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.     

Electron backscatter diffraction characterization of inlaid cu lines for interconnect applications

Automated electron backscatter diffraction (EBSD) techniques have been used to characterize the microstructures of thin films for the past decade or so. The recent change in strategy from an aluminum‐based interconnect structure in integrated circuits to one based on copper has necessitated the development of new fabrication procedures. Along with new processes, complete characterization of the microstructures is imperative for improving manufacturability of the Cu interconnect lines and in‐service reliability. Electron backscatter diffraction has been adopted as an important characterization tool in this effort. Cu microstructures vary dramatically as a function of processing conditions, including electroplating bath chemistry, sublayer material, stacking sequence of sublayers, annealing conditions, and line widths and depths. Crystallographic textures and grain size and grain boundary character distributions, all of which may influence manufacturability and reliability of interconnect lines, are ideally characterized using EBSD. The present discussion presents some results showing structural dependence upon processing parameters. In addition, the authors identify an in‐plane orientation preference in inlaid Cu lines {111} normal to the line surface and 〈110〉 aligned with the line direction. This relationship tends to strengthen as the line width decreases.     

The complementary use of electron backscatter diffraction and ion channelling imaging for the characterization of nanotwins

On the example of electrodeposited nickel films, it is shown that unique information on twins with dimensions on the nanoscale can be obtained by suitable combination of ion channelling imaging and electron backscatter diffraction analysis, whereas both (routine) single techniques cannot meet the requirements for analysis of these films. High‐resolution electron backscatter diffraction is inadequate for full characterization of nanotwins, but image quality maps obtained from electron backscatter diffraction at least yield a qualitative estimation of the location and number of nanotwins. Complementing this information with ion channelling imaging provides more representative insights into the microstructure, because it supplements the quantitative investigation of the number and width of twin lamellae with additional crystallographic orientation analysis provided by EBSD. To this end, two methods for adjusting EBSD data based on ion channelling images are proposed. Thorough selection of the complementary techniques opens future perspectives for the investigation of other challenging samples with nanoscale features in the microstructure.     

Is fast mapping good mapping? A review of the benefits of high‐speed orientation mapping using electron backscatter diffraction

Orientation mapping using automated electron backscatter diffraction (EBSD) is now a common technique for characterizing microstructures. Improvements in software and hardware have resulted in high‐speed mapping capabilities above 80 000 points h^?1. For ‘routine’ microstructural analyses of materials such as steel and aluminium (e.g. texture and grain size measurements and high angle boundary characterization), high‐speed orientation mapping is an ideal approach with minimal penalty on the final statistics. However, for the accurate analysis of very low angle boundaries and for routine analyses of more difficult materials (e.g. most rock samples), we advocate a more patient approach to orientation mapping with an emphasis on data accuracy and reliability. It is important that the objectives of any EBSD analysis are carefully considered before starting – in this way the maximum potential of an EBSD system can be achieved.     

Making EBSD on water ice routine

Electron backscatter diffraction (EBSD) on ice is a decade old. We have built upon previous work to select and develop methods of sample preparation and analysis that give >90% success rate in obtaining high‐quality EBSD maps, for the whole surface area (potentially) of low porosity (<15%) water ice samples, including very fine‐grained (<10 μm) and very large (up to 70 mm by 30 mm) samples. We present and explain two new methods of removing frost and providing a damage‐free surface for EBSD: pressure cycle sublimation and ‘ironing’. In general, the pressure cycle sublimation method is preferred as it is easier, faster and does not generate significant artefacts. We measure the thermal effects of sample preparation, transfer and storage procedures and model the likelihood of these modifying sample microstructures. We show results from laboratory ice samples, with a wide range of microstructures, to illustrate effectiveness and limitations of EBSD on ice and its potential applications. The methods we present can be implemented, with a modest investment, on any scanning electron microscope system with EBSD, a cryostage and a variable pressure capability.     

Transmission EBSD from 10 nm domains in a scanning electron microscope

The spatial resolution of electron diffraction within the scanning electron microscope (SEM) has progressed from channelling methods capable of measuring crystallographic characteristics from 10 μm regions to electron backscatter diffraction (EBSD) methods capable of measuring 120 nm particles. Here, we report a new form of low‐energy transmission Kikuchi diffraction, performed in the SEM. Transmission‐EBSD (t‐EBSD) makes use of an EBSD detector and software to capture and analyse the angular intensity variation in large‐angle forward scattering of electrons in transmission, without postspecimen coils. We collected t‐EBSD patterns from Fe–Co nanoparticles of diameter 10 nm and from 40 nm‐thick Ni films with in‐plane grain size 15 nm. The patterns exhibited contrast similar to that seen in EBSD, but are formed in transmission. Monte Carlo scattering simulations showed that in addition to the order of magnitude improvement in spatial resolution from isolated particles, the energy width of the scattered electrons in t‐EBSD is nearly two orders of magnitude narrower than that of conventional EBSD. This new low‐energy transmission diffraction approach builds upon recent progress in achieving unprecedented levels of imaging resolution for materials characterization in the SEM by adding high‐spatial‐resolution analytical capabilities.     

