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At least 1,009 records · Page 56

Understanding Formation of Irradiation-Induced Defects through 4D-STEM, Electron Tomography, and WBDF-STEM

A major challenge in advancing nuclear materials for next-generation fission and proposed fusion reactors is to comprehensively understand the formation of irradiation-induced defects. Here it is essential to correlate the evolution of irradiation-induced defects and the degradation of mechanical properties, as they collectively dictate the material's lifespan and ensure nuclear safety. Scanning transmission electron microscopy (STEM) based techniques have emerged as indispensable tools for irradiation-induced defect characterization, offering high spatial resolution imaging and chemical analysis, such as electron energy loss spectroscopy (EELS) and energy dispersive X-ray spectroscopy (EDXS). These techniques have been effectively used to obtain an atomic-scale view of the defect structure. Recent advances in electron microscopy, particularly in 4D-STEM, offer detailed insight into microstructural evolution by capturing full 2D diffraction patterns at every pixel position. Using high-speed direct electron detectors, this technology generates a four-dimensional dataset, overcoming the limitations of traditional STEM imaging.

36 MATERIALS SCIENCE↗

Understanding Oxide–Metal Interactions During Hot Isostatic Pressing to Diffusion Bond Aluminum Alloy 6061 Plates

The interaction between Mg, Si, and Al 2 O 3 during hot isostatic pressing diffusion bonding of aluminum alloy 6061 (AA6061) plates was investigated through thermodynamic calculations and experimental microstructural characterization. Thermodynamic calculations as functions of temperature, pressure, and composition revealed that the interaction among Mg, Si, and Al 2 O 3 yields Mg 2 Si and either MgO + Al or MgAl 2 O 4 + Al, facilitating the reduction of Al 2 O 3 and allowing Al/Al metallic bonds to form. Total pressure variation had a negligible influence on the oxygen partial pressure, and consequently, the reaction product formation. Oxygen partial pressure variation as a function of temperature and initial amount of Al 2 O 3 determined the formation of either MgO or MgAl 2 O 4 . Experimental Hot Isostatic Pressure (HIP) bonding at 723 K and 833 K under a constant pressure of 1017 atm documented the cooling rate-dependent formation of β–Mg 2 Si precipitates. High-resolution transmission electron microscopy imaging and selected area electron diffraction patterns verified the formation of β–Mg 2 Si and MgO at the interface but did not detect MgAl 2 O 4 . In conclusion, findings from this study clarify the role of thermochemical interactions in oxide disruption and bonding mechanisms during HIP diffusion bonding of AA6061 and provide guidance for optimizing joining processes for monolithic nuclear fuel assemblies.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Establishment of a Vertically Integrated Domestic Manufacturing Process for Production of Substrates Needed for Manufacture of Gas Diffusion Layers

In this project, AvCarb, LLC evaluated the baseline performance metrics of commercial carbon veils and their corresponding Gas Diffusion Layers (GDLs) with the goal of establishing an optimized, vertically integrated production system for wet-laid nonwoven substrates used in gas diffusion media for electrochemical energy storage and conversion devices. Mechanical testing and microstructural characterization were conducted and used to develop a multiscale computational model capable of simulating and predicting the performance of GDLs in fuel cells. Although the project successfully generated foundational transport and modeling data, it was terminated prior to identifying the critical GDL design parameters necessary for full optimization. The program aimed to improve carbon veil fabrication through enhanced fiber dispersion, fiber-fiber adhesion control, and improved web formation, enabling the production of high-quality, uniform substrates. Simulations were intended to guide mixing and solution delivery system design and process conditions, followed by production-scale trials to evaluate fiber dispersion, web uniformity, and mechanical robustness. At full deployment, the proposed production line would have been capable of producing approximately 650,000 m² of carbon veil annually. This capability remains strategically important, as the United States currently lacks a domestic source of wet-laid nonwoven carbon substrates that satisfy the stringent quality requirements for fuel-cell GDLs and electrolyzers representing an ongoing supply-chain vulnerability. Beyond supply-chain benefits, the project established a robust benchmarking dataset for existing commercial carbon veils while advancing next-generation material concepts targeting improved performance and manufacturing consistency.

