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At least 73 records · Page 4

In-situ measurement and control of the tool-workpiece interface temperature during friction stir processing of 304/304L stainless steel

Friction stir processing of 304/304L stainless steel is an area of interest for repair of spent nuclear fuel canisters. To enable repair without canister deflection or fracture, it is necessary to define the limitations for the depth of the processing zone which will be critically dependent on the thermal history of the material. Here, this work provides the first direct measurement of the interface temperature for friction stir processing of steel. The measured temperature is in the range of 850–1050 °C which is 20–30 % higher than previously reported values. Notably, the peak temperature occurs at the pin tip which is attributed to a higher sticking fraction and subsequently higher strain rate near the tool axis of rotation. Furthermore, a clear correlation between the temperature, grain size, and hardness is established within a single weld nugget and across different processing conditions. In the future, this data may lead to improved process modelling through direct validation and allow for property optimization through direct microstructure control.

304 stainless steel↗

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↗

Mechanical rolling and annealing of wire-arc additively manufactured stainless steel plates

Thin walls of 304L stainless steel were fabricated by wire-arc additive manufacturing (WAAM) followed by post build thermomechanical processing to modify the as built microstructure and properties. The walls were made using a high-deposition-rate robotically controlled gas-metal arc welding system and were characterized using optical microscopy and tensile tested for mechanical properties. Post processing consisted of mechanical rolling the walls to 25% and 40% strains, followed by annealing at 1050°C to demonstrate a wide range of properties. Results show that WAAM can be used to build custom sized semi-finished parts or blanks that can later be thermomechanically processed to increase strength and ductility through recrystallization of the as built microstructure, and/or processed into desired shapes with improved mechanical properties.

304L stainless steel↗

Dislocation channel broadening–A new mechanism to improve irradiation-assisted stress corrosion cracking resistance of additively manufactured 316 L stainless steel

Additively manufactured (AM) 316 L stainless steel (SS) after hot isostatic pressing (HIP) was found to exhibit superior resistance to irradiation-assisted stress corrosion cracking (IASCC) in high-temperature water, as compared to wrought 316 L SS. The well-accepted IASCC factors of radiation-induced segregation (RIS) and radiation hardening are not accurate descriptions of IASCC susceptibility in this case. A decreased strain localization along grain boundaries, caused by dislocation channel broadening, was confirmed to suppress crack initiation. A unique distribution of irradiation-induced defects in HIP AM 316 L SS eased dislocation cross-slip compared to those in the wrought counterpart, thus increasing the channel width near the grain boundaries. Here for the first time, this study highlights the importance of dislocation channel broadening as a potential mechanism to further improve the IASCC resistance of 316 L SS and provides direct experimental evidence based on commercial-grade materials.

316L stainless steel↗

Development and testing of coarse-grained models for ultrasonic simulations of cast austenitic stainless steel

Ultrasonic inspection of cast austenitic stainless steel (CASS) in the nuclear industry is particularly challenging because of sound field scatter and attenuation caused by the coarse-grained microstructure. Modeling and simulation are important tools in ultrasonic testing, as they can be used to help address key aspects of inspections, such as developing new probe designs, predicting inspection reliability, and testing phased-array focal laws. However, developing a useful and reliable CASS model is challenging due to the many grain interfaces and crystalline orientations that must be captured. We demonstrate a method of creating a realistic CASS model that is usable in CIVA, a commercially available modeling and simulation software platform. Using polished and chemically etched sections, we generate models of a coarse-grained equiaxed specimen and a columnar specimen. We also test an alternative method of generating a coarse-grained model using Voronoi regions. We qualitatively compare sound field scatter and quantitatively compare sound field attenuation and beam partitioning in simulated sound fields to those of laboratory-measured sound fields. Results show that the Voronoi models perform as well as or better than the models based on actual grain morphology. Here we also show that model-to-model randomness in Voronoi grain structure can impact the magnitude of a simulated echo response by a factor of two or more. Although CASS models are potentially a good depiction of reality for a given scenario, they should not be considered representative since CASS morphology can change significantly from specimen to specimen or within the same specimen.

