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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 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

In-service corrosion and grain boundary oxidation in neutron-irradiated 316 stainless steel baffle-former bolts

Reactor core internal components such as baffle-former bolts (BFBs) are subjected to significant mechanical stress, corrosive environment, and neutron irradiation from the reactor core during the plant operation. Over the long operation period, these conditions lead to potential degradation and of the bolts. In this work, characterization was performed on the oxidized surface of stainless steel BFBs harvested from a commercial pressurized water reactor (PWR) after 40 years of operation. The analysis shows that a complex multilayered surface oxide with six identified layers formed that is different from 2-layer structure commonly observed in model experiments. The oxide varies by composition – predominantly Fe, Cr, and Ni, grain size, and phase, and has features resembling both unirradiated and radiation/ corrosion experiments likely due to the low radiation flux compared to ion-irradiation or the test reactor radiation. In addition, grain boundary oxidative attack featured a pathway for Fe and other elements to move from the metal matrix to the outermost oxide. In conclusion, the results help assess PWR lifetime extension, put into context previous experimental studies, and provide input for designing experiments combining radiation and corrosion effects.

Baffle-former bolt↗
DOE OSTI2022

Using lifetime of point defects for dislocation bias in bcc Fe

The interaction between dislocations and point defects is key to deformation processes and microstructural evolution of structural materials. In this work, we compute the lifetime of point defects to describe their interaction with dislocations. This approach can accurately account for the effects of the dislocation core and anisotropic defect dynamics to accumulatively determine the capture efficiency, sink strength, and dislocation bias at different temperatures and dislocation densities. Particularly, the absorption of point defects by straight screw and edge dislocations in a model bcc iron system is studied. The maximum swelling rates based on the obtained bias factors are in close agreement with a variety of experimental measurements, including both neutron and ion-irradiation data, especially when considering the survival fraction for point defects from displacement cascades. Further, this approach applies to many other processes and sinks, such as dislocation loops and interfaces, providing a powerful means to develop fundamental insights critical for improving radiation resistance and mechanical properties of structural materials through controlling defect interaction and evolution.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Plasticity in irradiated FeCrAl nanopillars investigated using discrete dislocation dynamics

Here, in this paper, we investigate plasticity in irradiated FeCrAl nanopillars using discrete dislocation dynamics simulations (DDD), with comparisons to transmission electron microscopic (TEM) in situ tensile tests of ion- and neutron-irradiated commercial C35M FeCrAl alloy. The effects of irradiation-induced defects, such as a/2<111> and a<100> type loops and composition fluctuations representative of phase separation in irradiated FeCrAl alloys, are investigated separately as well as superposed together in simulations. We explore the effects of defects on the stress-strain behavior, specifically yield strength and hardening response, of FeCrAl nanopillars. Our simulations confirm the widely accepted fact that irradiated alloys exhibit a stress-strain response with higher yield strength as compared to unirradiated alloys. However, our DDD calculations reveal an atypical superposition of the hardening contributions due to composition inhomogeneity and irradiation loops wherein composition inhomogeneity annihilates the hardening due to irradiation loops at small scales. As a result, we observe that the yield strength in irradiated alloys, after taking into consideration the effects of both composition inhomogeneity and irradiation loops, is smaller than the yield strength of the alloys with only irradiation loops and is approximately same for the alloy with composition inhomogeneity alone. This is referred to as “destructive interference” between the hardening contributions due to composition fluctuations and irradiation loops in the paper. We also identify this destructive interference in the superposition in our parallel TEM in situ tensile tests on unirradiated, ion-irradiated, and neutron-irradiated C35M FeCrAl alloy. This destructive interference in the hardening contributions contrasts with the dispersed barrier hardening (DBH) models widely utilized by the experimental community to model the hardening contributions due to different irradiation induced defects. The effects of the loading orientations on the yield strength and hardening are investigated and the mechanisms for the hardening in irradiated FeCrAl alloys are also reported.

