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DOE OSTI2021

Microstructure and mechanical properties of high Mn-containing ferritic-martensitic alloys exposed to cyclical thermal treatment

Substantial residual tensile stress tends to accumulate in currently available high-Cr ferritic martensitic steels that are subjected to cyclical heat treatment, which leads to premature brittle fracture. By tailoring the alloy composition, this thermal cycling can be exploited to induce a high number density of nanoprecipitates and phase transformations countering residual tensile stresses. In this work, three new variants of ferritic-martensitic steels have been designed with computational thermodynamics to meet the goals of mitigating residual tensile stresses by lowering martensite start temperatures and of enhancing mechanical strength and irradiation sink strength by increasing the number density of nanoprecipitates. Furthermore, ctenast materials were subjected to cyclical heat treatment. The thermally cycled samples were evaluated with mechanical testing and microstructural analysis to identify the optimal composition in which figures of merit include low residual stress and a high density of nanoscale MX (M = metal, X = C/N) precipitates, leading to high yield strength with reasonable ductility. The noticeably higher density of nanoprecipitates in the optimal alloy favor its higher yield strength, which is supported by the microstructure-derived yield strength calculation and precipitation kinetics simulation.

36 MATERIALS SCIENCE↗

DOE OSTI2025

The effect of heat treatment on the defect evolution in LPBF 316H stainless steel

This work investigates the effect of processing and heat treatment on defect evolution and irradiation response of laser powder bed fusion (LPBF) 316H stainless steel, with comparisons to LPBF 316L and wrought 316L/316H. Using in-situ and ex-situ ion irradiations across a wide parameter space—temperature (300–675 °C), dose (0.2–25 dpa), dose rate (10 -3 –10 -5 dpa/s), and helium co-implantation (20–2500 appm)—we correlated void swelling, dislocation loop evolution, and segregation behavior with pre-irradiation microstructures (as-built, stress-relieved, solution-annealed, and cold-worked). Results show that swelling is strongly controlled by dislocation density: intermediate densities maximize swelling, while solution annealing or cold working reduce susceptibility to levels comparable to wrought alloys. Low dose rates and helium both promote cavity nucleation and lower the incubation barrier, with helium suppressing the role of dislocation density and driving swelling behavior toward wrought-like response. Loop evolution in SA LPBF 316H resembles wrought 316L but shows localized denuded zones near low-angle grain boundaries. STEM-EDS mapping further revealed Ni segregation at voids and sparse Al-rich oxides, without evidence of Ni–Si precipitates. Collectively, these findings identify dislocation density, helium content, and dose rate as the factors governing swelling in LPBF 316H and provide mechanistic datasets for model validation, supporting LAIN and the qualification of AM austenitic steels for nuclear service.

316 stainless steel↗

DOE OSTI2024

Thermomechanical Processing for Improved Mechanical Properties of HT9 Steels

Thermomechanical processing (TMP) of ferritic–martensitic (FM) steels, such as HT9 (Fe–12Cr–1MoWV) steels, involves normalizing, quenching, and tempering to create a microstructure of fine ferritic/martensitic laths with carbide precipitates. HT9 steels are used in fast reactor core components due to their high-temperature strength and resistance to irradiation damage. However, traditional TMP methods for these steels often result in performance limitations under irradiation, including embrittlement at low temperatures (<~430 °C), insufficient strength and toughness at higher temperatures (>500 °C), and void swelling after high-dose irradiation (>200 dpa). This research aimed to enhance both fracture toughness and strength at high temperatures by creating a quenched and tempered martensitic structure with ultrafine laths and precipitates through rapid quenching and unconventional tempering. Mechanical testing revealed significant variations in strength and fracture toughness depending on the processing route, particularly the tempering conditions. Tailored TMP approaches, combining rapid quenching with limited tempering, elevated strength to levels comparable to nano-oxide strengthened ferritic alloys while preserving fracture toughness. For optimal properties in high-Cr steels for future reactor applications, this study recommends a modified tempering treatment, i.e., post-quench annealing at 500 °C or 600 °C for 1 h, possibly followed by a brief tempering at a slightly higher temperature.

