退火对MgO/NiFe/MgO多层膜平面霍尔效应的影响

采用磁控溅射的方法制备了结构为Ta(5 nm)/Mg O(6 nm)/Ni Fe(t_(NiFe))/Mg O(4 nm)/Ta(3 nm)的磁性多层膜,Ni Fe的厚度t_(NiFe)从5 nm增加到100 nm,之后在真空退火炉中经过400℃,1 h的退火处理并且进行随炉冷却,整个过程中沿着薄膜易轴方向施加大约4378 A·m-1的磁场。采用四探针的方法来测量平面霍尔电压(PHE)和相对电阻变化率,通过X射线衍射(XRD)和高分辨透射电子显微镜(HRTEM)来分析多层膜退火前后的微结构变化。研究结果表明:对于制备态和退火态的Ta/Mg O/Ni Fe/Mg O/Ta纳米磁性多层膜结构,当t_(NiFe)40 nm时,霍尔输出电压骤减,随着t_(NiFe)的继续增加,霍尔电压基本保持不变。然而,所有的制备态同一厚度的样品经过退火处理之后,霍尔电压都有一定程度的提高,当t_(NiFe)=5 nm时,平面霍尔输出电压增加最大。随着Ni Fe厚度的继续增加,退火处理所导致的输出电压的提高幅度逐渐减小,当t_(NiFe)=100 nm时,霍尔电压退火之后几乎保持不变。不同Ni Fe厚度的样品,霍尔电压经退火处理后之所以提高幅度不同,主要与两个因素有关,一是Mg O/Ni Fe异质界面会增强电子自旋相关散射提高PHE输出电压,二是Ni Fe层因分流也会导致PHE输出电压下降。     

TC4钛合金微弧氧化膜层高温氧化性能研究

利用微弧氧化(MAO)技术在TC4钛合金表面原位制备陶瓷膜层,并通过硅酸钠水溶液对膜层进行了封孔处理。采用X射线衍射仪(XRD)分析了膜层相组成,通过扫描电子显微镜(SEM)观察了膜层表面形貌。通过粘结拉伸测试,比较了膜层在封孔前后与基体的结合强度。利用高温氧化实验,考察了TC4基体及膜层试样封孔前后的抗高温氧化性能。结果表明:微弧氧化膜层与基体间的结合强度较高,经封孔处理及高温氧化100 h后,膜基结合强度降低至4.29 MPa。与TC4基体相比,微弧氧化膜层的高温氧化增重量小,抗高温氧化性能得到了显著的提高。封孔处理提高了微弧氧化膜层的致密性,使其能更好地阻止氧透过膜层向基体内侵入,进一步提高了膜层的抗高温氧化性能。     

热等静压温度对V-4Cr-4Ti/HR2钢连接界面及性能的影响

以AuNi合金作为过渡层材料,采用热等静压(HIP)方法进行V-4Cr-4Ti/HR2钢(SS)扩散连接.利用扫描电镜(SEM)、能谱仪(EDS)及剪切试验分析了接头的扩散层显微组织、微区成分和力学性能.研究表明:采用AuNi过渡层材料,能够实现V-4Cr-4Ti/HR2的扩散连接;HIP温度为850℃时,接头质量良好,其剪切强度为39MPa;V、Fe、Ni等主要元素的平均扩散深度为20μm左右;在SS侧,扩散层较为均匀,在V-4Cr-4Ti侧,形成了Au的富集层和NixVy的富集层,两层呈相互交替的层状分布.     

取向电磁钢板高温退火初期采用Ar气作为保护气氛对镁橄榄石被膜质量的影响#br#

高温退火低保温期，采用惰性气体作保护气体能改善被膜质量。惰性气体Ar与H2、N2相比黏度高， Ar气难于侵入钢卷的各层间挤压出水分子，水分子就在钢板层间保持下来，将会进一步促进被膜的生成。之后导入氢气，促进了退火隔离剂MgO的表面活化性，由于钢板层间是湿氢保护气氛，钢板表面的副氧化层中、难于被还原的Fe2SiO4，将与MgO发生反应，生成Fe2 xMgxSiO4，又继续形成完善的Mg2SiO4镁橄榄石被膜，在这种条件下所生成的被膜将吸收隔离涂层中的Ti，增强了被膜的强度。     

