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At least 19 records

Development of Surveillance Test Articles for Materials Degradation Management in MSR Environments

Materials in molten salt reactors (MSR) undergo accelerated degradation from corrosion, irradiation, and cyclic loads at elevated temperatures. Establishing a materials surveillance program to enable the assessment of material deterioration is critical to assure structural integrity of MSRs components. This presentation summarizes recent efforts towards the development of surveillance test articles for collecting various damages for monitoring materials degradation. Surveillance test articles with reduced dimensions were designed to capture creep-fatigue damage from cyclic loading at elevated temperatures. The strain evolution of test articles during thermal cycling was analyzed both numerically and experimentally. Out-of-reactor thermal cycling demonstrated successful capture of strain range for materials assessment. Moreover, test articles were subject to both mechanical loads and molten salt exposure, and the damage due to stress and corrosion was investigated. Additionally, damage inference models were developed to predict the remaining life of materials based on the accumulated damage in surveillance test articles.

36 - MATERIALS SCIENCE

FY24: LEMMs: Long-term, Electrochemical Materials degradation Models

FY24 progress for LEMMs: Long-term, Electrochemical Materials degradation Models LDRD project are presented. Significant progress toward creating validated corrosion models was made in this FY paving success in future FY’s for success with battery model development and validation. Specifically, models for various forms of corrosion were probed for sensitivities showing a significant influence of reactive transport parameters for hydroxide species on the run time of the models. Further, cryo-genic time-of-flight secondary ion mass spectroscopy was utilized to map ions in a frozen corrosion droplet showing the precipitates/precipitate species near corroding locations. Additionally, a realistic corrosion droplet was created that accounted for evaporation and condensation coupled with corrosion. This pushes the boundary of corrosion modeling and will be validated in future FY’s.

36 MATERIALS SCIENCE

Geospatial modeling of near subsurface temperatures of the contiguous United States for assessment of materials degradation

Abstract Understanding subsurface temperature variations is crucial for assessing material degradation in underground structures. This study maps subsurface temperatures across the contiguous United States for depths from 50 to 3500 m, comparing linear interpolation, gradient boosting (LightGBM), neural networks, and a novel hybrid approach combining linear interpolation with LightGBM. Results reveal heterogeneous temperature patterns both horizontally and vertically. The hybrid model performed best achieving a root mean square error of 2.61 °C at shallow depths (50–350 m). Model performance generally decreased with depth, highlighting challenges in deep temperature prediction. State-level analyses emphasized the importance of considering local geological factors. This study provides valuable insights for designing efficient underground facilities and infrastructure, underscoring the need for depth-specific and region-specific modeling approaches in subsurface temperature assessment.

Science & Technology - Other Topics

On-line Inductively Coupled Plasma Mass Spectrometry Reveals Material Degradation Dynamics of Au and Cu Catalysts during Electrochemical CO 2 Reduction

A significant challenge in commercializing electrochemical CO 2 reduction (CO 2 R) is achieving catalyst durability. Here, in this study, online inductively coupled mass spectrometry (ICP–MS) was used to investigate catalyst degradation via nanoparticle detachment and/or dissolution into metal ions under CO 2 R operating conditions in 0.1 M KHCO 3 . We developed an experimental framework with ex situ characterization to validate the online ICP–MS method for in situ evaluation of degradation from metal foils. By varying the applied potential and microenvironment (CO 2 vs N 2 -saturated electrolyte), we gained insights into the degradation of Au and Cu foils under CO 2 R and hydrogen evolution reaction (HER) conditions. While both Au and Cu foils were observed to be stable to dissolution in these regimes, degradation via nanoparticle detachment from the foil surface at the femtogram scale was observed as a function of reaction conditions, providing new insights into material degradation mechanisms. When applying potential steps at −0.1 and −1.0 V vs the reversible hydrogen electrode (RHE), Au was found to degrade via nanoparticle detachment under CO 2 R operating conditions more than under HER conditions, while Cu was found to degrade via nanoparticle detachment in similar amounts during both reactions. Au lost ∼1.8× more mass and ∼7.5× more nanoparticles than Cu under CO 2 R operating conditions. This study demonstrates the use of online ICP–MS to gain insight into the degradation of Au and Cu, the importance of studying unconventional degradation mechanisms such as nanoparticle detachment, and that online ICP–MS can be further utilized to gain fundamental understanding of catalyst durability for a variety of reaction systems.

