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At least 343 records · Page 19

Experiments for electromagnetic levitation in microgravity

Containerless processing is a promising research tool for investigating the properties of undercooled melts and their solidification. For conducting samples RF-electromagnetic levitation offers the possibility to obtain large undercoolings by avoiding heterogeneous nucleation at container walls. On earth, however, strong magnetic fields are needed to compensate the gravitational force which imposes a lower limit on the available temperatures and on the accessible undercooling range. Under microgravity conditions the magnetic positioning fields can be minimized and hence, undercooling becomes feasible under ultra-high vacuum conditions and lower temperatures become accessible. In contrast to other undercooling and solidification techniques, electromagnetic levitation allows for diagnostic measurements during the early steps of nucleation and phase selection. Experiments cover a wide field of research topics: nucleation, directional solidification at high velocities, generation of metastable phases, evolution of microstructures, properties of undercooled liquids. Examples from these classes including experiments selected for the IML-2 mission are discussed with emphasis on technical requirements. An overview is given on the German TEMPUS (electromagnetic levitation facility) program.

Willnecker, R.↗

Stacking Defects in Synthetic and Meteoritic Hibonites: Implications for High-Temperature Processes in the Solar Nebula

Hibonite (CaAl12O19) is a primary, highly refractory phase occurring in many Ca-Al-rich inclusions (CAIs) from different chondrite groups, except CI chondrites. Hibonite is predicted to be one of the earliest minerals to condense during cooling of the solar nebula at higher temperatures than any other major CAI mineral. Therefore, hibonite has great potential to reveal the processes and conditions of the very early, high-temperature stages of the solar nebular evolution. Previous microstructural studies of hibonite in CAIs and their Wark-Lovering (WL) rims showed the presence of numerous stacking defects in hibonite. These defects are interpreted as the modification of the stacking sequences of spinel and Ca-containing blocks within the ideal hexagonal hibonite structure, as shown by experimental studies of reaction-sintered ceramic CaO-Al2O3 compounds. We performed preliminary experiments in the CaO-Al2O3-MgO system to understand the formation processes and conditions of defect-structured hibonite found in meteorites.

Han, J.↗

Cluster Dynamics Modeling Needs for the Advanced Materials and Manufacturing Technologies Program

This milestone report aims to identify and assess the cluster dynamics (CD) modeling requirements within the Department of Energy's Office of Nuclear Energy (DOE-NE) Advanced Materials and Manufacturing Technologies (AMMT) program and to communicate these needs to the DOE-NE Nuclear Energy Advanced Modeling and Simulation (NEAMS) program. The goal is to ensure NEAMS is well-informed about the CD modeling requirements to support AMMT's mission of accelerating the development, qualification, demonstration, and deployment of advanced structural materials and manufacturing for nuclear energy applications. CD modeling is an essential tool for predicting the degradation of structural materials under irradiation, which is a key component of AMMT's accelerated qualification process. The AMMT program focuses on both additively manufactured and wrought structural alloys, such as laser powder-bed fusion 316H austenitic stainless steel, alloy 709, Haynes 244, and alloy 617. These materials require a generalized CD modeling framework to facilitate rapid model development and computational simulation. A flexible, generalized CD software, similar to the Multiphysics Object-Oriented Simulation Environment (MOOSE) finite element framework, would enable modeling of various cluster types, including defect clusters, defect-solute clusters, and multicomponent clusters, incorporating thermodynamics and kinetics parameters. Radiation effects, microstructural feature evolution, and multi-dimensional modeling are critical considerations for the CD model. The usability of the CD code should allow for easy modification and coupling with MOOSE-based simulations. Additionally, the software should adhere to Nuclear Quality Assurance-1 standards, include a testing suite for verification and validation, and be version-controlled within a national laboratory-managed Git repository. Benchmark problems are needed to assess code predictions and performance.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Porosity, swelling, and composition evolution in high-burnup monolithic U-Mo fuel

