荆西刚
,
李文建
,
杨建设
,
郭传玲
,
褚巍
,
金晓东
,
王菊芳
,
周立斌
原子核物理评论
doi:10.3969/j.issn.1007-4627.2006.01.008
以体外培养的人类胃癌细胞系BGC823为材料,用兰州重离子加速器提供的能量为20 MeV/u的12C6+离子,分别在富氧(95% O2+5% CO2)和自然条件下辐照细胞,测得这种离子的氧增比近似为1,说明在中等能量区12C6+离子有很低的氧效应.
关键词:
氧效应
,
碳离子
,
人胃癌细胞系BGC823
,
兰州重离子加速器
工程热物理学报
根据《吴仲华奖励基金章程》（吴奖[2008]01号），经各高等院校、中国工程热物理学会和中国科学院工程热物理研究所认真评选和推荐，吴仲华奖励基金理事会评审并确定授予青年学者戴巍、罗坤、唐桂华“吴仲华优秀青年学者奖”，授予程雪涛等10位同学“吴仲华优秀学生奖”。
关键词:
基金
,
奖励
,
评选
,
获奖者
,
中国科学院
,
青年学者
,
物理研究所
,
高等院校
张跃
,
王燕斌
,
褚武扬
,
肖纪美
中国腐蚀与防护学报
ＴｉＡｌ金属间化合物在水溶液和甲醇溶液中的应力腐蚀张跃，王燕斌，褚武扬，肖纪美（北京科技大学）Ｔｉ３Ａｌ基金属间化合物已用于制作新一代宇航飞机的发动机和受力件［１］，而ＴｉＡｌ则是下一代发动机的候选材料［２］．由于构件在装配、储运过程中有可能和水及有机溶剂接触，因此需研究它们在水和有机溶剂中产生应力腐蚀的可能性．但到目前为止，还未见这方面的报导．本文则报导Ｔｉ３Ａｌ，Ｔｉ３Ａｌ＋Ｎｂ和ＴｉＡ?...
关键词:
乔利杰
,
徐荣杰
,
刘辉
,
褚武扬
,
肖纪美
中国腐蚀与防护学报
氢对黄铜应力腐蚀开裂敏感性的影响乔利杰，徐荣杰，刘辉，褚武扬，肖纪美（北京科技大学北京１１０８３）１引言对氢致开裂型的应力腐蚀，阴极反应进入金属的氢控制了应力腐蚀裂纹的形核和扩展过程；对阳极溶解型的应力腐蚀，虽然阳极溶解过程控制了应力腐蚀的形核和扩展，但当阴极过程是析氢反应时，进入试样的原子氢有可能起一定作用．在这种条件下，应力、腐蚀、氢这三个因素将同时起作用．到目前为止，关于氢对阳极溶解型?...
关键词:
null
,
SCC
,
Hydrogen
褚治德
,
杨俊红
,
孟宪玲
,
诸凯
,
李春英
,
江菊元
,
焦士龙
工程热物理学报
本文研究了初含水率、干燥周期、料层厚度相同时,不同供热方式(热风、热风与辐射、热风与辐射并加湿)的白菜种子在固定床的干燥动力学及其活性,与传统的只热风供热相比,当干球温度相同时辐射加热风干燥的种子终含水率比低13.8%、发芽率比高0.3%,而辐射加热风并加湿干燥其终含水率比低5.8%,发芽率比高0.8%.为确保种子活力,建立了褚-杨白菜种子临界温度Tcv 方程,并已验证其正确性.该方程为蔬菜种子干燥提供了理论基础并有重要的工程意义.