Yan, Katherine [Stanford Univ., CA (United States)

Design, Fabrication and Testing of Surveillance Test Articles for MSR Materials Degradation Management

This report details the design, fabrication, and testing of surveillance test articles aimed at assessing material damage in reactor-relevant environments for effective degradation management. Two types of surveillance test articles with reduced sizes were developed based on design algorithms and finite element modeling: welded design and interlocking design. A furnace heating setup was adopted to apply multiple thermal cyclic loading profiles on the test articles with a temperature range of 500°C - 700°C, while the strain response was monitored using a digital image correlation technique. The testing results demonstrated the successful capturing of expected strain range for welded design while machining tolerance should be improved to engage strain coupling in the interlocking design. Mid-term (500 hours) and long-term (1500 hours) cyclic tests were conducted on welded test articles. A constant strain range of ~0.6% was observed at the specimen with testing under 500 hours, while a gradual decrease of strain at specimen was observed after 500 hours. Non-destructive evaluation through X-ray computed tomography confirmed the microcracks in the welds at specimen-driver joints after cyclic test that caused the strain change. Creep testing of the specimen after long-term cyclic test revealed a short creep life than expected. A multi-profile cyclic test was also conducted on a test article and demonstrated consistent strain response under different temperature ramp rates. The report also briefly discussed the challenges and future research efforts to advance test article development for material surveillance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS

Materials Degradation in Extreme Environments: Novel In-situ Measurements of Cracking in Molten Salt

The safety and reliability of next-gen reactors, i.e. molten salt reactors (MSR), depends on materials performance and longevity in extreme environments, yet no in-situ, validated measurement techniques for environmentally assisted cracking (EAC), one potential degradation mechanism, exist for these conditions. This project combined the use of in-situ direct current potential drop (DCPD) crack growth rate determination applied to a horizontal load frame with high temperature fittings and novel sample geometries to enable evaluation in MSR environments and develop a full in-situ SCC measurement capability for extreme environments (high conductivity and elevated T), necessary to predict materials reliability. A successful demonstration of DCPD measurement in molten NaNO 3 /KNO 3 salts at 340 o C was accomplished and validated through post-test fractography imaging. This is the first ever public example, to the authors knowledge, of an in-situ crack growth rate measurement in a molten salt environment.

22 GENERAL STUDIES OF NUCLEAR REACTORS

Coupling Microstructural Evolution Simulations to Material Property Degradation Predictions for Plasma-Facing Materials

Reliable material performance is required for plasma-facing material (PFM) candidates. Previous research has shown that plasma and neutron radiation exposure induces microstructural changes in PFMs; changes in thermal and electrical conductivities and in material hardening and embrittlement were also observed after neutron irradiation. These material property changes will negatively impact the performance of the PFMs in a fusion reactor. Despite the well-known connection between material microstructure, properties, and performance, there is a need for validated modeling capabilities connecting PFM property degradation with microstructural evolution under fusion-relevant conditions. We are developing a simulation capability to couple plasma-induced microstructural evolution to material property degradation. Our approach relies on deliberate mapping between individual simulation models and experimental characterization for validation. The open-source Multiphysics Object-Oriented Simulation Environment (MOOSE) software was used for this simulation capability development. A MOOSE phase-field model was coupled with the cluster dynamics code, Xolotl, to predict microstructural evolution. Microstructure characterization techniques, including scanning electron microscopy (SEM), transmission electron microscopy (TEM), and laser scanning confocal microscopy (LSCM) are used to validate these microstructural evolution simulations. Calculation of thermal and electrical conductivities with first principles simulations was performed for bulk material and for grain boundaries; these results are used within MOOSE models to calculate effective thermal and electrical conductivities as a function of grain characteristics. Thermoreflectance and four-probe techniques were employed to measure the thermal and electrical conductivities, respectively. A MOOSE crystal plasticity model was adapted to predict microstructure-sensitive deformation behavior, and X-ray diffraction (XRD) was used to collect bulk dislocation density data for validation. After individual simulation validation, these models are coupled to predict material property changes resulting from plasma exposure. We focused here on an experimental design to emphasize the separate effects of moderate thermal loads and plasma exposure using tungsten. Annealing of tungsten was performed under a protective environment for temperatures ranging from 500 C to 1500 C. The plasma exposure was completed in the Tritium Plasma Experiment at Idaho National Laboratory under a deuterium flux of 1e22 D/m^2-s. This incremental approach is employed to build confidence in the modeling capability: separate-effects tests ensure that the models capture key mechanisms from single environmental conditions before predicting PFM property degradation under combined loads. We will show our early results from coupling these simulation models to predict PFM property changes from microstructural evolution. Comparisons of the simulation results with preliminary validation data will be discussed.

