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DOE OSTI2023

Survey Corrosion Testing Methodologies for Additively Manufactured Materials – PNNL

The Advanced Materials and Manufacturing Technology (AMMT) Program intends to develop cross-cutting technologies in support of a broad range of nuclear reactor technologies, and to maintain U.S. leadership in materials and manufacturing technologies for nuclear energy applications. The overarching vision of the AMMT Program is to accelerate the development, qualification, demonstration, and deployment of advanced materials and manufacturing technologies to enable reliable and economical nuclear energy.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Operando carbon corrosion measurements in fuel cells using boron-doped carbon supports

Carbonaceous materials are the most common catalyst supports in proton exchange membrane fuel cell (PEMFCs), yet their corrosion is one of the limiting factors in achieving high durability. Herein, we doped carbon supports with boron (B) to increase the corrosion-resistance of the support. Two types of B-doped carbons were synthesized and studied as platinum support materials. Further, they varied in their morphologies, surface areas, and the types of boron species. The durability of Pt/B-doped carbon catalysts was investigated using the US-DOE catalysts’ supports accelerated stress test (AST) and a mass-spectrometer connected to the fuel cell effluent stream to quantify the mass of corroded carbon support in operando. The addition of boron to the carbon increased the stability of Pt catalysts in long-term usage of PEMFC. After 4000 AST cycles, more than 50% of initial current density was preserved for the boron-containing systems, while less than 30% of it remained with Vulcan carbon (Pt/V). Also, the Pt/B-doped carbon samples demonstrated better electrochemical active surface area (ECSA) stability when compared to Pt/V. Carbon loss measurements showed that B-doped carbons have higher resistance to electrochemical corrosion than unmodified carbon. Specifically, the substitutional boron-doped carbon demonstrated an extremely high stability and low corrosion rate.

25 ENERGY STORAGE↗

NASA NTRS2014

Film Cooled Recession of SiC/SiC Ceramic Matrix Composites: Test Development, CFD Modeling and Experimental Observations

SiCSiC ceramic matrix composites (CMCs) systems will play a crucial role in next generation turbine engines for hot-section component applications because of their ability to significantly increase engine operating temperatures, reduce engine weight and cooling requirements. However, the environmental stability of Si-based ceramics in high pressure, high velocity turbine engine combustion environment is of major concern. The water vapor containing combustion gas leads to accelerated oxidation and corrosion of the SiC based ceramics due to the water vapor reactions with silica (SiO2) scales forming non-protective volatile hydroxide species, resulting in recession of the ceramic components. Although environmental barrier coatings are being developed to help protect the CMC components, there is a need to better understand the fundamental recession behavior of in more realistic cooled engine component environments.In this paper, we describe a comprehensive film cooled high pressure burner rig based testing approach, by using standardized film cooled SiCSiC disc test specimen configurations. The SiCSiC specimens were designed for implementing the burner rig testing in turbine engine relevant combustion environments, obtaining generic film cooled recession rate data under the combustion water vapor conditions, and helping developing the Computational Fluid Dynamics (CFD) film cooled models and performing model validation. Factors affecting the film cooled recession such as temperature, water vapor concentration, combustion gas velocity, and pressure are particularly investigated and modeled, and compared with impingement cooling only recession data in similar combustion flow environments. The experimental and modeling work will help predict the SiCSiC CMC recession behavior, and developing durable CMC systems in complex turbine engine operating conditions.

Recession↗

DOE OSTI2025

Field‐Relevant Degradation Mechanisms in Metal Halide Perovskite Modules

Field testing, failure analysis, and understanding of degradation mechanisms are essential to advancing metal halide perovskite (MHP) photovoltaic (PV) technology toward commercialization. Here, we present performance data from up to 1 year of outdoor testing of MHP modules in Golden, Colorado. The module encapsulation architecture and encapsulant materials have a significant impact on module reliability, with modules containing a polyolefin elastomer (POE) in addition to a desiccated polyisobutylene (PIB) edge seal outlasting modules with only a PIB edge seal or PIB blanket. Nondestructive and destructive characterization of the field-tested modules points to module scribes and interfaces as areas of potential mechanical weakness and chemical migration, resulting in shunt pathways and increased series resistance. Finally, indoor accelerated stress testing with light and elevated temperatures is performed, demonstrating failure with similar scribe degradation signatures as compared to the field-tested modules. In conclusion, under both outdoor testing and light and elevated temperature conditions, electrochemical corrosion between the copper electrode and the mobile iodine ions appeared dominant, with a significant progression at the scribes that is speculated to result from an interplay between the initial laser damage and joule heating from enhanced ion diffusion under bias.

