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DOE OSTI2017

Neutron Characterization of Encapsulated ATF-1/LANL-1 Mockup Fuel Capsules

Twenty pellets of mock-up accident tolerant fuels UN-U3Si5 were produced at LANL and loaded in two rodlet/capsule assemblies. Tomographic imaging and diffraction measurements were performed to characterize these samples at the Flight-Path 5 and HIPPO beam lines at LANSCE/LANL between November 2016 and January 2017 as well as in August 2017. The entire ~10 cm long, ~1 cm diameter fuel volume could be characterized, however due to time constraints only 2 mm slices in 4mm increments were characterized with neutron diffraction and a 28mm subset of the entire sample was characterized with energy-resolved neutron imaging. The double encapsulation of the fuel into two steel containers does not pose a problem for the neutron analysis and the methods could be applied to enriched as well irradiated fuels.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2018

Role of heat treatment and build orientation in the microstructure sensitive deformation characteristics of IN718 produced via SLM additive manufacturing

The benefits of additive manufacturing have been well documented, but prior to these materials being used in critical applications, the deformation mechanisms must be properly characterized. In this work, the role of heat treatment and build orientation of selective laser melting IN718 is investigated through detailed characterization. The microstructure of this material is probed through a combination of electron microscopy to identify the precipitate structure, electron backscatter diffraction to quantify the grain-level features, and synchrotron-based X-ray microcomputed tomography to detect porosity. A high degree of porosity is observed spatially near the free surface of the part, where the contour during the build process meets the interior hatch. Further, microstructure based deformation mechanisms are explored through digital image correlation relative to the grain features after monotonic and cyclic loading and in situ high-energy X-ray diffraction to identify the lattice strain evolution in these materials. Demarcations between the behaviors of the as-built versus post-processed materials are discussed; specifically, in terms of anisotropy with respect to build direction and values of the strength properties, based on the grain morphology, coherent twin formation, and precipitate structure. In conclusion, the presence of dislocation sub-structures within the grains is observed to homogenize deformation within the as-built sample, while strain partitioning is observed during loading of the post-processed sample.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Four-dimensional microstructurally small fatigue crack growth in cyclically loaded nickel superalloy specimen

Here, we nondestructively image a low-solvus high refractory (LSHR) nickel base specimen microstructure during cyclic loading to characterize crack propagation during the microstructurally small crack (MSC) growth regime. Micro-computed tomography (uCT) is used to characterize the material density and identify crack interfaces, while high-energy diffraction microscopy (HEDM) provides snapshots of the microstructural orientation field changes. From these measurements, data are computationally reconstructed and coregistered to describe the specimen’s configuration before load, before crack nucleation, and throughout the crack propagation/loading process. An MSC forms at a FIB-cut notch, which was previously placed to concentrate stress at the center of the specimen gauge, and propagates along a facet parallel to the local {1 1 1} crystallographic plane. Analysis of available crystallographic slip directions and measured point-to-point disorientation axes indicate probable single and coplanar slip activity along FCC octahedral planes within this region. Similar analyses of other crack propagation facets reveal generally slower growth along directions favoring zig-zag cross and codirectional cross slip, which are often disfavored at room temperature.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Hints of Growth Mechanism Left in Supercrystals

Supercrystals of DNA-functionalized nanoparticles arevisualizedin three dimensions using X-ray ptychographic tomography, and theirreciprocal spaces are mapped with small-angle X-ray scattering inorder to better understand their internal defect structures. X-rayptychographic tomography reveals various types of defects in an assemblythat otherwise exhibits a single crystalline diffraction pattern.On average, supercrystals composed of smaller nanoparticles are smallerin size than supercrystals composed of larger particles. Additionally,supercrystals composed of small nanoparticles are typically aggregatedinto larger "necklace-like" structures. Within theselarger structures, some but not all pairs of connected domains arecoherent in their relative orientations. In contrast, supercrystalscomposed of larger nanoparticles with longer DNA ligands typicallyform faceted crystals. The combination of these two complementaryX-ray techniques reveals that the crystalline assemblies grow by aggregationof smaller assemblies followed by rearrangement of nanoparticles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Achieving superior mechanical properties: Tailoring multicomponent microstructure in AISI 9254 spring steel through a two-stage Q&P process and nanoscale carbide integration

