Scanning electron microscopy imaging of dislocations in bulk materials, using electron channeling contrast

The imaging and characterization of dislocations is commonly carried out by thin foil transmission electron microscopy (TEM) using diffraction contrast imaging. However, the thin foil approach is limited by difficult sample preparation, thin foil artifacts, relatively small viewable areas, and constraints on carrying out in situ studies. Electron channeling imaging of electron channeling contrast imaging (ECCI) offers an alternative approach for imaging crystalline defects, including dislocations. Because ECCI is carried out with field emission gun scanning electron microscope (FEG-SEM) using bulk specimens, many of the limitations of TEM thin foil analysis are overcome. This paper outlines the development of electron channeling patterns and channeling imaging to the current state of the art. The experimental parameters and set up necessary to carry out routine channeling imaging are reviewed. A number of examples that illustrate some of the advantages of ECCI over thin foil TEM are presented along with a discussion of some of the limitations on carrying out channeling contrast analysis of defect structures.     

Preparation of lithium specimens for transmission electron microscopy

A method of preparing undeformed thin lithium specimens for TEM is described. A solution of dehydrated methanol and toluene is used both for initial dishing of the foil by chemical polishing and also for final thinning. Under electron beam irradiation in the TEM, new pure Li crystals can grow out of the existing Li specimen. These in situ crystals can be used for the study of the microstructure and electronic structure of Li using TEM and electron energy loss spectrometry.     

Initiation and growth of buckling in the biaxial diagonal tensile test on steel sheet

Initiation and growth of buckling, a main cause of surface deflection in large steel press-formed components such as automobile outer panels, is simulated by the biaxial diagonal tensile test on square steel sheet specimens. The effects of the properties of the steel sheets and the biaxial loading conditions on the initiation and growth of buckling are examined by the tests and by FEM analysis.It is found that both the initiation and the growth of buckling are strongly affected by the yield strength of the material, σ_s, and by the tensile stress in the breadth direction, p_Y, and that buckling is restrained when p_Y/σ_s is high: this is because the compressive stress at the center of the specimen, the compressive stress area, and the development of the buckling area are largely affected by these factors.     

Application of Trefftz theory in thin-plate buckling with in-plane pre-buckling deformations

The paper presents the application of Trefftz initial stress theory in determining the elastic buckling load of rectangular thin plates under in-plane stress resultants, with allowance for in-plane pre-buckling deformations. Exact buckling solutions for simply supported plates are obtained and compared with earlier results furnished by Ziegler (1983, Ing.-Arch.53, 61 [1]). Although somewhat different, due to the use of different theories, both sets of results show that the buckling loads may be reduced when pre-buckling deformations are accounted for. This observation is contrary to that for column buckling where it has been shown that the allowance for pre-buckling shortening results in a higher buckling load. This reduction in plate-buckling load is significant especially for plates with large thickness-to-span ratios and subject to a combination of tensile and compressive in-plane stress resultants that increase pre-buckling deformations.     

Tuning of nanogap size in high tensile stress silicon nitride thin films

High tensile stress suspended structures are demanded for high mechanical quality factor applications. However, high tensile stress causes distortion of the original shapes by contracting, buckling, and bending the suspended structures. We demonstrate a method to compensate for the shape deformation of suspended structures due to intrinsic tensile stress after they are released. With a new design, the distance between two suspended structures after wet etch can easily be tuned by a single fabrication beyond the lithographic resolution limits. The technique is simulated by finite element analysis and experimentally implemented to demonstrate a gap tuning capability with 2.4 nm standard error.     

Location specific in situ TEM straining specimens made using FIB

A method has been devised and demonstrated for producing in situ straining specimens for the transmission electron microscope (TEM) from specific locations in a sample using a dual-beam focused ion beam (FIB) instrument. The specimen is removed from a polished surface in the FIB using normal methods and then attached to a pre-fabricated substrate in the form of a modified TEM tensile specimen. In this manner, specific features of the microstructure of a polished optical mount can be selected for in situ tensile straining. With the use of electron backscattered diffraction (EBSD), this technique could be extended to select specific orientations of the specimen as well.     

Linear and nonlinear buckling analysis of a locally stretched plate

Uniformly stretched thin plates do not buckle unless they are in special boundary conditions. However, buckling commonly occurs around discontinuities, such as cracks, cuts, narrow slits, holes, and different openings, of such plates. This study aims to show that buckling can also occur in thin plates that contain no defect or singularity when the stretching is local. This specific stability problem is analyzed with the finite element method. A brief literature review on stretched plates is presented. Linear and nonlinear buckling stress analyses are conducted for a partially stretched rectangular plate, and various load cases are considered to investigate the influence of the partial loading expanse on the critical tensile buckling load. Results are summarized in iso-stress areas, tables and graphs. Local stretching on one end of the plate induces buckling in the thin plate even without geometrical imperfection.     

