Results for “Failure mechanisms” — Page 12

DOE OSTI2023

ANS MiNES 2023 Poster

The dynamic mechanical properties of four varieties of high purity graphite as well as the depth of penetration (DoP) of a small-scale shaped charge into these grades was experimentally determined. The grades chosen were PCEA, NBG-18, and NBG-25. These grades provide a wide range of physical properties: in density from 1.80 – 1.85 g/cc, in maximum particle size from 10s to 1000s of µm, and in porosity from 18% to 20%. The quasistatic and dynamic compressive strengths of each grade were determined and correlated to their physical properties. The split Hopkinson pressure bar experiments showed both the dynamic strength and dominant shear failure mechanisms. A small scale shaped charge was used to compare the resistance of graphite to hypervelocity jet impacts: the Teledyne RP-4. The RP-4 has a 1.01” outer diameter and 3.44 g of RDX with an RP-80 booster (86 mg PETN + 123 mg RDX). A select number of samples were analyzed using X-Ray Computed Tomography (XCT), allowing for the full characterization of the undisturbed wound channel. A selection of other samples were physically sectioned and wound channels mapped from the sections. In addition to DoP, the wound geometry was characterized in terms of total volume and diameter at different depths. The wound channel characteristics for each grade were correlated to the compressive strengths and physical properties. In several of the test samples, the wound channel diameter was smaller than the diameter of the shaped charge slug just behind where the slug had penetrated the sample. These results indicated that the wound geometry was dependent on the compressive hysteresis behavior of graphite.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Electrolyte and Cutoff Potential Effects on Cycle Life of Li4Ti5O12/LiNi0.9Mn0.1O2 Batteries for Behind-the-Meter Storage Applications

Behind-the-Meter Storage (BTMS) is a stationary battery energy storage system that is connected to the electrical distribution system on the customer's side of the utility's service meter. BTMS systems are used to store electrical energy from the grid as well as inconstant, renewable energy, such as local solar and wind generation. A successful BTMS system will allow the customer to pair their energy generation and storage to optimize electrical consumption from the grid, improving reliability and minimizing cost. For BTMS applications, batteries must be designed and optimized with different set of criteria from other leading segments of the Li-ion battery market, like transportation, due the system being stationary and proximal to the residential or commercial building it's benefitting. BTMS applications prioritize safety, cost (low/no-critical materials), reliability (20-year calendar life), and durability (10,000 cycle life), while having the ability to (minimally) compromise energy density and rate capability. Lithium titanate (Li4Ti5O12-, LTO) is a promising anode candidate for BTMS applications due to its high safety and capacity retention, while maintaining a reasonable 160 mAhg-1 reversable capacity and composition of relatively abundant materials. (1) Specifically, LTO has a high working voltage which helps to prevent Li dendrite formation, improving safety. Furthermore, LTO also has negligible lithiation-based volume change, leading to less mechanical pulverization, or loss of active material, upon cycling. For the cathode, materials with little or no Co are of high interest due to the high cost and low abundance of Co. LiMn2O4 (LMO) has been paired with LTO for BTMS applications in the past due to its safety, low cost (abundancy), and reasonably high operating voltage. (2-4) However, the low capacity of LMO limits energy density and specific energy. While not the highest priority for BTMS applications, increasing energy density will enable deployment in space constrained BTMS applications and decrease total cost. LiNi0.9Mn0.1O2 (LN-MO) is a recently developed material with promise due to its high operating voltage and relatively low price. (5) However, Ni-rich layered oxides, including LNMO, tend to struggle with capacity retention during high-voltage cycling due to mechanical pulverization, irreversible phase transitions, and unstable solid-electrolyte interphase. The study presented here focuses on building an understanding of how electrolyte solvent and varied cutoff potentials will impact the cycle life of LTO/LN-MO cells. Specifically, a comparison is provided between ethylene carbonate (EC), ethyl methyl carbonate (EMC), fluoroethylene carbonate (FEC), and Gen2 electrolyte solvents with 1M Lithium hexafluorophosphate (LiPF6) salt, cycling to two upper termination potentials, 2.6V and 2.7V. Electrochemical testing and diagnostics (e.g., differential capacity analysis, area specific impedance, constant voltage hold, and rate capability) and post-mortem characterization will be used to understand the aging behavior and failure mechanisms of the 8 cell combinations (four electrolytes and two voltage cutoffs). Cells with FEC electrolyte showed a lower initial capacity compared to cells with Gen2, EMC, and EC cycling at both voltages; however, the cells with FEC showed consistent trends in capacity retention with 2.6V and 2.7V termination potentials, while the cells with the other electrolytes showed much higher rates of capacity loss when cycling to the higher voltage. These results indicate that FEC may play a role in improving durability of high-voltage, Ni-rich electrode systems for use in high-cycle applications, such as BTMS.