The microstructural progression of very high-burnup (>8 × 10 21 fissions/cm 3 ) monolithic uranium-molybdenum (U-10wt.%Mo) was analyzed, providing crucial insights into the behavior of post-recrystallized nuclear fuel, where scant data exists. Three focused ion beam cuboids sourced from a fuel plate with varying local burnups of 8.86 × 10 21 , 9.05 × 10 21 , and 9.36 × 10 21 fissions/cm 3 were characterized. The porosity and composition of the samples were evaluated to characterize the evolution of the microstructure as a function of fission density and different locations on the fuel plate, while simultaneously isolating plate-specific parameters such as Zr diffusion barrier thickness, hot-isostatic-pressing conditions, enrichment, and reactor conditions. The porosity was segmented, and the three-dimensional distribution of the porosity was extrapolated from the two-dimensional segmentation. The composition was assessed and quantified using energy-dispersive X-ray spectroscopy areal mapping. The porosity fraction increased as a function of the burnup from 27.77±0.51, 35.12±1.54, and 37.71±0.44 % for 8.86 × 10 21 , 9.05 × 10 21 , and 9.36 × 10 21 fissions/cm 3 , respectively. When compared to literature, the porosity volume fraction plateaus at burnups greater than 6 × 10 21 fissions/cm 3 , while the pore size grows linearly as a function of fission density. The number of large pores increased in number density as a function of burnup, while the smallest pores (<0.3 µm) increased up to 9.05 × 10 21 fissions/cm 3 , followed by a decrease at 9.36 × 10 21 fissions/cm 3 . The delamination and cracking in the fuel plate propagated through an interconnected porosity sublayer identified ∼5 µm from the diffusion barrier. The local swelling of the specimens was within or near the prediction bounds of the Robinson-Williams model for local swelling. The fission products, strontium, barium, cerium, and cesium, precipitated into the pores, while neodymium accumulated adjacent to the pores. Furthermore, these findings have direct implications for the development of fuel performance codes and the accurate documentation of the microstructure evolution in high burnup U-Mo, thus enhancing the safety and efficiency of nuclear fuel usage.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Redox-Induced Microstructure and Phase Dynamics in Nickel: Insights from In Situ Synchrotron X-ray Diffraction

Using in situ synchrotron X-ray diffraction, we interrogate the microstructural and phase evolution of polycrystalline nickel (Ni) during redox cycling in O 2 , H 2 , and H 2 O environments. Oxidation in O 2 promotes strong (111) texturing in both the NiO overlayer and the underlying Ni substrate. However, this crystallographic alignment is lost following reduction in H 2 and subsequent reoxidation, demonstrating irreversible microstructural changes. H 2 exposure leads to proton dissolution into the Ni lattice, triggering a localized phase transition from face-centered cubic (FCC) to hexagonal close-packed (HCP) Ni in hydrogen-saturated regions. In H 2 O-containing atmospheres, dissociative H 2 O adsorption produces protons that permeate the NiO layer, forming γ-NiOOH within the NiO lattice and HCP Ni beneath the NiO overlayer as protons accumulate. Kinetic analysis via the Johnson-Mehl-Avrami–Kolmogorov model uncovers distinct growth mechanisms: preoxidized Ni surfaces follow one-dimensional (1D) kinetics for NiO, γ-NiOOH, and HCP growth, whereas pristine Ni exhibits three-dimensional (3D) kinetics due to island-like nucleation and growth of NiO. Furthermore, these results highlight the critical interplay between H 2 O dissociation, hydrogen permeation, and redox-driven phase transformations, with practical implications in engineering nickel-based catalysts and hydrogen storage systems through controlled microstructural and phase evolution.

