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At least 73 records · Page 4

Electrically Conductive and Protective Coating Compatibility with LSCF Cathodes

Ferritic stainless-steel interconnect materials are used in intermediate or high-temperature SOFCs because of their oxidation resistance, high formability, and low cost. Their corrosion resistance is due to the formation of a protective chromium oxide scale during operation. However, the protective oxide layer produces Cr-containing volatile species at SOFC operating temperatures and conditions, which can cause cathode poisoning. Spinel coatings have been developed to prevent cathode poisoning while maintaining an electrically conductive pathway through SOFC stacks. Generally, Mn-Co-O spinel has been the material of choice, but PNNL has developed an Mn-Cu-O spinel protective coating to remove the costly Co and enhance the electrical conductivity. This paper will focus on the electrically conductive coating’s compatibility with LSCF in high-temperature operating environments.

Choi, Jung-Pyung↗

Variations in Creep Performance of P92 Steel Within Its Composition Range: Influence of N Solubility

Underspecified composition ranges often lead to alloys with unpredictable mechanical performance. To better understand the changes in microstructure and mechanical performance associated with variations of key elements, three versions of P92 are formulated within, or close to, the specified allowable for N, B, and C ranges. Chromium and Si are also varied to influence N solubility. Different service conditions (i.e., temperature and stress) are explored. It is observed that >80% decrease in creep life occurs at 625 °C and 155 MPa for the highest B and N containing alloy. Multiscale characterization reveals key changes due to the trace element variation. The high B and N containing alloy forms deleterious BN precipitates with morphology that promotes crack nucleation and damage accumulation, but this alloy additionally forms higher fractions of beneficial MX precipitates. The alloy with the lowest B and N concentrations but greater C content shows the best creep performance—a consequence of the refined M 23 C 6 carbide precipitate population and the absence of large-scale inclusions or BN precipitates. Calculations of creep activation energy reveal that the high B and N containing alloy is more prone to damage accumulation which causes an early onset of accelerating creep and greater minimum creep rate.

36 MATERIALS SCIENCE↗

Influence of carbon nanotubes on microstructure and corrosion performance of additively manufactured 316L stainless steel

For this study, laser powder bed fusion (LPBF) was performed on feedstock-modified 316L stainless steel powder with 1 and 2 vol% carbon nanotubes (CNT). The corrosion resistance was evaluated following cyclic potentiodynamic polarization tests conducted in 0.6 M NaCl at room temperature, 35 and 50 °C, and immersion tests in 6 % FeCl 3 . The CNT addition has increased the pitting potential and decreased number of pits formed during immersion in FeCl 3 solution, which could be attributed to Mn-Si-O nano inclusions refinement and segregation of chromium around the inclusions. The observed corrosion behavior was correlated with the altered microstructure due to CNT addition.

36 MATERIALS SCIENCE↗

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↗

Preliminary results addressing material qualification using combined ion irradiation and modeling data

Additively-manufactured (AM) materials have attracted increasing attention in recent years as a new method to make novel and customized components. While AM and conventionally produced materials are compositionally similar, they do possess different microstructures, necessitating assessment of materials produced via AM for their behavior in reactor environments. Some microstructures unique to AM materials, such as compositional micro-inhomogeneity and dislocation cell structures, are of particular importance since they may lead to different radiation performance. The performance of AM materials for advanced nuclear reactor applications is of interest to the Advanced Materials and Manufacturing Technologies (AMMT) program under the Department of Energy Office of Nuclear Energy. The AMMT program aims to demonstrate its new accelerated development and qualification methods via laser powder bed fusion (LPBF) 316 stainless steel (SS). Focusing on material bearing both 316L and 316H specifications, we integrate ion irradiation and modeling. This year, we focus on answering foundational questions related to process variability, alloy chemistry variation, and microchemical segregation. Experimental results provide information and motivate questions to the modeling effort, which aims to develop the ability to model radiation-driven microstructural evolution in additively-manufactured 316 stainless steel under a variety of advanced reactor conditions, including different temperatures, neutron spectra, and fluxes, in a sort of "virtual experiment". We perform in-situ and ex-situ ion irradiations and microstructural characterizations to support the development of AM materials for reactor applications, develop a phase field model of radiation-induced segregation in additively manufactured material with high angle grain boundaries and dislocation cells, and investigate the effect of carbon and chromium content on point defect behavior.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Corrosivity Screening of Pyrolysis Bio-Oils by Short-Term Alloy Exposures. Laboratory Analytical Procedure (LAP), Issue Date: May 12, 2022

