单晶体心立方金属铌裂纹尖端位错增殖行为的 原位研究

位错的增殖对体心立方金属材料的塑性性能有着非常重要的意义,目前对于体心立方位错增殖机制的动态研究主要依赖于计算模拟,实验研究很少见到报道,其位错增殖机制尚存在不确定性.本文利用透射电镜原位拉伸技术,实现了单晶体心立方金属铌(Nb)裂纹尖端位错增殖的原位动态实验观察,并提出了两个位错模型来解释位错增殖以及运动的机制.从实验上不仅证实了之前模拟的预测,而且对现有的模型进行了很好的补充,为体心立方金属材料的塑性变形机制提供了基础实验数据.     

G115钢中变形机制的原位透射电镜研究

新型马氏体耐热钢-G115钢以其优异的性能成为我国650℃超超临界火电机组厚壁部件的候选钢种。本文采用透射电镜中的原位拉伸力学实验，研究了G115钢室温变形条件下的位错行为和塑性变形机制。研究发现，位错间的相互反应、位错墙-位错的相互作用及多尺寸颗粒-位错的交互作用是材料塑性变形的主要机制。位错墙所构成的亚晶界不仅可以阻碍位错的运动，也可以选择性地传输位错。同时，析出相与位错之间的反应非常丰富。晶内随机分布的几十纳米左右粒径的富铜相可以有效钉扎位错并促进颗粒周围的位错增殖，而几百纳米左右粒径的M₂₃C₆颗粒则会强烈地阻碍位错滑移，形成位错的塞积和缠结。这些机制对材料的均匀塑性变形均有促进作用。     

纯锡的速率相关性变形行为

考察了纯锡在拉伸载荷下的力学性能及形变,探讨了应变速率对纯锡的变形机制的影响。采用扫描电镜形貌观察,对比不同应变速率(0.001~0.1 s–1)下样品表面的晶粒形貌、形变特征、断口信息。发现在较低的应变速率(0.001 s–1)下,纯锡的形变机制以蠕变为主要模式;在较高的应变速率(0.1 s–1)下,形变机制以位错滑移为主要特征。     

不同应变速率下Fe-29Mn-3Al-3Si钢的冲击性能及微观组织研究

采用分离式Hopkinson压杆对冷轧退火态Fe-29Mn-3Al-3Si TWIP钢进行650 s^-1～3 800 s^-1范围内高应变速率的动态冲击压缩实验。采用扫描电镜(SEM)、电子背散射衍射技术(EBSD)、X射线衍射(XRD)和透射电镜(TEM)等研究手段对冲击前后试样的微观组织结构进行表征。结果表明,在高速冲击条件下该TWIP钢具有正应变速率强化特性,且主要变形机制是孪生诱导塑性(TWIP)。随着应变速率及应变量增大,材料强度增加,形变孪晶数量增加,孪晶与位错交割加剧。在压缩变形过程中,〈001〉取向的晶粒易产生滑移和孪生,为软的晶体取向;而〈110〉取向晶粒中孪生和滑移的概率减少,为硬的晶体取向。随形变量的增加,逐渐形成〈110〉丝织构。高速冲击变形中的绝热效应使位错发生动态回复而对形变孪晶影响较少。TWIP效应、加工硬化、动态回复以及形变孪晶界的动态Hall-Petch效应大幅提高材料的高强度并保持高的塑性。     

