贾巍
,
徐茂文
,
包淑娟
,
贾殿赠
无机材料学报
doi:10.3724/SP.J.1077.2010.10267
以介孔碳为模板, 成功合成了具有较大比表面积的多孔TiO2, 并研究了煅烧时间对所获材料结构及电化学性能的影响. 采用X射线粉末衍射、场发射扫描电镜、高分辨透射电镜、氮气吸附?脱附实验和电化学测试对合成的材料进行了表征. 测试结果表明所合成的材料是由很小的纳米颗粒组成, 表面积大, 孔分布窄. 经500℃热处理2h的样品为锐钛矿型, 继续延长热处理时间至12h, 所得样品出现了金红石相, 且12h所得材料的初始容量高于2h所得样品, 这可能和样品的结晶度有关.
关键词:
TiO2
,
mesoporous carbon
,
lithium ion batteries
贾巍
,
范承玉
连铸
doi:10.3969/j.issn.1007-5461.2015.02.016
压电陶瓷致动器具有体积小、推力大、高频响和分辨率高等特点,广泛应用于精密制造、光学仪器、振动控制等领域.为提高压电陶瓷型快速倾斜镜的控制精度和稳定性,根据压电陶瓷致动器对其驱动电源的要求,设计了一种基于高压运算放大器PA96的驱动电源.介绍了该电源电路的基本原理,并对放大器的外围电路进行了稳定性设计.最后通过实验测试表明,该电源线性度大于99％、静态纹波小于10 mV、动态性能稳定,能够达到自适应光学系统中快速倾斜镜的控制要求.
关键词:
自适应光学
,
快速倾斜镜
,
压电陶瓷
,
高压运算放大器
,
驱动电源
贾巍
,
徐茂文
,
包淑娟
,
贾殿赠
无机材料学报
doi:10.3724/SP.J.1077.2010.10267
以介孔碳为模板,成功合成了具有较大比表面积的多孔TiO2,并研究了煅烧时间对所获材料结构及电化学性能的影响.采用X射线粉末衍射、场发射扫描电镜、高分辨透射电镜、氮气吸附-脱附实验和电化学测试对合成的材料进行了表征.测试结果表明所合成的材料是由很小的纳米颗粒组成,表面积大,孔分布窄.经500℃热处理2h的样品为锐钛矿型,继续延长热处理时间至12h,所得样品出现了金红石相,且12h所得材料的初始容量高于2h所得样品,这可能和样品的结晶度有关.
关键词:
TiO2
,
介孔碳
,
锂离子电池
张小琴
,
王宇池
,
王永青
,
韩力挥
合成材料老化与应用
目前,低渗透油藏在各大油田分布广泛,其石油储量占未开发石油总量的比重较大.贾敏效应是导致低渗透油藏难以开采、采收率低的一个重要影响因素.采用贾敏指数来评价贾敏损害程度,制取了三种非离子表面活性剂JN-1、JN-2和JN-3,通过筛选得知JN-3降低油水界面张力的能力最强.根据贾敏效应产生的机理以及水井转抽机理,开展了减缓贾敏效应的室内试验研究,结果表明,针对性地向注入水中加入非离子表面活性剂JN-3,可以降低油水界面张力,同时适时地采用水井转抽逆向驱油来增大驱动压差,有效地抑制和减缓了贾敏效应,提高原油采收率.
关键词:
低渗透油藏
,
贾敏效应
,
非离子表面活性剂
,
水井转抽
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
姜小敏
,
凌志光
,
邓兴勇
工程热物理学报
本文在含尘流透平叶片流道内气固两相流动数值模拟的基础上，发展了叶片冲蚀的数值分析方法，提出了便于工程应用的有限区域内质量加权、面积平均的冲蚀率统计分布计算方法，对建造中的江苏徐州贾旺增压流化床联合循环中试电站燃气轮机叶片冲蚀问题进行了数值模拟，给出了计算结果的数据图象资料，就叶片冲蚀状况进行了分析。
关键词:
透平机械
,
叶片冲蚀
,
数值分析
董彦，龚志翔，肖国华
钢铁研究学报
以指导无取向电工钢热轧工艺为目的，采用Gleeble 1500热模拟试验机进行高温等温压缩，在应变速率为0.01~10s-1和变形温度500~1200℃条件下，对试样进行试验研究。结果表明：随着变形温度的升高，在回复与再结晶过程中发生α-Fe向γ-Fe相的?洌贾挛忍鞅溆αΤ氏帧耙斐！北浠２捎肁rrhenius关系模型，模型参数能很好的与试验结果相吻合。利用模型分别计算得500~800℃时，应力水平因子α=0.0390MPa-1，应力指数n=7.93，结构因子A=1.9×1018 s-1，热变形激活能Q=334.8kJ/mol；1050~1200℃时，应力水平因子α=0.1258MPa-1，应力指数n=5.29，结构因子A=1.0×1028 s-1，热变形激活能Q=769.9kJ/mol。
关键词:
无取向
,
electrical steel
,
high temperature
,
plastic deformation
,
flow stress
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
,
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.
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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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