36 MATERIALS SCIENCE↗

Focused Ion Beam Tomography of Alloy 617 Corroded in Molten Chloride Salt

Materials qualification of reactor structural materials is a critical step in rapid implementation of advanced nuclear reactor technologies, particularly to assess the corrosion performance in these designs. Accelerated qualification of reactor structural materials requires incorporating powerful computational toolsets, such as phase field modelling in the Multiphysics Object-Oriented Simulation Environment (MOOSE) framework, to predict the evolution of structural materials due to corrosion. Accordingly, computational toolsets will require experimental data generated at appropriate length scales to validate accuracy. Focused ion beam (FIB) provides a high degree of control over manipulation of materials for analytical purposes, including capturing data on the evolution in the microstructure and elemental composition of materials at the mesoscale, an appropriate length scale for phase field modelling of intergranular diffusion phenomena using the MOOSE framework. For instance, the FEI Helios G4 UX dual beam plasma FIB microscope at the Irradiated Materials Characterization Laboratory (IMCL) is capable of backscatter diffraction (EBSD) and energy-dispersive x-ray spectroscopy (EDS) documenting the evolution in the microstructure and elemental composition, respectively. The Helios can perform EDS and EBSD three-dimensionally (3D) using tomography, which is then combined using different software packages to visualize 3D volumes correlating elemental composition to microstructural data. The purpose of this investigation was to develop a streamlined characterization and data processing workflow for 3D tomography studies on the FEI Helios G4 plasma FIB. The investigation is segmented into three parts: 1) Optimizing the data collection workflow, 2) identifying appropriate data processing and visualization software (i.e. DREAM.3D, MIPAR, and VGStudioMax), and 3) establishing an infrastructure for public release. The optimization of the data collection workflow is in collaboration with members of the U220 department to setup formal training on the tomography operation of the G4, through ThermoFisher Scientific, and exploring DREAM.3D, MIPAR, and VGStudioMax data processing/visualization software packages. VGStudioMax currently demonstrates the most promise for future use. Optimization of the data collection and processing workflow is still ongoing. A collaboration with INL High Performance Computing (HPC) established an open-source license for expediting the public release of FIB tomography datasets through HPC. FIB tomography data generated by the G4 will provide comprehensive data for validating 3D phase field mesoscale modelling tools within the MOOSE framework for accelerated qualification of reactor structural materials.

Copeland-Johnson, Trishelle↗

The continuing battle against defects in nickel-base superalloys

In the six decades since the identification of age hardenable nickel-base superalloys their compositions and microstructures have changed markedly. Current alloys are tailored for specific applications. Thus their microstructures are defined for that application. This paper briefly reviews the evolution of superalloy microstructures and comments on the appearance and implications of microstructural defects in high performance superalloys. It is seen that new alloys and proceses have generated new types of defects. Thus as the industry continues to develop new alloys and processes it must remain vigilant toward the identification and control of new types of defects.

