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At least 19 records

3D printed carbon fiber reinforced carbon as an energy efficient alternative to graphite for EFAS tooling

As Electric Field Assisted Sintering (EFAS) gains more industrial acceptance and use, it becomes more important to develop more efficient means to implement this technology. To this aim, 3D printed continuous carbon fiber reinforced carbon (CCC) was manufactured and fabricated into tooling for EFAS systems as an alternative to traditional graphite tooling. The impact of fiber orientation on the thermal and electrical properties of the CCC was characterized. Sample material was sintered in Tokai G535 graphite tooling, under common processing conditions and compared with CCC tooling. There was nearly 50 % energy savings compared to graphite while maintaining equivalent sample density and microstructure plus keeping ram temperatures 39 % cooler. This is due to spatial control of generated heat and thermal diffusivity within the molds, by means of fiber orientation anisotropy. Finite element modeling of the tooling design supported the experimental results as well as displays the effect of optimization of this 3D printed CCC material.

36 MATERIALS SCIENCE↗

Development and Validation of MALAMUTE model for Electric Field Assisted Sintering of Structural Materials

Fusion power plant designs feature extreme material performance requirements for structural material candidates. In addition to conventional alloys, more advanced composites and oxide dispersion strengthened (ODS) alloys are being explored, however, achieving the desired microstructures to maximize performance using traditional manufacturing methods can be challenging. The advanced manufacturing (AM) electric field-assisted sintering (EFAS) technique offers improved control over the final microstructure through higher heating and cooling rates and moderate pressures. Modeling and simulation tools show promise in elucidating the process-structure-property-performance (PSPP) correlation for AM-produced parts, including the EFAS process. An inherently multiscale process, the EFAS technique aligns well with the multiscale modeling capability of the open-source Multiphysics Object-Oriented Simulation Environment (MOOSE)[cite]. We present here an electro-thermo-mechanical approach to modeling the EFAS process using the MOOSE Application Library for Advanced Manufacturing UTilitiEs (MALAMUTE) code. Prediction of the field and gradient distributions across the EFAS tooling is required to accurately describe the conditions for the lower-scale microstructural evolution models. In this work we present the MALAMUTE model developed to predict the electrical potential, temperature, and mechanical stress distribution across the EFAS graphite tooling and part at the larger engineering-scale. Validation of the MALAMUTE engineering-scale model is completed using data from experimental densification and pre-densified runs of iron powder via EFAS at 1000oC. These runs were conducted using a Thermal Technology DCS-5 EFAS system. Data collected during the experiment runs include the direct current (DC) supplied to the graphite tooling, the temperature of the graphite tooling as measured with a pyrometer, and the force applied to the top of the graphite tooling stack, and the data were recorded every 10 seconds. Our validation approach used the current and force data from the EFAS run as boundary condition inputs to the MAMALUTE simulation; the temperature data were used to evaluate the MALAMUTE EFAS model prediction. Results of the MALAMUTE simulations are employed to connect the external pyrometer temperature measurement to the temperature profile across the part undergoing consolidation. We investigate the impact of material property variation and mesh deformation on the temperature profile as predicted by MALAMUTE. We conclude by highlighting projects where the MALAMUTE EFAS modeling and simulation capabilities will be used to assist experimental design.

36 - MATERIALS SCIENCE↗

Accelerating the Discovery of New, Single Phase High Entropy Ceramics via Active Learning