Bio-oils contain organic acids and oxygenated compounds that can lead to corrosion issues during bio-oil processing and storage. This Laboratory Analytical Procedure (LAP) allows for rapid screening of a bio-oil's corrosivity without the need for complex equipment and long-term exposures. A robust and repeatable method for assessing the corrosivity of bio-oils is necessary in order to remove materials degradation as an obstacle to research, upgrading, use and storage of bio-oils. This LAP involves the incubation of a representative alloy, 410 stainless steel (410 SS), specimen in bio-oil over a period of 48 hours at 50 degrees C in a sealed container. The corrosive species in the bio-oil react with and deplete alloy elements such as iron (Fe) and/or chromium (Cr) from the specimen into the bio-oil solution. The depletion of Fe and Cr from the specimen results in a significant mass loss that can be recorded. The mass loss is directly correlated to the corrosivity of a bio-oil. Examples of bio-oils in scope include the ones produced by fast pyrolysis and catalytic fast pyrolysis, as well as liquids produced from hydrothermal liquefaction.

09 BIOMASS FUELS↗

Multilayer Architecture Barriers for High Temperature Nuclear Applications

Innovative thin film multilayer metal/ceramic barrier coatings have been developed by Argonne National Laboratory to protect fuel cladding against different phenomena that can be encountered under the harsh operating conditions of advanced nuclear reactors. One phenomenon is Fuel-Cladding Chemical Interaction (FCCI), which can represent a challenge to the performance of steel-clad metallic fuels in sodium-cooled fast reactors (SFRs), especially when operating to high burnups at elevated cladding temperatures, and long fuel residence time. Another phenomenon is the corrosion of zirconium-based cladding under prototypic boiling water reactor (BWR) conditions and associated cladding during off normal conditions, including loss of coolant accidents (LOCA). This work provides details of the development and testing of a thin film (few microns) multilayer metal/ceramic (CrY/Y 2 O 3 ) coatings on steel cladding and its performance against FCCI. The coating architecture evolved through systematic mechanical testing, radiation tolerance assessments, and high-temperature diffusion studies from a preliminary multilayer concept to an optimized high-performance design. The optimized structure leverages stoichiometric Y 2 O 3 for its exceptional radiation stability, chemical inertness, and ultra-low fission product diffusivity (e.g., Ce diffusivity ~10 -20 m 2 /s in irradiated Y 2 O 3 at 650 °C). This is paired with ductile chromium-rich interlayers (Cr 95 Y 5 ), which significantly enhance fracture toughness and mechanical resilience. Design refinements, including increased ceramic layer thickness and optimized Cr–Y interlayer composition, eliminated fracture propagation and preserved coating integrity under extreme mechanical stress (>10× typical reactor conditions) and prolonged radiation exposure (~300 dpa). Those conditions are well beyond expected conditions during normal operations in SFR, and cover some of the transient conditions as well. In addition, the coating deposition was demonstrated to be applied uniformly to the inner surface of steel tubes representing prototypic SFR cladding. Another phenomenon under consideration in this work is the corrosion of zirconium-based cladding under prototypic boiling water reactor (BWR) conditions and associated off normal conditions including loss of coolant accident (LOCA). Another multilayer thin film coating is considered for mitigation of this phenomenon, where a coating of yttrium aluminum and yttrium aluminum ceramic/metal thin film coating. Preliminary results on the coating performance during high temperature thermal cycling (up to 1000 C) have shown promising performance of the coating. On-going optimization of the coating will continue in FY26.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Strategic Plan: Decrease Critical Minerals Waste Through Enabling Advanced Manufacturing Techniques

In this report we developed a strategic outlook derived from previous findings by our Phase-2 Scorecard Report and the Critical Mineral Evaluation Report. In addition, Phase 2 Materials Scorecards have been developed in 2022 to provide a detailed justification and traceability for the adoption of additively manufactured structural materials and ceramics for nuclear deployment. The report provides a strategic vision to harvest the benefits of reduced material and energy demands by enhanced deployment of advanced manufacturing in nuclear technology. The objective of this report is to address the needs for imminent experimental/computational studies to optimize the deployment of advanced manufacturing for its energy-, cost-, and critical materials saving potentials. We display what further actions are needed to minimize supply risks of critical minerals and to lower the economic vulnerability when implementing the additional nuclear capacity projected by 2050, in support of the U.S. goal of net-zero carbon emission. The critical minerals essential for Gen-IV nuclear technology show either low disruption potential (supply risks) combined with high economic vulnerability, such as: copper, nickel, and chromium; or low supply risks combined with medium economic vulnerability, such as: manganese, molybdenum, tungsten, vanadium, tantalum, and zirconium. Enhancements in quality and yield of critical mineral recycling and the recovery of critical minerals from solid and industrial waste streams are needed to enhance supply security for stainless-steel production and to shift the time to scarcity for society to future years.

