Atom probe tomography (APT) helps elucidate the link between the nanoscale chemical variations and physical properties, but it has a limited structural resolution. Field ion microscopy (FIM), a predecessor technique to APT, is capable of attaining atomic resolution along certain sets of crystallographic planes albeit at the expense of elemental identification. We demonstrate how two commercially available atom probe instruments, one with a straight flight path and one fitted with a reflectron lens, can be used to acquire time-of-flight mass spectrometry data concomitant with a FIM experiment. We outline various experimental protocols making the use of temporal and spatial correlations to best discriminate field-evaporated signals from the large field-ionized background signal, demonstrating an unsophisticated yet efficient data mining strategy to provide this discrimination. We discuss the remaining experimental challenges that need to be addressed, notably concerned with accurate detection and identification of individual field-evaporated ions contained within the high field-ionized flux that contributes to a FIM image. Our hybrid experimental approach can, in principle, exhibit true atomic resolution with elemental discrimination capabilities, neither of which atom probe nor FIM can individually fully deliver—thereby making this new approach, here broadly termed analytical field ion microscopy (aFIM), unique.

Analysis and understanding of the role of hydrogen in metals is a significant challenge for the future of materials science, and this is a clear objective of recent work in the atom probe tomography (APT) community. Isotopic marking by deuteration has often been proposed as the preferred route to enable quantification of hydrogen by APT. Zircaloy-4 was charged electrochemically with hydrogen and deuterium under the same conditions to form large hydrides and deuterides. Our results from a Zr hydride and a Zr deuteride highlight the challenges associated with accurate quantification of hydrogen and deuterium, in particular associated with the overlap of peaks at a low mass-to-charge ratio and of hydrogen/deuterium containing molecular ions. We discuss possible ways to ensure that appropriate information is extracted from APT analysis of hydrogen in zirconium alloy systems that are important for nuclear power applications.

Although atom probe tomography (APT) reconstructions do not directly influence the local elemental analysis, any structural inferences from APT volumes demand a reliable reconstruction of the point cloud. Accurate estimation of the reconstruction parameters is crucial to obtain reliable spatial scaling. In the current work, a new automated approach of calibrating atom probe reconstructions is developed using only one correlative projection electron microscopy (EM) image. We employed an algorithm that implements a 2D cross-correlation of microstructural features observed in both the APT reconstructions and the corresponding EM image. We apply this protocol to calibrate reconstructions in a Cu(In,Ga)Se2-based semiconductor and in a Co-based superalloy. This work enables us to couple chemical precision to structural information with relative ease.

Atom probe tomography (APT) is rising in influence across many parts of materials science and engineering thanks to its unique combination of highly sensitive composition measurement and three-dimensional microstructural characterization. In this invited article, we have selected a few recent applications that showcase the unique capacity of APT to measure the local composition at structural defects. Whether we consider dislocations, stacking faults, or grain boundary, the detailed compositional measurements tend to indicate specific partitioning behaviors for the different solutes in both complex engineering and model alloys we investigated.

A detailed knowledge of the atomic structure of magnetic semiconductors is crucial to understanding their electronic and magnetic properties, which could enable spintronic applications. Energy-dispersive X-ray spectrometry (EDX) in the scanning transmission electron microscope and atom probe tomography (APT) experiments reveal the formation of Cr-rich regions in Cd1−x Cr x Te layers grown by molecular beam epitaxy. These Cr-rich regions occur on a length scale of 6–10 nm at a nominal Cr composition of x=0.034 and evolve toward an ellipsoidal shape oriented along <111> directions at a composition of x=0.083. Statistical analysis of the APT reconstructed volume reveals that the Cr aggregation increases with the average Cr composition. The correlation with the magnetic properties of such (Cd,Cr)Te layers is discussed within the framework of strongly inhomogeneous materials. Finally, difficulties in accurately quantifying the Cr distribution in the CdTe matrix on an atomic scale by EDX and APT are discussed.