关键词:
红外辐射种子干燥
,
种子活性
,
种子强化传热传质
金属学报(英文版)
桑危郑牛樱裕桑牵粒裕桑希巍。希啤。龋伲模遥希牵牛巍。桑危模眨茫牛摹。模眨茫裕桑蹋拧。拢遥桑裕裕蹋拧。裕遥粒危樱桑裕桑希巍。桑巍。罚保罚怠。粒蹋眨停桑危眨汀。粒蹋蹋希?##2##3##4##5INVESTIGATIONOFHYDROGENINDUCEDDUCTILEBRITTLETRANSITIONIN7175ALUMINUMALLOY$R.G.Seng:B.JZhong,MG.ZengandP.Geng(DepartmentofMaterialsScierce,ScienceCollege,NorthearsternUniveisity,Shenyang110006,ChinaMaruscriptreceived4September1995inrevisedform20April1996)Abstrac:Effectsofhydrogenonthemechanicalpropertiesofdifferentlyaged7175aluminumalloyswereinvestigatedbyusingcathodicH-permeation,slowstrainratetensionandsoon.Theresultsindicatethatboththeyieldstressandthepercentagereductionofareadecreasewithincreasinghydrogenchargingtime,andthedegreeofreductiondecreasesasagingtimeincreasesforthesamehydrogenchargingtime.Keywords:hydrogeninducedductile-brittletransition,7175aluminumalloy,mechanicalproperty,cathodicH-permeation1.IntroductionForalongtimehydrogenembrittlementproblemwasthoughttobeabsentinhighstrengthaluminiumalloybecausethesolutiondegreeofhydrogeninaluminumatcommontemperatureandpressureisverysmall.However,hydrogenembrittlementphenomenonwasfoundinaluminumalloyduringtheinvestigationofstresscorrosionandcorrosionfatigue[1-5].Therehavebeenonlyafewreportsofhydrogeninducedsofteningandhardening.Inthispaper,theeffectsofhydrogenonmechanicalpropertiesof7175aluminumalloywereinvestigatedbyusingcathodicalchargingwithhydrogenandslowtensiontests.2.ExperimentalProcedureTheexperimentalmaterialwas7175aluminumalloyforgingintheformofa43mminthicknessandwithcomposition(wt%).5.41Zn,2.54Mg.1.49Cu,0.22Cr,0.1Mn.0.1Ti,0.16Fe.0.11Si,balancedbyA1.Alloyplateof1.5mminthicknesswasobtainedbyhot(465℃)andtoldrollingto83%reductioninthickness.Thelongaxisofhydrogenchargedspecimensisalongtherollingdirection.Allspecimensweresolidsolutionedat480℃for70min,followedtyimmediatequenchinginwaterandthenagedat140℃for6h(A),16h(B)and98h(C).Thetreatmentof6hiscorrespondingtotheunderagedstate.16hthefirstpeak-agedstateand98hthesecondpeak-agedstate.Thespecimenswerepolishedsuccessivelyusingemerypaperbeforehydrogencharging.Thetensilespecimenswerecathodicallychargedina2NH_2SO_4solutionwithasmallamountofAs_2O_3forpromotinghydrogenabsorption,andwithacurrentdensityof20±1mA/cm￣2atroomtemperature.ThehydrogencontentanalysiswascarriedoutonanLT-1Amodelionmassmicroprobeafterthesputteringdepthreached8nm.Theioncurrentsofhydrogenandaluminuminvariousagedstateswererecordedunderthesamecondition.ThetensiletestswereperformedonanAG-10TAmodeltestmachinewhichwascontrolledbycomputer.3.ExperimentalResultsTheratioofioncurrentstrengthofhydrogentoaluminumisrelatedtohydrogenconcentrationinhydrogenchargedspecimen.TheresultswereshowninTable1Thehydrogencontentincreaseswiththeincreaseincharingtime.Ofthethreeagedstates,theunderagedspecimenhasthehighesthydrogencontent.Theratioofyieldstrengthofhydrogenchargedandunchargedspecimenschangeswithhydrogenchargingtime,asshowninFig.1Itcanbeseenthattheyieldstrengthofhydrogenchargedspecimendecreasewithincreasinghydrogenchargingtime.Atthesamechargingtime,theyieldstressdecreasestheleastinthesecondpeak-agedstate,anddecreasesthemostintheunderagedstate.Itindicatesthattheunderagedspecimenismostsensitivetohydrogeninducedsoftening,whichisconsistentwiththeresultsofanotherhighstrengthaluminumalloy[6].TherelativechangesoftheradioofreductionofareawithhydrogenchargingtimearesummarizedinFig.2,whereΨ￣0andΨ￣Harethepercentagereductionofareaofthesamplewithoutandwithhydrogenchargingrespectively.Theradioofreductionofareareduceswhenhydrogenchargingtimeincreases,andthedecreasingdegreeofreductionofareaincreaseswithincreasingagingtime,ie,,theunderagedstateisthemostsensitivetohydrogenembrittlement.4.DiscussionItisknownfromtheresultsabovethatcathodicalchargingwithhydrogenleadstotheobviousdecreaseinthetensilestrengthandplasticityThisisbecausealargeamountofsolidsolutionhydrogenentersthespecimenintheprocessofhydrogenchargingSolidsolutionhydrogenisliabletoenterthecentreofdislocationundertheactionofdislocationtrap,henceraisingthemovabilityofdislocation.Thereforethedislocationsinhydrogenchargedspecimenmoveeasierthaninunchargedspecimen.soresultinginthereductionofyieldstrength[7].Whendislocationstartstomove,thecrystallatticeresistance(P-Nforce)whichitmustovercomeisgivenby:whereμismodulusofshear,visPoissonratio,aisspanofslipplane,bisatomspanofslipdirection.Moreover.theotherresistanceofdislocationmotionmayarisefromtheelasticinteractionofdislocation,theactionwithtreedislocationandetc.,itcanbeexpressedasfollows:whereαisconstant,XisdislocationspanSotheresistanceofdislocationmotioncanbewrittenasfollows:Becausehydrogenatomsreducetheatombondingstrengthafterhydrogencharging,shearmodulusμdecreasesandresultsinthereductionoff,therebytheyieldstressdecreases.Asthecentreofdislocationistheseriousdistortionzoneoflattice.thestresscanberelaxedafterhydrogenatomstuffing,andthesystemenergydecreases.Thusthecentreofdislocationisastrongtrapofhydrogen[8].Therefore,amovabledislocationcaptureshydrogenandmigratestograinboundaries.phaseboundariesorsurfaceofthespecimen,promotingthecrackiesformationandgrowth,thuscausingthelossofplasticity.Sincethelocalenrichmentofhydrogenisrealizedbydislocationtransporting(inthestageofdeformation),thelargerthereductionofyieldstress.theearlierarehydrogenatomstransportedtotheplaceofenrichment.Inaddition,thedamageofatombondingstrengthinducedbyhydrogenmakesthefracturestressdecrease[9]:whereCHishydrogenconcentration.σ_thisfracturestrengthbeforehydrogenchargingandisfracturestrengthafterhydrogencharging.Eq.(4)showsthatthematerialsmaybefracturedatalowerstraini.e.,brittlefractureoccurs.5.Conclusions(1)Hydrogencontentofdifferentlyagedspecimensincreaseswithincreasinghydrogenchargingtimethecapabilityofthealloytoabsorbhydrogeninunderagedstateisthestrongest.(2)Theyieldstressaswellasthepercentagereductionofareaof7175aluminumalloydecreaseashydrogenchargingtimeincreasesundervariousagedstates.(3)Underagedstateismostsensitivetohydrogeninducedsofteningandhardening.(4)Anexplanationwasofferedforthephenomenonofhydrogeninducedsofteninginthestageofdeformation,andhardeninginthestageoffracture.REFERENCES｜｜1G.KKock,Corrosion35(1979)73.2M.K.TsengandH.LMarcus,Scr.Metall.15(1981)427.3PSFao.M.GaoandR.P.Wei,Scr.Metall.19(1985)265.4R.G.SongandM.K.TsengJ.NortheasternUniversity15(1994)5(inChinese).5R.K.Viswanadham,T.S.sunandJ.A.S.Green,Metall.Trans.11A(1980)85.6J.Liu,M.KTsengandB.R.Liu.NonferrousMiningandMetallrgy5(1989)33(inChinese).7LChen,WXChen,ZHLiuandZ.Q.Hu,InFrocofthe1stNationalConfonAl-LiAlloys(Sheryang.China,1991)p.328(inChinese).8Z.HLiuL.ChenW.XChenY.X.ShaoandZ.Q.Hu,InProc.ofthe1stNationalConfonAl-LiAlloys(Shenyang,China,1991)p.334(inChinese).9R.A.OrianiandF.H.Josephic,ActaMetall.22(1974)1065.##61G.KKock,Corrosion35(1979)73.2M.K.TsengandH.LMarcus,Scr.Metall.15(1981)427.3PSFao.M.GaoandR.P.Wei,Scr.Metall.19(1985)265.4R.G.SongandM.K.TsengJ.NortheasternUniversity15(1994)5(inChinese).5R.K.Viswanadham,T.S.sunandJ.A.S.Green,Metall.Trans.11A(1980)85.6J.Liu,M.KTsengandB.R.Liu.NonferrousMiningandMetallrgy5(1989)33(inChinese).7LChen,WXChen,ZHLiuandZ.Q.Hu,InFrocofthe1stNationalConfonAl-LiAlloys(Sheryang.China,1991)p.328(inChinese).8Z.HLiuL.ChenW.XChenY.X.ShaoandZ.Q.Hu,InProc.ofthe1stNationalConfonAl-LiAlloys(Shenyang,China,1991)p.334(inChinese).9R.A.OrianiandF.H.Josephic,ActaMetall.22(1974)1065.##A##BINVESTIGATION OF HYDROGEN INDUCED DUCTILE BRITTLE TRANSITION IN 7175 ALUMINUM ALLOY$$$$R.G.Seng: B.J Zhong, MG. Zeng and P. Geng(Department of Materials Scierce, Science College,Northearstern Univeisity, Shenyang 110006, China Maruscript received 4 September 1995 in revised form 20 April 1996)Abstrac:Effects of hydrogen on the mechanical properties of differently aged 7175 aluminum alloys were investigated by using cathodic H-permeation, slow strain rate tension and so on. The results indicate that both the yield stress and the percentage reduction of area decrease with increasing hydrogen charging time, and the degree of reduction decreases as aging time increases for the same hydrogen charging time.
关键词:
:hydrogen induced ductile-brittle transition
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null
,
null
,
null
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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null
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null
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null
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null
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
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: Fe38Ni39Si10B13
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