In the pursuit of lightweight, durable steel, we have successfully developed a multicomponent structure in AISI 9254 spring steel using a two-stage quenching and partitioning (Q&P) process. The primary objective of this process was to engineer an optimized microstructure consisting of nanobainite, martensite, and nano-carbides. Utilizing the insights gained from the results of advanced techniques such as X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and atom probe tomography (APT) performed on the as-received AISI 9254 spring steel, we refined the quenching and partitioning (Q&P) path, leading to the successful establishment of a bainitic transformation for superior mechanical properties. Our tensile tests revealed a high yield strength (≈ 1600 ± 25 MPa) and ultimate tensile strength (≈ 1850 ± 50 MPa), along with considerable elongation (≈ 11.15 ± 0.25%). We also identified that pre-formed martensite lath defects and high silicon content play crucial roles during the Q&P process, preventing carbide coalescence and increasing strain-hardening capacity. Finally, this study demonstrates the potential of a Q&P process to generate high-strength, ductile steel for automotive and aerospace applications.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Mechanistic study of shape-anisotropic nanomaterials synthesized via spontaneous galvanic displacement

Among the broad portfolio of preparations for nanoscale materials, spontaneous galvanic displacement (SGD) is emerging as an important technology because it is capable of creating functional nanomaterials that cannot be obtained through other routes and may be used to thrift precious metals used in a broad range of applications including catalysis. With advances resulting from increased understanding of the SGD process, materials that significantly improve efficiency and potentially enable widespread adoption of next generation technologies can be synthesized. In this work, PtAg nanotubes synthesized via displacement of Ag nanowires by Pt were used as a model system to elucidate the fundamental mechanisms of SGD. Furthermore, characterization by X-ray diffraction (XRD), small-angle X-ray scattering (SAXS), and atom probe tomography (APT) indicates nanotubes are formed as Ag is oxidized first from the surface and then from the center of the nanowire, with Pt deposition forming a rough, heterogeneous surface on the PtAg nanotube.

36 MATERIALS SCIENCE↗

NASA NTRS1987

Image analysis of particle field by means of computed tomography

In order to visualize and investigate spray structures, computed tomography technique is applied to analyze droplet information. From the transmitted light intensity through the spray and/or the data of particle size distribution obtained from a Fraunhofer diffraction principle, the quantitative volume of spray droplet or local particle size was calculated and the reconstruction of spray structures was made. The background of computed tomography is described along with some experimental results of the structure of intermittent spray such as diesel spray.

Nakayama, Mitsushige↗

DOE OSTI2024

Alpha-Quartz Plastic Strength Investigation Via Diffraction Experiments on Novaculite Using A D-Dia and Elastic Plastic Self- Consistent Interpretation [Thesis}

X-Ray Tomography. Porosity is commonly measured using mercury injection (MI) or water immersion porosimeter (WIP). Both MI and WIP utilize pressure to fill open voids with mercury or water respectively. A measure of the volume change of the sample is then used to estimate the percentage of open voids. However, for the purpose of rheological study it is important to get an accurate measure of open and closed voids. X-ray tomography has been selected as it offers a three-dimensional view into the sample that can quantify all pores limited only by the voxel size which is in the micron range for this study. Radiographs for tomography were collected at the Material Science and Technology Division at Los Alamos National Lab using the Carl Zeiss Xradio 520 instrument and Scout-and-Scan version 16.1 operating software. Two samples were imaged, the starting material and the deformed sample SiO2_65. 3001 radiographs were taken of the starting material with a 6 second exposure time using a 4x objective lens. The x-ray beam was set to 60 kilovoltage peak (kVp) and 5 watts. 1901 radiographs were taken of SiO2_65 with a 25 second exposure time using a 10x objective lens. The x-ray beam was set to 80 kVp and 7 watts. Radiograph files were analyzed by Brian Patterson using Avizo. Void and inclusion volumes were output by voxel sized (1.03 μm) slices, used to calculate a total percentage volume for the starting material.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Protein Data Bank: A Comprehensive Review of 3D Structure Holdings and Worldwide Utilization by Researchers, Educators, and Students

