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US 9,905,856 B1 10 potasium-containingaloysorintermetaliccompoundsof anodecurentcolector,ananodeelectrode(e.g.thinSi Si,Ge,Sn,Pb,Sb,Bi,Zn,A1,Ti,Co,Ni,Mn,Cd,andtheir coatinglayer),aporousseparator,acathodeelectrode(e.g. mixtures;(c)Sodium-orpotasium-containingoxides,car- sulfurlayer),andacathodecurentcolector; bides,nitrides,sulfides,phosphides,selenides,tellurides,or FIG.1(B)schematicofapriorartlithium-ionbatery, antimonidesofSi,Ge,Sn,Pb,Sb,Bi,Zn,Al,Fe,Ti,Co,Ni, 5 whereintheelectrodelayeriscomposedofdiscreteparticles Mn,Cd,andmixturesorcompositesthereof;(d)Sodiumor ofanactivematerial(e.g.graphiteortinoxideparticlesin potassium salts;and(e)Graphenesheetspre-loadedwith the anode layer or LiCoo , in the cathode layer); FIG.1(C)Schematicofaprocesforproducingarope Insomepreferedembodiment,thesecondorfirstelec- shapedflexibleandshape-conformablealkalimetal-sulfur sodium orpotasium ontheirsurfaces;andcombinations thereof. trodeactivematerialcontainsalithiumintercalationcom- batery; poundorlithium absorbingcompoundselectedfrom the FIG.1(D)Fourexamplesoftheprocedureforproducing groupconsistingoflithiumcobaltoxide,dopedlithium anelectrode(anodeorcathode)inacontinuousandauto cobaltoxide,lithiumnickeloxide,dopedlithiumnickel matedmanner;and oxide,lithiummanganeseoxide,doped lithiummanganese FIG.1(E)Schematicofapresentlyinventedprocesfor oxide,lithium vanadium oxide,dopedlithium vanadium 15continuouslyproducinganalkalimetal-sulfurbateryelec oxide,lithiummixed-metaloxides,lithiumironphosphate, trode. lithium vanadium phosphate,lithiummanganesephosphate, lithium mixed-metalphosphates,metalsulfides,lithium selenide,lithium polysulfide,andcombinationsthereof. pheneshets. Incertainembodiments,thesecondorfirstelectrode20 FIG.3(A)Examplesofconductiveporousrods:metal activematerialcontainsasodiumintercalationcompoundor grid/meshandcarbonnano-fibermat. a potasium intercalation compound selected from FIG.3(B)Examplesofconductiveporousrods:graphene NaFePO4, Na(1-x)KPO4, KFePO4, Nao,FePO4 foamandcarbonfoam. Na1,5VOPO_F0.53 NazV2(PO4)3, NazV2(PO4)2F3, FIG.3(C)Examplesofconductiveporousrods:graphite Na,FePO4F,NaFeF3,NaVPO4F,KVPO_F,NazV2(PO4)2F3,25foamandNifoam. Na,5VOPO4F0.5;NazV2(PO4)3,Nav.015,NaVO2, FIG.3(D)Examplesofconductiveporousrods:Cufoam Nao33V205,NaC002,Na2/3[Ni1/3Mn2/3]O2,Na(Fe1/2 andstainlesstelfoam. Mn2O4, Na,MnO4, A-MnO4, Na,K1-MnO2, Nao MnO2, NO.4MnO2/C, NaMn,018. NaFe,Mn FIG . 2 An electron microscopic image of isolated gra FIG.4(A)Schematicofacommonlyusedprocesfor producing exfoliated graphite,expanded graphite flakes " 30(thicknes>10nm),andgrapheneshets(thicknes<10 (PO4)3,NaTiz07,N113M1,3C01302,Cu.56Ni.4HCF, NiHCF, NaMnO2, NaCrO2, KCrO2, NazTi,(PO4)3, NiCo204,NizSz/FeS2,Sb2O4,NaFe(CN)6/C,NaV1-x CrPO_F,Se,S,y/z=0.01to10,Se,sodium polysulfide, sulfur,Aluaudites,oracombinationthereof,whereinxis containalithiumsaltorsodiumsaltdisolvedinaliquid densityvs.energydensity)ofNaion-sulfurbaterycels, solventandwhereintheliquidsolventiswater,anorganic containinghardcarbonparticlesastheanodeactivematerial solvent,anionicliquid,oramixtureofanorganicsolvent andsodiumpolysulfideparticlesasthecathodeactivemate andanionicliquid.Theliquidsolventmaybemixedwitha rials(alongwithelectrolyte)residinginporesofgraphene polymertoform apolymergel. andisolatedgrapheneshets. Thefirstelectrolyteand/orthesecondelectrolytemay 35 FIG.5Ragoneplots(gravimetricandvolumetricpower from0.1to1.0. chemicalydepositedinporesofgraphitefoam asthe Insomeprefered embodiments,theelectricalyconduc- 5 cathodeactivematerial,andlithium salt(LiPF.)