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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Dose and dose rate effects on the microstructural and mechanical stability of long-range ordered precipitates in Inconel 718

Nickel-based alloys offer exceptional mechanical properties and corrosion resistance for various applications in extreme environments such as high neutron flux, temperature, and stress. Precipitates, resulting from thermal treatments, increase the strength and creep resistance of these alloys. Here, heavy ion irradiation is shown to destabilize the γ' and γ" precipitates in Inconel 718 nickel-based alloy by disordering and dissolution processes. Transmission electron microscopy and atom probe tomography reveal that the disordering and dissolution rates of the precipitates are proportional to both irradiation dose and dose rate. Irradiation induced disordering occurs at a higher rate than the dissolution. From analyzing the hardening contributions, microscale mechanical results suggest radiation-induced disordering is responsible for the majority of the softening response at low dose. In addition, low dose radiation-induced disordering results in strain localization and is believed to be the primary cause for the drastic degradation of uniform elongation and toughness in irradiated Inconel 718.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Decoupling of strain and temperature effects on microstructural evolution during high shear strain deformation

The interplay between defect generation by shear strain and defect annihilation by local heating is difficult to predict in shear-assisted processing techniques. In this study, we decoupled the effects of high shear strain and external heating in an immiscible Cu-Nb alloy using a pin-on-disk tribometer to mimic the microstructural evolution of material during solid-phase processing. The change in sub-surface deformation, strain distribution, and redistribution of the second phase as a function of temperature were examined using transmission electron microscopy and atom probe tomography. Zener-Hollomon parameter is used to semi-quantify the deformation of Cu-Nb alloys as a function of strain and temperature.

36 MATERIALS SCIENCE↗
DOE OSTI2020

High Critical Current Density in Internally-oxidized Nb 3 Sn Superconductors and its Origin

In this paper, we report achievement of non-Cu-matrix critical current density $(J_c)$ in internally-oxidized Nb 3 Sn superconductors that surpasses the best state-of-the-art Nb 3 Sn and the $J_c$ specification of the Future Circular Collider. We then explore the mechanism of the improvement, which was believed to be caused by refined grain size. However, our experiment showed that even with similar grain size, internally-oxidized wires had significantly higher $J_c$ than non-oxidized wires. This, combined with transmission electron microscopy and atom probe tomography studies which showed a high density of intragranular nano-precipitates with suitable sizes as pinning centers in internally-oxidized wires, demonstrates a significant contribution from the nano-precipitates.

43 PARTICLE ACCELERATORS↗
DOE OSTI2022

Thermal Stability and Mechanical Properties of Cold-Sprayed Nickel-Yttria Coating

The microstructural evolution under the extreme environments imposed during cold spray deposition of cermet coatings and the microstructural recovery during post-processing annealing treatments is rather complex and not well understood. Here, Ni-Yttria cermet coatings on an SS304 substrate were produced using cold spray technique, resulting in a bimodal grain structure. The grain growth, phase stability, hardness, and wear properties are observed in as-deposited and annealed (at 400 °C) Ni-Yttria and pure Ni coatings. A multimodal microstructural characterization using electron microscopy, and atom probe tomography shows the structural and compositional stability of yttria particles and Ni grains. A fragmentation of Y-rich particles and dispersion in Ni was observed, however, no forced mixing/dissolution of Y in Ni is detected. Nano-yttria dispersed within the Ni grains slowed the grain growth during annealing. After annealing, Yttria reinforced coating was 1.5 times harder and showed better thermal and mechanical stability compared to the Ni coating.

Gwalani, Bharat↗
DOE OSTI2023

Visualizing oxygen transport pathways during intergranular oxidation in Ni-Cr

The transport paths of O during intergranular oxidation in binary Ni-Cr were investigated. To isolate the selective oxidation of Cr, oxidation was performed with a CO/CO 2 gas mixture in which the oxygen partial pressure was kept under the NiO dissociation pressure. A combination of electron microscopy and atom probe tomography (APT) was used to study the nanometer-scale details of the passivation and penetrative intergranular oxidation processes at high-energy grain boundaries. Oxygen transport towards the terminating oxidation front is elucidated with dedicated usage of oxygen tracer exchange experiments. Secondary ion mass spectroscopy and APT support classical theories of internal oxidation, revealing preferred transport paths at the oxide/alloy interface with sub-nanometer resolution.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Intergranular corrosion of Ni-30Cr in high-temperature hydrogenated water after removing surface passivating film