electrolyte↗

DOE OSTI2023

Understanding the limits of Li-NMC811 half-cells

As we push the boundaries of state-of-the-art lithium-ion intercalation materials, such as nickel-rich chemistries, the ability to isolate and understand specific degradation and performance limitations is becoming increasingly important. Half-cells, wherein lithium metal is employed as a dual counter and reference electrode, are commonly used in industry and academia for this purpose. However, the high reactivity of lithium metal drives premature electrolyte degradation and limits cell lifetime, bringing into question the reliability and validity of this cell configuration. Here we explore the limitations of half-cell studies of LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC811) electrodes with commercially relevant loading. We identify the failure mechanism of this cell configuration through a combination of electrochemical, chemical, and spectroscopic techniques and show that the Li has a direct detrimental impact on the NMC811 chemistry. Our measurements show that vinylene carbonate is critical for these half-cell studies and underpins the cycle limits. Furthermore, we demonstrate the use of Li 4 Ti 5 O 12 (LTO) as an alternative counter electrode for understanding the performance of NMC positive electrode materials, due to its high coulombic efficiency and low reactivity with the organic carbonates routinely employed in lithium-ion battery cell chemistries. These data confirm that NMC811 electrodes can tolerate high voltages (stressed) conditions and that cell failure is mainly a result of crossover effects.

25 ENERGY STORAGE↗

DOE OSTI2021

Temperature and radiation effects on brittle versus ductile fracture behavior in miscible phase boundaries: insight from atomistic simulations

Temperature- and irradiation-assisted failure mechanisms in miscible phase boundaries are clarified via atomistic calculations. We first establish the temperature-dependent brittle-to-ductile transition in U–Zr miscible phase boundaries. Our results confirm that these boundaries are mostly brittle at low temperatures and ductile at elevated temperatures. We then investigate the changes induced by irradiation on the fracture mechanisms in such phase boundaries. The irradiation-induced defect accumulation follows a multi-stage process that starts with the accumulation of isolated small dislocation loops before transitioning to the saturation and growth of larger dislocation loops and end up with a reorganization into forest dislocations. The accumulation of loops is the primary feature to participate in the delineation between brittle and ductile interfacial fracture in irradiated phase boundaries. At low damage levels, radiation defect interactions with the crack tip are limited and U–Zr miscible boundaries fail through the emission of dislocations ahead of the crack tip followed by brittle cleavage in agreement with the classical Griffith’s criterion for crack stability. At higher damage levels, the failure mode transitions from brittle crack growth to ductile void growth. In this case, the microcrack tip is blunted by the high density of pre-existing, radiation-induced defects in the vicinity of the crack. This interaction leads to the development and growth of a cavity at the interface as opposed to interfacial cleavage.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Qualitative and quantitative analysis of neutron irradiation effects in SiC/SiC composites using X-ray computed tomography

Silicon carbide fiber-reinforced silicon carbide matrix (SiC/SiC) composites are candidate materials for cladding of light water reactor (LWR) fuels. Loss of fission product gas retention due to the formation of microcrack networks is considered a potential failure mechanism for SiC/SiC-cladded fuels. In this work, a variety of SiC/SiC composite tubes were irradiated with and without an LWR-relevant radial heat flux in the High Flux Isotope Reactor, followed by detailed characterization with X-ray computed tomography (XCT). This first set of XCT data for neutron-irradiated samples confirmed that the internal stresses arising from a combination of temperature gradients and irradiation-induced swelling act as the primary driver for cracking. Consequently, while the observed cracking patterns varied depending on the tube architectures, the sharp edges of relatively large pores were found to be the common stress concentrator. These findings are useful to help improve the design and manufacturing of SiC/SiC fuel claddings for reduced failure probability.