工业纯钛板激光冲击形变的特征微结构

用输出波长为1064nm、脉冲宽度为20ns的调Q钕玻璃激光器对TA2工业纯钛板料进行了激光连续冲击无模弯曲形变试验,用扫描电镜(SEM)和透射电镜(TEM)分析了激光冲击变形全断面的特征微结构。根据变形区的应力状态,观察到3种主要的特征微结构。一是位于压缩应变区域的近纳米级微孪晶栅,认为是由接近同一方向的高密度层错聚集的产物;同时由于新生微结构之间的交互作用而诱发的第三类微观内应力,在基体间形成高密度的位错网络和位错胞。二是同在压缩应变区域,在超高应变率和强大的冲击能量作用下局部切变诱发的α→α′的逆相变。三是在激光冲击超高速形变条件下,受高度约束的HCP晶系材料塑性变形阻力增大,在拉伸变形区域诱发沿解理方向的局部层状集群滑移现象。上述3种现象源于激光冲击形变时材料微观约束条件和形变方式,造成形变区域微结构和硬度的不均匀性,在重复冲击条件下,不利于钛板的均匀变形。     

温度对体心立方钼中位错行为影响的原位透射电镜研究

本文通过原位透射电镜下的拉伸试验,在不同温度下研究了具有室温韧脆转变行为的体心立方钼中的位错行为。结果表明,室温下钼的变形过程中主要以刃位错和混合位错的运动为主,位错运动受扭结对机制控制,存在大量刃位错的快速运动和螺位错交滑移行为,位错运动情况复杂。低温下,刃位错运动被抑制,螺位错运动为主导变形行为。螺位错以长直形态存在,以非连续跳跃方式运动。这种低温下活跃的螺位错行为以及温度与位错行为变化的关系尚无法用传统热激活理论解释,声子拖拽机制或变为位错运动的激活机制。     

原位观察Shockley不全位错的发射

纳米晶体材料与传统的多晶材料相比，具有较高的强度和硬度，其优越的力学性能归因于它们独特的变形机制。在纳米材料中，随着晶粒尺寸的不同，其形变方式主要有晶界转动、晶界扩散、不全位错发射形成层错、孪晶等，这些形变机制已被分子动力学模拟计算所预测。     

TiAl合金形变孪晶恢复过程的原位拉伸观察

ＴｉＡｌ合金形变孪晶恢复过程的原位拉伸观察＊梁伟杨德庄＊赵兴国陆路郑维能（太原工业大学测试中心，太原０３００２４）（＊哈尔滨工业大学热处理教研室）（１／６）〈１１２］｛１１１｝形变孪生及（１／２）〈１１０］普通位错滑移是双相ＴｉＡｌ基合金的两个主要变...     

孪晶界移动的动态过程

通过原位拉伸高分辨透射电镜观察,研究纳米孪晶铜中孪晶界的动态形变过程.实验发现,与以往分子动力学模拟计算预测的结果不同,Shockley不全位错主要从孪晶界与晶界的交叉点处发射,沿着孪晶界面运动,导致孪晶界移动.并对孪晶界移动作为纳米孪晶铜在塑性变形初期的一种主要形变方式进行了讨论.     

淬火回火钢的形变位错结构与强化

淬火回火钢的流变应力和形变特性直接影响它的加工性能和使用性能。应用位错理论研究金属拉伸形变机制,形变位错结构的变化规律,对改进材料的力学性能可提供理论依据,因而这种研究具有重要的实用意义[1.2]。本文应用电子衍衬分析方法研究淬火高温回火的低碳铬镍钢的拉伸加载形变位错结构。观察了碳化物对位错的钉扎作用,分析了位错的增殖机制,讨论了位错之间、位错与碳化物之间、位错与铁素体晶条界之间的相互作     

In-situ metrology and testing of nanotwinned copper pillars for potential air gap applications

We have performed in-situ nanocompression testing in a transmission electron microscope (TEM) of copper pillars having dimensions of the same order of typical via and line structures used in the semiconductor industry. We show direct evidence that twin boundaries can withstand extensive plastic deformation and still retain their structure when compared to regular grain boundaries. Through real-time TEM observations we have verified the deformation mechanisms of twin boundaries predicted by molecular dynamic (MD) simulations. Our quantitative in-situ stress measurements are also in close agreement with those reported by MD and energetics based calculations.     

