Problems in determining the misorientation axes, for small angular misorientations, using electron backscatter diffraction in the SEM

The errors associated with calculating misorientation axes from electron backscatter diffraction (EBSD) data have been assessed experimentally. EBSD measurements were made on the same grains after imposed rotations of 2°, 5°, 7°, 10°, 12°, 17°, 27° and 180° around the normal to the specimen surface. The misorientation magnitudes and the misorientation axes associated with the imposed rotations have been calculated from the EBSD data. Individual measurements of misorientation axes are precise for misorientation magnitudes greater than ≈ 20°. The errors must be appreciated when assessing misorientation data at lower misorientation magnitudes and particularly at magnitudes less than 5°. Where misorientation axes can be characterized by the distribution of axes from a number of individual measurements, current EBSD techniques are satisfactory, for data sets of 30 measurements, as long as misorientation magnitudes are 10° or more. With larger data sets it may be possible to extend this approach to smaller misorientation magnitudes. For characterization of individual misorientations less than 5°, new EBSD techniques need to be developed.     

Crystallographic analysis of facets using electron backscatter diffraction

Applications of electron backscatter diffraction (EBSD), also known as backscatter Kikuchi diffraction in the scanning electron microscope (SEM) are first and foremost microtexture and grain boundary misorientation analysis on a single polished section in the specimen. A more subtle and revealing approach to analysis of these data is to use EBSD to probe the orientations of planar surfaces, i.e. facets, which bound crystals. These surfaces include: • grain or phase boundaries • fractures • cracks It is of great interest to know the crystallography of such facets since it provides a key to understanding the physical properties of them.
As far as investigation methodology is concerned, surfaces or facets associated with polycrystals are of two types: exposed or unexposed. Exposed facets, such as a fracture surface, can be viewed directly in the SEM, whereas unexposed facets, such as a grain boundary, are usually revealed as an etched trace on a polished surface. Photogrammetric methods can be used to obtain the positional orientation of an exposed facet, and the crystallographic orientation is obtained either directly from the surface or by indirect sectioning. Calibrated sectioning is required to obtain the equivalent parameters for an internal surface. The present paper compares the methods for obtaining and interpreting the crystallography of facets, with illustrations from several materials.     

Crystallographic preferred orientation (CPO) of gypsum measured by electron backscatter diffraction (EBSD)

An investigation by electron backscatter diffraction on gypsum shows that this technique can be used to study the microstructures and crystallographic preferred orientation of gypsum. Presented here are the methods, verification tests and data obtained from a naturally deformed sample of gypsum‐rich rock. The electron backscatter diffraction data show the sample has a strong crystallographic preferred orientation.     

Crystallographic Characteristic of Intermetallic Compounds in Al-Si-Mg Casting Alloys Using Electron Backscatter Diffraction

The Al-Si-Mg alloy which can be strengthened by heat treatment is widely applied to the key components of aerospace and aeronautics. Iron-rich intermetallic compounds are well known to be strongly influential on mechanical properties in Al-Si-Mg alloys. But intermetallic compounds in cast Al-Si-Mg alloy intermetallics are often misidentified in previous metallurgical studies. It was described as many different compounds, such as AlFeSi, Al8Fe2Si, Al5(Fe, Mn)3Si2 and so on. For the purpose of solving this problem, the intermetallic compounds in cast Al-Si alloys containing 0.5% Mg were investigated in this study. The iron-rich compounds in Al-Si-Mg casting alloys were characterized by optical microscope(OM), scanning electron microscope(SEM), energy dispersive X-ray spectrometer(EDS), electron backscatter diffraction(EBSD) and X-ray powder diffraction(XRD). The electron backscatter diffraction patterns were used to assess the crystallographic characteristics of intermetallic compounds. The compound which contains Fe/Mg-rich particles with coarse morphologies was Al8FeMg3Si6 in the alloy by using EBSD. The compound belongs to hexagonal system, space group P2m, with the lattice parameter a=0.662 nm, c=0.792 nm. The β-phase is indexed as tetragonal Al3FeSi2, space group I4/mcm, a=0.607 nm and c=0.950 nm. The XRD data indicate that Al8FeMg3Si6 and Al3FeSi2 are present in the microstructure of Al-7Si-Mg alloy, which confirms the identification result of EBSD. The present study identified the iron-rich compound in Al-Si-Mg alloy, which provides a reliable method to identify the intermetallic compounds in short time in Al-Si-Mg alloy. Study results are helpful for identification of complex compounds in alloys.     

Comparison of convergent beam electron diffraction and geometric phase analysis for strain measurement in a strained silicon device

Convergent beam electron diffraction and geometric phase analysis were used to measure strain in the gate channel of a p-type strained silicon metal-oxide-semiconductor field-effect transistor. These measurements were made on exactly the same transmission electron microscopy specimen allowing for direct comparison of the relative advantages of each technique. The trends in the strain values show good agreement in both the [110] and [001] directions, but the absolute strain values are offset from each other. This difference in the absolute strain measured using the two techniques is attributed to the way the reference strain is defined for each.     

