A preliminary electron backscattered diffraction study of sintered NdFeB-type magnets

This paper reports, for the first time, the use of electron backscattered diffraction (EBSD) to study orientation in sintered NdFeB type magnets. The magnetic properties of NdFeB magnets are greatly improved if a strong crystallographic texture is firstly achieved, namely, the direction of the c‐axis is along the direction of magnetization. A systematic survey of sample preparation techniques showed that samples that were mechanically polished and then etched gave the most reliable EBSD data. Analyses were made using both fully automated EBSD scans and by EBSD measurements taken after manual movement of the beam. The EBSD results are presented as secondary electron SEM micrographs, orientation images and 001 pole figures. For the selection of grains investigated, the deviation of the c‐axis was shown to be between 10° and 30° from the ideal [001]//magnetization direction. It is demonstrated that EBSD is a valuable tool for characterizing the microstructure and texture relationships and for assessing the performance of the processing routes of NdFeB magnets.     

Characterizing the deformed state in Al-0.1 Mg alloy using high-resolution electron backscattered diffraction

The application of high resolution electron backscatter diffraction (EBSD) in a field emission gun scanning electron microscope to the characterization of a deformed aluminium alloy is discussed and the results are compared with those obtained by transmission electron microscopy. It is shown that the adequate spatial resolution, accompanied by the improvement in angular resolution to ~0.5° that can be achieved by data processing, together with the extensive quantitative data obtainable, make EBSD a suitable method for characterizing the cell or subgrain structures in deformed aluminium. The various methods of analysing EBSD data to obtain subgrain sizes are discussed and it is concluded that absolute subgrain reconstruction is the most accurate.     

'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.     

Quantitative metallography by electron backscattered diffraction

Although electron backscattered diffraction (EBSD) in the scanning electron microscope is used mainly to investigate the relationship between local textures and microstructures, the technique has now developed to the stage where it requires serious consideration as a tool for routine quantitative characterization of microstructures. This paper examines the application of EBSD to the characterization of phase distributions, grain and subgrain structures and also textures. Comparisons are made with the standard methods of quantitative metallography and it is shown that in many cases EBSD can produce more accurate and detailed measurements than the standard methods and that the data may sometimes be obtained more rapidly. The factors which currently limit the use of EBSD for quantitative microstructural characterization, including the speed of data acquisition and the angular and spatial resolutions, are discussed, and future developments are considered.     

Progressive steps in the development of electron backscatter diffraction and orientation imaging microscopy

Ten years ago electron backscatter diffraction (EBSD) became available to a wider group active in materials research. This paper highlights some of the more significant developments in camera technology and software developments that have arisen since then. The use of slow‐scan charge couple device cameras for phase identification and rapid determination of orientation image micrographs is reviewed. The current limiting spatial resolution of the technique is shown to be less than 10 nm. A procedure for improving lattice spacing measurement by utilizing the full resolution of the camera is described with experimental measurements on silicon and nickel showing relative errors of plus/minus 3%. An investigation of partially recrystallized aluminium shows how the recrystallized fraction can be extracted with confidence but that the mapping of substructure in the highly deformed regions is questionable. Phase identification is described for complex cases in which the phase data tabulated in standard databases do not correspond to what is observed in the EBSD patterns. Phase mapping in a complex mineral in which chemical data and EBSD data are collected simultaneously is shown to be improved by recording both the chemical and the EBSD data into computer memory and proceeding with the phase discrimination and orientation measurement in off‐line analysis.     

Practical method for noise removal in scanning electron microscopy

A new smoothing filter has been developed for noise removal of scanning electron microscopy (SEM) images. We call this the complex hysteresis smoothing (CHS) filter. It is much easier to use for SEM operators than any other conventional smoothing filter, and it rarely produces processing artifacts because it does not utilize a definite mask (which usually has processing parameters of size, shape, weight, and the number of iterations) like a common averaging filter or a complicated filter shape in the Fourier domain. Its criterion for distinguishing noise depends simply on the amplitude of the SEM signal. When applied to several images with different characteristics, it is shown that the present method has a high performance with some original advantages.     

Microstructural and microtextural characterization of oxide scale on steel using electron backscatter diffraction

High‐temperature oxidation of steel has been extensively studied. The microstructure of iron oxides is, however, not well understood because of the difficulty in imaging it using conventional methods, such as optical or electron microscopy. A knowledge of the oxide microstructure and texture is critical in understanding how the oxide film behaves during high‐temperature deformation of steels and more importantly how it can be removed following processing. Recently, electron back‐scatter diffraction (EBSD) has proved to be a powerful technique for distinguishing the different phases in scales. This technique gives valuable information both on the microstructure and on the orientation relationships between the steel and the scale layers. In the current study EBSD has been used to investigate the microstructure and microtexture of iron oxide layers grown on interstitial free steel at different times and temperatures. Heat treatments have been carried out under normal oxidation conditions in order to relate the results to real steel manufacturing in industry. The composition, morphologies, microstructure and microtexture of selected conditions have been studied using EBSD.     