36 MATERIALS SCIENCE↗

Combining four-point bending and corrosion to map stress-dependent corrosion susceptibility of 316H stainless steel in FLiNaK

Understanding the effect of stress on the corrosion of steels in molten salts is important for material screening and safety assessment of molten salt reactors. We present a method that combines four-point bending with corrosion testing, enabling the mapping of corrosion susceptibility as a function of local stress from a single specimen. Guided by finite element analysis, a four-point bending setup was used to bend a 316H stainless-steel bar under controlled elastic stress during a 100-hour exposure in FLiNaK at 700 °C. Post-exposure characterization using scanning electron microscopy and energy-dispersive X-ray spectroscopy revealed a pronounced correlation between stress and corrosion. Regions under tensile stress exhibited significantly deeper attack depths and greater chromium depletion along grain boundaries, whereas compressive zones showed shallower corrosion cracks. The stress effect is attributed to stress concentration under tensile loading, which promotes chromium dissolution and crack propagation. This technique can be readily applied to other structural alloys, enabling quantitative measurement of corrosion susceptibility as a function of local stress.

316H↗

Effect of Microstructural Bands on the Localized Corrosion of Laser Surface-melted 316L Stainless Steel

The localized corrosion of laser surface melted (LSM) 316L stainless steel is investigated by a combination of potentiodynamic anodic polarization in 0.1M HCl and microscopic investigation of the initiation and propagation of localized corrosion. The pitting potential of LSM 316L is significantly lower than the pitting potential of wrought 316L. The LSM microstructure is highly banded as a consequence of the high laser power density and high linear energy density. The bands are composed of zones of changing modes of solidification, cycling between very narrow regions of primary austenite solidification and very wide regions of primary ferrite solidification. Pits initiate in the outer edge of each band where the mode of solidification is primary austenite plane front solidification and primary austenite cellular solidification. The primary austenite regions have low chromium concentration (and possibly low molybdenum concentration), which explains their susceptibility to pitting corrosion. The ferrite is enriched in chromium, which explains the absence of pitting in the primary ferrite regions. The presence of the low chromium regions of primary austenite solidification explains the lower pitting resistance of LSM 316L relative to wrought 316L. The influence of banding on localized corrosion is applicable to other rapidly solidified processes such as additive manufacturing.

36 MATERIALS SCIENCE↗

Environmental degradation of electroplated nickel and copper coated SS316H in molten FLiNaK salt

Corrosion of nickel and copper electroplated coatings on SS316H in molten FLiNaK salt was studied. 500- and 1000-hour static corrosion tests were performed in molten FLiNaK at 700 degrees Celsius. Characterization of the coatings following corrosion indicated that they did not degrade in the molten salt during the corrosion experiment and fully protected the underlying SS316H from chromium dissolution. Interdiffusion between the copper coating and SS316H was extremely limited, interdiffusion between the nickel coating and SS316H. Diffusion modelling revealed that the nickel coatings still significantly reduced chromium dissolution over 60 years despite the interdiffusion.

36 MATERIALS SCIENCE↗

Enhancing cold spray coatings: Microstructural dynamics and performance attributes of Inconel 625 with chromium carbide incorporation for hydropower applications

The incorporation of chromium carbide (CrC) particles into the cold spray (CS) process is known to mitigate nozzle clogging, although at the expense of deposition efficiency. This study explores the intricate microstructural changes induced by varying amounts of CrC powder (12.5 % and 6 %) in conjunction with Inconel-625 (Inc-625) powder. The deposition was carried out onto A27 cast steel under different CS parameters. Microstructural characterization, including detailed electron microscopy studies, reveals a complex yet structurally stable coating. Noteworthy features include grain fragmentation and a cellular structure enriched with Nb and Mo, with minimal plastic deformation of CrC in the matrix. The cold-sprayed coatings exhibit a significant (~4 times) increase in microhardness compared to the A27 substrate. Mechanical and cavitation erosion properties were systematically investigated. Coatings subjected to higher particle energy conditions with a gas pressure of 600 psi and gas temperature of 650 °C, demonstrated superior resistance to cavitation erosion. This resistance is attributed to a combination of factors, including microstructural characteristics and porosity. Altogether, the study provides valuable insights into the structural dynamics and performance of CS coatings enriched with CrC particles.

