Novel combination of orientation measurements and transmission microscopy for experimental determination of grain boundary miller indices in silicon and other semiconductors

The determination of grain boundary planes in multicrystalline material has only been restricted to transmission electron microscope investigations (Jang et al., 1992; Elgat et al., 1985) or to metallograpical investigations of the grain boundary (Randle et al., 1993). The first method is expensive, and both are complex and time consuming in grain boundary preparation. This paper proposes the determination of grain boundary planes in semiconductor wafer by a combined application of Electron Back Scatter Diffraction and Infrared Transmission Microscopy. In particular, the new method is demonstrated with directional solidificated multicrystalline silicon.     

Evaluation of misindexing of EBSD patterns in a ferritic steel

The systematic misindexing caused by pseudo‐symmetry Kikuchi diffraction patterns in automated Electron Backscatter Diffraction analysis has been studied in a 9Cr‐1Mo ferritic steel. Grains with its [1 1 1] directed towards detector centre were found to be prone to misindexing, and the solutions exhibit a relative orientation of ±30° and 60° about the common [1 1 1] axis (as compared to the true orientation). Fictitious boundaries were detected within such grains, which satisfy the Σ3 or Σ13b type coincidence site lattice boundary criteria. Misindexing rate was reduced with more than six detected bands, but 30° rotated solution was comparatively more persistent, as the additional bands of (3 1 0)‐type exhibited a nearly good pattern match. Increase in detector collection angle to 0.96 sr or number of detected bands to nine were found to be beneficial in preventing the misindexing problem.     

基于纳米操作机的多晶ZnO晶界电学特性研究

文中基于安装在扫描电子显微镜（Scanning Electron Microscopy, SEM）中的纳米操作机,对具有微米级细晶粒的氧化锌（ZnO）压电陶瓷进行了单晶粒边界的直接电学测量。由纳米操作机操纵的双探针作为微电极夹在机械手上,测量了ZnO压电陶瓷晶界的伏安特性曲线、非线性系数以及20个晶粒的平均尺寸。在20 Hz~1 MHz的频率范围内,通过等效电路拟合,以阻抗复平面表示实验数据。实验表明低频直流高阻阻抗的本质可归因于晶界,同时20 Hz下的电阻分布可用于预测ZnO压电陶瓷在某些较低频率下的阻抗特性。     

Application of acoustic microscopy to the measurement of some physical parameters of ceramics

The scanning acoustic microscope is a valuable tool for the ultrasonic non-destructive testing of ceramic materials or sintered metals, like titanium compounds. Bulk defects, responsible for the mechanical aging and breakdown of parts, are easily detected and imaged. Moreover, diffuse structures are evidenced in these images, forming a continuous background. In this paper, we present a method which enables the determination of physical parameters, like the density and the bulk grain size of the materials, from this background. This information is extracted, using a statistical approach, from the histograms pertaining to materials with a spectrum of different microstructures, based on a principal component analysis (PCA). It may be noted that the size of the microstructure elements accessible by this method can be lower than the spatial resolution of the microscope.     

The influence of low-strain thermo-mechanical processing on grain boundary network characteristics in type 304 austenitic stainless steel

Grain boundary engineering of austenitic stainless steel, through the introduction of plastic strain and thermal annealing, can be used to develop microstructures with improved resistance to inter‐granular degradation. The influence of low‐strain thermo‐mechanical processing on grain boundary network development, with systematic variations of annealing treatments, has been investigated. Three stages of the microstructure development during grain boundary engineering in low‐strain processing conditions are identified, and correlated with changes in grain boundary character and deviation distributions. Low‐energy connected length segments at triple junctions, which have been proposed to be responsible for crack bridging during inter‐granular stress corrosion cracking, can be influenced by the choice of the annealing treatment parameters. The development of individual grain boundary length segments of different character showed consistent trends with increasing grain size. Crack length predictions are consistent with the beneficial effect of designing microstructures with high fractions of twin grain boundaries and smaller grain size.     

Determining the orientations of ice crystals using electron backscatter patterns

Knowing the orientations of the ice crystals in a polycrystalline aggregate is essential for understanding and modeling the flow of naturally occurring ice. Here we show, for the first time, that the orientation of crystals in polycrystalline ice can be determined with a higher angular and spatial resolution and more rapidly than any currently used method by using electron backscatter patterns (EBSPs) in a cold-stage equipped scanning electron microscope. We also present an orientation image map constructed from EBSPs, and discuss possible applications of the technique for ice. The results indicate that obtaining EBSPs and orientation images from other frozen water-containing materials, such as clathrate hydrates, may also be possible.     

A new method for investigating the undersurface of cell monolayers by scanning electron microscopy

Glow discharge is commonly used for cleaning the inside of coating units and for cleaning hard surfaces before carbon or metal evaporation procedures. In this study it has been used to remove the embedding medium to reveal, for scanning electron microscope (SEM) study, the undersurfaces of Balb/c 3T3 fibroblastic cells that have been cultured on Thermanox discs and embedded in LR White resin. Ten to twenty-minute ionization times were found to reveal the largest area of the undersurface without causing damage to the cells. Chemical etching of the resin was also shown to reveal the undersurface of the cells, but caused some damage, preventing successful re-embedding for transmission electron microscopy, and at higher magnifications revealed less detail. A circular impression within the main outline of the cells was observed in many cells, which is considered to reflect the presence of a nucleus. The undersurfaces of most cells, after applying both methods of etching, displayed a number of very short processes. Subsequent transmission electron microscopy of ultrathin sectioned, re-embedded, areas of the gold sputter-coated blocks revealed the depth of ionization that had occurred and confirmed that the specimens observed in SEM were the undersurfaces of cells. This method can be modified to study the attaching surface of any organism to a substratum.     