36 MATERIALS SCIENCE↗

Effect of thermal treatments on electrochemical behavior of binder jetted 17-4 PH stainless steel

Binder jetted 17–4 PH stainless steel was post-processed to relate heat treatment, microstructure, and corrosion in 3.5 wt% NaCl. Specimens were sintered at 1380 or 1400 °C, solution-annealed at 1055 °C for 1 h, and aged at 482 °C for 1 h. Here, as-sintered parts showed α′-martensitic matrix with a δ-ferrite network and Cu-rich precipitates in ferrite; inclusions (MnS, NbC) promoted localized attack. solutionizing redistributed elements and reduced ferrite, while aging generated coherent Cu nano-precipitates. Corrosion resistance was highly sensitive to post-processing in which aged specimens exhibited the lowest corrosion current density and formed a thicker, stable Cr 2 O 3 -rich passive film, whereas sintered specimens degraded most. Pitting potential depended on sintering temperature and microstructure, with 1400 °C sintering yielding more positive pitting potentials and the best overall performance after aging. Although the 1400-solutionized condition showed a relatively noble pitting response versus 1380-solutionized, it displayed unstable corrosion kinetics attributed to an imperfect passive film linked to higher NbC density. XPS depth profiles corroborated these trends, showing thicker, more continuous Cr 2 O 3 in aged states and discontinuous/thinning oxides in less resistant conditions. Practically, high-temperature sintering (∼1400 °C) followed by solutionizing and aging is recommended, with further gains expected from reducing NbC/MnS populations and porosity via powder and process control.

36 MATERIALS SCIENCE↗

Corrosion Compatibility of Stainless Steels and Nickel in Pyrolysis Biomass-Derived Oil at Elevated Storage Temperatures

Corrosion compatibility of stainless steels and nickel (Ni200) was assessed in fast pyrolysis bio-oil produced from pyrolysis of high ash and high moisture forest residue biomass. Sample mass change, ICP-MS and post-exposure electron microscopy characterization was used to investigate the extent of corrosion. Among the tested samples, type 430F and type 316 stainless steels (SS430F and SS316) and Ni200 (~98.5% Ni) showed minimal mass changes (less than 2 mg∙cm−2) after the bio-oil exposures at 50 and 80 °C for up to 168 h. SS304 was also considered to be compatible in the bio-oil due to its relatively low mass change (1.6 mg∙cm−2 or lower). SS410 samples showed greater mass loss values even after exposures at a relatively low temperature of 35 °C. Fe/Cr values from ICP-MS data implied that Cr enrichment in stainless steels would result in a protective oxide layer associated with corrosion resistance against the bio-oil. Post exposure characterization showed continuous and uniform Cr distribution in the surface oxide layer of SS430F, which showed a minimal mass change, but no oxide layer on a SS430 sample, which exhibited a significant mass loss.

09 BIOMASS FUELS↗

Deuterium permeation and retention in 316L Stainless Steel Manufactured by Laser Powder Bed Fusion

Deployment of additively manufactured materials into nuclear energy systems requires investigation of the full range of the unique environmental effects on these materials. Hydrogen isotopes are common gaseous species in nuclear reactors and exhibit ample high mobility in most materials. While hydrogen isotopes mobility in wrought stainless steel is well understood, this property is not thoroughly studied for its additively manufactured variants. In this study, we investigated the deuterium permeation and retention in 316L stainless steel manufactured by laser powder bed fusion. The results showed that the deuterium permeability in the as-built additively manufactured 316L stainless steel (AM SS316L) is greater than that of the reference wrought 316L stainless steel by a factor of 2.8. However, the stress-relieved and solution-annealed AM SS316L samples exhibit lower deuterium permeability in comparison with the as-built condition. Following the solution annealing, the deuterium permeability of AM SS316L is comparable with that of the reference wrought SS316L. Deuterium retention in the as-built AM SS316L is 45% higher than that of the wrought 316L stainless steel and slightly higher than that of the two thermally annealed AM SS316L materials. Finally, transmission electron microscopy and positron annihilation lifetime spectroscopy were used to obtain microstructural information used to determine deuterium permeation and retention behavior in the studied materials.