Olson, Cynthia Lemay↗

Friction Stir Dovetailing of AA7099 to Steel with AA6061 Interlayer for Reduced Zn Embrittlement at Dissimilar Interface

Joining of high strength Al alloy (AA7099) to steel (rolled homogeneous armor) with and without AA6061 interlayer was achieved using a friction stir dovetailing (FSD) method. Detailed investigations were conducted to establish correlations between mechanical performance and microstructural evolution of FSD joints. Lap shear tensile testing revealed that incorporation of the AA6061 interlayer combined with tailored processing methodology significantly improved both mechanical interlocking and load transmission across the dovetail interface. Following incorporation of the interlayer, the maximum load carrying capacity and peak extension (of the AA7099/AA6061/steel joint) are 60% and 210% higher, respectively, than results obtained from an AA7099/steel joint without an interlayer. Without an AA6061 interlayer, formation of zinc rich intermetallic compounds led to brittle interfacial failure of the AA7099-steel FSD joint. Incorporation of novel tool and joint configuration eliminated asymmetric joint performance as a function of loading direction, which is generally observed in friction stir lap welding. The efficacy of the use of an AA6061 interlayer in joining AA7099 to steel was demonstrated through mechanical testing as well as high resolution analytical electron microscopy characterization.

Dissimilar metal joining, Friction stir dovetailin↗

Review on the growth, properties and applications of self-assembled oxide–metal vertically aligned nanocomposite thin films—current and future perspectives

Self-assembled oxide–metal nanocomposite thin films have aroused great research interest owing to their wide range of functionalities, including metamaterials with plasmonic and hyperbolic optical properties, and ferromagnetic, ferroelectric and multiferroic behaviors. Oxide–metal nanocomposites typically self-assemble as metal particles in an oxide matrix or as a vertically aligned nanocomposite (VAN) with metal nanopillars embedded in an oxide matrix. Among them, the VAN architecture is particularly interesting due to the vertical strain control and highly anisotropic structure, enabling the epitaxial growth of materials with large lattice mismatch. In this review, the driving forces behind the formation of self-assembled oxide–metal VAN structures are discussed. Specifically, an updated in-plane strain compensation model based on the areal strain compensation concept has been proposed in this review, inspired by the prior linear strain compensation model. It provides a guideline for material selection for designing VAN systems, especially those involving complex orientation matching relationships. Based on the model, several case studies are discussed, comparing the microstructure and morphology of different oxide–metal nanocomposites by varying the oxide phase. Specific examples highlighting the coupling between the electrical, magnetic and optical properties are also discussed in the context of oxide–metal nanocomposites. Finally, future research directions and needs are also discussed.

36 MATERIALS SCIENCE↗

Effects of cobalt on the microstructure of Udimet 700

Cobalt, a critical and "strategic" alloying element in many superalloys, was systematically substituted by nickel in experimental alloys Udimet 700 containing 0.1, 4.3, 8.6, 12.8 and the standard 17.0 wt.% cobalt. Electrolytic and chemical extraction techniques, X-ray diffraction, scanning electron and optical microscopy were used for the microstructural studies. The total weight fraction of gamma' was not significantly affected by the cobalt content, although a difference in the size and quantities of the primary and secondary gamma' phases was apparent. The lattice parameters of the gamma' were found to increase with increasing cobalt content while the lattice mismatch between the gamma matrix and gamma' phases decreased. Other significant effects of cobalt on the weight fraction, distribution and formation of the carbide and boride phases as well as the relative stability of the experimental alloys during long-time aging are also discussed.

Engel, M. A.↗

Effects of cobalt, boron, and zirconium on the microstructure of Udimet 738

A structural study was carried out on Co modified Udimet 738 alloys containing 0.04, 0.10, and 0.20 wt % Zr at 0.01 and 0.03 wt % B levels. Samples in the as-cast and solution-treated conditions were exposed at 843 C to study structural stability. The structures produced by the interactions of Co, Zr, and B were studied by SEM, X-ray diffraction, and dispersive analysis techniques. The additions of large amounts of Zr and B were found to increase the solidification range of the U-738. Structural changes involved eutectic gamma prime islands, formation of low melting point compounds, and precipitation of borides and Zr rich phases. Boron and zirconium additions did not show substantial changes in mechanical properties. Removal of Co from the alloys resulted in reduction of the matrix solubility for carbon and increase in the gamma prime solvus. Structural instabilities found were continuous grain boundary M23C6 films, MC breakdown, and plate-like phases. Removal of cobalt resulted in a slight decrease in tensile and stress rupture properties. Detailed structural results presented.