36 MATERIALS SCIENCE↗
DOE OSTI2022

The effect of helium on cavity swelling in dual-ion irradiated Fe and Fe-10Cr ferritic alloys

We report Ferritic-martensitic (FM) steels for in-vessel components in proposed fusion reactors are expected to suffer from high levels of displacement damage and helium (He) generation by neutron transmutation. However, a thorough understanding of the He synergistic effects on the cavity swelling in FM steels is still not well established. To gain fundamental insights into the He effect on cavity swelling, high purity Fe and Fe-10 wt.% Cr ferritic model alloys were irradiated with 8 MeV Ni ions and co-implanted He ions at 400 to 550 °C up to 30 displacements per atom (dpa) with He implantation rates of 0.1, 10 and 50 appm He/dpa. The current study focuses on the 50 appm He/dpa, 500 °C behavior vs. 0.1 and 10 appm He/dpa. Irradiation-induced defects, including cavities, dislocation loops, and dislocation networks were characterized using transmission electron microscopy (TEM). In the grain interior, a bimodal cavity size distribution was observed in the 10 and 50 appm He/dpa samples, but not for 0.1 appm He/dpa. Cavity swelling was maximized at intermediate He implantation rates of ~10 appm He/dpa for both ion-irradiated Fe and Fe-10Cr alloys. The cavity swelling behavior as a function of He implantation rate appears to be controlled by the He/dpa-dependent variation of cavity sink strengths. Treating small bubbles as biased sinks for interstitial absorption can significantly increase the ratio of biased to unbiased sink strengths (Q) and results in maximized cavity swelling for a Q ratio close to one.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Flash electropolishing of BCC Fe and Fe-based alloys

The preparation of transmission electron microscopy (TEM) samples is a critical step in the characterization of materials, and the focused ion beam (FIB) technique is a commonly used method. However, a significant limitation of this technique is the FIB-induced damages on the foil surfaces, which can obscure the real features of interest, particularly in radiation effects studies. To overcome this limitation, this study presents a detailed description of the flash electropolishing technique, which can be used to remove the FIB damage from samples. The flash electropolishing technique has been successfully applied to a range of materials, including Fe, Fe-based model alloys, commercial Fe-Cr alloys, and advanced Fe-Cr alloys, both in their as-received and ion-irradiated states. Furthermore, the parameters used for Fe-Cr model alloys can be adjusted for commercial and advanced alloys with minimal modifications. Further, the study also examined the effects of electropolishing variables, such as perchloric acid concentration, electropolishing temperature, Cr concentration, and voltage. Qualitatively, a general trend and scoping test strategy is explored in our experiments. Overall, the flash electropolishing technique offers a promising solution to the challenges posed by FIB-induced damages in the preparation of TEM samples.

36 MATERIALS SCIENCE↗
DOE OSTI2024

In-situ kinetic study of irradiation induced crystallization in amorphous Al 2 O 3

In the last ten years amorphous alumina coatings, deposited by Pulsed Laser Deposition, emerged as potential key enabling technology in the fields of heavy liquid metal fast reactors (lead and lead-bismuth) and fusion. In the former, as coating of the steel fuel cladding and in the latter as multifunctional coating providing a barrier against tritium permeation, steel corrosion and electrical insulation. Nevertheless, a detailed knowledge of the behavior of this thermodynamically metastable material at high temperatures and under neutron irradiation is still unknown. A knowledge gap that is mandatory to fill up for the deployment of this barrier technology. In the present work, we present a first step towards this goal, by the in-situ dynamic observation of the radiation induced crystallization processes of thin films of amorphous Al 2 O 3 , induced by ion-irradiation over an extensive range of temperatures (400-800 °C). The study was performed at the Intermediate Voltage Electron Microscope (IVEM)-Tandem Facility at Argonne National Laboratory. The experimental findings allow to elucidate the dependence of the grain growth on ion dose and temperature. A kinetic approach has been used to derive the process activation energies and other important parameters.