Abstract High-resolution transmission electron microscopy and atom probe tomography are used to characterize the initial passivation and subsequent intergranular corrosion of degraded grain boundaries in a model Ni-30Cr alloy exposed to 360 °C hydrogenated water. Upon initial exposure for 1000 h, the alloy surface directly above the grain boundary forms a thin passivating film of Cr 2 O 3 , protecting the underlying grain boundary from intergranular corrosion. However, the metal grain boundary experiences severe Cr depletion and grain boundary migration during this initial exposure. To understand how Cr depletion affects further corrosion, the local protective film was sputtered away using a glancing angle focused ion beam. Upon further exposure, the surface fails to repassivate, and intergranular corrosion is observed through the Cr-depleted region. Through this combination of high-resolution microscopy and localized passive film removal, we show that, although high-Cr alloys are resistant to intergranular attack and stress corrosion cracking, degradation-induced changes in the underlying metal at grain boundaries make the material more susceptible once the initial passive film is breached.

(S)TEM↗
DOE OSTI2023

A High-Speed Rotational Diamond Anvil Cell for In Situ Analysis of Hierarchical Microstructural Evolution of Metallic Alloys during Extreme Shear Deformation

High speed shear deformation is ubiquitous in engineering applications, ranging from material processing methods such as friction stir processing/extrusion and in tribological contacts. However, analyzing the microstructural evolution of materials while they are undergoing high speed shear deformation have been a long-standing challenge. This led to predominant reliance on ex situ microscopy before and after shear deformation. But ex situ microscopy lacks the ability to analyze dynamic and transient hierarchical microstructural evolution mechanisms that could occur during shear deformation of materials. Therefore, to better understand the dynamic mechanisms of mass and energy transfer in materials under shear deformation, we developed a first of its kind high-speed rotational diamond anvil cell (HS-RDAC) for synchrotron-based in situ high-energy x-ray diffraction (XRD). We studied the time resolved lattice strain evolution, XRD peak broadening and changes in spatial variation of shear deformation induced alloying in pure metal and metal alloy sheets and powder mixture using the HS-RDAC. These in situ results were combined with detailed ex situ microstructural characterization before and after the shear deformation using transmission electron microscopy and atom probe tomography, which revealed the different stages of evolution of a shear deformation induced hierarchical nanostructure. Multiscale computational simulations including computational fluid dynamics, crystal plasticity, molecular dynamic simulation and density functional theory uncovered the mechanisms behind morphological changes, evolution of defect structures and changes in driving force for shear deformation induced intermixing. In conclusion, this in situ HS-RDAC capability, in combination with ex situ microstructural characterization and computational simulations, can provide new insights into the hierarchical microstructural evolution pathway during shear deformation.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Post Irradiation Examination of Pressurized Water Reactor Stainless Steel Internal Components

Internal structural components of pressurized water reactors (PWR), such as baffle former bolts, are subjected to significant neutron irradiation and mechanical stresses at elevated temperatures during plant operation. Over the long operation of the power plant, these conditions lead to potential degradation and reduced load-carrying capacity of these bolts. To understand property degradation more fully, to confirm the results of experimental irradiation programs, and to predict operational lifetime performance of structural materials in internal components, post irradiation examination of harvested materials from operating nuclear reactors is required. In this work, two high fluence 316 stainless steel baffle former bolts were retrieved from a commercial Westinghouse two-loop downflow type PWR and then sectioned for analysis via mechanical testing and microstructural characterization. The irradiation damage fluctuated along the bolt length with damage levels from 15 to 41 displacements per atom with the bolt head receiving approximately twice the neutron damage levels as that of the bolt thread section. Mechanical testing evaluations showed extensive irradiation hardening and a sharp decrease in fracture toughness in all parts of the bolt, though with limited variation along the bolt length. Microstructural characterization using analytical scanning transmission electron microscopy and atom probe tomography showed significant radiation induced precipitation, segregation, and dislocation loop and cavity formation. However, unlike the mechanical behavior, there was considerable variation along the bolt length but opposite of what may be expected, with more precipitation and cavity formation in the bolt thread where the neutron radiation dose is less than in the bolt head where the neutron radiation dose is higher. The cause of this variation is likely due to gradients in temperature, neutron energy spectra, and gamma irradiation.

