Standardizing Spatial Reconstruction Parameters for the Atom Probe Analysis of Common Minerals

Well-defined reconstruction parameters are essential to quantify the size, shape, and distribution of nanoscale features in atom probe tomography (APT) datasets. However, the reconstruction parameters of many minerals are difficult to estimate because intrinsic spatial markers, such as crystallographic planes, are not usually present within the datasets themselves. Using transmission and/or scanning electron microscopy imaging of needle-shaped specimens before and after atom probe analysis, we test various approaches to provide best-fit reconstruction parameters for voltage-based APT reconstructions. The results demonstrate that the length measurement of evaporated material, constrained by overlaying pre- and post-analysis images, yields more consistent reconstruction parameters than the measurement of final tip radius. Using this approach, we provide standardized parameters that may be used in APT reconstructions of 11 minerals. The adoption of standardized reconstruction parameters by the geoscience APT community will alleviate potential problems in the measurement of nanoscale features (e.g., clusters and interfaces) caused by the use of inappropriate parameters.

The Prospect of Spatially Accurate Reconstructed Atom Probe Data Using Experimental Emitter Shapes

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.

Real-time observation of the effect of oxygen storage materials on Pd-based three-way catalysts under ideal automobile exhaust conditions: an operando study

The dynamic behavior of Pd species and the CeO2 support of 1 wt% Pd/Al2O3 and Pd/CeO2 catalysts during three-way catalysis was examined in real time with operando multi-probe analysis.