Nakanishi, T. G.↗

Application of an Elongated Kelvin Model to Space Shuttle Foams

Spray-on foam insulation is applied to the exterior of the Space Shuttle s External Tank to limit propellant boil-off and to prevent ice formation. The Space Shuttle foams are rigid closed-cell polyurethane foams. The two foams used most extensively on the Space Shuttle External Tank are BX-265 and NCFI24-124. Since the catastrophic loss of the Space Shuttle Columbia, numerous studies have been conducted to mitigate the likelihood and the severity of foam shedding during the Shuttle s ascent to space. Due to the foaming and rising process, the foam microstructures are elongated in the rise direction. As a result, these two foams exhibit a non-isotropic mechanical behavior. In this paper, a detailed microstructural characterization of the two foams is presented. The key features of the foam cells are summarized and the average cell dimensions in the two foams are compared. Experimental studies to measure the room temperature mechanical response of the two foams in the two principal material directions (parallel to the rise and perpendicular to the rise) are also reported. The measured elastic modulus, proportional limit stress, ultimate tensile stress and the Poisson s ratios for the two foams are compared. The generalized elongated Kelvin foam model previously developed by the authors is reviewed and the equations which result from this model are presented. The resulting equations show that the ratio of the elastic modulus in the rise direction to that in the perpendicular-to-rise direction as well as the ratio of the strengths in the two material directions is only a function of the microstructural dimensions. Using the measured microstructural dimensions and the measured stiffness ratio, the foam tensile strength ratio and Poisson s ratios are predicted for both foams. The predicted tensile strength ratio is in close agreement with the measured strength ratios for both BX-265 and NCFI24-124. The comparison between the predicted Poisson s ratios and the measured values is not as favorable.

Sullivan, Roy M.↗

Ionic conductivity optimization of composite polymer electrolytes through filler particle chemical modification

The addition of filler particles to polymer electrolytes is known to increment their ionic conductivity (IC). A detailed understanding of how the interactions between the constituent materials are responsible for the enhancement remains to be developed. A significant contribution is ascribed to an increment of the polymer amorphous fraction, induced by the fillers, resulting in the formation of higher ionic conductivity channels in the polymer matrix. However, the dependence of IC on the particle weight load and its composition on the polymer morphology is not fully understood. This work investigates Li-ion transport in composite polymer electrolytes (CPE) comprising Bi-doped LLZO particles embedded in PEO:LiTFSI matrixes. We find that the IC optimizes for very low particle weight loads (5-10%) and that both its magnitude and the load are required, strongly dependent on the garnet particle composition. Based on structural characterization results and electrochemical impedance spectroscopy, a mechanism is proposed to explain these findings. It is suggested that the Li-molar content in the garnet particle controls its interactions with the polymer matrix, resulting at the optimum loads reported, in the formation of high ionic conductivity channels. We propose that filler particle chemical manipulation of the polymer morphology is a promising avenue for the further development of composite polymer electrolytes.

bismuth↗

Effect of temperature on the formation of creep substructure in sodium chloride single crystals

The effect of temperature on the substructure morphology and the cell and subgrain size was investigated experimentally in NaCl single crystals under creep in the temperature range 573-873 K. It is found that the effect of temperature on the cell and subgrain sizes is weak in comparison with the effect of stress. However, there was a qualitative change in the substructure morphology with temperature, with the cells and subgrains better defined at higher temperatures. The volume fraction of the cell boundaries decreased with increasing temperature, thereby indicating a refinement of the microstructure at higher temperatures.

Raj, Sai V.↗

Characterization of multi-material 316L-Hastelloy X fabricated via laser powder-bed fusion

The aim of this work is to provide firsthand knowledge of 316 L stainless steel (316 L) and Hastelloy X (HX) multi-material processing via laser powder bed fusion (PBF). Specifically, microstructure of the interface is studied using scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), and X-ray diffraction (XRD). Surface metrology is performed to characterize the resulting surface roughness at the interface followed by tensile and flexural testing of multi-material samples to characterize the mechanical properties of the interfaces. Results showed that use of proper process parameters for each individual material led to formation of a compositional gradient at the interface that stretched for 240 μm (10–12 layers) with no evidence of cracking or porosity. The interface exhibited higher surface roughness compared to 316 L or HX as measured by arithmetic mean height, Sa, and maximum valley depth, Sv, parameters. During tensile testing, samples failed in the 316 L region away from the interface, with comparable yield strength, ultimate strength, and ductility. Finally, it was concluded that the “naturally” formed interface created a compositional gradient which was defect free due to similar values of coefficient of thermal expansion, input energy density, and different Marangoni numbers of the materials.