The Research Collaboratory for Structural Bioinformatics Protein Data Bank (RCSB PDB), funded by the United States National Science Foundation, National Institutes of Health, and Department of Energy, supports structural biologists and Protein Data Bank (PDB) data users around the world. The RCSB PDB, a founding member of the Worldwide Protein Data Bank (wwPDB) partnership, serves as the US data center for the global PDB archive housing experimentally-determined three-dimensional (3D) structure data for biological macromolecules. As the wwPDB-designated Archive Keeper, RCSB PDB is also responsible for the security of PDB data and weekly update of the archive. RCSB PDB serves tens of thousands of data depositors (using macromolecular crystallography, nuclear magnetic resonance spectroscopy, electron microscopy, and micro-electron diffraction) annually working on all permanently inhabited continents. RCSB PDB makes PDB data available from its research-focused web portal at no charge and without usage restrictions to many millions of PDB data consumers around the globe. It also provides educators, students, and the general public with an introduction to the PDB and related training materials through its outreach and education-focused web portal. This review article describes growth of the PDB, examines evolution of experimental methods for structure determination viewed through the lens of the PDB archive, and provides a detailed accounting of PDB archival holdings and their utilization by researchers, educators, and students worldwide.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2020

Ptychographic atomic electron tomography: Towards three-dimensional imaging of individual light atoms in materials

Through numerical simulations, we demonstrate the combination of ptychography and atomic electron tomography as an effective method for low dose imaging of individual low-Z atoms in three dimensions. After generating noisy diffraction patterns with multislice simulations of an aberration-corrected scanning transmission electron microscope through a 5-nm zinc-oxide nanoparticle, we have achieved three-dimensional (3D) imaging of individual zinc and oxygen atoms and their defects by performing tomography on ptychographic projections. The methodology has also been simulated in 2D materials, resolving individual sulfur atoms in vertical WS 2 /WSe 2 van der Waals heterostructure with a low total electron dose where annular-dark-field images fail to resolve. Overall, we envision that the development of this method could be instrumental in studying the precise 3D atomic structures of radiation sensitive systems and low-Z atomic structures such as 2D heterostructures, catalysts, functional oxides, and glasses.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2016

Analysis of compositional uniformity in Al{sub x}Ga{sub 1−x}N thin films using atom probe tomography and electron microscopy

Calculated frequency distributions of atom probe tomography reconstructions (∼80 nm field of view) of very thin Al{sub x}Ga{sub 1−x}N (0.18 ≤ x ≤ 0.51) films grown via metalorganic vapor phase epitaxy on both (0001) GaN/AlN/SiC and (0001) GaN/sapphire heterostructures revealed homogeneous concentrations of Al and chemically abrupt Al{sub x}Ga{sub 1−x}N/GaN interfaces. The results of scanning transmission electron microscopy and selected area diffraction corroborated these results and revealed that neither superlattice ordering nor phase separation was present at nanometer length scales.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2024

Pore Structures in Detritusphere of Soils Under Switchgrass and Restored Prairie Vegetation Community

Root detritusphere, that is, the soil in the vicinity of decomposing root residues, plays an important role in soil microbial activity and C sequestration. Pore structure (size distributions and connectivity of soil pores) in the detritusphere serves as a major driver for these processes and, in turn, is influenced by the physical characteristics of both soil and roots. This study compared pore structure characteristics in the root detritusphere of soils of contrasting texture and mineralogy subjected to > 6 years of contrasting vegetation: monoculture switchgrass and polyculture prairie systems. Soil samples were collected from five experimental sites in the US Midwest representing three soil types. Soil texture and mineralogy were measured using a hydrometer and x-ray powder diffraction, respectively. The intact cores were scanned with x-ray computed micro-tomography to identify visible soil pores, biopores, and particulate organic matter (POM). We specifically focused on pore structure within the detritusphere around the POM of root origin. Results showed that the detritusphere of coarser textured soils, characterized by high sand and quartz contents, had lower porosity in the vicinity of POM compared with finer textured soils. POM vicinities in finer textured soils had high proportions of large (> 300 μm diameter) pores, and their pores were better connected than in the coarser soils. Lower porosity in the outer (> 1 mm) parts of the detritusphere of switchgrass than of prairie suggested soil compaction by roots, with the effect especially pronounced in the coarser soils. Here, the results demonstrated that soil texture and mineralogy played a major, while vegetation played a more modest, role in defining the pore structure in the root detritusphere.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2017