36 - MATERIALS SCIENCE

Demonstration of the surveillance test article for an advanced reactor surveillance test program

Operational environments in generation IV reactors involve corrosive and irradiative conditions at elevated temperatures. Typical reactor operations consist of transients which impose cyclic loads on reactor components. These cyclic loads, combined with corrosive and irradiative environments, result in synergistic degradation of component materials. However, limited data exists on the coupled damage effects on materials for reactor environments. While the surrogate material surveillance concept has been used in light water reactors to assess irradiation damage, existing material surveillance technologies are not suitable for in-situ monitoring of coupled material degradation. The materials surveillance program focuses on material degradation management and the estimation of remaining life of reactor components through surveillance test articles. This paper presents the design and analysis methodology of a bi-metal surveillance test article, which uses difference in thermal expansion coefficient between two metals to induce in-situ cyclic loads. This report presents the work conducted in FY 25, to test the surveillance test article in air and salt environments. These test specimens were evaluated after thermal cycle exposure and remaining life is measured through creep test.

36 - MATERIALS SCIENCE

Summary of LWRS Research in Addressing RPV Research Gaps in NRC EMDA Report

Reactor Pressure Vessels (RPVs) are critical components in nuclear reactors, housing the reactor core and coolant under extreme conditions of temperature, pressure, and radiation. These harsh environments contribute to the degradation of RPV materials over time, presenting challenges for extending reactor operations beyond their original design lifespans. The NRC Expanded Materials Degradation Assessment (EMDA) report volume 3 have been instrumental in guiding research to support extending the operational life of light water reactors (LWRs) up to 80 years. It provides a comprehensive framework to address technical challenges related to aging and degradation mechanisms in RPVs. The LWRS program has played a key role in advancing this research, supporting projects such as the UCSB ATR-2 Experiment, material testing from Zion and Palisades reactors, and the development of advanced mini-compact tension testing techniques. These efforts have been crucial in identifying and addressing gaps in our understanding of RPV aging, contributing to the successful subsequent license renewals of eight LWR units in the U.S. The EMDA report volume 3, built on the Phenomena Identification and Ranking Table (PIRT) analysis from earlier versions of the EPRI Materials Degradation Matrix (MDM) and Issue Management Tables (IMTs), provides a detailed assessment of RPV degradation mechanisms. However, as EPRI has updated the MDM and IMT, it is important to revisit research priorities and methodologies to reflect these changes. The revised MDM and IMT may introduce new factors affecting long-term RPV performance and safety, highlighting the need for continued research and updated guidance to ensure the reliable and safe operation of reactors beyond 80 years.

22 GENERAL STUDIES OF NUCLEAR REACTORS

ENVIRONMENTAL DEGRADATION OF HARD AND SOFT MAGNETIC MATERIALS IN GASEOUS AND SUPERCRITICAL CO2 ENVIRONMENTS

It may be beneficial to use hermetic designs for supercritical CO2 (sCO2) cycles machinery as they would eliminate CO2 leakage through shaft end seals. This would reduce CO2 emissions and operating costs for makeup of lost process fluid. Those designs may replace traditional oil-lubricated bearings with actively controlled magnetic bearings operating at high temperatures in the process fluid environment (to reduce the need for active cooling). This paper investigates the material degradation of various types of magnets in CO2. Included are several permanent and soft magnetic materials (Alnico 9C, Alnico 5-7C, and 18-T550 grade SmCo, and Hiperco 50) with or without coatings (nickel plating or C5 coating). The materials were exposed to: (1) flowing gaseous CO2 at 1,022 °F (550 °C) and atmospheric pressure in a furnace and (2) sCO2 at 842 °F (450 °C) and 1,500 psi (103 bar) in an autoclave. The preliminary mass change measured after total exposures of 1,000 hours and 2,000 hours are included.