36 MATERIALS SCIENCE↗

DOE OSTI2022

The influence of temperature on the strain-hardening behavior of Fe-22/25/28Mn-3Al-3Si TRIP/TWIP steels

In this work, the influence of temperature and stacking fault energy (SFE) on the strain-hardening behavior and critical resolved shear stress for twinning was investigated for three Fe–22/25/28Mn–3Al–3Si wt.% transformation- and twinning-induced plasticity (TRIP/TWIP) steels. The SFEs were calculated by two different methods, density functional theory and statistical thermodynamic modeling. The dislocation structure, observed at low levels of plastic deformation, transitions from “planar” to “wavy” dislocation glide with an increase in temperature, Mn content, and/or SFE. The change in dislocation glide mechanisms from planar to wavy reduces the strain hardening rate, in part due to fewer planar obstacles and greater cross slip activity. Additionally, the alloys exhibit a large decrease in strength and ductility with increasing temperature from 25 to 200 °C, attributed to a substantial reduction in the thermally activated component of the flow stress, predominate suppression of TRIP and TWIP, and a significant increase in the critical resolved shear stress for mechanical twinning. Interestingly, the increase in SFE with temperature had a rather minor influence on the critical resolved shear stress for mechanical twinning, and other temperature dependent factors which likely play a more dominant role are discussed.

36 MATERIALS SCIENCE↗

DOE OSTI2022

The influence of nitrogen and nitrides on the structure and properties of proton irradiated ferritic/martensitic steel

The 12Cr1MoWV (wt%) ferritic/martensitic steel HT9 is a candidate material for fuel cladding in advanced nuclear reactors, such as the Versatile Test Reactor currently under development. As such, understanding the relationship between microstructure and mechanical properties in the context of irradiation environments for these steels is critical. N content, and more specifically interstitial N, has been hypothesized to be detrimental to irradiated properties at lower temperatures (less than 0.3T m ) to a total of 6 dpa; however, in this work at a dose of 1 dpa the irradiated microstructure was improved with added N, leading to less irradiation hardening. Three variants of HT9 were irradiated with 1.5 MeV protons to a dose of 1 dpa at 300°C. The HT9 variants included Low (10 ppm), Mid (190 ppm), and High (440 ppm) N alloys that were otherwise nearly identical. Changing the N content had a variety of effects on the irradiated defect structures. As N content increased, the average dislocation loop diameter decreased, while the number density of loops increased. Additionally, extensive Ni clustering was observed on dislocations and interfaces. The Mid and High N specimens exhibited significantly less hardening (ΔHV≃100) relative to the Low N specimen (ΔHV≃160). The decrease in hardening is attributed to vanadium carbonitride acting as a sink for Ni clusters that would otherwise form on dislocations. Under the irradiation conditions used, these results suggest increasing the N content in HT9 may have a desirable effect on the irradiated structure and properties at the dose studied, as well as the swelling resistance at higher doses. In other words, N content appears to be a powerful tool for tailoring the self-interstitial atom cluster mobility in F/M steels for different temperature and dose applications.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Application of the Chloride Susceptibility Index to Study the Effects of Ni, Cr, Mn and Mo on the Repassivation of Stainless Steels

The effects of Ni, Cr, Mn and Mo on the very earliest stages of repassivation of stainless steels are quantified using the Chloride Susceptibility Index (CSI), which is an ab initio-based index for the evaluation of repassivation tendency. The quinary system of Fe-Ni-Cr-Mn-Mo is studied with density functional theory analysis and an electrochemisorption model developed previously by the authors, which are required to determine the CSI. The adsorption energies of O and Cl to different surface configurations are calculated, and then surface coverage maps of different species on the surface are obtained from the adsorption energies based on the Langmuir isotherm. Finally, CSI is calculated for different compositions of stainless steels. It is found that the effect of alloying elements on promoting repassivation of Fe alloys is in the order of Mn > ≈Ni > Cr > Mo when solute composition is less than 28 wt.%. A strong synergy is found between Cr and Mo such that a combination of these two elements at a certain ratio can give an optimal (low) CSI. Here, the usage of CSI for evaluating repassivation tendency of CRAs is validated by experimental measured repassivation potential, which shows a strong monotonic negative relation with CSI.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Model Parameter Development for Complex Materials: Species-Specific Diffusion Barriers in 316 Stainless Steel from Systematic DFT Calculations

