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system,whichiswel-knownintheart. 35 36 be derived from the electrolyte solution. Theelectrolytesolutionisthenpouredintoachamberor 2HCl+Na2S2O3?2NaCl+SJ+S021+H20. US 9,905,856 B1 C.for1h.Thethermalycuredpolyimide(PI)websamples Theprocedurebeganwithading0.58gNaSintoaflask were carbonized at1,000° C.toobtain carbonizednano thathadbeen filedwith25mldistiledwatertoform aNa, fiberswithanaveragefibrildiameterof67nm.Suchaweb solution.Then,0.72gelementalSwassuspendedinthe canbeusedasaconductivesubstrateforananodeactive NaSsolutionandstiredwithamagneticstirerforabout2 material.Weobservethattheimplementationofanetwork 5hoursatroom temperature.Thecolorofthesolution ofconductivenano-filamentsattheanodeofaLi—Sor room temperatureNa—Scelcanefectivelysupresthe initiationandgrowthoflithiumorsodium dendritesthat otherwise could lead to internal shorting. Example 9:ElectrochemicalDepositionofSon VariousWebsorPorousStructures(External ElectrochemicalDeposition)forLi-SandNa—S Bateries changed slowlytoorange-yelow asthesulfurdisolved. Afterdisolutionofthesulfur,asodiumpolysulfide(Na2S2) solutionwasobtained(x=4-10). Subsequently,agraphene-impregnatedstructurewaspre 10 pared by a chemical deposition method in an aqueous solution. A layer of nano-fiber mat was dipped into the NaS,solution.Aproximately10mlof2mol/LHCOOH solutionwasaddedintotheNaS,solutionatarateof30-40 drops/minandstiredfor2hours.AfterdepositionofSinthe Theelectrochemicaldepositionmaybeconductedbefore 15matwas alowed toproceed for3hours,theporousmat thecathodeactivelayerisincorporatedintoanalkalimetal structurewaswashedwithacetoneanddistiledwatersev sulfurbaterycel(Li—SorNa—Scel).Inthisaproach, eraltimestoeliminatesaltsandimpurities.Thereactionmay theanode,theelectrolyte,andtheintegrallayerofporous berepresentedbythefolowingreaction:S,-+2H*>(x-1) graphenestructure(servingasacathodelayer)areposi- S+H,S.Subsequently,theS-impregnatedmatwasdriedat tionedinanexternalcontaineroutsideofalithium-sulfur2050°C.inadryingoven for48hours. cel.Theneededapparatusissimilartoanelectro-plating Example1:RedoxChemicalReaction-Induced In a typical procedure, a metal polysulfide (M .S ) is Deposition ofSulfurinGraphiteFoam disolvedinasolvent(e.g.mixtureofDOL/DME ina volumeratiofrom1:3to3:1)toformanelectrolytesolution.25 Inthischemicalreaction-baseddepositionproces, Anamountofalithiumsaltmaybeoptionalyadded,but sodiumthiosulfate(Na2S203)wasusedasasulfursource thisisnotrequiredforexternalelectrochemicaldeposition. andHClasareactant.Arodofgraphitefoamwasprepared Awidevarietyofsolventscanbeutilizedforthispurpose andthenimersedintoasolutioncontainingthetwo andthereisnotheoreticallimittowhattypeofsolventscan reactants(HClandNa2S203).Thereactionwasallowedto beused:anysolventcanbeusedprovidedthatthereissome 30proceedat25-75°C.for1-3hours,leadingtotheprecipi solubilityofthemetalpolysulfideinthisdesiredsolvent.A tationofSparticlesdepositedonsurfacesofGOshets.The greatersolubilitywouldmeanalargeramountofsulfurcan reactionmayberepresentedbythefolowingreaction: reactorunder adryand controledatmosphere condition 35 (e.g.HeorNitrogengas).Ametalfoilcanbeusedasthe Example12:PreparationofS-ImpregnatedFoam anodeandalayeroftheporousgraphenefoam orcarbon ViaSolutionDeposition foam structure as the cathode;both being immersed in the electrolytesolution.Thisconfigurationconstitutesanelec Sulfurpowderwasmixedanddispersedinasolvent(CS2) trochemicaldepositionsystem.Thestepofelectrochemi-40toformasolution.ApieceofNifoamwasimersedintothe calydepositingnano-scaledsulfurparticlesorcoatingon solutionandsubsequently,thesolventwasevaporated, thegraphenesurfacesisconductedatacurentdensity alowingStogetprecipitatedouttoyieldaS-impregnated preferablyintherangeof1mA/gto10Alg,basedonthe structure. layerweightoftheporousgraphenestructure. Thechemicalreactionsthatoccurinthisreactormaybe 45 representedbythefolowingequation:M.S,>M.Sc +zS (typicalyz=1-4).Quitesurprisingly,theprecipitatedSis preferentialy nucleated and grown onmasive graphene surfacesto form nano-scaledcoatingornano particles.The Example 13:Graphene-EnhancedNano Silicon Fabricatedfrom TEOSasanAnodeActive MaterialofaLithium-IonBatery Dilute 1wt.% N002-PS to 0.2wt.% N002-PS by DI coatingthicknesorparticlediameterandtheamountofS50water,andplacethedilutedPSsolutiontotheultrasonicbath coating/particlesmaybecontroledbythespecificsurface andultrasonicprocessfor30minutes.GraduallyaddTEOS area,electro-chemicalreactioncurentdensity,temperature (0.2wt.%N002-PS:TEOS=5:2)whilestiringthePSsolu andtime.Ingeneral,alowercurentdensityandlower tion.Then,keepstiringfor24hourstogetacomplete reactiontemperatureleadtoamoreuniformdistributionof hydrolysisofTEOS.Dropwiseadd10%NH2-H,Otilthe Sandthereactionsareeasiertocontrol.Alongerreaction 5 formationofgel,andthegelcanbecaledasTPgel.Grind timeleadstoalargeramountofSdepositedonsurfacesof theTPgeltotinyparticles.Ovendriesat120°C.for2hours, porewallsandthereactionisceasedwhenthesulfursource at150°C.for4hours.MixthedriedTPparticleswithMg isconsumedorwhenadesiredamountofSisdeposited inaratioof10:7.Use20timesamountof7mmSSbalsand TheseS-coatedfoamstructureswerethenusedasthe balmillunderArgonprotection,gradualyincreasethe cathodelayerofacable-shapeLi– SorNa—S cel. Example 10:ChemicalReaction-Induced DepositionofSulfurParticlesinCarbon Nano-FiberMat 60 rotating speed to 250 rpm.Put certain amount of TPM powdersinNickelcrucibleandheattreatmentat680°C. Preparecertainamountof2M HClsolution.Thengradualy adheattreatedTPMpowderstotheacidsolution.Keepthe reactionfor2-24hours,andthenputtheturbidliquidtothe 65 ultrasonic bath and ultrasonic process for 1hour.Pour out Achemicaldepositionmethodishereinutilizedtoprepare thesuspensiontothefiltrationsystem.Discardthebotom Scoatingdepositedintheporesofacarbonnano-fibermat. largeparticles.UseDIwatertorinsethretimes.DrythePDF Image | FLEXIBLE AND SHAPE-CONFORMAL ROPE-SHAPE ALKALI METAL-SULFUR BATTERIES
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