溶剂热法合成纳米结构四氧化三铁空心微球磁性研究

406Vol．40No．6201112JOURNALOFSYNTHETICCRYSTALSDecember2011230039Fe3O4。XXRD、TEMSEM。Fe3O4400nm40nm。VSMFe3O4。Ms。12hFe3O41000OeM-T778KH=5000Oe100K200K300KFe3O4MsHc。TQ138．1A1000-985X201106-1557-06MagneticPropertiesofNano-structureFe3O4HollowMicrospheresbySolvothermalMethodLVQing-rongFANGQing-qingLIUYan-meiSchoolofPhysicsandMaterialsScienceAnhuiUniversityAnhuiKeyLaboratoryofInformationMaterialsandDevicesHefei230039ChinaReceived13September2011accepted21October2011AbstractFe3O4hollowmicrospheresweresynthesizedbysolvothermalmethod．ThestructureofsynthesizedproductswerecharacterizedbyX-raydiffractionXRDscanningelectronmicroscopySEMandtransmissionelectronmicroscopyTEM．TheresultsshowedthatmonodisperseFe3O4hollowmicrosphereswithpolycrystalstructureareassembledbynanoparticlesandtheiraveragediameterisabout400nm．ThemagneticpropertieswereevaluatedbyavibratingsamplemagnetometerVSM．Theresultsatroomtemperatureindicateas-preparedFe3O4hollowmicrospheresexhibitaferromagneticbehaviorthesaturationmagnetizationMsfirstincreasesthendecreasesasthereactiontimeincreasing．TheresultsatdifferenttemperatureindicatethesaturationmagnetizationMsandcoercivityHcofFe3O4hollowmicropheresfor12hdecreasedasthemeasuretemperatureincreasingandthehysteresisloopsatdifferenttemperatureareallsymmetrical．ThecruietemperatureofFe3O4hollowmicropheresfor12hisabout778KaccordingtoM-Tcurvesat1000Oe．2011-09-132011-10-210904141771972-。[e-mail]rtiesnano-structureFe3O4hollowmicrospheressolvothermalmethodDOI:10.16553/j.cnki.issn1000-985x.2011.06.0021558401、、、。Fe3O4、、Fe3O4、。1-3、45。6-10。Fe3O411-14。Fe3O4Fe3O4Fe3O4。22mmolFeCl3·6H2O20mmol25mL180℃、200℃220℃12h16h20h24h50℃20h。PhilipsX'PertProXXRDSEMXEDSHitachiS-4800TEM、HRTEMSAEDJEOLJEM-2010。BHV-55VSM。33．1Fe3O41200℃、12hXRD7220、311、400、422、511、440533JCPDS79-0419。X311Scherrer1540nm。200℃、12hFe3O4261559C0．27keVAl1．49keVO、FeFe3O4。200℃、12hFe3O4SEMTEM3。3a400nm、、40nmXRD。3bTEM、。3cTEMFe3O440nmFe3O4。HRTEM3dSAED0．25nmFe3O4311。HRTEMSAEDFe3O4。3200℃、12hFe3O4SEMTEMFig．3SEMandTEMimagesofFe3O4hollowmicrospheresat200℃for12hFe3O416-18。Fe3O4。FeCl3·6H2O0．02wt%。Fe3O4NH4Ac+H2O→HAc+NH3·H2ONH3·H2O→NH4++OH－Fe3++3OH－→FeOH3Fe2++2OH－→FeOH22FeOH3+FeOH2→Fe3O4-。3．24SEM4a4b4c200℃、SEM、。。3412h20h24h。4d220℃、12hSEM。3a220℃。180℃、12hFe3O4。5a200℃、12h16h20h24h5bc12h、180℃220℃。180℃、12hFe3O4Fe3O4。1560405a。19Fe-O-Fe。。。20。。12h、180℃Fe3O4。200℃220℃。3．3Fe3O46200℃12hFe3O4H=5000Oe61561100K200K300K。6Fe3O4。21CoFe2O4Co2+。7H=1000Oe200℃、12hFe3O4Fe3O4778KFe3O4858K22。23。4Fe3O4。、400nm40nm。200～220℃12～24hFe3O4。