合金的玻璃形成能力对激光重熔Zr基非晶热影响区晶化的影响

通过脉冲激光重熔Zr55All 0Ni5Cu30非晶合金和Zr65Al7.5Ni10Cu17.5非晶合金,分析了具有不同玻璃形成能力的非晶合金热影响区晶化行为的差异。结果表明,玻璃形成能力稍差的Zr65Al7.5Ni10Cu17.5非晶合金比玻璃形成能力强的Zr55All 0Ni5Cu30非晶合金热影响区晶化严重。激光重熔Zr55Al10Ni5Cu30非晶合金4次后,热影响区仅有稀疏的球状晶粒析出;而激光重熔Zr65Al7.5Ni10Cu17.5非晶合金1次时,热影响区布满球状晶粒,激光重熔4次后,晶化晶粒长大明显,且在球状晶粒的内部呈现树枝状放射生长形态。激光重熔热影响区非晶合金的晶化行为与该合金的玻璃形成能力密切相关。玻璃形成能力越高,越有利于保持热影响区的非晶状态。     

Mg-Y-Nd合金{1011}孪晶界面稀土原子偏聚的电子显微研究北大核心CSCD

本文综合利用电子显微镜表征手段对冷轧后时效处理Mg-4Y-3Nd(wt.%)合金中[1102](1101)共格孪晶界面的稀土溶质原子偏聚行为进行研究,发现在经423 K+5 h时效后,合金中Nd元素在孪晶界面存在明显的偏聚析出,而Y元素的偏聚则并不明显。这表明镁合金中固溶的Nd原子相较Y原子具有更高的扩散速率和向{1011}孪晶界偏聚析出的驱动力。另外,本实验还揭示了相较于共格孪晶界面,孪晶界面上存在的孪晶台阶具有较大的晶格错配,稀土溶质原子优先选择在孪晶台阶处偏聚。     

MCM-D多层金属布线互连退化模式和机理

介绍了MCM-D多层金属互连结构的工艺及材料特点，并就Cu薄膜布线导体的结构特点和元素扩散特性。说明了多层布线互连退化的模式和机理，以及防止互连退化的技术措施，实验分析表明，Au/Ni/Cu薄膜布线结构的互连退化原因是，Cu元素沿导带缺陷向表层扩散后，被氧化腐蚀，导致互连电阻增大，而Cu元素在温度应力作用下向PI扩散，导致PI绝缘电阻下降。     

扫描速率对激光熔覆Cu80Fe20偏晶涂层组织与耐磨性能的影响

采用激光熔覆技术制备了Cu80Fe20偏晶涂层,研究了扫描速率对液相分离特征以及偏晶涂层显微硬度、耐磨性能的影响。研究结果表明:Cu80Fe20偏晶涂层内出现了分层现象,大量由体心立方结构α-Fe、面心立方结构γ-Fe组成的富铁颗粒弥散分布于上层的面心立方ε-Cu基体内,大量面心立方ε-Cu富铜颗粒分布于下层的α-Fe基体内;随着激光扫描速率增大,激光熔池的冷却速率增大,富铁颗粒粒径逐渐减小,面密度逐渐增大,相邻富铁颗粒间的间距减小,富铁颗粒对铜基体的阴影保护效应增强,使得偏晶涂层的显微硬度与耐磨性能增加,且均优于黄铜。     

Ni金属诱导晶化非晶硅(a-Si:H)薄膜

对在氢化非晶硅薄膜（a-Si：H）上溅射金属Ni的样品进行金属诱导晶化（MIC）／金属诱导横向晶化（MILC），制备多晶硅薄膜（p-Si）的上艺及薄膜特性进行了研究。XRD测最结果表明非晶硅在500℃退火1h后就已经全部晶化。金属诱导晶化的优选晶向为（220）．而且晶粒随退火时间的延长而长大。非晶硅薄膜样品500℃下退火6h后的扫描电镜照片显示，原金属镍覆盖区非晶硅全部晶化．晶粒均匀．平均晶粒大小约为0．3μm，而且已经发生横向晶化。EDS测试Ni在晶化的非晶硅薄膜中的原子百分含量分析表明，金属Ni在MILC过程中的作用只是催化晶化．除了少量残留在MILC多晶硅中外．其余的Ni原子都迁移至晶化的前沿。500℃下退火20h后样品的Raman测试结果也表明．金属离子向周边薄膜扩散．横向晶化了非晶硅薄膜。     