36 MATERIALS SCIENCE↗

Long-term interactive corrosion between International Simple Glass and stainless steel

The interactive corrosion between stainless steel 316 (SS) and International Simple Glass (ISG) has been studied for 12 months. The samples were placed in intimate contact to create crevice corrosion conditions on SS in a 0.6 M NaCl solution with and without 142 ppm dissolved silica species enriched in 29 Si. Corrosion on SS was observed with large pits located close to the crevice mouth at the end of 1 year in 0.6 M NaCl solution. The SS corrosion was also associated with the dissolution of nearby glass in a highly localized manner. When the leaching solution was saturated with silica species, the corrosion rate of SS was suppressed. However, the presence of SS enhances ISG dissolution in both conditions. The implications of the observed phenomena on the long-term storage of nuclear waste are discussed.

36 MATERIALS SCIENCE↗

Defect Production and Microstructural Feature Impact for Radiation Damage in Additively Manufactured 316 Stainless Steel

This milestone presents multi-scale modeling research results for additively manufactured 316 stainless steel. A combination of phase field, cluster dynamics, molecular dynamics, and density functional theory with machine learning is used, allowing for predictions of radiation-driven microstructural evolution in additively manufactured 316 stainless steel over a range of temperatures, damage rates, neutron spectra, and microstructures, and supporting the development of combined ion and neutron irradiation for material qualification. Informed by ion irradiation and neutron irradiation results across the Advanced Materials and Manufacturing Technologies program, we investigate the unique aspects of radiation-driven microstructure evolution in additively manufactured 316 stainless steel. In particular, we focus on understanding the impact of carbon concentration (varying, for example, between the 316L and 316H standards) on void formation; radiation-induced segregation at dislocation cells and grain boundaries; and the evolution of dislocation loops and network dislocation populations. We find that the unique characteristics of the additively manufactured microstructures must be accounted for in understanding the evolution of dislocation populations under thermal and irradiation conditions, such as the variation in sink strengths arising due to the variation in dislocation density. We also find that the radiation-induced segregation of Cr and Ni to grain boundaries and cell walls differs due to the differences in their defect sink biases. We also find that increasing the Ni content can slow vacancy diffusion, which may provide a mechanism for the observed reduction in transient swelling rate for austenitic Fe-Cr-Ni alloys with increasing Ni content. In addition, ion irradiations have shown that increasing carbon content in 316 SS results in a larger population of smaller voids, suggesting reduced vacancy diffusion. Our results show that the carbon content of additively manufactured 316 SS has a significant impact on the migration rate of defect clusters. The presence of carbon atoms results in carbon-vacancy trapping, significantly reducing the diffusion rate of vacancies. Carbon atoms may also be trapped near the surface of a void, which may reduce void growth by trapping vacancies that diffuse toward the void.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Evolution of the role of molybdenum in duplex stainless steels during thermal aging: From enhancing spinodal decomposition to forming heterogeneous precipitates

Thermal aging of ferrite in duplex stainless steels leads to a complex microstructural evolution that can give way to large deleterious changes in mechanical properties. The microstructural evolution mechanisms that happen concurrently are strongly linked to minor changes in composition. By characterizing duplex stainless steels with various compositions over a range of aging conditions, it was revealed that adding a modest amount of Mo to cast austenitic stainless steel (such as changing from grade CF3 to grade CF3M) not only increases the kinetics of spinodal decomposition and Ni-Si-Mn-rich G-phase precipitation, but it also forms a separate Mo-rich phase. At shorter equivalent aging times, Mo segregates from Fe and towards Cr accelerating spinodal decomposition. At longer aging times, Mo enriches in the Ni-Si-Mn clusters before phase separating into an adjoined Mo-rich cluster. We found that these phase changes and precipitation events result in a rather steep drop in fracture and impact toughness. These results will inform the design of similar alloys for use at high temperatures.