14 SOLAR ENERGY↗

DOE OSTI2023

Optimized purification methods for metallic contaminant removal from directly recycled Li-ion battery cathodes

Metallic contaminants pose a significant challenge to the viability of directly recycling Li-ion batteries. To date, few strategies exist to selectively remove metallic impurities from mixtures of shredded end-of-life material (black mass; BM) without concurrently damaging the structure and electrochemical performance of the target active material. We herein present tailored methods to selectively ionize two major contaminants—Al and Cu—while retaining a representative cathode (LiNi 0.33 Mn 0.33 Co 0.33 O 2 ; NMC-111) intact. This BM purification process is conducted at moderate temperatures in a KOH-based solution matrix. We rationally evaluate approaches to increase both the kinetic corrosion rate and the thermodynamic solubility of Al 0 and Cu 0 , and evaluate the impact of these treatment conditions on the structure, chemistry, and electrochemical performance of NMC. Specifically, we explore the impacts of chloride-based salts, a strong chelating agent, elevated temperature, and sonication on the rate and extent of contaminant corrosion, while concurrently evaluating the effects on NMC. The reported BM purification process is then demonstrated on samples of “simulated BM” containing a practically relevant 1 wt% concentration of Al or Cu. Increasing the kinetic energy of the purifying solution matrix through elevated temperature and sonication accelerates the corrosion of metallic Al and Cu, such that ∼100% corrosion of 75 μm Al and Cu particles is achieved within 2.5 hr. Further, we determine that effective mass transport of ionized species critically impacts the efficacy of Cu corrosion, and that saturated Cl – hinders rather than accelerates Cu corrosion by increasing solution viscosity and introducing competitive pathways for Cu surface passivation. The purification conditions do not induce bulk structural damage to NMC, and electrochemical capacity is maintained in half-cell format. Testing in full cells suggests that a limited quantity of residual surface species are present after treatment, which initially disrupt electrochemical behavior at the graphite anode but are subsequently consumed. Process demonstration on simulated BM suggests that contaminated samples—which prior to treatment show catastrophic electrochemical performance—can be recovered to pristine electrochemical capacity. The reported BM purification method offers a compelling and commercially viable solution to address contamination, particularly in the “fine” fraction of BM where contaminant sizes are on the same order of magnitude as NMC and where traditional separation approaches are unfeasible. Thus, this optimized BM purification technique offers a pathway towards viable direct recycling of BM feedstocks that would otherwise be unusable.

25 ENERGY STORAGE↗

DOE OSTI2023

Accelerating Nuclear Fuels and Materials Qualification by Multi-Level Irradiation Experiment Campaign

The advanced reactor technologies feature fuels, coolants, and materials that promise safer operating conditions under normal and accident scenarios. However, the nuclear fuels and materials qualifications require several decades (for example, new reactor fuel qualification from conceptualization requires about 20 years). Therefore, accelerating nuclear fuels and materials qualification is essential, and it can be achieved by combining high through-put materials irradiation and testing, advanced post-irradiation examinations, and Multiphysics modeling. This paper addressed the associated challenges in accelerating nuclear fuels and material qualification for new and advanced reactor designs, which differ based on fuel, coolant, operating conditions, and structural materials. These challenges vary for radiation level, operating conditions (e.g., temperature and pressure), and coolant type (e.g., corrosion environment). In addition, the challenges and limitations in modeling tools, experimental facilities, and licensing guidelines are also discussed, and a general solution path forward is recommended.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2023

Presentation: Accelerating Nuclear Fuels and Materials Qualification by Multi-Level Irradiation Experiment Campaign

