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At least 37 records · Page 2

Materials Fingerprinting Classification

Significant progress in many classes of materials could be made with the availability of experimentally-derived large datasets composed of atomic identities and three-dimensional coordinates. Methods for visualizing the local atomic structure, such as atom probe tomography (APT), which routinely generate datasets comprised of millions of atoms, are an important step in realizing this goal. However, state-of-the-art APT instruments generate noisy and sparse datasets that provide information about elemental type, but obscure atomic structures, thus limiting their subsequent value for materials discovery. The application of a materials fingerprinting process, a machine learning algorithm coupled with topological data analysis, provides an avenue by which here-to-fore unprecedented structural information can be extracted from an APT dataset. As a proof of concept, the material fingerprint is applied to high-entropy alloy APT datasets containing body-centered cubic (BCC) and face-centered cubic (FCC) crystal structures. A local atomic configuration centered on an arbitrary atom is assigned a topological descriptor, with which it can be characterized as a BCC or FCC lattice with near perfect accuracy, despite the inherent noise in the dataset. Finally, this successful identification of a fingerprint is a crucial first step in the development of algorithms which can extract more nuanced information, such as chemical ordering, from existing datasets of complex materials.

36 MATERIALS SCIENCE↗

Assessment of Local Observation of Atomic Ordering in Alloys via the Radial Distribution Function: A Computational and Experimental Approach

As a powerful analytical technique, atom probe tomography (APT) has the capacity to acquire the spatial distribution of millions of atoms from a complex sample. However, extracting information at the Ångstrom-scale on atomic ordering remains a challenge due to the limits of the APT experiment and data analysis algorithms. The development of new computational tools enable visualization of the data and aid understanding of the physical phenomena such as disorder of complex crystalline structures. Here, we report progress towards this goal using two steps. We describe a computational approach to evaluate atomic ordering in the crystal structure by generating radial distribution functions (RDF). Atomic ordering is rendered as the Fractional Cumulative Radial Distribution Function (FCRDF) which allows for greater visibility of local compositions at short range in the structure. Further, we accommodate in the analysis additional parameters such as uncertainty in the atomic coordinates and the atomic abundance to ascertain short-range ordering in APT data sets. We applied the FCRDF analysis to synthetic and experimental APT data sets for Ni 3 Al. The ability to observe a signal of atomic ordering consistent with the known L1 2 crystal structure is heavily dependent on spatial uncertainty, irrespective of abundance. Detection of atomic ordering is subject to an upper limit of spatial uncertainty of atoms described with Gaussian distributions with a standard deviation of 1.3 Å. The FCRDF analysis was also applied to the APT data set for a six-component alloy, Al 1.3 CoCrCuFeNi. In this case, we are currently able to visualize elemental segregation at the nanoscale, though unambiguous identification of atomic ordering at the Ångstrom (nearest-neighbor) scale remains a goal.

36 MATERIALS SCIENCE↗

Data on Cu- and Ni-Si-Mn-rich solute clustering in a neutron irradiated austenitic stainless steel

The data presented in this article is supplementary to the research article “Phase instabilities in austenitic steels during particle bombardment at high and low dose rates” (Levine et al.). Needle-shaped samples were prepared with focused ion beam milling from a 304L stainless steel that was irradiated with fast neutrons (E 0.1 MeV) in the BOR-60 reactor at 318 °C to 47.5 dpa. Atom probe tomography (APT) experiments in voltage mode were then conducted on a Cameca LEAP 5000X HR. Atom position, range, and mass spectrum files after reconstruction with Cameca’s IVAS software are included. Cu- and Ni-Si-Mn-rich solute nanoclusters were identified and analyzed using the Open Source Characterization of APT Reconstructions (OSCAR) program. Python code for OSCAR, information on the program’s underlying algorithm, and sample output files are provided. A proximity histogram of a Ni-Si-Mn-rich cluster and a 1D density/solute concentration profile of a Cu-rich cluster are given to demonstrate OSCAR’s analytical functionalities. The provided APT dataset is valuable for benchmarking phase instabilities in neutron-irradiated austenitic stainless steels that occur at high doses. The OSCAR program can be reused to process other APT data sets where solute nanoclustering is of interest.