Vacancy-mediated diffusion barriers in 316 stainless steel have been systematically calculated using density functional theory to provide essential parameters for mesoscale microstructure evolution models. A statistical sampling approach employing 210 nudged elastic band calculations across multiple special quasi-random structures captures the effects of local chemical environments in this concentrated alloy. The computational methodology addresses challenges specific to chemically disordered systems, including proper magnetic treatment throughout multi-step calculations and validation against experimental structural properties. The calculated activation barriers reveal clear species-dependent diffusion behavior with the hierarchy Ni >> Fe ˜ Cr >> Mo. Nickel exhibits the highest barriers (0.74–1.31 eV, mean 1.045 eV), confirming its role as the slowest-diffusing major component. Iron and chromium show similar moderate barriers averaging 0.587 eV and 0.522 eV, respectively. Remarkably, molybdenum demonstrates exceptionally low barriers (0.12–0.28 eV, mean 0.194 eV), suggesting much higher mobility than previously recognized and potentially significant implications for precipitation kinetics and microstructure evolution. The barrier ranges remain consistent across different 316 SS compositions, supporting parameter transferability for modeling applications. The overall mean barrier of 0.64 eV provides a practical approximation for phase field simulations, while species-specific values enable detailed treatments of diffusion-controlled processes. This systematic approach establishes a validated framework for generating diffusion parameters in other concentrated alloys where experimental data are limited, while providing the first systematic set of species-specific barriers for predictive modeling of 316 stainless steel microstructure evolution.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Direct utilization of gaseous fuels in metal supported solid oxide fuel cells

Direct utilization and internal reforming of gaseous fuels is investigated on symmetric-architecture metal supported solid oxide fuel cells (MS-SOFCs) with thin ceramic electrolyte and scaffold backbone layers, and low cost ferritic stainless steel supports on both sides. Infiltrated Pr-oxide and Ni/samarium-doped ceria catalysts are added to the cathode and anode electrodes, respectively. Initial performance and durability is evaluated for MS-SOFCs operating with natural gas, propane, ammonia, and dimethyl ether at 700 °C. Cells for natural gas and propane utilize a novel high entropy alloy (HEA) catalyst for internal reforming with performance and degradation rates similar to H 2 (0.5W cm -2 and ~12%/100 h). In conclusion, initial testing with sulfur shows reversible degradation for levels found in natural gas and irreversible degradation for higher levels found in commercial propane. Overall, MS-SOFCs show successful fuel flexibility.

08 HYDROGEN↗

DOE OSTI2020

Effect of Solute Elements on Boron Segregation in Boron-Containing Steels

The addition of boron to steel alloys results in an increase in both hardenability and casting defects. The casting difficulties are predicted to stem from a metatectic reaction, δ + γ → L + γ, where a fully solidified material begins to locally remelt as the temperature decreases. Another possible source of casting defects is a boride-rich phase that is predicted to remain liquid at low temperatures. To experimentally determine which reaction is the likely source of the casting defects, the predicted reactions and the effect of solute elements on those reactions are investigated. Levitation zone melting is used to control segregation in a ternary Fe–C–B alloy and a commercial 22MnB5 alloy. Carbon segregation and a peritectic reaction result in a peritectic jump during directional solidification where the first directionally solidified (DS) zone undergoes δ-bcc solidification followed by a peritectic jump to steady state planar solidification of γ-fcc in the second DS zone. The presence of other solute elements in the zone melted 22MnB5 alloy lead to a breakdown in the planar solidification front before steady state solidification could be achieved in the second DS zone. With a cellular solid/liquid interface, boron-rich intercellular liquid formed low melting iron boro-carbide particles. The controlled solidification conditions in a levitation zone melter were unable to prevent ~0.003 wt% boron from segregating to high enough levels to form boride particles. Therefore, it is likely that during commercial casting, the formation of the low melting boride phase from interdendritic segregation is a key source of the casting issues.