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2023

Novel pyrolytic boron nitride coating to reduce graphite interactions in molten fluoride salt

Future salt reactors like the Fluoride-salt-cooled-High Temperature Reactor require varying material flavors. Graphite is required for neutron moderation and potential fuel forms, while structural metals are required for containment. Studies show graphite/metal interactions exist when both materials share a salt medium. These interactions may accelerate the corrosion of the metal and change the surface of graphite materials. A novel pyrolytic boron nitride coating on graphite is investigated for reducing graphite/metal interactions. Finally, this is the first known application of such a coating, and salt exposure tests reveal the pyrolytic boron nitride coating reduces the interactions between stainless steel and uncoated graphite.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2020

Corrosion of AISI 310 and 316 in Molten Hydroxide Under Steam Electrolysis Conditions

Steam electrolyzers, utilizing molten hydroxide electrolyte, offers potential for improvement in electrochemical efficiency, cost reduction, use of conventional materials of construction and process scale up for large scale hydrogen production. Stainless steels, used for the fabrication of cell components (current collector, gas separator, wet seals, and manifolds) experience accelerated corrosion in the presence of molten hydroxide electrolyte in both oxidizing (anodic) and reducing (cathodic) atmospheres. In this study, the corrosion behavior of AISI 310 and 316 in hydroxide melt has been studied at 600°C for 50 h. Melt immersion tests revealed formation of the porous lithium iron oxide at the melt-oxide interface for both AISI 310 and 316. Inductively coupled plasma optical emission spectrometry (ICP-OES) analysis showed the presence of Cr in the electrolyte melt obtained from samples exposed to oxidizing atmosphere. Thermochemical analysis was performed to validate the experimental results.

corrosion↗

DOE OSTI2023

Measurement and Reporting Guidelines for Solar Mirror Aging Tests Using Xenon Arc Lamp Exposure (XALE)

This technical report provides a guideline for accelerated aging tests on solar reflectors. Solar reflectors must have a high durability, with goal lifespans reaching 30 years. To test and develop state-of-the-art solar reflectors, relevant durability tests must be conducted. Existing guidelines for materials testing include isothermal testing, humidity testing, corrosion, etc., but many tests do not specify to include solar irradiance or address its relevance to solar reflector durability. The guideline focuses on test design and reporting guidelines for using Xenon Arc Lamp Exposure (XALE). The XALE environmental chambers can subject samples to a combination of relevant environmental factors including concentrated solar irradiance, heat, humidity, and weathering cycles. The guideline is meant to provide information on developing relevant test conditions, exposure times, reflectance characterization procedures, and data reporting.

14 SOLAR ENERGY↗

DOE OSTI2023

Acceleration Factors for Combined‐Accelerated Stress Testing of Photovoltaic Modules

Combined‐accelerated stress testing (C‐AST) is developed to establish the durability of photovoltaic (PV) products, including for degradation modes that are not a priori known or examined in standardized tests. C‐AST aims to comprehensively represent the sample, stress factors, and their combinations using levels at the statistical tails of the natural environment. Acceleration factors for relevant climate sequences within the C‐AST cycle with respect to the Florida USA climate are estimated for selected degradation mechanisms. It is found that for degradation of the outer backsheet polymer layer, the acceleration factor of the tropical climate sequence (the longest of the climate sequences) is f ( T , G ) = 17.3 with ultraviolet photodegradation; for polyethylene terephthalate hydrolysis (backsheets), f ( T , RH ) = 426; for electrochemical corrosion (PV cell), f ( I ) = 14.1; and for PbSn solder fatigue f (Δ T , r ( T )) = 17.3. Here, T is the module temperature, G is the broadband spectrum irradiance on the plane of array of the module, RH is the relative humidity on the module surface, I is the leakage current through the module packaging, and r ( T ), the number of temperature reversals. The methods discussed herein are generally applicable for evaluating acceleration factors in other accelerated test methods.