Ni/Bi0.4Sb1.6Te3热电材料的界面性能

Bi_0.4Sb_1.6Te₃热电材料和金属电极之间的阻挡层是热电器件稳定服役的控制性因素,本文以不同温度下退火后的高致密Ni箔和Bi_0.4Sb_1.6Te₃合金为原料,采用放电等离子烧结扩散焊连接法在Bi_0.4Sb_1.6Te₃表面制备Ni层作为Ni/Bi_0.4Sb_1.6Te₃电极接头的阻挡层。采用X射线衍射仪对阻挡层进行物相分析,用扫描电镜及能谱仪观察和分析电极接头的界面形貌与元素分布。结果表明,在700℃退火后的Ni箔具有优良的防扩散效果,扩散厚度为9μm,用700℃退火后的Ni箔与Bi_0.4Sb_1.6Te₃扩散焊结合,获得13.19 MPa的结合强度。随Ni箔的退火温度升高,Ni/Bi_0.4Sb_1.6Te_3<...     

喷射成形及轧制钢/Al-Pb合金复合板材的界面结合强度

对喷射成形钢/Al-Pb复合板的界面结合进行了研究,结果表明喷射成形的钢/Al-Pb复合板经变形量达50%左右的轧制和320℃×5h退火处理后可获得良好的界面结合,其剪切强度可达72MPa。分析显示双金属界面结合强度的提高是扩散层形成的结果。     

溅射AlY涂层对Ni基合金抗热腐蚀性能的影响

采用磁控溅射方法在镍基合金表面制备AlY涂层,并对涂层试样分别进行预氧化和真空扩散退火处理,对比研究镍基合金、预氧化AlY涂层试样和真空扩散退火AlY涂层试样在900℃硫酸盐膜下的热腐蚀动力学及腐蚀产物的组成。结果表明,各试样的腐蚀动力学均分段遵循抛物线规律。对于24 h的腐蚀增重,涂层试样明显小于镍基合金,预氧化试样略低于真空扩散退火试样。镍基合金腐蚀膜分层且开裂,外层主要是Cr_2O_3及NiO的混合物,其下有不连续的Al_2O_3;真空扩散退火试样的腐蚀膜外层是连续的Al_2O_3,其下是Cr和Ni的氧化物,再下是连续的Y_2O_3;预氧化试样形成了与真空扩散退火试样相似的腐蚀膜,但略薄于真空扩散退火Al Y涂层试样。表面连续Al_2O_3膜及连续的Y_2O_3层的形成,提高了腐蚀膜的保护性和粘附性,不同方法处理的AlY涂层提高了镍基合金的抗热腐蚀性能。     

真空退火对TC4钛合金表面Ti/TiN多层复合涂层性能的影响

金属基体材料表面硬质膜层在服役过程中,残余应力在膜基界面以及膜层内部界面之间的积聚会导致膜层发生界面剥落失效。以TC4钛合金基体表面Ti/TiN多层复合膜层为研究对象,探讨真空退火对复合膜层结构及性能的影响,并表征退火前后复合膜层的界面划痕失效以及抗粒子冲蚀性能。结果表明,真空退火促进了膜层内部以及膜基界面两侧原子的热扩散,使得界面结构特征明显弱化。界面状态的改变使得复合膜层的表面显微硬度降低以及膜基结合强度提高。在划痕载荷作用下,复合膜层抵抗裂纹沿界面扩展的能力得到增强。真空退火有助于提高膜层的强韧性匹配,可有效抵抗小角度冲蚀粒子的犁削以及大角度粒子冲蚀下的疲劳,因此Ti/TiN多层复合膜层表现出较好的抗冲蚀性能。     

取向电磁钢板高温退火初期采用Ar气作为保护气氛对镁橄榄石被膜质量的影响

高温退火低保温期,采用惰性气体作保护气体能改善被膜质量。惰性气体Ar与H2、N2相比黏度高,Ar气难于侵入钢卷的各层间挤压出水分子,水分子就在钢板层间保持下来,将会进一步促进被膜的生成。之后导入氢气,促进了退火隔离剂MgO的表面活化性,由于钢板层间是湿氢保护气氛,钢板表面的副氧化层中、难于被还原的Fe2SiO4,将与MgO发生反应,生成Fe2-xMgxSiO4,又继续形成完善的Mg2SiO4镁橄榄石被膜,在这种条件下所生成的被膜将吸收隔离涂层中的Ti,增强了被膜的强度。     