Dreshfield, R. L.↗

Gravitational Effects on Distortion in Sintering

During sintering a powder compact gains strength through low-temperature interparticle bonding, usually induced by solid-state surface diffusion, followed by further strength contributions from high-temperature densification. In cases where a liquid phase forms, sintering densification is accelerated and shape retention is sustained while open pores remain and contribute capillary forces. Unfortunately, sintering densification requires the compact become thermally softened to a point where creep strain rates reach levels near 10(exp -2)/s when the liquid forms. On the other hand, thermal softening of the powder compact substantially reduces the strength at high temperatures. Therefore, the in situ strength evolution during sintering is a primary focus to separate compact densification (as required for high performance) with minimized distortion (as required for net-shaping). With respect to gravitation effects on distortion during sintering there are two points of substantial weakness - prior to significant interparticle bonding and during final pore closure. This research is focused on understanding the competition among interparticle neck growth, densification, thermal softening, grain boundary wetting, capillary effects associated with liquid wetting and residual porosity, and gravity. Most surprising is the apparent role of gravity, where the deviatoric stress acting on the powder structure induces skeletal formation that reduces distortion. In contrast with theory, microgravity samples exhibit more distortion yet fail to fully densify. Results are presented on the experimental concepts supporting an emerging model of sintering strength evolution that enables understanding of both distortion and densification. The experiments have relied on tungsten heavy alloys, various combinations of dihedral angle, pore size, initial porosity, liquid:solid ratio, and heating rates. On Earth, the dominant factor with respect to distortion is the starting body heterogeneity. Current modeling efforts are seeking some means to uniformly predict the distortion based on a starting pore structure heterogeneity parameter. Densification is largely unaffected by the initial pore structure, but distortion is highly variable, suggesting that nonuniform pore closure might be a significant parameter during sintering. With respect to flight experiments, plans include removal of the solid body forces acting on the solid grains, allowing stabilization of the pore structure and examination of the buoyancy effects with regard to distortion. In microgravity there is the surprising result that compacts do not densify, yet distort a factor that is contrary to all current sintering models. Densification without distortion during liquid phase sintering was achieved by manipulating microstructure and its evolution during sintering. Microstructure parameters such as the solid volume fraction, dihedral angle, initial porosity, and pore size were varied to measure densification and distortion behavior during LPS using W-Ni-Cu alloys. Green compacts were formed using ethylene-bis-stearamide as a pore-forming agent with the amount of polymer controlling the initial porosity. Different initial pore sizes were generated by varying the polymer particle size. Dihedral angle was varied by changing the Ni:Cu ratio in the alloys. Finally, the solid volume fraction was adjusted via the tungsten content. Distortion was quantified using profiles determined with a coordinate measuring machine to calculate a distortion parameter. Sintering results showed that solid volume fraction and dihedral angle are the dominant factors on densification and distortion during liquid phase sintering. Distortion decreases with increasing solid volume fraction and dihedral angle, while initial porosity and pore size have no observable effect on distortion at nearly full densification. Various strategies emerge to improve distortion control in liquid phase sintering.

German, Randall M.↗

Evolution and Control of 2219 Aluminum Microstructural Features Through Electron Beam Freeform Fabrication

The layer-additive nature of the electron beam freeform fabrication (EBF3) process results in a tortuous thermal path producing complex microstructures including: small homogeneous equiaxed grains; dendritic growth contained within larger grains; and/or pervasive dendritic formation in the interpass regions of the deposits. Several process control variables contribute to the formation of these different microstructures, including translation speed, wire feed rate, beam current and accelerating voltage. In electron beam processing, higher accelerating voltages embed the energy deeper below the surface of the substrate. Two EBF3 systems have been established at NASA Langley, one with a low-voltage (10-30kV) and the other a high-voltage (30-60 kV) electron beam gun. Aluminum alloy 2219 was processed over a range of different variables to explore the design space and correlate the resultant microstructures with the processing parameters. This report is specifically exploring the impact of accelerating voltage. Of particular interest is correlating energy to the resultant material characteristics to determine the potential of achieving microstructural control through precise management of the heat flux and cooling rates during deposition.

Taminger, Karen M.↗

Evolution and Control of 2219 Aluminum Microstructural Features through Electron Beam Freeform Fabrication

Electron beam freeform fabrication (EBF3) is a new layer-additive process that has been developed for near-net shape fabrication of complex structures. EBF3 uses an electron beam to create a molten pool on the surface of a substrate. Wire is fed into the molten pool and the part translated with respect to the beam to build up a 3-dimensional structure one layer at a time. Unlike many other freeform fabrication processes, the energy coupling of the electron beam is extremely well suited to processing of aluminum alloys. The layer-additive nature of the EBF3 process results in a tortuous thermal path producing complex microstructures including: small homogeneous equiaxed grains; dendritic growth contained within larger grains; and/or pervasive dendritic formation in the interpass regions of the deposits. Several process control variables contribute to the formation of these different microstructures, including translation speed, wire feed rate, beam current and accelerating voltage. In electron beam processing, higher accelerating voltages embed the energy deeper below the surface of the substrate. Two EBF3 systems have been established at NASA Langley, one with a low-voltage (10-30kV) and the other a high-voltage (30-60 kV) electron beam gun. Aluminum alloy 2219 was processed over a range of different variables to explore the design space and correlate the resultant microstructures with the processing parameters. This report is specifically exploring the impact of accelerating voltage. Of particular interest is correlating energy to the resultant material characteristics to determine the potential of achieving microstructural control through precise management of the heat flux and cooling rates during deposition.

