Interfaces play critical roles in materials and are usually both structurally and compositionally complex microstructural features. The precise characterization of their nature in three-dimensions at the atomic scale is one of the grand challenges for microscopy and microanalysis, as this information is crucial to establish structure–property relationships. Atom probe tomography is well suited to analyzing the chemistry of interfaces at the nanoscale. However, optimizing such microanalysis of interfaces requires great care in the implementation across all aspects of the technique from specimen preparation to data analysis and ultimately the interpretation of this information. This article provides critical perspectives on key aspects pertaining to spatial resolution limits and the issues with the compositional analysis that can limit the quantification of interface measurements. Here, we use the example of grain boundaries in steels; however, the results are applicable for the characterization of grain boundaries and transformation interfaces in a very wide range of industrially relevant engineering materials.

We introduce an efficient, automated computational approach for analyzing interfaces within atom probe tomography datasets, enabling quantitative mapping of their thickness, composition, as well as the Gibbsian interfacial excess of each solute. Detailed evaluation of an experimental dataset indicates that compared with the composition map, the interfacial excess map is more robust and exhibits a relatively higher resolution to reveal compositional variations. By field evaporation simulations with a predefined emitter mimicking the experimental dataset, the impact of trajectory aberrations on the measurement of the thickness, composition, and interfacial excess of the decorated interface are systematically analyzed and discussed.

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.

Cemented tungsten carbide has been analyzed using laser-pulsed atom probe tomography (APT). The influence of experimental parameters, including laser pulse energy, pulse repetition rate, and specimen base temperature, on the acquired data were evaluated from different aspects, such as mass spectrum, chemical composition, noise-to-signal ratio, and multiple events. Within all the applied analysis conditions, only 1 MHz pulse repetition rate led to a strong detector saturation effect, resulting in a largely biased chemical composition. A comparative study of the laser energy settings showed that an ~12 times higher energy was required for the less focused green laser of the LEAPTM 3000X HR system to achieve a similar evaporation field as the finer spot ultraviolet laser of the LEAPTM 5000 XS system.