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DOE OSTI2020

Manufacturing control systems and logic for prognosis of defects in composite materials

Presented are manufacturing control systems for composite-material structures, methods for assembling/operating such systems, and transfer molding techniques for predicting and ameliorating void conditions in fiber-reinforced polymer panels. A method for forming a composite-material construction includes receiving a start signal indicating a fiber-based preform is inside a mold cavity, and transmitting a command signal to inject pressurized resin into the mold to induce resin flow within the mold cavity and impregnate the fiber-based preform. An electronic controller receives, from a distributed array of sensors attached to the mold, signals indicative of pressure and/or temperature at discrete locations on an interior face of the mold cavity. The controller determines a measurement deviation between a calibrated baseline value and the pressure and/or temperature values for each of the discrete locations. If any one of the respective measurement deviations exceeds a calibrated threshold, a void signal is generated to flag a detected void condition.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Providing Experimental Infrastructure for Accelerating Advanced Reactor Demonstrations through the National Reactor Innovation Center

A suite of experimental infrastructure projects has been developed by the National Reactor Innovation Center to accelerate advanced reactor demonstrations and facilitate their development, addressing crucial gaps in data, materials characterization, and modeling. First, the Molten Salt Thermophysical Examination Capability (MSTEC) provides a specialized platform for post-irradiation characterization of molten salt reactor fuel, coolant salts, and structural materials, essential for supporting the design and operation of advanced reactors and future commercial molten salt reactor development and licensing. The Virtual Test Bed (VTB) complements these efforts by leveraging advanced modeling and simulation tools to evaluate reactor performance and safety. Serving as a library of reference models, the VTB offers a database of multiphysics reactor models, facilitating rapid safety evaluations and includes continuous software quality assurance, crucial for accelerating deployment while maintaining reliability. Additionally, the Helium Component Test Facility (HeCTF) addresses the need for high-temperature helium-cooled reactor component testing. As the first-of-its-kind facility in the United States, HeCTF emulates high-temperature gas reactor conditions, reducing time and cost associated with component validation, thereby accelerating reactor development. Finally, In-cell Thermal Creep Frames provide a unique solution for obtaining thermal creep data from irradiated materials, critical for materials qualification and licensing. Developed by the National Reactor Innovation Center, these compact frames enable the examination of previously irradiated materials, overcoming traditional limitations and enhancing the understanding of mechanical properties crucial for reactor development. Collectively, these experimental infrastructure projects form a comprehensive framework aimed at expediting advanced reactor demonstrations, fostering innovation, and ensuring the viability of next-generation nuclear energy solutions.

22 - GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2020

Resiliency of Degraded Built Infrastructure

Infrastructure resiliency depends on the ability of infrastructure systems to withstand, adapt, and recover from chronic and extreme stresses. In this white paper, we address the resiliency of infrastructure assets and discuss improving infrastructure stability through development of our understanding of cement and concrete degradation. The resiliency of infrastructure during extreme events relies on the condition, adaptability, and recoverability of built infrastructure (roads, bridges, dams), which serves as the backbone of existing infrastructure systems. Much of the built infrastructure in the US has consistently been rated D+ by the American Society of Civil Engineers (ASCE). Aged infrastructure introduces risk to the system, since unreliable infrastructure increases the likelihood of failures under chronic and extreme stress and are particularly concerning when extreme events occur. To understand and account for this added risk from poor infrastructure quality, more research is needed on (i) how the changing environment alters the aging of new and existing built infrastructure and (ii) how degradation causes unique failure mechanisms. The aging of built infrastructure is based on degradation of the structural materials, such as concrete and steel supports, which causes failure. Current work in cement/concrete degradation is based on (i) the development of high strength and degradation resistance concrete mixtures, (ii) methods of assessing the age and reliability of existing structures, and (3) modeling of structural stability and the microstructural evolution of concrete/cement from degradation mechanisms (sulfide attack, carbonation, decalcification). Sandia National Laboratories (SNL) has made several investments in studying the durability and degradation of cement based materials, including using SNL-developed codes and methodologies (peridynamics, PFLOTRAN) to focus on chemo-mechanical fracture of cement for energy applications. Additionally, a recent collaboration with the University of Colorado Boulder has included fracture of concrete gravity dams, scaling the existing work to applications in full sized infrastructure problems. Ultimately, SNL has the experience in degradation of cementitious materials to extend the current research portfolio and answer concerns about the resilience of aging built infrastructure.