Phase identification of individual crystalline particles by electron backscatter diffraction

Recently, an electron backscatter diffraction (EBSD) system was developed that uses a 1024 × 1024 CCD camera coupled to a thin phosphor. This camera has been shown to produce excellent EBSD patterns. In this system, crystallographic information is determined from the EBSD pattern and coupled with the elemental information from energy or wavelength dispersive X-ray spectrometry. Identification of the crystalline phase of a sample is then made through a link to a commercial diffraction database. To date, this system has been applied almost exclusively to conventional, bulk samples that have been polished to a flat surface. In this investigation, we report on the application of the EBSD system to the phase identification analysis of individual micrometre and submicrometre particles rather than flat surfaces.     

Motor current signature analysis via four-channel FIR filter banks

Motor current signature analysis (MCSA) is capable of providing continuous monitoring of induction motors in a non-intrusive manner. Fourier based techniques have been used widely in processing of stator current but these techniques have a shortcoming in processing non-stationary signals such as the stator current. Recently, wavelet packet decomposition (WPD) has become popular in such applications since it gives better results in the case of non-stationary signals. The latter approach has much higher computational complexity limiting its use in motor diagnostics applications. In this study, the use of four-channel FIR filter banks is proposed to provide lower computational complexity. Four-channel filter banks employ higher level of parallel processing than currently used two-channel filter banks. FPGA implementation of the proposed algorithm would result in even further reduction in overall computation time.     

Low-angle subgrain misorientations in deformed NaCl

The development of subgrain boundary misorientations with strain in NaCl polycrystals has been investigated. At low strains, a power law relationship exists between strain and average misorientations. The accuracy of this relationship is assessed in terms of material and electron backscattered diffraction (EBSD) processing parameters and is found to hold for a material of constant grain size deformed in compression, providing EBSD mapping and processing conditions were similar. Average misorientations are strongly influenced by grain orientation, suggesting that the misorientation–strain relationship may also be texture dependent in materials with high plastic anisotropy. A slight grain size dependency of the average misorientations was observed.     

The role of misorientation and phosphorus content on grain growth and intergranular fracture in iron–carbon–phosphorus alloys

The relationship between the crystallography of intergranular fracture and phosphorus segregation has been investigated in a Fe?0.06wt%P?0.002wt%C alloy aged for 1 h at temperatures between 600 °C and 1000 °C. Two novel techniques were devised for the investigation: first, electron back‐scatter diffraction (EBSD) across the reconstructed fracture surface and, second, a combination of Auger electron spectroscopy, stereophotogrammetry and microscopy to measure phosphorus and carbon on fracture facets combined with EBSD measurements direct from the fracture surface. In total, 700 misorientations were measured from across the reconstructed fracture surface and in ‘control’ areas away from the fracture. It was found that Σ 3s were in general more resistant to brittle fracture than were random boundaries, and it was suggested that alloys of this type could be grain boundary engineered to improve fracture resistance by a short anneal in the austenite region to increase the final proportion of Σ 3s. Sixteen fracture facets yielded combined Auger/EBSD data. The combined Auger/EBSD methodology to acquire joint crystallographic and segregation information from facets was shown to be feasible, although laborious. There were significantly more {110} planes than any other type in the sample population of facets from which combined segregation/crystallography data had been collected. The data suggested that there was on average lower phosphorus segregation on fracture facets that were near {110} than on other intergranular fracture facets.     

Use of an energy filter to improve the spatial resolution of electron backscatter diffraction

The electron backscatter diffraction (EBSD) analytical technique is invaluable for determining the crystallography of bulk alloys, thin films, and nanoparticles. However, our physical understanding of EBSD pattern generation is incomplete, which hinders our ability to push the limits of EBSD analysis. Here, by using an energy filter with better than 10 eV resolution, an improvement in the spatial resolution of the EBSD pattern was experimentally demonstrated. A signal depth of less than 15 nm for an aluminum film was achieved by controlling the cutoff energy of the energy filter. Additionally, a two‐fold improvement in the spatial resolution across a grain boundary was observed using the energy filter. SCANNING 31: 114–121, 2009. © 2009 Wiley Periodicals, Inc.     