Ni80Fe20/Cu基磁性多层膜和自旋阀的微结构

用高分辨电子显微学及平行电子能量损失谱方法研究了Ni80Fe20/Cu基磁性多层膜和自旋阀的显微结构.高分辨像显示,磁性多层膜及自旋阀均具有沿薄膜生长方向的柱晶结构.Ni,Fe,Cu和Mn元素的成分分布图显示,柱晶内仍保持完整的层状结构.沿薄膜生长方向的自旋阀元素分布曲线分析表明,NiFe层中的Ni元素沿柱晶晶界向相邻Cu层扩散.讨论了这些低维磁电子学材料的显微结构对磁输运性能的影响.     

Microstructure in Ni_(80) Fe_(20)/Cu magneticmultilayers and spin valve

用高分辨电子显微学及平行电子能量损失谱方法研究了Ni80Fe20Cu基磁性多层膜和自旋阀的显微结构。高分辨像显示,磁性多层膜及自旋阀均具有沿薄膜生长方向的柱晶结构。Ni,Fe,Cu和Mn元素的成分分布图显示,柱晶内仍保持完整的层状结构。沿薄膜生长方向的自旋阀元素分布曲线分析表明,NiFe层中的Ni元素沿柱晶晶界向相邻Cu层扩散。讨论了这些低维磁电子学材料的显微结构对磁输运性能的影响。     

N元素偏聚对2205双相不锈钢微观组织结构的影响

采用金相、SEM、XRD和EBSD等分析方法,对双相不锈钢管N元素偏聚区域组织进行成分及结构的分析.结果表明:双相不锈钢管有100μm宽的带状N元素偏聚区,中心开裂,该区域基本为奥氏体单相组织,内部晶粒粗大且为等轴晶,以Σ3重位点阵(CSL)晶界为主,出现频率约为40%.而远离偏聚区中,铁素体奥氏体双相组织的相比例正常,奥氏体晶粒细小呈条状,也以Σ3晶界为主,出现频率降为27%.N偏聚区奥氏体与正常区奥氏体组织均可形成<111>∥RD及<110>∥ND方向的织构,但偏聚区奥氏体织构强度较之正常区域弱.     

二次退火对Au/Ni/Au/Ni/p-AlGaN欧姆接触组织结构的影响

在蓝宝石衬底上,利用金属-有机物化学气相沉 积(MOCVD)方法制备p-i-n结构AlGaN基体,采 用常规工艺制作台面型紫外探测器。电子束蒸发蒸镀Ni/Au/Ni/Au(20nm/20 nm)结构制备 p 电极。经空气中550℃/3min一次退火和N₂气氛中750℃/30s二次退火后得到欧姆接触。利用高分 辨透射电镜(HRTEM)和能谱(EDS)研究不同退火条件下p 电极接触的组织结构演变。结果 表明:一 次退火p电极金属层出现明显扩散,但仍维持初始的分层状态,金属/半导体接触界面产生 厚约4nm 的非晶层;二次退火后,金属电极分层现象和界面非晶层消失。金/半界面结构表现为半共 格关系,界面结 构有序性提高。Ni向外扩散,Au向内扩散,Ga扩散至金属电极,造成界面附近金属层富 集Au、Ga元素,导致p电极欧姆接触的形成。     

