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US 2020/0051709A1 Feb.13,2020 8 canbespin-coatedalongwithanapropriatesolventto sizeofaproximately18um,weredispersedin1,0mLof removethesurfactantsimultaneously.Indipcoating,the benzene.Anultrasonicenergylevelof250W(Branson5450 substratecanbedipedintothesolutionforaperiodoftime. Ultrasonicator)wasusedfortheexfoliationandseparation Thismayformpaternedorrandomnetworksofgraphene, ofgrapheneplanesforaperiodof1.5hours.Theaverage graphene/nanowire,orgraphene/nanotubehybrids.Ina thicknesoftheresultingNGPswas3.2nm.Whenalower printingproces,thegraphenenetworkmaybetransfered fromonesubstratetoanotherbymeansofastamp.The 1.91mN/mandcontactangleof23degres)wasused,the stampmaybemadefromPolydimethyl-siloxane(PDMS). averageNGPthickneswas0.61nm,indicatingthatmostof Thetransfercanbeaidedbygentleheating(upto10°C.) thepristinegrapheneshetsweresingle-layergraphene. andpresure.Inavacum filtrationproces,thesolution/ suspension/inkcanbefilteredthroughaporousmembrane Example4:PreparationofPristineNGPsfrom undertheasistanceofavacum pump.Afilmofgraphene, graphene/nanowire,andgraphene/nanotubeisdepositedon topofthefilteringmembrane.Thefilmcanbewashedwhile NaturalGraphiteParticlesandMCMBsUsing Potassium Intercalation [0092]NaturalgraphitewasobtainedfromHuadong onthefilterwithaliquidmediumtoremovesurfactant, GraphiteCo.,Qingdao,China.Thefirst-stageintercalation functionalizationagents,orunwantedimpurities. compound,KC8,wassynthesizedbyadingastoichiomet [0087]Itmaybenotedthat,foracoatingorcasting ricamountofpotasium,81.4mg(0.021moles)to20mg proces,onemaydepositthemetalnanowiresorCNTsto (0.0167moles)ofgraphiteparticlesinaPyrextubecaped formafilmfirst,whichcanbesuportedonasubstrate.A withastopcock.Altransferswerecariedoutinahelium protectivegraphenefilmisthendepositedontothenanowire fileddrybox.Thereactantfiledtubewasevacuated,sealed ornanotubefilm.Alternatively,onemaychosetodisperse andheatedfor16hoursat20°C.Thecompoundformed nanowiresand/ornanotubesintoagraphenesolution/sus wasbrightgoldincolor.TheobtainedGICwaspouredinto pensiontoformasuspensionorink.Then,thenanowires amixtureofethanolanddistiledwater(50:50byvolume). and/ornanotubesareco-depositedwithgraphenetoforman Thematerialturnsfromgoldtoblackasthegraphitegot integrallayerofconductivespecies. exfoliated and bublingwas observed,sugestingthat [08]Thefolowingexamplesservetoprovidethebest hydrogenwasproduced.Theresultingsolutionwasbasic modesofpracticeforthepresentdisclosureandshouldnot duetotheformationofpotasiumethoxide.Thedispersion beconstruedaslimitingthescopeofthedisclosure: ofnanographeneshetsinaqueousethanolsolutionwas Example1:DirectUltrasonicationProductionof PristineGraphenefromNaturalGraphiteinaLow Surface TensionMedium then allowed to setle. The solventwas decanted and the productwashedseveraltimeswithethanoluntilaneutralpH wasobtained.RemovalofwaterledtopristineNGPpowder. Another batch of samples was prepared from MCMBS [0089]Asanexample,fivegramsofnaturalgraphite, folowingthesameprocedures. groundtoaproximately20um orlesinsizes,were dispersedin1,0mLofn-Heptanetoform agraphite suspension.Anultrasonicatortipwasthenimmersedinthe suspension,whichwasmaintainedatatemperatureof0-5° C.duringsubsequentultrasonication.Anultrasonicenergy levelof20W(Branson5450Ultrasonicator)wasusedfor exfoliation and separation of graphene planes from dis persedgraphiteparticlesforaperiodof1.5hours.The averagethicknesoftheresultingpristinegrapheneshets was1.1nm,havingmostlysingle-layergrapheneandsome few-layergraphene. Example2:PreparationofPristineGraphenefrom NaturalGraphiteinWater-SurfactantMedium UsingDirectUltrasonication Example5:PreparationofPristineNGPsUsing SupercriticalFluids [0093] Anaturalgraphitesample(aproximately5grams) wasplacedina10mililiterhigh-presurevesel.The veselwasequipedwithsecurityclampsandringsthat enableisolationoftheveselinteriorfrom theatmosphere. Theveselwasinfluidcomunicationwithhigh-presure carbon dioxide by way of piping means and limited by valves.Aheatingjacketwasdisposedaroundtheveselto achieve and maintain the critical temperature of carbon dioxide. [0094] High-presurecarbondioxidewasintroducedinto theveselandmaintainedataproximately1,10psig(7.58 [090]Asanotherexample,fivegramsofgraphiteflakes, MPa).Subsequently,theveselwasheatedtoabout70°C. groundtoaproximately20umorlesinsizes,were atwhichthesupercriticalconditionsofcarbondioxidewere dispersedin1,0mLofdeionizedwater(containing0.15% achievedandmaintainedforabout3hours,alowingcarbon byweightofadispersingagent,Zonyl®FSOfromDuPont) dioxidetodifuseintointer-graphenespaces.Then,the toobtainasuspension.Anultrasonicenergylevelof175W veselwasimediatelydepresurized"catastrophicaly’ata (Branson5450Ultrasonicator)wasusedforexfoliation, rateofabout3mililiterspersecond.Thiswasacomplished separation,andsizereductionforaperiodof1.5hour.This byopeningaconectedblow-ofvalveofthevesel.Asa procedurewasrepeatedseveraltimes,eachtimewithfive result,delaminatedorexfoliatedgraphenelayerswere gramsofstartinggraphitepowder,toproduceasuficient formed.ThissamplewasfoundtocontainpristineNGPs quantityofpristinegrapheneforthinfilmdeposition. withanaveragethicknesjustunder10nm. [095] Aproximatelytwo-thirdsofthesampleweresub Example3:PristineGraphenefromMeso-Carbon Micro-Beads(MCMBs) jectedtoanothercycleofsupercriticalCO,intercalationand de-presurizationtreatments(i.e.,theaboveprocedureswere repeated),yieldingmuchthinerNGPswithanaverage [0091]Fivegramsofartificialgraphite,MCMBS(suplied thicknesof2.1nm.Thespecificsurfacearea,asmeasured fromShanghaiShanShanTechCo.)withanaverageparticle bytheBETmethod,wasaproximately430m2/g.TEMand surfacetensionliquid(Perfluorohexane,surfacetensionofPDF Image | HIGHLY CONDUCTING AND TRANSPARENT FILM AND PROCESS
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