High-entropy ceramics have garnered interest due to their remarkable hardness, compressive strength, thermal stability, and fracture toughness; yet the discovery of new high-entropy ceramics (out of a tremendous number of possible elemental permutations) still largely requires costly, inefficient, trial-and-error experimental and computational approaches. The entropy forming ability (EFA) factor was recently proposed as a computational descriptor that positively correlates with the likelihood that a 5-metal high-entropy carbide (HECs) will form the desired single phase, homogeneous solid solution; however, discovery of new compositions is computationally expensive. If you consider 8 candidate metals, the HEC EFA approach uses 49 optimizations for each of the 56 unique 5-metal carbides, requiring a total of 2744 costly density functional theory calculations. Here, we describe an orders-of-magnitude more efficient active learning (AL) approach for identifying novel HECs. To begin, we compared numerous methods for generating composition-based feature vectors (e.g., magpie and mat2vec), deployed an ensemble of machine learning (ML) models to generate an average and distribution of predictions, and then utilized the distribution as an uncertainty. Here we then deployed an AL approach to extract new training data points where the ensemble of ML models predicted a high EFA value or was uncertain of the prediction. Our approach has the combined benefit of decreasing the amount of training data required to reach acceptable prediction qualities and biases the predictions toward identifying HECs with the desired high EFA values, which are tentatively correlated with the formation of single phase HECs. Using this approach, we increased the number of 5-metal carbides screened from 56 to 15,504, revealing 4 compositions with record-high EFA values that were previously unreported in the literature. Our AL framework is also generalizable and could be modified to rationally predict optimized candidate materials/combinations with a wide range of desired properties (e.g., mechanical stability, thermal conductivity).

36 MATERIALS SCIENCE↗

Microbiological Characterization of the International Space Station Water Processor Assembly External Filter Assembly S/N 01

The External Filter Assembly (EFA) S/N 01 is a mesh screen filter with a pore size of approximately 300 micron that was installed in the International Space Station (ISS) Water Processor Assembly (WPA) between the Waste Tank and the Mostly Liquid Separator (MLS) on February 11, 2010 to protect clearances in the MLS solenoid valve SV_1121_3. A removal & replacement of the EFA Filter was performed on March 22, 2011 in response to increasing pressure across the Waste Tank solenoid valve SV_1121_1 and the EFA Filter. The EFA Filter was returned on ULF6 and received in the Boeing Huntsville Laboratory on June 13, 2011. The filter was aseptically removed from the housing, and the residual water was collected for enumeration and identification of bacteria and fungi. Swab samples of the filter surface were also collected for microbiological enumeration and identification. Sample analyses were performed by Boeing Huntsville Laboratory and NASA Johnson Space Center Microbiology for comparison. Photographic documentation of the EFA filter was performed using a stereo microscope and environmental scanning electron microscope. This paper characterizes the amount and types of microorganisms on the filter surface and in the residual water from the filter housing following 1 year of utilization in the ISS WPA.

Weir, Natalee↗

Electric-field-assisted-sintering of rare-earth oxide dispersion strengthened Fe-Cr-Mo alloys

Oxide dispersion-strengthened (ODS) alloys are widely recognized for their exceptional high-temperature strength, creep resistance, and radiation tolerance, making them indispensable for advanced nuclear reactors, aerospace, and energy systems. Achieving a fine and stable dispersion of oxide nanoparticles is critical, as these particles act as strong barriers to dislocation motion and effective sinks for irradiation-induced defects, ensuring structural integrity under extreme conditions. Here, in this study, Fe–Cr–Mo-based ODS alloys were fabricated via mechanical alloying and consolidated using electric-field-assisted sintering (EFAS) with additions of Y 2 O 3 , La 2 O 3 , and CeO 2 . EFAS processing produced ultrafine-grained microstructures (average grain size <1 μm) with uniformly distributed oxide clusters (2–4 nm). Atom probe tomography revealed that La 2 O 3 -containing alloys exhibited the highest nanoparticle number density, resulting in superior tensile strength compared to yttria- and ceria-bearing counterparts. The combined effect of grain refinement and rare-earth oxide dispersion significantly enhanced mechanical performance, demonstrating the potential of EFAS for developing high-strength ferritic alloys for demanding environments such as nuclear systems.

36 - MATERIALS SCIENCE↗

High-throughput synthesis of high-entropy alloys via parallelized electric field assisted sintering

Materials discovery and design is an expensive and time-consuming process, though necessary to advance many engineering fields. In this work, a novel tooling design is utilized in conjunction with electric field assisted sintering (EFAS) to effectively create a new high-throughput synthesis technique: parallelized EFAS. Through this technique, a wide range of material compositions and geometries can be synthesized in parallel as isolated samples or as part of contiguous arrays. Multiple tooling designs are explored to examine both the flexibility and limitations of the technique. A series of increasing complex alloys is produced simultaneously using in situ alloying, beginning with pure Ni and adding equimolar constituents up to the septenary high-entropy alloy AlCoCrCuFeMnNi. Microstructural characterization reveals each sample is effectively fully dense and chemically homogenous while exhibiting phases in agreement with CALPHAD predictions. Scalability of parallelized EFAS is then experimentally demonstrated and the implications for materials discovery and automation are discussed.