-PC/DEC as tiveporousrodinthefirstelectrodeortheelectricaly organicliquidelectrolyte.Thedataareforbothlithium conductiveporouslayerinthesecondelectrodehasatleast metal-sulfurcelspreparedbythepresentlyinventedmethod 95%byvolumeofpores,thefirstorsecondelectrodehasa (ropecels)andthosebytheconventionalslurycoatingof diameterorthicknesnolesthan300umorhasanactive electrodes. massloadingoccupyingatleast35%byweightorby60 FIG.8RagoneplotofaseriesofLiion-Scels(graphene volumeoftheentirebaterycel,orthefirstandsecond wrappedSinanoparticles)preparedbytheconventional electrodeactivematerialscombinedocupiesatleast60% slurycoatingprocesandtheRagoneplotofcoresponding byweightorbyvolumeoftheentirebaterycel. byweightorbyvolumeoftheentirebaterycel. BRIEFDESCRIPTIONOFTHEDRAWINGS rope-shapecelspreparedbythepresentlyinventedproces. FIG.9Thecel-levelgravimetric(Wh/kg)andvolumetric 65 energy densities (Wh/L)ofLi ion-S cel(Pre-lithiated FIG.1(A)schematicofapriorartlithium-ionbaterycel graphiteanode+graphene-supportedScathode)plotedover (asanexampleofanalkalimetalbatery)composedofan theachievablecathodethicknesrangeoftheS/RGOcath nm,moretypicaly<10nm,andcanbeasthinas0.34nm). FIG.4(B)Schematicdrawingtoilustratetheproceses forproducingexfoliatedgraphite,expandedgraphiteflakes, 40 foam.Twoofthe4datacurvesareforthecelsprepared Thefirstelectrolyteand/orsecondelectrolytepreferably containsalithium saltorsodium saltdisolvedinaliquid solventhaving a salt concentration greater than 2.5 M (preferably >3.0 M ,further preferably >3.5 M , even more preferably>5.0M,stilmorepreferably>7.0M,andmost45powerdensityvs.gravimetricandvolumetricenergyden preferably>10M,buttypicalynogreaterthan15M). sity)oftwoNa-Scels,bothcontaininggraphene-em Inthealkalimetal-sulfurbatery,theelectricalyconduc bracedNananoparticlesastheanodeactivematerialand tiveporousrodinthefirstelectrodeortheelectricaly sulfurcoatedongrapheneporewallsasthecathodeactive conductiveporouslayerinthesecondelectrodehasatleast material.Thedataareforbothsodiumioncelspreparedby 90%by volumeofpores,thefirstorsecondelectrodehasa 50thepresentlyinventedmethod(ropecels)andthosebythe diameterorthicknesnolesthan20um orhasanactive 30 conventionalslurycoatingofelectrodes. mass loading occupying atleast 30% by weight orby FIG . 7Ragone plots of Li- S bateries containing a volumeoftheentirebattery cel,orthefirstandsecond electrodeactivematerialscombinedoccupiesatleast50% lithiumfoilastheanodeactivematerial,sulfurelectro according to an embodiment of instant invention (rope shapecels)andtheothertwobytheconventionalslury coatingofelectrodes(rol-coating). FIG . 6 Ragone plots (both gravimetric and volumetricPDF Image | FLEXIBLE AND SHAPE-CONFORMAL ROPE-SHAPE ALKALI METAL-SULFUR BATTERIES
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