42 ENGINEERING↗

DOE OSTI2021

Redefining Resource Adequacy for Modern Power Systems: A Report of the Redefining Resource Adequacy Task Force

Today's rapidly increasing levels of wind, solar, storage, and load flexibility require the industry to rethink reliability planning and resource adequacy methods for modern power systems. Periods with a risk of shortfall often no longer coincide with peak demand - reliability risks are less about peak load and more about the daily setting of the sun, extended cloud cover, wind speeds, cold snaps, and heat waves. In addition, demand is increasingly flexible. Key resources are time-sensitive, as batteries need time to recharge and electricity customers can only be asked to provide demand response for just so long. And reliability failures are often correlated - with one another and with the weather. Two driving factors require the industry to reconsider its analytical approach for resource adequacy: (1) Chronological grid operations: The increasing importance of variable renewable resources (such as wind and solar) and of energy-limited resources (storage and demand response) make it essential to understand the full year of chronological operation of the grid. Specific attention must be paid to hourly, seasonal, and inter-annual resource variability. The sequence of the variability is key, as energy-limited resources such as batteries or demand response require either a preceding period or subsequent period of high production to be useful for grid reliability. (2) Correlated events: Historically, resource adequacy analysis focused on shortfalls caused by random, discrete mechanical failures of large generating units. In contrast, shortfalls today are often caused by multiple, correlated events caused by common weather patterns. Resource adequacy analysis must increasingly shift its focus to these correlated events. The redesign of resource adequacy methods will benefit from a set of guiding principles to better allow for sharing of insights and best practices, interregional resource coordination, and a smoother regulatory process for resource procurement. The objective of this report is to move this redesign forward. It provides an overview of key drivers changing the way resource adequacy needs to be evaluated, identifies shortcomings of conventional approaches, and outlines first principles for practitioners to consider as they adapt their approaches. The central message is: what got us here won't get us there.

24 POWER TRANSMISSION AND DISTRIBUTION↗

DOE OSTI2023

Advanced Monitoring and Control in the ANL METL Facility Using an Engineering Digital Twin

The potential benefits of using an engineering digital twin to achieve greater autonomy for monitoring and control functions in advanced reactors was investigated for the Mechanisms Engineering Test Loop (METL) liquid sodium facility at Argonne National Laboratory. The METL sodium purification system served as a representative system as it requires significant human in-the-loop interaction to accomplish its design function. The objective was to demonstrate how real-time operation could be automated while preserving oversight of the operator for ensuring that the system design functions are met. A digital twin model of the purification system was developed for both the cold trap purification loop and plugging meter diagnostic loop using information from the METL piping and instrumentation diagram (P&ID). Automated monitoring and diagnosis of component degradation in the METL facility was demonstrated in tests using the PRO-AID health monitoring software with the digital twin model incorporated in the library of components. Component failures were introduced and were successfully diagnosed in real time. These tests serve to demonstrate an advanced monitoring capability able to differentiate sensor degradation from component degradation, to generate a rank ordering of probabilities of different failure mechanisms that serves to circumvent the false alarm problem with current anomaly detection methods, and how facility monitoring can be transformed from anomaly detection to identification of a specific fault. Automated control of the purification system was demonstrated through simulations that exercised a model predictive controller designed using the digital twin model. Results of these simulations compared favorably with experimental data showing very good reference tracking response with negligible overshoot. In conclusion, these pilot tests and simulations successfully demonstrated the use of a digital twin for improved automation of monitoring and control. It was shown how the digital twin enables switching between control modes from cold trap operation where impurities are removed to plugging meter operation where impurity concentrations are measured.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2026

Chemo-Mechanics of α-V 2 O 5 During Lithiation and Implications for Rechargeable Battery Cathodes

