羧基化氧化石墨烯的制备及其电化学性能

201322286－90CN53－1192/NISSN1672－8513doi10．3969/j．issn．1672－8513．2013．02．003http//xb.ynni.edu.cn2012－12－11．2007B148M－MZY111611HXYJS07．1987－．．1962－．．－650500Hummers．、、XRD．．．TQ127.1A1672－8513201302－0086－05SynthesisofcarboxylationofgrapheneoxideandcharacteristicsofelectrochemicalpropertiesWANGZheng-weiXIONGLiGAOYun-taoWANGZhen-fengYANLi-liZHANGHong-jiaoZHAOJieMAOChang-yingKeyLaboratoryofChemistryinEthnicMedicinalResourcesStateEthnicAffairsCommissionandMinistryofEducationYunnanUniversityofNationalitiesKunming650500ChinaAbstractThisresearchsynthesizedgrapheneoxideandcarboxylgrapheneoxidebasedonHummersmethod．ThestructureandpropertiesofcarboxylatedgraphemewereanalyzedwiththermogravimetryFouriertransforminfraredspectrophotometerX－raydiffractionspectroscopyandscanningelectronmicroscope．Theelectrochemicalproper-tiesweredetectedbythecyclicvoltammetrymethodandthedifferentialpulsevoltammetrymethod．Theresultsshowthatthecarboxylatedgraphemenotonlyhasbettersolubilityinwaterbutalsohasbettercatalysis．KeywordsgrapheneoxidecarboxylgrapheneoxidecyclicvoltammetrymethodelectrochemicalpropertiesGrapheneG2004．sp2、、1．、2－3．4－6．、、、7．8．GrapheneOxideGO．、9．sp3p．ReducedGrapheneOxideR－GOπ－π．GO－COOH10－1112．．Hummers132．．11.195%～98%30%．EPED－20TH．TDL80－2BAS3120AD280WMEC－12B．/GO－COOH/GCE223NICOLET－iS10USAXD/max－3BFEIQuanta200．1.22.0g3.0g96.5mL500mL80±3℃5h．6～8℃1.0g、12.5g8℃．1h35±3℃2h．200mL40～60℃94℃0.5h．100mL17.0mL30%．4000r/min20min1.5L5%．、、．65℃．1.314100mg100mLGO6.0gNaOH5.0g3h．65℃．1.4FTIR10℃/minTGCuKαλ=0.154nm40kV200mA10°/min2θ5°～80°XRDSEM．1.510mg10mL10mL5h1mg/mL．10μLGlassyCarbonElectrodeGCE．0.2mmol/L－/GO－COOH/GCE、－0.2～0.8VCVDPVCVDPV．22.1．1、2、3、4h．3h．2.2NaOH．．．80℃．7822.3GO、R－GOGO－COOH2.3.1GO、R－GOGO－COOHTGGOa、R－GObGO－COOHc1GOaGO－COOHc200℃R－GOb100℃．200～230℃GOGO25%．R－GO．GO－COOHGO．900℃GO－COOH．2.3.2GO、R－GOGO－COOHFTIR．2aGO—OH3438.71cm－1CO1711.12cm－11650cm－1C—O—C1127.38cm－11264.78cm－1R－GO2b—OH3480.00cm－13188.88cm－1CO1695.00cm－1C—O—C1127.76cm－11206.12cm－1R－GOCOC—O—C2c—OH3445.07cm－13142.06cm－1CO1599.72cm－1C—O—CGOC—O—C．2.3.3XRD3GOa、R－GObGO－COOHcX．、、、3aGO2θ=12．14°、Bragg2dsinθ=λdθλXd．R－GO2θ=22.72°3b、．3cGO－COOH2θ=31.83°8822．2.3.4GOa、R－GObGO－COOHc64．4aGO．4bGOR－GOR－GOπ－πGO．R－GO4cGO－COOHGO．2.4R－GOGO－COOH5h5ab．π－π．—OH—COOH、．2.56GCEa、R－GOR－GO/GCEbGO－COOHGO－COOH/GCEc0．2mmol/LK3FeCN6/K4FeCN6．K3FeCN6/K4FeCN6R－GOGO－COOHGO－COOH．GO－COOH．982K3FeCN6/K4FeCN6．3、．TG、FTIR、XSEM．GO－COOHR－GO．1NOVOSELOVKSGEIMAKMOROZOVSVetal．ElectricfieldeffectinatomicallythincarbonfilmsJ．Science20043065696666－669．2KUILLATBHADRASYAODa-huetal．Recentad-vancesingraphenebasedpolymercompositesJ．Pro-gressinPolymerScience201035111350－1375．3FRAZIERRMHOUGHWLCHOPRANetal．Ad-vancesingraphene－relatedtechnologiessynthesisde-vicesandoutlookJ．RecentPatentsonNanotechnology201262079－98．4．J．20119205327．5KUILATBOSESKHANRAPetal．Recentadvancesingraphene－basedbiosensorsJ．BiosensorsandBio-electronics201126124637－4648．6LIZai-junXIAQF．Recentadvancesonsynthesisandapplicationofgrapheneasnovelsensingmaterialsinana-lyticalchemistryJ．ReviewsinAnalyticalChemistry201231157－81．7．J．2011266561－570．8．J．20113414－10．9BASAVARAJACKIMWJKIMYDetal．Synthesisofpolyaniline-gold/grapheneoxidecompositeandmicrowaveabsorptioncharacteristicsofthecompositefilms．MaterialsLetters2011659/203120－3123．10DONGHai-qingZHAOZhi-leiWENHui-yunetal．Polyethyleneglycolconjugatednano-grapheneoxideforphotodynamictherapyJ．SciChinaChem201053112265－2271．11．J．2011421104－107．12．J．201030830－34．13HUMMERSWSOFFEMANRE．PreparationofgraphiticoxideJ．JournalofAmericanChemicalSociety19588061339．14HERMANSONGT．BioconjugatetechniquesM．2ed．SanDiegoAcademicPress1996．0922