Site-specific specimen preparation for atom probe tomography (APT) is a challenging task. Small features need to be located using a suitable imaging technique and captured within a volume of less than 0.01 μm3. Correlative microscopy has shown to be helpful for target preparation as well as to gain complementary information about the material. Current strategies developed in that direction can be highly time-consuming and not always ensure the correct site extraction in complex microstructures. In this work, we present a methodology to study grain boundaries and interfaces in martensitic steels by combining electron backscattered diffraction, transmission Kikuchi diffraction (TKD), and APT. Furthermore, we include the design of a sample holder that allows to perform TKD and scanning transmission electron microscopy on the specimen during preparation without breaking the vacuum of the scanning electron microscope/focused ion beam workstation. We show a case study where a prior austenite grain boundary is traced from the bulk material to the apex of the APT specimen. The presence of contamination due to the specimen exposure to the electron beam and the use of plasma cleaning to minimize it are discussed.

Plasma focused ion beam microscopy (PFIB) is a recent nanofabrication technique that is suitable for site-specific atom probe sample preparation. Higher milling rates and fewer artifacts make it superior to Ga+ FIBs for the preparation of samples where large volumes of material must be removed, for example, when trying to avoid lift-out techniques. Transmission Kikuchi diffraction (TKD) is a method that has facilitated phase identification and crystallographic measurements in such electron transparent samples. We propose a procedure for preparing atom probe tomography (APT) tips from mechanically prepared ribbons by using PFIB. This is highly suitable for the preparation of atom probe tips of interfaces such as interphase boundaries from challenging materials where lift-out tips easily fracture. Our method, in combination with TKD, allows the positioning of regions of interest such as interfaces close to the apex of the tip. We showcase the efficacy of the proposed method in a case study on Alloy 718, where the interface between γ-matrix and δ-phase has not been yet extensively explored through APT due to preparation challenges. Results show depletion of γ″-precipitates near the γ/δ interface. A quantitative evaluation of the composition of phases in the bulk versus near the interface is achieved.

Two advanced, automated crystal orientation mapping techniques suited for nanocrystalline materials—precession electron diffraction (PED) in transmission electron microscopy (TEM) and on-axis transmission Kikuchi diffraction (TKD) in scanning electron microscopy (SEM)—are evaluated by comparing the orientation maps obtained from the identical location on a 30 nm-thick nanocrystalline tungsten (W) thin film. A side-by-side comparison of the orientation maps directly showed that the large-scale orientation features are almost identical. However, there are differences in the fine details, which arise from the fundamentally different nature of the spot pattern and Kikuchi line pattern in terms of the excitation volume and the angular resolution. While TEM-PED is more reliable to characterize grains oriented along low-index zone axes, the high angular resolution of SEM-TKD allows the detection of small misorientation between grains and thus yields better quantification and statistical analysis of grain orientation. Given that both TEM-PED and SEM-TKD orientation mapping techniques are complementary tools for nanocrystalline materials, one can be favorably selected depending on the requirements of the analysis, as they have competitive performance in terms of angular resolution and texture quantification.

The finding of this study is that the interaction volume in electron microscopy in transmission is well ordered laterally, with a remarkable and unexpected consequence being that lateral subsections of the interaction volume produce subsections of the Kikuchi diffraction pattern. It makes the microstructure of samples directly visible in Kikuchi patterns. This is first illustrated with polycrystalline Ti–10Al–25Nb with an on-axis transmission Kikuchi diffraction set-up in a scanning electron microscope. It is then shown via a Monte Carlo simulation and a large-angle convergent-beam electron diffraction experiment that this phenomenon finds its origin in the nature of the differential elastic and quasi-elastic cross sections. This phenomenon is then quantified by a careful image analysis of Kikuchi patterns recorded across a vertical interface in a silicon sample specifically designed and fabricated. A Monte Carlo simulation reproducing all the geometric parameters is conducted. Experiments and simulations match very well qualitatively, but with a slight quantitativity gap. The specificity of the thermal diffuse scattering cross-section, not available in the simulation, is thought to be responsible for this gap. Beside Kikuchi diffraction, the case of diffraction spots and diffuse background present in the pattern is also discussed.

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.

Electron backscatter diffraction (EBSD) is a micro-analytical technique typically attached to a scanning electron microscope (SEM). The vast majority of EBSD measurements is applied to planar and polished surfaces of polycrystalline bulk specimen. In this paper, we present examples of using EBSD and energy-dispersive X-ray spectroscopy (EDX) to analyze specimens that are not flat, not planar, or not bulk – but pillars, needles, and rods. The benefits of low vacuum SEM operation to reduced drift problems are displayed. It is further demonstrated that small and thin specimens enhance the attainable spatial resolution for orientation mapping (by EBSD or transmission Kikuchi diffraction) as well as for element mapping (by EDX).