Chemo-mechanical degradation of layered oxide electrodes is strongly influenced by crystallographic anisotropy, local stress evolution, and ion insertion, yet the intrinsic mechanical response of layered materials remains incompletely understood. Indeed, most prior studies have focused on polycrystalline materials but single crystals enable direct observation of coupling between anisotropic ion diffusion and mechanical response. This study aims to determine how crystallographic anisotropy and lithiation affect deformation, fracture, and mechanical properties in single-crystal V 2 O 5 , and compares this behavior with polycrystalline counterparts. Polycrystalline V 2 O 5 thin films and single-crystal α-V 2 O 5 were studied using nanoindentation, scanning electron microscopy, focused ion beam cross-sectioning, and Raman spectroscopy. Single crystals were tested in pristine and chemically lithiated states, including experiments in which crystals were first plastically deformed via nanoindentation and subsequently lithiated. Polycrystalline films exhibited significantly higher hardness and elastic modulus than single crystals. Single crystals indented normal to the exposed (001) basal plane exhibited pronounced anisotropic deformation, including directional slip, crystallographically-guided cracking, anisotropic crack propagation, interlayer separation, and shear localization. Lithiation caused substantial softening, reduced hardness and modulus, and suppressed displacement bursts during nanoindentation, while previously indented regions showed crack formation and growth upon lithiation. Mechanical behavior of α-V 2 O 5 is strongly governed by crystallographic anisotropy and further altered by lithiation, with pre-existing deformation serving as a strong driver of fracture during ion insertion. These findings illuminate the coupling among ion insertion, deformation, and fracture in layered oxides and provide a basis for understanding and mitigating mechanical failure in electrochemical energy-storage materials.

Anisotropy↗

DOE OSTI2025

Destructive PIE and Safety Testing of Six AGR-5/6/7 Capsule 2 Compacts

This study evaluates fission product retention and particle failure mechanisms in AGR-5/6/7 Capsule 2 uranium carbide and uranium oxide (UCO) tristructural isotropic (TRISO) fuel under high-temperature gas reactor accident-relevant conditions using high-temperature safety tests and destructive post-irradiation examination. Three Capsule 2 compacts were held isothermally at 1600°C for approximately 300 hours and one compact at 1800°C for approximately 300 hours; two additional compacts were examined in the as-irradiated state. Post-test deconsolidation–leach–burn–leach (DLBL) quantified nuclide inventories in matrix and particles. Individual particles were surveyed for radioisotope inventories, and microanalytical approaches resolved microstructural evolution and fission product distributions within the coating layers. At 1600°C, no krypton was detected above the minimum detectable limit, and cesium releases were far below a single particle equivalent, indicating the absence of full TRISO failure or SiC failures. Silver releases were limited and primarily reflected depleted post-irradiation inventories, consistent with prior compact-level exams indicating substantial in-pile 110m Ag loss. At 1800°C, cumulative 134 Cs release of approximately 2.5 particle equivalents and delayed 85 Kr totaling approximately 0.53 particle equivalents were consistent with one full TRISO failure and two SiC failures. Europium and strontium releases were roughly one order of magnitude higher than at 1600°C and comparable to AGR-1/AGR-2 high-temperature tests, with sustained late-hold rates indicating diffusion through intact coatings coupled with matrix depletion. Overall, AGR-5/6/7 Capsule 2 UCO fuel demonstrated fission product retention during safety testing consistent with prior AGR campaigns, while distinctive in-pile 110m Ag depletion and measurable 1600°C europium loss motivate targeted follow-on studies.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2022

Microstructural heterogeneity of the buffer layer of TRISO nuclear fuel particles

Tristructural isotropic (TRISO) nuclear fuel particles contain a layered spherical shell designed to retain fission products; however, failure occurs in rare cases—commonly initiated in the porous pyrocarbon buffer layer. Achieving a comprehensive understanding of the buffer-initiated failure mechanisms requires detailed characterization of the buffer porosity and its heterogeneous distribution across multiple length scales. Here we performed FIB-SEM tomography across the buffer layer thickness (~100 µm) to produce 3D reconstructions of the buffer microstructure with 50 nm spatial resolution. We found an average overall porosity of ~14%, which does not solely account for the low density of the buffer (50% of the theoretical density). Additionally, the local porosity and its fluctuation increase from the kernel interface towards the inner pyrocarbon (IPyC) layer, which we attribute to the chemical vapor deposition process conditions during the TRISO particle fabrication. Detailed characterization of the porous microstructure—including analysis of the pore size, distribution, shape, and orientation—provides insight into the process-structure-property-performance relations of TRISO nuclear fuel particles and will inform multiscale models designed to predict the failure of TRISO particles under irradiation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

Stress relaxation cracking susceptibility evaluation in 347H stainless steel welds