14 SOLAR ENERGY↗

NASA NTRS1991

Microbial biofilm studies of the Environmental Control and Life Support System water recovery test for Space Station Freedom

Analysis of biofilm accumulation, studies of iodine disinfection of biofilm, and the potential for microbially influenced corrosion in the water recovery test (WRT) are presented. The analysis of WRT components showed the presence of biofilms and organic deposits in selected tubing. Water samples from the WRT contained sulfate-reducing and acid-producing organisms implicated in corrosion processes. Corrosion of an aluminum alloy was accelerated in the presence of these water samples, but stainless steel corrosion rates were not accelerated.

Obenhuber, D. C.↗

NASA NTRS2006

Methodology for Life Testing of Refractory Metal/Sodium Heat Pipes

The focus of this work was to establish an approach to generate carefully controlled data that can conclusively establish heat pipe operating life with material-fluid combinations capable of extended operation. To accomplish this goal acceleration is required to compress 10 years of operational life into 3 years of laboratory testing through a combination of increased temperature and mass fluence. Specific test series have been identi3ed, based on American Society for Testing and Materials (ASTM) specifications, to investigate long term corrosion rates. The refractory metal selected for demonstration purposes is a Molybdenum-44.5%Rhenium alloy formed by powder metallurgy. The heat pipe makes use of an annular crescent wick design formed by hot isostatic pressing of Molybdenum-Rhenium wire mesh. The heat pipes are filled using vacuum distillation and purity sampling is considered. Testing of these units is round-the-clock with 6-month destructive and non-destructive inspection intervals to identify the onset and level of corrosion. Non-contact techniques are employed for providing power to the evaporator (radio frequency induction heating at I to 5 kW per unit) and calorimetry at the condenser (static gas gap coupled water cooled calorimeter). The planned operating temperature range would extend from 1123 to 1323 K. Accomplishments prior to project cancellation included successful demonstration of the heat pipe wick fabrication technique, establishment of all engineering designs, baselined operational test requirements and procurement/assembly of supporting test hardware systems.

Martin, James J.↗

DOE OSTI2025

Preliminary Plan to Inform Testing of a Heat Exchanger Test Article

This report presents a preliminary plan to guide the qualification testing of advanced heat exchanger (HX) components for nuclear-to-industrial heat transfer applications. The objective is to establish a defensible, physics-based methodology that integrates computational modeling, targeted experimentation, and in-service inspection considerations to demonstrate component performance and reliability under representative reactor conditions. The analysis identifies Sodium-cooled Fast Reactor (SFR) and High-Temperature Gas-cooled Reactor (HTGR) systems as reference configurations in terms of temperature, pressure, and chemical environment. Within these operating envelopes, dominant degradation mechanisms— including creep–fatigue interaction, flow-induced vibration, corrosion, and diffusion-bond deterioration—were evaluated to define test requirements. A comprehensive computationalexperimental framework is proposed to support life prediction and qualification activities. The framework couples high-fidelity structural-mechanics, thermal-hydraulic, and fluid-structure interaction models with accelerated degradation testing to produce a traceable linkage between microstructural evolution, mechanical performance, and remaining useful life (RUL). The approach adheres to established Verification, Validation, and Uncertainty Quantification (VVUQ) standards (ASME V&V 10/20; NUREG-2152) and incorporates a digital-twin architecture for continuous model refinement through data assimilation. The plan further outlines testing methodologies, including pre-test analyses, test-loop design parameters, and sensor placement strategies that maximize information yield while maintaining mechanistic fidelity. Complementary sections describe in-service inspection (ISI), on-line monitoring (OLM), and structural-health-monitoring (SHM) techniques applicable to compact HX geometries typical of advanced reactors. Collectively, these activities establish the technical foundation for demonstrating 40-60-year equivalent service life of advanced heat exchangers in support of the U.S. Department of Energy’s Advanced Reactor and Integrated Energy Systems programs. The forthcoming phase will execute the defined pre-test analyses, initiate hardware fabrication, and implement the integrated testing campaign to validate the proposed qualification methodology.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

NASA NTRS1981

Investigation of test methods, material properties, and processes for solar cell encapsulants

