FLEXIBLE AND SHAPE-CONFORMAL ROPE-SHAPE ALKALI METAL-SULFUR BATTERIES

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FLEXIBLE AND SHAPE-CONFORMAL ROPE-SHAPE ALKALI METAL-SULFUR BATTERIES ( flexible-and-shape-conformal-rope-shape-alkali-metal-sulfur- )

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31 32 ficientsbetweennickelandgraphene,riplesandwrinkles10 were formed on the graphene films. Four types of foams madeinthisexamplewereusedasacurentcolectorinthe presentlyinventedlithiumbateries:Nifoam,CVD gra phene-coatedNiform,CVD graphenefoam (Nibeing Example4:PreparationofGrapheneOxide(GO) andReducedGrapheneOxide(RGO)NanoShets fromNaturalGraphitePowder US 9,905,856 B1 “Thre-dimensionalflexibleandconductiveinterconected rateofaproximately1.5degreC./minwithreleaseof graphenenetworksgrownbychemicalvapordeposition," presureatarateofapproximately2psi/min.Finalfoam NatureMaterials,10,424-428(2011).Nickelfoam,aporous temperatureswere630°C.and800°C.Duringthecooling structurewithaninterconected3Dscafoldofnickelwas cycle,presureisreleasedgradualytoatmosphericcondi chosenasatemplateforthegrowthofgraphenefoam.5 tions.Thefoamwasthenheattreatedto1050°C.(carbon Briefly,carbonwasintroducedintoanickelfoambydecom- ized)underanitrogenblanketandthenheattreatedin posingCH4at1,000°C.underambientpressure,andgra- separaterunsinagraphitecrucibleto2500°C.and2800°C. phenefilmswerethendepositedonthesurfaceofthenickel (graphitized)inArgon.Thegraphitefoamlayersareavail foam.Duetothediferenceinthethermalexpansioncoef ableinathicknesrangeof75-50um. etchedaway),andconductivepolymerbondedCVDgra-15 NaturalgraphitefromHuadongGraphiteCo.(Qingdao, phenefoam. China)wasusedasthestartingmaterial.GO wasobtained Inordertorecover(separate)graphenefoamfromthe byfollowingthewell-knownmodifiedHummersmethod, supportingNifoam,Niframewasetchedaway.Inthe whichinvolvedtwooxidationstages.Inatypicalprocedure, procedureproposedbyChen,etal.,beforeetchingawaythe thefirstoxidationwasachievedinthefolowingconditions: nickelskeletonbyahotHCl(orFeCl3)solution,athinlayer2010mgofgraphitewasplacedina10mLboilingflask. ofpoly(methylmethacrylate)(PMMA)wasdepositedon thesurfaceofthegraphenefilmsasasuporttopreventthe Then,20gofK2S208,20gofP205,and40mLofa graphenenetworkfromcolapsingduringnickeletching. concentratedaqueoussolutionofH,SO,(96%)wereadded AfterthePMMAlayerwascarefulyremovedbyhot intheflask.Themixturewasheatedunderrefluxfor6hours acetone,afragilegraphenefoam samplewasobtained.The 25 andthenletwithoutdisturbingfor20hoursatroom tem useofthePMMAsupportlayerwasconsideredcriticalto perature.Oxidizedgraphitewasfilteredandrinsedwith preparingafre-standingfilmofgraphenefoam.Instead,a abundantdistiledwateruntilneutralpH.Awetcake-like conductingpolymerwasusedasabinderresintohold materialwasrecoveredattheendofthisfirstoxidation. graphenetogetherwhileNiwasetchedaway.Thegraphene Forthesecondoxidationprocess,thepreviouslycolected foam orNifoamthicknesrangewasfrom35umto600um.30wetcakewasplacedinaboilingflaskthatcontains69mL ThelayersofNifoamortheCVDgraphenefoamused ofaconcentratedaqueoussolutionofH,SO.