36 MATERIALS SCIENCE↗

Forming Limits of Thin Ferritic Stainless Steel for Fuel Cell Application

To lower the cost of fuel cell bipolar plate (BPP), less expensive ferritic stainless steel (FSS) BPP substrate materials are investigated. A series of tensile tests and multistage microchannel-forming tests were conducted on 85-µm-thick ferritic stainless steel foils, 439L, 444, and Chromeshield® 22, to understand the effect of the forming temperatures, tooling geometry, and processes on their formability. Three microchannel-forming processes were conducted, which are 1-Hit (single-stage forming), 2-Hit (two-stage forming) with 50% preform, and 2-Hit with 80% preform. FLC o s at various microchannel-forming conditions were obtained to address the formability of the ferritic stainless steel foils under plane strain conditions. It has been found that the larger the microchannel radius, the better the formability, two-stage forming is superior to the single-stage process, and a larger draw percentage in preform (stage I) leads to a higher FLC o or better formability. It has also been found from tensile tests that the thermal effect (higher temperature) has a negative impact on the failure strains. A similar phenomenon was also observed through channel-forming tests conducted at room temperature, 100 °C, and 200 °C.

08 HYDROGEN↗

Microstructural development in DED stainless steels: applying welding models to elucidate the impact of processing and alloy composition

Austenitic stainless steel microstructures produced by directed energy deposition (DED)are analogous to those developed during welding, particularly high energy density welding. To better understand microstructural development during DED, theories of microstructural evolution,which have been established to contextualize weld microstructures, are applied in this study to microstructural development in DED austenitic stainless steels. Phenomenological welding models that describe the development of oxide inclusions, compositional microsegregation, ferrite,matrix austenite grains, and dislocation substructures are utilized to clarify microstructural evolution during deposition of austenitic stainless steels. Two different alloys, 304L and 316L, arecompared to demonstrate the broad applicability of this framework for understanding microstmctural development during the DED process. Despite differences in grain morphology and solidification mode for these two alloys (which can be attributed to compositional differences),similar tensile properties are achieved. It is the fine-scale compositional segregation and dislocation structures that ultimately determine the strength of these materials. The evolution of microsegregation and dislocation structures is shown to be dependent on the rapid solidification and thermomechanical history of the DED processing method and not the composition of the starting material.

36 MATERIALS SCIENCE↗

Effects of Surface Treatments on the Outgassing of 3D-Printed 316L Stainless Steel.

Fermi National Accelerator Laboratory (Fermilab) is a world leader in designing and operating particle accelerators for nuclear and particle physics research. These accelerators rely on electric fields to propel particle beams, which are then directed and focused using magnetic fields. To ensure these beams travel without interference, they must move through an ultra-high vacuum environment, typically around 10⁻⁹ torr. Maintaining such a vacuum requires materials with exceptionally low outgassing rates. 316L stainless steel is a common material choice for vacuum systems due to its low outgassing rates, excellent corrosion resistance, non-magnetic properties, and high mechanical strength. When manufactured using traditional methods like machining, extrusion, and casting, the vacuum properties of 316L stainless steel are well understood. However, the behavior of 316L stainless steel produced through additive manufacturing, such as Direct Metal Laser Sintering (DMLS), is not as well documented. This study aims to determine the outgassing rate of 316L stainless steel fabricated using DMLS. The investigation focuses on measuring the outgassing rates of 1.5 2 vacuum reducers and evaluating the effects of surface preparation techniques, such as mechanical polishing and electropolishing, on the outgassing performance. Understanding the outgassing performance of 3D-printed 316L stainless steel could enable Fermilab engineers to adopt this fabrication method for producing complex parts designed for ultra-high vacuum environments. These advancements have the potential to benefit projects, such as the Long-Baseline Neutrino Facility (LBNF) and the Proton Improvement Plan-II (PIP-II), by improving design flexibility and fostering innovation in accelerator development.

