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US 2020/0051709A1 Feb.13,2020 9 AFMexaminationsindicatedthatthereweremanysingle coating.Then,AgNWinkwasspin-coatedonaglassub layergrapheneshetsinthissample. filmswerepreparedbychangingspin-coatingspedfrom identicalsupercriticalCo,conditions,withtheexception 250to2,0rpmtoinvestigatetheefectofspin-coating [09] Anothersamplewaspreparedunderesentialy spedonopticalandelectricalpropertiesofAgNW films. ofZonyl®FSO)wasmixedwith5gramsofnaturalgraphite TransparentelectrodefilmsofAgNW-RGOandAgNW majorityoftheNGPsaresingle-layerordouble-layershets. transmitanceofAgNW,AgNW-RGO,andAgNW-pristine Thespecificsurfaceareaofthissampleafterarepeated graphenefilms.Theshetresistancesweremeasuredbya cyclewasaproximately90m/g.Itisclearthatthe non-contactRsmeasurementinstrument.Theshetresis presenceofasurfactantordispersingagentpromotessepa tanceandopticaltransparencydataofthinfilmsprepared rationofgraphenelayers,perhapsbypreventingtherefor fromvariousdiferentmaterialsandconditionsaresumma mationofvanderWaalsforcesbetweengrapheneshets rizedinFIG.2(a)andFIG.2(b).Severalsignificantobser thatasmalamountofsurfactant(aproximately0.05grams beforethemixturewassealedinthepresurevesel.The pristinegraphenehybridwerealsopreparedinasimilar resultingNGPshaveasurprisinglylowaveragethicknes, manner.Separately,theAgNW-graphenehybridtransparent 3.1nm.Afterthepresurizationandde-presurizationpro electrodefilmswerepreparedbycoatingRGOorpristine cedureswererepeatedforanothercycle,theresultingNGPs grapheneontotheAgNWfilm. haveanaveragethickneslesthan1nm,indicatingthata [0101]AnUV/Vis/NIRwasusedtomeasuretheoptical onceseparated. Example6:ThermalExfoliationandSeparationof GraphiteOxide [0097] Graphite oxide was prepared by oxidation of graphiteflakeswithsulfuricacid,nitrate,andpermanganate acordingtothemethodofHummers[U.S.Pat.No.2,798, 878,Jul.9,1957].Uponcompletionofthereaction,the mixturewaspouredintodeionizedwaterandfiltered.The graphiteoxidewasrepeatedlywashedina5%solutionof HCltoremovemostofthesulfateions.Thesamplewasthen washedrepeatedlywithdeionizedwateruntilthepHofthe filtratewasneutral.Theslurywasspray-driedandstoredin avacumovenat60°C.for24hours.Theinterlayerspacing oftheresultinglaminargraphiteoxidewasdeterminedby theDebye-SchererX-raytechniquetobeaproximately 0.73 nm (7.3 Å). vationscanbemadefromthesefigures:(A)TheAgNW pristine graphene filmssignificantly out-perform both AgNW andAgNW-RGO filmsintermsofhightransmit tanceand/orlowshetresistance.(B)WithhybridAgNW pristinegraphenefilms,wewereabletoachieveashet resistance value of 54 and 432/1 at 95 % and 97 % trans mitance,respectively.Thesevaluesaresuperiortothoseof un-dopedCVD grapheneorCVD graphene-AgNW films. Theseoutstandingcombinedperformancesareachievedby usinghighlyscalable,morecost-efective,lestedious,and vacum equipment-freproceses.Thisismostsurprising. (C)Shetresistancevaluesaslowas10and892/0 have benobtained,whicharecomparabletoorbeterthanthose ofhigh-endITOglas.Thesesurprisinglylowshetresis tance valueswere achieved atan opticaltransmitance higherthan80%. Example8:FabricationofOrganicPhotovoltaic DeviceswithAgNW,AgNW-RGO,and [098] Driedgraphiteoxidepowderwasthenplacedina tubefurnacemaintainedatatemperatureof1,050°C.for60 AgNW-PristineGrapheneTransparentElectrodes minutes.Theresultingexfoliatedgraphitewassubjectedto low-powerultrasonication(60wats)for10minutestobreak upthegraphitewormsandseparategrapheneoxidelayers. Severalbatchesofgraphiteoxide(GO)plateletswerepro ducedunderidenticalconditionstoobtainaproximately2.4 kgofoxidizedNGPsorGO platelets.Asimilaramountof GO plateletswasobtainedandthensubjectedtochemical reductionbyhydrazineat140°C.for24hours.TheGO-to hydrazinemolecularratiowasfrom1/5to5/1.Theresulting productsareRGOswithvariouscontroledoxygencontents. Example7:PreparationofThinFilmsfrom Silver Nanowires(AgNW),AgNW/RGO Hybrid,and AgNW/PristineGrapheneHybridMaterials [0102] TotesttheperformanceofAgNW-RGO filmasthe transparentelectrodeinanelectro-opticdevice,weused AgNW,AgNW-RGO,andAgNW-pristinegraphenefilmsas anodelayersinbulkheterojunctionpolymersolarcelsas examples.First,anAgNW paternfortheanodelayerwas prepared onto a glas substrate by spin coating and a photolithographyproces.Then,fortheAgNW-RGO and AgNW-pristinegraphenetransparentelectrodes,paterned AgNW filmwasdipedintotheaqueoussolutionofRGOor pristinegraphene.Thebulkheterojunctionsolarcelswere thenfabricatedonthetransparentelectrodewitha30nmof poly(3,4-ethylenedioxy thiophene):poly(styrenesulfonate) (PEDOT:PSS),100nm ofaP3HTandPCBM blendwitha 1:1ratio,andLiF/Alcathode. [09]SilvernanowireswerepurchasedfromSeashel [0103]Furtherspecificaly,anAgNWtransparentelec Technologies(LaJola,Calif.,USA)assuspensioniniso propylalcoholwithconcentrationsof25mg/ml.Asmal imediatelyspin-coatedwithapoly-3,4-ethyleneoxythio volumeofdispersionwasdiluteddowntoaproximately1 phene:poly-4-sytrensulfonate(PEDOT:PSS).Thethicknes mg/mlwithisopropylalcohol.Thiswassubjectedtohalf an-hoursonicationinasonicbath.Then,thissuspensionwas apliedtoa50mmx100mm poly(ethyleneterephthalate) (PET)substratesbyamanuallycontroledwire-wound,i.e., pushingthesuspensionontopofthesubstratewitharod. [0100]Inadition,AgNWfilmswerepreparedbyspin weightratioof1:1,weredisolvedindichlorobenzene. coatingAgNWinksonglassubstrates.ToprepareAgNW Next,theP3HT:PCBMsolutionwasspin-coatedontopof filmsonglassubstrates,wetreatedglassubstrateswith thePEDOT:PSSlayeranddriedfor60minat50°C.and UV/OzonetomakehydrophilicsurfacesforAgNWspin thenanealedfor10minat10°C.inagloveboxtoform strateandthendriedat120°C.for5min.SeveralAgNW trodewasplacedinanUV/Ozchamberfor3minutesand ofthespin-coatedlayerwasaproximately20nm,andthen thePEDOT:PSScoatedAgNW glassubstratewasanealed on a hot plate for 10 min at 150° C. in a glove box. Poly(3-hexylthiophene)(P3HT)and[6,6]-phenyl-C61-bu tyricacidmethylester(PCBM),whichwereblendedinaPDF Image | HIGHLY CONDUCTING AND TRANSPARENT FILM AND PROCESS
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