36 - MATERIALS SCIENCE↗

Microstructure development of novel composite heating elements for steel decarbonization

The iron and steel industry is critical for the modern world but is also responsible for 7% of the total energy sector CO2 emissions. It is a difficult industry to decarbonize due to the high temperature heat required for the production of steel, such as reheating steel slabs to ~1250 °C for hot rolling. Electrification of this process using resistive heating is currently not possible due to the poor creep resistance of MoSi2 heating elements, which need to be operated well below their maximum temperatures when mounted horizontally. To solve this problem, novel MoSi2 composite heating elements with SiBCN ceramic reinforcements are being developed using high energy ball milling and electric field assisted sintering (EFAS). The microstructure and density of the composites after sintering depends on the sintering parameters chosen. Herein we present the effects of EFAS sintering parameters on the microstructure and density of the MoSi2-SiBCN composites.

36 - MATERIALS SCIENCE↗

Hybrid Additive Manufacturing and Electric Field-Assisted Sintering of High-temperature Heat Exchangers via Sacrificial Channel Molds

A hybrid manufacturing approach, integrating additive manufacturing (AM) with powder methodology via electric field-assisted sintering (EFAS), was developed for the fabrication of high-temperature compact heat exchangers (CHX) from refractory metals. The methodology employed additively manufactured sacrificial channel molds (SCMs) as shapeholders for CHX channels, which were embedded in metal powders using EFAS. Following embedding, the SCMs were chemically dissolved to form the internal channel network. SCMs were fabricated using both digital light processing (DLP) and direct ink writing (DIW) from chemically reactive, calcium-based ceramic feedstocks with varying ratios of Al2O3 reinforcement. The microstructure, phase composition, and dissolution behavior of both as-printed and embedded SCMs were investigated. The shrinkage behavior of the SCMs embedded in refractory metals, as well as the interfacial characteristics between the SCMs and metal matrix, were studied. The results showed that the SCMs containing sufficient chemical reactive ceramics dissolved effectively before and after embedding. The as-printed SCMs retained the phase composition of their feedstocks, but the embedded SCMs containing calcium-based ceramics and Al2O3 exhibited the formation of calcium aluminates due to high temperature exposure during embedding. Most SCMs exhibited a cellular Al2O3 network filled with Ca-rich ceramics. Shrinkage after embedding was strongly dependent on SCM density, with lower density SCMs exhibiting greater shrinkage. A thin SCM-affected zone was observed at the metal matrix surface, characterized by increased porosity compared to the bulk matrix. This effect was attributed to infiltration of the SCM materials into powder particle boundaries under pressure, followed by their removal during dissolution. This study demonstrates the feasibility of manufacturing CHXs from hard-to-process refractory metals for use in harsh environments.

36 - MATERIALS SCIENCE↗

Electric field enhanced diffusion welding of alloy 617: Microstructural characteristics and mechanical properties

This study investigated the microstructural characteristics and mechanical behavior of diffusion welded nickel-based Alloy 617 obtained by electric field-assisted sintering (EFAS) using various parameters. The interfacial microstructure exhibited different characteristics including good grain boundary (GB) migration across the interface in the samples diffusion-welded at 1100 °C and a flat interface in the samples joined at 1000 °C and 1050 °C. The interface consisted of fine Al 2 O 3 oxides, while precipitation of interfacial M 23 C 6 carbides was not observed. Grain boundaries migrated across the Al 2 O 3 oxides, leaving these oxides within the grains. Graded grain size was observed, with grain coarsening being more significant near the sample surface due to the temperature gradient induced by EFAS. Tensile testing revealed that the specimens fractured in the matrix away from the interface, indicting strong diffusion-welded joints. Further, the peak tensile strength of 807 MPa was obtained in the samples welded at 1000 °C due to minimal grain growth. The materials obtained at 1100 °C exhibited reduced tensile strength but improved ductility. Strain maps revealed by digital image correlation showed alternating high and low strain segments in the samples produced at 1000 °C and 1050 °C, indicating that the flat interfaces with no GB migration were less ductile compared to the matrix. A greater strain uniformity was observed along the bond interfaces with improved GB migration. The hardness reduced near the sample surfaces due to enlarged grains induced by temperature gradient. This study demonstrates that GB migration and enhanced mechanical strength can be achieved in diffusion-welded Alloy 617.