316L stainless Steel↗

A Comparison between Growth Morphology of "Eutectic" Cells/Dendrites and Single-Phase Cells/Dendrites

Directionally solidified (DS) intermetallic and ceramic-based eutectic alloys with an in-situ composite microstructure containing finely distributed, long aspect ratio, fiber, or plate reinforcements are being seriously examined for several advanced aero-propulsion applications. In designing these alloys, additional solutes need to be added to the base eutectic composition in order to improve heir high-temperature strength, and provide for adequate toughness and resistance to environmental degradation. Solute addition, however, promotes instability at the planar liquid-solid interface resulting in the formation of two-phase eutectic "colonies." Because morphology of eutectic colonies is very similar to the single-phase cells and dendrites, the stability analysis of Mullins and Sekerka has been extended to describe their formation. Onset of their formation shows a good agreement with this approach; however, unlike the single-phase cells and dendrites, there is limited examination of their growth speed dependence of spacing, morphology, and spatial distribution. The purpose of this study is to compare the growth speed dependence of the morphology, spacing, and spatial distribution of eutectic cells and dendrites with that for the single-phase cells and dendrites.

Tewari, S. N.↗

Field Testing of High Current Electrokinetic Nanoparticle Treatment for Corrosion Mitigation in Reinforced Concrete

This work examines field performance of nanoscale pozzolan treatments delivered el ctrokinetically to suppress chloride induced corrosion of concrete reinforcement. The particles are 20 nm silica spheres coated with 2 nm alumina particles that carry a net positive charge. Earlier work demonstrated that the alumina particles were stripped from the silica carriers and formed a dense phase with an interparticle spacing that is small enough to inhibit the transport of solvated chlorides. A D.C. field was used to inject the particles into the pores of concrete specimens, directly toward the mild steel bars that were embedded within each 3 inch diameter by 6 inch length concrete specimen. The voltage was held constant at 25 v per inch of concrete cover for a period of 7 days. These voltages permitted current densities as high as 3 A/sq m. During the final 3 days, a 1 molar solution of calcium nitrate tetrahydrate was used to provide a source of calcium to facilitate stronger and more densified phase formation within the pores. In a departure from prior work the particle treatments were started concurrent with chloride extraction in order to determine if particle delivery would inhibit chloride transport. Following treatment the specimens were immersed in seawater for 4 weeks. After this posttreatment exposure, the specimens were tested for tensile strength and the steel reinforcement was examined for evidence of corrosion. Scanning electron microscopy was conducted to assess impact on microstructure.

Calle, Luz Marina↗

Microstructural evolution, defect mitigation, and precipitation behavior in AA6061 via laser powder bed fusion with high-temperature substrate heating

Defects, particularly solidification cracking, remain persistent challenges in the laser powder bed fusion (LPBF) processing of AA6061 aluminum alloy. This study systematically investigates defect mitigation, microstructural evolution, and mechanical properties associated with high-temperature substrate preheating at 500 °C. Comprehensive microstructural analyses, including characterization of defects, grain structures, and precipitation behavior, were performed on samples in both as-built and T6 heat-treated states. Elevated preheating substantially reduced solidification cracking across a wide processing window, while demonstrating decreased crack sensitivity to laser parameters. Columnar cracks along the build direction were observed despite substrate preheating. Lack-of-fusion and keyhole porosity were effectively eliminated, though gas-induced microporosity persisted at higher powers. In-depth characterization of two distinct laser power and speed conditions confirmed the formation of micron-sized, non-coherent Mg 2 Si precipitates under heated substrate conditions, alongside α-AlFeCrMnSi intermetallic phases indicative of in-situ thermal effects during fabrication. Subsequent T6 heat treatment revealed the formation of fine, coherent needle-shaped β″ strengthening precipitates. Despite substantial differences in processing parameters, comparable mechanical properties were measured in the as-built samples (∼52 MPa yield strength, ∼130 MPa tensile strength), primarily due to reduced strain hardening effects and consistent precipitation characteristics. Meanwhile, the T6 heat treatment led to significant improvement in properties, enhancing yield strength by over 400%, aligning closely with the performance of conventional wrought AA6061-T6. These findings underscore that high-temperature substrate preheating offers an effective means to suppress cracks, control precipitation, and enhance mechanical performance in LPBF-processed AA6061.

