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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 595 records · Page 33
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Collaborative or competitive phase transformation processes in an additively manufactured-maraging steel M300

Although retained austenite is present in minor amounts in as-built additively manufactured-maraging steels, its evolution during ageing is key to controlling the final microstructure. This study investigates the relationship between austenite reversion and precipitation evolution during ageing, particularly whether these processes compete or cooperate. Using Scanning/Transmission Electron Microscopy, Atom Probe Tomography and Thermo-Calc® PRISMA simulations, the presence and evolution of retained austenite, Ni 3 Ti and Fe 7 Mo 6 intermetallic phases was characterised across different ageing conditions. Experimental results revealed the presence of non-enriched austenite in the as-built condition. Nevertheless, with increasing ageing temperature, Ni and Mo segregation became evident. High-Resolution Transmission Electron Microscopy revealed that Ni 3 Ti precipitation primarily occurred within the martensitic matrix, while Fe 7 Mo 6 nucleated preferentially at the austenite-martensite interface. PRISMA simulations indicated early and rapid precipitation in solute-enriched areas (i.e., intercellular regions), with Ni 3 Ti forming prior to Fe 7 Mo 6 . Both experimental and simulation results suggested Ni diffusion controls retained austenite growth, while Ti and Mo drive Ni 3 Ti and Fe 7 Mo 6 precipitation, respectively. The evidence reported in this work supports a both collaborative and independent phase transformation mechanism, where austenite reversion and precipitation co-evolve.

42 ENGINEERING↗
DOE OSTI2025

Residual strain and microstructure evolution in 316L stainless steel fabricated by hybrid additive/subtractive manufacturing

The extreme thermal gradients in additive manufacturing (AM) result in residual strains. Subsequent machining operations can relieve the AM strains but can introduce additional strains. AM and machining on the same platform, also called interleaving, during hybrid manufacturing has been shown to improve productivity. However, the impacts of these operations on the resulting residual strains are not well understood. In this investigation, neutron diffraction was used to measure residual strains in hybrid manufactured 316L stainless steel where blown-powder laser directed energy deposition (DED), and machining operations were interleaved in 1-inch intervals. We observe that the dominant texture developed during AM, resulting from different spot sizes and deposition parameters, significantly affects residual strain evolution. A dominant <011> texture along the build direction does not show any strain localization during interleaved deposition and machining whereas a dominant <001> texture shows strong tensile strain localization consistent with the pauses for machining at the end of AM step. Using coolant during machining can further alter the residual strain evolution. Our work shows that a combination of AM parameters and machining strategy can be used to influence the nature and magnitude of residual strains in components fabricated using convergent manufacturing technologies.

Hybrid manufacturing↗
DOE OSTI2020

Microstructural banding of directed energy deposition-additively manufactured 316L stainless steel

The microstructures of 316 L stainless steel created by rapid solidification are investigated here by comparing the similar microstructures of individual hatches of directed energy deposition additive manufacturing (DED-AM) and those of single, laser surface-melted tracks formed on a solid plate. High recoil pressure, which is exponentially dependent on the laser beam power density, induces convection of the melt pool, which causes formation of microstructural bands in the as-solidified microstructure. The microstructural bands are associated with changes in the chromium concentration and are a significant component of the inhomogeneous microstructure of DED-AM.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Dislocation loop evolution in F/M steel T91 under in-situ ion irradiation: Influence of the presence of initial dislocations

Ferritic/Martensitic (F/M) steel T91 was irradiated in-situ to 4 and 10 dpa at 470 °C using 1 MeV Kr 2+ . Additionally, the microstructure evolution under irradiation was followed and characterized by in-situ Transmission Electron Microscopy (TEM), in terms of dislocation loop Burgers vector, average size and density as a function of dose. Furthermore, the influence of the presence of dislocations in the pre-irradiated matrix was investigated by comparing the radiation induced defect evolution in grains with and without initial dislocations.