36 MATERIALS SCIENCE↗

DOE OSTI2024

High-Throughput Microstructural Characterization and Process Correlation Using Automated Electron Backscatter Diffraction

The need to optimize the processing conditions of additively manufactured (AM) metals and alloys has driven advances in throughput capabilities for material property measurements such as tensile strength or hardness. High-throughput (HT) characterization of AM metal microstructure has fallen significantly behind the pace of property measurements due to intrinsic bottlenecks associated with the artisan and labor-intensive preparation methods required to produce highly polished surfaces. This inequality in data throughput has led to a reliance on heuristics to connect process to structure or structure to properties for AM structural materials. In this study, we show a transformative approach to achieve laser powder bed fusion (LPBF) printing, HT preparation using dry electropolishing and HT electron backscatter diffraction (EBSD). This approach was used to construct a library of > 600 experimental EBSD sample sets spanning a diverse range of LPBF process conditions for AM Kovar. This vast library is far more expansive in parameter space than most state-of-the-art studies, yet it required only approximately 10 labor hours to acquire. Build geometries, surface preparation methods, and microscopy details, as well as the entire library of >600 EBSD data sets over the two sample design versions, have been shared with intent for the materials community to leverage the data and further advance the approach. Using this library, we investigated process–structure relationships and uncovered an unexpected, strong dependence of microstructure on location within the build, when varied, using otherwise identical laser parameters.

Characterization and Analytical Technique↗

DOE OSTI2024

Bayesian Conavigation: Dynamic Designing of the Material Digital Twins via Active Learning

Scientific advancement is universally based on the dynamic interplay between theoretical insights, modeling, and experimental discoveries. However, this feedback loop is often slow, including delayed community interactions and the gradual integration of experimental data into theoretical frameworks. This challenge is particularly exacerbated in domains dealing with high-dimensional object spaces, such as molecules and complex microstructures. Hence, the integration of theory within automated and autonomous experimental setups, or theory in the loop-automated experiment, is emerging as a crucial objective for accelerating scientific research. The critical aspect is to use not only theory but also on-the-fly theory updates during the experiment. Furthermore, we introduce a method for integrating theory into the loop through Bayesian conavigation of theoretical model space and experimentation. Our approach leverages the concurrent development of surrogate models for both simulation and experimental domains at the rates determined by latencies and costs of experiments and computation, alongside the adjustment of control parameters within theoretical models to minimize epistemic uncertainty over the experimental object spaces. This methodology facilitates the creation of digital twins of material structures, encompassing both the surrogate model of behavior that includes the correlative part and the theoretical model itself. While being demonstrated here within the context of functional responses in ferroelectric materials, our approach holds promise for broader applications, such as the exploration of optical properties in nanoclusters, microstructure-dependent properties in complex materials, and properties of molecular systems.

Microscopy↗

DOE OSTI2021

Iridium metallene oxide for acidic oxygen evolution catalysis

Exploring new materials is essential in the field of material science. Especially, searching for optimal materials with utmost atomic utilization, ideal activities and desirable stability for catalytic applications requires smart design of materials’ structures. Herein, we report iridium metallene oxide: 1 T phase-iridium dioxide (IrO 2 ) by a synthetic strategy combining mechanochemistry and thermal treatment in a strong alkaline medium. This material demonstrates high activity for oxygen evolution reaction with a low overpotential of 197 millivolt in acidic electrolyte at 10 milliamperes per geometric square centimeter (mA cm geo –2 ). Together, it achieves high turnover frequencies of 4.2 s UPD –1 (3.0 s BET –1 ) at 1.50 V vs. reversible hydrogen electrode. Furthermore, 1T-IrO 2 also shows little degradation after 126 hours chronopotentiometry measurement under the high current density of 250 mA cm geo –2 in proton exchange membrane device. Theoretical calculations reveal that the active site of Ir in 1T-IrO 2 provides an optimal free energy uphill in *OH formation, leading to the enhanced performance. The discovery of this 1T-metallene oxide material will provide new opportunities for catalysis and other applications.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Report on the Update and Codification of Expert Knowledge into ASTM Standard Practice E521