(96%).The hereinisintendedasconductiveporouslayers(CPL)to flaskwaskeptinanicebathas9gofKMnO4wasslowly accommodatetheingredients(anodeorcathodeactivemate added.Carewastakentoavoidoverheating.Theresulting rial+optionalconductiveaditive+liquidelectrolyte)forthe mixturewasstiredat35°C.for2hours(thesamplecolor anodeorcathodeorboth.Forinstance,Sinanoparticlesor35turningdarkgren),folowedbytheaditionof140mLof surface-stabilizedLiparticlesdispersedinanorganicliquid water.After15min,thereactionwashaltedbyadding420 electrolyte(e.g.1.0-5.5MofLiPF,disolvedinPC-EC) mLofwaterand15mLofanaqueoussolutionof30wt% weremadeintogel-likemass,whichwasdeliveredtoa H2O2.Thecolorofthesampleatthisstageturnedbright poroussurfaceofaNifoamcontinuouslyfedfromafeeder yellow.Toremovethemetallicions,themixturewasfiltered rolertomakeananodeelectroderoler(asinSchematicA 40andrinsedwitha1:10HClaqueoussolution.Thecolected material was gently centrifuged at 2700 g and rinsed with Graphene-suportedlithiumpolysulfidenanoparticles deionizedwater.Thefinalproductwasawetcakethat dispersedinthesameliquidelectrolyteweremadeinto contained1.4wt%ofGO,asestimatedfromdryextracts. cathodeslury,whichwassprayedovertwoporoussurfaces Subsequently,liquiddispersionsofGOplateletswere ofacontinuousNifoamlayertoformacathodeelectrode.45obtainedbylightlysonicatingwet-cakematerials,which ofFIG.1(C). AporousfoamrodcontainingSinanoparticle-electrolyte WA Surfactant-stabilizedRGO (RGO-BS)wasobtainedby waswrappedaroundbyaporousseparatorlayer(porous dilutingthewet-cakeinanaqueoussolutionofsurfactants PE-PPcopolymer),whichinturnwaswrappedaroundbya insteadofpurewater.Acommerciallyavailablemixtureof lithiumsulfide-basedcathodelayer.Thecylindricalstructure 50 cholatesodium (50wt.%)anddeoxycholatesodium (50wt. isthenencasedinathinpolymersheathtoobtainacable- %)saltsprovidedbySigmaAldrichwasused.Thesurfactant mixtureimpregnatedintothefoampores(thefirstelectrode) shapelithium-ionbatery. Example3:GraphiticFoam-BasedConductive PorousLayersfromPitch-BasedCarbonFoams weight fractionwas 0.5wt.%.Thisfractionwas kept constantforalsamples.Sonicationwasperformedusinga BransonSonifierS-250Aequippedwitha13mm step 5disruptorhornanda3mm taperedmicro-tip,operatingata 20kHzfrequency.Forinstance,10mL ofaqueoussolutions Pitchpowder,granules,orpeletsareplacedinaalumi- containing0.1wt.%ofGOwassonicatedfor10minand nummoldwiththedesiredfinalshapeofthefoam.Mit subsequentlycentrifugedat2700gfor30mintoremoveany subishiARA-24meso-phasepitchwasutilized.Thesample non-disolvedlargeparticles,aggregates,andimpurities. isevacuated to lesthan 1 torand thenheated to a60 Chemicalreductionofas-obtainedGO toyieldRGO was temperatureaproximately30°C.Atthispoint,the conductedbyfolowingthemethod,whichinvolvedplacing vacuumwasreleasedtoanitrogenblanketandthena 10mLofa0.1wt.%GOaqueoussolutioninaboilingflask presureofupto1,0psiwasaplied.Thetemperatureof of50mL.Then,10uLofa35wt.%aqueoussolutionof thesystemwasthenraisedto800°C.Thiswasperformed NH (hydrazine)and70mLofa28wt.%ofanaqueous atarateof2degreC./min.Thetemperaturewasheldfor65 solutionofNH OH (ammonia)wereaddedtothemixture, atleast15minutestoachieveasoakandthenthefurnace whichwasstabilizedbysurfactants.Thesolutionwasheated powerwasturnedofandcooledtoroomtemperatureata to90°C.andrefluxedfor1h.ThepHvaluemeasuredafter ter

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