36 MATERIALS SCIENCE↗
DOE OSTI2021

In situ high-energy X-ray study of deformation mechanisms in additively manufactured 316L stainless steel

A key structural material planned to be used in the core of the Transformational Challenge Reactor is the additively manufactured 316L stainless steel (AM 316L SS). While the deformation of conventionally-manufactured 316 SS have been extensively studied, the deformation mechanism of AM 316L SS is less known. Here the room-temperature tensile behavior of AM 316L SS was studied in situ using high-energy X-ray diffraction and X-ray tomography. Diffraction yielded the lattice strains and the dislocation densi-ties of the AM 316L SS, which were compared to those of a conventionally processed 316H SS. It was found that while the conventional 316H SS had three distinct deformation stages, namely stage II ather-mal hardening, stage III dynamic recovery, and stage IV, the AM 316L experienced only the stages III and IV after an initial transitional period. The plastic instability stresses (PIS), i.e. the true ultimate tensile strength, were nearly the same in both materials. The AM 316L had very low dislocation barrier strength throughout the plastic deformation, which, in combination with the invariant PIS, explained its high dis-location storage capability and the attractive combination of strength and ductility. Tomography revealed morphological changes of the built-in pores in the AM 316L during deformation and fracture, and it was concluded that large pores close to the surface might have significant roles in the necking stage.

316 stainless steel↗
DOE OSTI2021

Correlative STEM-APT characterization of radiation-induced segregation and precipitation of in-service BWR 304 stainless steel

In this study, radiation induced segregation and precipitation phenomena in an in-service boiling water reactor 304 stainless steel component were investigated using directly correlated 3D-atom probe tomography and scanning transmission electron microscopy. Significant quantitative differences in measured segregation at grain boundaries were found between the atom probe and energy dispersive spectroscopy measurements of the exact same locations. In particular, a much stronger Si segregation (~10 atomic% via atom probe versus ~4 atomic% via electron microscopy) and different Cr profile shapes were detected that are critical to models of radiation induced segregation and stress corrosion cracking behavior. These quantitative differences highlight the need for comparative microscopy and critical evaluation of limitations in each analytical method. Elemental segregation to dislocations and conjoined-clusters were also highlighted by atom probe; confirming and expanding upon what has been observed in test reactor neutron and accelerator-based ion irradiations.

36 MATERIALS SCIENCE↗
DOE OSTI2021

In-situ ion irradiation study of alloy 709 stainless steels with different processing histories

Alloy 709 stainless steel (A709 SS) has gained an increased interest in nuclear applications due to its advanced properties at high temperatures over the widely used Type 316 SS. However, how this alloy behaves under irradiation with concurrent environmental factors, such as mechanical deformation and/or thermal annealing, has not been studied. In this work, we used in-situ ion irradiation inside a transmission electron microscope (TEM) to investigate the effects of irradiation on the microstructures of A709 SS samples with different prior processing histories, including as-received, annealed, and creep-deformed. It was found that, compared to room temperature irradiation, 600 degrees C irradiation led to larger dislocation loop sizes and lower loop densities. Furthermore, with 600 degrees C irradiation, the creep-deformed sample, which had the highest precipitate density and the highest dislocation density, had the smallest loop size and the lowest loop density compared to others. This observation has been rationalized with quantitative evaluation of the sink strength factors in each sample. This study shows that in-service deformation can significantly affect the irradiation performance in structural materials at reactor operating conditions.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Effect of heat treatment on creep behavior of 316 L stainless steel manufactured by laser powder bed fusion

The objective of this study is to understand the thermal stability of microstructure and its effect on the creep behavior of additively-manufactured 316L stainless steel (AM 316L SS). Creep specimens were fabricated from rods printed by a laser powder bed fusion process. Six different heat treatments, namely 650 °C/1 h, 700 °C/1 h, 750 °C/1 h, 800 °C/1 h, 900 °C/1 h and 1050 °C/1 h were applied to the creep specimens. The heat-treated specimens were creep-tested under the same condition, 550 °C/275 MPa to evaluate the effect of post-build heat treatment on the creep behavior of AM 316L SS. In the temperature range of 650-750 °C, dislocation density within cells, and cell size and wall thickness were affected by the heat treatment, while elemental segregation at boundaries remained unchanged and Mn-enriched Si oxide particles remained stable. In the temperature range of 750-900 °C, concurrent changes were observed in dislocation cell structures, elemental segregation and oxide particles. The 1050 °C-heat treatment removed cell structures and boundary solute segregations, leading to formation of equiaxed grains; Mn-enriched Si oxide particles in the as-built specimen were replaced by more stable Mn-enriched Cr oxides. The creep life of AM 316L SS increased after the heat treatment at 650 °C and then decreased with increasing temperature up to 900 °C where cell/subgrain structures still existed. The creep rate and creep elongation followed an opposite trend. The creep rate can be correlated with the structural parameters of cell/subgrain size and cell wall/boundary thickness and can be rationalized by different strengthening mechanisms of dislocation cells and subgrains. The heat treatment affected strongly the primary and secondary creep but had a minimal effect on the tertiary creep of AM 316L SS.