A combined APT and SANS investigation of α' phase precipitation in neutron-irradiated model FeCrAl alloys

Here, FeCrAl alloys are currently under consideration for accident-tolerant fuel cladding applications in light water reactors owing to their superior high-temperature oxidation and corrosion resistance compared to the Zr-based alloys currently employed. However, their performance could be limited by precipitation of a Cr-rich α' phase that tends to embrittle high-Cr ferritic Fe-based alloys. In this study, four FeCrAl model alloys with 10–18 at.% Cr and 5.8–9.3 at.% Al were neutron-irradiated to nominal damage doses up to 7.0 displacements per atom at a target temperature of 320 °C. Small angle neutron scattering techniques were coupled with atom probe tomography to assess the composition and morphology of the resulting α' precipitates. It was demonstrated that Al additions partially destabilize the α' phase, generally resulting in precipitates with lower Cr contents when compared with binary Fe-Cr systems. The precipitate morphology evolution with dose exhibited a transient coarsening regime akin to previously observed behavior in aged Fe-Cr alloys. Similar behavior to predictions of the LSW/UOKV models suggests that α' precipitation in irradiated FeCrAl is a diffusion-limited process with coarsening mechanisms similar to those in thermally aged high-Cr ferritic alloys.

36 MATERIALS SCIENCE↗

DOE OSTI2026

In-Situ Visualization of a Growing Brittle Crack in Aluminum Oxynitride Using Synchrotron X-Rays and the Double-Cleavage Drilled Compression Geometry

Brittle fracture is difficult to study in situ due to the speed of a growing crack and the often-catastrophic nature of failure in brittle materials. As a result, the influence of microstructural considerations, such as orientation, grain boundary locations, and strain field, on the crack path remains poorly understood. Presented in this study is a method addressing this knowledge gap, which utilizes the double-cleavage drilled compression geometry to achieve quasi-stable fracture in aluminum oxynitride (AlON). Synchrotron X-ray micro-computed tomography is used to characterize the crack shape and length, while high-energy diffraction microscopy provides information on the strains, orientations, and shapes of grains in the microstructure surrounding the crack tip. During testing, the crack grew in discrete and irregular jumps while the fracture toughness falls within reported ranges. The crack in AlON is found to have no greater tendency to crack intergranularly as compared to transgranularly, and grains which are cracked transgranularly do not display a trend in orientation or stress when compared to those around which the crack followed a grain boundary. The high resolution of the crack path and microstructural data provides a path forward for modeling and understanding 3D brittle fracture.

Gorske, Sara F.↗

DOE OSTI2024

Formation of uranium nitride nanoparticles via mechanical alloying of uranium-molybdenum alloy fuels in gaseous nitrogen

Uranium-molybdenum (U-Mo) alloys show promise as a nuclear fuel system due to their high thermal conductivity and fuel loading capability. However, U-Mo systems are susceptible to irradiation induced swelling ultimately affecting the cladding via mechanical and chemical interactions. To address these shortcomings, this research investigated the formation of uranium mononitride (UN) nanoparticles within a 90 wt% U/10 wt% Mo (U-10Mo) matrix to act as a prospective defect sink for fission products at nanometric hetero-interfaces. To promote the formation of UN, U-10Mo powders were mechanically alloyed under a high purity nitrogen atmosphere. Variations of the milling process investigated included media size, duration of milling, and number of times the milling jar was re-aerated with nitrogen gas. Characterization of the fuel microstructure was completed using light element analysis, X-ray diffraction, scanning and transmission-electron microscopy, electron energy loss spectroscopy, and atom probe tomography. UN nanoparticles measuring 1–5 nm in radius were observed in the U-Mo matrix as early as 1 h into the mechanical alloying process. Milling time in excess of 10 h was found to lead to deleterious effects induced by the stainless-steel milling media.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2018

Meta-equilibrium transition microstructure for maximum austenite stability and minimum hardness in a Ti-stabilized supermartensitic stainless steel