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 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.     

Combined application of electron backscatter diffraction and stereo-photogrammetry in fractography studies

The main aim of this paper is to report on recent experimental developments that have succeeded in combining electron back-scatter diffraction (EBSD) with stereo-photogrammetry, compared with two other methods for study of fracture surfaces, namely visual fractography analysis in the scanning electron microscope (SEM) and EBSD directly from facets. These approaches will be illustrated with data relating to the cleavage plane orientation analysis in a ferritic and C-Mn steel. It is demonstrated that the combined use of EBSD and stereo-photogrammetry represents a significant advance in the methodology for facet crystallography analysis. The results of point counting from fractograph characterization determined that the proportions of intergranular fracture in C-Mn and ferritic steels were 10.4% and 9.4%, respectively. The crystallographic orientation was determined directly from the fracture surface of a ferritic steel sample and produced an orientation distribution with a clear trend towards the {001} plane. A stereo-photogrammetry technique was validated using the known geometry of a Vickers hardness indent. The technique was then successfully employed to measure the macroscopic orientation of individual cleavage facets in the same reference frame as the EBSD measurements. Correlating the results of these measurements indicated that the actual crystallographic orientation of every cleavage facet identified in the steel specimens is {001}.     

Comparison of EBSD patterns simulated by two multislice methods

The extraction of crystallography information from electron backscatter diffraction (EBSD) patterns can be facilitated by diffraction simulations based on the dynamical electron diffraction theory. In this work, the EBSD patterns are successfully simulated by two multislice methods, that is, the real space (RS) method and the revised real space (RRS) method. The calculation results by the two multislice methods are compared and analyzed in detail with respect to different accelerating voltages, Debye–Waller factors and aperture radii. It is found that the RRS method provides a larger view field of the EBSD patterns than that by the RS method under the same calculation conditions. Moreover, the Kikuchi bands of the EBSD patterns obtained by the RRS method have a better match with the experimental patterns than those by the RS method. Especially, the lattice parameters obtained by the RRS method are more accurate than those by the RS method. These results demonstrate that the RRS method is more accurate for simulating the EBSD patterns than the RS method within the accepted computation time.     

Comparison of quartz crystallographic preferred orientations identified with optical fabric analysis,electron backscatter and neutron diffraction techniques

Three techniques are used to measure crystallographic preferred orientations (CPO) in a naturally deformed quartz mylonite: transmitted light cross‐polarized microscopy using an automated fabric analyser, electron backscatter diffraction (EBSD) and neutron diffraction. Pole figure densities attributable to crystal‐plastic deformation are variably recognizable across the techniques, particularly between fabric analyser and diffraction instruments. Although fabric analyser techniques offer rapid acquisition with minimal sample preparation, difficulties may exist when gathering orientation data parallel with the incident beam. Overall, we have found that EBSD and fabric analyser techniques are best suited for studying CPO distributions at the grain scale, where individual orientations can be linked to their source grain or nearest neighbours. Neutron diffraction serves as the best qualitative and quantitative means of estimating the bulk CPO, due to its three‐dimensional data acquisition, greater sample area coverage, and larger sample size. However, a number of sampling methods can be applied to FA and EBSD data to make similar approximations.     

Comparison of three‐dimensional analysis and stereological techniques for quantifying lithium‐ion battery electrode microstructures

Lithium‐ion battery performance is intrinsically linked to electrode microstructure. Quantitative measurement of key structural parameters of lithium‐ion battery electrode microstructures will enable optimization as well as motivate systematic numerical studies for the improvement of battery performance. With the rapid development of 3‐D imaging techniques, quantitative assessment of 3‐D microstructures from 2‐D image sections by stereological methods appears outmoded; however, in spite of the proliferation of tomographic imaging techniques, it remains significantly easier to obtain two‐dimensional (2‐D) data sets. In this study, stereological prediction and three‐dimensional (3‐D) analysis techniques for quantitative assessment of key geometric parameters for characterizing battery electrode microstructures are examined and compared. Lithium‐ion battery electrodes were imaged using synchrotron‐based X‐ray tomographic microscopy. For each electrode sample investigated, stereological analysis was performed on reconstructed 2‐D image sections generated from tomographic imaging, whereas direct 3‐D analysis was performed on reconstructed image volumes. The analysis showed that geometric parameter estimation using 2‐D image sections is bound to be associated with ambiguity and that volume‐based 3‐D characterization of nonconvex, irregular and interconnected particles can be used to more accurately quantify spatially‐dependent parameters, such as tortuosity and pore‐phase connectivity.     