316L stainless steel↗
DOE OSTI2022

Corrosion of 316H stainless steel in flowing FLiNaK salt

In this report type 316H stainless steel samples were exposed to flowing FLiNaK salt for 1000 h in a monometallic thermal convection loop (TCL) with a maximum temperature of 650 °C and a minimum of 540 °C. Samples in the hottest part of the TCL lost mass, with a maximum mass loss of 1.4 mg/cm 2 , while samples in the coldest parts of the TCL gained mass, with a maximum mass gain of 1.0 mg/cm 2 . Analysis of the samples that gained mass showed an Fe-rich layer on the sample surfaces, indicating that Fe, not Cr, was the primary deposition product in the TCL. Cr loss was apparent to a depth of ~5 µm in the hot leg. Post-exposure analysis of the salt showed major increases in the Cr, Fe, and Mn contents. The TCL was modeled using the TRANSFORM code. Modeled values matched the experimental temperature measurements showing that TRANSFORM is capable of accurately simulating the TCL conditions.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Cavity evolution and void swelling in dual ion irradiated tempered martensitic steels

Microstructural evolutions in two variants of the F82H 8 wt%Cr tempered martensitic steel under dual (He + plus Fe 3+ ) ion irradiations at 500 °C have been characterized by transmission electron microscopy. Emphasis is on understanding the combined effects of displacements per atom (dpa) and the helium/dpa ratio (He/dpa) on cavity evolution and void swelling (f v ). The dual ion database includes 231 alloy-dpa-He/dpa conditions for irradiations up to ~ 82 dpa and 3700 appm helium. Here, we hypothesize that the large “scatter” observed in the f v data is primarily due to local microstructural variations, especially those that shield regions at shallower depths from the effects of injected interstitial atoms, which would otherwise reduce f v . More generally, our hypothesis is that the highest f v data, at a specified dpa and He/dpa, provides the most appropriate estimate of swelling for fusion neutron irradiation conditions. The dose dependence of f v can be described by an incubation dpa i , marking the onset of significant void growth, and a post-incubation swelling rate, f v ’ = Δf v /Δdpa. Both dpa i and f v ’ decrease with increasing He/dpa. The f v ’ data are quantitatively consistent with a simple model for defect partitioning between evolving bubble, void, and dislocation sinks strengths and biases. Most notably, the model correctly predicts both the incubation dpa i , and the subsequent f v ’, in spite of the fact that they reflect somewhat different physics. Our analysis also suggests that defect recombination is modest at 500 °C. Along with other considerations, this supports the hypothesis that, even at high dpa rates, dual ion irradiations can be used to reasonably emulate void nucleation and growth for a range of fusion-relevant neutron irradiation service conditions. A companion paper incorporates the results of this study in a reduced-order, data-driven void swelling model.