36 MATERIALS SCIENCE↗

Embedding of Optical Fibers with Electric Field Assisted Sintering

The Electric Field Assisted Sintering (EFAS) technique was used for embedding the fibers, involving rapid heating via an electric current and pressure, reducing fiber exposure to high temperatures. Stainless steel guide tubes were inserted at the fiber-matrix junctions to prevent fiber breakage during the sintering process. The study varied key EFAS parameters—temperature (800°C to 980°C), pressure (40-50 MPa), and hold time (5-10 minutes)—to assess how they influenced fiber embedding. After embedding, the fibers were inspected using optical frequency domain reflectometry (OFDR) to evaluate optical losses and strain along the fiber length. The OFDR scans confirmed that the fibers remained intact, and subsequent transmission tests demonstrated no macroscopic fractures. The embedded samples were also analyzed using scanning electron microscopy (SEM) and X-ray computed tomography (CT) scans. These tests confirmed good bonding between the fiber and matrix with no cracking, though some porosity was present in samples fabricated at lower temperatures. At higher temperatures (980°C), the fiber-matrix bonding was continuous and defect-free, with metal coatings aiding in the bonding process. Elemental analysis showed interdiffusion between the fiber coatings and matrix materials, particularly between the gold coating and stainless steel. Helium leak tests revealed that lower sintering temperatures resulted in matrix porosity, causing leaks, but samples fabricated at 980°C were leak-tight.

46 - INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AN↗

ExMASS: A viable model for authentic student-scientist research partnerships

The Exploration of the Moon and Asteroids by Secondary Students (ExMASS) program provides students the opportunity to conduct authentic, student-led, open-inquiry research with assistance from their teacher and a scientist. One goal of the program is to enhance participants’ attitudes toward science. Most students enter the ExMASS program with positive attitudes toward science. However, the attitude survey developed for ExMASS measured small but statistically significant increases in attitudes. This paper discusses the ExMASS program, an attitude towards science survey designed for the program’s specific audience, and the results of statistical analyses of the survey. The validity of the attitudes survey was tested with an exploratory factor analysis (EFA). The results of the EFA revealed two salient factors measured by the survey: 1) Personal Importance of Science and 2) Importance of Science to Society. A reliability analysis revealed a Cronbach alpha value of 0.89. Paired t-tests revealed statistically significant differences in students’ attitudes before and after the program. For Factor 1, participants’ before scores were statistically significantly lower than their post scores, t(88) = 3.16, p<0.05. For Factor 2, participants’ before scores were statistically significantly lower than their post scores, t(88) = 4.47, p<0.05. ExMASS has been shown to be a practical model for programs designed to increase high school student attitudes toward science. More information on the ExMASS program is available at https://www.lpi.usra.edu/exploration/education/hsResearch/.

science↗

Microstructural Characteristics, Mechanical Properties, and Corrosion Behavior of Field-Assisted Diffusion Welded Alloy 617

This study investigated the microstructural characteristics, mechanical response, and corrosion resistance of Alloy 617 diffusion welded by electric field-assisted sintering (EFAS). The microstructure exhibited good grain boundary (GB) migration across the interface and flat interface in the samples bonded at different conditions. Graded grain size was observed, with grain coarsening being more significant near sample surface due to EFAS-induced temperature gradient. Tensile testing revealed that the specimens fractured in the matrix away from the interface. The peak strength of 807 MPa was obtained in the samples welded at 1000°C. The materials obtained at 1100°C exhibited reduced tensile strength but improved ductility. Strain maps revealed by digital image correlation showed the flat interfaces were less ductile compared to the matrix. The hardness reduced near sample surfaces due to enlarged grains induced by temperature gradient. The interfaces with GB migration exhibited improved corrosion resistance in molten salt compared to the flat interfaces.

