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17 18 US 9,905,856 B1 than95%byvolume.Thebackboneofthefoamorthefoam Walsforcesinthethicknesdirectionwithaninter-gra walsformsanetworkofelectron-conductingpathways. pheneplanespacingofaproximately0.354nmiscom Thesefoam structurescanbereadilymadeintoany monlyreferredtoasamulti-layergraphene.Amulti-layer cros-sectionalshape.Theyalsocanbeveryflexible;typi grapheneplatelethasupto300layersofgrapheneplanes caly,non-metallicfoamsbeingmoreflexiblethanmetallic 5 (<100nm inthickness),butmoretypicallyupto30gra foams.However,metalnano-fiberscanbemadeintohighly pheneplanes(<10nminthicknes),evenmoretypicalyup flexiblefoams.Sincetheelectrolyteisineitheraliquidor to20grapheneplanes(<7nminthicknes),andmost gelstate,theresultingcablebattery canbevery flexibleand typicalyupto10grapheneplanes(commonly referredtoas canbemadetobeconformaltoesentialyanyoddshape. few-layergrapheneinscientificcommunity).Single-layer Evenwhenthesaltconcentrationinaliquidsolventishigh 10grapheneandmulti-layergrapheneshetsarecollectively (e.g.from2.5Mto15M),thefoamstructurecontaining caled“nanographeneplatelets”(NGPs),asshownisFIG. electrolyteinsidetheirporesremainsdeformable,bendable, 2.Grapheneshets/platelets(colectively,NGPs)areanew twistable,andconformabletoevenanodshape. clasofcarbonnanomaterial(a2-Dnanocarbon)thatis Insomeembodiments,theelectricalyconductiveporous distinctfromthe0-Dfulerene,the1-DCNTorCNF,and rodinthefirstorsecondelectrodecontainsaconductive15the3-Dgraphite.Forthepurposeofdefiningtheclaimsand polymerfiber,acarbon/graphitefiber,afibertow,fiberyarn, asiscommonlyunderstoodintheart,agraphenematerial fiberbraid,fiberknitstructurethatismadeofaconductive (isolatedgrapheneshets)isnot(anddoesnotinclude)a polymer,carbon,orgraphitefiberandisporous. carbonnanotube (CNT)oracarbonnano-fiber(CNF). Preferably,substantialy alofthepores intheoriginal Inoneprocess,graphenematerialsareobtainedbyinter conductiveporousrodsorfilamentsarefiledwith the20calatingnaturalgraphiteparticleswithastrongacidand/or electrodeactivematerial(anodeorcathode),electrolyte,and anoxidizingagenttoobtainagraphiteintercalationcom optionalconductiveaditive(nobinderresinneeded).Since pound(GIC)orgraphiteoxide(GO),asilustratedinFIG. therearegreatamountsofpores(moretypicaly70-99%or 4(A)andFIG.4(B)(schematicdrawings).Thepresenceof preferably85%-99%)relativetotheporewalsorconduc- chemicalspeciesorfunctionalgroupsintheinterstitial tivepathways(1-30%),verylitlespaceiswasted(“being 25 spacesbetweengrapheneplanesinaGIC orGO servesto wasted”meansnotbeingoccupiedbytheelectrodeactive increasetheinter-graphenespacing(dom,asdeterminedby materialandelectrolyte),resultinginhighproportionof X-raydifraction),therebysignificantlyreducingthevander electrodeactivematerial-electrolytemixture(highactive Waalsforcesthatotherwiseholdgrapheneplanestogether materialloadingmass). alongthec-axisdirection.TheGIC orGO ismostoften Insuchbateryelectrodeconfigurations(e.g.FIG.1(C),30 produced by immersingnaturalgraphitepowder (10 in theelectronsonlyhavetotravelashortdistance(halfofthe FIG.4(B)inamixtureofsulfuricacid,nitricacid(an poresize,onaverage;e.g.nanometersorafewmicrometers) oxidizingagent),andanotheroxidizingagent(e.g.potas beforetheyarecolectedbytheporewallssinceporewals siumpermanganateorsodiumperchlorate).Theresulting arepresenteverywherethroughouttheentireelectrodestruc- GIC(102)isactualysometypeofgraphiteoxide(GO) ture(theconductivefoam