Electron backscatter diffraction of grain and subgrain structures — resolution considerations

Characterization of microstructures containing small grains or low-angle grain boundaries by electron backscattered diffraction (EBSD) is limited by the spatial and angular resolution limits of the technique. It was found that the best effective spatial resolution (60 nm) for aluminium alloys in a tungsten-filament scanning electron microscope (SEM) was obtained for an intermediate probe current which provided a compromise between pattern quality and specimen interaction volume. The same specimens and EBSD equipment when used with a field-emission gun SEM showed an improvement in spatial resolution by a factor of 2–3. For characterizing low-angle boundary microstructures, the precision of determining relative orientations is a limiting factor. It was found that the orientation noise was directly related to the probe current and this was interpreted in terms of the effect of probe current on the quality of the diffraction patterns.     

Microstructural characterization of plasma sprayed Ln2Zr2O7 thermal barrier coatings by electron microscopy methods

The presented article characterized microstructural aspects of thermal barrier coatings (TBCs) analysis using methods of electron microscopy such as electron backscatter diffraction (EBSD), transmission/scanning electron microscopy (S/TEM), and TEM. The analyzed TBC system is based on gadolinium zirconate deposited by air plasma spraying method, and additionally, it was subjected to an oxidation test for 500 hr at a temperature of 1,100°C. Moreover, the morphological characterization of feedstock powder was showed. EBSD analysis revealed the inhomogeneity of feedstock materials in the form of complex phase composition. In the case of deposited coating, this method was used to characterize the crystallite size of zirconate coating and phase composition of thermally grown oxide zone. S/TEM and TEM analysis showed morphological details of this zone but not revealed such phase as perovskite oxide of GdAlO₃ type.     

Study of dynamic grain growth by electron microscopy and EBSD

The effect of hot deformation on fully recrystallized aluminium–copper alloys (Al-4wt%Cu and Al-33wt%Cu) with different volume fractions of CuAl₂ has been studied. The alloys are Zener pinned systems with different superplastic properties. Strain-induced grain growth, observed in both alloys, was quantitatively estimated by means of electron microscopy and EBSD and compared with the rate of static grain growth. Surface marker observations and in situ hot-deformation experiments combined with EBSD were aimed at clarifying the mechanisms responsible for the changes in the deformed microstructures. A sequence of secondary and backscattered electron images and EBSD maps was obtained during in situ SEM deformation with different testing conditions. Overlaying EBSD maps for the Al-4wt%Cu with channelling contrast images showed that grain boundary motion occurred during deformation, creating a layered structure and leading to an increase in size of some grains and shrinkage of others. Of a particular interest are results related to behaviour of CuAl₂ in superplastic Al-33wt%Cu during deformation, including several problems with the use of EBSD in this alloy.     

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).     

Analysis of local orientation gradients in deformed single crystals

Grain fragmentation and local orientation gradients in deformed single crystals are characterized using electron backscatter diffraction (EBSD) to obtain statistically reliable information. Interrogation of the dislocation substructure is accomplished by extracting information gleaned from small point-to-point misorientations as measured by EBSD. Along with an estimate of the geometrically necessary dislocation (GND) content, the point-to-point deviation from an average grain orientation is described by an orientation difference vector defined in Rodrigues space. Mapping of parameters such as GND, and divergence and gradient fields created from analysis of the difference vectors provide an alternative approach to obtain quantitative information and images from EBSD data.     

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.     

Improving EBSD precision by orientation refinement with full pattern matching

We present a comparison of the precision of different approaches for orientation imaging using electron backscatter diffraction (EBSD) in the scanning electron microscope. We have used EBSD to image the internal structure of WC grains, which contain features due to dislocations and subgrains. We compare the conventional, Hough-transform based orientation results from the EBSD system software with results of a high-precision orientation refinement using simulated pattern matching at the full available detector resolution of 640 × 480 pixels. Electron channelling contrast imaging (ECCI) is used to verify the correspondence of qualitative ECCI features with the quantitative orientation data from pattern matching. For the investigated sample, this leads to an estimated pattern matching sensitivity of about 0.5 mrad (0.03°) and a spatial feature resolution of about 100 nm. In order to investigate the alternative approach of postprocessing noisy orientation data, we analyse the effects of two different types of orientation filters. Using reference features in the high-precision pattern matching results for comparison, we find that denoising of orientation data can reduce the spatial resolution, and can lead to the creation of orientation artefacts for crystallographic features near the spatial and orientational resolution limits of EBSD.     

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.