Correlative microscopy approaches offer synergistic solutions to many research problems. One such combination, that has been studied in limited detail, is the use of atom probe tomography (APT) and transmission Kikuchi diffraction (TKD) on the same tip specimen. By combining these two powerful microscopy techniques, the microstructure of important engineering alloys can be studied in greater detail. For the first time, the accuracy of crystallographic measurements made using APT will be independently verified using TKD. Experimental data from two atom probe tips, one a nanocrystalline Al–0.5Ag alloy specimen collected on a straight flight-path atom probe and the other a high purity Mo specimen collected on a reflectron-fitted instrument, will be compared. We find that the average minimum misorientation angle, calculated from calibrated atom probe reconstructions with two different pole combinations, deviate 0.7° and 1.4°, respectively, from the TKD results. The type of atom probe and experimental conditions appear to have some impact on this accuracy and the reconstruction and measurement procedures are likely to contribute further to degradation in angular resolution. The challenges and implications of this correlative approach will also be discussed.

Using an in situ load frame within a scanning electron microscope, a microstructural section on the surface of an annealed tantalum (Ta) polycrystalline specimen was mapped at successive tensile strain intervals, up to ~20% strain, using electron backscatter diffraction. A grain identification and correlation technique was developed for characterizing the evolving microstructure during loading. Presenting the correlated results builds on the reference orientation deviation (ROD) map concept where individual orientation measurements within a grain are compared with a reference orientation associated with that grain. In this case, individual orientation measurements in a deformed grain are measured relative to a reference orientation derived from the undeformed (initial) configuration rather than the current deformed configuration as has been done for previous ROD schemes. Using this technique helps reveal the evolution of crystallographic orientation gradients and development of deformation-induced substructure within grains. Although overall crystallographic texture evolved slowly during deformation, orientation spread within grains developed quickly. In some locations, misorientation relative to the original orientation of a grain exceeded 20° by 15% strain. The largest orientation changes often appeared near grain boundaries suggesting that these regions were preferred locations for the initial development of subgrains.

Cast AZ31B-H24 magnesium alloy, comprising Mg with 3.27 wt% Al and 0.96 wt% Zn, was cold rolled and subsequently annealed. Global texture evolutions in the specimens were observed by X-ray diffractometry after the thermomechanical processing. Image-based microstructure and texture for the deformed, recrystallized, and grown grains were observed by electron backscattered diffractometry. Recrystallized grains could be distinguished from deformed ones by analyzing grain orientation spread. Split basal texture of ca. ±10–15° in the rolling direction was observed in the cold-rolled sample. Recrystallized grains had widely spread basal poles at nucleation stage; strong {0001} basal texture developed with grain growth during annealing.

Electron backscatter diffraction (EBSD) is a powerful technique for surface microstructure analysis. EBSD analysis of cubic yttria-stabilized zirconia (YSZ) is demonstrated. The statistics related to EBSD indexing reliability shows that the probability of accurate grain orientation detection increased significantly when the electron beam energy was increased from 10 to 30 kV. As a result of better sampling with increased interaction volume, a disparity between local and average grain misorientation angle also exhibited the dependence of the electron beam energy to determine the accuracy of grain orientation. To study EBSD indexing reliability as a function of surface roughness and overlayer formation, rapid EBSD measurement tests were performed on (a) YSZ surfaces ion-polished at ion beam energies of 65 nA at 30 kV and 1 nA at 30 kV and (b) carbon-coated versus uncoated YSZ surfaces. The EBSD results at both 10 and 30 kV electron beam energies indicate that EBSD indexing reliability is negatively affected by higher ion beam milling current and amorphous overlayer formation.

The ability to map plastic deformation around high strain gradient microstructural features is central in studying phenomena such as fatigue and stress corrosion cracking. A method for the visualization of plastic deformation in electron back-scattered diffraction (EBSD) data has been developed and is described in this article. This technique is based on mapping the intragrain misorientation in polycrystalline metals. The algorithm maps the scalar misorientation between a local minimum misorientation reference pixel and every other pixel within an individual grain. A map around the corner of a Vickers indentation in 304 stainless steel was used as a test case. Several algorithms for EBSD mapping were then applied to the deformation distributions around air fatigue and stress corrosion cracks in 304 stainless steel. Using this technique, clear visualization of a deformation zone around high strain gradient microstructural features (crack tips, indentations, etc.) is possible with standard EBSD data.

The boundary parameters between contacting spherical bcc-Fe particles have been characterized with the Large Angle Convergent Beam Electron Diffraction (LACBED) technique. The average accuracy of measurements can reach 0.07°. The rotation parameters are interpreted using matrix algebra and evaluated according to the CSL model. The deviation between the experimental results and the reference misorientations given in the CSL model is determined. It is possible to reveal preferential misorientations between irregularly shaped particles with a size less than 100 nm. The method can be applied to nanoparticles and nanocrystalline materials with a wide range of grain orientations, and it is possible to modify it into an automatic method for TEM measurements.