Taminger, Karen M.↗

LAROMance Grade 91 Model Integration in NEML2

New reactor designs are targeting higher operating temperatures for increased thermal efficiency when compared to the current fleet of light water reactors. Designing structural components for these high temperature environments with reliable long-term operations requires material models that can accurately capture the deformation mechanisms active in these environments. The LAROMance surrogate material models are based on a database of mechanistic crystal plasticity simulations for high-temperature conditions. Inputs to the LAROMance models reflect the microstructural pedigree of the material, like dislocation densities and precipitate contents. Based on the evolution of these microstructural features, the LAROMance model provides the engineering scale constitutive model response. The LAROMance model was recently parameterized for Grade 91, a high temperature alloy. In the present work, the Grade 91 LAROMance model is implemented in the New Material Model Library, version 2 (NEML2). NEML2 provides a modular way to build material models from smaller blocks and was developed to vectorize the material update to efficiently run on modern computational architectures with graphics processing unit accelerators. NEML2 constitutive models can be used in simulations based on the multiphysics object-oriented simulation environment (MOOSE). This report provides details on the implementation of the Grade 91 LAROMance model in NEML2 and its verification of engineering scale finite element simulations in MOOSE.

42 - ENGINEERING↗

Structure evolution and tin redistribution during oxidation of Zircaloy-4 at 500°C

Zirconium (Zr) alloys are widely used as fuel cladding in nuclear power reactors due to their thermal stability, mechanical durability, corrosion resistance, and low neutron absorption cross-section. However, their performance is challenged by oxidation in reactor environments, making the study of Zr alloy corrosion behavior crucial for ensuring the safety, longevity, and economic viability of nuclear power systems. While the oxidation behavior of Zr-based cladding materials has been extensively studied since the 1950s, a mechanistic understanding into the relationship between structure evolution, solute element redistribution, and properties remains elusive. Valuable insights may be obtained through advanced experimental methods, such as in-situ and high resolution microscopy techniques. Here, in this study, the oxidation behavior of Zircaloy-4 at 500 °C in O 2 is characterized using a multimodal advanced characterization approach. Using in-situ X-ray diffraction, the phase evolution from metastable to stable oxides is tracked in real time. Complementary high-resolution techniques, including electron microscopy and atom probe tomography, reveal nanoscale insights into the microstructural changes and solute redistribution across the oxide/metal interface. Nanohardness mapping across the oxide/metal interface highlights localized mechanical property variations that may be linked to changes in microstructure and crystal structure within the oxide layer. These findings offer valuable insights into the microstructure and property evolution of Zircaloy-4 during oxidation, contributing to a better understanding of microstructural changes in Zr-based alloys under oxidative environments.

APT↗

Image processing workflow yielding high contrast synchrotron nanoscale computed tomography data from Ni-YSZ electrodes

The operating lifetime of Ni-YSZ fuel electrodes used in solid oxide electrolysis cells and fuel cells (SOECs and SOFCs) is limited by Ni redistribution, one of the primary degradation mechanisms that must be overcome to extend the longevity and maximize the performance of SOECs and SOFCs. To achieve this, 3D microstructural data is needed to relate both initial performance and performance loss over time to microstructural properties and their evolution throughout operation under various conditions. However, 3D microstructure data remains relatively scarce within the literature due to multiple challenges in acquiring and analyzing such data reliably. This work presents a workflow for acquiring and processing synchrotron X-ray nanoscale computed tomography (nano-CT) data from Ni-YSZ electrodes. Parameters for each step in the nano-CT workflow are described up to the final result (a 3D reconstruction), with particular emphasis on image alignment using freely available software. Following the results of a parametric sweep of the image alignment step, high contrast, low signal-to-noise 3D nano-CT data is obtained with relatively short compute times. While the exact methods best suited to samples with different microstructural qualities, or similar Ni-YSZ nano-CT data obtained from other sources may deviate from the solution found herein, this work also generalizes the decision points and evaluation of each step to provide a starting point to adapt this workflow to other datasets.