Zr基大块非晶合金的激光焊接

采用激光焊接技术,对Zr基大块非晶合金(BAA)Zr45Cu48Al7(原子数分数(%))进行了焊接实验,研究在激光焊接下不同工艺参量对焊接接头组织的影响,初步探讨了在焊接热循环过程中焊缝和热影响区的晶化行为。结果表明,在激光输出功率1200 W,焊接速率8 m/min的条件下,成功地获得了无气孔和裂纹等缺陷的焊接接头。焊缝和热影响区均没有出现晶化现象,仍然保持非晶结构。而当激光输出功率不变,焊接速率分别为2 m/min,4 m/min的工艺条件下,焊接后的接头则出现了不同程度的晶化现象。利用光镜和微区X射线衍射(XRD)实验分析确定:2 m/min条件下焊缝和热影响区均出现了晶化现象,晶化相主要为ZrCu相和Zr38Cu36Al26相(5τ);4 m/min条件下焊缝未出现晶化现象而热影响区出现晶化,晶化相主要为ZrCu相和5τ相。     

六种城市行道树叶表皮重金属元素含量及形态结构的研究

利用扫描电子显微镜(SEM)和X-射线能谱仪(EDS)对哈尔滨6种城市行道树叶表皮重金属(铬、镍、锌、铜、铅、镉)含量和形态结构特征进行了观察和分析。结果表明:交通流量大的路段、交通流量相对较小的路段、公园中的行道树叶表皮重金属含量(Cu、Zn除外)呈下降趋势;垂榆(Ulmus pumila var.pendula)中Cr元素含量较高,榆叶梅(Prunus triloba)Ni元素的含量较高,旱柳(Salix matsudana)Cd元素含量较高,小叶丁香(Syringa microphylla)和紫丁香(S.oblata)Pd元素含量较高。行道树叶表皮具有脊状突起和不规则排列的气孔;仅旱柳下表皮蜡质表层较厚;家榆(U.pumila)具有纤毛,小叶丁香具有腺毛,榆叶梅具有单细胞不分支的毛。通过对行道树叶表皮的重金属元素含量分析及形态结构的观察,探讨了城市行道树对重金属元素颗粒吸滞能力,为城市防污绿化树种的选择、生物监测和环境质量评价提供科学理论依据和参考价值。     

Electron microscopy analysis of the boundary layer structure of SrTiO3 semiconducting ceramic

In a boundary layer (BL) semiconducting SrTiO3-based ceramic condenser, the BL structure has been investigated using high-resolution field-emission scanning electron microscopy (FE-SEM) and field-emission (scanning) transmission electron microscopy (FE-(S)TEM). In an initial TEM observation, a double layered structure was observed at the grain boundary region. It consisted of a grain boundary (second phase) and a pair of the metal diffusion layers of up to several nanometres in width across the grain boundary where the change of the crystal lattice distance was undetected by the high-resolution TEM image. A facet structure was often observed on the grain boundaries. It was particularly formed on (020) plane of the grain crystal. High resolution SEM showed a jagged striped structure on the surface of the bulk material and on the inside grain as revealed by fracture. Using the similarity in shape and size, it can be identified to correspond to the facet boundary structure. Its formation mechanism can be explained as that during the reoxidization process when the oxide flux of the mixture of Bi2O3, PbO and CuO, painted on the bulk material, surfaces migrates into the ceramic along the grain boundary. The oxide corrodes the grain surfaces including the bulk surfaces. This corrosion particularly occurs on (020) plane of the grain so that the facet structure is produced. In this paper, by using the atomic scale high angle annular dark field STEM, it has been determined that Bi atoms preferentially replace Sr atoms on (020) in the diffusion layers. The atom position displacement was also detected at the grain surfaces and this altered atomic assignment can be determined as an origin of production of Sr2Bi4Ti5O18 at the grain boundary. Also, it was observed that the layer width of the metal diffusion layers was often different between the both grains and changed locally so that the ribbon of the diffusion layers meandered around the straight grain boundary. Its possible mechanism is also proposed.     