36 MATERIALS SCIENCE↗

Sputter deposition of high electrical resistivity Au-Ta alloy coatings on rotating substrates

Sputter deposition of gold-tantalum alloy coatings is a key process for manufacturing hohlraums for magnetically-assisted inertial confinement fusion implosions. In this report we describe direct current magnetron sputter deposition of ~ 10 - μ~ 10 - μm-thick films of Au-80 at.% Ta onto rotating sphero-cylindrical hohlraum and planar Si witness substrates. Emphasis is given to how film microstructure and properties are affected by main deposition parameters, including argon working gas pressure, substrate bias, and the source composition (a single alloyed target compared to co-sputtering from two elemental targets). Experimental findings are correlated with distributions of landing energies and incident angles of depositing species calculated by Monte Carlo simulations of ballistic collisions and gas phase atomic transport. Deposition conditions characterized by low energetics of depositing species favor the formation of a β-Ta-like phase. Implications of these results to hohlraum fabrication are discussed.

36 MATERIALS SCIENCE↗

Optimization of La 2 NiO 4+δ Electrolysis Cell Oxygen Electrode through Surfactant-Enabled LaCoO 3±δ Nanocatalyst Deposition

Lanthanum nickelate (LNO) has shown promise as a Cr-resistant air electrode material for SOECs but has suboptimal surface oxygen exchange properties. Nanocoating of the LNO surface with lanthanum cobaltite (LCO) was chosen to improve cell performance as a surface oxygen conductor. The work focused on the implementation of a two-step nano-LCO film deposition utilizing catechol molecules in a porous LNO electrode. The subgoals of the work were to maintain nanosized LCO particles/ grains to increase active surface area and to control the regularity/ homogeneity of the coating across the microstructure. To achieve these goals, a novel surfactant-enhanced liquid infiltration method was utilized, where nucleation sites were spread across the electrode structure to control the location and size of LCO particles. Various catechol surfactant compositions were evaluated for their ability to control the kinetics of nanoparticle deposition and the homogeneity of the coating. Chelated LCO was characterized by X-ray diffraction (XRD), which found a substantial improvement in LCO formation with surfactant addition and determined polymerized norepinephrine to be the best-performing surfactant, with 88.4% pure LCO formed at low temperature. X-ray photoelectron spectroscopy (XPS) confirmed LCO nanostructures formed by the two-step infiltration process, showing no impurities and a stable perovskite structure. Deposition kinetics were analyzed using atomic force microscopy (AFM), correlating infiltration times and solution molarity to nanoparticle size and distribution, the results of which were confirmed in symmetrical cell samples by scanning electron microscopy (SEM). Electrochemical impedance spectroscopy (EIS) testing demonstrated substantial improvements in polarization resistance, where the nanocoating reduced the resistance by ∼55% to 0.152 Ω·cm 2 at 700 °C and 0.039 Ω·cm 2 at 800 °C. Electrical conductivity relaxation (ECR) at this temperature confirmed an improved surface oxygen exchange coefficient of the LCO + LNO heterostructure predicted by the Bode data from EIS, alongside a reduction in activation energy by about 30%.

Deposition↗

Understanding and Strategies for Controlled Interfacial Phenomena in Lithium-Ion Batteries and Beyond

Electrolyte chemistry and properties and electrode structure and chemical properties particularly at the interfaces are crucial for the development of advanced battery components. This project focused on elucidating the roles of the electrolyte and electrode on the formation and evolution of the SEI layer and cell electrochemical performance on silicon and on Li metal anodes. For Si nano/microstructures we evaluated lithiation, volume changes, reactivity, and chemo-mechanical transformations as functions of nanoparticle size, shape, presence of coatings, electrolyte composition, electron leakage to the electrolyte, and cycling. For Li metal anodes we provided detailed analyses of the electrode and electrolyte effects on interfacial reactivity and as a function of microstructural evolution and underlying stochasticity as dendrites nucleate and grow. We thoroughly investigated and simulated how the chemistry of the various components of the electrolyte and the electrode architecture may affect the electrochemical reactions as well as cell degradation. A multiscale modeling approach was utilized, where atomistic simulations informed about the microscopic behavior of the system, and intermediate time and length scales were investigated with mesoscopic models. Results were also tested against selected experiments from our collaborators. The combined theoretical-experimental strategy saves costs by utilizing predictions from computational analyses to guide experimentation.

25 ENERGY STORAGE↗