金属学报(英文版)
茫遥伲樱裕粒蹋蹋桑冢粒裕桑希巍。希啤。疲錩(38)Ni_(39)Si_(10)B_(13) METALLIC GLASS UNDER HELIUM ION IRRADIATION##2##3##4##5CRYSTALLIZATIONOFFe_(38)Ni_(39)Si_(10)B_(13)METALLICGLASSUNDERHELIUMIONIRRADIATION$YANGQifa(ChinaInstituteofAtomicEnergy,Beijing)ZHANGGuoguang;SHENWanshui(UniversityofScienceandTechnologyBeijing)Manuscriptreceived20February1995ThecrystallizationfeaturesofFe38Hi39Si10B13metallicglassunder100keVand6μA/cm2heliumionirradiationwithdifferentdosesarereported.ItisfoundthattheFe38Ni39Si10B13metallicglasscrystallizedundertheheliumionirradiationatthetemperaturelowerthantheordinarythermalcrystallizationtemperature.ThepreferentialprecipitationphaseisFeSi,andfollowedbytheeutecticphaseα-Fe.Thecriticaldosefortheformationofheliumbubblesinthematerialisaround5x10￣16/cm2.Thesensitivityofcrystallizationduetothetemperaturerisingunderheliumionirradiationandthemechanismofthesequenceofprecipitatedphasearebrieflydiscussed.Keywords:Fe38Ni39Si10B13,metallicglass,crystallization,helium,ionirradiationTheblisteringorflakingoffirstwallmaterialsinducedbyheliumionbombardment,whichisrelevanttothefirstwallsurfaceerosionandplasmacontamination,isacriticalproblemtobeconsideredinfusionengineering.Becauseofthefavourablyphysical,chemicalandotherproperties,especially,thebetterresistanceofblistering,metallicglassesareexpectedtobeapromisingcandidatematerialforthefirstwall.TyagiandNanderkarstudiedsystematicallytheblisteringphenomenaofsomemetallicglassmaterialsunderheliumionandprotonbombardmentwithvariousionenergy,ioncurrentdensityanddose,andfoundthecriticaldoseforblisteringofthesematerials[1-3].However,itisverysuspiciousthatmetallicglasseswillcrystallizeunderheliumionirradiationtolosetheiramorphouscharacter,whichwilldeterioratetheirproperties.GusevaandGordeevareportedthatFe40Ni40B20metallicglassbombardedbyheliumionwithenergyof40keVandionbeamcurrentdensitiesof5-40μA/cm2partiallycrystallizedbelowitsordinarythermalcrystallizationtemperature[4].ByusingXRDexamination,itwasfoundthatα-FeandM3B,M2BandMBwereprecipitated(whereM=FeandNi)underheliumionbombardmentwith5μA/cm2and100μA/cm2ioncurrentdensitiesrespectively.Nevertheless,TyagiandNanderkarfoundthatsomemetallicglassescrystallizedandsomedidnotundersameirradiatedparameters[1-3].Consequently,itisnecessarytoinvestigatetheirradiation-assisted-crystallizationfeatureofmetallicglassesbyheliumionirradiationfortheirapplicationinfusionengineering.Inpresentexperiment,thecrystallizationfeatureofFe38Ni39Si10B13metallicglassunderheliumionirradiationwithenergy100keVandvariousdosesintherangeof5×1016/cm2to1×1018/cm2,andthedistributionofheliumbubblesinmaterialaremeasuredbyusingtransmissionelectronmicroscope(TEM)andX-raydiffraction(XRD).1.ExperimentalApproachTheas-receivedFe-Ni-Si-Bmetallicglassribbonswith10mminwidthand0.2mminthicknessweresuppliedbyBeijingInstituteofMetallurgy.Thenominalcomposition(wt%)ofthematerialisNi47.37,Fe43.91,Si5.81andB2.91fromthechemicalanalysisandthecalculatedconstituentisFe38Ni39Si10B13.TheX-raydiffractogramofas-receivedmaterialdemonstratedthattheas-receivedmaterialhasagoodamoophouscharacter.Thetheimalcrystallizationprocessoftheas-receivedmaterialwastestedbydifferentialthermalanalysis(DTA).Theordinarythermalcrystallizationtemperaturewasdeterminedtobeabout490℃.Rectangularsampleswithanareaof1×2cmanddiscsampleswith3mmindiameterwereemployedrespectivelyforXRDandTEMexperiments.ThesamplesforXRDweremechanicallypolishedtomirrorsurfaee.Ontheotherhand,formakingTEMsamples,thepiecescutfromtheribbonwerethinnedto30μmthicknessfirst,thenpunchedout3mmdiscs,electrothinnedinamixedsolutionof10%perchloricacidand90%ethanolandfinally,thediscswereionmilledtoextendthethinarea.HeliumionirradiationofsampleswascarriedoutonTS51-200/ZKionimplanterinChinaInstituteofAtomicEnergy.ThesampleswerefixedonacopperholderwhichwascooledbyF-113coolant.Thevacuumintargetwasbetterthan3×10-3Paandthescanningareaofionbeamwasabout3×7cm.Thetemperatureridingofthesamplescausedbyionbeambombardmentwasmeasuredbythermalcouple.Undertheirradiationparametersofionbeamenergy100keVandionbeamcurrentdensity6μA/cm2,thetemperaturerisingofsampleswaslowerthan200℃.Theiondosesofimplantedsampleswerechosenfrom5×10￣16/cm2to1×10￣18/cm2inpresentexperiment.AJEOL-100CXTEMoperatedat100kVwasused.Thecalculatedmeanprojectrangeandrangestragghngofheliumionwithenergy100keVinthematerialwere306.9nmand85.5nmrespectively,whichwassimulatedbycodeTRIM86.2.Results2.1CrystallizationunderionirradiationTheselectedareadiffraction(SAD)patternsofun-irradiatedandirradiatedsamplesareshowninFig.l.Fortheun-irradiatedsample,thepatterniscomposedoftwoconcentricringswhichexhibitatypicalamorphousdiffractionfeature(Fig.la).Ontheotherhand,forirradiatedsamples,agroupofnewconcentricringsappearsonthebaseofamorphousdiffractionrings,whichmeanstheoccurrenceofpartialcrystallizationandtheformationofsomenewprecipitationphasesinoriginalamorphousmaterialsbyionirradiation.Withtheincreaseofiondose,theinitialamorpohousdiffractionringsbecomefainterandtheintensitiesofdiffractionringsprodueedbyprecipitatesdevelopehigher.Itisexpectedthatthecrystallizationinsamplesincreaseswiththeincreaseiniondose.Moreover,iftheiondoseislowerthan5×10￣17/cm2,thepatternsshowtypicalpolycrystallinediffractionfeaturewithrandomorientationandveryfinegrains(Figs.lbandlc),butfor1×10￣18/cm2iondose,somebrightspotsarise(Fig.ld),thismeansthatsomerelativelargegrainsformedinsampleunderirradiation.FromtheX-raydiffractogramofthesampleirradiatedbyheliumiontodoseof5×10￣17/cm2,thediffractionpoaksarestillamorpohousfeatureandnonewpeaks.Itispredictedthatthecrystallizationonlyoccursintheprojectedrangeofions.2.2AnalysisofprecipitationphaseFromindexingofdiffractionringsinFig.lbandFig.lc,theprecipitatephaseisanfcccrystallinestructure.InFig.ld,anadditionalbccphaseisfound(ring3,ring5andring8).Thecalculatedlatticeparametersforprecipitatephasesundervariousiondosesareasfollows:5×1016/cm2a=0.412nm(fcc)l×1017/cm2a=0.42lnm(fcc)5×1017/cm2a=0.428nm(fcc)l×1018/cm2a=0.478nm(fcc)a=0.292nm(bcc)UsingASTMindex,itisidentifiedthatthebccphaseisα-Fe(a=0.2866nm).Todeterminethefccprecipitatephase,weinspectedallcompoundswithfcccrystallinestructurecomposedofelementsFe,Ni,SiandB,foundthatthreecompoundsFeSi(a=0.446nm),FeNi3(a=0.353nm)andFe3Si(a=0.564nm),butthemostfavourablecompoundwasFeSi.Therefore,itisassumedthatthepreferentialprecipitatephaseisFeSi,andisfollowedbytheeutectcphaseα-Feundertheheliumionirradiation.2.3HeliumbubbledistributionThemorphologiesofheliumbubblesformedbyagglomerationofimplantedheliumionsareshowninFig.2.Thesmallblackdotspresentbubblesunderbrightfieldwiththeunderfocusingoperation.FromFig.2,itisrevealedthatbubbleslowerthedensity,butinflateinthedimensionwiththeincreaseiniondose.Moreover,underthehigherdosethebubblesjoinedtogether.Fig.3plotsthechangesofdensitiesanddiametersofbubbleswiththeiondose.ItisevidentthatthecriticaldosetoformbubblesinFe38Ni39Si10B13islowerthan5×1016/cm2,whichisslightdifferentfrom1×1017/cm2reportedbyTyagi[1].3.DiscussionAstheresultsreportedbyGusevaandGordeeva[4],theheliumirradiationcantrulybringonthepartialcrystallizationinmetallicglassFe38Ni39Si10B13belowitsordinarythermalcrystallizationtemperature.GusevaandGordeevaconfirmedthattheprecipitatesinFe40Ni40B20wasα-Fephaseunderheliumionirradiationof40keVenergyand5μA/cm2currentdensity,inwhichthetemperaturerisingofthesampleswaslowerthan200℃.Howerve,inpresentexperiment,thoughα-Fephaseisdetermined,notraceofM3B,M2BandMBprecipitatephaseisobserved,whichwasreportedbyaboveauthorsunderirradiationwithenergyof40keVandioncurrentdensityof30μA/cm2.Inaddition,theprecipitationprocessinpresentexperimentissomewhatdifferentfromtheprecipitationprocessreportedbyaboveauthors,thepreferentialprecipitationphaseisFeSi,andfollowedbytheeutecticphaseα-Fe.CrystallizationofamorphousFe40Ni40B20wasnotobservedbyTyagi,whichwasthesamematerialasthatusedbyGusevaandGordeeva,undertheirradiationwith100keVionenergyand30μA/cm2ioncurrentdensity[3].Itmayrelatetothetemperaturerisingofsamplesorsomethingelse.Accordingtothecomparisonandanalysis,itmaybeconcludedthatthecrystallizationofmetallicglassesisverysensitivetothetemperaturerisinginsamplescausedbyionbeamirradiation.ThereasonofthepreferentialphasetobeFeSiandfollowedα-Femaybethatinanamorphousmaterial,themetalloidelementsshouldkeepatthetotalcontentsabove20at%,otherwisesomeelementsorcompoundswillprecipitatetoremainthebalanceofchemicalcomposition.Therefore,astheprecipitationofFeSianddeclineofSicontentsinasample,FeandNimayprecipitateasaneutecticphaseaccordingtoaboveidea.Inthisexperiment,Feprecipitatedfirstly.ThedifferenceoflatticeparametersbetweenexperimentaldataandASTMstandarddatamayresultsintheexistencesofNiandBetcandincompletecrystallizationinsample.Thegeneralviewpointforirradiation-assisted-crystallizationofmetallicglassbelowtheirthermalcrystallizationtemperatureisthedisplacementdamagesinducedbycollosion-cascadebetweenincidentionsandtargetatoms.Thedisplacementdamagesprovidethenucleatingcentresandtheirradiation-assistedmigrationincreasesthecrystallizeddrivingforce,butnodirectrelationshipbetweenheliumandcrystallization.Thegrowthofagrainiscloselyattributedtothediffusionofneighbouringatomstothegrowingnucleus,whichisreliedonthetemperatureextremely,accordingly,thecrystallizationofmetallicglassisverysensitivetothetemperaturerisingfromionbeambombardmentinanirradiatedsample.4.Summary(l)TheFe38Ni39Si10B13metallicglasswillcrystallizebelowitsordinarythermalcrystallizationtemperatureunderheliumionirradiationwith100keVenergyand6μA/cm2ionbeamcurrentdensity.(2)ThepreferentialprecipitationphaseofthemetallicglassisFeSi,andfollowedbyaneutecticphaseα-Fe.(3)Thecriticaldoseformingheliumbubblesinthemetallicglassisabout5×1016/cm2,whichisslightlylowerthanthedosereportedbyTyagi.(4)Theirradiation-assisted-crystallizaofametallicglassesisverysensitivetothetemperaturerisingcausedbyionbeambombardmentinanirradiatedsample.Acknowledgements─TheauthorswouldliketothankthecolleaguesofIonImplantationGroupinChinaInstituteof.AtomicEnergy.forhelpinginsampleirradiation,alsotoProfe
关键词:
: Fe38Ni39Si10B13
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方文兵
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钱海霞
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曾燮榕
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谢盛辉
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黎晓华
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张爽
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盛洪超
材料热处理学报
研究了40 kV Ti离子辐照对Zr55Cu30Al10Ni5非晶合金晶化行为和腐蚀性能的影响.通过X射线衍射和差示扫描量热分析,结果表明离子辐照导致样品发生晶化,其物相与退火晶化物相有明显差异.与8.1×1017 ions/cm2剂量相比,辐照剂量为2.7×107 ions/cm2时晶化量更多.电化学极化曲线和扫描电镜结果表明,辐照后样品在NaCl溶液中的腐蚀类型为点蚀,在NaOH溶液中为均匀腐蚀,辐照后样品在两种测试溶液中的耐腐蚀性能均比铸态样品好.
关键词:
Zr基非晶合金
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离子辐照
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晶化
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耐腐蚀性