Buckling of columns: Allowance for axial shortening

This paper investigates the effect of axial shortening on (i) the elastic buckling of columns with a continuous elastic restraint, (ii) the elastic buckling of rotating columns and (iii) the free vibration of columns under a static axial load. These column problems can be solved in a unified approach because the resulting energy functional is similar. The field differential equation is derived by minimizing the energy functional with respect to the lateral displacement function via calculus of variations. The buckling load or fundamental frequency may be obtained by analytically solving the two-point boundary-value problem. It was found that the boundary conditions and the restraint parameter or angular velocity parameter affect the influence of axial shortening on the buckling load. In vibrating columns, tensile forces enhance the effect of axial stretching on the fundamental frequency.     

内衬油管井抽油杆断脱分析

以胜利油田东辛采油厂DXX109X106油井为例,对其断脱形式按强度分析、疲劳分析以及屈曲分析逐层计算。计算表明,该油井抽油杆断裂处最大应力172.45 M Pa,远远小于抗拉强度795~965 M Pa,不属于拉伸强度破坏;疲劳特性分析表明,此井的实际平均应力-应力幅点在持久极限曲线图以内,属于非正常疲劳断裂;示功图分析表明,该井抽油杆柱的下冲程存在严重的屈曲现象,宜将抽油杆简化为受压杆件。     

Synergistic effects of anisotropy and image force on TEM diffraction contrast of dislocation loops

Based on column approximation (CA) assumption, many-beam Schaeublin–Stadelmann diffraction equations are employed for simulating the transmission electron microscopy (TEM) diffraction image contrast of dislocation loops within thin TEM foil of finite thickness, and two beam and many beam diffraction conditions are compared. Moreover, the effects of materials anisotropy and free surface relaxation induced elastic fields distortion of dislocation loops on the black-white image contrast are specially focused. It is found that anisotropy has a remarkable impact on the TEM image contrast of dislocation loop, and free surface relaxation induced image forces can change the black-white contrast features when dislocation loops are near TEM foil free surfaces. Thus, in order to make reliable judgment on the nature of defects, effects of free surface and anisotropy should be included when analysing irradiation induced dislocation loops and other type of defects in in-situ electron, proton, heavy-ion irradiation experiments under TEM environments.     

304不锈钢薄板微塑性成形尺寸效应的研究

针对五种厚度304不锈钢薄板进行了单向拉伸试验和微弯曲试验,测得的屈服应力和回弹角均随板厚减薄而增大,表现出“越薄越强”的尺寸效应现象。通过在Hall-Petch公式中引入相对厚度项对公式进行修正,使得对屈服应力的预测与试验结果更吻合。采用修正的Nix-Gao应变梯度强化模型预测了回弹角与板厚的关系,预测结果与试验结果吻合。
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Cross-sectional deformations of rectangular hollow sections in bending: Part II — analytical models

In this part, analytical models to predict the deflection of cross-sectional members such as flanges and webs are developed. The models are based on the deformation theory of plasticity along with the energy method, using appropriate shape functions capable of including the restraining effect of adjacent members. The present method provides explicit solutions of cross-sectional deformations prior to buckling, onset of buckling, as well as post-buckling deformations at different stages of bending. The predictions show that the suck-in of the tensile flange is closely related to geometry parameters, particularly the flange width. Plastic anisotropy appears to be the most significant material parameter. The width-to-thickness ratio tends to be the governing parameter with respect to buckling of the inner (compressive) flange. Also, the strain hardening of the material has a major effect on onset of buckling as well as post buckling deformations. Upon continued bending after buckling, the wavy deformation of the inner flange develops more rapidly than the more uniform deformation of the outer (tensile) flange. For relatively compact sections, however, the deformation mode of the compressive flange resembles that of the tensile flange without any typical buckling waves. There are also obvious interactions between deformations of different members. Comparing the theoretical predictions with the experimental results presented in Part I, a reasonably good agreement was found.     

Preparation of carbon-free TEM microgrids by metal sputtering

A new method for preparing carbon-free, temperature-stable Transmission Electron Microscope (TEM) grids is presented. An 80% Au/20% Pd metal film is deposited onto a ‘holey’ microgrid carbon supported on standard mixed-mesh Au TEM grids. Subsequently, the carbon film is selectively removed using plasma cleaning. In this way, an all-metal TEM film is made containing the ‘same’ microgrid as the original carbon film. Although electron transparency of the foil is reduced significantly, the open areas for TEM inspection of material over these areas are maintained. The metal foil can be prepared with various thicknesses and ensures good electrical conductivity. The new Au/Pd grids are stable to at least 775 K under vacuum conditions.     

