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While application of clustering algorithms to atom probe tomography data have enabled quantification of solute clusters in terms of number density, size, and subcomposition there exist other properties (e.g., volume, surface area, and composition) that are better determined by defining an interface between the cluster and the surrounding matrix. The limitation in composition results from an ion selection step where the expected matrix ion types are omitted from the cluster search algorithm to enhance the contrast between the matrix and cluster and to reduce the complexity of the search. Previously, composition determination within solute clusters has utilized a secondary envelopment and erosion step on top of conventional methods such as maximum separation. In this work, we present a novel stochastic method that combines the particle identification fidelity of a conventional clustering algorithm with the analytical flexibility of mesh-based approaches through the generation of alpha shapes for each identified cluster. The corresponding mesh accounts for concave components of the clusters and determines the volume and surface area of the clusters; additionally, the mesh boundary is utilized to update the total composition according to the internal ions.
The high precision offered by small-scale mechanical testing has allowed the relationships between mechanical behavior and specific microstructural features to be determined to an unprecedented degree. However, of most interest to scientists and engineers is often the behavior of materials under service conditions in an extreme environment, such as high/low temperatures, high strain rates, hydrogen atmosphere, or radiation. In this article, we detail progress made to adapt nanomechanical testing systems and techniques to observe materials behavior in situ in extreme environments.
Atom probe tomography (APT) is a powerful technique to characterize buried three-dimensional nanostructures in a variety of materials. Accurate characterization of those nanometer-scale clusters and precipitates is of great scientific significance to understand the structure–property relationships and the microstructural evolution. The current widely used cluster analysis method, a variant of the density-based spatial clustering of applications with noise algorithm, can only accurately extract clusters of the same atomic density, neglecting several experimental realities, such as density variations within and between clusters and the nonuniformity of the atomic density in the APT reconstruction itself (e.g., crystallographic poles and other field evaporation artifacts). This clustering method relies heavily on multiple input parameters, but ideal selection of those parameters is challenging and oftentimes ambiguous. In this study, we utilize a well-known cluster analysis algorithm, called ordering points to identify the clustering structures, and an automatic cluster extraction algorithm to analyze clusters of varying atomic density in APT data. This approach requires only one free parameter, and other inputs can be estimated or bounded based on physical parameters, such as the lattice parameter and solute concentration. The effectiveness of this method is demonstrated by application to several small-scale model datasets and a real APT dataset obtained from an oxide-dispersion strengthened ferritic alloy specimen.
Ceramic fiber–matrix composites (CFMCs) are exciting materials for engineering applications in extreme environments. By integrating ceramic fibers within a ceramic matrix, CFMCs allow an intrinsically brittle material to exhibit sufficient structural toughness for use in gas turbines and nuclear reactors. Chemical stability under high temperature and irradiation coupled with high specific strength make these materials unique and increasingly popular in extreme settings. This paper first offers a review of the importance and growing body of research on fiber–matrix interfaces as they relate to composite toughening mechanisms. Second, micropillar compression is explored experimentally as a high-fidelity method for extracting interface properties compared with traditional fiber push-out testing. Three significant interface properties that govern composite toughening were extracted. For a 50-nm-pyrolytic carbon interface, the following were observed: a fracture energy release rate of ∼2.5 J/m2, an internal friction coefficient of 0.25 ± 0.04, and a debond shear strength of 266 ± 24 MPa. This research supports micromechanical evaluations as a unique bridge between theoretical physics models for microcrack propagation and empirically driven finite element models for bulk CFMCs.
We employ intense and short pulses of energetic lithium (Li+) ions to investigate the relaxation dynamics of radiation induced defects in single crystal silicon samples. Ions both create damage and track damage evolution simultaneously at short time scales when we use the channeling effect as a diagnostic tool. Ion pulses, ∼20 to 600 ns long and with peak currents of up to ∼1 A are formed in an induction type linear accelerator, the Neutralized Drift Compression eXperiment at Lawrence Berkeley National Laboratory. By rotating silicon (<100>) membranes of different thicknesses and changing the incident ion energy, the fraction of channeled ions in the transmitted beam could be varied. In preliminary experiments we find that the Li ion intensity is not high enough to generate overlapping cascades (in time and space) that would be necessary to measure a change in the shape of the current waveform of the transmitted ion beam. We discuss the concept of pump-probe type experiments with short ion beam pulses to access defect dynamics in materials and outline a path to increasing damage rates with heavier ions and by the application of longitudinal and lateral pulse compression techniques.
Small-scale testing techniques such as nanoindentation and micro-/nanocompression are promising methods for addressing mechanical properties of ion-beam-irradiated materials. We performed different proton irradiations and critically evaluated the results obtained from nanoindentation and pillar compression, both performed parallel and perpendicular to the irradiation direction. Experiments parallel to beam direction suffer from variation of material properties with penetration depth. This is improved by cross-sectional experiments, thereby probing the effect of different doses along the beam penetration depth on mechanical properties. Finally, we demonstrate that, compared with nanoindentation, miniaturized uniaxial compression experiments offer a more reliable and straightforward interpretation of the mechanical data, as they impose a nominally uniaxial stress on a well-defined volume at a specific position. Moreover, the exposed pillar geometry is not influenced by surface contamination and enables in situ observation of the governing mechanical processes, which is typically not possible during indentation experiments in a half-space geometry.
In advanced nuclear applications, high temperature and a corrosive environment are present in addition to a high dose radiation field causing displacement damage in the material. In recent times it has been shown that Nanostructured Ferritic Alloys (NFA’s) such as advanced Oxide Dispersion Strengthened (ODS) steels are suitable for this environment as they tolerate high dose irradiation without significant changes in microstructure or relevant mechanical properties.
Ion beam irradiation is a fast and cost effective way to induce radiation damage in materials but has limited penetration depth. Therefore, small scale mechanical testing such as nanoindentation and micro compression testing in combination with FIB based sample preparation for micro structural characterization has to be performed allowing a full assessment of the materials’ behavior under radiation environment. In this work two different ODS materials have been irradiated using proton and combined proton and He beams up to 1 dpa at different temperatures. Nanoindentation and LEAP measurements were performed in order to assess the changes in properties of these alloys due to irradiation. The same techniques were applied to intermetallic nanostructured alloys in order to investigate the effectiveness of the metal-intermetallic interface to provide defect sinks for He and radiation damage. It was found that irradiation can cause the formation of intermetallic particles even at room temperature while increasing the material strength significantly.
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