Zhigang YANG
,
Hongsheng FANG
,
Jiajun WANG
,
Yankang ZHENG and Chunming LI(Dept. of Materials Science and Engineering
,
Tsinghua University
,
Beijing 100084
,
China)
材料科学技术(英文)
Scanning tunneling microscopy (STM ) has been first employed to study the surface relief accompanying bainite transformation in a Fe-2.17C-12.18Cr-0.31Si-0.26Mn (wt pct) steel. With the exclusive vertical resolution of STM, we observed that the surface relief associated with bainite is a group of surface reliefs related to subplates, subunits and sub-subunits. As a whole, the relief group is in a tent shape, not of invariant plane strain (IPS) type, which is obviously different from that of martensite, and implying that bainite is not formed by shear mechanism. The fine structure of bainite in Fe-1.0C-4Cr-2.0Si (wt pct) alloy has also been studied with STM and TEM. It is found that the bainite plate is composed of subplates, subunits and sub-subunits. On the basis of the fine structure inside a bainitic ferrite plate observed under STM, a sympathetic-ledgewise mechanism of bainite formation is proposed
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金属学报(英文版)
粒裕希停桑谩。疲希遥茫拧。停桑茫遥希樱茫希校佟。希拢樱牛遥郑粒裕桑希巍。希啤。停粒牵危牛裕遥希巍。樱校眨裕裕牛遥牛摹。粒蹋眨停桑危眨停樱桑蹋桑茫希巍。粒蹋蹋希佟。疲桑蹋停?##2##3##4##5ATOMICFORCEMICROSCOPYOBSERVATIONOFMAGNETRONSPUTTEREDALUMINUM-SILICONALLOYFILMSJ.W.Wu,J.H.FangandZ.H.Lu(NationalLaboratoryofMoleculeandBiomoleculeElectronics,SoutheastUniversity,Nanjing210096,ChinaManuscriptreceived27October1995)Abstrcat:Twodifferentsurfacemorphologycharacteristicsofmagnetronsputteredaluminumsilicon(Al-Si)alloyfilmsdepositedat0and200℃wereobservedbyatomicforcemicroscopy(AFM).Oneisirregularlyshapedgrainsputtogtheronaplane.TheotherisirregularlyshapedgrainsPiledupinspace.Nanometer-sizedparticleswithheightsfrom1.6to2.9nmwerefirstobserved.Onthebasisoftheseobservationsthegrowthmechanismofmagnetronsputteredfilmsisdiscussed.Keywords:magnetronsputtering,Al-Sialloy,surfacemorphology,atomicforcemicroscopy,filmgrowthmechanism1.IntroductionTheuseofaluminumalloys[1,2],inparticularAl-Si,isacommonfeatureinmanysinglelevelandmultilevelinterconnectionschemesadoptedinthemanufactureofmicroelectronicdevicesbecauseofseveraldesirableproperties.TheAl-Sigrainmorphology(size.geometryanddistributionofgrainsisassociatedwithstepcoverage[3],electromigration[4]andinterconnectsresistivity[5]etc..Thus,characterizationofAl-Sialloysurfacemorphologyisveryimportant,especiallywhenintegratedintensityincreasesandlinewidthsof0.3to0.5μmbecomecommon.Inthepasttwentyyears,theAl-Sialloysurfacemorphologywhichaffectsthereliabilityofmicroelectronicdeviceshasbeenwidelyinvestigatedbyscanningelectronmicroscopy(SEM),transmissionelectronmicroscopy(TEM)etc.