MsMsHC。Fe3O4。12hFe3O41000OeM-T778K。Fe3O4。1KimSWKimMLeeWYetal．FabricationofHollowPalladiumSpheresandTheirSuccessfulApplicationtotheRecyclableHeterogeneousCatalystforSuzukiCouplingReactionsJ．J．Am．Chem．Soc．20021247642-7643．2TanBRankinSE．DualLatex/SurfactantTemplatingofHollowSphericalSilicaParticleswithOrderedMesoporousShellsJ．Langmuir2005218180-8187．3DingYHuYJiangXetal．Polymer-MonomerPairsasaReactionSystemfortheSynthesisofMagneticFe3O4-PolymerHybridHollowNanospheresJ．Angew．Chem．Int．Ed．2004436369-6372．4ZhuLPXiaoHMZhangWDetal．One-PotTemplate-FreeSynthesisofMonodisperseandSingle-CrystalMagnetiteHollowSpheresbyaSimpleSolvothermalRouteJ．Cryst．GrowthDes．20088957-963．5LouXWYuanCRhoadesEetal．EncapsulationandOstwaldRipeningofAuandAu-ClComplexNanostructuresinSilicaShellsJ．Adv．Funct．Mater．2006161679-1684．6ChenXYZhangZJLiXXetal．HollowMagnetiteSpheresSynthesisCharacterizationandMagneticPropertiesJ．Chem．Phys．Lett．2006422294-298．7JiaBPGaoL．MorphologicalTransformationofFe3O4SphericalAggregatesfromSolidtoHollowandTheirSelf-AssemblyunderanExternalMagneticFieldJ．JPhys．Chem．C2008112666-671．8YuDBSunXQZouJWetal．OrientedAssemblyofFe3O4NanoparticlesintoMonodisperseHollowSingle-CrystalMicrospheresJ．JPhys．Chem．B200611021667-21671．9LiXHZhangDHChenJS．SynthesisofAmphiphilicSuperparamagneticFerrite/BlockCopolymerHollowSubmicrospheresJ．JAm．Chem．Soc．20061288382-8383．10HuPYuLZuoAetal．FabricationofMonodisperseMagnetiteHollowSpheresJ．J．Phys．Chem．C2009113900-906．11．-Fe3O4J．200723121958-1962．YanGQGuanJGWangW．MonodispersedFe3O4HollowSubmicro-SpheresPreparedbyPyrolysis-DeoxidizationJ．ActaPhys-Chim．Sin．200723121958-1962inChinese．12．J．2010393656-659．LvQRFangQQLiuYMetal．SynthesisandMagneticPropertiesofNano-structureFe3O4HollowMicrospheresJ．JournalofSyntheticCrystals2010393656-659inChinese．13HuangZBTangFQ．PreparationStructureandMagneticPropertiesofMesoporousMagnetiteHollowSpheresJ．J．ColloidInterfaceSci．20052812432-436．15624014．Fe3O4J．200882394-397．YuLJYuanFLWangX．SynthesisofFe3O4MicrosphereswithHollowStructurebySoftTemplateMethodJ．TheChineseJournalofProcessEngineering200882394-397inChinese．15．XM．1996103-122．FanX．MetallicX-rayPhysicsM．BeijingMechanicalIndustryPress1996103-122inChinese．16SunYXiaY．Shape-ControlledSynthesisofGoldandSilverNanoparticlesJ．Science20022982167-2170．17WangYJiangYXiaY．ASolution-PhasePrecursorRoutetoPolycrystallineSnO2NanowiresthatCanbeUsedforGasSensingunderAmbientConditionsJ．JAm．Chem．Soc．200312516176-16177．18DengHLiXLPengQetal．MonodisperseMagneticSingle-CrystalFerriteMicrosph