Abstract Stress relaxation cracking (SRC) has been reported as a dominant failure mechanism for 347H stainless steel welds at elevated service temperatures, occurring in either the heat-affected zone (HAZ) or fusion zone (FZ). In this study, SRC susceptibility of physically simulated HAZ and cross-welded E347-347H stainless steel welds was studied using a four-step accelerated SRC test with a thermomechanical physical simulator. The stress and temperature range studied represents weld-induced residual stress at 150–600 MPa and post-weld heat treatment temperatures between 800 and 1050 °C. For all temperature conditions, the cross-welded samples failed at a lower critical stress threshold than the simulated HAZ. A finite element model of a 50.8-mm-thick single-V groove weld was used to generate the residual stress maps induced by a 40-pass welding procedure, which in combination with the experimental threshold stress map predicted potential SRC failure locations. Postmortem microstructural evaluations were performed to identify contributing characteristics to SRC. It was found that HAZ samples exhibited a combination of creep void development, secondary cracks with intergranular fracture near grain boundary carbides, and eutectic phases. FZ samples showed brittle fracture with cracks propagating along straight, non-tortuous interdendritic grain boundaries.

42 ENGINEERING↗

DOE OSTI2020

Heterogeneous solute segregation suppresses strain localization in nanocrystalline Ag-Ni alloys

Solute segregation to individual grain boundaries is used by design to produce strong and stable nanocrystalline metallic alloys. Grain-boundary segregation, however, is known to cause adverse embrittlement effects from a strain-localization failure mechanism that imposes significant material limitations for structural applications. Here, using atomistic simulations, it is discovered that heterogeneous Ni segregation in nanocrystalline Ni-mixed Ag alloys dramatically shuts down localized shear bands during plastic deformation, while simultaneously increasing the tensile strength. Nanocrystalline Cu-mixed Ag metals are predicted to exhibit standard homogeneous Cu segregation and a tensile strength that saturates above a solute concentration of 8 at.% due to glass-like shear localization induced by grain boundaries. By contrast, it is found that heterogeneous Ni segregation in nanocrystalline Ag-Ni alloys forms solute-rich clusters along interfaces leading to strain delocalization at high strain and continuous strengthening at high solute concentrations up to 15 at.%. As a result, this study reveals the importance of heterogeneous versus homogeneous segregation behaviors on strain localization and points to a fundamentally new strategy to design failure-resistant nanostructured materials through grain boundary segregation engineering.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Direct Imaging of the Structural and Morphological Evolution of Epitaxial LiCoO 2 Films during Charge and Overcharge

The capacity decay of layered cathodes in high-voltage applications underscores the need to utilize accurate and precise techniques to understand the underlying mechanisms. Here, we use well-defined epitaxial LiCoO 2 (LCO) films on SrRuO 3 /SrTiO 3 (SRO/STO) with controlled orientations and defect structures along with in situ electrochemical atomic force microscopy to probe the structural and morphological evolutions during the charge and overcharge processes. We quantitatively show the morphological changes in both the reversible delithiation regime and the irreversible over-delithiation regime and correlate the overall electrochemical behaviors to atomic scale defect evolutions in the films. Further, we also observe a significantly lower charging capacity for LCO/SRO/STO(111) compared to that of LCO/SRO/STO(001) films of the same thickness, which is ascribed to different types of atomic scale defects formed during the film growth process. Our high- resolution scanning transmission electron microscopy (STEM) and electron energy loss spectroscopy (EELS) studies reveal that the antiphase boundaries in LCO/SRO/STO(111) act as viable channels for Li migration but are more susceptible to irreversible phase transitions, which then block subsequent Li diffusion. The failure mechanisms developed here may provide insight into the design of future cathode materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Thermal Runaway of Li-Ion Cells: How Internal Dynamics, Mass Ejection, and Heat Vary with Cell Geometry and Abuse Type

Thermal runaway of lithium-ion batteries can involve various types of failure mechanisms each with their own unique characteristics. Using fractional thermal runaway calorimetry and high-speed radiography, the response of three different geometries of cylindrical cell (18650, 21700, and D-cell) to different abuse mechanisms (thermal, internal short circuiting, and nail penetration) are quantified and statistically examined. Correlations between the geometry of cells and their thermal behavior are identified, such as increasing heat output per amp-hour (kJ Ah −1 ) of cells with increasing cell diameter during nail penetration. High-speed radiography reveals that the rate of thermal runaway propagation within cells is generally highest for nail penetration where there is a relative increase in rate of propagation with increasing diameter, compared to thermal or internal short-circuiting abuse. For a given cell model tested under the same conditions, a distribution of heat output is observed with a trend of increasing heat output with increased mass ejection. Finally, internal temperature measurements using thermocouples embedded in the penetrating nail are shown to be unreliable thus demonstrating the need for care when using thermocouples where the temperature is rapidly changing. All data used in this manuscript are open access through the NREL and NASA Battery Failure Databank.