We report that the maximization of stable reverted austenite at room temperature through inter-critical tempering is a widely used method to reduce hardness in supermartensitic stainless steels. Nevertheless, partial martensitic transformation might occur due to insufficient compositional stabilization. In this work, we conducted a time-resolved triple-step inter-critical tempering, specially designed to obtain maximum austenite stability and minimum hardness through the progressive suppression of the martensitic transformation. The mechanism behind the progressive increase in stable reverted austenite was the generation of a meta-equilibrium state, which imposed a limit in both high temperature austenite reversion and room temperature austenite stabilization. Such limit corresponded to the high temperature volume fraction of austenite, obtained right before cooling from the first cycle. Additionally, this effect was associated to the Ni-rich fresh martensite laths acting as local Ni compositional pockets, providing site-specific austenite reversion; and to the suppression of any additional nucleation at the Ni-poor matrix as the T0 temperature for austenite reversion was strongly increased. The softening mechanism was mainly controlled by the carbon arrest effect by the precipitation of Ti (C, N), which was completed after the first tempering cycle. Nevertheless, maximizing reverted austenite and suppressing fresh martensite at room temperature did not result in additional hardness reductions.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Effects of Neutron Irradiation on the Micro/Nano Scale Structure and Fission Product Distribution of TRISO Coated Particle Fuel Kernels from AGR Experiments

The Advanced Reactor Technologies (ART) Program at Idaho National Laboratory (INL) includes the Advanced Gas Reactor (AGR) fuel development and qualification program that consists of fuel fabrication, experiment irradiations, post-irradiation examination (PIE) and safety testing to assess tristructural isotropic (TRISO) fuel performance during normal irradiation and under potential accident conditions. Advanced microscopy work on selected AGR-1 and AGR-2 unirradiated and irradiated fuel specimens is performed as part of the PIE effort. PIE work on fuel from the first experiment irradiation, AGR-1, began at INL in April 2010, and AGR-2 PIE began at INL in July 2014. This work scope includes University of Florida (UF) performing advanced electron microscopy examination and analysis using facilities at the Center for Advanced Energy Studies (CAES), INL or UF’s electron microscopy facilities. Electron microscopic examination and analysis may include scanning transmission electron microscopy (STEM), transmission electron microscopy (TEM), selected area diffraction (SAD), electron energy loss spectroscopy (EELS), electron dispersive spectroscopy (EDS) and atom probe tomography (APT) on the fuel kernels of TRISO-coated fuel particles. The electron microscopy lamellae will be provided by INL and will be available at CAES or Irradiated Materials Characterization Laboratory (IMCL).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS2009

Spatial Modulation Improves Performance in CTIS

Suitably formulated spatial modulation of a scene imaged by a computed-tomography imaging spectrometer (CTIS) has been found to be useful as a means of improving the imaging performance of the CTIS. As used here, "spatial modulation" signifies the imposition of additional, artificial structure on a scene from within the CTIS optics. The basic principles of a CTIS were described in "Improvements in Computed- Tomography Imaging Spectrometry" (NPO-20561) NASA Tech Briefs, Vol. 24, No. 12 (December 2000), page 38 and "All-Reflective Computed-Tomography Imaging Spectrometers" (NPO-20836), NASA Tech Briefs, Vol. 26, No. 11 (November 2002), page 7a. To recapitulate: A CTIS offers capabilities for imaging a scene with spatial, spectral, and temporal resolution. The spectral disperser in a CTIS is a two-dimensional diffraction grating. It is positioned between two relay lenses (or on one of two relay mirrors) in a video imaging system. If the disperser were removed, the system would produce ordinary images of the scene in its field of view. In the presence of the grating, the image on the focal plane of the system contains both spectral and spatial information because the multiple diffraction orders of the grating give rise to multiple, spectrally dispersed images of the scene. By use of algorithms adapted from computed tomography, the image on the focal plane can be processed into an image cube a three-dimensional collection of data on the image intensity as a function of the two spatial dimensions (x and y) in the scene and of wavelength (lambda). Thus, both spectrally and spatially resolved information on the scene at a given instant of time can be obtained, without scanning, from a single snapshot; this is what makes the CTIS such a potentially powerful tool for spatially, spectrally, and temporally resolved imaging. A CTIS performs poorly in imaging some types of scenes in particular, scenes that contain little spatial or spectral variation. The computed spectra of such scenes tend to approximate correct values to within acceptably small errors near the edges of the field of view but to be poor approximations away from the edges. The additional structure imposed on a scene according to the present method enables the CTIS algorithms to reconstruct acceptable approximations of the spectral data throughout the scene.

Bearman, Gregory H.↗