A27 cast steel↗

Analysis of Microwave Resonant Cavity Transducer Degradation Mechanisms

We are investigating a microwave resonant cavity transducer for flow sensing in the vessel of a high temperature fluid advanced reactor (AR), such as a molten salt cooled reactor (MSCR) or a sodium fast reactor (SFR). This transducer is a hollow metallic cylindrical cavity, with the flat wall of the cylinder flexible enough to undergo microscopic deflection due to dynamic fluid pressure. Membrane deflection leads to a shift in the resonant frequency, which can be detected with a spectrum analyzer. Because the transducer is intended for immersion in a high temperature corrosive fluid, understanding of material degradation is crucial for estimation of transducer performance lifetime, and development of measurement interpretation algorithms. We conducted a preliminary computational investigation of relevant damage mechanisms of a stainless steel 316 cylindrical resonator in FLiBe salt. The two main damage mechanisms, creep and corrosion, were modeled using multiphysics COMSOL software. Degradation was modeled for a temperature range 500°C to 700°C. Coupling of the damage mechanisms was not considered. These models predict significant inelastic deformation at most temperatures due to creep, and qualitatively predict chromium depletion both along the liquid/solid interface and along the grain boundaries. An algorithmic approach for compensation of these degradation effects during fluid flow measurements will be developed in the future work.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Second Annual Report on Development of Microwave Resonant Cavity Transducer for Fluid Flow Sensing

We are investigating a microwave resonant cavity transducer for flow sensing in the vessel of a high temperature fluid advanced reactor (AR), such as a molten salt cooled reactor (MSCR) or a sodium fast reactor (SFR). This transducer is a hollow metallic cylindrical cavity, with the flat wall of the cylinder flexible enough to undergo microscopic deflection due to dynamic fluid pressure. Membrane deflection leads to a shift in the resonant frequency, which can be detected with a spectrum analyzer. Because the transducer is intended for immersion in a high temperature corrosive fluid, understanding of material degradation is crucial for estimation of transducer performance lifetime, and development of measurement interpretation algorithms. We conducted a preliminary computational investigation of relevant damage mechanisms of a stainless steel 316 cylindrical resonator in FLiBe salt. The two main damage mechanisms, creep and corrosion, were modeled using multiphysics COMSOL software. Degradation was modeled for a temperature range 500°C to 700°C. Coupling of the damage mechanisms was not considered. These models predict significant inelastic deformation at most temperatures due to creep, and qualitatively predict chromium depletion both along the liquid/solid interface and along the grain boundaries. An algorithmic approach for compensation of these degradation effects during fluid flow measurements will be developed in the future work. To validate sensor physics, we have performed proof-of-principle test of flow sensing in water. For this test, we have developed a cylindrical resonator for K-band, which was machined from brass. The cavity was excited through WR-42 waveguide through a subwavelength hole on the side of the wall of the cylinder. To increase the spectral signal visibility, we developed a signal processing method for baseline subtraction. A flow loop for proof-of-principle test of transducer performance in water was assembled. A commercial flow meter was installed in the loop for reference measurements. Cylindrical cavity was excited in the TE 011 mode with resonant frequency f ≈ 17.8GHz. Frequency shift of cavity spectral response was obtained by gradually increasing water flow rate from 0 to 60gpm. Corresponding monotonic increase of resonant frequency shift by several MHz was observed. Approximate figure of merit of sensitivity to flow rate is 100KHz/GPM. In addition, we have identified an existing liquid sodium experimental setup for demonstration of flow sensing in environment similar to that of an advanced reactor. The setup consists of a cylindrical vessel and center feed line, where transducer inserted through the lid will measure velocity of the impinging liquid jet. As a calibration experiment, we have assembled a water vessel with center feed with the same dimensions as those of the liquid sodium setup. We have also developed and insertion probe consisting of a 50cm brass waveguide enclosed in protective SS316 tube. Using the water loop, we have demonstrated feasibility of sensing the impinging liquid jet in the vessel.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Corrosion Response of Ni-19Cr-5Fe in Molten NaCl-MgCl 2 Salt

Ni-based alloys are strong candidates for use in high-temperature molten salt reactors due to their superior corrosion resistance and mechanical stability compared to stainless steels. In this study, the static corrosion behavior of a Ni-19Cr-5Fe model alloy was systematically evaluated in a purified molten NaCl-MgCl 2 salt at 700°C for 30, 240, and 500 h. Post-exposure analyses were conducted to assess microstructural evolution, corrosion depth, and elemental depletion profiles. Corrosion rates, quantified by chromium depletion depth, followed an inverse power-law trend with increasing exposure time, indicating diffusion-limited kinetics. This trend is attributed to limitations in mass transport in the static salt and to the progressive local depletion of reactive chromium species. Coupled electron backscatter diffraction and energy dispersive X-ray spectroscopy analysis further revealed that the grain boundary character significantly influences corrosion susceptibility: high-angle grain boundaries exhibited pronounced Cr depletion and pitting, while low-angle and Σ3 boundaries remained comparatively resistant. These results offer valuable insight into the role of microstructure in corrosion processes and reinforce the importance of time-dependent material evaluation in molten salt environments relevant to advanced reactor designs.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

