Yuanzheng YANG
,
Qiaoshen LI
,
Youlan ZHU
,
Xueming MA
,
Yu
,
a DONG
材料科学技术（英文）
Amorphous and nanostructural Fe-B alloys made by mechanical alloying of elemental Fe and amorphous B powders have been studied using X-ray diffraction, differential scanning calorimetry and Mössbauer spectroscopy. It has been shown that the milling conditions have a strong effect on the alloying. The single-phase amorphous alloy, which is limited at nominal composition of Fe60B40, has been produced only by milling in Ar atmosphere and in other composition range the mixture of nanostructure Fe-like phase and Fe2B compound with a little amorphous phase are obtained. While by milling in air atmosphere the introduction of oxygen in air may suppress the formation of amorphous phase, thus the compounds Fe2B may be synthesized with no trace of amorphous phase. The crystallization temperatures of amorphous phase in the resultant products are higher than those of a single amorphous alloy Fe60B40, and hardly independent of the milling conditions and the composition. In addition, it is revealed that detectable B content in the final products is lower than the nominal composition of all the initial samples, which indicates that some B atoms may be located in the disordered interfacial regions of the nanostructural alloyed mixtures.
关键词:
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.
关键词:
:magnetron sputtering
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