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US 9,905,856 B1 phonium,andtrialkylsulfonium.CommonanionsofRTILS ionicliquid)andasulfursource(e.g.metalpolysulfide) 25 26 disolvedordispersed inthesolvent.Thiselectrolyte CH,CHBFz; CF3BF3, CF3BFz; n-C2F%BF3; canbethesameelectrolyteasintheintendedbatery; n-C_F,BF3,PF6,CF3C02,CF3S03;N(SO,CF3)2; c)Preparingananode; N(COCF3)(S02CF3),N(SO2F)2,N(CN)2,C(CN)3,5 d)Bringingtheintegrallayerofporousgraphene/carbon/ SCN-,SeCNC,CuCl2,A1C14,F(HF)2.37,etc.Relatively graphitestructureandtheanodeinioniccontactwith include,butnotlimitedto,BF4,B(CN),,CH BF,, speaking,thecombinationofimidazolium-orsulfonium basedcationsand complexhalideanionssuchasA1C14", BF4,CF2C02,CF2803,NTf2,N(SO,F)2,orF(HF)2,3 resultsinRTILswith goodworkingconductivities. 10 RTILs can possess archetypical properties such as high theelectrolyte(e.g.by immersingalthesecomponents inachamberthatisexternaltotheintendedLi-Scel, orencasingthesethrecomponentsinsidetheLi-S cel)and imposing an electriccurentbetween the anodeandtheintegrallayerofporousgraphene/carbon/ graphitestructure(servingasacathode)with asufi cientcurentdensity forasuficientperiodoftimeto intrinsicionicconductivity,highthermalstability,lowvola tility,low (practicalyzero)vaporpresure,non-flammabil ity,theabilitytoremainliquidatawiderangeoftempera electrochemicalydepositnano-scaledsulfurparticles turesaboveandbelowroom temperature,highpolarity,high 15 viscosity,andwideelectrochemicalwindows.Theseprop erties,exceptforthehighviscosity,aredesirableatributes whenitcomestousinganRTILasanelectrolyteingredient (asaltand/orasolvent)inabatery. orcoatingonthegraphenesurfacesorinternalpore wallsofagraphite/carbonstructuretoform apre sulfurizedfoam structure(e.g.arodorlayer); TheSparticlesorcoatinginthepresently invented pre-sulfurizedfoam structuretypicalyhaveathicknesor ThespecificcapacityandspecificenergyofaLi–Scel20diametersmalerthan20nm (preferablyandtypicaly<10 orNa-Scelaredictatedbytheactualamountofsulfurthat nm,morepreferably<5nm,andfurtherpreferably<3nm) canbeimplementedinthecathodeactivelayer(relativeto andwhereinthenano-scaledsulfurparticlesorcoating othernon-activeingredients,suchasthebinderresinand ocupyaweightfractionofatleast70%(preferably>80%, conductivefiler)andtheutilizationrateofthissulfur morepreferably>90%,andmostpreferably>95%)basedon amount(i.e.theutilizationefficiencyofthecathodeactive 25thetotalweightsofthesulfurparticlesorcoatingandthe materialortheactualproportionofSthatactivelypartici graphenematerialcombined.Itisadvantageoustodepositas patesinstoringandreleasinglithiumions).Ahigh-capacity muchSasposibleyetstilmaintainultra-thinthicknesor andhigh-energyLiSorNa—Scelrequiresahighamount diameteroftheScoatingorparticles(e.g.>80%and<3nm; ofSinthecathodeactivelayer(i.e.relativetotheamounts >90% and <5nm;and >95% and <10nm ,etc.). ofnon-activematerials,suchasthebinderresin,conductive30 Therodofporousgraphene/graphite/carbonstructure aditive,andothermodifyingorsuportingmaterials)and recitedinstep(a)maycontainagraphenematerialoran ahighSutilizationeficiency).Thepresentinventionpro- exfoliatedgraphitematerial,whereinthegraphenematerial videssuchasulfurorsulfide-containingcathodeactivelayer isselectedfrompristinegraphene,grapheneoxide,reduced andamethodofproducingsuchacathodeactivelayer(e.g. grapheneoxide,graphenefluoride,graphenechloride,gra apre-sulfurizedactivecathodelayer). 