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STRUCTURE AND PHYSICAL PROPERTIES OF SUBMICROCRYSTALLINE METALS PREPARED BY SEVERE PLASTIC DEFORMATION

R. R. Mulyukov and M. D. Starostenkov( 1) Institute for Metals Superplasticity Problems of Russian Academy of Sciences , Khalturina 39 , Ufa 450001 , Russia 2)Altai State Technical University)

金属学报(英文版)

The results of investigations of structure and physical properties of submicrocrystalline (SMC) metals are presented. The SMC structure was formed by severe plastic deformation.The structure was investi- gated by calorimetric and mossbauer measurements and TEW stuidies. The behavior of physical proper- ties of SMC metals were analysed taking into account spectific features of their structure.

关键词: submicrocrystal , null , null , null

The Effect of B Doping on the Martensitic Transitions, Magnetocaloric and Magnetic Properties in Ni48Mn39In13-xBx Ribbons

Ieee Transactions on Magnetics

The influence of boron substitution for indium on phase transformation, magnetocaloric and exchange bias (EB) properties in annealed Ni48Mn39In13-xBx (x = 1-4) ribbons has been investigated. It is observed that an increase in B concentration strongly affects the magnetic state of the martensitic phase, the magnetic entropy change and the EB properties of the ribbons. These ribbons crystallize in a partially ordered B2 phase structure. The martensitic structural transition temperature (T-M) decreases from 270 K for x = 0 to 175 K for x = 2 with increasing B content. A further increase in B content results in an increase of T-M to 268 K for x = 4. The peak value of positive magnetic entropy change (Delta S-M) decreases from 20.2 J/kg K for x = 0 to 2.8 J/kg K for x = 4 for a magnetic field change H = 50 kOe. The values of exchange bias field (H-E) and the coercivity (H-C) change from 258 Oe and 192 Oe to 397 Oe and 600 Oe, respectively, as x is increased from 0 to 4. The phenomena are attributed to the change of exchange interactions in B-substituted Ni-Mn-In ribbons due to the change of distance between Mn atoms.

关键词: Exchange bias;martensitic transformation;magnetocaloric properties;melt-spun ribbon;transformation;alloys

GH39合金拉伸应变硬化行为与断口形貌

王辉 , 陈明和 , 张成祥 , 赵海艳 , 王鹏飞 , 雷晓晶

航空材料学报 doi:10.11868/j.issn.1005-5053.2016.5.013

采用不同应变速率(0.0001~0.1s-1)下单轴拉伸实验对 GH39合金应变硬化行为与断口特征进行了研究。结果表明:应变硬化指数在不同应变量下表现出多重性,真应力应变不完全遵循 Hollomon 对数线性关系。塑性变形开始阶段,应变硬化指数n为恒定;真应变ε在0.014~0.13,n随着应变的增加而增加,在此过程由于形成大量形变孪晶,孪晶与位错相互作用,硬化能力增强;随着应变速率的提高,材料的应变硬化指数略下降;在低应变速率时段合金的拉伸断口为延性断裂,随着应变速率的增加从韧窝状延性断裂向半解理断裂过渡。

关键词: GH39合金 , 形变孪晶 , 应变硬化 , 应变速率 , 断口形貌

氧化处理Ti-39Nb-13Ta-4.6Zr合金表面生物活性研究

李述军 , 郝玉琳 , 杨锐 , 崔玉友 , M.Niinomi

金属学报 doi:10.3321/j.issn:0412-1961.2002.z1.180

对氧化处理后的Ti-39Nb-13Ta-4.6Zr合金进行碱处理,其表面具有了生物活性.将处理后的合金在仿生溶液中浸泡后,有类似骨组织的磷酸钙生成.

关键词: Ti-39Nb-13Ta-4.6Zr合金 , 氧化处理 , 碱处理 , 仿生溶液 , 磷酸钙

内蒙金厂沟梁金矿床39号脉含矿性地球化学预测

朴寿成 , 孙景贵 , 江裕标 , 贾洪杰 , 翟玉峰 , 张宝庆

黄金 doi:10.3969/j.issn.1001-1277.2005.12.004

金厂沟梁金矿床39号脉为总体走向近南北、向西凸出的弧形矿脉,Au在弧形矿脉的两翼更为富集.As、Sb、Hg、F为前缘元素, Mo、Co为尾晕元素.前缘、尾晕元素以及由这些指示元素构成的因子得分和累加指数等是矿脉含矿性预测的有效的地球化学标志.根据地球化学预测标志,预测39号脉在南翼十五中段以下和北翼十三中段以下还有矿体存在.矿脉在深部铜矿化增强,推测金厂沟梁向深部可能转变为金铜矿床.