The application of a hot deformation SEM stage, backscattered electron imaging and EBSD to the study of thermomechanical processing

The technique of combining in situ hot‐deformation and high resolution electron backscattered diffraction (EBSD) has been applied to study the mechanisms operating during the thermomechanical processing of metals. A simple hot tensile‐straining stage is installed in a field emission gun scanning electron microscope equipped with an EBSD system and has been used successfully for a number of preliminary investigations. These investigations include substructure formation, dynamic subgrain and grain growth, superplastic deformation in aluminium alloys, and dynamic recrystallization in copper. Despite the surface topography, which inevitably increases during plastic deformation, channelling contrast backscattered electron micrographs have been successfully obtained after strains of up to ～50%. Good quality EBSD maps have been obtained after strains of up to 100%. Most observations and measurements from the in situ experiments are consistent with what is known about the mechanisms occurring in the bulk. The microstructures revealed in the centre of the in situ samples after later repolishing are generally similar to those at the surface.     

Energy-filtered electron backscatter diffraction

The electron backscatter diffraction (EBSD) analytical technique is invaluable for determining the crystallography of bulk alloys, thin films, and nanoparticles. However, our physical understanding of EBSD pattern generation is incomplete, which hinders our ability to push the limits of EBSD analysis. Here, using an energy filter with better than 10 eV resolution, we experimentally demonstrate the energy dependence of EBSD patterns from elements over a large atomic number range. We verify that low-loss electrons are the major contributors to EBSD patterns, but that there is still a diffraction contribution from electrons with only 80% of the incident beam energy. Additionally, the bands in filtered EBSD patterns have contrast that is more than twice the contrast of their unfiltered counterparts. The band contrast reaches a maximum for a cutoff energy in the filter of about 3% below the energy of the incident beam. Different mechanisms are used to explain the drop in contrast on each side of the maximum. With the cutoff set very close to the energy of the incident beam, the patterns become more blurred. We used a Monte Carlo simulation in the analysis of these experiments.     

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.     

The degradation of EBSD-patterns as a tool to investigate surface crystallized glasses and to identify glassy surface layers

Surface crystallized samples of glass-ceramics containing cordierite, rhombohedral BaAl₂B₂O₇ and fresnoite were analyzed using electron backscatter diffraction (EBSD). The first two materials were chosen because surface crystallized samples of these materials have previously been shown to contain crystals covered by a very thin layer of glass. In all materials, EBSD pattern degradation occurs if the step size of a scan is chosen to be small. It is shown that the minimum step size enabling an evaluable EBSD-scan increases notably, if the crystals are covered by a thin layer of glass. It is also shown that pattern degradation may be utilized to prove the existence of such a thin glass or otherwise thermally sensitive layer. This provides significant information concerning the nucleation process of glasses also with respect to nucleation theory of glass-ceramics. It is also possible to describe the quantity of crystalline surface covered by the thermally sensitive layer.     

High resolution surface morphology measurements using EBSD cross-correlation techniques and AFM

The surface morphology surrounding wedge indentations in (0 0 1) Si has been measured using electron backscattered diffraction (EBSD) and atomic force microscopy (AFM). EBSD measurement of the lattice displacement field relative to a strain-free reference location allowed the surface uplift to be measured by summation of lattice rotations about the indentation axis. AFM was used in intermittent contact mode to determine surface morphology. The height profiles across the indentations for the two techniques agreed within 1 nm. Elastic uplift theory is used to model the data.     

The characterization of low-angle boundaries by EBSD

A method of accurately measuring misorientations by electron backscatter diffraction (EBSD), which is an extension of that proposed by Wilkinson and based on the comparison of diffraction patterns, is described. The method has been applied to linescans, and found to improve the angular resolution by a factor of more than 30. The consequent improvement in determining misorientation axes is also analysed. Small changes of orientation very close to some low-angle boundaries were investigated and found to be artefacts of the analysis. Measurements of the area from which diffraction patterns are generated show this to be much larger than the effective spatial resolution of EBSD, and it is concluded that this may be a limiting factor in the use of EBSD for microstructural characterization.     

Misorientation distributions in hot deformed NaCl using electron backscattered diffraction

EBSD orientation mapping has been used to derive subgrain boundary misorientation distributions in a series of hot deformed and etched NaCl samples. The main objective of this study has been to examine the influence of data processing, noise caused by angular resolution limits and step size on the subgrain misorientation distributions in hot deformed NaCl. Processing of non‐indexed EBSD patterns increased the average misorientations in etched NaCl. Noise contributed significantly to low angle misorientation peaks for step sizes less than the minimum subgrain size. Orientation data collected using a step size larger than the average subgrain size cumulated misorientations across individual subgrains and effectively measured an orientation gradient between steps. Orientation gradient distributions were not influenced by noise. Average misorientation values calculated from large step data correlated well with average misorientation from small step size data. Average misorientations showed a power law relationship with strain. Three types of substructures were identified using scanning electron microscopy and EBSD mapping, equiaxed subgrains, long subgrain boundaries and a core‐mantle subgrain arrangement.