42 ENGINEERING↗

Atom Probe Tomography and Three-Dimensional Atomic Scale Characterisation of Interplanetary Dust Particles: Inorganic and Organic, Hydrous and Anhydrous Assemblages

Interplanetary dust particles (IDPs)preserve primordial fragments from our Solar System and external stellar systems, sampled from a vast range of dust forming bodies that often display smaller degrees of parent body processing than is seen in meteorites. IDPs preserve some of the smallest astromaterials from our Solar System, many of which are believed to be among the most important materials for studying physical and chemical processing, and formation mechanisms occurring within the interstellar medium (ISM), Solar Nebula and external planetary systems[1]. However, their formation processes and provenance are poorly constrained, owing in part to spatial resolution limitations of traditional analytical techniques. Atom probe tomography (APT) uses a pulsed laser to field-evaporate material at the atomic scale from needle-shaped samples, and time-of-flight spectrometry for 3D reconstruction of element and isotope distribution in samples after data acquisition. This technique has the highest spatial resolution available of any technique used within the geoscience field[2]. However, measuring multi-phase specimens and porous media in APT can be challenging, two primary characteristics of IDPs. Here we present a custom method for APT needle design and the first results of a 3Datomic scale study of interplanetary dust particles, salt crystals and extraterrestrial insoluble and soluble organic matter designed to overcome the challenges of studying IDP-like materials.

N D Nevill↗

Strengthening model development and effects of low diffusing solutes to coarsening resistance in aluminum alloys

A modified Orowan strengthening model is proposed to account for finite rod-shaped precipitates with hemispherical caps in aluminum alloy systems. A combined computational and experimental approach is used to study the influences of anisotropic Orowan looping and solute-dislocation interaction on temperature-dependent yield strength. Here, the strengthening model is validated with a dataset containing 297 experimental precipitate geometries, chemistries, temperatures, and strength measurements, and achieves a strong predictive correlation of 0.8713 with experimentally measured yield strengths. Under conditions that are applicable to coarsening, constant particle volume fraction and aspect ratio, the model predicts that short rod precipitates provide far superior strengthening effects compared to plate precipitates. A cast Al-Si-Mg-Cu alloy with rod-shaped Q-phase (Al 3 Cu 2 Mg 9 Si 7 ) precipitates was developed with a novel chemistry exploring the use of low-diffusivity elements (Mn, Ni, V, Zr) to limit precipitate coarsening. The thermodynamic behavior of Mn, Ni, V, and Zr across the Q-phase interface is examined using transmission electron microscopy (TEM), first-principles density-functional theory (DFT) calculations. and atom-probe tomography (APT). DFT calculations utilizing TEM identified Q-phase/Al-matrix interfaces show that Mn, Ni, V, and Zr preferentially segregate to the Q-phase precipitate boundaries which suggests inhibition of precipitate coarsening and higher strengths after temperature exposure. Atom-probe tomography confirms solute atom partitioning/segregation at the Q-phase/Al-matrix interface, found in the modified commercial AS7GU alloy (A356 +0.5%Cu), which supports these observations.

36 MATERIALS SCIENCE↗

Atom Probe Tomography for the Observation of Hydrogen in Materials: A Review

Atom probe tomography (APT) is an emerging microscopy technique that has high sensitivity for hydrogen with sub-nanometre-scale spatial resolution, which makes it a unique method to investigate the atomic-scale distribution of hydrogen at interfaces and defects in materials. This article introduces the basics of APT-based hydrogen analysis, particularly the challenge of distinguishing a hydrogen background signal in APT by using hydrogen isotopes, along with strategies to yield high-quality analysis. This article also reviews several important findings on hydrogen distribution in a range of materials, including both structural alloys and functional materials, enabled by using APT. Limitations and future opportunities for hydrogen analysis by APT are also discussed.

42 ENGINEERING↗

Nanocluster Evolution in D9 Austenitic Steel under Neutron and Proton Irradiation

Austenitic stainless steel D9 is a candidate for Generation IV nuclear reactor structural materials due to its enhanced irradiation tolerance and high-temperature creep strength compared to conventional 300-series stainless steels. But, like other austenitic steels, D9 is susceptible to irradiation-induced clustering of Ni and Si, the mechanism for which is not well understood. This study utilizes atom probe tomography (APT) to characterize the chemistry and morphology of Ni–Si nanoclusters in D9 following neutron or proton irradiation to doses ranging from 5–9 displacements per atom (dpa) and temperatures ranging from 430–683 °C. Nanoclusters form only after neutron irradiation and exhibit classical coarsening with increasing dose and temperature. The nanoclusters have Ni 3 Si stoichiometry in a Ni core–Si shell structure. This core–shell structure provides insight into a potentially unique nucleation and growth mechanism—nanocluster cores may nucleate through local, spinodal-like compositional fluctuations in Ni, with subsequent growth driven by rapid Si diffusion. This study underscores how APT can shed light on an unusual irradiation-induced nanocluster nucleation mechanism active in the ubiquitous class of austenitic stainless steels.

