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1、Chem.Mater.2005,17,6819-68346819ThermalOxidationProfilingofSingle-WalledCarbonNanotubesBrianJ.Landi,²,³CoryD.Cress,²,³ChrisM.Evans,²andRyneP.Raffaelle*,²,³,§NanoPowerResearchLaboratories(NPRL),DepartmentofMicrosystemsEngineering,andDepartmentofPhysics,RochesterInstituteofTechnol
2、ogy,Rochester,NewYork14623ReceiVedSeptember5,2005.ReVisedManuscriptReceiVedOctober27,2005Theuseofthermaloxidationprofiling(TOP)tomonitorthepropertiesofsingle-walledcarbonnanotube(SWNT)-containingsamplesatincrementaltemperatureintervalshasbeendeveloped.Specifically,thethermaldeco
3、mpositionofrawandacid-refluxedSWNTsamplesisevaluatedbyasystematicseriesofoxidativethermaltreatmentswithconcomitantpurityassessmenttoascertaintheSWNTmassretention.TheTOPresults,supportedbyRamanspectroscopy,indicatethattheSWNTdecompositioncoincideswiththeonsetofrawsootcombustion.T
4、hetemperatureforthisSWNTcombustiononsetisequivalenttopuremetal-catalystoxidation,particularlyforthehighlyexothermicCometal.Thus,therearenodiscernibleregionsofarawsootthermogravimetricanalysis(TGA)curvethatcanbeascribedtoSWNTcombustionindependentofmetalimpurityinfluence.Incontras
5、t,theacid-refluxedSWNTsampleshowsthatchemicaloxidationofthemetalcanenableoptimizationofSWNTretentionduringthermalpurification.Theestablishedunderstandingbetweentimeandtemperatureonthermaloxidationallowsforpurificationefficiencies(thehighestpurityatthemaximumretention)of75%w/wtob
6、eachievedinlaser-producedSWNTs,withoutmodificationtothediameterdistribution.Introductionbutthereisnosinglemetricwhichaccuratelyquantifiesthetypes,amount,andmorphologyofSWNT-containingmateri-Single-walledcarbonnanotubes(SWNTs)arebeingals.Ingeneral,themostimportantcriterionistheªp
7、urityº,investigatedforavarietyofapplicationsbasedontheiruniqueelectrical,optical,andmechanicalproperties.1-4orquantityofSWNTspresentinrelationtootherbyproductsfromthesynthesis.Therefore,itisessentialthatapreciseWhilesuchpropertiesaretrulysignificant,thepracticaldefinitionbeestab
8、lishedforbothmeasurementandterminol-realization