不同界面Ag基纳米多层膜热稳定性的研究

本文研究了Ag/Cu纳米多层膜和Ag/Nb纳米多层膜室温下及退火状态下的界面结构。通过X射线衍射分析以及透射电镜对形貌进行了表征。结果表明,调制周期为20nm时,Ag/Cu多层膜界面为半共格结构,Ag/Nb多层膜界面为共格结构。经200℃～500℃退火处理后,Ag/Cu多层膜在400℃时层状结构破坏,而Ag/Nb多层膜在500℃下仍保持很好的结构稳定性。研究结果说明,共格界面比半共格界面具有更高的热稳定性。     

热镀锌TRIP钢还原铁/基板界面表征

预氧化还原工艺是改善热镀锌先进高强钢(AHSS)可镀性的有效手段之一。当它用于生产热镀锌先进高强钢时,有时也会出现镀层附着性不良的问题。为了明确还原铁/基板界面对热镀锌高强钢镀层附着性的影响,以预氧化还原工艺生产的、镀层附着性不同的热镀锌TRIP钢为研究对象,采用GDOES、SEM、FIB、TEM等手段研究了还原铁/基板界面位置的微观特征。结果表明,镀层附着性不良表现为150～300 nm厚的还原铁层与镀层一起从基板表面脱落,失效发生在还原铁/基板界面,而非镀层/还原铁界面,与常见的镀层/基板界面Fe₂Al₅抑制层缺失引起的镀层附着性不良明显不同。镀层附着性不同的试样在还原铁/基板界面位置均存在硅、锰元素富集,但硅、锰富集程度有差异,镀层附着性不良试样的界面硅、锰富集更高。还原铁/基板界面氧化物形态显著影响了还原铁/基板界面的结合力,当还原铁与基板之间形成连续的氧化膜时,界面结合力较差,易发生界面分离;当还原铁/基板界面形成细小的、不连续的氧化物颗粒时,界面结合力较好。在对热镀锌先进高强钢实施预氧化还原工艺时,为了获得良好的还原铁/基板界面结...     

Infrared brazing of Ti-6Al-4V and 17-4 PH stainless steel with a nickel barrier layer

Infrared brazing of Ti-6Al-4V and 17-4 PH stainless steel using the BAg-8 filler metal was performed in this study. A nickel barrier layer 10 μm thick was introduced on the 17-4 PH stainless steel before infrared brazing. For the specimen that was infrared brazed at 800 °C and 850 °C for less than 300 seconds, the Ni layer served as an effective barrier layer to prevent the formation of Ti-Fe intermetallics. Experimental results show that the average shear strength of the joint can be greatly improved for the specimen by Ni plating. Comparing the specimens with and without electroless-plated Ni film, the former has no Ti-Fe intermetallic compound, but interfacial CuNiTi and NiPTi phases are observed in the latter. The fractured location of the joint after the shear test is changed from the interfacial TiFe (without Ni plating) into the TiCu reaction layer (with Ni plating). The plated Ni layer is consumed for the specimen that was infrared brazed at 880 °C for 300 seconds, and its bonding strength is impaired. Consequently, a lower brazing temperature and/or time are still preferred even though a plated Ni barrier layer is applied.     

Strength Improvement Through Grain Refinement of Intermetallic Compound at Al/Fe Dissimilar Joint Interface by the Addition of Alloying Elements

Dissimilar material joining between Al alloys and steel may be effective in decreasing the weight of automobile bodies. In this study, dissimilar lap joining of Al alloys containing certain alloying elements, such as Ni, Cr, Mn, Ti, or Si, to interstitial-free steel was performed by tungsten inert gas arc brazing, and the effect of the alloying element on the joint strength associated with the Al-Fe intermetallic compound layer at the dissimilar interface was examined. The addition of an appropriate amount of an alloying element to the alloy increased the joint strength; the addition of Ni exhibited the most effective improvement. The additions of some elements changed the grain structure of the η-Fe₂Al₅ layer but not its chemical composition. This is the first study to clarify that smaller grain size of η-Fe₂Al₅ correlated to greater strength of the Al/Fe dissimilar joint.     

