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US 9,905,856B1 graphite(e.g.100inFIG.4(B)areintercalatedinanacid hardcarbon,carbonnano-fiber,andcarbonnano-tube);(b) solutiontoproducegraphiteintercalationcompounds(GICs, Silicon(Si),germanium(Ge),tin(Sn),lead(Pb),antimony 102).TheGICsarewashed,dried,andthenexfoliatedby (Sb),bismuth(Bi),zinc(Zn),aluminum(Al),nickel(Ni), exposuretoahightemperatureforashortperiodoftime. cobalt(Co),manganese(Mn),titanium(Ti),iron(Fe),and Thiscausestheflakestoexpandorexfoliateinthec-axis 5 cadmium (Cd);(Si,Ge,Al,andSnaremostdesirabledueto directionofthegraphiteupto80-300timesoftheiroriginal theirhighspecificcapacities;(c)Alloysorintermetallic dimensions.Theexfoliatedgraphiteflakesarevermiformin compoundsofSi,Ge,Sn,Pb,Sb,Bi,Zn,Al,orCdwith appearanceand,hence,arecommonlyreferredtoasgraphite otherelements,whereinthealloysorcompoundsarestoi worms104.Thesewormsofgraphiteflakeswhichhave chiometricornon-stoichiometric(e.g.SiAl,SiSn);(d) been greatly expanded can be formed without the use of a 10 Oxides, carbides, nitrides, sulfides, phosphides, selenides, binderintocohesiveorintegratedshetsofexpandedgraph- andteluridesofSi,Ge,Sn,Pb,Sb,Bi,Zn,Al,Fe,Ni,Co, ite,e.g.webs,papers,strips,tapes,foils,matsorthelike Ti,Mn,orCd,andtheirmixturesorcomposites(e.g.SnO, (typicalyreferedtoas“flexiblegraphite”106)havinga TiO2,Co204,etc.);(e)Pre-lithiatedorpre-sodiatedversions typicaldensityofabout0.04-2.0g/cm formostaplica- thereof(e.g.pre-lithiatedTiO2,whichislithiumtitanate);(f) tions. 15Pre-lithiatedorpre-sodiatedgrapheneshets;andcombina Acids,suchassulfuricacid,arenottheonlytypeof tionsthereof. intercalatingagent(intercalant)thatpenetrateintospaces Inanotherpreferedembodiment,theanodeactivemate betweengrapheneplanestoobtainGICs.Manyothertypes rialisapre-sodiatedorpre-lithiatedversionofgraphene ofintercalatingagents,suchasalkalimetals(Li,K,Na,Cs, shetsselectedfrompristinegraphene,grapheneoxide, and their aloys or eutectics),can be used to intercalate 20 reduced grapheneoxide,graphene fluoride,graphene chlo graphitetostage1,stage2,stage3,etc.Stagenimpliesone ride,graphenebromide,grapheneiodide,hydrogenatedgra intercalantlayerforeveryngrapheneplanes.Forinstance, phene,nitrogenatedgraphene,chemicallyfunctionalized astage-1potasium-intercalatedGICmeansthereisone graphene,oracombinationthereof.Thestartinggraphitic layerofKforeverygrapheneplane;or,onecanfindone materialforproducinganyoneoftheabovegraphene layer of K atoms inserted between two adjacent graphene 25 materials may be selected from natural graphite, artificial planesinaG/K/G/K/G/KG...sequence,whereGisa graphite,meso-phasecarbon,meso-phasepitch,meso-car grapheneplaneandKisapotasiumatomplane.Astage-2 bonmicro-bead,softcarbon,hardcarbon,coke,carbon GICwillhaveasequenceofGG/K/GG/K/GG/K/GGanda fiber,carbonnano-fiber,carbonnano-tube,oracombination stage-3GIC willhaveasequenceofGGG/K/GGG/K/G thereof.Graphenematerialsarealsoagoodconductive GG ..,etc.TheseGICscanthenbebroughtincontactwith 30 aditiveforboththeanodeandcathodeactivematerialsof waterorwater-alcoholmixturetoproduceexfoliatedgraph- analkalimetalbatery. iteand/orseparated/isolatedgrapheneshets. Intherechargeablealkalimetal-sulfurbatery,theanode Exfoliatedgraphitewormsmaybesubjectedtohigh- maycontainanalkaliionsourceselectedfromanalkali intensitymechanicalshearing/separationtreatmentsusinga