The overall purpose of the Grand Challenge Integrated Research Project (IRP), Accelerating the Qualification of Materials to Enable Rapid Deployment of Advanced Reactors, is to fulfill several objectives. The first objective is to complete and demonstrate/establish the process for predicting the microstructure and properties of structural materials in reactor and at high doses using ion irradiation as an accurate predictive tool for assessing behavior under reactor irradiation. The second objective is for this process to be adopted as part of an ASTM standard, and to work with the US Nuclear Regulatory Commission to utilize this standard in licensing decisions on advanced reactor designs for which such data are nonexistent or impractical to achieve. The need for standardized procedures is apparent based on the outcomes of a recent round-robin experiment from laboratories using ion beams for radiation damage studies and the roadmap for ion beam technologies to address challenges for the advancement of nuclear energy technologies.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2026

Report on the Update and Codification of Expert Knowledge into ASTM Standard Practice E521

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

NASA NTRS2015

Low-Cost, High-Performance Combustion Chamber

Ultramet designed and fabricated a lightweight, high-temperature combustion chamber for use with cryogenic LOX/CH4 propellants that can deliver a specific impulse of approx.355 seconds. This increase over the current 320-second baseline of nitrogen tetroxide/monomethylhydrazine (NTO/MMH) will result in a propellant mass decrease of 55 lb for a typical lunar mission. The material system was based on Ultramet's proven oxide-iridium/rhenium architecture, which has been hot-fire tested with stoichiometric oxygen/hydrogen for hours. Instead of rhenium, however, the structural material was a niobium or tantalum alloy that has excellent yield strength at both ambient and elevated temperatures. Phase I demonstrated alloys with yield strength-to-weight ratios more than three times that of rhenium, which will significantly reduce chamber weight. The starting materials were also two orders of magnitude less expensive than rhenium and were less expensive than the C103 niobium alloy commonly used in low-performance engines. Phase II focused on the design, fabrication, and hot-fire testing of a 12-lbf thrust class chamber with LOX/CH4, and a 100-lbf chamber for LOX/CH4. A 5-lbf chamber for NTO/MMH also was designed and fabricated.

Fortini, Arthur J.↗

DOE OSTI2021

Resin transfer molding systems and control logic for manufacturing fiber-reinforced composite parts

Presented are manufacturing control systems for fabricating composite-material structures, methods for making/operating such systems, and resin transfer molding techniques for ameliorating race-tracking effects in fiber-reinforced polymer panels. A method for forming a composite-material construction includes confirming, via a system electronic control unit (ECU), that a fiber-based preform is placed in a mold cavity and that opposing mold segments of the molding apparatus are sealed together. A filler, such as a compressible bladder, a cluster of spring-biased pins, or a spray-chopped fiber bed, is introduced into a void between the fiber-based preform and a tool face of one mold segment to thereby eliminate an unwanted resin race track. The system ECU commands a resin pump to inject resin through a primary gate of the molding apparatus and into the mold cavity to thereby impregnate the fiber-based preform with the resin. One or more vents operate to evacuate air from the mold.

