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首页 简单水热方法合成自组装镍球及其磁性能研究.doc

简单水热方法合成自组装镍球及其磁性能研究.doc

简单水热方法合成自组装镍球及其磁性能研究.doc

上传者: 薛言宇 2017-12-22 评分 0 0 0 0 0 0 暂无简介 简介 举报

简介:本文档为《简单水热方法合成自组装镍球及其磁性能研究doc》,可适用于综合领域,主题内容包含简单水热方法合成自组装镍球及其磁性能研究简单水热方法合成自组装镍球及其磁性能研究第卷期年月安徽师范大学(自然科学版)JournalofAnhuiNo符等。

简单水热方法合成自组装镍球及其磁性能研究简单水热方法合成自组装镍球及其磁性能研究第卷期年月安徽师范大学(自然科学版)JournalofAnhuiNormalUniversity(NaturalScience)VNoMayASimpleHydrothermalRoutetoSelfAssemblyMetallicNickelSphereswithOrientedAttachmentStructureandMagneticPropertySANGYan,ZHANFangming,GENGBaoyou(CollegeofChemistryandMaterialsScience,AnhuiKeyLaboratoryofFunctionalMolecularSolids,AnhuiNormalUniversity,Wuhu,Chim)Abstract:Wereportarationalsynthesisofselfassemblymetallicnickelspheresbyaconvenienthydrothermalmethod,anddemonstrateahovel,feasible,andlargescalesynthesisofmetallicnickelmicrostructuresThepresenceofdiacetyldioximewasfoundtoplayanimportantroleintheformationofspheralstructureTheassynthesizedNispheresshowremarkablyenhancedcoereivitySincetheformationofarelativelystablecomplexisuniversalforvarioustransitionmetals,webelievesucharationallowtemperaturesyntheticroutemaybeversatileandcanbeadaptedforthefabricationofothertransitionmetalsortheiralloysKeywords:metallicnickelsphereselfassemblyhydrothermalmethodmagneticpropertyClassificationNo:(Documentcode:APaperNo:()Magneticnanoparticleshavereceivedconsiderableattentionbecauseoftheircrucialapplicationsinthefieldsofhighdensitymagneticstoragedevices,magneticfluids,magneticrefrigerationsystems,contrastenhancementinmagneticresonanceimaging,andmagneticcarriersfordrugtargetingandcatalysis【'Moreovermagneticassemblynanostructureshavebeenpaidparticularattentionfortheiruniquepropertiesandpotentialapplicationsinelectron,magneticrecording,biomedicaldiagnosis,etcGenerally,therearemainlytworoutesforthepreparationofassembledmagneticnanostructuresOneishashingthemolecularinteractionsofsurfacefunctionedparticles,includingvanderWaalsforces,一不interactionselectrostaticforcesandhydrogenbondingL'Forexample,assemblyofmagnetiteandmaghemitefilmsselfassembledbymonodisperseFePtnanopartieleswereallconstructedbythemediationofsurfactantsorpolymersInthismethod,thecontentofthesurfactantsorpolymersintheassembledstructureswasrelativelyhighandsometimestheassembliescollapsedwhenthesurfacecoatedsurfactantswereremoved,whichresultedindifficultiesintheirpotentialapplicationsasnanodevicesTheotherefficientmethodfortheassemblyofmagneticnanopartielesismakinguseoftheexternalmagneticfieldTheapplicationofamagneticfieldtoasuspensionofmagneticparticlestypicallyproducesonedimensional(D)chainsofparticleswiththeirmagneticdipolesalignedheadtotailparalleltothemagneticfieldTheDmicrowiresofCoPtnanocrystals,elongatedclustersofFeznanoparticles,nanochainsofcolloidalnickelnanoparticleswereallformedunderastrongmagneticfield引ButtheseselfassembliesusuallyrequiredanexternalmagneticfieldtoremainstableandwhentheexternalmagneticfieldwasremovedthestructureswoulddestabilizeCurrently,itisstillchallengingforexploringsimpleandconvenientapproachestothepreparationofselfassemblystructuresNanosizedparticlesofnickelshowdiverseapplicationsascatalysts,magnetrecordingmedia,medicaldiagnosisandconductingmaterials【'Inthepastdecades,variousshapednickelnanostructureshadbeenReceiveddate:ooFoundationitem:SupportedbytheNationalScien~FoundationofChina(No)theProgramforInnovativeResearchTeaminAnhuiNormalUniversityAuthor'sbrief:SangYan(一),female,borninSuzhongCity,AnhuiProvince,Mast日,Majorinmaterialschemistry安徽师范大学(自然科学版)O年fabricatedwithrespecttothedependenceofprope~iesonmorphology,includingnanorods,nanoprisms,nantubeS,hollowspheres,nanobelts,nanoflowers,nanochain,etc'HereinwedescribeasimplehydrothermalreductionroutetosynthesizehighlyorderedmetallicnickelselfassemblysphereswithhighyieldTheselfassemblynickelspherescanbeexpectedtobringaboutnewopportunitiesinvastresearchandapplicationfields,suchassensors,micronanodevices,eteThechemicalreductioncanbeformulatedasfollows:Ni(CHNO)NHOH一*NiN千HOCHN()ThemagneticbehavioroftheselfassemblymetallicNinanospheresisthenstudiedExperimentsamplepreparationandpretreatmentsAnthereagentsusedwerepurchasedfromBeijingChemicalReagentLtdandusedwithourtherpurificationDistilledwaterwasusedthroughoutInatypicalprocedure,g(retoo)NiCHOwasdissolvedintomdistilledwaterwithvigorousstirringThenanethanolsolutionofmLwtdiacetyldioximewasaddeddropwiseAfterbeingstirredwithamagneticblenderformin,thesolutionturnedredThecoordinationcompoundNi(CHN)solutionareobtainedThen,gNaOH(Omo)wasaddedslowlytotheabovesolutionFinally,amlofwthydrazinehydratesolution(NHHO)wasaddeddropwisetotheabovesolutionwithvigorousstirringAfterstirringforlOmin,themixturewastransferredintoamofTeflonlinedstainlesssteeautoclavewhichwastreatedatCforhAftertheautoclavehadcooledtoroomtemperature,ablacksolidproductwasdepositedonthebottomoftheTefloncupThefinalproductwascentrifugedandrinsedwithdistilledwaterandethanolforseveraltimes,andthenwasdriedinavacuumovenatCforhCharaeterizationXraypowderdiffraction(ram)wascarriedoutonanXRI)(Japan)XraydiffraetometerwithCuKaradiation(k=A)atascanningrateof'sScanningelectronmicroscopy(SEM)micrographsweretakenusingaHitachiSScanningelectronmicroscopeTransmissionelectronmicroscopy(TEM)micrographswereperformedusingJEMFmicroscopesoperatedatoptimumdefocuswithacceleratingvoltagesofkVMagnetichysteresisloopsaremeasuredusingavibratingsamplemagnetometer(VSM,BHV)FormagnetizationmeasurementsthepowderispressedstronglyandfixedinasmallcylindricalplasticboxResultsanddiscussionThephasepurityoftheaspreparedsampleswascharacterizedby暑powderXRDFigureshowstheXRDpatternofaspreparedself一言assemblymetallicNinanospheresAlldiffractionpeaksinthis重patternareingoodagreementwiththestandardJointCommitteeonPowderDiffractionStandards(JCPDS)cardNoNocharacteristicpeaksduetotheimpuritiesofnickeloxidesorhydroxidesaredetected,indicatingthattheaspreparedproductsThetadegreeobtainedbythepresentsyntheticrouteconsistofasinglephaseofa'…一FigureXRDpatternoftheaSpreparedselflacecenteredcubicmetallicN…Themorphologiesofaspreparedsampleswerestudiedbyfieldemissionscanningelectronmicroscopy(FESEM),AsshowninFigure,sphericalparticleswithasizeofcanmhavebeenobservedMostofthespheresarewellseparated,althoughasmallnumberoftheappeartoaggregatetogetherHighmagnificationSEMimagesindicatethatthespheresconsistof卷第期桑艳,詹方明,耿保友:简单水热方法合成自组装镍球及其磁性能研究alInpanidesAsreportedpreviously,metallicFespherestendtoformnanlresinanaqueussVstembecauSeofmternalattractiveforces儿