36 MATERIALS SCIENCE↗

DOE OSTI2021

SURFACE FINISHING AND ELECTROLESS NICKEL PLATING OF ADDITIVELY MANUFACTURED (AM) METAL COMPONENTS

This study investigates the application of electroless nickel deposition on additively manufactured stainless steel samples. Current additive manufacturing (AM) technologies produce metal components with a rough surface. Rough surfaces generally exhibit fatigue characteristics, increasing the probability of initiating a crack or fracture to the printed part. For this reason, the direct use of as-produced parts in a finished product cannot be actualized, which presents a challenge. Post-processing of the AM parts is therefore required to smoothen the surface. This study analyzes chempolish (CP) and electropolish (EP) surface finishing techniques for post-processing AM stainless steel components CP has a great advantage in creating uniform, smooth surfaces regardless of size or part geometry EP creates an extremely smooth surface, which reduces the surface roughness to the sub-micrometer level. In this study, we also investigate nickel deposition on EP, CP, and as-built AM components using electroless nickel solutions. Electroless nickel plating is a method of alloy treatment designed to increase manufactured component's hardness and surface resistance to the unrelenting environment. The electroless nickel plating process is more straightforward than its counterpart electroplating.. We use low-phosphorus (2-5% P), medium-phosphorus (6-9% P), and high-phosphorus (10-13% P). These Ni deposition experiments were optimized using the L9 Taguchi design of experiments (TDOE), which compromises the prosperous content in the solution, surface finish, plane of the geometry, and bath temperature. The pre-and post-processed surface of the AM parts was characterized by KEYENCE Digital MicroscopeVHX-7000 and Phenom XL Desktop SEM. The experimental results show that electroless nickel deposition produces uniform Ni coating on the additively manufactured components up to 20 μm per hour. Mechanical properties of as-built and Ni coated AM samples were analyzed by applying a standard 10 N scratch test. Nickel coated AM samples were up to two times scratch resistant compared to the as-built samples. This study suggests electroless nickel plating is a robust viable option for surface hardening and finishing AM components for various applications and operating conditions.

Keywords: additive manufacturing, fatigue, chempol↗

DOE OSTI2020

PORFLOW Implementation of Vadose Zone Conceptual Model for Naval Reactor Component Disposal Areas in the E-Area Low Level Waste Facility Performance Assessment

PORFLOW models have been developed to implement the proposed conceptual models for the two Naval Reactor Component Disposal Areas (NRCDAs), 643-7E and 643-26E, for the purpose of evaluating dose impacts and producing disposal limits for the E-Area Low-Level Facility (LLWF). New NRCDA conceptual models were proposed by Wohlwend and Butcher (2019) for two areas within/adjacent to the E-Area LLWF used as storage/disposal sites for reactor components from the U.S. Navy since 1987. Naval Reactor (NR) waste is comprised of highly radioactive components consisting of activated corrosion-resistant metal alloy contained within welded thick-walled steel casks, and auxiliary equipment primarily contaminated with lower levels of Activated Corrosion Products (ACPs) residing on the metal surfaces and contained within thinner-walled bolted containers.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2022

PORFLOW Implementation of Vadose Zone Conceptual Model for Naval Reactor Component Disposal Area in the E-Area Low Level Waste Facility Performance Assessment

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2026

Accelerated creep profiling: a high-throughput thermal- and stress-gradient approach applied to additive and wrought stainless steel

Here, this study investigates logarithmic creep behavior at temperatures near room temperature in wrought and additively manufactured (AM) 316 L austenitic stainless steel. A novel high-throughput (HiTp) methodology employed thermal gradients to obtain stress- and temperature-dependence of creep behavior. The findings, based on 104 two-week creep tests, reveal significant differences in creep response between wrought and AM materials. Compared to the wrought material, the AM material exhibited a higher activation energy and a lower activation volume. These differences were attributed to the materials’ distinct microstructural features, e.g., dislocation cell structures and precipitate distributions, which alter the susceptibility to dislocation glide creep, particularly at stresses below the yield stress. The HiTp methodology provides both an accelerated determination of low-temperature creep mechanisms, offering critical data for the design and optimization of alloys in near-ambient, high stress applications.

316 L Stainless steel↗

DOE OSTI2025

Corrosion susceptibility and chromium loss in Austenitic steels and Nickel-based alloys in molten FLiNaK at 700 °C

A comparative study was conducted to evaluate the corrosion susceptibility of 316L, 316H, Ni 200, Inconel 625, and Hastelloy N in molten FLiNaK at 700 °C for 100 h. Top-view and cross-sectional scanning electron microscopy (SEM) imaging, combined with energy-dispersive X-ray spectroscopy (EDS) mapping, was performed to investigate microstructural and compositional changes. SEM images were further processed by introducing a contrast threshold to map cavity distribution. Using EDS mapping, intergranular and intragranular Cr loss were separately characterized. The ranking of mass loss after corrosion, from highest to lowest, is as follows: 316H > 316L > Inconel 625 > Hastelloy N > Ni 200. Cr loss was found to be correlated with Mo concentration, in agreement with many previous studies, with higher Mo content resulting in reduced Cr loss. On the other hand, there is no evidence that the high carbon content in 316H enhances corrosion resistance. The relatively low solubility of carbon in austenite at the testing temperature limits the amount of dissolved carbon. Therefore, the carbon-retarded vacancy diffusion, and consequently the reduced Cr diffusion, were not observed.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2022