In situ TEM/SEM electronic/mechanical characterization of nano material with MEMS chip

Our investigation of in situ observations on electronic and mechanical properties of nano materials using a scanning electron microscope （SEM） and a transmission electron microscope （TEM） with the help of tradi- tional micro-electro-mechanical system （MEMS） technology has been reviewed. Thanks to the stability, continuity and controllability of the loading force from the electrostatic actuator and the sensitivity of the sensor beam, a MEMS tensile testing chip for accurate tensile testing in the nano scale is obtained. Based on the MEMS chips, the scale effect of Young＇s modulus in silicon has been studied and confirmed directly in a tensile experiment using a transmission electron microscope. Employing the nanomanipulation technology and FIB technology, Cu and SiC nanowires have been integrated into the tensile testing device and their mechanical, electronic properties under different stress have been achieved, simultaneously. All these will aid in better understanding the nano effects and contribute to the designation and application in nano devices.     

A review of focused ion beam technology and its applications in transmission electron microscopy

The role of focused ion beam (FIB) fabrication in the development of sample preparation techniques for transmission electron microscopy (TEM) has been described in this paper. Since the repeatability of FIB sampling and TEM observations has become important, the microsampling and in situ lift-out methods are currently in wide use. Furthermore, artifacts induced during FIB milling and the consequent difficulties with energy dispersive X-ray spectroscopy are detailed. The remarkably increased capability of scanning ion microscopy and its applications are also discussed.     

In-situ transmission electron microscopy study of the nanoindentation behavior of Al

Nanoindentation is a useful technique for investigating fundamental mechanisms associated with small-volume deformation, processes that are often obscured on coarser scales. Recently, a novel experimental technique of in-situ nanoindentation for the transmission electron microscope (TEM), which provides real-time observations of the mechanisms associated with localized deformation, has been developed. Calibration of the force-displacement-voltage relation and load-frame compliance associated with this instrument allows quantitative force-displacement measurements to be obtained in the manner of traditional indentation experiments. Here, we describe the experimental technique along with methods for quantifying the load-displacement response. Additionally, results from experiments into Al thin films are presented.     

In situ tensile testing of tin (Sn) whiskers in a focused ion beam (FIB)/scanning electron microscope (SEM)

Tin and tin-alloyed electroplated films are known to be susceptible to whisker growth under a range of conditions, many of which result in the generation of compressive stresses in the film. Compressive stress is considered to be one of the primary causes for whisker nucleation and growth. While extensive investigations have been performed on whisker growth, there have been few studies on the mechanical properties of tin whiskers themselves. We report on the tensile behavior of tin whiskers that were obtained by indentation and furnace aging of electroplated tin films on copper disks. Tensile tests of the whiskers were conducted in situ in a dual beam focused ion beam (FIB)-scanning electron microscope (SEM) system using a micro electro-mechanical systems (MEMS) based tensile testing stage. The strength of the whiskers was found to decrease with an increase in gage length and aged whiskers were found to be weaker than their indented counterparts. The observed gage length effect can be attributed to the probability of finding more defects as the whisker length increases. The effect of processing on the observed strength variation was investigated by analyzing the oxygen content in the whiskers via energy dispersive spectroscopy and the microstructure through transmission electron microscopy (TEM). The deformation mechanisms of whiskers were also inferred using post-mortem TEM. It was observed that the whiskers grown by indentation were dislocation free both before and after deformation. In contrast, whiskers grown by aging showed notable dislocation content (arranged in low energy configurations) even before deformation.     