Rodgers, William R.↗

DOE OSTI2025

Non-destructive structural characterization of graphite components using mechanical resonance and deep learning

As compared to conventional nuclear reactors, microreactors have the potential to significantly reduce construction timelines and capital costs, decreasing the barriers for advanced nuclear reactor technologies. However, the lower power output of these microreactors (typically < 20 MWe) creates challenging economics if operation and maintenance costs cannot be sufficiently reduced. The compact size of these designs presents an opportunity for comprehensive in-situ structural health monitoring to provide real-time feedback in order to reduce operational costs associated with maintenance and downtime. Many microreactor concepts use graphite for both in-core neutron moderation and as a structural material, which has typically required some form of periodic and laborious inspection. This report provides a description and assessment of recent work with graphite to couple acoustic-based experimental measurements and characterization with machine learning models to mature structural health monitoring capabilities and generate benefits for the nuclear microreactor industry. With resilient embedded sensors in development in other programs funded by the US Department of Energy’s Office of Nuclear Energy and elsewhere, the work described herein builds upon previously funded efforts to mature non-destructive testing technology that relates measured vibrational signatures to structural changes, using a combination of new experimental measurements and machine learning processing. Building on past successful demonstrations of predictive workflows to identify structural changes in a hexagonal stainless steel test article with excellent acoustic propagation, we first performed baseline characterization on graphite samples with canonical geometries to ensure compatibility and confidence in the applied techniques for a material with distinctly different mechanical properties. In contrast to efforts in previous years, we worked exclusively with unidirectional vibration data that is more comparable to those expected from the existing embedded sensor technologies which are suitable for deployment in a reactor setting. Established acoustic and modern machine-learning-based characterization approaches were applied to the resulting datasets from these simple geometries. Both approaches were found to be highly capable of detecting even small geometric irregularities amongst nominally identical samples. As such, we then moved to testing these approaches for detection of artificial local stress perturbations introduced into a more complex geometry: a hexagonal block with drilled holes. A main outcome of this work is that a generalizable ML workflow can be used to detect and predict the characteristics of small artificial anomalies in a graphite component with a relevant geometry. While this work was performed using surficial vibration data, we expect the approach to be flexible and viable for other monitoring scenarios, such as those with different arrangements or types of sensor arrays. As compared to previously funded efforts, an existing ML workflow based on neural networks was enhanced through the addition of recently developed Fourier neural operators. As applied to previously collected and new vibration datasets, prediction accuracies of anomaly characterizations were greatly improved with minimal added computational cost. As trained on small durations of vibration data (tens of seconds) collected over a realistic number of locations, the model was able to reliably determine the presence of a subtle stress anomaly and begin to provide location estimates. Such an approach is likely to be viable for more relevant reactor damage scenarios for graphite components, such as progressive crack growth or creep.

36 MATERIALS SCIENCE↗

NASA NTRS2025

High-density Boron Nitride Nanotube Composites via Surfactant-stabilized Lyotropic Liquid Crystals for Enhanced Space Radiation Shielding

Despite significant technological advancements in space exploration, human space travel and colonization remain limited by the health risks associated with space radiation. Boron nitride nanotubes (BNNTs) have been proposed as an advanced material for space applications due to their high specific strength and efficient radiation shielding capabilities. However, the practical implementation of BNNTs has been slow, primarily due to technological challenges in fabricating structural materials incorporating BNNTs. In this study, a method is presented for fabricating high-density BNNT films that are mechanically robust, exhibit high thermal conductivity, and effectively attenuate space radiation. The key advancement enabling high-density BNNT films is the successful preparation of BNNT liquid crystals (LCs), achieved through the strategic use of a commercial dodecylbenzenesulfonic acid surfactant. This surfactant ensures exceptional BNNT stability in aqueous dispersion, even at concentrations exceeding the LC phase transition threshold. Simulations, estimating the equivalent radiation dose to the human body in space, indicate that a high-density BNNT film with a surface density of 50 g cm−2 reduces the total dose equivalent rate by 56% compared to zero shielding. This enhancement would allow astronauts to extend their mission duration on the lunar surface by a factor of two.

