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US 9,905,856 B1 33 thereactionwasaproximately9.Thecolorofthesample exfoliatedgraphite(HEG)waspreparedfromintercalated turneddarkblackduringthereductionreaction. compound CF.xC1Fz.HEG was further fluorinatedby RGOwasusedasaconductiveaditiveineitherorboth vaporsofchlorinetrifluoridetoyieldfluorinatedhighly oftheanodeandcathodeactivematerialincertainlithium exfoliatedgraphite(FHEG).Pre-coledTeflonreactorwas bateriespresentlyinvented.Pre-lithiatedRGO (e.g.RGO+ 5 filedwith20-30mLofliquidpre-coledCIF3,thereactor lithiumparticlesorRGOpre-depositedwithlithiumcoating) wasclosedandcooledtoliquidnitrogentemperature.Then, wasalsousedasananodeactivematerialthatwasmixed nomorethan1gofHEGwasputinacontainerwithholes withaliquidelectrolytetoformwetanodeactivematerial forCIFzgastoaccessandsituatedinsidethereactor.In7-10 mixturesforuseinselectedlithium-ioncels.Selected daysagray-beigeproductwithapproximateformulaCF cathode active materials (Li2S nano particles) and non- 10 was formed. lithiatedRGO shetsweredispersedinaliquidelectrolyteto Subsequently,asmallamountofFHEG (approximately preparewetcathodeactivematerialmixture.Thewetanode 0.5mg)wasmixedwith20-30mLofanorganicsolvent active mixture and cathode active mixtures were separately (methanol and ethanol, separately ) and subjected to an deliveredtosurfacesofgraphitefoamsforformingananode ultrasoundtreatment(280W)for30min,leadingtothe layerandacathodelayer,respectively.Cable-shapebateries15 formation ofhomogeneousyelowish dispersions.Upon were then fabricated,wherein the core structure (first elec removal ofsolvent,the dispersion became abrownish pow trode)waseitherananodeoracathodeandthesecond der.Thegraphenefluoridepowderwasmixedwithsodium electrodewasacorrespondingcounterelectrode(eithera chipsinaliquidelectrolyte,allowingforpre-sodiationto cathode or an anode). occurbefore or after impregnation into pores of an anode Forcomparisonpurposes,slurycoatinganddryingpro-20 currentcolector. cedureswereconductedtoproduceconventionalelectrodes. Electrodes andaseparatordisposed betwen twodried Example7:PreparationofNitrogenataedGraphene electrodeswerethenasembledandencasedinanAl-plastic NanoShetsandPorousGrapheneStructures laminatedpackagingenvelop,folowedbyliquidelectrolyte injectiontoformaconventionallithiumbaterycel. 25Grapheneoxide(GO),synthesizedinExample1,was finely ground with different proportions of urea and the Example5:PreparationofPristineGrapheneShets peletizedmixtureheatedinamicrowavereactor(90W) (0% Oxygen) for 30 s. The product was washed several times with deionizedwaterandvacuum dried.Inthismethodgraphene Recognizingtheposibilityofthehighdefectpopulation 30oxidegetssimultaneouslyreducedanddopedwithnitrogen. inGOshetsactingtoreducetheconductivityofindividual Theproductsobtainedwithgraphene:ureamassratiosof grapheneplane,wedecidedtostudyiftheuseofpristine 1:0.5,1:1and1:2aredesignatedasNGO-1,NGO-2and grapheneshets(non-oxidizedandoxygen-fre,non-halo- NGO-3respectivelyandthenitrogencontentsofthese genatedandhalogen-fre,etc.)canleadtoaconductive sampleswere14.7,18.2and17.5wt%respectivelyasfound aditivehavingahighelectricalandthermalconductivity.35byelementalanalysis.Thesenitrogenataedgrapheneshets Pre-lithiatedpristinegrapheneandpre-sodiatedpristinegra- remaindispersibleinwater.Twotypesofdispersionswere phenewerealsousedasananodeactivematerialfora thenprepared.Oneinvolvedadingwater-solublepolymer lithium-ionbateryandasodium-ionbatery,respectively. (e.g.polyethyleneoxide)intothenitrogenatedgraphene Pristinegrapheneshetswereproducedbyusingthedirect shet-waterdispersiontoproduceawater-basedsuspension. ultrasonicationorliquid-phaseproductionproces. 40 Theotherinvolveddryingthenitrogenatedgrapheneshet Inatypicalprocedure,fivegramsofgraphiteflakes, waterdispersiontorecovernitrogenatedgrapheneshets, groundtoaproximately20umorlesinsizes,were whichwerethenadedintoprecursorpolymer-solventsolu dispersedin1,000mLofdeionizedwater containing0.1% tionstoobtainorganicsolvent-basedsuspensions. byweightofadispersingagent,Zonyl®FSO fromDuPont) Theresultingsuspensionswerethencast,dried,carbon toobtainasuspension.Anultrasonicenergylevelof85W 45izedandgraphitizedtoproduceporousgraphenestructures. (BransonS450Ultrasonicator)wasusedforexfoliation, Thecarbonizationtemperaturesforcomparativesamplesare separation,andsizereductionofgrapheneshetsfora 90-1,350°C.Thegraphitizationtemperaturesarefrom period of 15 minutes to 2 hours. The resulting graphene 2,200° C. to 2,950° C. The porous graphene layers are used shetsarepristinegraphenethathaveneverbeenoxidized astheporouscurrentcolectorsforboththeanodeandthe andareoxygen-freandrelativelydefect-fre.Pristinegra-50cathodeofLi–Scels. pheneisesentialyfrefrom anynon-carbonelements. Pristinegrapheneshets,asaconductiveaditive,along Example8:ConductiveWebofFilamentsfrom withananodeactivematerial(orcathodeactivematerialin thecathode)werethenincorporatedinabateryusingboth thepresently invented procedure and conventionalproce- 5 dureofslurycoating,dryingand layerlaminating.Both lithium-ionbateriesandlithiummetalbateries(impregna preparedbycopolymerizingofpyromeliticdianhydride 10 tionintoanodeonly)wereinvestigated.Sodium-ioncels (Aldrich)and4,4'-oxydianiline(Aldrich)inamixedsolvent oftetrahydrofurane/methanol(THF/MeOH,8/2byweight). 60 ThePAAsolutionwasspunintofiberwebusinganelec Example6:PreparationofPre-SodiatedGraphene trostaticspiningaparatus.Theaparatusconsistedofa15 FluorideShetsasanAnodeActiveMaterialofa kV d.c.powersuplyequipedwiththepositivelycharged Sodium-SulfurBatery capilaryfrom which thepolymersolutionwasextruded, andanegativelychargeddrum forcolectingthefibers. Severalproceseshavebeen usedbyustoproduce65SolventremovalandimidizationfromPAAwereperformed graphenefluoride(GF),butonlyoneprocesisherein concurentlybystepwiseheattreatmentsunderairflowat describedasanexample.Inatypicalprocedure,highly 40°C.for12h,10°C.for1h,250°C.for2h,and350° werealsopreparedandstudied. 34 Electro-SpunPAA FibrilsasaSupportingLayerfor theAnode Poly (amic acid)(PAA)precursors forspiningwerePDF Image | FLEXIBLE AND SHAPE-CONFORMAL ROPE-SHAPE ALKALI METAL-SULFUR BATTERIES
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