Al-Cu-Li合金中T1相的演变规律研究

利用扫描透射电镜技术结合第一原理计算,研究了新型高强Al-4.0Cu-1.0Li(wt.%)合金在165℃单级时效过程中T1相(Al2CuLi)的演变规律。实验结果表明:随着时效时间的延长,T1相存在两种生长方式,一种是沿着它的c轴方向正常生长,另一种是通过T1相的变体成核生长。T1相的变体由两个T1相单胞组成,并在两个单胞中间存在一层Li原子。通常,T1相的变体存在于Li原子过剩区,这种变体既可以单独形核,也可在T1相上形核。第一原理计算结果表明:对于T1相的结构,Van Smaalen模型能量最稳定,T1相的两种生长方式都具有能量合理性。     

Kinetics of the Au-Ni-Sn ternary intermetallic layer redeposition at the solder/under-bump metallurgy interface during aging treatment

The Au-Ni-Sn ternary intermetallic layer redeposition at the interface between the solder and the Au/Ni/Cu under-bump metallurgy (UBM) was measured experimentally and analyzed theoretically. The predicted thicknesses of the layer, assuming Au diffusion in the Sn-3.5Ag solder matrix, were thicker than those measured experimentally. The thicknesses predicted in the Sn-37Pb solder matrix, on the other hand, were thinner than those measured experimentally. The discrepancies between the predicted and measured thicknesses were discussed based on findings, such as formation of the ternary phase and presence of AuSn₄ depletion zones in the solder matrices, and the stoichiometry of the ternary phase.     

Effects of Electromigration on Interfacial Reactions in the Ni/Sn-Zn/Cu Solder Interconnect

Electromigration in the Ni/Sn-Zn/Cu solder interconnect was studied with an average current density of 3.51 × 10⁴ A/cm² for 168.5 h at 150°C. When the electrons flowed from the Ni side to the Cu side, uniform layers of Ni₅Zn₂₁ and Cu₅Zn₈ were formed at the Ni/Sn-Zn and Cu/Sn-Zn interfaces. However, upon reversing the current direction, where electron flow was from the Cu side to the Ni side, a thicker Cu₆Sn₅ phase replaced the Ni₅Zn₂₁ phase at the Ni/Sn-Zn interface, whereas at the Cu/Sn-Zn interface, a thicker β-CuZn phase replaced the Cu₅Zn₈ phase.     

Ag-Cu-Ti合金与ZrO_2陶瓷的润湿性及界面特征

通过改良座滴法研究了Ag-Cu-Ti/ZrO2陶瓷体系的润湿行为和界面特征[1]。采用ADSA(axisymmetric drop shape analysis)-SESDROPD分析软件,X射线衍射仪(XRD),场发射扫描电镜(FESEM)以及配有能谱仪(EDS)的扫描电镜(SEM)测量表征了温度变化下,不同Ti含量的Ag-Cu-Ti合金在ZrO2陶瓷基板上的润湿性及其界面微观结构的影响规律。结果表明:Ag-Cu-Ti/ZrO2陶瓷体系的润湿机制为反应性润湿。Ag-Cu-Ti合金在ZrO2陶瓷基板上的润湿性随Ti含量的增加逐渐改善。Ag54Cu43Ti4合金熔体在ZrO2陶瓷基板上的润湿性对温度具有明显的反常依赖性,Ag53Cu41Ti6合金的润湿性较好。随温度的升高,Ag54Cu43Ti4/ZrO2和Ag53Cu41Ti6/ZrO2界面反应产物TiO反应层逐渐增厚,Cu3Ti3O反应层有逐渐变薄的趋势。Ag50Cu40Ti10/ZrO2的界面,出现大块状的金属间化合物Cu3Ti3O,容易使合金和陶瓷界面发生剥离。     