supercritical CO2, magnetic material

Current and Future Technological Issues Challenges for Nuclear Graphite Components

Historical and current data requirements for component qualification, as-manufactured graphite material properties, Irradiated & degraded material issues, code rules – Construction & Operation, status of current ASME code rules, progress in design rules, degradation, construction vs. operation, what should we be planning, and new technical areas getting started.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS

Compaction and Morphology of Lost Circulation Materials

Lost circulation material (LCM) selection is critical to effectively and efficiently treating wellbore fluid losses in geothermal drilling where costs of treatment can be as much as 30% of the total drilling cost. We conducted several uniaxial compaction experiments on 10 different materials and several material mixtures to identify critical mechanical parameters of each. Materials degraded at 200°C were also investigated to understand how elevated temperatures in geothermal wells would degrade their compaction behavior. Granular materials tended to have lower compressibility and higher compression resistance, while more elongated and softer materials had less mechanical stiffness. Mixing materials tended to moderate the mechanical behaviors while heating universally increased the compaction of materials. Microscopy showed that particle strength tended to correlate positively with roundness and circularity and negatively with elongation of a material. Convexity of the degraded and undegraded materials showed heating may have increased the convexity or roughness of the individual particles. In conclusion, we concluded that granular materials are likely to provide the best seals in wells but that a mixture of size distribution, mechanical rigidity, and elongation is more likely to form a better seal for geothermal wells.

annular pressure drilling

Molecular Imaging of Microbially Induced Corrosion of Synthetic Archeological Glasses by a Rhizosphere Bacterium

Microbially induced corrosion (MIC) focuses on the degradation of solid materials, such as glass or metal. Soil microbes are often associated with the corrosion of foreign objects in the rhizosphere. Paenibacillus polymyxa SCE2, a facultative anaerobic bacterium in soil, is of the same genus as bacteria found near nuclear waste disposal sites. Time-of-flight secondary ion mass spectrometry (ToF-SIMS) was used for imaging surface changes induced by P. polymyxa SCE2 cultured on two synthetic glass coupons to represent natural analogs of materials that were studied in relation to the vitrification of nuclear waste. Multimodal imaging was used to verify bacterial coverage across the glass surface after long-term growth. ToF-SIMS spectral analysis showed detection of glass component ions, such as silicon oxide (m/z – 59.96 SiO 2 – ) and aluminum oxide (m/z – 101.95 Al 2 O 3 – ), and biofilm’s extracellular polymeric substance (EPS) components, such as pentadecanoic acid (m/z – 241.22 C 15 H 29 O 2 – ) and sterol lipids (m/z – 311.16 C 20 H 23 O 3 – ). ToF-SIMS spectral, imaging, and depth profiling analyses showed that the glass rich in silica and other light elements (“granite glass”) had more “corrosion related” peaks than the glass that was less silica-rich and contained more iron (“dike glass”). Furthermore, these surface and interface compositional and spatial differences observed in the mass spectra and imaging were attributed to bacterial metabolism and an electron transfer mechanism influenced by morphological and compositional differences between the two types of glasses. ToF-SIMS is effective in studying microbial effects, bringing new molecular insights into MIC in a broader context of materials degradation.

Amorphous materials

In-situ ETEM study of plasma-facing tungsten nanofuzz oxidation at atmospheric pressure: Microstructure evolution and substrate-free oxidation kinetics