Analysis of Kikuchi band contrast reversal in electron backscatter diffraction patterns of silicon

We analyze the contrast reversal of Kikuchi bands that can be seen in electron backscatter diffraction (EBSD) patterns under specific experimental conditions. The observed effect can be reproduced using dynamical electron diffraction calculations. Two crucial contributions are identified to be at work: First, the incident beam creates a depth distribution of incoherently backscattered electrons which depends on the incidence angle of the beam. Second, the localized inelastic scattering in the outgoing path leads to pronounced anomalous absorption effects for electrons at grazing emission angles, as these electrons have to go through the largest amount of material. We use simple model depth distributions to account for the incident beam effect, and we assume an exit angle dependent effective crystal thickness in the dynamical electron diffraction calculations. Very good agreement is obtained with experimental observations for silicon at 20 keV primary beam energy.     

晶体取向显微成像的应用

扼要介绍LINK OPAL电子背散射衍射技术中的一种全新的图像--晶体取向显微成像图,并讨论晶体取向显微成像技术在钢铁材料研究中的应用。     

Application of electron backscatter diffraction to the study of phase transformations: present and possible future

This paper first underlines the main advantages, use and limitations of the electron backscatter diffraction technique from the viewpoint of phase transformations. To get a deeper understanding of physical mechanisms involved in phase transformations, several evolutions are now in progress to get an insight into both three-dimensional and real-time information. Two of them, in particular, improvement of data collection versus improvement of data processing are discussed in the second part of this paper.     

A novel method for acquiring large-scale automated scanning electron microscope data

Recent software and hardware advances in the field of electron backscatter diffraction have led to an increase in the rate of data acquisition. Combining automated stage movements with conventional beam control have allowed researchers to collect data from significantly larger areas of samples than was previously possible. This paper describes a LabVIEW? and AutoIT^© code which allows for increased flexibility compared to commercially available software. The source code for this software has been made available in the online version of this paper.     

3D visualization and quantification of rat cortical bone porosity using a desktop micro-CT system: a case study in the tibia

Although micro-computed tomography (micro-CT) has become the gold standard for assessing the 3D structure of trabecular bone, its extension to cortical bone microstructure has been relatively limited. Desktop micro-CT has been employed to assess cortical bone porosity of humans, whereas that of smaller animals, such as mice and rats, has thus far only been imaged using synchrotron-based micro-CT. The goal of this study was to determine if it is possible to visualize and quantify rat cortical porosity using desktop micro-CT. Tibiae (n = 10) from 30-week-old female Sprague-Dawley rats were imaged with micro-CT (3 μm nominal resolution) and sequential ground sections were then prepared. Bland-Altman plots were constructed to compare per cent porosity and mean canal diameter from micro-CT (3D) versus histology (2D). The mean difference or bias (histology-micro-CT; ±95% confidence interval) for per cent porosity was found to be -0.15% (±2.57%), which was not significantly different from zero (P= 0.720). Canal diameter had a bias (±95% confidence interval) of -5.73 μm (±4.02 μm) which was found to be significantly different from zero (P < 0.001). The results indicated that cortical porosity in rat bone can indeed be visualized by desktop micro-CT. Quantitative assessment of per cent porosity provided unbiased results, whereas direct analysis of mean canal diameter was overestimated by micro-CT. Thus, although higher resolution, such as that available from synchrotron micro-CT, may ultimately be required for precise geometric measurements, desktop micro-CT--which is far more accessible--is capable of yielding comparable measures of porosity and holds great promise for assessment of the 3D arrangement of cortical porosity in the rat.     

Determination of pattern centre in EBSD using the moving-screen technique

The ‘moving‐screen’ or ‘pattern magnification’ method of calibration for electron backscatter diffraction (EBSD) was reformulated to develop a high‐precision technique requiring no crystallographic knowledge of the specimen and no initial estimates of the calibration parameters. The technique depends upon the accurate displacement of the screen and camera assembly. Corresponding points are selected, interactively, from EBSD patterns. It is suggested that, as an alternative, the selection of points from the Hough transform could lead to a completely automated routine.     

采用电子背散射衍射技术研究变形温度对压缩后1235铝合金织构的影响

采用电子背散射衍射技术对经不同温度热压缩后1235铝合金的织构进行了研究,分析了在50%变形量、0.1s-1应变速率下,变形温度对该合金晶粒取向、晶界特征及织构组分的影响。结果表明:随着变形温度的升高,织构的取向聚集性弱化,织构相对体积总含量降低,晶粒内小角度晶界更稀疏,大角度晶界更加平直且连通性好,再结晶晶粒长大更充分。     

Spatially resolved diffractometry with atomic-column resolution

We demonstrate spatially resolved diffractometry in which diffraction patterns are acquired at two-dimensional positions on a specimen using scanning transmission electron microscopy (STEM), resulting in four-dimensional data acquisition. A high spatial resolution of about 0.1 nm is achieved using a stabilized STEM instrument, a spherical aberration corrector and various post-acquisition data processings. We have found a few novel results in the radial and the azimuthal scattering angle dependences of atomic-column contrast in STEM images. Atomic columns are clearly observed in dark field images obtained using the excess Kikuchi band intensity even in small solid-angle detection. We also find that atomic-column contrasts in dark field images are shifted in the order of a few tens of picometers on changing the azimuthal scattering angle. This experimental result is approximately interpretable on the basis of the impact parameter in Rutherford scattering. Spatially resolved diffractometry provides fundamental knowledge related to various STEM techniques, such as annular dark field (ADF) and annular bright field (ABF) imaging, and it is expected to become an analytical platform for advanced STEM imaging.