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US 9,905,856 B1 38 AcertainamountofthedriedTPMparticlesisthenput and,separately,impregnatedafoamedcathodecurentcol intomuflefurnaceandcalcinedat40°C.-60°C.for25lectorwiththesecondsuspensiontoformacathodelayer. hoursunderairpurgingtoremovethecarboncontentfrom Theanodelayer,aporousseparatorlayer,andthecathode thenanocomposite,producinggraphene-freyelow-color layerwerethenassembledandhousedinapouchtoforma siliconnanopowders.BothSinanopowderandgraphene cel.Withtheinstantmethod,typicalynobinderresinis wrappedSinanoparticleswereusedasahigh-capacity neededorused,saving8%weight(reducedamountof 37 yelowpasteandblendtheyelowpastetopowders.The cathodecurentcolector.Thepouchwasthensealed.In as-preparednanoparticlehasaSSAvaluerangeof30m?lg otherexamples,weimpregnatedafoamedanodecurent to20m2/gduetodiferentratioofgraphenecontents colectorwiththefirstsuspensiontoform ananodelayer anodeactivematerial. 10 non-activematerials). Thecyclicvoltammetry(CV)measurementswerecaried Example14:Graphene-EnhancedTinOxide outusinganArbinelectrochemicalworkstationatatypical ParticulatesasanAnodeActiveMaterial scanning rateof 1mV/s.In addition,theelectrochemical performances ofvarious celswere also evaluatedby gal Tinoxide(SnO2)nanoparticles,ananodeactivematerial,15vanostaticcharge/dischargecyclingatacurentdensityof wereobtainedbythecontroledhydrolysisofSnC14.5H20 from50mA/gto10Alg.Forlong-termcyclingtests, withNaOHusingthefolowingprocedure:SnC14.5H20 multi-chanelbaterytestersmanufacturedbyLANDwere (0.95g,2.7m-mol)andNaOH(0.212g,5.3m-mol)were used. disolvedin50mL ofdistiledwatereach.TheNaOH Itmaybenotedthat,inlithium-ionbateryindustry,itis solutionwasadeddrop-wiseundervigorousstiringtothe20acommonpracticetodefinethecyclelifeofabateryasthe tinchloridesolutionatarateof1mL/min.Thissolutionwas numberofcharge-dischargecyclesthatthebaterysufers homogenizedbysonicationfor5min.Subsequently,the 20%decayincapacitybasedontheinitialcapacitymea resultinghydrosolwasreactedwiththeGOdispersionfor3 suredaftertherequiredelectrochemicalformation.The hours.Tothismixedsolution,fewdropsof0.1MofH,SO. samedefinitionforthecyclelifeofaLi–Sorroom wereaddedtofloculatetheproduct.Theprecipitatedsolid 25temperatureNa-Scelishereinfollowed. was colectedby centrifugation,washed withwaterand ethanol,anddriedinvacuum.Thedriedproductwasheat treatedat40°C.for2hunderAratmosphere. Example 15:PreparationandElectrochemical TestingofVariousBateryCels Example16:RepresentativeTestingResults Foreach sample,severalcurentdensities(representing 30 charge/dischargerates)wereimposedtodeterminetheelec trochemicalresponses,alowingforcalculationsofenergy densityandpowerdensityvaluesrequiredoftheconstruc Formostoftheanodeandcathodeactivematerials tionofaRagoneplot(powerdensityvs.energydensity). investigated,wepreparedalkalimetal-sulfurcelsoralkali ShowninFIG.5areRagoneplots(gravimetricandvolu metalion-sulfurcelsusingboth thepresentlyinvented 35metricpowerdensityvs.energydensity)ofNa-ionbatery celscontaininghardcarbonparticlesastheanodeactive Withtheconventionalmethod,atypicalanodecomposi materialandactivatedcarbon/sulfurcompositeparticlesas tionincludes85wt.%activematerial(e.g.,Sn-or thecathodeactivematerials.Twoofthe4datacurvesarefor Na2C2H404-coatedgrapheneshetsforNaion-sulfur thecelspreparedacordingtoanembodimentofinstant anode;graphiteorSiparticlesforLiion-sulfuranode),7wt.40inventionandtheothertwoby theconventionalslury %acetyleneblack(Super-P),and8wt.%polyvinylidene coatingofelectrodes(rol-coatingofslury).Severalsig fluoridebinder(PVDF,5wt.%solidcontent)disolvedin nificantobservationscanbemadefromthesedata: N-methyl-2-pyrolidinoe(NMP).Aftercoatingthesluries Boththegravimetricandvolumetricenergydensitiesand onCu foil,theelectrodesweredriedat120°C.invacuum powerdensitiesoftheroom-temperaturesodium ion-Sbat for2htoremovethesolvent.Cathodelayersaremadeina45 terycelspreparedbythepresentlyinventedmethod(de similarmanner(usingAlfoilasthecathodecurentcolec- notedas“cable”inthefigurelegend)aresignificantlyhigher tor).Ananodelayer,separatorlayer(e.g.Celgard2400 thanthoseoftheircounterpartspreparedviatheconven membrane),andacathodelayerarethenlaminatedtogether tionalrol-coatingmethod(denotedas"conventional”).A andhousedinaplastic-Alenvelop.Thecelistheninjected changefromananodethicknesof150um(coatedonaflat with1MLiPF orNaPF,electrolytesolutiondissolvedina50 solidCufoil)toathicknessof225um (alaccommodated mixtureofethylenecarbonate(EC)anddiethylcarbonate inporesofaNifoamhaving85%porosity)andacorre (DEC)(EC-DEC,1:1v/v).Insomecels,ionicliquidswere spondingchangeinthecathodetomaintainabalanced usedastheliquidelectrolyte.Thecelassembliesweremade capacityratioresultsinagravimetricenergydensity inanargon-filedglove-box. increasefrom 15Wh/kgto185Wh/kg.Evenmoresur Inthepresentlyinventedprocess,incertain examples,the 5 prisingly,thevolumetric energy density is increased from anodecurentcolector(conductiveporousstructureforthe 232Wh/Lto314Wh/L. anode),theseparator,andthecathodecurentcolector Thesesignificantdiferencescanotbesimplyascribedto (conductiveporousstructureforthecathodeside)are theincreasesintheelectrodethicknesandthemassloading. assembledinaprotectivehousingbeforeoraftertheinject- Thediferencesarelikelyduetothesignificantlyhigher ing(orimpregnation ofthefirstsuspensionand/orthe60activematerialmassloading(relativetoothermaterials) injecting(orimpregnation)ofthesecondsuspension.In asociatedwiththepresentlyinventedcels,reducedpro someexamples,weassembledanemptyfoamedanode portionofoverhead(non-active)componentsrelativetothe currentcolector,aporousseparatorlayer,andanempty activematerialweight/volume,noneedtohaveabinder foamedcurrentcolectortogethertoformanassemblythat resin,surprisinglybeterutilizationoftheelectrodeactive washousedinapouch(madeofAl-nylonbi-layerfilm).The 65material(most,ifnotal,ofthehard carbon particlesand firstsuspensionwastheninjectedintotheanodecurrent C/Sparticlescontributingtothesodiumionstoragecapac colectorandthesecondsuspensionwasinjectedintothe ity;nodrypocketsorinefectivespotsintheelectrode, methodandtheconventionalmethod.PDF Image | FLEXIBLE AND SHAPE-CONFORMAL ROPE-SHAPE ALKALI METAL-SULFUR BATTERIES
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