Second group of irradiation capsules: property data of irradiated welded stainless steel 347 and irradiated, welded, and hydrogen charged Zircaloy-4 for SHINE

Zircaloy-4 and AISI 347 stainless steel were irradiated to low doses (10 20 and 10 21 n/cm 2 ) at low temperature (~60°C) in the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory (ORNL). These materials were under consideration for some of the structural components of the medical isotope production facility developed by SHINE Technologies. Zircaloy-4 base metal, as welded, welded and post-weld heat treated (PWHT), and hydrogen charged samples were irradiated. AISI 347 base metal from Sandmeyer Steel, Penn Stainless, and Rolled Alloys suppliers were irradiated. AISI 347 gas tungsten arc welding (GTAW) and flux-cored arc welding (FCAW) samples of Penn Stainless and Rolled Alloys were also irradiated. The irradiated materials were tested with microhardness and tensile tests at room temperature in air. The AISI 347 materials had more elongation after irradiation than the Zircaloy-4 materials. In fact, the Zircaloy-4 welded without PWHT and with H charging had the lowest elongation of any of the materials. This report is the final in a series of reports on this project.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Alloying of U-Al-SS as a Simulant for Pu-Al-SS Alloying

The Savannah River National Laboratory evaluated several options for disposition of stainless steel (SS)–clad plutonium metal, particularly Pu-10.6 at. % Al (Pu- 1.3 wt% Al) alloy fuel. One technology considered was alloying fuel with SS. The goal of the alloying would be to make a SS-Pu alloy that was a nonproliferable waste form with secondary Pu-rich microencapsulated regions distributed throughout the refractory SS. The microencapsulation of the Pu regions should therefore allow the waste form to meet the requirements for a low attractiveness waste as defined by the U.S. Department of Energy. Plutonium-bearing alloys at these levels could potentially be suitable for disposal at a waste isolation pilot plant. Four metal ingots were successfully fabricated using U and Al as a surrogate for Pu-Al. The U was distributed and microencapsulated by the alloy matrix, thereby setting the stage for subsequent tests using SS-clad fuel elements containing Pu-10.6Al.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Flux and estimated spectra from a low-intensity laser-driven X-ray source

Laser-driven X-rays as probes for high-energy-density physics spans an extremely large parameter space with laser intensities varying by 8 orders of magnitude. We have built and characterized a soft X-ray source driven by a modest intensity laser of 4 × 10 13 W/cm 2 . Emitted X-rays were measured by diamond radiation detectors and a filtered soft X-ray camera. A material-dependence study on Al, Ti, stainless steel alloy 304, Fe, Cu and Sn targets indicated 5-μm-thick Cu foils produced the highest X-ray yield. X-ray emission in the laser direction and emission in the reverse direction depend strongly on the foil material and the thickness due to the opacity and hydrodynamic disassembly time. The time-varying X-ray signals are used to measure the material thinning rate and is found to be ~1.5 μm/ns for the materials tested implying thermal temperature around 0.6 eV. The X-ray spectra from Cu targets peaks at ~2 keV with no emission >4 keV and was estimated using images with eight different foil filters. One-dimensional hydrodynamic and spectral calculations using HELIOS-CR provide qualitative agreement with experimental results. Modest intensity lasers can be an excellent source for nanosecond bursts of soft X-rays.

47 OTHER INSTRUMENTATION↗

DOE OSTI2023

Internal carburization and scale formation on austenitic steels in supercritical carbon dioxide

Direct-fired supercritical CO 2 (sCO 2 ) power cycles are being commercialised to revolutionise fossil energy as a low-emission power source. In order to lower the cost of this technology, less expensive steels are needed in the lower temperature segments of the cycle. However, there are concerns about internal carburisation of steels in sCO 2 . A consistent observation is that thin, Cr-rich oxides appear to reduce C ingress compared to thick Fe-rich oxides formed on 9–12% Cr ferritic-martensitic steels. Advanced austenitic stainless steels (SS) like alloy 709 (20Cr-25Ni) are able to continue to form Cr-rich oxides at 650°C, while a conventional type 316 H SS formed a Fe-rich scale. The C diffusion profiles in SS specimens were quantified at 550°C–650°C using glow discharge optical emission spectroscopy and electron probe microanalysis. Analytical transmission electron microscopy was used to compare the thin protective Cr-rich oxide formed on alloy 709 in sCO 2 at 650°C to that formed in ambient air.

36 MATERIALS SCIENCE↗