Lach, Tim↗
DOE OSTI2022

Microstructural Characterization of the Second High Fluence Baffle-Former Bolt Retrieved from a Westinghouse Two-loop Downflow Type PWR

As one of the pressurized water reactor (PWR) internal components, baffle-former bolts (BFBs) are subjected to significant mechanical stress and neutron irradiation from the reactor core during the plant operation. Over the long operation period, these conditions lead to potential degradation and reduced load-carrying capacity of the bolts. In support of evaluating long-term operational performance of materials used in core internal components, the Oak Ridge National Laboratory (ORNL), through the Department of Energy (DOE), Light Water Reactor Sustainability (LWRS) Program, Materials Research Pathway (MRP) has harvested two high fluence BFBs from a commercial Westinghouse two-loop downflow type PWR. The two bolts of interest, i.e. bolts # 4412 and 4416, were withdrawn from service in 2011 as part of a preventative replacement plan. No identification of cracking or potential damage was found for these bolts during their removal in 2011. However, the bolts required a lower torque for removal from the baffle structure than the original torque specified during installation. Irradiation displacement damage levels in the bolts range from 15 to 41 displacements per atom. The goal of this project is to perform detailed microstructural and mechanical property characterization of BFBs following in-service exposures. The information from these bolts will be integral to the LWRS program initiatives in evaluating end of life microstructure and properties. Furthermore, valuable data will be obtained that can be incorporated into model predictions of long-term irradiation behavior and compared to results obtained in high flux experimental reactor conditions. In this report, we present our latest study in FY22 on microstructural characterizations of the second high fluence baffle-former bolt, i.e., bolt # 4412. Analytical electron microscopy and atom probe tomography characterization were performed. The radiation-induced defects in the material add to the large wealth of knowledge for neutron-induced defects in 304/316 grades of stainless steels, specifically for radiation-induced precipitation after high fluence commercial PWR irradiation. The main findings are summarized as follows: 1) The cavity size was considerably larger in the bolt thread section than in the bolt head, with the bolt thread section having a bimodal distribution of cavities greater than ~6 nm in diameter and less than ~3 nm in diameter. The bolt head only had the small-sized cavities. In addition, there was a denuded zone of large cavities near grain boundaries in the thread section of the bolt. 2) Radiation-induced precipitation in the BFB #4412 was highly complex, with the volume fraction, size, and number density of Ni/Si and Cu-rich precipitates depending strongly on the radiation temperature/dose. In many cases, co-precipitates of adjoined clusters were found with Ni/Si-rich precipitates sandwiched between Cu-rich clusters and Mo/Cr/P-rich clusters. 3) Solute segregation out of solution was highest for most solutes in the thread section of the bolt #4412 with the exception of Cu, which experienced more separation out of solution into Curich clusters in the bolt head section. This highlights the difference in the mechanisms for precipitation of Ni/Si clusters, which have the Ni 3 Si phase composition, and precipitation of Cu-rich clusters. 4) There appear to be multiple simultaneous influences that affect the microstructural variation along the length of the bolt that overcomes the ~2X difference in irradiation dose between the bolt head and the bolt thread. The irradiation temperature, thermal/fast neutron ratio variation, potential strain gradient, and exposure to PWR coolant water that each section of the bolt sees may have more influence on the microstructural evolution than the total irradiation dose. The bolt thread and shank, with higher temperature, higher relative fast neutron flux, higher strain, and exposure to coolant but lower dose, underwent more enhanced cavity formation, precipitation, and solute segregation than the bolt head section.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
DOE OSTI2023

Oxidized structure and Compositional properties of 1144 phase FBS by analytical electron microscopy

The 1144 phase (Ae1A1Fe4As4) shows a strong advantage of engineering fabrication among Fe Iron)-based superconductor (FBS) family due to the robustness of its superconducting properties with respect to chemical inhomogeneities, granted by its uniform crystalline-layered structure. This regularity is furthermore associated to crystalline defects capable of acting as efficient pinning centers, which high critical currents achieved at high fields for these superconductors. Like other FBS phases, its lossless current-carrying capability can be remarkably degraded by distractions at grain boundaries (GBs). GB oxidation is an issue of upmost importance to the realization of the practical FBS application for high field (> 20T) magnet. In this study, we explore oxidized grain boundary and intrinsic grain structural properties of 1144 polycrystalline samples by applying analytical electron microscopy such as atomic resolution scanning transmission electron microscopy and atom probe tomography. These structural properties of samples produced by a mechanochemically assisted synthesis are evaluated following the degradation of superconducting properties due to oxidation. We observe a strong correlation between the contamination at grain boundaries and the decrease of transport properties of the bulk sample, while the crystallin structure seems to be not affected by the oxidation.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2022

Alloy Partitioning Effect on Strength and Toughness of κ-Carbide Strengthened Steels

