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15 selectedfromthegroupconsistingofnaturalgraphite,artifi cialgraphite,graphiteoxide,graphitefluoride,graphitefiber, carbonfiber,carbonnano-fiber,carbonnano-tube, mesophase carbon micro-bead (MCMB) or carbonaceous micro-sphere(CMS),softcarbon,hardcarbon,andcombi nationsthereof. Graphiteoxidemaybepreparedbydispersingorimmers ingalaminargraphitematerial(e.g.,powderofnaturalflake graphiteorsyntheticgraphite)inanoxidizingagent,typicaly 16 between5%and20%byweight.Theoxygencontentcanbe determinedusingchemicalelementalanalysisand/orX-ray photoelectronspectroscopy(XPS). MultiplegrapheneshetsSuspendedinaliquid(e.g.water) may be spray-deposited to form a continuous film of graphenematerials,whichisdepositedwithacoatingofa cathode active material. The coated film is then broken into pieces of active material-coated graphene shets. These coatedgrapheneshetsarere-dispersedintoaliquidtoform aSuspension. TheresultingSuspensioncanbeconvertedintomicron scaleddroplets(particulates)usingseveralapproaches.For instance,theSuspensionmaybeaerosolizedoratomizedto formfineaerosolparticles.ConcurrentlyorSubsequently,the liquidorsolventisremovedtoformsolidparticlesthatare typicalysphericalorelipsoidalinshapewithadiameteror majoraxistypicalylesthan10.Thisproceduremaybe executedbyusinganaerosolgeneration,atomization,spray drying,orinkjetprintingaparatus.Asanoptionalbutpre feredprocedure,thesolidparticlesaresimultaneouslyor SubsequentlySubjectedtoapyrolysisorcarbonizationtreat menttoconverttheorganicorpolymericmaterial,ifexisting, intoacarbonmaterial.Theheattreatmentofpetroleumor coal-basedheavyoilorpitchwilservetoconvertatleastpart oftheoilorpitchintoameso-phase,anopticalyanisotropic orliquidcrystalinephaseofafusedaromaticringstructure. Theconvertedpitchiscaledameso-phasepitch.SinceNGPs areesentialypuregraphite-basedorgraphenematerials, thislowtemperatureheattreatment(350-1200°C.)hasno adverseefectontheNGPstructure.Esentialy,onecanuse aspraypyrolysistechnique,suchasultrasonicspraypyroly sisorelectro-spraypyrolysis,toaccomplishboththeaerosol generationandpyrolysisprocedures Anotherembodimentofthepresentinventionisalithium baterycathodecomprisingmultiplenanographene-en hancedcathodeparticulatesasdescribedabove.Afurther embodimentisalithiumbaterycomprisingSuchacathode, ananode,aseparatordisposedbetweentheanodeandthe cathode,andelectrolyteinphysicalcontactwithboththe anodeandthecathode. amixtureofanintercalant(e.g.,concentratedSulfuricacid)10 andanoxidant(e.g.,nitricacid,hydrogenperoxide,sodium perchlorate,potassiumpermanganate)atadesiredtempera ture(typicaly0-70°C.)forasuficientlengthoftime(typi caly30minutesto5days).Inordertoreducethetime requiredtoproduceaprecursorSolutionorSuspension,one may choose to oxidize the graphite to some extent for a shorterperiodoftime(e.g.,30minutes)toobtaingraphite intercalationcompound(GIC).TheGICparticlesarethen exposedtoathermalshock,preferablyinatemperaturerange of600-1,100°C.fortypicaly15to60secondstoobtain exfoliatedgraphiteorgraphiteworms,whichareoptionaly (butpreferably)Subjectedtomechanicalshearing(e.g.using amechanicalshearingmachineoranultrasonicator)tobreak upthegraphiteflakesthatconstituteagraphiteworm.The un-brokengraphitewormsorindividualgraphiteflakesare25 thenre-dispersedinwater,acid,ororganicsolventandultra SonicatedtoobtainagraphenepolymerSolutionorSuspen S1O. Thepristinegraphenematerialispreferablyproducedby oneofthefollowingthreproceses:(A)Intercalatingthe30 graphiticmaterialwithanon-oxidizingagent,followedbya thermalorchemicalexfoliationtreatmentinanon-oxidizing environment;(B)SubjectingthegraphiticmaterialtoaSuper criticalfluidenvironmentforinter-graphenelayerpenetration andexfoliation;or(C)Dispersingthegraphiticmaterialina 35 powderformtoanaqueousSolutioncontainingasurfactantor dispersingagenttoobtainaSuspensionandSubjectingthe Suspensiontodirectultrasonication. US9,203,084B2 15 InProcedure(A),aparticularlypreferedstepcomprises (i)intercalatingthegraphiticmaterialwithanon-oxidizing40 agent,selectedfromanalkalimetal(e.g.,potassium,Sodium, lithium,orcesium),alkalineearthmetal,oranaloy,mixture, Thereisnoparticularrestrictiononthetypeandnatureof oreutecticofanalkalioralkalinemetal;and(i)achemical exfoliationtreatment(e.g.,byimmersingpotassium-interca latedgraphiteinethanolsolution). 45 thecathodeactivematerial,whichcanbeselectedforprac ticingthepresentinvention.Thecathodeactivematerialmay bepreferablyselectedfromametaloxide/phosphate/sulfide, aninorganicmaterial,anorganicorpolymericmaterial,ora combinationthereof: InProcedure(B),apreferedstepcomprisesimmersingthe graphiticmaterialtoaSupercriticalfluid.Suchascarbon dioxide(e.g.,attemperatureT-31°C.andpressureP-7.4 MPa)andwater(e.g.,atT>374°C.andPd22.1MPa),fora sulfidesconsistingoflithiumcobaltoxide,lithiumnickel periodoftimeSuficientforinter-graphenelayerpenetration50 (tentativeintercalation).ThisstepisthenfollowedbyaSud dende-presurizationtoexfoliateindividualgraphenelayers. Othersuitablesupercriticalfluidsincludemethane,ethane, ethylene,hydrogenperoxide,oZone,wateroxidation(water containingahighconcentrationofdissolvedoxygen),ora mixturethereof. InProcedure(C),apreferedstepcomprises(a)dispersing particlesofagraphiticmaterialinaliquidmediumcontaining thereinasurfactantordispersingagenttoobtainasuspension orslury;and(b)exposingtheSuspensionorslurytoultra Sonicwaves(aprocesscommonlyreferedtoasultrasonica tion)atanenergylevelforaSuficientlengthoftimeto producetheseparatednano-scaledplatelets,whicharepris tine,non-oxidizedNGPs. NGPscanbeproducedwithanoxygencontentnogreater than25%byweight,preferablybelow20%byweight,further preferably below 5%. Typicaly, the oxygen content is 55 60 65 oxide,lithiummanganeseoxide,lithiumVanadiumoxide, lithiumtransitionmetaloxide,lithium-mixedmetaloxide, lithium iron phosphate, lithium manganese phosphate, lithiumVanadiumphosphate,lithiummixedmetalphos phates,transitionmetalSulfides,andcombinationsthereof. a. In particular, the lithium Vanadium oxide may be selectedfromthegroupconsistingofVO, LiVO, V2Os, LiV2Os. VOs, LiVOs, LiVO7. VO9. LiVO,VO, LiVO,theirdopedversions,their derivatives, and combinations thereof, wherein 0.1PDF Image | CATHODE ACTIVE MATERIAL-COATED DISCRETE GRAPHENE SHEETS FOR LITHIUM
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