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↗

Influence of Powder Characteristics and Processing Methods on Creep Performance of Powder Metallurgy Hot Isostatic Pressed SS316

The U.S. nuclear energy expansion goals are driving the demand for manufacturing routes that can rapidly produce large, complex, near net shape components. Powder metallurgy hot isostatic pressing (PM HIP) is an advanced manufacturing technique that can be economically scaled-up, while alleviating the supply chain challenges that forging and casting face in terms of cost and lead time constraints. This makes PM-HIP a viable technology to aid and accelerate large-scale part manufacturing for nuclear applications. However, large-scale qualification and deployment of this technology require a thorough understanding of the influence of powder feedstock quality, powder handling history, hot isostatic pressing (HIP) parameters, and subsequent heat treatment on microstructural evolution and elevated temperature mechanical performance. The present work focusses on 316 austenitic stainless steel (SS316) which is most commonly used in high temperature environments for nuclear applications Results from this study show that PM HIPed SS316 meets ASME tensile requirements at room temperature and at elevated temperature. However, creep performance of PM-HIPed SS316 remains inferior to its wrought counterpart, demonstrating that tensile performance alone is not a reliable metric for long duration high temperature integrity. Further, this report delineates powder derived microstructural features that govern creep damage, with key evidences pointing to “microstructural inheritance” from gas atomized powder feedstocks. Commercial SS316 powders of varying chemical compositions and recycling histories were studies, and the results showed large differences in elemental segregation, oxide surface layers and secondary phase distributions. Multi-scale characterization revealed segregation of chromium, molybdenum, manganese and silicon at the boundaries and the precipitation of manganese-, silicon-, and molybdenum-oxides. During HIP consolidation, these surface oxides transform into decorated prior particle boundaries (PPBs) and grain boundary inclusions that persist through conventional post-HIP solution annealing treatment. The retained oxides in post-HIP microstructures were found to influence grain growth, precipitation behavior, and ultimately creep cavitation and fracture. Such post-HIP heat treatments are therefore limited by a complex trade-off between grain growth, and oxide coarsening which aggravate creep damage by acting as nucleation sites for cavities. The objective of this work is to establish an integrated processing–structure–property framework for PM-HIP 316 stainless steel by investigating the influence of powder feedstock characteristics in pre- and post-HIP processing as well as to understand the significance of post-HIP heat treatment on microstructural evolution and creep properties. The results from this report emphasize the significance of powder feedstock integrity in improving creep performance of PM-HIPed SS316, by highlight the effect of rapid solidification, elemental segregation, oxide formation and powder recycling on microstructural defect inheritance following HIP consolidation. Rather than considering HIP processing, solution annealing, and mechanical performance independently, this report treats powder production, HIP consolidation, post-HIP thermal processing, and creep deformation as interconnected stages within a continuous metallurgical process. The resulting framework will provide a scientific basis for developing feedstock engineering strategies capable of improving long-term reliability of PM-HIP stainless steels and accelerating their qualification for advanced nuclear applications.

Ajjarapu, Pavan [Oak Ridge National Laboratory (OR↗

Preliminary Report on Compositional Specification for Printed 316SS

The Advanced Materials and Manufacturing Technologies Program is focused on accelerating the development and deployment of advanced materials and components fabricated via additive manufacturing (AM). A key challenge for the widespread adoption of AM is the variability in material properties, which can originate from powder feedstock, process parameters, geometry, and the machine. AM powder feedstock compositions are based on those developed for conventional manufacturing. However, the smaller melt pools combined with multiple melt cycles over the course of a build can have substantial effects on the local phase selection resulting from minor batch-to-batch feedstock variability. Therefore, this report focuses on coupling CALPHAD calculations with data mining and visualization to aid the development of compositional specifications for stainless steel 316, an important alloy for nuclear applications and suitable for AM. This work reports that δ-ferrite formation has a stronger dependence on the amount of nickel in the alloy despite nickel being an austenite stabilizer. These findings show the need for exercising a tighter control on the amount of nickel in the alloy compared with the amount of chromium, which is a ferrite stabilizer.

36 MATERIALS SCIENCE↗