36 - MATERIALS SCIENCE↗

Densification, microstructure, and mechanical properties of Mo–30W alloys fabricated from conditioned powders

Refractory alloys, such as molybdenum-based systems, are attracting growing interest for applications in extreme environments, such as in the nuclear and aerospace industries. Recent advances in sintering technologies, coupled with mechanical alloying, have enabled the tailored design of these alloys by leveraging powder characteristics to control final microstructures and mechanical properties. In this study, Mo-30W alloys were fabricated using electric field-assisted sintering (EFAS) from ball-milled powders with and without hydrogen treatment to investigate the influence of surface oxides on material properties and sintering behavior. The results revealed that samples processed from as-ball-milled powder contained a high density of oxides within the microstructure, whereas oxide presence was significantly reduced in samples fabricated from hydrogen-treated powders. Interestingly, the two powder types led to opposite trends in grain size distribution: samples from untreated powders exhibited grain refinement from sample periphery to the center, while samples from hydrogen-treated powders showed grain coarsening toward the center. This behavior is attributed to temperature gradients present during sintering due to electrical percolation pathway differences during Joule heating. The powder surface oxides may have influenced the temperature distribution and grain evolution. Microhardness profiles measured along both axial and thickness directions were consistent with the grain size distribution. Furthermore, oxide films on powder surfaces have delayed densification by hindering particle necking and atomic diffusion during sintering.

36 - MATERIALS SCIENCE↗

CICE on a C-grid: new momentum, stress, and transport schemes for CICEv6.5

Abstract. This article presents the C-grid implementation of the CICE sea ice model, including the C-grid discretization of the momentum equation, the boundary conditions (BCs), and the modifications to the code required to use the incremental remapping transport scheme. To validate the new C-grid implementation, many numerical experiments were conducted and compared to the B-grid solutions. In idealized experiments, the standard advection method (incremental remapping with C-grid velocities interpolated to the cell corners) leads to a checkerboard pattern. A modal analysis demonstrates that this computational noise originates from the spatial averaging of C-grid velocities at corners. The checkerboard pattern can be eliminated by adjusting the departure regions to match the divergence obtained from the solution of the momentum equation. We refer to this novel approach as the edge flux adjustment (EFA) method. The C-grid discretization with edge flux adjustment allows for transport in channels that are one grid cell wide – a capability that is not possible with the B-grid discretization nor with the C-grid and standard remapping advection. Simulation results match the predicted values of a novel analytical solution for one-grid-cell-wide channels.

Lemieux, Jean-François (ORCID:0000000320845759)↗

Report on the Assessment of Ion Irradiations on High Entropy Alloys

Idaho National Laboratory (INL) initiated a joint international effort with the Czech Republic to explore the feasibility of manufacturing High Entropy Alloys for high-temperature nuclear applications using Additive Manufacturing. This effort was funded at INL by the United States Department of Energy’s Office of Nuclear Energy under the Advanced Reactor Technologies and Advanced Materials and Manufacturing Technologies (AMMT) Program. The High Entropy Alloys were specifically designed for the corrosive and irradiation environments as experienced in gas fast reactors, molten salt reactors, and fusion power. These alloys were manufactured by multiple processes to determine the impact of manufacturing processes on the performance of the alloys in corrosive and irradiation environments. Preliminary results show that MoNbTiV and MoNbTi alloys exhibit no degradation after multiple corrosion tests. These MoNbTiV and MoNbTi alloys were also evaluated after irradiation experiments were conducted at the Michigan Ion Beam Laboratory at the University of Michigan, which is the focus of this milestone report. For these irradiation experiments, the MoNbTiV and MoNbTi alloys manufactured by arc melting and Electric Field Assisted Sintering (EFAS) were tested at 500 C at a dose of 30 dpa to evaluate the microstructural stability and decomposition.

