Reliable spatially resolved compositional analysis through atom probe tomography requires an accurate placement of the detected ions within the three-dimensional reconstruction. Unfortunately, for heterogeneous systems, traditional reconstruction protocols are prone to position some ions incorrectly. This stems from the use of simplified projection laws which treat the emitter apex as a spherical cap, although the actual shape may be far more complex. For instance, sampled materials with compositional heterogeneities are known to develop local variations in curvature across the emitter due to their material phase specific evaporation fields. This work provides three pivotal precursors to improve the spatial accuracy of the reconstructed volume in such cases. First, we show scanning probe microscopy enables the determination of the local curvature of heterogeneous emitters, thus providing the essential information for a more advanced reconstruction considering the actual shape. Second, we demonstrate the cyclability between scanning probe characterization and atom probe analysis. This is a key ingredient of more advanced reconstruction protocols whereby the characterization of the emitter topography is executed at multiple stages of the atom probe analysis. Third, we show advances in the development of an electrostatically driven reconstruction protocol which are expected to enable reconstruction based on experimental tip shapes.

An improved reconstruction method for atom probe tomography is presented. In this approach, the curvature of the field emitter is variable, in contrast to the conventional reconstruction technique. The information about the tip shape at different stages of the reconstruction is directly extracted from the local density of events on the detector. To this end, the detector and the tip surface are split into different segments. According to the density distribution of events observed on the detector, the size of the corresponding segment on the tip surface is calculated, yielding an emitter profile which is not necessarily spherical. The new approach is demonstrated for emitter structures with radial symmetry that contain a spherical precipitate with a substantially lower or higher evaporation field compared to the surrounding matrix. A comparison to the conventional point projection approach is made.

In creep resistant Z-phase strengthened 12% Cr steels, MX (M=Nb, Ta, or V, and X=C and/or N) to Z-phase (CrMN, M=Ta, Nb, or V) transformation plays an important role in achieving a fine distribution of Z-phase precipitates for creep strengthening. Atom probe tomography was employed to investigate the phase transformation in a Nb-based Z-phase strengthened trial steel. Using iso-concentration surfaces with different concentration values, and subtracting the matrix contribution enabled us to reveal the core-shell structure of the transient precipitates between MX and Z-phase. It was shown that Z-phase forms by diffusion of Cr into NbN upon ageing, and Z-phase has a composition corresponding to Cr1+xNb1−xN with x=0.08.

Atom probe tomography was utilized to measure directly the chemical compositions of Al3(Zr1−xTix) precipitates with a metastable L12 structure formed in Al-0.1Zr-0.1Ti (at.%) alloys upon aging at 375°C or 425°C. The alloys exhibit an inhomogeneous distribution of Al3(Zr1−xTix) precipitates, as a result of a nonuniform dendritic distribution of solute atoms after casting. At these aging temperatures, the Zr:Ti atomic ratio in the precipitates is about 10 and 5, respectively, indicating that Ti remains mainly in solid solution rather than partitioning to the Al3(Zr1−xTix) precipitates. This is interpreted as being due to the very small diffusivity of Ti in α-Al, consistent with prior studies on Al-Sc-Ti and Al-Sc-Zr alloys, where the slower diffusing Zr and Ti atoms make up a small fraction of the Al3(Sc1−xTix/Zrx) precipitates. Unlike those alloys, however, the present Al-Zr-Ti alloys exhibit no interfacial segregation of Ti at the matrix/precipitate heterophase interface, a result that may be affected by a significant disparity in the evaporation fields of the α-Al matrix and Al3(Zr1−xTix) precipitates and/or a lack of local thermodynamic equilibrium at the interface.