Encapsulant materials and processes for the production of cost-effective, long-life solar cell modules were investigated. The following areas were explored: (1) soil resistant surface treatment; (2) corrosion protecting coatings from mild steel substrates; (3) primers for bonding module interfaces; and (4) RS/4 accelerated aging of candidate encapsulation compounds

Willis, P. B.↗

DOE OSTI2021

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

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

36 MATERIALS SCIENCE↗

DOE OSTI2023

Development of an accelerator-based neutron source to prototype Mo-99 production, part I: A liquid LBE windowless target

In this article, Molybdenum-99 (Mo-99)’s decay product, technetium-99 (Tc-99 m), is one of the most critical isotopes for medical diagnostics. To provide U.S. domestic supply of Mo-99 without using high-enriched uranium (HEU), a subcritical uranium target assembly (UTA) is irradiated by an accelerator-based neutron source to create Mo-99 through fission. This study discusses the development of the accelerator-based neutron source. The high-energy electrons from the accelerator irradiate a liquid lead-bismuth eutectic (LBE) target to produce neutrons. Part I of this work focuses on numerical and experimental analysis towards the development of a liquid LBE windowless target. Unlike the existing windowless targets in literature, the current design creates a vertical free surface for a beam to irradiate. First, a hydrodynamic analysis of the LBE windowless target is performed. Simplified analytical calculations are assisted by 2D computational fluid dynamics (CFD) simulations to design the target, with the focus on eliminating recirculation zones and avoiding cavitation. With the optimized geometry, the experimental study is performed to investigate the flow hydrodynamics using liquid LBE. The experiments (1) compare pressure drop in the system to correlation predictions; (2) visualize the free surface liquid LBE flow from the beam view; (3) validate the LBE flow profile using temperature sensitive paint from the side view; and (4) validate the liquid LBE film thickness using gamma densitometer measurements. Second, the power handling capability of the designed windowless target is investigated. The divider plate in the current design is susceptible to overheating due to the thin LBE film in front. As LBE erosion and corrosion is likely to occur at an LBE velocity of 2.0 m/s and temperature above 500 °C, a power limit of 10 kW of beam power was established to prevent this corrosion from occurring, which is calculated by a Nusselt number correlation. The divider plate surface temperature at 10 kW agrees well with the 3D CFD simulation results. Part I demonstrates the fundamental physics in liquid LBE windowless target design and associated testing. A companion paper, Part II will demonstrate how to couple this windowless target into the Mo-99 production system, including an accelerator system operating under an ultra-high vacuum and the UTA cooled by water at room temperature.

43 PARTICLE ACCELERATORS↗

NASA NTRS2013

Closeout Report for the Refractory Metal Accelerated Heat Pipe Life Test Activity

With the selection of a gas-cooled reactor, this heat pipe accelerated life test activity was closed out and its resources redirected. The scope of this project was to establish the long-term aging effects on Mo-44.5%Re sodium heat pipes when subjected to space reactor temperature and mass fluences. To date, investigators have demonstrated heat pipe life tests of alkali metal systems up to .50,000 hours. Unfortunately, resources have not been available to examine the effect of temperature, mass fluence, or impurity level on corrosion or to conduct post-test forensic examination of heat pipes. The key objective of this effort was to establish a cost/time effective method to systematically test alkali metal heat pipes with both practical and theoretical benefits. During execution of the project, a heat pipe design was established, a majority of the laboratory test equipment systems specified, and operating and test procedures developed. Procurements for the heat pipe units and all major test components were underway at the time the stop work order was issued. An extremely important outcome was the successful fabrication of an annular wick from Mo-5%Re screen (the single, most difficult component to manufacture) using a hot isostatic pressing technique. This Technical Publication (TP) includes specifics regarding the heat pipe calorimeter water-cooling system, vendor design for the radio frequency heating system, possible alternative calorimeter designs, and progress on the vanadium equilibration technique. The methods provided in this TP and preceding project documentation would serve as a good starting point to rapidly implement an accelerated life test. Relevant test data can become available within months, not years, and destructive examination of the first life test heat pipe might begin within 6 months of test initiation. Final conclusions could be drawn in less than a quarter of the mission duration for a long-lived, fission-powered, deep space probe.

Martin, J.↗