Cryogenic EBSD on ice: preserving a stable surface in a low pressure SEM

Naturally deformed ice contains subgrains with characteristic geometries that have recently been identified in etched surfaces using high-resolution light microscopy (LM). The probable slip systems responsible for these subgrain boundary types can be determined using electron backscattered diffraction (EBSD), providing the etch features imaged with reflected LM can be retained during EBSD data acquisition in a scanning electron microscope (SEM). Retention of the etch features requires that the ice surface is stable. Depending on the pressure and temperature, sublimation of ice can occur. The equilibrium temperature for a low pressure SEM operating at 1 × 10(-6) hPa is about -112°C and operating at higher temperatures causes sublimation. Although charging of uncoated ice samples is reduced by sublimation, important information contained in the etch features are removed as the surface sublimes. We developed a method for collecting EBSD data on stable ice surfaces in a low pressure SEM. We found that operating at temperatures of <-112°C reduced sublimation so that the original etch surface features were retained. Charging, which occurred at low pressures (<1.5 × 10(-6) to 2.8 × 10(-5) hPa) was reduced by defocusing the beam. At very low pressures (<1.5 × 10(-6) hPa) the spatial resolution with a defocused beam at 10 kV was about 3 μm in the x-direction at -150°C and 0.5 μm at -120°C, because at higher temperature charging was less and only a small defocus was needed to compensate it. Angular resolution was better than 0.7° after orientation averaging. Excellent agreement was obtained between LM etch features and EBSD mapped microstructures. First results are shown, which indicate subgrain boundary types comprised of basal (tilt and twist) and nonbasal dislocations (tilt boundaries).     

金相图像的晶界恢复与重建

针对定量金相分析中金相图像的晶界恢复与重建以及数学形态学在图像处理中的特殊作用,从理论上证明了传统膨胀运算对图像灰度连续性的影响及影响程度与结构元素尺寸的关系,并对传统的膨胀运算的定义做了改进,据此提出了多尺度测地膨胀算法并以此恢复和重建金相图像的晶界.首先依据改进的膨胀运算对金相图像进行预处理;然后用多尺度迭代腐蚀和...     

Shaping the lens of the atom probe: fabrication of site specific, oriented specimens and application to grain boundary analysis

The random sampling provided by classical atom probe sample preparation methods is one of the major factors limiting the types of problems that can be addressed using this powerful technique. A focused ion beam enables not only site-specific preparation, but can also be used to give the specimen, which acts as the lens in an atom probe experiment, a specific shape. In this paper we present a technique that uses low accelerating voltages (10 and 5 kV) in the focused ion beam (FIB) to reproducibly produce specimens with selected grain boundaries <100 nm from the tip at any desired orientation. These tips have a high rate of successfully running in the atom probe and no Ga contamination within the region of interest.This technique is applied to the analysis of grain boundaries in a high purity iron wire and a strip-cast steel. Lattice resolution is achieved around the boundary in certain areas. Reconstruction of these datasets reveals the distribution of light and heavy elements around the boundary. Issues surrounding the uneven distribution of certain solute elements as a result of field-induced diffusion are discussed.     

Estimation of true dihedral angles and relative grain boundary energies in polycrystals using the disector

Relative grain boundary energies can be simply related to true dihedral angles, which are the angles between grain boundary planes meeting at triple edges in polycrystals. Some limited efforts in the measurement of true dihedral angles have used the technique of serial sectioning, which is usually cumbersome and time consuming. In this study the three‐dimensional probe called the ‘disector’ has been employed to evaluate true dihedral angles. This probe, combined with automated image processing, introduces precision as well as efficiency, overcomes the disadvantages of the two‐dimensional probe and is far less tedious and less complicated than serial sectioning. It is shown that the technique is relatively simple and therefore can be applied to obtain a significantly large and accurate statistical sample of true dihedral angles. The application of this method is demonstrated by evaluating the triple junction geometry and the associated relative grain boundary energies in polycrystalline 316L austenitic stainless steel.     

Inter‐ and intragranular delta phase quantitative characterization in Inconel 718 by means of image analysis

This paper describes an image processing method for discriminating the inter‐ and intragranular delta phase precipitates in Inconel 718 (IN 718). The successive practical operations and the motivations of their choices are presented in detail. The method was applied to IN 718 specimens heat treated with different parameters to produce microstructures containing various amounts of both types of precipitates. They were characterized by electron microscopy in backscattered electron imaging. The main difficulty arose from the fact that the brightness distributions of inter‐ and intragranular precipitates partially overlap. Additional information on their morphology and their spatial distribution had to be exploited in order to differentiate them. The shape and the orientation of the precipitates were evaluated using the structure tensor, an operator that quantifies the directionality of the intensity distribution in an image. The distance between parallel precipitates was also used as an additional property to identify clusters of intragranular precipitates.     