36 MATERIALS SCIENCE↗
DOE OSTI2023

The effect of secondary phases on microstructure and irradiation damage in an as-built additively manufactured 316 L stainless steel with a hafnium compositional gradient

Additive manufacturing (AM) or rapid prototyping has become a crucial tool for reducing both cost and time while increasing efficiency in qualifying structural materials for reactor use. In this study, directed energy deposition (DED) was used to develop an as-built 316 L stainless steel sample with three regions of increasing Hf-dopant to study the effects of Hf on the irradiation response of the material. Morphological and microstructural changes were analyzed before and after 2 MeV proton irradiation at 360 °C to a damage of 2.5 dpa at ~ 10 µm below the surface. The addition of Hf effectively suppressed radiation-induced damage (dislocation loops, radiation-induced segregation) due to enhanced point defect recombination. The radiation damage seen in the as-built sample was further compared to a thermo-mechanically treated counterpart of the same fabrication and irradiation parameters which was found to behave superiorly. In conclusion, the increased radiation resistance of this material may be attributed to the as-built microstructure, which includes undissolved Hf particles, delta ferrite grains and cellular sub-grain boundaries that can hinder defect motion.

316L Stainless Steel↗
DOE OSTI2025

Effect of cold forging on the microstructure and corrosion behavior of type 316L stainless steel in molten FLiNaK salt

Here, the effect of cold forging on the microstructure and corrosion behavior of 316L stainless steel (SS) in molten salt was investigated. Static corrosion experiments were performed in FLiNaK (LiF-NaF-KF: 46.5–11.5–42 mol.%) at 600 °C for 50 h in a glove box. The results show that cold forging gives rise to enhanced corrosion of 316L SS in molten fluoride salt due to the increase of crystallographic defects. Based on the potentiodynamic polarization results, the corrosion current density of 50 % cold-forged 316L SS is about 2.1 times larger than that of the as-received 316L SS in molten FLiNaK salt at 600 °C.

316L stainless steel↗
DOE OSTI2025

Deformation band corrosion as a result of applied stress and cold-work in 304 stainless steel in simulated pressurized water reactor primary water conditions

Stainless steels like 304SS are commonly used in pressurized water reactor primary water environments due to their excellent resistance to stress corrosion cracking (SCC). However, SCC susceptibility has been observed in cold-worked 304SS. Cold-rolling introduces a high density of defects, such as deformation bands or dislocations, into the microstructure; applied stress, even if macroscopically below the yield stress, can result in regions with high localized stresses. Cold-worked and non-cold-worked samples were exposed to 360 °C simulated PWR primary water for 1500 h with and without active loading. Corrosion susceptibility of dislocations and deformation bands induced by cold-rolling and/or applied stress was studied using high-resolution (analytical) transmission electron microscopy. Deformation bands were generated in all specimens examined in the study. Penetrative oxidation was observed in some deformation bands in each specimen. The depth of penetrative deformation band oxidation frequently exceeded the depth of grain boundary oxidation in all specimens. However, deformation band oxides generally were narrowly confined to the deformation band plane. Highly Ni-rich regions were observed beyond all oxidation fronts. Surface oxides were thicker in the specimens exposed under active loading. In conclusion, the implications of these findings at surfaces for deformation bands intersecting stress corrosion crack paths are discussed.

EFTEM↗
DOE OSTI2025

Characterization of in-situ and ex-situ ion-irradiated additively manufactured 316L and 316H stainless steels

Additively manufactured (AM) 316 stainless steel (SS) differs from its wrought counterpart in its unique dislocation cell structure and the presence of segregation and oxide particles at the cell walls. This work investigated the evolution of the microstructure in laser powder bed fusion (LPBF) 316L and 316H SS under in-situ 1 MeV Kr ion irradiation at 600 °C to 5 dpa, and ex-situ 4 MeV Ni ion irradiation at 300 °C and 600 °C from 0.2 dpa to 10 dpa, with a dose rate for all experiments of 10 -3 dpa/s. The results reveal that the dislocation cell structure results in heterogeneous formation of dislocation loops and voids, particularly at 600 °C, where loops tend to form within the cell interiors while voids form at the cell boundaries. LPBF 316H has a reduced level of swelling compared to LPBF 316L due to prolonged incubation. Energy Dispersive X-ray Spectroscopy (EDS) mapping indicates Ni and Si segregation at void surfaces due to radiation-induced segregation. At 300 °C, where voids are absent, the distribution of dislocation loops and stacking fault tetrahedra appears to be uniform. Dislocation cell structures mostly disappeared by 2 dpa for all conditions in this work. M 23 C 6 carbides were observed in LPBF 316H at 600 °C as early as 0.2 dpa, but not in LPBF 316L. Nanoindentation was performed to obtain the hardness of irradiated materials. In conclusion, this work illustrated the influence of additive manufacturing processes on microstructure evolution under irradiation, revealing the differences as well as the similarities as compared with wrought 316 SS, and the AM-related phenomenon that can potentially occur under neutron irradiation in nuclear reactors.

