'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.     

The preferred CSL misorientation distribution in polycrystalline SrTiO3

Electron backscattered diffraction is used to investigate the preferred CSL (coincidence site lattice) distribution of polycrystalline SrTiO₃ as a function of annealing times (1 h and 16 h). Comparison of the CSL misorientations suggests that the CSL boundary energy plays a role in the preferred grain growth.     

Extracting twins from orientation imaging microscopy scan data

Automated electron backscatter diffraction or orientation imaging microscopy (OIM) provides spatially specific measurements of crystallographic orientation. These measurements are typically collected on regular grids. By inspecting the misorientation between neighbouring measurements on the grid, potential twin boundaries can be identified. If the misorientation is within some given tolerance of a specified twin misorientation, the boundary separating the two measurements may be identified as a potential twin boundary. In addition, for a coherent twin, the twinning planes must be coincident with the grain boundary plane. As OIM scans are inherently two‐dimensional, the scan data provide only limited information on the boundary plane. Thus, it is not possible to ascertain definitively whether the twinning planes are coincident with the boundary plane. Nonetheless, the alignment of the surface traces of the twinning planes with the trace of the boundary provides a partial indication of coincidence. An automated approach has been developed that allows data concerning both twin criterion to be extracted from OIM scans. Application of the methodology to deformed zirconium suggests that the twinning planes remain coherent during deformation. The methodology was also used to improve grain size distributions measured by OIM. These results more closely match those obtained by conventional metallography.     

Calibration of an electron back-scattering pattern set-up

The determination of lattice orientations from electron back-scattering patterns (EBSPs) in a scanning electron microscope (SEM) requires accurate knowledge of the position of the pattern centre and the source point to screen distance. This paper outlines a new procedure that enables the determination of these parameters for any given set-up of the EBSP/SEM system. The calibration procedure simply requires the positions and indices of at least four poles in a pattern obtained from an arbitrary specimen, and eliminates the need for standard specimens or special attachments to the EBSP/SEM system. The pattern centre is shown to be located with a precision of approximately 0·5° and the source point to screen distance can be determined with a relative precision of approximately 0·5%.     

New developments in the characterization of dislocation loops from LACBED patterns

The characterization of the Burgers vector of dislocations from large‐angle convergent‐beam electron diffraction (LACBED) patterns is now a well‐established method. The method has already been applied to relatively large and isolated dislocation loops in semiconductors. Nevertheless, some severe experimental difficulties are encountered with small dislocation loops. By using a 2 µm selected‐area aperture and a carbon contamination point to mark the loop of interest, we were able to characterize both the plane and the Burgers vector of dislocation loops of a few tens of nanometres in size present in Al‐Cu‐Mg alloys.     

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.     

CBED and LACBED characterization of crystal defects

Convergent‐beam electron diffraction (CBED) obtained with a focused incident beam is well known for the identification of the point and space groups but it can also be used for the analysis of stacking faults and antiphase boundaries. Large‐angle convergent‐beam electron diffraction (LACBED) is performed with a large defocused incident beam and is well adapted to the characterization of most types of crystal defects: point defects, perfect and partial dislocations, stacking faults, antiphase boundaries and grain boundaries. Among the advantages of these methods with respect to the conventional transmission electron microscopy methods, are that one or few patterns are required for a full analysis and the interpretations are easy and unambiguous. The LACBED technique is particularly useful for the analysis of dislocations present in anisotropic and beam‐sensitive materials.     

Towards sub-A atomic resolution electron diffraction imaging of metallic nanoclusters: a simulation study of experimental parameters and reconstruction algorithms

A simulation study is carried out to elucidate the effects of dynamical scattering, electron beam convergence angle and detection noise on atomic resolution diffraction imaging of small particles and to develop effective reconstruction procedures. Au nanoclusters are used as model because of their strong scattering. The results show that the dynamical effects of electron diffraction place a limit on the size of Au nanoclusters that can be reconstructed from the diffraction intensities with sufficient accuracy. For smaller Au nanoclusters, the simulations show that diffraction patterns recorded under the experimental conditions can be reconstructed using a combination of phase retrieval algorithms. The use of a low-resolution image is shown to be effective for reconstructing diffraction patterns without the central beam. A new algorithm for estimating the object support is proposed.     

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.     

Scanning electron microscopy and transmission electron microscopy in situ studies of grain boundary migration in cold-deformed aluminium bicrystals

The crystallography of recrystallization has been investigated in channel‐die deformed pure aluminium bicrystals with {100}<011>/{110}<001> orientations. The microstructural and microtextural changes during the early stages of recrystallization were followed by systematic local orientation measurements using scanning and transmission electron microscopes. In particular, orientation mapping combined with in situ sample heating was used to investigate the formation and growth of new grains at very early stages of recrystallization. Grain boundary migration and ‘consumption’ of the as‐deformed areas was always favoured along directions parallel to the traces of the {111} slip planes that had been most active during deformation.