Cloud, Jaiden [Central State University]↗

Tribocorrosion of stainless steel sliding against graphite in FLiNaK molten salt

The molten salt reactor (MSR) concept recently gained renewed interest in developing Generation IV nuclear reactors. One MSR design uses fluoride molten salts to cool tri-structural isotropic particle fuel encapsulated by a carbon matrix into spherical pebbles, which would inevitably contact the reactor's stainless steel container wall during salt circulation. Characterizing this interaction is crucial for reactor safety. Here, in this work, we report the tribocorrosion behavior of graphite sliding against Type 316H stainless steel lubricated by a FLiNaK (LiF:NaF:KF; 46.5:11.5:42 mol %) molten salt in an argon environment. Accelerated wear loss was observed at a higher temperature because of a lower molten salt viscosity and a higher corrosion rate. The graphite had a more rapid material loss at a higher sliding speed than stainless steel because of its higher vulnerability to vibration-induced microfracture. The salt-starved condition caused more material loss than either the no-salt or the salt-flooded condition because neither a graphite transfer film nor stable boundary lubrication could be established at salt starvation. An interesting dual-layer surface film was discovered on the stainless steel worn surface: a chromium-rich top film and a nickel-accumulated but chromium-depleted interlayer. The film composition and structure provide fundamental insights to the mechanochemical interactions between stainless steel and graphite in a molten salt environment.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Equation of state for 304L stainless steel

Here, a new equation of state for 304L stainless steel has been constructed and entered in the Los Alamos National Laboratory SESAME database with material ID 4273. The equation of state is based on a multiphase approach. The solid and liquid phases were fitted to available experimental data for thermal expansion, heat capacity, and shock Hugoniot, as well as to data from density functional theory calculations of the cold curve and quantum molecular dynamics of the liquid regime. The electronic thermal contribution over the entire equation of state range is based on Tartarus (Green’s functions) average atom calculations. For this low-carbon stainless steel both the density functional and electronic thermal calculations are comprised of 19 wt% Cr, 10 wt% Ni, and the remainder Fe.

36 MATERIALS SCIENCE↗

Automated Grain Boundary (GB) Segmentation and Microstructural Analysis in 347H Stainless Steel Using Deep Learning and Multimodal Microscopy

Austenitic 347H stainless steel offers superior mechanical properties and corrosion resistance required for extreme operating conditions such as high temperature. The change in microstructure due to composition and process variations is expected to impact material properties. Identifying microstructural features such as grain boundaries thus becomes an important task in the process-microstructure-properties loop. Applying convolutional neural network (CNN)-based deep learning models is a powerful technique to detect features from material micrographs in an automated manner. In contrast to microstructural classification, supervised CNN models for segmentation tasks require pixel-wise annotation labels. However, manual labeling of the images for the segmentation task poses a major bottleneck for generating training data and labels in a reliable and reproducible way within a reasonable timeframe. Microstructural characterization especially needs to be expedited for faster material discovery by changing alloy compositions. Here, in this study, we attempt to overcome such limitations by utilizing multimodal microscopy to generate labels directly instead of manual labeling. We combine scanning electron microscopy images of 347H stainless steel as training data and electron backscatter diffraction micrographs as pixel-wise labels for grain boundary detection as a semantic segmentation task. The viability of our method is evaluated by considering a set of deep CNN architectures. We demonstrate that despite producing instrumentation drift during data collection between two modes of microscopy, this method performs comparably to similar segmentation tasks that used manual labeling. Additionally, we find that naïve pixel-wise segmentation results in small gaps and missing boundaries in the predicted grain boundary map. By incorporating topological information during model training, the connectivity of the grain boundary network and segmentation performance is improved. Finally, our approach is validated by accurate computation on downstream tasks of predicting the underlying grain morphology distributions which are the ultimate quantities of interest for microstructural characterization.

36 MATERIALS SCIENCE↗