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US9,203,084B2 56 phthalocyaninechloride,cadmiumphthalocyanine, Inapreferedversionoftheproces,thecontinuousfilmof chlorogalliumphthalocyanine,cobaltphthalocya nine,silverphthalocyanine,ametal-frephthalocya nine,achemicalderivativethereof,oracombination thereof. agraphenematerialmaybeproducedby(a)sprayinga graphene Suspension onto a solid Substrate, wherein the grapheneSuspensioncontainsagraphenematerialdispersed inaliquidmedium,and(b)byremovingsaidliquidmedium. Alternatively,thecontinuoussheetofagraphenematerial maybeproducedbychemicalvapordepositionofagraphene materialontoasolidSubstrate. Thecoatedfilm(theshetofacathodeactivematerial coatedgraphenematerialfilm)preferablyhasacathode activematerialcoatingthickneslesthan500nm,more preferablylesthan100nm,furtherpreferablylesthan50 nm,mostpreferablylesthan20nm.Thecoatedfilmmaybe producedthroughchemicalvapordeposition,physicalvapor Multipleshetsofcathodeactivematerial-coatedgraphene15 maybecombined,withaditionalgrapheneshets(optional) orotherconductiveaditives(optional),toformasecondary particlehavingasizepreferablylesthan20um,further preferablylesthan10 Lim,andmostpreferablylesthan5 um.Theaditionalconductiveaditiveincorporatedintothe secondaryparticlesmaybeacarbonorgraphitematerial selectedfrompolymericcarbon,amorphouscarbon,chemi calvapordepositioncarbon,coaltarpitch,petroleumpitch, meso-phasepitch,carbonblack,coke,acetyleneblack,acti vatedcarbon,fineexpandedgraphiteparticlewithadimen25 sionSmallerthan100nm,artificialgraphiteparticle,natural um,preferablylesthan10um,andmorepreferablylesthan Thegraphenematerialisselectedfrompristinegraphene, grapheneoxide,reducedgrapheneoxide,graphenefluoride, graphenebromide,grapheneiodide,boron-dopedgraphene, nitrogen-doped graphene, chemically functionalized graphene,oracombinationthereof,andthegraphenemate10 rialcomprisessingle-layerorlesthan10grapheneplanes. Preferably,thecathodeactivematerialcoatinghasathickness lesthan100nm,morepreferablylesthan50nm,andmost preferablylesthan20nm. graphiteparticle,oracombinationthereof. Theinventionalsoprovidesalithiumbaterycontainingan anodeelectrode,acathodeelectrodeasdescribedabove,a porousseparatorand/orelectrolyteincontactwiththeanode30 electrodeandthecathodeelectrode.Thelithiumbaterymay furthercompriseananodecurentcolectorand/oracathode curentcolector.Thelithiumbaterymaybealithiummetal secondarybatery,whereintheanodeelectrodecontainsa lithiummetal,lithiummetalaloy,orlithiumcompoundasan35 5um.Preferably,thissecondaryparticleissphericalinshape. Thestepofshapingmultiplepiecesofcathodeactivemate rial-coatedgraphenematerialintoasecondaryparticlemay comprisedispersingthemultiplepiecesofcathodeactive material-coatedgrapheneinaliquidmediumtoformamulti componentsuspensionanddryingthemulti-componentsus pensiontoformthesecondaryparticleusingaspray-drying, spray-pyrolysis,fluidized-beddrying,atomization,oraero Solizingtechnique. 