Reflections on the Analysis of Interfaces and Grain Boundaries by Atom Probe Tomography.

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.

Enhancing Element Identification by Expectation-Maximization Method in Atom Probe Tomography.

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.

Contribution of Local Analysis Techniques for the Characterization of Iron and Alloying Elements in Nitrides: Consequences on the Precipitation Process in Fe⁻Si and Fe⁻Cr Nitrided Alloys.

Atom Probe Tomography (APT), Transmission Electron Microscopy (TEM), and 3D mechanical calculations in complex geometry and anisotropic strain fields were employed to study the role of minor elements in the precipitation process of silicon and chromium nitrides in nitrided Fe⁻Si and Fe⁻Cr alloys, respectively. In nitrided Fe⁻Si alloys, an original sequence of Si3N4 precipitation was highlighted. Al⁻N clusters form first and act as nucleation sites for amorphous Si3N4 nitrides. This novel example of particle-simulated nucleation opens a new way to control Si3N4 precipitation in Fe⁻Si alloys. In nitrided Fe⁻Cr alloys, both the presence of iron in chromium nitrides and excess nitrogen in the ferritic matrix are unquestionably proved. Only a certain part of the so-called excess nitrogen is shown to be explained by the elastic accommodation of the misfit between nitride and the ferritic matrix. The presence of immobile excess nitrogen trapped at interfaces can be highly suspected.

In Situ Investigation of the Iron Carbide Precipitation Process in a Fe-C-Mn-Si Q&P Steel.

Quenching and Partitioning (Q&P) steels are promising candidates for automotive applications because of their lightweight potential. Their properties depend on carbon enrichment in austenite which, in turn, is strongly influenced by carbide precipitation in martensite during quenching and partitioning treatment. In this paper, by coupling in situ High Energy X-Ray Diffraction (HEXRD) experiments and Transmission Electron Microscopy (TEM), we give some clarification regarding the precipitation process of iron carbides in martensite throughout the Q&P process. For the first time, precipitation kinetics was followed in real time. It was shown that precipitation starts during the reheating sequence for the steel studied. Surprisingly, the precipitated fraction remains stable all along the partitioning step at 400 °C. Furthermore, the analyses enable the conclusion that the iron carbides are most probably eta carbides. The presence of cementite was ruled out, while the presence of several epsilon carbides cannot be strictly excluded.

True Atomic-Scale Imaging in Three Dimensions: A Review of the Rebirth of Field-Ion Microscopy.

This article reviews recent advances utilizing field-ion microscopy (FIM) to extract atomic-scale three-dimensional images of materials. This capability is not new, as the first atomic-scale reconstructions of features utilizing FIM were demonstrated decades ago. The rise of atom probe tomography, and the application of this latter technique in place of FIM has unfortunately severely limited further FIM development. Currently, the ubiquitous availability of extensive computing power makes it possible to treat and reconstruct FIM data digitally and this development allows the image sequences obtained utilizing FIM to be extremely valuable for many material science and engineering applications. This article demonstrates different applications of these capabilities, focusing on its use in physical metallurgy and semiconductor science and technology.

Microstructural Evolution in 2101 Lean Duplex Stainless Steel During Low- and Intermediate-Temperature Aging.

The microstructural evolution of a 2101 lean duplex stainless steel (DSS) during isothermal aging from room temperature to 470 °C was investigated using thermoelectric power (TEP) measurements to follow the kinetics, atom probe tomography, and transmission electron microscopy. Despite the low Ni, Cr, and Mo contents, the lean DSS was sensitive to α-α' phase separation and Ni-Mn-Si-Al-Cu clustering at intermediate temperatures. The time-temperature pairs characteristic of the early stages of ferrite decomposition were determined from the TEP kinetics. Considering their composition and locations, the clusters are most likely G phase precursors.

Nanometer scale tomographic investigation of fine scale precipitates in a CuFeNi granular system by three-dimensional field ion microscopy.

The microstructure of Cu80Fe10Ni10 (at. %) granular ribbons was investigated by means of three-dimensional field ion microscopy (3D FIM). This ribbon is composed of magnetic precipitates embedded in a nonmagnetic matrix. The magnetic precipitates have a diameter smaller than 5 nm in the as-spun state and are coherent with the matrix. No accurate characterization of such a microstructure has been performed so far. A tomographic characterization of the microstructure of melt spun and annealed Cu80Fe10Ni10 ribbon was achieved with 3D FIM at the atomic scale. A precise determination of the size distribution, number density, and distance between the precipitates was carried out. The mean diameter for the precipitates is 4 nm in the as-spun state. After 2 h at 350°C, there is an increase of the size of the precipitates, while after 2 h at 400°C the mean diameter of the precipitates decreases. Those data were used as inputs in models that describe the magnetic and magnetoresistive properties of this alloy.