[5-7].However,SEMandTEMhavetheirlimitationorinconvenience,forexample,theverticalresolutionofSEMisnothighandTEMneedscomplexsamplepreparation.Recently,anewgrainboundaryetchingmethodwasproposed ̄[8]whichalsoneedstroublesomechemicaletching.Atomicforcemicroscopy(AFM),sinceitsemerging,hasbecomemoreandmoreusefulinphysics,chemistry,materialsscienceandsurfacescience,becauseofitshighresolution,easeofsamplepreparationandrealsurfacetopography.Recently,discussion[9,10]waspresentedonhowAFMwillplayaroleinsemiconductorindustry.Asaresponsetothisdiscussion,weusedAFMtoinvestigateAl-SialloysurfacemorphologyandhaveobtainedsomeresultswhichcannotberevealedbySEMorTEM.ThisindicatesthatAFMisagoodcharacterizationtoolinsemiconductorindustry.2.SamplePreparationInourexperiments,aluminumwith30ppmsiliconwassputteredonsiliconsubstrateinbatchdepositionmodeAllthreefilmswiththicknessof1.6μmweredepositedusinganargonsputteringpressureof4.2×10 ̄-3Pa.TheotherdepositionparametersaredescribedinTable1.Thesubstratewascleanedusingstandardpremetallizationcleaningtechniquespriortofilmdeposition.3.ExperimentalResultsandDiscussionTheAFMmeasurementswereperformedonacommercialsystem(NanoscopeIII,DigitalInstruments,SantaBarbara).Thetipismadeofmicrofabricatedsiliconnitride(Si_3N_4)Itisattachedtoa200μmcantileverwithaforceconstantofabout0.12N/m.Beforethesurfaceofsamplewasexamined.agoodtipwithananometer-sizedprotrusionatitsendwasselectedbeforehand,whichcanbeobtainedbyimagingtheatomicstructureofmicasubstrateandagoldgrid.AtypicaloperatingforcebetweenthetipandAl-Sisamplesurfaceisoftheorderof10 ̄-8Nandallimagesweretakenatroomtemperatureinair.AtypicaltopographicviewoftheAl-SifilmsisshowninFig.1(allimagescansizeis5by5μma,bandcarerespectivelyforsample1,2,and3).FromFig.la,itcanbeseenthatirregularlyshapedgrainstiltinginvaryingdegreespileupinspace,andgroovesamongtheirregularlyshapedgrainsaredifficulttodecideatacertainarea(wedefineitascharacteristicA).Toourknowledge,onreportsonthesurfacemorphologyhavebeenpresentedbefore.InFig1b,however,irregularlyshapedgrainsassembleonaPlaneandgroovesamongtheirregularlyshapedgrainsareeasytodecide(wedefineitascharacteristicB),whichisinagreementwithmanypreviousreports[5-7].InFig.1c,bothcharacteristicA(arrowA)andcharacteristicB(arrowB)wereobserved.IndoingAFMexperiments,weselectedfivedifferentscanareastobeimagedforeachsampleandfoundthatallimagesofeachsamplearerespectivelysimilartoFig.1a,bandc.Also,wenotedthatthesurfaceofinFig.1a.WethinkthatdepositionparameterswillinfluenceAl-Sisurfacemorphology,andthetiltedgrainsmaybesusceptibletomicrocracking.Byreducingthescansizeareato2by2μm(Fig.2aandb).Weobtainedmanyidenticalresultsasdescribedabove,suchasirregularlyshapedgrainsetc.Forthefirsttime,wefoundnanometersizedparticlesonirregularlyshapedgrainsurfacewhichcannotberevealedbySEMbecausethediameterofthesenanoparticlesisabout10nmandtheheightofthesenanoparticlesisintherangeof1.6to2.9nm.Inimaging,wenotedthatrotatingthescandirectionandchangingthescanfrequencydidnotaffectthestructureofthesegrainsasshowninFig.2aandb,rulingoutthepossibilitythatscanninginfluencedtheshapeoftheseparticlesorcausedsomesimilarimagingartifacts.Also,wenotedthatthenanoparticleswerenotobservedontheslopesofthegrooves(Fig.2aandb).Thisphenomenoncanbeexplainedasfollows:thepotentialenergyattheslopeislargerthanthatelsewhere,sotheparticlesseemmorelikelytobedepositedontheseareaswithlowerpotentialenergy.Fig.2c,scansize250by250nm,isazoomtopographicimage(whiteoutlineinb).Itshowsunevendistributionofthenanoparticles.Andtheheightdifferenceofthenanoparticlesindicatesdifferentgrowingspeed.Wethinkbasedonthemorphologyofnanoparticles,thattheheightdifferenceandunevendistributionofthesenanoparticlesshowdifferentgrowingadvantageandindicatethatatomshaveenoughenergytomovetoasuitablegrowingspot.Theenergymaybefromthefollowingsources:surfacetemperaturefluctuation,stressdifferenceorcollisionbetweenhighspeedsputteredatoms.Thesenanoparticlesgoongrowingandformmanyirregularlyshapedgrains.AndtheseirregularlyshapedgrainsfurtherconnecteachotheraccordingtocharacteristicAorB,finallyformingtheAl-Sisurfacemorphology.4.ConclusionWecandrawthefollowingconclusionsfromtheabove.First,theexperimentalresultsshowedthatAFMisapowerfultooltoinvestigatethedetailsofAl-Sisurfacemorphologywhichcangreatlyenrichourknowledgeofthefilmgrowthmechanism.Second,depositionconditionsplayanimportantroleindeterminingtheAl-Sisurfacemorphology.Third,thetwoAl-Sisurfacemorphologycharacteristicsarethatirregularlyshapedgrainsassembleonaplaneandirregularlyshapedgrainstiltinginvaryingdegreespileupinspace.Fourth,forthefirsttime,nanoparticleswereobservedonirregularlyshapedgrainsurfacewhichsuggestedthatthefilmgrowthmechanismwasbyinhomogeneousnucleation.Acknowledgements-BeneficialdiscussionswereheldwithDr.ZhenandMr.Zhu.ThisworkwaspartiallysupportedbytheNationalNaturalScienceFoundationofChina.RFFERENCES||1D.pramanikandA.N.Saxena,SolidStateTechnol.26(1983)127.2D.pramanikandA.N.Saxena,SolidStateTechnol.26(1983)131.3D.pramanikandA.N.Saxena,SolidStateTechnol.33(1990)73.4S.S.IyerandC.Y.Worg,J.Appl.phys.57(1985)4594.5J.F.Smith,SolidStateTechnol.27(1984)135.6D.GerthandD.Katzer,ThinSolidFilm208(1992)67.7R.J.WilsonandB.L.Weiss,ThinSolidFilm207(1991)291.8E.G.Solley,J.H.Linn,R.W.BelcherandM.G.Shlepr,SolidStateTechnol33(1990)409I.SmithandRHowland,SolidStateTechnol.33(1990)53.10L.Peters,SemiconductorInternational16(1993)62.##61D.pramanikandA.N.Saxena,SolidStateTechnol.26(1983)127.2D.pramanikandA.N.Saxena,SolidStateTechnol.26(1983)131.3D.pramanikandA.N.Saxena,SolidStateTechnol.33(1990)73.4S.S.IyerandC.Y.Worg,J.Appl.phys.57(1985)4594.5J.F.Smith,SolidStateTechnol.27(1984)135.6D.GerthandD.Katzer,ThinSolidFilm208(1992)67.7R.J.WilsonandB.L.Weiss,ThinSolidFilm207(1991)291.8E.G.Solley,J.H.Linn,R.W.BelcherandM.G.Shlepr,SolidStateTechnol33(1990)409I.SmithandRHowland,SolidStateTechnol.33(1990)53.10L.Peters,SemiconductorInternational16(1993)62.##A##BATOMIC FORCE MICROSCOPY OBSERVATION OF MAGNETRON SPUTTERED ALUMINUM-SILICON ALLOY FILMS$$$$J.W.Wu,J.H. Fang and Z.H.Lu (National Laboratory of Molecule and Biomolecule Electronics,Southeast University,Nanjing 210096, China Manuscript received 27 October 1995)Abstrcat:Two different surface morphology characteristics of magnetron sputtered aluminumsilicon(Al-Si)alloy films deposited at 0 and 200℃ were observed by atomic force microscopy(AFM).One is irregularly shaped grains put togther on a plane.The other is irregularly shaped grains Piled up in space. Nanometer-sized particles with heights from 1.6 to 2.9 nm were first observed. On the basis of these observations the growth mechanism of magnetron sputtered films is discussed.
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:magnetron sputtering
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