However,inthepresentsystem,largeNisphereSappeaLrtostayweseparated,whichmaybeattributedtothestericeffectofdiacetyldioximemoleculeSInFigured,aSEMimagewithhighermagnificationisshown,revealingthesurfacetpographyfSeveralindividualparticlesThesurfaceofeachparticleiscomposedofalargenumberofra【ndmlyarranged,irreguarnanoscaleprotrusionsapproximatelynminsizeEachparticleappearStoconsistofmanvnanometersized,crystallinesubunitswithwelldefinedgrainboundariesThestructureofthepartjcJeSarisfrOmthesubunitgm叭handaggregationthatoccurduringthemildreductionAccordingtotheparticlegrowthmodeproposedbyMatijevicJandVanBlaaderen,anucleationburstoccursncethecncentrationfthemetaatOmsreacheSacnticalsupersaturationThenthenucleationsitesgrowintonanoscaleprimaryparticesbvdtusncaptureoftheremainingatomsTheseprimaryparticlesthenformaggregates,underappropriatereactOncndltlons,leadingtotheformationoflargersphericalaggregateswithasurprisinglynamwDanice"gurea,b,c)SEMimagesofthesynthesizedmetallicNispheresatdifferentmagnicationsd)MagnifiedSEMimageofsinglemetallicNisphereFurtherinsightintothemorphologyandmicrostructureofthemetallicNinanOstruetureswasgainedusingtransmissionelectronmicroscopy(TEM)FigureashowsatypicalTEMimageofmetallicNiproducts,'ndicatingthattheproductsconsistedofalargequantityofspheresInFigureb,aTEMimagewithhighermagnificationisshown,revealingallNinanoparticleswereselfassembledintothesphericalaggregateswithlargerdimensionsBasedontheaboveSEMandTEMimages,theformationprocessofthemetallicNinanosDherescanbeproposedaSoccurringby"conglomeration"ofthenanoparticlesprecursors,untilspheresareformedTheformationoftheNisphericalaggregatedparticlescanbesuggestedaSfollows:nonodispersedNinanoparticeswiththenanometeredsizearefirstlyformedthroughthereductionofNi(CHN)byhydrazinehydrateWiththeIncreaseofheatingtime,thesenanoparticlesthenslowlyselfaSsembIewitheachOthertfrmtheNi安徽师范大学(自然科学版)矩nmFigurea)TEM~llgesofthesynthesizedmetallicNispheresb)MagnifiedTEMimageofsinglemetallicNispheresphericalaggregatedparticlesinthepresenceofdiacetyldioximeWefoundthatifnodiacetyldioximeexistinthereactionsolution,thesmallNinanoparticlescanalsobegenerated,buttheywereaggregatedinarandommanner,resultinginirregularagglomeratesTherefore,diacetyldioximecontributedtoformingsphericallyaggregatedparticlesandeffectivelypreventingtheNinanoparticlesfromrandomagglomerationThemaindrivingforcefororientedaggregationofnanoparticlescanbegenerallyattributedtothetendencyforreducingthehighsurfaceenergythroughboththeattachmentamongtheprimarynanoparticlesandtherotationoftheseprimarynanoparticlestogivecoherentlatticestructureatgraininterfaces,ie,orientedattachmentfororientedaggregation)一HeretheNinanoparticlesstabilizedwithdiacetyldioximeCanformanalmostperfectorientedstructurewithinaggregatedspheresAnditisbelievedthatdiacetyldioximemolecules,whichattachedonthesurfaceoftheNinanoparticlesinthenonaqueoussystem,playanimportantroleinformingsuchanorientedstructurebyfacilitatingtherotationoftheNinanoparticlesThemagneticpropertiesofnanomaterialshavebeenbelievedtobehighlydependentonthesampleshape,crystallinity,magnetizationdirection,andsoonThus,aremarkablyenhancedferromagneticpropertyOftheassynthesizedmetallicNispheres,comparabletothatofNi量nanoparticles,shouldbesupposedFigureshowsmagnetichysteresiscurveforthesynthesizedmetallic,,一一f,,NispheresmeasuredatroomtemperatureThesaturationmagnetizationHfe,硼舢(Ms),remanentmagnetization(Mr),coercivity(Hc)arecaemug,,FigureMagnetichyseresisemug,andOe(emu=Amkg一,lOe=lOnmeaseledatempeTatueo印heIesAm)forthesynthesizedmetallicNispheres,respectivelyWhile,relativetothatofthebulknickel(emug,,emug,,Oe),thereducedvalueofMscouldbeduetotheinclusionofsomenonmagneticresiduesfromtheproductionDr()cessaswelasduetotheincreasedinteractionsbetweenthenanocontactedsubunitswhichreducethetotalmagneticmomentInaddition,ascomparedtothecoercivityvalueofthebulkNitheselfassemblyNinanometersizedspheresexhibitmuchenhancedcoercivity,whichmaybeattributedtotheirsphericalselfassemblystructuresConclusionsInsummary,wehavefoundasimpleandmildhydrothermalreductionmethodtopreparespheresofIceNiinhighyieldTherearetwokeypointsforthepreparationofNinanopheresinaqueoussolution:the卷第期桑艳,詹方明,耿保友:简单水热方法合成自组装镍球及其磁性能研究preformationofthecomplexNi(CHN)andtheselectiveuseofthereducingagentNHHOTothebestofourknowledge,thisworkisthefirstconcerningthesynthesisofferromagneticmetalspheresinaqueoussolutionTheassynthesizedNispheresshowrenmrkablyenhancedcoercivitySincetheformationofarelativelystablecomplexisuniversalforvarioustransitionmetals,webelievesucharationallowtemperaturesyntheticroutemaybeversatileandcanbeadaptedforthefabricationofothertransitionmetalsortheiralloysReferences:sIs,Recentadvanceinchemicalsynthesis,assemblyandapplicationsofFePtnanopartielesJAdvMater,,:BAIAK,FRANIABL'UZUNO,etaModulationofspacingandmagneticprope~iesofironoxidenanoparticlesthroughpolymermediated"bricksandmortar"selfassemblyJChemMater,,:CARUSOF,CARUSOR,MOHWALDH,NanoengineeringofInorganicandHybridHollowSpheresbyColloidalTemplatingJScience,:一lMIRKINCA,LETSINGERRL,etaADNAbasedmethodforrationallyassemblingnanoparticlesintomacroscopicmaterialsJNature,:TANASEM,BAUERLA,卜n『ITGRENA,etaMagneticAlignmentofHuorescentNanowiresJNanoLett,,:SAH(X)Y,cHEONM,LUOH,PRASADPN,FielddirectedselfassemblyofmagneticnanoparticlesJJPhysChemB,,:ZHANGWX,WANGCB,LIENHL,TreatmentofchlorinatedorganiccontaminantswithnanoscalebimetallicparticlesJCafAlToday,,:PIT】VF,KRISHNANKM,ALIsAT()SAP,ColloidalNanoerystalShapeandSizeControl:TheGaseofCobaltJScience,,:BRADLEYJS,TESCHEB,REETZMT,SurfaceSpectroscopicStudyoftheStabilizationMechanismforShapeSelectivelySynthesizedNanostmcturedTransitionMetalColloidsJJAmChemSoc,,:BAOJ,TIEC,xUz,ZHOUQ,SHEND,MAQ,TemplatesynthesisofanarrayofnickelnanotubulesanditsmagneticbehaviorJAdvMater,,:LULR,AIZH,LIJP,ZHENGZ,LIQ,ZHANGLZ,SynthesisandCharacterizationofFeFeCoreShellNanowiresandNanonecldacesJCrystGrowthDes,,:EERDJI,ARcND,JAGLICICZ,NIEDERBERGERM,NonaqueousSynthesisofManganeseOxideNanoparticles,StructuralCharacterizationandMagneticPropertiesJJJPhysChemC,,:GOIADV,MATUEcE,PreparationofmonodispersedmetalparticlesJNewJChem,,:VELIKOVKP,ZEGERSGE,BlaaderenAvan,SynthesisandCharacterizationofLargeColloidalSilverParticlesJLangmuir,,:】一】简单水热方法合成自组装镍球及其磁性能研究桑艳,詹方明,耿保友(安徽师范大学化学与材料科学学院,安徽芜湖)摘要:报道了一种获得自组装镍球的简单方法,丁二酮肟在镍球的合成中起到了非常关键的作用所获得的镍球表现出非常大的矫顽力,具有重要的应用前景同时,这种低温合成方法有望用来制备其他的过渡金属及其合金关键词:金属镍球自组装水热方法磁性能纠mHrrir}rLfL

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