36 - MATERIALS SCIENCE↗

REFRACTORY COMPACT HEAT EXCHANGERS WITH EMBEDDED SENSORS ENABLED BY HYBRID ADVANCED SINTERING AND ADDITIVE APPROACH

Structural health monitoring (SHM) of compact heat exchangers (CHXs) operating in extreme environments is essential for ensuring system reliability, safety, and longevity. This study presents the development of high-temperature sensors fabricated via aerosol jet printing (AJP) using platinum ink, selected for its exceptional thermal stability, oxidation resistance, and electrical conductivity. AJP enables precise deposition of fine-feature sensor patterns onto complex geometries, making it well-suited for integration within CHX architectures. To enhance sensor durability, an alumina-based ceramic protective layer was printed over the platinum sensing elements. The sensors demonstrated stable, repeatable performance up to 900?°C during extended thermal cycling. A custom test setup was developed to evaluate sensor accuracy and robustness under steady-state and transient conditions. Substrate screening identified HG-1 ceramic-coated stainless steel as the most effective platform, offering strong adhesion and low resistance. Furthermore, electric field-assisted sintering (EFAS) was employed to embed the sensors into stainless steel 316L matrices without degrading their functionality. Post-embedding electrical tests confirmed sensor integrity, and initial characterization suggests strong potential for in-situ monitoring. This work provides a scalable strategy for integrating high-performance temperature sensors directly into refractory components, advancing embedded SHM technologies for harsh operating environments.

36 - MATERIALS SCIENCE↗

Synthesis, Characterization, and Testing of High-Lithium-Density Composite Breeders

Solid tritium breeder materials must first and foremost have sufficiently high concentrations of lithium to enable a plant-scale tritium breeding ratio greater than 1:1. However, in addition to lithium content, such breeder materials must also meet other performance metrics including high tritium release rates, thermal conductivities, and irradiation damage tolerance. Perhaps most importantly, tritium breeders must maintain their mechanical integrity during reactor operation so as to avoid degradation which can jeopardize the functionality of the tritium breeder blanket module, which in most designs takes the form of a pebble bed geometry. Unfortunately, the mechanical robustness of most lithium-bearing ceramics under investigation for fusion applications is often inversely related to the lithium atom density. For example, a material such as lithium oxide (Li2O), which has one of the highest lithium atom densities, has a much lower mechanical splitting strength than lithium metatitanate (Li2TiO3), though Li2TiO3 has less than half the lithium atom density of Li2O. This work seeks to provide an alternative to monolithic ceramic tritium breeders, in the form of metal-reinforced composite tritium breeders. Specifically, composite tritium breeders have been synthesized combining Li2O with various ferrous metal reinforcements via electric field assisted sintering (EFAS), also known as spark plasma sintering (SPS). As the metal reinforcement content is increased, metallic networks are observed, via electron microscopy and X-ray computed tomography, to form throughout the composite material. Through destructive mechanical testing, even dilute metal reinforcement loading enables drastic mechanical strength improvements over pure Li2O while higher loadings give rise to quasi-ductile behavior and higher ultimate strengths than Li2TiO3 – while still maintaining a higher density of lithium atoms than Li2TiO3 and many other breeder candidates. In addition to microstructural characterization and mechanical testing, thermal property measurements and hydrogen permeability testing are underway to further assess the suitability of such composites for fusion reactor applications.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Electrochemical grand potential-based phase-field simulation of electric field-assisted sintering

Here, an electrochemical grand potential functional was proposed to describe the sintering of an ionic ceramic green body. The resultant phase-field description enables simulation of the consolidation of an arbitrary number of granular particles and their interactions with the surrounding void phase. The model includes the effects of charged vacancies and the associated interactions between internal and applied electric fields. Defect segregation to grain boundaries is also accounted for, as well as enhanced interfacial defect mobilities. The model was parameterized for Y 2 O 3 . Simulations of two-particle systems showed that the applied electric field had an increasingly important impact on neck growth as particle size increased. A sudden rapid increase in temperature occurred for larger field strengths, which has been reported to be correlated to the onset of a flash event in flash sintering. Simulations of many particles showed that internal heat generation by Joule heating was localized at particle–particle contacts (grain boundaries), even though their conductivities were lower than nearby internal particle-void interfaces. A percolative path for ionic charge across the green body and the ceramic sintered solid was thus defined, accelerating the Joule heating process as the porosity of the green body is removed.

36 MATERIALS SCIENCE↗