25 ENERGY STORAGE↗

DOE OSTI2025

Chemical Interaction of Palladium in Uranium Oxycarbide Nuclear Fuel Kernel

Chemical Interaction of Palladium in Uranium Oxycarbide Nuclear Fuel Kernel Jana Howard1,3, Guang Yang3, Haiyan Zhao1*, Patrick Warren4, Tiankai Yao3, Steven Cavazos4 Elizabeth Sooby Wood4*, Ching-heng Shiau2 1 University of Idaho, Environmental Science, Idaho Falls, Idaho, USA 2 Boise State University, Microscopy and Characterization Suite, Idaho Falls, Idaho, USA 3 Idaho National Laboratory, Idaho Falls, Idaho, USA 4 University of Texas San Antonio, Department of Physics and Astronomy, San Antonio, Texas, USA *Corresponding author: haiyanz@uidaho.edu; elizabeth.soobywood@utsa.edu Tri-structural Isotropic (TRISO) particle fuel is the preferred choice for the newest and next-generation high-temperature nuclear reactors due to its robust construction [1]. The fuel design effectively contains fission products inside the particle at extremely high temperatures [2]. However, the effect of transition metal fission products on fuel performance and structural integrity remains largely unknown, creating uncertainties in predicting fuel performance and potential failure mechanisms [2]. For example, palladium (Pd) has a strong tendency to form intermetallic phases with uranium (U). These new phases tend to be hard and brittle which could lead to fracture of fuel kernel during irradiation [3,4]. Pd is not normally produced in high concentrations in normal fission reactions however, driving the production of Pd into the locality of a Uranium Oxycarbide (UCO) nuclear fuel provides an opportunity to closely observe the diffusion and chemical interactions. This study focuses on detailed transmission electron microscopy characterization of the intermetallic phases formed by the interaction between a UCO kernel and a Pd bar after annealing at 1100 °C for 100 hours. Figure 1 provides an overview of the UCO kernel in contact with the Pd bar. The UCO-Pd sample surface was examined using a Focused Ion Beam (FIB) Quanta 3D FEG FEI in VCD detector mode at 10kV, 83pA to reveal surface features. Several key surface features in the interaction region were observed including: (1) a small area with dendritic microstructure, (2) color contrast near the UCO kernel and Pd boundary, and (3) darker and lighter regions throughout the sample surface. To analyze diffusion behavior, FIB was used to prepare lamellae from five different areas of the UCO-Pd sample, as well as one for the as-received sample. These lamellae were examined using a Scanning Transmission Electron Microscope ThermoFisher Spectra 300 (STEM-Spectra). Energy Dispersive Spectroscopy results confirmed the diffusion between the UCO fuel and Pd bar. Figure 2 shows the identified phases of UC, UO2, and Pd dispersed throughout the interaction region. It was also found that the Pd concentration decreases as the radial distance from the UCO-Pd interface increases. The Pd concentration was 36.93% atomic fraction 11µm from the interaction region then decreased to 7.51% atomic fraction at 257 µm away from the interaction region. Figure 3 shows how concentrations of U and Pd vary across the interaction zone, highlighting the extent of diffusion. This study confirms that Pd interacts with surrounding material to form U-Pd phase and diffusion zones. These diffusion zones vary in composition depending on its radial distance from the point of contact with the Pd bar. These findings contribute to a deeper understanding of the fission product behavior in high temperature nuclear fuels, aiding in the prediction and mitigation of potential fuel degradation mechanisms. A B C Fig. 1. SEM micrographs of UCO fuel kernel in contact with solid Pd bar and the lift out locations. Figure 1A shows UCO fuel kernel in contact with solid Pd bar. Figure 1B shows a higher magnification image of the UCO fuel-Pd interaction zone. Figure 1C shows lift out sites for the lamellae. A B C Fig 2. EDS maps reveal the distribution of U, O, and Pd in location 3. Figure 2A shows the distribution of uranium. Figure 2B shows the distribution of oxygen. Figure 2C shows the distribution of palladium. A B C Fig 3. Palladium and uranium concentration across interaction zone in location 2. Figure 3A shows EDS map of lift out number 2. Figure 3B shows a zoomed in EDS map taken from the interaction zone. Figure 3C shows a line graph of uranium and palladium concentrations across the interaction zone. References: 1. B.E. Wells, N.R. Phillips, K.J. Geelhood. Pacific West Laboratory. (2021). TRISO Fuel: Properties and Failure Modes. https://www.nrc.gov/docs/ML2117/ML21175A152.pdf (Accessed January 16, 2025). 2. American Nuclear Society. TRISO Fuel Development Progresses in INL, ORNL. https://www.gen-4.org/gif/upload/docs/application/pdf/2014-03/nov13nn_fuel_reprint.pdf (Accessed January 16, 2025) 3. Clark R.A., M.A. Con