To enable sustainable carbon-free fusion energy, managing reactor structural material degradation during normal operation as well as accident scenarios is vital. Tungsten (W) plasma-facing materials (PFMs) are susceptible to aggressive high-temperature oxidation during air-ingress fusion reactor accidents, yet there's a lack of oxidation kinetic data for irradiated tungsten. Here, in this study, we utilize atmospheric environmental transmission electron microscopy (ETEM) to present the first kinetic data for substrate-free W nanofuzz oxidation at 400 ºC and 500 ºC in 1 bar dry air. Comparison with pristine bulk W during the early parabolic stage suggests an irradiationdecelerated oxidation for W nanofuzz. Our time-resolved in-situ characterization reveals a durable amorphous surface oxide, likely promoted by high-flux He + irradiation-induced surface defects, serving as an effective passivating layer that impedes nanofuzz oxidation onset. This surface oxide layer also interfaces well with newly formed orthorhombic WO 3 , facilitated by stress relief through He bubble shrinkage, providing lasting passivating protection throughout the nanofuzz parabolic oxidation. This new finding challenges conventional notions of irradiation's negative impact on metal oxidation, and calls for advanced characterization to enhance our understanding of fusion energy materials degradation, informed by further accident modeling.

36 MATERIALS SCIENCE

Carbon Fiber Oxidation in 4D

The oxidation of carbon fibers at high temperatures is the primary degradation process in the thermal protection system of many hypersonic flight vehicles. Predicting the rate and the extent of oxidation is critical to ensure a safe and effective design. An oversized thermal protection system adds unnecessary mass, while an under-designed one risks system failure and mission loss. Resolving high-temperature material degradation due to oxidation has been a long-standing challenge in designing for re-entry flight environments. Using time-resolved in situ X-ray microtomography, the oxidation of carbon fibers at high temperatures is directly imaged, resolving the two limiting degradation regimes: diffusion- and reaction-limited. The ability to resolve material degradation in time at the sub-micron scale sheds light on the ablation phenomenon and enables predictions of material constitutive properties evolving in time, with profound implications on the ability to model the aerothermal response of heat shield materials in hostile environments.

ablation

Iso-cost-performance of thermal energy storage

As thermal energy storage (TES) systems gain increasing recognition as next-generation energy storage solutions, evaluating their techno-economic performance is crucial. This perspective analyzes the cost-performance of latent heat-based TES systems and introduces the concept of iso-cost-performance—maintaining a constant cost per unit energy ($\$$/kWh) despite material degradation. Using an empirical degradation model, we show that after 1200 thermal cycles, the thermal conductivity and volumetric energy density of a paraffin-based phase change material (PCM) decreased by 36.0% and 26.1%, respectively, resulting in a 31.2% reduction in the figure of merit (FOM) and, consequently, the system cost-performance. However, by introducing thermally conductive additives to enhance effective thermal conductivity, the TES system can recover its initial FOM, achieving iso-cost-performance operation. This framework quantitatively demonstrates how degradation-mitigation strategies—such as improving thermal conductivity—can offset material degradations and maintain long-term cost-effectiveness. Beyond PCM-based TES, the proposed FOM-based approach provides a generalized pathway for cost-performance optimization across various TES technologies.

25 ENERGY STORAGE

A Multiphysics Multiscale Simulation Platform for Damage, Environmental Degradation, and Life Prediction of CMCs in Extreme Environments

This project successfully developed a multiphysics, multiscale computational framework to enhance the design and development of CMCs, with a focus on modeling highly nonlinear, time-dependent damage mechanisms and material degradation under extreme conditions, such as those experienced in turbine service environments. The project made significant advances in improving our understanding of progressive damage, oxidative degradation, and time-dependent inelastic deformation in CMCs, with particular attention to the role of uncertainties in predictions. Key outcomes include the integration of advanced material characterization, uncertainty quantification, and multiphysics constitutive models to predict the behavior of CMCs over their service life. A novel multiscale methodology was employed, which integrated microscale constituent behaviors with structural-scale responses, enabling the manufacturing defects in the microstructure that are prone to damage nucleation. Through the development of DL algorithms, the project advanced the prediction of damage initiation and crack propagation, taking into account the defect morphology and statistical variations across multiple scales. The framework was rigorously validated using thermomechanical experiments, which tested CMCs under various mechanical loadings at elevated temperatures, further enhancing the model's predictive capability. Overall, the research outcomes have provided a more accurate, reliable method for predicting CMC component life, significantly advancing material design, and improving component reliability in extreme environments. This work has strong implications for the optimization of turbine components and other high-performance applications where CMCs are used.

03 NATURAL GAS