35phenebromide,grapheneiodide,hydrogenatedgraphene, Itmaybenotedthatsulfurorasulfurcompound(e.g. nitrogenatedgraphene,boron-dopedgraphene,nitrogen particlesoflithiumpolysulfide,sodiumpolysulfide,carbon dopedgraphene,chemicalyfunctionalizedgraphene,ora polymercompound,sulfurcariedbyactivatedcarbonpar- combinationthereof,andwhereintheexfoliatedgraphite ticles,sulfurorsulfidecariedongraphenesurfaces,etc.) materialisselectedfromexfoliatedgraphiteworms, maybeincorporatedintotheporesofafoamstructureas40expandedgraphiteflakes,orrecompresedgraphiteworms describedearlierandilustratedinFIG.1(D)andFIG.1(E). orflakes(muststilexhibitahighspecificsurfacearea, Aditionalyandpreferably,ahighlyinovativemethod >10m2/g,acesibletoelectrolyte). maybeusedtoincorporatesulfurorsulfurcompound,with Once alayerofporousgraphene/carbon/graphitestruc orwithouttheeventualelectrolyte,intoafoamstructure. tureisprepared,thislayercanbeimmersedinanelectrolyte Suchapre-sulfurizationmethodenablesustoachieveboth 45 (preferably liquid electrolyte),which comprisesasolvent ahighsulfurcontentandthinsulfurcoating/particlesizes, andasulfursourcedisolvedordispersedinthesolvent. twofeaturesthatwerepreviouslyregardedasmutually Thislayerbasicalyservesasacathodeinanexternal exclusive.Asanexampleofsulfurpre-loadingprocedures, electrochemicaldepositionchamber. this method comprises the following four steps,(a)-(d): Subsequently, an anode layer is also immersed in the a)Preparingalayerofporousgraphene/graphite/carbon 50 chamber.Anyconductivematerialcanbeusedasananode structurehavingporesandmassivesurfaceswitha material,butpreferablythislayercontainssomelithiumor specificsurfaceareagreaterthan10m2/g(these sodium.Insuchanarrangement,thelayerofporousgra surfacesmustbeaccessibletoelectrolyte).Theporous phene/carbon/graphitestructureandtheanodeareinionic graphene/carbon/graphitestructurehaveaspecificsur- contactwiththeelectrolyte.Anelectriccurrentisthen faceareapreferably >50m?lgandmorepreferably 5 supliedbetweentheanodeandtheintegrallayerofporous >700m2/g,andmostpreferably>1,0m2/g.Many graphenestructure(servingasacathode)withasuficient typesofgraphene/carbon/graphitefoamstructuresmay curentdensityforasuficientperiodoftimetoelectro beused,includingcarbonfoam,graphitefoam,carbon chemicallydepositnano-scaledsulfurparticlesorcoatingon aerogelfoam,graphenefoam,grapheneaerogelfoam, thegraphenesurfacestoformthepre-sulfurizedactive electron-spuncarbonfoam,carbon/graphitefibermat,60 cathodelayer.Therequiredcurrentdensitydependsuponthe carbon/graphitefibercloth,carbon/graphitecarbon desiredspedofdepositionanduniformityofthedeposited paper,carbonnano-fibermat/paper/cloth,carbonnano- material. tube mat/paper/cloth, activated carbon particles ThiscurentdensitycanbereadilyadjustedtodepositS (bondedtogethertoformafoam,forinstance),and particlesorcoatingthathaveathicknesordiametersmaller exfoliatedgraphite foam,etc. 65 than20nm (preferably<10nm,morepreferably<5nm,and b)Preparinganelectrolytecomprisingasolvent(e.g. furtherpreferably<3nm).Theresultingnano-scaledsulfur non-aqueoussolvent,suchasorganicsolventandor particlesorcoatingocupyaweightfractionofatleast70%PDF Image | FLEXIBLE AND SHAPE-CONFORMAL ROPE-SHAPE ALKALI METAL-SULFUR BATTERIES
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