36 MATERIALS SCIENCE↗

Scanning Transmission Electron Microscopy–Atom Probe Tomography Correlative Analysis for the Characterization of Solute-defect Interactions

Atom probe tomography (APT) and (scanning) transmission electron microscopy ((S)TEM) are complementary techniques that provide spatially resolved chemical and structural information at the atomic scale. Here, in this study, we employ two different STEM/APT correlative analysis methods to investigate Cr segregation at dislocation loops in ultra-high purity Fe–Cr alloys. APT needles for the correlative analysis were extracted either from bulk material or from thinned TEM lamellae. STEM analysis was used to determine the Burgers vectors of ion-irradiation-induced dislocation loops, while APT reconstruction of the same region revealed the Cr segregation to these loops. We extended the g•b = 0 invisibility criterion of dislocation loops from TEM mode in a lamella to STEM mode in a needle-shaped specimen. STEM and APT analysis on the same needle provide straightforward correlative analysis, although it is limited by a small observation volume. In contrast, iterative STEM analysis of TEM lamellae, followed by the selective extraction of specific regions of interest for APT analysis, expands the observation area by up to 100 times but requires additional time-consuming steps for APT needle extraction from the lamellae.

47 OTHER INSTRUMENTATION↗

Atom Probe Tomography Analysis of Mica

Laser-assisted atom probe tomography (APT) is a relatively new, powerful technique for sub-nanometric mineral and biomineral analysis. However, the laser-assisted APT analysis of highly anisotropic and chemically diverse minerals, such as phyllosilicates, may prove especially challenging due to the complex interaction between the crystal structure and the laser pulse upon applying a high electric field. Micas are a representative group of nonswelling clay minerals of relevance to a number of scientific and technological fields. In this study, a Mg-rich biotite was analyzed by APT to generate preliminary data on nonisotropic minerals and to investigate the effect of the crystallographic orientation on mica chemical composition and structure estimation. Here, the difference in results obtained for specimens extracted from the (001) and ( hk 0) mica surfaces indicate the importance of both experimental parameters and the crystallography. Anisotropy of mica has a strong influence on the physicochemical properties of the mineral during field evaporation and the interpretation of APT data. The promising results obtained in the present study open the way to future innovative APT applications on mica and clay minerals and contribute to the general discussion on the challenges for the analysis of geomaterials by atom probe tomography.

3D reconstructions↗

Development of Automated Atom Probe Tomography capability to study the influence of applied voltage and laser power on the final apparent composition of the analyzed specimen

This study presents the development and implementation of an autonomous Bayesian optimization (BO) framework for controlling and optimizing experimental parameters in Atom Probe Tomography (APT). Using commercial silicon needle samples as a benchmark system, we demonstrate that BO can efficiently navigate the complex parameter space of voltage and laser power to achieve target charge state ratios (specifically Si + /(Si + +Si 2+ )) with minimal experimental evaluations. Our implementation integrates Gaussian Process modeling with the CAMECA atom probe control framework, enabling autonomous adjustment of experimental conditions in real-time. Results show that the algorithm successfully converges to target ratios under different scenarios: maintaining a reference ratio, increasing the ratio (favoring Si 1+ ), and decreasing the ratio (favoring Si 2+ ). The system adapts to specimen evolution during analysis, compensating for changes in apex geometry while maintaining optimization targets. This work establishes a proof of concept for AI-driven optimization in APT, addressing the traditional challenges of manual parameter tuning and paving the way for applications to more complex materials where compositional accuracy is critical.