Impact of thermal cycling on the evolution of grain, precipitate and dislocation structure in Al, 0.5% Cu, 1% Si thin films

Thermal cycles have been performed both outside and inside a transmission electron microscope (TEM) in order to analyze the evolution of the microstructure of Al, 0.5% Cu, 1% Si thin films deposited onto oxidized Si substrates. It is shown that grain growth and dislocation activity start almost simultaneously and cooperate throughout the plastic regime of the stress–temperature curve to generate bamboo-type grains with low dislocation density. Si precipitates serve as anchoring points for dislocations and grain boundaries. Thermal cycling and diffusion cause the growth of these precipitates and a diminution of their number. Diffusion also proves to play an important role regarding plastic relaxation at the Al/SiO_x interface and at the grain boundaries where an intense hillock and whisker formation has been observed in scanning electron microscope (SEM). The stress–temperature evolution is discussed in light of these observations.     

电子束致沉积手控生长碳纳米线

用电子束致沉积(EBID)来制备各种纳米尺寸的结构在纳米材料的制备和器件构建方面有着良好的应用前景。相对于聚焦离子束(FIB),它具有对样品损伤小和所得结构尺寸更小等优点。此前,电子束致沉积的工作大多数在扫描电镜中完成,而在透射电镜中沉积直到近两年才发展起来。本文尝试在普通热发射透射电镜中,手动控制生长碳纳米线、点等结构。对碳纳米线的生长过程进行了原位观测,并对电子束斑的大小、形状和辐照时间对沉积物形状的影响作了初步的研究。最后对电子束致沉积可控生长无定型碳纳米线可能的应用作了一些探索。     

Identification of crack path of inter- and transgranular fractures in sintered silicon nitride by in situ TEM

Inter- and/or transgranular crack paths in sintered silicon nitride (Si3N4) during fracture were investigated by in situ straining experiments in a transmission electron microscope at room temperature, using a high-precision micro-indenter. By this technique, cracks introduced in an in situ manner were observed to propagate in the grain interior and along grain boundaries. High-resolution electron microscopy (HREM) observation revealed that the crack propagation takes place at an interface between Si3N4 grains and an intergranular glassy film (IGF) in the case of intergranular fractures. According to the results by previous molecular dynamics simulations, a number of dangling bonds are present at the Si3N4/IGF interface, which should result in the observed fracture behavior at the interface. On the other hand, the crack path introduced during transgranular fracture of Si3N4 grains was found to be sharp and straight. The observed crack propagated towards [1120] inside the Si3N4 grain with the crack surface parallel to the (1100) plane. The HREM observations of crack walls revealed them to be atomically flat. The atomic termination of the crack walls was identified in combination with image simulations based on atomic models of the cleaved crack walls.     

The Effect of He Implantation on the Tensile Properties and Microstructure of Cu/Fe Nano‐Bicrystals

In situ uniaxial tensile experiments on as‐fabricated and helium‐implanted 100 nm‐diameter Cu/Fe bicrystals unearth the effect of individual face‐centred‐cubic/body‐centred‐cubic (fcc‐bcc) interfaces on improving radiation‐damage tolerance and helium absorption. Arrays of nanotensile specimens, each containing a single Cu grain in the bottom half and a single Fe grain on top, were fabricated by templated electron‐beam lithography and electrodeposition. Helium is implanted at 200 keV to a dose of 10¹⁴ ion/cm² nominally into the interface region. High‐resolution, site‐specific transmission electron microscopy (TEM) and through‐focus analysis reveal that the interfaces are nonplanar and contain ≈5 nm‐spaced He bubbles with diameters of 1–2 nm. Nanomechanical experimental results show that the irradiated samples exhibit yield and ultimate tensile strengths more than 60% higher than the as‐fabricated ones, while they retain comparable ductility. Tensile failure always occurs gradually, along the interfaces, with no noticeable shape localization. The absence of brittle failure in He‐irradiated metals might be explained, in part, by the inability of the small He bubbles to serve as sufficient stress concentrators for cracking. In addition, the non‐orthogonal orientation of the interfaces with respect to the loading axes results in the development of both normal‐ and shear‐stress components. Tensile loading along the pillar axes may cause those interfacial regions subjected to normal stresses to detach, while the inclined regions, subjected to shear, to carry plastic deformation until final fracture.