36 MATERIALS SCIENCE↗
DOE OSTI2026

A dual dynamic shutter system for accelerating ion irradiation sample throughput via lateral gas implantation gradients

Ion irradiation for material performance testing is limited due to its serial nature, which allows for only one value of the implantation (appm) versus dose (dpa) parameter space to be explored for each ion and experiment at a time. While ion irradiation can accelerate the process by up to three orders of magnitude compared to neutron irradiation experiments, the sample throughput for ion irradiation remains relatively low. To address these limitations, a novel capability has been developed at the Michigan Ion Beam Laboratory (MIBL), enabling for the creation of single- and two-dimensional lateral ion implantation gradients using recently installed motorized-controlled ion-beam shutters. This advancement can generate a wide scope of the two-dimensional (H+, He2+) implantation parameter space within a single sample. Integration of this new capability now allows for dual- and triple-ion beam experiments to be performed with full user control over not only the ion implantation depth, but also laterally across the sample by imposing ion implantation concentration gradients, thus providing researchers with a high-throughput means for material testing under various irradiation conditions. Furthermore, recent improvements in MIBL's microbeam ion-beam analysis (IBA) target station now allow for probing these concentration gradients in irradiated alloys with exceptional spatial resolution, down to 10 µm. These two approaches promise to significantly improve ion irradiation capabilities and increase the sample throughput by several orders of magnitude. The application of the shutter technique plus the subsequent microbeam characterization of the imposed implantation gradients are showcased by two proof-of-principle ion-irradiated experiments, one performed on single-crystal Si and the other on the fusion-candidate alloy F82H-IEA. These advancements mark a substantial leap in ion-beam technology, offering researchers a robust, high-throughput method to efficiently investigate candidate alloys with high technological readiness for both advanced fission and fusion reactor applications, in a time- and cost-effective manner.

36 - MATERIALS SCIENCE↗
DOE OSTI2022

Effects of Au2+ irradiation induced damage in a high-entropy pyrochlore oxide single crystal

Here, we report an ion-irradiation study of a compositionally complex (high-entropy) pyrochlore oxide. The damage produced from 4 MeV Au 2+ ion irradiation on single crystal (Yb 0.2 Tm 0.2 Lu 0.2 Ho 0.2 Er 0.2 ) 2 Ti 2 O 7 aligned along the [100] direction is investigated at room temperature by Rutherford backscattering spectrometry in channeling mode (RBS/C). Damage profiles based on RBS/C are presented and compared to single-component pyrochlore titanate oxides to evaluate the relative resistance to irradiation-induced amorphization. The results show that this high-entropy pyrochlore goes amorphous at a dose of 0.13 dpa, which is comparable to that of single-component pyrochlores previously studied. Transmission electron microscopy images unveil the damaged surface layer, which is consistent with the RBS/C results.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Physics-based reward driven image analysis in microscopy

The rise of electron microscopy has expanded our ability to acquire nanometer and atomically resolved images of complex materials. The resulting vast datasets are typically analyzed by human operators, an intrinsically challenging process due to the multiple possible analysis steps and the corresponding need to build and optimize complex analysis workflows. We present a methodology based on the concept of a Reward Function coupled with Bayesian Optimization, to optimize image analysis workflows dynamically. The Reward Function is engineered to closely align with the experimental objectives and broader context and is quantifiable upon completion of the analysis. Here, cross-section, high-angle annular dark field (HAADF) images of ion-irradiated (Y, Dy)Ba 2 Cu 3 O 7–δ thin-films were used as a model system. The reward functions were formed based on the expected materials density and atomic spacings and used to drive multi-objective optimization of the classical Laplacian-of-Gaussian (LoG) method. These results can be benchmarked against the DCNN segmentation. This optimized LoG* compares favorably against DCNN in the presence of the additional noise. We further extend the reward function approach towards the identification of partially-disordered regions, creating a physics-driven reward function and action space of high-dimensional clustering. We pose that with correct definition, the reward function approach allows real-time optimization of complex analysis workflows at much higher speeds and lower computational costs than classical DCNN-based inference, ensuring the attainment of results that are both precise and aligned with the human-defined objectives.