metal,analkalimetalaloy,amixtureofalkalimetalor high-intensityairjetmill,high-intensitybalmill,orultra-35 alkalimetalaloywithanalkaliintercalationcompound,an sonicdevicetoproduceseparatednanographeneplatelets alkalielement-containingcompound,oracombination (NGPs)withalthegrapheneplateletsthinerthan10nm, thereof.Particularlydesiredisananodeactivematerialthat mostlythinnerthan10nm,and,inmanycases,being containsanalkaliintercalationcompoundselectedfrom single-layergraphene(alsoilustratedas12inFIG.4(B). petroleumcoke,carbonblack,amorphouscarbon,hard AnNGP iscomposedofagraphenesheetorapluralityof40 carbon,templatedcarbon,hollow carbonnanowires,hollow grapheneshetswitheachshetbeingatwo-dimensional, carbonsphere,naturalgraphite,artificialgraphite,lithiumor hexagonalstructureofcarbonatoms.Amassofmultiple sodiumtitanate,NaTi,(PO4)3,NaTi20,(Sodiumtitanate), NGPs(includingdiscreteshets/plateletsofsingle-layer Na2C2H404(Disodium Terephthalate),Na,TP(Sodium and/orfew-layergrapheneorgrapheneoxidemaybemade Terephthalate),TiO2,NaTiO2(x=0.2to1.0),carboxylate intoaporousgraphenefilm (14inFIG.4(B)usinga45based materials, C2H_Na_04, C2H604, C2HzNa04, film-makingproces.Alternatively,withalow-intensity CgNa2F404,C10HNa_03,C14H406,C14H_Na_03,ora shearing,graphitewormstendtobeseparatedintothe combinationthereof.Inanembodiment,theanodemay so-caledexpandedgraphiteflakes(108inFIG.4(B)having containamixtureof2or3typesofanodeactivematerials athickness >100 nm.These flakescanbe formed into (e.g.mixedparticlesofactivatedcarbon+NaTi,(PO ),ora graphitematornonwoven 106usingmat-makingproces,50mixtureofLiparticlesandgraphiteparticles). with orwithoutaresin binder,to form an expanded graphite The first or second liquid electrolyte in the invented foam.Graphitefoamscanbemadebygraphitizationof procesorbaterymaybeselectedfromanaqueouselec carbonfoamsaswell. trolyte,organicelectrolyte,ionicliquidelectrolyte,mixture Insomeembodiments,thefirstelectrodeorsecondelec- ofanorganicelectrolyteandanionicelectrolyte,ora trodecontainsparticles,foil,orcoatingofLi,Na,ora5mixturethereofwithapolymer.Insomeembodiments,the combination thereofasan electrodeactivematerial. aqueouselectrolytecontainsasodium saltorapotasium Thereisnoparticularrestrictiononthetypesofanode saltdisolvedinwateroramixtureofwaterandalcohol.In activematerialsthatcanbeusedinpracticingtheinstant someembodiments,thesodiumsaltorpotassiumsaltis invention.Preferably,intheinventedprocess,theanode selectedfromNa,SO2,K,SO4A9,amixturethereof,NaOH, activematerialabsorbsalkaliions(e.g.lithium ions)atan 60 LiOH,NaCl,Lici,NaF,LiF,NaBr,LiBr,Nal,Lil,ora electrochemicalpotentialoflesthan1.0volt(preferably mixturethereof. lesthan0.7volts)abovetheLi/Li+(i.e.relativetoLiLi++ Awiderangeofelectrolytescanbeusedforpracticingthe easthestandardpotential)theNa/Nareferencewhenthe instantinvention.Mostpreferedarenon-aqueousorganic battery ischarged.Inonepreferredembodiment,theanode and/orionicliquid electrolytes.Thenon-aqueouselectrolyte activematerialisselectedfromthegroupconsistingof:(a)65tobeemployedhereinmaybeproducedbydisolvingan Particlesofnaturalgraphite,artificialgraphite,meso-carbon electrolyticsaltinanon-aqueoussolvent.Anyknownnon microbeads(MCMB),andcarbon(includingsoftcarbon aqueoussolventwhichhasbenemployedasasolventforPDF Image | FLEXIBLE AND SHAPE-CONFORMAL ROPE-SHAPE ALKALI METAL-SULFUR BATTERIES
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