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This article presents a fast and highly efficient algorithm developed to reconstruct a three-dimensional (3D) volume with a high spatial precision from a set of field ion microscopy (FIM) images, and specific tools developed to characterize crystallographic lattice and defects. A set of FIM digital images and image processing algorithms allow the construction of a 3D reconstruction of the sample at the atomic scale. The capability of the 3D FIM to resolve the crystallographic lattice and the finest defects in metals opens a new way to analyze materials. This spatial precision was quantified on tungsten, analyzed at different analyzing conditions. A specific data mining tool, based on Fourier transforms, was also developed to characterize lattice distortions in the reconstructed volumes. This tool has been used in simulated and experimental volumes to successfully locate and characterize defects such as dislocations and grain boundaries.
Atom probe tomography (APT) analysis conditions play a major role in the composition measurement accuracy. Preferential evaporation (PE), which significantly biases the apparent composition, more than other well-known phenomena in APT, is strongly connected to those analysis conditions. One way to optimize them, in order to have the most accurate measurement, is therefore to be able to predict and then to estimate their influence on the apparent composition. An analytical model is proposed to quantify the PE. This model is applied to three different alloys such as NiCu, FeCrNi, and FeCu. The model explains not only the analysis temperature dependence, as in an already existing model, but also the dependence to the pulse fraction and the pulse frequency. Moreover, the model can also provide an energetic constant directly linked to the energy barrier required to field evaporate atom from the sample surface.
This paper describes an alternative way to assign elemental identity to atoms collected by atom probe tomography (APT). This method is based on Bayesian assignation of label through the expectation–maximization method (well known in data analysis). Assuming the correct shape of mass over charge peaks in mass spectra, the probability of each atom to be labeled as a given element is determined, and is used to enhance data visualization and composition mapping in APT analyses. The method is particularly efficient for small count experiments with a low signal to noise ratio, and can be used on small subsets of analyzed volumes, and is complementary to single-ion decomposition methods. Based on the selected model and experimental examples, it is shown that the method enhances our ability to observe and extract information from the raw dataset. The experimental case of the superimposition of the Si peak and N peak in a steel is presented.
We summarize the findings from an interlaboratory study conducted between ten international research groups and investigate the use of the commonly used maximum separation distance and local concentration thresholding methods for solute clustering quantification. The study objectives are: to bring clarity to the range of applicability of the methods; identify existing and/or needed modifications; and interpretation of past published data. Participants collected experimental data from a proton-irradiated 304 stainless steel and analyzed Cu-rich and Ni–Si rich clusters. The datasets were also analyzed by one researcher to clarify variability originating from different operators. The Cu distribution fulfills the ideal requirements of the maximum separation method (MSM), namely a dilute matrix Cu concentration and concentrated Cu clusters. This enabled a relatively tight distribution of the cluster number density among the participants. By contrast, the group analysis of the Ni–Si rich clusters by the MSM was complicated by a high Ni matrix concentration and by the presence of Si-decorated dislocations, leading to larger variability among researchers. While local concentration filtering could, in principle, tighten the results, the cluster identification step inevitably maintained a high scatter. Recommendations regarding reporting, selection of analysis method, and expected variability when interpreting published data are discussed.
Irradiation of reactor pressure vessel (RPV) steels causes the formation of nanoscale microstructural features (termed radiation damage), which affect the mechanical properties of the vessel. A key tool for characterizing these nanoscale features is atom probe tomography (APT), due to its high spatial resolution and the ability to identify different chemical species in three dimensions. Microstructural observations using APT can underpin development of a mechanistic understanding of defect formation. However, with atom probe analyses there are currently multiple methods for analyzing the data. This can result in inconsistencies between results obtained from different researchers and unnecessary scatter when combining data from multiple sources. This makes interpretation of results more complex and calibration of radiation damage models challenging. In this work simulations of a range of different microstructures are used to directly compare different cluster analysis algorithms and identify their strengths and weaknesses.
A high chromium ferritic Oxide Dispersion Strengthened steel was produced by mechanical alloying of Fe-18Cr-1W-0.3Ti-0.3Ni-0.15Si and 0.5% Y2O3 (wt.%) powders in industrial attritor, followed by hot extrusion at 1100°C. The material was characterized by Atom Probe Tomography on each step of manufacturing process: as-milled powder and in final hot extruded state. In addition, to get information on clustering kinetics the powder was also characterized after annealing at 850°C during 1 hour. Atom Probe Tomography revealed that the oxide dispersion strengthened steel Fe-18Cr contains nanometer scale yttrium- and oxygen-enriched nanoclusters in as-milled state. Their evolution is shown after subsequent annealing and hot extrusion. More well defined nanophases also enriched in Ti are observed. A mechanism of their formation is proposed. Mechanical alloying results in supersaturated solid solution with presence of small Y- and O-enriched clusters. Subsequent annealing stimulates incorporation of Ti to the nucleii that were previously formed during mechanical alloying.
A low copper reactor pressure vessel steel was characterised by atom probe tomography after neutron irradiation at different fluences. The specimens were irradiated within the frame of the Surveillance Program of a production reactor. Roughly spherical clusters enriched in nickel, manganese, silicon and, in a lesser extent, phosphorus and copper were observed at all fluences. The chemical composition of these clusters shows no evolution with fluence, as well as their diameter, close to 3 nm. Their number density increases linearly with the neutron fluence. A continuous segregation of the elements found in the clusters is also observed along dislocation lines, with similar enrichments.
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