36 - MATERIALS SCIENCE↗
DOE OSTI2021

Complexity of deformation mechanism in neutron-irradiated 304L austenitic stainless steel at microstructural scale

The deformation mechanisms of neutron-irradiated 304 L stainless steel have been investigated using the in-situ electron backscattered diffraction (EBSD) technique. To decipher the role of irradiation, a detailed analysis was performed on irradiated miniature samples and compared with nonirradiated samples. Furthermore, at three levels of engineering strain, —0.0%, 4.8%, and 14.5%—microstructural features as well as EBSD were recorded at the identical location during in-situ deformation testing. Post-mortem analysis of the EBSD data revealed that the neutron-irradiated samples had higher fractions of the slip bands even at low amounts of deformation. Along with the slip bands, the neutron-irradiated sample showed the twins and martensitic phase formed almost parallel to the slip bands. In addition, the image results also indicated that the formation of twins and phases associated with the slip bands. A detailed mechanistic understanding has been investigated to identify the (111)γ planes orientation with respect to the loading direction associated with the formation of twins and martensite. The newly formed deformation twins and martensite were also found to maintain this relationship when they existed together.

304L austenitic stainless steel↗
DOE OSTI2021

Unearthing principal strengthening factors tuning the additive manufactured 15-5 PH stainless steel

Additive manufactured (AM) materials exhibit enhanced performance, while post-processing is essential to reinforce its properties. Controlling the tunable factors and the underlying strengthening mechanisms during the post-processing are a key to answering the calls from the industry and end users. We identified the principal strengthening factors that contribute to AM stainless steel under heat-treatment and weighed their importance. The as-built sample exhibited a unique microstructure with a heterogeneous grain size distribution, a small amount of retained austenite, high dislocation density, and dispersed oxide particles. The strengthening primarily by dislocation forest and additionally by heterogeneous grain size contributed to the as-built sample. Although aging slightly decreased dislocation strengthening, superior aging enhancement was achieved by Cu-precipitates. The solid-solutionizing not only increased the effective grain size but also reduced the dislocation density by eliminating the heterogeneous microstructure, which deteriorated the precipitation hardenability. Our findings shed light on the performance optimization of AM metals.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Investigation of the fatigue crack behavior of 304 stainless steels using synchrotron X-ray tomography and diffraction: Influence of the martensite fraction and role of inclusions

Here, the effect of fatigue on the microstructure of four-point bend specimens of three variations of 304 stainless steels (Commercial 304, 304H, and 304 L) was investigated using synchrotron x-ray tomography and diffraction. X-ray tomography revealed the formation of the fatigue-induced microvoids and crack while the diffraction data was used to quantify the amount of deformation-induced martensite found after fatigue in all samples. Transmission electron microscopy evidenced the role of the precipitates/inclusions on the microvoid formation. It was found to depend on their chemical nature. The shape of the precipitates/inclusions was also found to have an effect on the microvoid shape.

304 stainless steel↗
DOE OSTI2024

Microscopy modality transfer of steel microstructures: Inferring scanning electron micrographs from optical microscopy using generative AI

Scanning electron microscopy (SEM) is resource intensive, which limits its throughput in some applications. As an alternative, we propose applying computer vision and machine learning to generate high-quality synthetic SEM micrographs from micrographs obtained using light optical microscopy (LOM). Working with a correlated LOM/SEM dataset of dual-phase steel images, we test generative models of various architectures, including encoder-decoder networks, generative adversarial networks (GANs), and diffusion-based models. We find that the diffusion models significantly outperform other methods on both qualitative and quantitative assessments, while preserving key metallurgical meaning. This work establishes diffusion as the state-of-the-art for microscopy modality transfer and demonstrates the potential of AI-powered microscopy to enhance LOM with micron scale structural recreation.

Computer vision↗