47 OTHER INSTRUMENTATION↗
DOE OSTI2022

Thermal conductivity evaluation of ion irradiated Si 3 N 4 and ZrN ceramics using spatial domain thermoreflectance

Nitride ceramics have been investigated for different applications in the nuclear industry, such as space nuclear power, fusion reactor diagnostics and plasma heating, inert matrix fuels, and accident tolerant fuels. Although thermal conductivity remains one of the most important properties to track following irradiation, traditional techniques such as laser flash and xenon flash are limited to bulk sample characterization, which requires lengthy and cost-consuming neutron irradiation. This work used spatial domain thermoreflectance (SDTR) for the micrometer-scale measurement of thermal conductivity in 15 MeV Ni ion-irradiated silicon nitride and zirconium nitride from 1 to 50 dpa and 300 to 700 °C. Here, the SDTR-measured unirradiated thermal conductivity was found to be consistent with the published data on bulk samples. Electrically conductive ZrN exhibits modest reduction after irradiation which is minimal at the highest irradiation temperatures. In electrically insulating Si 3 N 4 , the reduction is more significant and unlike ZrN, the reduction remains significant even at a higher irradiation temperature. The thermal resistance evolution following irradiation was compared with lattice swelling, which was determined using grazing incidence x-ray diffraction, and radiation-induced defects were observed using transmission electron microscopy. A saturation value was observed between 15 and 50 dpa for thermal conductivity degradation in both nitride ceramics and a direct correlation with high-temperature defect recombination was observed, as well as the potential presence of additional carrier scattering mechanisms.

36 MATERIALS SCIENCE↗
DOE OSTI2024

The self-annealing of irradiation induced defects in magnetite Fe 3 O 4 : Revealing reversible irradiation-induced disorder transformation through in situ TEM

This work reports heavy ion-irradiation effects in polycrystalline Fe 3 O 4 . For this matter, Fe/Fe 3 O 4 heterostructures were irradiated in situ in a transmission electron microscopy with 1 MeV Kr ions at 50 K. Evidence of cubic to monoclinic transformation (a.k.a Verwey transition) was recorded in some magnetite grains upon cooling the sample (around 90 K); however, most of the oxide grains retain their cubic spinel structure. Irradiation effects were analyzed in the cubic phase up to a maximum dose of 38 dpa without the sign of amorphization. The extinction of first-order reflections was recorded at doses below 1 dpa, indicating the formation of a new (metastable) phase with half of the lattice parameters compared to the unirradiated Fe 3 O 4 crystal. The formation of the new crystalline phase, which also presents a high resistance to amorphization, is related to the disordering of the cation lattice and the high mobility of the cation interstitials. The metastable phase readily recovers around 225 K during the natural warming of the sample from 50 K to room temperature.

Atom irradiation effects↗
DOE OSTI2025

Neutron Total Scattering Analysis of Materials for the Nuclear Fuel Cycle

Here, this paper reviews recent experimental efforts at the University of Tennessee and Oak Ridge National Laboratory to comprehensively characterize the structural details of materials relevant for the nuclear fuel cycle by employing advanced neutron scattering techniques. For the study of nuclear ceramics, neutron scattering offers distinct advantages over traditional laboratory or synchrotron X-ray diffraction, including enhanced sensitivity to elements with a low atomic mass, such as oxygen, nitrogen, and carbon. The key to these efforts is the recent advancement in the neutron scattering infrastructure at the high-flux diffractometers at the Spallation Neutron Source. The high neutron flux at these instruments enables neutron total scattering, a nondestructive bulk technique that simultaneously captures both short-range structural effects through pair distribution function analysis and long-range order through diffraction pattern analysis. This approach is particularly important for a comprehensive description of defective, disordered, or amorphous nuclear materials. The case studies presented here include analyses of the local defect structure in hyperstoichiometric uranium oxides and short-range order of ion-irradiated ceramics. This advanced analytical methodology will improve our understanding of the behavior of materials in extreme environments and contribute to the development of more resilient nuclear materials.