36 MATERIALS SCIENCE↗

Micro‐ and Nanoscale Heterogeneities in Zeolite Beta as Measured by Atom Probe Tomography and Confocal Fluorescence Microscopy

Micro- and nanoscale information on the activating and deactivating coking behaviour of zeolite catalyst materials increases our current understanding of many industrially applied processes, such as the methanol-to-hydrocarbon (MTH) reaction. Atom probe tomography (APT) was used to reveal the link between framework and coke elemental distributions in 3D with sub-nanometre resolution. APT revealed 10–20 nanometre-sized Al-rich regions and short-range ordering (within nanometres) between Al atoms. With confocal fluorescence microscopy, it was found that the morphology of the zeolite crystal as well as the secondary mesoporous structures have a great effect on the microscale coke distribution throughout individual zeolite crystals over time. Additionally, a nanoscale heterogeneous distribution of carbon as residue from the MTH reaction was determined with carbon-rich areas of tens of nanometres within the zeolite crystals. Finally, a short length-scale affinity between C and Al atoms, as revealed by APT, indicates the formation of carbon-containing molecules next to the acidic sites in the zeolite.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Chapter 13: Time-of-Flight Secondary-Ion Mass Spectrometry and Atom Probe Tomography

Time-of-flight secondary-ion mass spectrometry (TOF-SIMS) and atom probe tomography (APT) have many similarities. Both detect the chemical makeup of a solid material at ppm or better sensitivity, while retaining the spatial location information from the signal. Both use a similar principle to measure a signal associated with a given charged secondary ion—the flight time it takes a secondary ion to reach the detector after it is generated. Both are destructive techniques—albeit destructive of very small volumes—because the signal measured is generated by the removal of material from the sample itself. Importantly, both techniques require ultra-high vacuum (UHV) to ensure that the secondary ions, once generated, can reach the detector without collision with other atoms in the gas phase. In the case of TOF-SIMS, the samples can vary from several mm to several inches in size, whereas for APT, the samples are cones several hundred microns in size that are prepared in a special manner (covered in detail later in the chapter). We will discuss the basic fundamentals of each technique and cover several examples of the technique applied to photovoltaic materials, which should give a good idea of the types of information one can gain from TOF-SIMS and APT and how they are complementary as they both operate at different length scales: at the hundreds of microns to hundreds of nanometer scale for TOF-SIMS and at the nanometer to a few angstroms scale for APT.

41 EE - Solar Energy Technologies Office (EE-4S)↗

Microstructural and Creep Properties of Boron- and Zirconium-Containing Cobalt-Based Superalloys

The effects of micro-additions of boron and zirconium on grain-boundary (GB) structure and strength inpolycrystalline γ(f.c.c.) plus γ’(L12) strengthened Co-9.5Al-7.5W-X at. % alloys (X=0-Ternary, 0.05B, 0.01B,0.05Zr, and 0.005B-0.05Zr at. %) are studied. Creep tests performed at 850 °C demonstrate that GB strength and cohesion limit the creep resistance and ductility of the ternary B- and Zr-free alloy due to intergranular fracture. Alloys with 0.05B and 0.005B-0.05Zr both exhibit improved creep strength due to enhanced GB cohesion,compared to the baseline ternary Co-9.5Al-7.5W alloy, but alloys containing 0.01B or 0.05Zr additions displayed no benefit. Atom-probe tomography (APT) is utilized to measure GB segregation, where B and Zr are demonstrated to segregate at GBs. A Gibbsian interfacial excess of 5.57 ± 1.04 atoms nm(exp) -2 was found for B at aGB in the 0.01B alloy and 2.88 ± 0.81 and 2.40 ± 0.84 atoms nm2 for B and Zr, respectively, for the 0.005B-0.05Zr alloy. The GBs in the highest B-containing (0.05B) alloy exhibit micrometer-sized boride precipitates with adjacent precipitate denuded-zones (PDZs), whereas secondary precipitation at the GBs is absent in theother four alloys. The 0.05B alloy has the smallest room temperature yield strength, by 6%, which is attributedto the PDZs, but it exhibits the largest increase in creep strength (with an ~2.5 order of magnitude decrease inthe minimum strain rate for a given stress at 850 °C) over the baseline Co-9.5Al-7.5W alloy.