36 - MATERIALS SCIENCE↗

DOE OSTI2025

Chemical Interaction of Palladium in Uranium Oxycarbide Nuclear Fuel Kernel

Chemical Interaction of Palladium in Uranium Oxycarbide Nuclear Fuel Kernel Jana Howard1,3, Guang Yang3, Haiyan Zhao1*, Patrick Warren4, Tiankai Yao3, Steven Cavazos4 Elizabeth Sooby Wood4*, Ching-heng Shiau2 1 University of Idaho, Environmental Science, Idaho Falls, Idaho, USA 2 Boise State University, Microscopy and Characterization Suite, Idaho Falls, Idaho, USA 3 Idaho National Laboratory, Idaho Falls, Idaho, USA 4 University of Texas San Antonio, Department of Physics and Astronomy, San Antonio, Texas, USA *Corresponding author: haiyanz@uidaho.edu; elizabeth.soobywood@utsa.edu Tri-structural Isotropic (TRISO) particle fuel is the preferred choice for the newest and next-generation high-temperature nuclear reactors due to its robust construction [1]. The fuel design effectively contains fission products inside the particle at extremely high temperatures [2]. However, the effect of transition metal fission products on fuel performance and structural integrity remains largely unknown, creating uncertainties in predicting fuel performance and potential failure mechanisms [2]. For example, palladium (Pd) has a strong tendency to form intermetallic phases with uranium (U). These new phases tend to be hard and brittle which could lead to fracture of fuel kernel during irradiation [3,4]. Pd is not normally produced in high concentrations in normal fission reactions however, driving the production of Pd into the locality of a Uranium Oxycarbide (UCO) nuclear fuel provides an opportunity to closely observe the diffusion and chemical interactions. This study focuses on detailed transmission electron microscopy characterization of the intermetallic phases formed by the interaction between a UCO kernel and a Pd bar after annealing at 1100 °C for 100 hours. Figure 1 provides an overview of the UCO kernel in contact with the Pd bar. The UCO-Pd sample surface was examined using a Focused Ion Beam (FIB) Quanta 3D FEG FEI in VCD detector mode at 10kV, 83pA to reveal surface features. Several key surface features in the interaction region were observed including: (1) a small area with dendritic microstructure, (2) color contrast near the UCO kernel and Pd boundary, and (3) darker and lighter regions throughout the sample surface. To analyze diffusion behavior, FIB was used to prepare lamellae from five different areas of the UCO-Pd sample, as well as one for the as-received sample. These lamellae were examined using a Scanning Transmission Electron Microscope ThermoFisher Spectra 300 (STEM-Spectra). Energy Dispersive Spectroscopy results confirmed the diffusion between the UCO fuel and Pd bar. Figure 2 shows the identified phases of UC, UO2, and Pd dispersed throughout the interaction region. It was also found that the Pd concentration decreases as the radial distance from the UCO-Pd interface increases. The Pd concentration was 36.93% atomic fraction 11µm from the interaction region then decreased to 7.51% atomic fraction at 257 µm away from the interaction region. Figure 3 shows how concentrations of U and Pd vary across the interaction zone, highlighting the extent of diffusion. This study confirms that Pd interacts with surrounding material to form U-Pd phase and diffusion zones. These diffusion zones vary in composition depending on its radial distance from the point of contact with the Pd bar. These findings contribute to a deeper understanding of the fission product behavior in high temperature nuclear fuels, aiding in the prediction and mitigation of potential fuel degradation mechanisms. A B C Fig. 1. SEM micrographs of UCO fuel kernel in contact with solid Pd bar and the lift out locations. Figure 1A shows UCO fuel kernel in contact with solid Pd bar. Figure 1B shows a higher magnification image of the UCO fuel-Pd interaction zone. Figure 1C shows lift out sites for the lamellae. A B C Fig 2. EDS maps reveal the distribution of U, O, and Pd in location 3. Figure 2A shows the distribution of uranium. Figure 2B shows the distribution of oxygen. Figure 2C shows the distribution of palladium. A B C Fig 3. Palladium and uranium concentration across interaction zone in location 2. Figure 3A shows EDS map of lift out number 2. Figure 3B shows a zoomed in EDS map taken from the interaction zone. Figure 3C shows a line graph of uranium and palladium concentrations across the interaction zone. References: 1. B.E. Wells, N.R. Phillips, K.J. Geelhood. Pacific West Laboratory. (2021). TRISO Fuel: Properties and Failure Modes. https://www.nrc.gov/docs/ML2117/ML21175A152.pdf (Accessed January 16, 2025). 2. American Nuclear Society. TRISO Fuel Development Progresses in INL, ORNL. https://www.gen-4.org/gif/upload/docs/application/pdf/2014-03/nov13nn_fuel_reprint.pdf (Accessed January 16, 2025) 3. Clark R.A., M.A. Con