Neutron scattering↗
DOE OSTI2024

An In Situ transmission electron microscopy study on the synergistic effects of Au-ion irradiation and high temperature on nuclear graphite microstructure

Abstract The combined effects of high-temperature and heavy-ion irradiation on Mrozowski cracks (MC) and nuclear graphite crystallographic dimensions have been studied using in situ heating and in situ ion-irradiation in the transmission electron microscope (TEM). Electron transparent lamella of nuclear graphite, IG-110, was irradiated using a 2.8 MeV Au beam at an ion flux of 3.991 ×10 10 ion cm −2 s −1 for 70 min at 800 °C. Upon high-temperature irradiation, Mrozowski crack closure was studied quantitatively. The analysis showed linear, positive expansion of nuclear graphite which is significantly different from the dimensional changes previously reported for low-dose neutron irradiation of nuclear graphite in which the material undergoes negative to positive expansion via a turnaround radiation dose. The trend of the thermal expansion coefficient (CTE) of pristine IG-110 in this study is consistent with previous reports in the 100 °C–800 °C temperature region in which the dimensional change ranges from negative to positive values.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Phase composition of polycrystalline HfNx (0.45 ≤ x ≤ 1.60) and effects of low-energy ion irradiation on microstructure, texture, and physical properties

We have investigated the phase composition of HfNx as a function of x and the effects of low-energy ion irradiation on the microstructure and physical properties of polycrystalline layers grown on SiO2 at 350 °C by ultrahigh vacuum reactive dc magnetron sputtering of Hf in mixed N2/Ar discharges. X-ray diffraction and Rutherford backscattering spectrometry results show that the phases obtained in polycrystalline HfNx layers with increasing x are hcp-structure α-Hf:N (x ≲ 0.6); multiphase mixtures consisting of α-Hf, NaCl-structure δ-HfN, rhombohedral ɛ-Hf3N2, and/or ζ-Hf4N3 (0.6 ≲ x ≲ 0.9); δ-HfN single phase (0.9 ≲ x ≲ 1.3); and mixtures of δ-HfN and higher nitrides (x ≳ 1.3). HfNx layers with 0.9 ≲ x ≲ 1.2 grown under mild ion irradiation (incident ion energy Ei ≃ 7 eV and ion-to-Hf flux ratios Ji/JHf = 1−3) are underdense with mixed orientation, low in-plane stress, and rough surface morphology due to limited adatom mobilities resulting in kinetic roughening and atomic shadowing during film growth. However, the use of intense ion irradiation (Ei = 25 eV and Ji/JHf = 4−20) results in HfNx layers, which are fully dense with strongly 111-oriented texture, compressive in-plane stress, and smooth surfaces due to ion irradiation enhanced adatom surface mobilities. In addition, the latter films have lower resistivity and higher hardness. For stoichiometric δ-HfN layers, ρ decreases from 69.7 to 35.2 μΩ cm and H increases from 22.1 to 27.4 GPa, with increasing ion-irradiation intensity. However, for HfNx layers with 1.2 ≲ x ≲ 1.6, the correspondingly higher steady state atomic N surface coverages during deposition alter growth kinetics in favor of 001 texture with a fully dense structure and compressive in-plane stress.

Materials Science↗
DOE OSTI2022

Irradiation-induced grain boundary facet motion: In situ observations and atomic-scale mechanisms

Metals subjected to irradiation environments undergo microstructural evolution and concomitant degradation, yet the nanoscale mechanisms for such evolution remain elusive. Here, we combine in situ heavy ion irradiation, atomic resolution microscopy, and atomistic simulation to elucidate how radiation damage and interfacial defects interplay to control grain boundary (GB) motion. While classical notions of boundary evolution under irradiation rest on simple ideas of curvature-driven motion, the reality is far more complex. Focusing on an ion-irradiated Pt Σ3 GB, we show how this boundary evolves by the motion of 120° facet junctions separating nanoscale {112} facets. Our analysis considers the short- and mid-range ion interactions, which roughen the facets and induce local motion, and longer-range interactions associated with interfacial disconnections, which accommodate the intergranular misorientation. We suggest how climb of these disconnections could drive coordinated facet junction motion. These findings emphasize that both local and longer-range, collective interactions are important to understanding irradiation-induced interfacial evolution.