Alloy partitioning during heat treatment in a lightweight precipitation hardened steel was investigated using transmission electron microscopy and atom probe tomography. The mechanical properties are discussed as a function of the effect of solution treatment temperature and aging time, giving rise to variations in chemical modulation. A wrought lightweight steel alloy with a nominal composition of Fe-30Mn-9Al-1Si-1C-0.5Mo (wt. %) was solution-treated between 1173–1273 K and aged at 773 K. Lower solution treatment temperatures retained a finer grain size and accelerated age hardening response that also produced an improved work hardening behavior with a tensile strength of -1460 MPa at 0.4 true strain. Atom probe tomography indicated these conditions also had reduced modulation in the Si and Al content due to the reduced aging time preventing silicon from diffusing out of the κ-carbide into the austenite. This work provides the framework for heat-treating lightweight, age hardenable steels with high strength and improved energy absorption.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Intergranular oxidation and oxygen transport in Ni-20Cr during exposure to model dry and wet oxidation environments

Selective oxidation is a critical component of the proposed internal oxidation mechanism of stress corrosion cracking (SCC) for Ni-based alloys in primary water reactor (PWR) operation. To isolate and study this process, the binary Ni-20Cr was exposed to pressurized water and a CO/CO2 gas mixture. In both environments, the oxygen potential was kept under the Ni/NiO line to stimulate penetrative intergranular attack. A combination of electron microscopy and atom probe tomography was used to study the nanometer-scale details of the passivation and penetrative intergranular oxidation processes at high-energy grain boundaries. Oxygen transport towards the terminating oxidation front is elucidated with dedicated usage of oxygen isotopic tracer exchange experiments to support classical theories of internal oxidation, revealing preferred oxygen transport paths were visualized with sub-nanometer resolution.

Weiser, Martin↗
DOE OSTI2022

Rapid assessment of interfacial stabilization mechanisms of metastable precipitates to accelerate high-temperature Al-alloy development

Precipitate strengthened high-temperature alloys are currently used in safety-critical applications. Understanding precipitate stability and solute segregation mechanisms at high temperatures is key to designing high-strength alloys. Rapid in-situ approaches, therefore, are pivotal in accelerating the alloy design process. Hereby using the test case of a promising high-temperature Al-Cu-Mn-Zr alloy, we demonstrate the value of in-situ atom probe tomography coupled with in-situ transmission electron microscopy to reveal atomic-scale mechanisms that lead to the emergence of non-equilibrium solute segregation. Mn and Zr segregation at strengthening precipitate(θ’)-matrix interface increases the kinetic barrier for phase transformation thus retaining high-temperature strength.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Microstructural Characterization of AGR-2 TRISO-coated Particle Buffer, IPyC, and Buffer-IPyC Interfaces

Investigating the microstructural, mechanical, and chemical behaviors of Tristructural Isotropic (TRISO) fuel particles is vital for its qualification and use in advanced reactors. Central to the study of TRISO particles is understanding the silicon carbide (SiC) layer's ability to confine fission products, with failure mechanisms linked to chemical degradation following mechanical degradation of the buffer and IPyC layers. Research has been done to quantify the micro-tensile properties of the buffer, inner pyrolytic carbon (IPyC), and buffer-IPyC interlayer regions and their interactions within both irradiated and un-irradiated TRISO particles. Techniques such as atom probe tomography (APT) and transmission electron microscopy (TEM) have also been deployed to examine microstructural defects and fission product distribution in detail. The goal is to understand layer delamination, establish connections between microstructure and mechanical attributes, and inform computational predictions of fuel performance. This work may help refine predictive models of TRISO fuel behavior and facilitating its certification for use in advanced reactors.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2026

Distribution of 7 Li implants in Nb films for a sterile neutrino search

The Beryllium-7 Electron capture in Superconducting Tunnel junctions (BeEST) experiment searches for sub-MeV sterile neutrinos by measuring the 7 Li recoil spectrum from 7 Be decay in Ta-based superconducting quantum sensors. Its sensitivity is limited by spectral broadening from interactions between 7 Be/ 7 Li and the Ta host material. This study investigates Nb as an alternative sensor material using scanning transmission electron microscopy (STEM) and atom probe tomography (APT) on 7 Li-implanted Nb films (∼0.5 at. %). STEM shows no 7 Li cluster formation and no implantation-induced microstructural degradation, while APT reveals some limited 7 Li segregation to grain boundaries. Although this segregation may slightly influence binding energies, it is unlikely to affect the broadening of the recoil spectrum significantly. These findings support Nb as a viable sensor material for future phases of the BeEST experiment.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Exploring structural transitions at grain boundaries in Nb using a generalized embedded atom interatomic potential