5 anodeactivematerial.Thelithiumbaterymaybealithium Inapreferredproces,Step(b)furthercomprisesdeposit sulfur cell wherein the anode electrode contains a lithium metal,lithiummetalaloy,orlithiumcompoundasananode activematerialandthecathodeelectrodecontainsSulfur, Sulfurcompound,orlithiumpolysulfideasacathodeactive40 material. ingalayerofcarbonorgraphitematerialontoasurfaceofthe shetofcathodeactivematerial-coatedgraphene.Thiscar bonorgraphitematerialcanactasaSupplementaryconduc tiveaditivethatworkswithgraphenetoformarobust3-D networkofelectron-conductingpaththatremainsincontact withthecathodeactivematerialduringthebaterychargeand discharge.Thiscarbonorgraphitematerialisselectedfrom polymericcarbon,amorphouscarbon,chemicalvapordepo sitioncarbon,coaltarpitch,petroleumpitch,meso-phase pitch,carbonblack,coke,acetyleneblack,activatedcarbon, fineexpandedgraphiteparticlewithadimensionSmallerthan Thepresentinventionalsoprovidesacathodeactivemate rial-coatedgrapheneshetsandaprocessforproducingSuch agraphene-enhancedcathodeactivematerial.Theprocess comprises(a)providingacontinuousfilmofagraphene45 materialintoadepositionZone;(b)introducingvaporor atomsofaprecursorcathodeactivematerialintothedeposi tionZone,allowingthevapororatomstodepositontoa 100nm,artificialgraphiteparticle,naturalgraphiteparticle, surfaceofthegraphenematerialfilmtoformacoatedfilmof acathodeactivematerial-coatedgraphene;and(c)mechani50 calybreakingthiscoatedfilmintomultiplepiecesofcathode activematerial-coatedgrapheneshets;whereinthegraphene materialisinanamountoffrom0.1%to99.5%byweightand thecathodeactivematerialisinanamountofatleast0.5%by weight,albasedonthetotalweightofthegraphenematerial55 andthecathodeactivematerialcombined. oracombinationthereof.Thepolymericcarbonoramor phouscarbonmaybeobtainedfrompyrolyzationofapoly merselectedfromthegroupconsistingofphenol-formalde hyde,polyacrylonitrile,Styrene-basedpolymers,celulosic polymers,epoxyresins,andcombinationsthereof. Theprocessmayfurthercompriseastepofseparatingor removingtheSupportinggrapheneshetfromthecathode activematerialsandastepofcolectingtheseparatedcathode activematerial.ThisisaSurprisinglysimpleandcost-effec tivewayofmass-producingfre-standing,nanometer-thin cathodeactivematerials(e.g.asthinas2-20nmwithalength/ widthfrom30nmtoseveralmicrons).Nopriorartmethod oferssuchaversatilecapability. Steps(a)and(b)canbeconductedinarol-to-rolmanner thatincludesfeedingacontinuousfilmofagraphenematerial fromafeederrolerintoadepositionZoneandcolectingthe coatedfilmontoawindingroler. 60 Thegraphenematerialmaybeselectedfrompristine graphene,grapheneoxide,reducedgrapheneoxide,graphene Alternatively,theprocesscanfurthercompriseastepof fluoride,graphenebromide,grapheneiodide,boron-doped graphene,nitrogen-dopedgraphene,chemicallyfunctional izedgraphene,oracombinationthereof,andthegraphene65 materialispreferablyofsingle-layerorfew-layershets(les than10grapheneplanes). mixingmultiplepiecesofcathodeactivematerial-coated grapheneshets,aditionalun-coatedgrapheneshet(s),and aconductivefilertoformasecondaryparticle.Suchasec ondaryparticlemaybecomposedofSmallactivematerial coatedgrapheneshets(e.g.<3uminlength)andconductive deposition,Sputering,orlaser-asistedthin-filmdeposition ofananodeactivematerialontoashetofagraphenemate rial. Intheproces,step(c)ofmechanicalbreakingcanbe conductedusingairjetmiling,impactmiling,grinding. mechanicalshearing,ultrasonication,oracombination thereof. Theprocesscanfurthercompriseastepofshapingthose multiplepiecesofcathodeactivematerial-coatedgraphene materialintoasecondaryparticlehavingasizelesthan20PDF Image | CATHODE ACTIVE MATERIAL-COATED DISCRETE GRAPHENE SHEETS FOR LITHIUM
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