74 ATOMIC AND MOLECULAR PHYSICS↗
DOE OSTI2025

Atomic-scale structure of ZrO 2 : Formation of metastable polymorphs

Metastable phases can exist within local minima in the potential energy landscape when they are kinetically “trapped” by various processing routes, such as thermal treatment, grain size reduction, chemical doping, interfacial stress, or irradiation. Despite the importance of metastable materials for many technological applications, little is known about the underlying structural mechanisms of the stabilization process and atomic-scale nature of the resulting defective metastable phase. Investigating ion-irradiated and nanocrystalline zirconia with neutron total scattering experiments, we show that metastable tetragonal ZrO 2 consists of an underlying structure of ferroelastic, orthorhombic nanoscale domains stabilized by a network of domain walls. The apparent long-range tetragonal structure that can be recovered to ambient conditions is only the configurational ensemble average of the underlying orthorhombic domains. This structural heterogeneity with a distinct short-range order is more broadly applicable to other nonequilibrium materials and provides insight into the synthesis and recovery of functional metastable phases with unique physical and chemical properties.

74 ATOMIC AND MOLECULAR PHYSICS↗
DOE OSTI2025

Mesoscale Modeling of Dislocation Cell Structure Evolution and Radiation-Induced Segregation in Additively Manufactured Austenitic Stainless Steel

Structural alloys under irradiation develop radiation-induced segregation (RIS) at point defect sinks, which lead to undesired changes in the alloy's properties. Additively manufactured austenitic stainless steels are expected to yield a distinct response to irradiation damage owing to their unique as-printed dislocation cell structure. In this talk, we present the development of a mesoscale model for dislocation cell structure evolution coupled with RIS using the MOOSE framework. The evolution of network dislocations within spatially distinct cells and cell walls are modeled using climb-mediated edge annihilation and generation processes. Starting with initial microstructures of as-printed non-equilibrium segregations at dislocation cell walls, our 2D and 3D simulations explore the effects of irradiation temperature, dose rate, dislocation sink bias, and specimen thickness on microstructure evolution. The results will be compared against experimental characterizations of in-situ and ex-situ ion-irradiated samples, and the implications of evolving cell structure on irradiation damage response will be discussed.

additive manufacturing↗
DOE OSTI2024

Experimental investigation of thermal conductivity of high entropy ceramics

In this talk, we will present the experimental investigation of thermal conductivity of high entropy carbides (HEC) and borides (HEB) with different compositions. Thermal conductivity determines the capability of a material to transport thermal energy and is considered as one critical physical property, specially in the energy industry. Due to the presences of disordered cation sublattice, it is expected that thermal conductivity of high entropy ceramics is lower than the counterparts with simpler compositions, but the experimental studies are relatively few. Using laser-based spatial-domain and frequency-domain thermoreflectance technique, we measured thermal conductivity of HECs and HEBs in a temperature range from 77K to 773K. Furthermore, by focusing the laser using an objective lens, we were able to perform the thermal property mapping on samples with the spatial resolution of micrometer. Such measurements could reveal important microstructure information in a rapid and efficient way without using scanning electron microscopy. The high spatial resolution also enables thermal conductivity measurements on ion-irradiated HECs with the damage layer of merely 1.1µm. These measurements can provide valuable information to predict the performances of HECs and HEBs with different compositions and from different manufacturing processes, and in the extreme environments such as nuclear reactors.

36 - MATERIALS SCIENCE↗