关键词: 金厂沟梁金矿床 , 39号脉 , 含矿性 , 地球化学预测

K7BeBW11O39配合物的气相渗镨及其导电性能研究

李中华 , 韦永德 , 郭元茹 , 周百斌

稀土 doi:10.3969/j.issn.1004-0277.2004.03.018

首次报道了通过固-气界面反应对K7BeBw11O39@25H2O配合物进行稀土Pr的扩渗.对配合物的TG-DTA分析确定了扩渗温度,扩渗后的试样经ICP测试表明:微量Pr可渗入到杂多配合物K7BeBW11O39@25H2O体相,采用直流四电极法和交流阻抗法对扩渗前后试样进行了导电性能的测定,扩渗后试样的室温电导率达到了1.49×10-1S@cm-1,交流阻抗谱显示材料为电子导体.

关键词: 杂多配合物 , 稀土多元渗 , 导电性

CRYSTALLIZATION OF Fe_(38)Ni_(39)Si_(10)B_(13) METALLIC GLASS UNDER HELIUM ION IRRADIATION

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 , null , null , null , null

钆对K7CrMnW11O39配合物的热扩渗及其导电性研究

王珩 , 周百斌

稀有金属 doi:10.3969/j.issn.0258-7076.2006.06.011

采用直接法合成了K7CrMnW11O39,利用固-气界面反应,研究了Gd对所合成样品的热扩渗.利用IR,XRD,TG-DTA对扩渗前后样品的结构进行了表征.结果表明,经稀土扩渗后,其Keggin结构已被破坏,生成了新相.测试了扩渗前后样品的电导率,扩渗后样品的电导率为扩渗前样品电导率的1×104倍.

关键词: , 杂多配合物 , 热扩渗 , 电导率

液相色谱-串联质谱法快速测定婴幼儿配方奶粉中39种激素残留量

祝伟霞 , 刘亚风 , 袁萍 , 杨冀州

色谱 doi:10.3724/SP.J.1123.2010.01031

建立了液相色谱-串联四极杆质谱同时测定婴幼儿配方奶粉中17种糖皮质激素、11种孕激素、3种雄性激素和8种雌激素残留的快速确证方法.采用乙腈提取奶粉中待测组分,提取液经冷冻离心与正己烷除脂、亲水-亲脂平衡固相萃取柱净化、甲醇洗脱.分别在正、负电喷雾离子化多反应监测模式下检测39种激素.正离子模式下的流动相为乙腈-0.1%甲酸,色谱柱为普通硅胶基质的C18柱;负离子模式下的流动相为乙腈-0.1%氨水,色谱柱为能耐受宽pH范围的超高效C18柱.在该优化条件下,39种激素定量限(S/N≥10)为0.02~5 μg/kg,方法回收率为59.5%~117.9%,相对标准偏差(RSD)为6.4%~16.3%.经测定多种市售婴幼儿配方奶粉,表明该方法操作简单、测定结果准确,可用于婴幼儿配方奶粉中多种内源性与化学合成类激素残留的快速测定.

关键词: 液相色谱-串联质谱 , 固相萃取 , 冷冻除脂 , 激素 , 婴幼儿奶粉

稀土杂多配合物K15[Ce (BW11O39)2]·17H2O与BSA的相互作用

曾芳 , 杨昌英 , 潘家荣 , 赵儒铭 , 周百斌

稀土 doi:10.3969/j.issn.1004-0277.2006.04.002

利用紫外光谱,以曙红Y(Eosin Y)为探针,考察了稀土杂多配合物K15[Ce(BW11O39)2]·17H2O与牛血清白蛋白(BSA)间的作用,K15[Ce(BW11O39)2]·17H2O与Eosin Y在BSA上有竞争结合,表面活性剂对两者间的竞争结合有增敏作用;并利用荧光光谱直接考察了K15[Ce(BW11O39)2]·17H2O与BSA的相互作用及其对BSA构象的影响.

关键词: 稀土杂多配合物 , 牛血清白蛋白 , 曙红Y(Eosin Y) , 紫外光谱法 , 荧光光谱法

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