离子束减薄对金属玻璃电镜样品的非均匀刻蚀

本文利用透射电子显微镜和原子力显微镜研究了金属玻璃样品在离子束作用后形成的厚度起伏特征。采用高分辨透射电镜和能谱分析结果表明金属玻璃样品中没有发生明显的结构和成分的变化。利用离子束与样品表面作用过程的粗化机理解释了出现这种特征厚度起伏的原因。这种厚度起伏是由材料本身性质和实验条件共同决定的。通过研究离子束与样品的作用方式,有利于确定合适的透射电镜样品制备方法,有助于利用透射电镜研究非晶样品的微观结构。     

Al-Mg-Si-Cu合金中晶界和晶内析出相粗化规律的研究

采用显微硬度测试仪、扫描电镜和透射电镜观察及能谱分析,研究了Al-0.5Mg-1.0Si-0.8Cu(wt.%)合金的晶界析出规律和晶内析出相的粗化机制。结果表明:180℃时效处理的Al-0.5Mg-1.0Si-0.8Cu(wt.%)合金晶界处存在富Si相和Q相两类不连续分布的析出相,它们的尺寸分别约为1 mm和几十纳米;时效0.5 h时晶界处有少量富Si相,时效5 h时晶界富Si相明显增多,时效36 h时富Si相开始粗化且间距变大,再进一步时效其形貌和分布变化不大;晶界Q相与相邻晶粒铝基体的界面取向关系是:[510]Al//[1120]Q;时效36 h晶内开始出现粗化析出相,且随时效继续进行合金晶内析出大量粗化相,存在明显的晶界无析出带现象。晶内粗化析出相主要含有Si元素,呈片状、球状和棒状3种形貌。其中,棒状Si析出相是沿〈001〉Al方向生长的,且〈112〉Si//〈001〉Al,{111}Si//{010}Al。     

Time‐resolved investigation of Cu(In,Ga)Se2 growth and Ga gradient formation during fast selenisation of metallic precursors

Ga segregation at the backside of Cu(In,Ga)Se₂ solar cell absorbers is a commonly observed phenomenon for a large variety of sequential fabrication processes. Here, we investigate the correlation between Se incorporation, phase formation and Ga segregation during fast selenisation of Cu–In–Ga precursor films in elemental selenium vapour. Se incorporation and phase formation are analysed by real‐time synchrotron‐based X‐ray diffraction and fluorescence analysis. Correlations between phase formation and depth distributions are gained by interrupting the process at several points and by subsequent ex situ cross‐sectional electron microscopy and Raman spectroscopy. The presented results reveal that the main share of Se incorporation takes place within a few seconds during formation of In–Se at the top part of the film, accompanied by outdiffusion of In out of a ternary Cu–In–Ga phase. Surprisingly, CuInSe₂ starts to form at the surface on top of the In–Se layer, leading to an intermediate double graded Cu depth distribution. The remaining Ga‐rich metal phase at the back is finally selenised by indiffusion of Se. On the basis of a proposed growth model, we discuss possible strategies and limitations for the avoidance of Ga segregation during fast selenisation of metallic precursors. Solar cells made from samples selenised with a total annealing time of 6.5 min reached conversion efficiencies of up to 14.2 % (total area, without anti‐reflective coating). The evolution of the Cu(In,Ga)Se₂ diffraction signals reveals that the minimum process time for high‐quality Cu(In,Ga)Se₂ absorbers is limited by cation ordering rather than Se incorporation. Copyright © 2014 John Wiley & Sons, Ltd.     

Cr3C2-CrB/Ni60激光熔覆层的耐蚀性研究

采用静态浸泡法对原位生长Cr3C2-CrB复合增强的镍基激光熔覆层的耐腐蚀性进行研究。使用扫描电镜和X射线衍射仪对熔覆层进行显微组织和物相分析,在光学显微镜下观察样品表面腐蚀形貌。结果表明：含16wt%（Cr2O3＋B2O3＋C）的Cr3C2-CrB/Ni60激光熔覆层在10%H2SO4溶液中表现出较好的耐腐蚀性能,与纯Ni60激光熔覆层相比,其耐蚀性提高1倍多。