陶瓷耐磨缸套真空钎焊接头组织性能研究

本文采用钴基焊料实现了氧化锆陶瓷与不锈钢的真空钎焊,并通过扫描电镜（SEM）和XRD对接头的微观组织结构进行了研究。结果表明：接头微观组织致密,镀镍层在真空钎焊过程中发生了扩散和迁移,增强了界面化学反应的活性,镍与ZrO2陶瓷易生成多种化合物（Ni3Zr、Ni5Zr、Ni7Zr2和Ni21Zr8）,在接头中还有Ni4Mo、Ni4Mn等新相生成,实现了部分化学键结合,使接头强度得到显著提高。     

Effect of Aging Temperature on the Microstructure and Shear Strength of SAC0307-0.1Ni Lead-Free Solders in Copper Joints

This paper presents an investigation of the effects of aging temperature on the microstructure and shear strength of SAC0307-0.1Ni/Cu solder joints. Single-overlap shear solder joints were aged for 1 h at 80, 130, and 180°C. The microstructure of the interface between the solder and the Cu substrate contained phase of the intermetallic compounds (IMCs) (Cu,Ni)6Sn5 formed along the interface. The shape of scallop-like (Cu,Ni)6Sn5 IMCs changed to the long dendrite and grew larger at the interface of solder joints after increased aging temperature. In addition, a phase of particle-like Ag3Sn IMCs was formed in the solder matrix. The growth of the interfacial IMC layer in the solder joints increased with increasing the aging temperature. The thickness of this layer was controlled by diffusion mechanism. The shear strength of the as-reflowed solder joints was greater than that of the aged solder joints, and the shear strength of all the aged solder joints decreased with increasing the aging temperatures. Therefore, the aging temperature mainly affected the thickness of the interfacial layer of IMCs and the shear strength of the solder joints.     

内氧化对热镀锌高强钢镀层/基板界面的影响

 由于高强钢中添加的Si、Mn等合金元素会在退火时会发生选择性氧化,从而影响镀液与带钢之间的润湿性,因此热镀锌高强钢生产存在可镀性的难题。为了提高热镀锌高强钢的镀层附着性,以不同镀层附着性的连续热镀锌0.2%C-1.8%Si-1.8%Mn高强钢为研究对象,采用GD-OES、SEM、FIB、TEM等研究了镀层/基板界面抑制层与基板次表层内氧化层的特征,同时采用模拟退火试验研究了退火气氛露点对内氧化层形成的影响,揭示了退火气氛露点、内氧化层厚度、抑制层覆盖率与镀层附着性之间的相关性。结果表明,该热镀锌高强钢镀层附着性优劣由镀层/基板界面位置抑制层决定,当抑制层覆盖率达到80%以上时,可获得良好的镀层附着性。内氧化层厚度对抑制层覆盖率的影响存在临界厚度,约为0.58 μm。当内氧化层厚度由0逐渐增加至0.58 μm时,抑制层覆盖率由约10%增加至约80%;当内氧化层厚度由0.58进一步增加至3.85 μm时,抑制层覆盖率略有增加,介于80%~90%之间。提高退火气氛露点可以促进基板次表层形成内氧化,在退火温度分别为800和870 ℃、保温时间为120 s、退火气氛为N₂-5% H₂(体积分数)的试验条件下,当退火气氛露点由-40 ℃提高到+10 ℃时,内氧化层厚度由基本为0提高至3~5 μm。为了获得合适的内氧化层厚度,建议将0.2%C-1.8%Si-1.8%Mn高强钢的退火气氛露点控制在-20~-10 ℃范围内。     

623K温度下SnxZn1-x/Ni扩散偶的界面反应

为研究Sn-Zn合金(无铅焊料的候选者)和Ni基体(Cu基上的扩散阻挡层)的界面反应,制备一系列原子分数x分别为14.8％、22％和31％的液固扩散偶Sn1-xZnx/Ni;在623 K温度下恒温退火后,用扫描电镜和电子探针检测与分析扩散偶的界面结构,研究退火时间和合金中的Zn含量对扩散层结构和形貌的影响.结果表明,S...     

Investigation of SiGe-on-Insulator Novel Structure

SiGe-on-Insulator (SGOI) is an ideal substrate material for realizing strained-silicon structures that are very competing and popular in present silicon technology. In this paper, two methods are proposed to fabricate SGOI novel structure. One is modified Separation by Implantation of Oxygen (SIMOX) starting from pseuodomorphic SiGe thin film without graded SiGe buffer layer. Results show that two-step annealing can improve the cystallinity quality of SiGe and block the Ge diffusion in high temperature annealing. SGOI structure with good quality has been obtained through two-step annealing. The second method is proposed to achieve SGOI with high content of Ge. High quality strained relax SiGe is grown on a compliant silicon-on-insulator (SOI) substrate by UHCVD firstly. During high temperature oxidation,Ge atoms diffuse into the top Si layer of SOI. We successfully obtain SGOI with the Ge content of 38%, which is available for the growth of strained Si.     