Creep↗

Atom Probe characterization of neutron irradiated commercial ZIRLO® and AXIOM X2® alloys

As part of the Mechanistic Understanding of ZIrconium Corrosion (MUZIC) program, this team has been instrumental to obtain EPRI and Westinghouse sponsorships to prepare the neutron irradiated ZIRLO® and X2® from Vogtle nuclear power plant and ship them from Studsvik’s (Sweden) hot cells to Idaho National Laboratory (INL) to be part of the NSUF library. The uniqueness of these sets of neutron irradiated alloys is that they are at the same two extremes of the fuel cycles, allowing us to study the microchemistry evolution as a function of irradiation doses, exposure time and solute content. Advanced commercial Zirconium-Niobium (Zr-Nb) alloys, such as ZIRLO® and AXIOM®, have been developed by Westinghouse to enhance the corrosion resistance of fuel cladding material for longer service time. This study specifically aims at investigating the neutron irradiation induced Nb redistribution in AXIOM® X2® to understand the effect of neutron irradiation induced microchemistry changes and the irradiation enhanced corrosion resistance observed in ZrNb alloys. The detailed sample information on chemical composition and irradiation is given in shown in Table 1a and 1b respectively. To study the neutron IIP/nanoclusters and Nb concentration in the solid solution, atom probe tomography (APT) is the primary tool to obtain reliable chemical information. APT specimens were prepared in shielded focused ion beam (FIB) at the Irradiated Materials Characterization Laboratory (IMCL) at INL followed by APT analysis at CAES facility using LEAP 4000XR

36 MATERIALS SCIENCE↗

Chromium and Tantalum Site Substitution Patterns in Ni3Al (L1(sub 2))gamma(prime)- Precipitates

The site substitution behavior of Cr and Ta in the Ni3Al (Ll2)-type gamma'-precipitates of a Ni-Al-Cr-Ta alloy is investigated by atom-probe tomography (APT) and first-principles calculations. Measurements of the gamma'-phase composition by APT suggest that Al, Cr, and Ta share the Al sublattice sites of the gamma'-precipitates. The calculated substitutional energies of the solute atoms at the Ni and Al sublattice sites indicate that Ta has a strong preference for the Al sites, while Cr has a weak Al site preference. Furthermore, Ta is shown to replace Cr at the Al sublattice sites of the gamma'-precipitates, altering the elemental phase partitioning behavior of the Ni-Al-Cr-Ta alloy.

Booth-Morrison, Christopher↗

Atom Probe Tomography Investigation of Clustering in Model P 2 O 5 -Doped Borosilicate Glasses for Nuclear Waste Vitrification

Atom probe tomography (APT) has been utilized to investigate the microstructure of two model borosilicate glasses designed to understand the solubility limits of phosphorous pentoxide (P 2 O 5 ). This component is found in certain high-level radioactive defence wastes destined for vitrification, where phase separation can potentially lead to a number of issues relating to the processing of the glass and its long-term chemical and structural stability. The development of suitable focused ion beam (FIB)-preparation routes and APT analysis conditions were initially determined for the model glasses, before examining their detailed microstructures. In a 3.0 mol% P 2 O 5 -doped glass, both visual inspection and sensitive statistical analysis of the APT data show homogeneous microstructures, while raising the content to 4.0 mol% initiates the formation of phosphorus-enriched nanoscale precipitates. This study confirms the expected inhomogeneities and phase separation of these glasses and offers routes to characterizing these at near-atomic scale resolution using APT.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

The synergistic role of Mn and Zr/Ti in producing θ'/L12 co-precipitates in Al-Cu alloys

Microstructural stability is a critical factor to consider when designing new alloys for high-temperature applications. An Al-Cu alloy with Mn and Zr additions has recently been developed to withstand extended exposures of up to 350 °C. The addition of Mn in combination with Zr and their segregation to precipitate interfaces play a significant role in stabilizing the metastable θ ' precipitates responsible for the alloy's hardness; however, adding Zr and Mn separately only improves the stability to 200 °C and 300 °C, respectively. To this end, the effect of the synergistic additions on interfacial structure and chemistry was studied in detail using atom probe tomography (APT) and scanning transmission electron microscopy (STEM) for Al-Cu-Mn-Zr/Ti-containing alloys subjected to long-term annealing (up to 2,100 h) in the critical temperature range, 300 °C and 350 °C, to investigate the role of Zr/Ti in increasing the θ '-precipitate stability. The APT and STEM results reveal that Mn additions stabilize θ ' long enough for the slower diffusing Zr atoms to segregate to coherent θ ' interfaces that eventually create a θ '/ L1 2 -Al 3 (Zr x ,Ti 1-x ) co-precipitate structure. The co-precipitate is highly stable, as shown by density functional theory calculations, and is a key factor that governs microstructural stability beyond 300 °C. This study reveals how solute additions with different stabilization mechanisms can work in concert to stabilize a desired microstructure, and the results provide insights that can be applied to other high-temperature alloy systems.

36 MATERIALS SCIENCE↗