecifiedPDFcard, region.Similarly,themonoclinicgammaphasesulfurhasaPDF Image | SYNTHESIS OF GAMMA MONOCLINIC SULFUR
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