The advancement in experimental techniques, like the atom probe tomography and high resolution electron microscopy, is fueling interest in studying structural transformations of grain boundaries in metal and alloys to uncover correlations between mechanical properties and solute or impurity segregation to grain boundaries. Atomistic modeling is an important tool that can pinpoint the intricate dynamics of grain boundary phase transitions, but the lack of accurate interatomic potentials needed to simulate the complex dynamics of grain boundary structural transitions and identify different metastable phases has been the bottleneck. To this end, we use niobium as a model body centered cubic (BCC) metal and develop an interatomic potential to study grain boundary phase transitions. The potential for Nb is based on a generalization of the embedded atomic method potential and has sufficient flexibility to learn complex energy landscapes using a small set of training structures. We systematically test and validate the using data from ab initio density functional theory calculations and experiments. Using this potential, we calculate energies of multiple symmetric-tilt grain boundaries spanning a wide range of misorientation angles. Additionally, we explore different metastable structures of the Σ 27(552) [$1\overline{1}0$] grain boundary and use molecular dynamic simulations to study the coexistence of metastable phases and grain boundary transitions at finite temperature.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Oxygen Distribution and Segregation at Grain Boundaries in Nb and Ta-Encapsulated Nb Thin Films for Superconducting Qubits

We report on atomic-scale analyses of oxygen distribution and segregation at grain boundaries (GBs) of Nb and Ta-encapsulated Nb (Ta/Nb) thin films for superconducting qubits using atom probe tomography (APT) and transmission electron microscopy (TEM). We observe oxygen segregation at grain boundaries (GBs) relative to the oxygen concentration within the grains for both Nb and Ta-capped Nb thin films and find that a higher oxygen concentration in the interior of Nb grains leads to greater oxygen segregation levels at GBs. This finding reveals that the formation of a local equilibrium of oxygen concentration between GBs and grain interiors of Nb is the primary driving force of the oxygen segregation behaviors in Nb and Ta-capped Nb. The enrichment factors (CGB/Cgrain) for oxygen segregation at GBs in Nb and Ta-capped Nb range from 2.4 ± 0.3 to 2.7 ± 0.4. The current results also highlight that controlling oxygen impurities in Nb during film deposition and fabrication processing is important to concomitantly reducing the level of oxygen segregation at GBs in Nb. Finally, we find that increases in the oxygen concentration in both Nb grains and GBs correlate with a suppression in the critical temperature for superconductivity (Tc). Together, our comparative chemical and charge transport property analyses provide atomic-scale insights into a potential mechanism, contributing to the decoherence in superconducting qubits.

Lee, Jaeyel [Fermilab] (ORCID:0000000185429612)↗
DOE OSTI2021

Evolution of {delta}ferrite in a CF3 cast stainless steel upon neutron irradiation to 3, 5, 10, 20, and 40 dpa

The microstructural evolution of delta ferrite in a CF3 cast stainless steel irradiated to 3, 5, 10, 20, and 40 dpa with two dose rates was studied with atom probe tomography (APT) and transmission electron mi-croscopy. Spinodal decomposition and G-phase precipitates induced by neutron irradiation and thermal aging were quantified systematically. The neutron irradiation significantly enhances the spinodal decom-position in delta ferrite as both the spinodal wavelength (i.e. a characteristic repeat distance) and am-plitude (i.e. magnitude of elemental concentration fluctuation) increase after irradiation. The wavelength only varies slightly when the dose increases from 5 to 40 dpa, while the amplitude increases dramatically from 10 to 20 dpa and starts to saturate before 20 dpa. The dose rate and irradiation temperature also have a notable effect on the spinodal wavelength and amplitude. The study shows that higher dose rate promotes a larger wavelength at given irradiation doses. Regarding the G-phase precipitates, a slightly lower irradiation temperature would result in a smaller mean size of G-phase precipitates, while a lower irradiation dose rate would lead to a larger G-phase precipitates at a given temperature and dose. Over-all, the spinodal decomposition and G-phase precipitates in the delta ferrite continue to evolve with the increasing dose beyond 10 dpa. This study confirms that the formation of G-phase precipitates at the in-terdomain region between alpha and alpha-prime is facilitated by the Si and Mo atoms rejected from Fe rich alpha phase and the Ni and Mn atoms rejected from Cr rich alpha-prime phase. Neutron irradiation plays a dominant role in the ferrite instability, and the effect of prior thermal aging at 400 degrees C for 10,000 hours is negligible as the dose is 3 dpa and above.

duplex stainless steel↗