servingasacurrentcollector).35particlesifanoxidizingagentispresentduringtheinterca Theseporewallsforma3-Dnetworkofinterconected lationprocedure.ThisGICorGOisthenrepeatedlywashed electron-transporting pathways with minimal resistance andrinsedinwatertoremoveexcessacids,resultingina Additionally,ineachanodeelectrodeorcathodeelectrode, graphiteoxidesuspensionordispersion,whichcontains alelectrodeactivematerialparticlesarepre-dispersedina discreteandvisualydiscerniblegraphiteoxideparticles liquid electrolyte (no wetability isue),eliminating the 40 dispersedinwater.Inordertoproducegraphenematerials, existenceofdrypocketscommonlypresentinanelectrode onecanfolowoneofthetwoprocesingroutesafterthis preparedbytheconventionalprocesofwetcoating,drying, rinsingstep,brieflydescribedbelow: packing, and electrolyte injection. Thus, the presently Route 1 involves removing water from the suspension to inventedprocesdeliversatotalyunexpectedadvantage obtain“expandablegraphite,”whichisesentialyamassof overtheconventionalbatterycelproductionprocess. 45 driedGIC ordriedgraphiteoxideparticles.Upon exposure Inapreferedembodiment,theanodeactivematerialisa ofexpandablegraphitetoatemperatureintherangeof prelithiatedorpre-sodiatedversionofgrapheneshets typicaly80-1,050°C.forapproximately30secondsto2 selectedfrompristinegraphene,grapheneoxide,reduced minutes,theGICundergoesarapidvolumeexpansionbya grapheneoxide,graphenefluoride,graphenechloride,gra- factorof30-300toform“graphiteworms”(104),whichare phenebromide,graphene iodide,hydrogenated graphene,50 each acolection ofexfoliated,butlargely un-separated nitrogenatedgraphene,chemicallyfunctionalizedgraphene, graphiteflakesthatremaininterconected. oracombinationthereof.Thestartinggraphiticmaterialfor InRoute1A,thesegraphiteworms(exfoliatedgraphiteor producinganyoneoftheabovegraphenematerialsmaybe “networksofinterconected/non-separatedgraphiteflakes”) selectedfromnaturalgraphite,artificialgraphite,meso- canbere-compressedtoobtainflexiblegraphiteshetsor phasecarbon,meso-phasepitch,meso-carbonmicro-bead,5 foils(106)thattypicalyhaveathicknesintherangeof0.1 softcarbon,hardcarbon,coke,carbonfiber,carbonnano- mm (100um)-0.5mm (500um).Alternatively,onemay fiber,carbonnano-tube,oracombinationthereof.Graphene choosetousealow-intensityairmillorshearingmachineto materialsarealsoagoodconductiveaditiveforboththe simplybreakupthegraphitewormsforthepurposeof anodeandcathodeactivematerialsofanalkalimetalbatery. producingtheso-caled“expandedgraphiteflakes”(108) Theconstituentgrapheneplanesofagraphitecrystalite60 whichcontainmostlygraphiteflakesorplateletsthickerthan inanaturalorartificialgraphiteparticlecanbeexfoliated 10nm(hence,notananomaterialbydefinition). and extracted or isolated to obtain individual graphene In Route 1B , the exfoliated graphite is subjected to shetsofhexagonalcarbonatoms,whicharesingle-atom high-intensitymechanicalshearing(e.g.usinganultrasoni thick,provided theinter-planarvanderWaals forcescanbe cator,high-shearmixer,high-intensityairjetmill,orhigh overcome.Anisolated,individualgrapheneplaneofcarbon 65 energybalmill)toform separatedsingle-layerandmulti atomsiscommonlyreferedtoassingle-layergraphene.A layergrapheneshets(colectivelycaledNGPs,12),as stackofmultiplegrapheneplanesbondedthroughvander disclosedinourU.S.aplicationSer.No.10/858,814(Jun.PDF Image | FLEXIBLE AND SHAPE-CONFORMAL ROPE-SHAPE ALKALI METAL-SULFUR BATTERIES
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