08 HYDROGEN↗

Effect of undercooling on the microstructure of Ni-35 at. pct Mo (eutectic) and Ni-38 at. pct Mo (hypereutectic) alloys

Ni-35 at. pct Mo and Ni-38 at. pct Mo alloy specimens have been solidified from various levels of undercooling in the differential thermal analysis and the electromagnetic levitation units in a pyrex/vycor bed. The evolution of the microstructure in the solified specimens has been examined in terms of the degree of undercooling, the nature of the first phase to nucleate from the melt, and the specimen cooling rate. The melt has been observed to undercool more in the presence of intermetallic NiMo (beta) phase as compared to that in the presence of nickel-rich solid solution (gamma). The 'anomalous eutectic' type of microstructure has been shown to result from the initial formation of the dendritic skeleton of either of the two phases, its segmentation due to convection and ripening, and the subsequent nucleation of the other phase in the interdendritic liquid regions. The recalescence behavior has been examined as a function of undercooling and the nature of the phase nucleating first in the melt.

Tewari, S. N.↗

Bulk nanocrystalline Al–Mg–Y alloys with amorphous grain boundary complexions display high strength and compressive plasticity

Although nanocrystalline alloys regularly exhibit high strengths, their use in structural applications often face challenges due to sample size limitations, unstable microstructures, and the limited ability to plastically deform. The incorporation of amorphous grain boundary complexions has been proposed to address these issues, by simultaneously stabilizing nanocrystalline grain structures for scale-up processing and improving alloy toughness. In the present study, the mechanical behavior of bulk nanocrystalline Al–Mg–Y is examined with macroscale compression testing, probing a length scale that is relevant to real-world structural applications. Bulk samples were fabricated via a simple powder metallurgy approach, with different hot-pressing temperatures and durations employed for consolidation in order to investigate microstructural and property evolution. All of the specimens contained primary face-centered cubic Al and secondary Al 4 C 3 and Al 3 Y phases, with the Al 3 Y particles exhibiting two populations of small equiaxed and larger elongated particles. Appreciable plasticity was measured along with high ultimate stresses over 800 MPa due to the presence of amorphous grain boundary complexions. Microstructural characterization of fracture surfaces revealed that the area fraction of dimpled regions increased with longer hot-pressing time. Most importantly, the elongated Al 3 Y particles formed regular cellular patterns with increasing hot-pressing time, delaying shear localization and significantly enhancing plasticity. The hierarchy present in the microstructure of the Al–Mg–Y alloy, from amorphous grain boundary complexions to secondary phases, gives rise to excellent bulk mechanical properties, which are attractive for structural applications.

Bulk nanocrystalline alloy↗

Shear History Extensional Rheology Experiment: A Proposed ISS Experiment

The Shear History Extensional Rheology Experiment (SHERE) is a proposed International Space Station (ISS) glovebox experiment designed to study the effect of preshear on the transient evolution of the microstructure and viscoelastic tensile stresses for monodisperse dilute polymer solutions. Collectively referred to as Boger fluids, these polymer solutions have become a popular choice for rheological studies of non-Newtonian fluids and are the non-Newtonian fluid used in this experiment. The SHERE hardware consists of the Rheometer, Camera Arm, Interface Box, Cabling, Keyboard, Tool Box, Fluid Modules, and Stowage Tray. Each component will be described in detail in this paper. In the area of space exploration, the development of in-situ fabrication and repair technology represents a critical element in evolution of autonomous exploration capability. SHERE has the capability to provide data for engineering design tools needed for polymer parts manufacturing systems to ensure their rheological properties have not been impacted in the variable gravity environment and this will be briefly addressed.

Hall, Nancy R.↗