The analysis of quartz c-axis fabrics using a modified optical microscope

A new fully automated microfabric analyzer (MiFA) is described that can be used for the fast collection of high‐resolution spatial c‐axis orientation data from a set of digital polarized light images. At the onset of an analysis the user is presented with an axial‐distribution diagram (AVA –‘Achsenverteilungsanalyse’) of a thin section. It is then a simple matter to build‐up c‐axis pole figures from selected areas of interest. The c‐axis inclination and colatitudes at any pixel site is immediately available to create bulk fabric diagrams or to select measurements in individual areas. The system supports both the interactive selection of c‐axis measurement sites and grid array selection. A verification process allows the operator to exclude dubious measurements due to impurities, grain boundaries or bubbles. We present a comparison of bulk and individual c‐axis MiFA measurements to pole figures measured with an X‐ray texture goniometer and to data collected from a scanning electron microscope furnished with electron backscatter diffraction (EBSD) facility. A second sample, an experimentally deformed quartzite, illustrates that crystal orientations can be precisely linked to any location within an individual grain.     

'Five-parameter' analysis of grain boundary networks by electron backscatter diffraction

This paper describes state‐of‐the‐art analysis of grain boundary populations by EBSD, with particular emphasis on advanced, nonstandard analysis. Data processing based both on misorientation alone and customised additions which include the boundary planes are reviewed. Although commercial EBSD packages offer comprehensive data processing options for interfaces, it is clear that there is a wealth of more in‐depth data that can be gleaned from further analysis. In particular, determination of all five degrees of freedom of the boundary population provides an exciting opportunity to study grain boundaries by EBSD in a depth that was hitherto impossible. In this presentation we show ‘five‐parameter’ data from 50 000 boundary segments in grain boundary engineered brass. This is the first time that the distribution of boundary planes has been revealed in a grain boundary engineered material.     

Visualization of flagellar interactions on bacterial carpets

Methods for the in-depth study of the physics of microscale actuation of microfluidics environments by flagellated bacteria 'teamsters' have been developed. These methods, which include single and multi-colour fluorescent labelling and electron microscopy allow for the analysis of the effect that individual flagellar filaments have on bacterially driven microstructures, and allow for the investigation of the interaction and coordination of flagellar filaments of neighbouring bacteria on densely packed monolayers of bacteria, 'bacterial carpets'. We show that the flagella of bacteria that are immobilized on a surface often interact with each other, and that the flagella of these bacteria do not often form multi-flagella bundles that are aligned with the cell body.     

Advantages of stereo imaging of metallic surfaces with low voltage backscattered electrons in a field emission scanning electron microscope

High emission current backscattered electron (HC-BSE) stereo imaging at low accelerating voltages (≤ 5 keV) using a field emission scanning electron microscope was used to display surface structure detail. Samples of titanium with high degrees of surface roughness, for potential medical implant applications, were imaged using the HC-BSE technique at two stage tilts of + 3° and − 3° out of the initial position. A digital stereo image was produced and qualitative height, depth and orientation information on the surface structures was observed. HC-BSE and secondary electron (SE) images were collected over a range of accelerating voltages. The low voltage SE and HC-BSE stereo images exhibited enhanced surface detail and contrast in comparison to high voltage (> 10 keV) BSE or SE stereo images. The low voltage HC-BSE stereo images displayed similar surface detail to the low voltage SE images, although they showed more contrast and directional sensitivity on surface structures. At or below 5 keV, only structures a very short distance into the metallic surface were observed. At higher accelerating voltages a greater appearance of depth could be seen but there was less information on the fine surface detail and its angular orientation. The combined technique of HC-BSE imaging and stereo imaging should be useful for detailed studies on material surfaces and for biological samples with greater contrast and directional sensitivity than can be obtained with current SE or BSE detection modes.     

磷在2.25CrlMo钢中的非平衡晶界偏聚动力学实验

采用2.25Cr1Mo工业用钢,通过俄歇电子能谱分析方法(AES),对磷在1050℃固溶处理、540℃恒温保持过程中的非平衡晶界偏聚浓度进行了测试,获得了磷在钢中的非平衡晶界偏聚动力学曲线,该曲线直接验证了非平衡晶界偏聚动力学理论中的Xu-Song模型。     

采用EBSD技术分析热浸镀铝层的显微组织

采用热浸镀方法在Q235钢板表面制备了镀铝层,通过扫描电镜观察了镀铝层的微观形貌,利用电子背散射衍射技术分析了镀铝层/基体界面的相分布、晶粒微观取向以及晶粒尺寸。结果表明:镀铝层的相组成包括最外层的铝和靠近基体的Fe2Al5,其中柱状Fe2Al5随浸镀时间的延长而逐渐长大;铁和铝扩散速率的不同导致镀铝层中形成一些孔洞;Fe2Al5晶粒优先选择沿着扩散方向从镀铝层表面向基体内部生长,导致镀铝层界面不均匀生长而形成舌型柱状晶;界面处基体中α-Fe的晶粒取向是随机分布的,并未受浸镀时扩散反应的影响;Fe2Al5柱状晶内部存在一些小于5°的小角度晶界;Fe2Al5晶粒的平均直径约为20μm,而基体中α-Fe的约为8μm。