The use of combined cathodoluminescence and EBSD analysis: a case study investigating grain boundary migration mechanisms in quartz

Grain boundary migration is an important mechanism of microstructural modification both in rocks and in metals. Combining detailed cathodoluminescence (CL) and electron backscatter diffraction (EBSD) analysis offers the opportunity to relate directly changes in crystallographic orientation to migrating boundaries. We observe the following features in naturally heated quartz grains from the thermal aureole of the Ballachulish Igneous Complex (Scotland, U.K.): (a) propagation of substructures and twin boundaries in swept areas both parallel and at an angle to the growth direction, (b) development of slightly different crystallographic orientations and new twin boundaries at both the growth interfaces and within the swept area and (c) a gradual change in crystallographic orientation in the direction of growth. All these features are compatible with a growth mechanism in which single atoms are attached and detached both at random and at preferential sites, i.e. crystallographically controlled sites or kinks in boundary ledges. Additionally, strain fields caused by defects and/or trace element incorporation may facilitate nucleation sites for new crystallographic orientations at distinct growth interfaces but also at continuously migrating boundaries. This study illustrates the usefulness of combined CL and EBSD in microprocess analysis. Further work in this direction may provide detailed insight into both the mechanism of static grain growth and the energies and mobilities of boundaries in terms of misorientation and grain boundary plane orientation.     

Validation of a method using Taguchi,response surface,neural network,and genetic algorithm

Piston is one of the important parts for aircraft engine, and the quality of piston affects the efficiency and safety of the engine. This study applies Taguchi method, response surface methodology (RSM), and back-propagation neural networks (BPNN) combining with genetic algorithm (GA) on the quality improvement of piston manufacturing processes to enhance the process yield. The Taguchi parameter design concerns three nominal-the-best specifications, including ring groove diameter specification, inner groove diameter specification, and inner diameter of pistons. Together with five control factors consisting of (1) type of carbon steel, (2) type of cutting fluid, (3) cutting depth, (4) spindle speed, and (5) chuck pressure, the L₂₇(3¹³) orthogonal array was selected for this experiment. Three models: (1) Taguchi model, (2) Taguchi_RSM model, and (3) Taguchi_BPNN_GA model were constructed to find the parameter combinations of five control factors for each model. Confirmation experiments were done for each model and the performances of three models were also compared to indict the enhancement of manufacturing quality of piston.     

A numerical study of the fluid flow and heat transfer around a single row of tubes in a channel using immerse boundary method

The analysis of the time-dependent and two-dimensional fluid flow and heat transfer around a single row of tubes in a channel is performed numerically. Due to its fundamental significance and practical importance, aerodynamic and heat transfer characteristics of tube bundle have been paid great attention by many researchers. In the present study, the immersed boundary method is applied by using a Cartesian grid system. Numerical solution for the governing equations of mass, momentum and energy conservation is obtained with the finite volume method. To validate the numerical approach with the immersed boundary method, the results have been compared with published data. The generation and evolution of vortical structures, wake interactions and their effects on the drag, lift and heat transfer are analyzed at different Reynolds numbers. The effect of hydraulic boundary layer development on the fluid flow and heat transfer is also investigated.     

Three-dimensional morphometry in scanning electron microscopy: a technique for accurate dimensional and angular measurements of microstructures using stereopaired digitized images and digital image analysis

A method for accurate dimensional and angular measurements of microstructures analysed in the scanning electron microscope is described. The method considers central and parallel projections and involves (a) digital image acquisition of stereopaired images from the scanning electron microscope's photodisplay, (b) generation of 3D-image representations, (c) setting of measuring points in the digitized stereopaired images, (d) computation of exact space coordinates ( x / y / z ) from the corresponding point coordinates ( x _L/ y _L; x _R/ y _R), (e) determination of distances and angles between consecutive corresponding points using vector equations, and (f) transfer of computed data into spreadsheets of the data analysis software using dynamic data exchange with simultaneous graphical display of the frequency distribution of variables.
Measurements performed on specimens with known dimensions (grid with 10 μm wide square meshes, polystyrene beads with 0.33 μm diameter) and angles (synthetic crystals of K(Al,Cr)[SO₄], CuSO₄.5H₂O and NaCl) revealed a high accuracy in dimensional as well as angular measurements (total error 1 ± 0.5%).
In Monte Carlo experiments the overall error was found to depend strongly on the size of the measured structure relative to the size of the measurement field (field width).     

Bundles of hexagonally arranged tubules in timothy grass pollen: Detection of a novel pollen component using anhydrous fixation and image analysis techniques in transmission electron microscopy

Pollen from timothy grass (Phleum pratense L.) was subjected to various aqueous and non‐aqueous fixation and preparation protocols for transmission electron microscopy. Only in the cytoplasm of anhydrously prepared pollen grains were conspicuous inclusions observed that range in size from less than 1 μm up to 8 or 10 μm. These bodies have so far not been described in the literature. Higher magnifications show that these inclusions consist of bundles of hexagonally arranged small tubules. In order to obtain details of the ultrastructure of this novel pollen component, TEM micrographs of ultrathin sections of hexagonally arranged tubules were analyzed using Fourier transform techniques of image analysis. It was found that the tubules form groups with quasi‐periodic hexagonal arrangement, with an average centre‐to‐centre spacing between the neighbouring tubules of approximately 42 nm. Individual tubules are formed by 12 or 13 particles. The outer diameter of the tubules ranges between 22 and 24 nm. From our experiments, we conclude that the quasi‐periodic hexagonally arranged tubules forming conspicuous cytoplasmic inclusions in dry timothy grass pollen grains are structurally similar to microtubules.