轻型薄壁箱形结构耐压强度研究

本文对薄壁装配式不锈钢水箱的轻型薄壁箱形结构的耐压强度进行了试验研究,得到了在冲压前后模压板不同区域的各项力学性能指标,发现其球冠区域屈服强度增加高达42%;获取了在内压载荷下箱体各控制部位的力学响应特性,箱体各模压板块中与加强槽毗邻的球冠边缘区域的应力始终占控制地位;得到了箱体的屈曲失效模式。有限元数值模拟结果与试验数据较为吻合,可为指导和规范其设计制造提供参考。     

在空气和真空中退火的316奥氏体不锈钢的力学性能及微观结构分析

对316奥氏体不锈钢在空气和真空条件下进行退火,在恒定的拉伸速度下进行室温拉伸强度试验,并利用扫描电镜和透射电镜观察拉伸试验后试样的表面和近表面的微观结构.退火试样的抗拉强度和应力值高于未退火试样;在真空炉中退火的试样,其抗拉强度及在特定应变量下的应力值均高于在空气炉中退火的试样.在真空炉中退火的316不锈钢的表面氧化层分内、外两层,外层由均匀、致密的亚微细晶粒组成;而在空气炉中生成的氧化层结构复杂,和基体的结合强度非常低.氧化层-基体界面是一个充满活力的位错源,真空炉退火试样的位错密度大于空气炉退火试样.氧化层的微观结构和两种试样位错密度的不同是导致产生不同拉伸性能的重要原因.     

A cellular finite element model for the cutting of softwood across the grain

In this paper, the mechanics of cutting wood across the grain are reexamined. A hybrid cellular/macroscopic finite element model of wood was developed to simulate the effects of cell collapse during the cutting process. Initially, the model was used to simulate the compression test across the grain. The linear elastic and cell collapse behaviours of the compression tests were sucessfully simulated. The model was then used to simulate two orthogonal cutting processes, wedge cutting and chip-forming cutting. The cellular/macroscopic model revealed that during the cutting process, the load compresses the wood until cell wall buckling occurs ahead of the tool. The collapse of the supporting cell wall results in a localized tensile stress in the longitudinal direction of the cell at the tip of the tool. It is postulated that this longitudinal tensile stress would lead to microfibrils being pulled out of the matrix and hence to failure of the cell wall. Therefore, the cellular/macroscopic model has been used to explain the mechanics of severing wood fibres during the process of cutting wood across the grain.     

Preparation of transmission electron microscopy cross-section specimens of crack tips using focused ion beam milling

The preparation of transmission electron microscope (TEM) thin foil specimens from metal alloys containing cracks is usually thwarted by the difficulty in preventing preferential erosion of material along the flanks and at the tips of cracks. Recent developments in focused ion beam (FIB) micromachining methods have the potential to overcome this inherent problem. In this article we describe the development of new procedures, one using FIB alone and the other using a combination of FIB with more conventional ion milling to generate TEM specimens that largely retain the microstructural information at stress corrosion cracks in austentic alloys. Examples of corrosion product phase identification and interfacial segregation are included to verify that detailed information is not destroyed by ion bombardment during specimen preparation.     

核级SA-508 Gr.3 Cl.1材料拉伸与压缩蠕变行为的比较研究

堆芯熔融物堆内滞留(In-vessel retention,IVR)是压水堆的严重事故缓解措施。IVR过程中,反应堆压力容器底封头(Reactor pressure vessels,RPV)沿壁厚方向同时存在拉伸和压缩应力。为保证IVR过程中RPV的结构完整性,有必要研究SA-508 Gr.3 Cl.1材料的拉伸和压缩蠕变行为及其差异。基于此,开展了SA-508 Gr.3 Cl.1材料的拉伸蠕变和压缩蠕变试验测试,分析了材料的拉伸和压缩蠕变行为以及变形机制的不同。结果表明：拉伸和压缩蠕变的第一、二阶段基本吻合,但压缩蠕变没有出现明显的蠕变第三阶段;拉伸蠕变在试验应力范围内的变形机制为单一的位错攀移,而随着应力的降低,压缩蠕变变形机制由位错攀移转变为晶界滑移/空位扩散;拉伸蠕变对亚晶组织演化程度的影响大于压缩蠕变,这可能与蠕变变形机制的转变相关。     

Foreword

The volume of thin foil specimens, which contain precipitate or other particles, viewed in the TEM is needed to determine particle density and spacing. It can be determined from the locations of the particles, measured using stereo pairs. A calculation that determines the volume between planes (not necessarily parallel or horizontal) that enclose the points is described. These planes will systematically underestimate the actual surface spacing and hence the volume, but a simple correction factor based on the number of points used in the fit can be used to estimate the actual volume. The method is tested, and its accuracy is evaluated using simulated data and applied to precipitate particles in creep-tested silicon carbide.     

Long-wave buckling of elastic square honeycombs subject to in-plane biaxial compression

In this study, long-wave and short-wave buckling of elastic square honeycombs subject to in-plane biaxial compression are analyzed using a two-scale theory of the updated Lagrangian type. By taking cell aggregates to be periodic units, the bifurcation and post-bifurcation behavior are analyzed so that the dependence of buckling stress on periodic length can be discussed. It is shown that buckling stress decreases as periodic length increases, and that very-long-wave buckling occurs just after the onset of macroscopic instability if the periodic length is sufficiently long. Then, a simple formula to evaluate the very-long-wave buckling stress under in-plane biaxial compression is derived by exploring the macroscopic instability condition in the light of the two-scale analysis. The resulting formula is verified using an energy method.