36 - MATERIALS SCIENCE↗

DOE OSTI2023

Interfacial microstructure and mechanical properties of rotary inertia friction welded dissimilar 422 martensitic stainless steel to 4140 low alloy steel joints

In this work, dissimilar rotary inertia friction welds between 422 martensitic stainless steel and 4140 martensitic low-alloy steel were made to fabricate prototype heavy-duty diesel engine pistons. The influence of the inertia friction welding process and post weld heat treatment (PWHT) temperature on the interfacial microstructure evolutions and corresponding effects on mechanical properties of the 422/4140 welds were evaluated in detail. Carbon diffused from the 4140 side to the 422 side during PWHT at 650 °C for 1.5 h, causing the formation of a hard carbide-rich layer on the 422 side, and a softer but discontinuous C-depleted layer the 4140 side. PWHT at 700 °C for 1.5 h greatly accelerated C diffusion across the interface relative to 650 °C, resulting in a thicker hard carbide-rich layer and a relatively thick and continuous layer of coarse C-depleted grains (ferrite) on the 4140 side. In addition, the PWHT temperature greatly influenced the tensile properties and fracture behavior of the welds, with the 650 °C PWHT-ed samples failing predominately in a ductile manner in the 4140 heat affected zone during tensile testing. Conversely, the 700 °C PWHT specimens exhibited a strength reduction compared with the 650 °C PWHT specimens because of additional coarsening of the interfacial ferrite layer and softening of the base materials during PWHT, with brittle fracture between the hard and soft layers the predominate failure mechanism. Based on the findings, a reduced PWHT temperature and/or time, minimizing the hardness differential of the base metals, and pre-heating the 422 steel prior to welding are the potential pathways to achieve a more optimal balance between desirable tempering and stress relief of the weld microstructure and undesirable C migration across the weld interface, and to reduce the strength mismatch across the weld.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Reliability Assessment of Cooling Fans for PV Inverters: Testing, Modeling, and Case Studies

The reliability of photovoltaic (PV) inverters is critical for long-term solar system performance, with cooling fan failures frequently leading to costly downtime. While much research exists on general cooling fan reliability, little attention has been given to fans operating within PV inverters and their unique environmental challenges. Here, this article proposes a comprehensive methodology to address this gap. First, a failure mode and effects analysis is performed on fans to identify the key failure mechanisms in PV applications, their corresponding stressors, and the models necessary for lifetime prediction. Second, an accelerated life test is designed and conducted to collect valuable experimental data for PV inverter fans in a reasonable amount of time. Third, a mathematical conversion of dynamic mission profiles into effective constant stress levels is derived. Fourth, case studies are given, showcasing lifetime estimates that account for geographic variations in mission profile data. The results demonstrate that this integrated approach leads to an accurate reliability assessment for PV inverter cooling fans.

accelerated life testing (ALT)↗