低温取向硅钢硅酸镁底层形成过程

 取向硅钢硅酸镁底层是产品结构的重要组成部分,低温取向硅钢底层的控制是难点,也是限制产品性能提升的瓶颈。以往对取向硅钢硅酸镁底层的形成研究较少,高磁感取向硅钢薄规格化高性能产品开发及品质提升缺乏理论支撑。为此,采用高温退火中断试验法对低温取向硅钢硅酸镁底层的形成过程进行了模拟,研究了底层的微观结构、成分特征的演变规律,明确了硅酸镁底层在高温退火过程中的反应形成过程。温度约为900 ℃时,样品表面开始发生Mg₂SiO₄颗粒的形核,随着温度继续升高,Mg₂SiO₄晶核不断长大;温度约为1 050 ℃时,样品表面的Mg₂SiO₄开始致密化,温度约为1 100 ℃时,表层硅酸镁的致密化基本完成,硅酸镁底层形成的关键温度为900～1 100 ℃。另外,研究中发现,在硅酸镁底层的下方生成的Al₂O₃·MgO尖晶石颗粒连结基体和Mg₂SiO₄,形成了“钉扎”结合层。硅酸镁底层形成过程MgO中的Mg2+由表面向氧化膜内扩散并与SiO₂反应,同时氧化膜内SiO₂发生熟化,1 000 ℃以上基板中的AlN分解释放出的铝则向氧化膜交界及通过氧化膜向表面扩散与Mg₂SiO₄等反应形成尖晶石。优良的底层结构形成是由原脱碳退火氧化膜表层1 μm左右形成致密的Mg₂SiO₄,其余2～3 μm厚度转化成一定数量的椭球Al₂O₃·MgO的尖晶石“钉扎”结合层,其主要控制方向为提高氧化膜活性、选用高活性MgO、添加低熔点反应助剂等。     

Brazing of Ti-6Al-4V and niobium using three silver-base braze alloys

Evaluations of the (infrared)-brazed Ti-6Al-4V and niobium joints using three silver-base braze alloys have been extensively studied. According to the dynamic wetting angle measurement results, the niobium substrate cannot be effectively wetted by all three braze alloys. Because the dissolution of Ti-6Al-4V substrate causes transport of Ti into the molten braze, the molten braze dissolved with Ti can effectively wet the niobium substrate during brazing. For infrared-brazed Ti-6Al-4V/Ag/Nb joint, it is mainly comprised of the Ag-rich matrix. The TiAg reaction layer is observed at the interface between the braze and Ti-6Al-4V substrate. In contrast, Ti-rich, Ag-rich, and interfacial TiAg phases are found in the furnace-brazed specimen. The dominated Ti-rich phase in the joint is caused by enhanced dissolution between the molten braze and Ti-6Al-4V substrate. The infrared-brazed Ti-6Al-4V/72Ag-28Cu/Nb joint is mainly comprised of the Ag-rich matrix and Ag-Cu eutectic. With increasing the brazing temperature or time, the amount of Ag-Cu eutectic is decreased, and the interfacial Cu-Ti reaction layer(s) is increased. The infrared brazed joint has the highest average shear strength of 224.1 MPa. The averaged shear strength of the brazed joint is decreased with increasing brazing temperature or time, and its fracture location changes from the braze alloy into the interfacial reaction layer(s) due to excessive growth of the Cu-Ti intermetallics. The infrared-brazed Ti-6Al-4V/95Ag-5Al/Nb joint is composed of Ag-rich matrix and TiAl interfacial reaction layer. With increasing the brazing time, the amount of Ag-rich phase is greatly decreased, and the interfacial reaction layer becomes Ti₃Al due to enhanced dissolution of Ti-6Al-4V substrate into the molten braze. The average shear strength of the infrared-brazed joint is 172.8 MPa. Additionally, the existence of an interfacial Ti₃Al reaction layer significantly deteriorates the shear strength of the furnace-brazed specimen.