Young-Kyeong Kim↗

DOE OSTI2021

Revealing the chemical environment of Cr, Fe, and Ni in high temperature-ultrafine precipitate strengthened steel subjected to low fluence neutron irradiation

High-temperature ultrafine-precipitate-strengthened (HT-UPS) steel has potential applications in advanced nuclear reactors as a structural material. However, little is currently known about its response to neutron irradiation. This research provides insight into the neutron irradiation-induced physicochemical changes of the major constituents in HT-UPS steels, including Fe, Cr, and Ni, using synchrotron X-ray absorption near edge structure (XANES) and diffraction. This study is the first known investigation using XANES to characterize HT-UPS steel to analyze the evolution of the atomic level chemistry. It was found that following irradiation, nucleation, ballistic dispersion, and/or coarsening of Cr 23 C 6 precipitates occurred at very low neutron irradiation fluences, from 0.003 displacements per atom (dpa) up to 0.3 dpa, at ~600°C, which were at least an order of magnitude lower than previous studies. Calculations of the angular momentum projections, partial density of states, and the XANES spectra confirmed the experimental findings of the Cr 23 C 6 precipitate evolution. In contrast, the local atomic structure around Fe and Ni atoms demonstrated irradiation resistance.

36 MATERIALS SCIENCE↗

NASA NTRS1976

Structural design of space telescope

Problematic areas are discussed relative to the design of the NASA Large Space Telescope with a view toward showing how these areas are currently being treated so that the primary goals of the program can be met. The discussion covers basic mission, design parameters, metering structural material, and measurements of thermal expansion coefficient and scale testing. Since the test program has not been completed, there are so far no data available to show comparison between the baseline metering structure design and test. However, graphite-epoxy appears very favorable for structural uses, where precise alignment is necessary and a high degree of thermal stability is desired. It is anticipated that there will be a convergence on a straightforward method of arranging the basic structure for the ease of manufacturing and cost savings.

Arnts, G. W., Jr.↗

NASA NTRS1980

Experimental investigation of graphite/polyimide sandwich panels in edgewise compression

The local and general buckling behavior of graphite/polyimide sandwich panels simply supported along all four edges and loaded in uniaxial edgewise compression was investigated. Material properties of adhesive and facings were determined from flatwise tension and sandwich beam flexure tests. Tensile and compressive material properties of the facings were determined at 116, R.T., and 589 K (-250, R.T., and 600 F) using the sandwich beam flexure test method. Results indicate that Gr/PI is a usable structural material for short term use at temperatures as high as 589 K (600 F). Buckling specimens were 30.5 X 33.0 cm (12 x 13 in.), had quasi-isotropic symmetric facings and a glass/polyimide honeycomb core. Core thicknesses varied and three panels of each thickness were tested in edgewise compression at room temperature to investigate failure modes and corresponding buckling formulas. Specimens 0.635 cm (0.25 in.) thick failed by overall buckling at loads close to the analytically predicted buckling load; all other panels failed by face wrinkling. Results of the winkling tests indicate that several buckling formulas were unconservative and therefore not suitable for design purposes; recommended wrinkling equations are presented.

Camarda, C. J.↗

NASA NTRS1991

Advanced technologies for rocket single-stage-to-orbit vehicles

A single-stage-to-orbit vertical takeoff/horizontal landing rocket vehicle was studied to determine the benefits of advanced technology. Advanced technologies that were included in the study were variable mixture ratio oxygen/hydrogen rocket engines and materials, structures, and subsystem technologies currently being developed in the National Aero-Space Plane Program. The application of advanced technology results in an 85 percent reduction in vehicle dry weight. With advanced materials, an external thermal protection system, like the Space Shuttle tiles, was not required. Compared to an all-airbreathing horizontal takeoff/horizontal landing vehicle using the same advanced technologies and mission requirements, the rocket vehicle is lighter in dry weight and has fewer subsystems. To increase reliability and safety, operational features were included in the rocket vehicle-robust subsystems, 5 percent additional margin, no slush hydrogen, fail-operational with an engine out, and a crew escape module. The resulting vehicle grew in dry weight and was still lower in dry weight than the airbreathing vehicle.

Wilhite, Alan W.↗

NASA NTRS2003

Mechanical Properties of Triaxial Braided Carbon/Epoxy Composites

In an on-going effort to increase the safety and efficiency of turbine engines, the National Aeronautics and Space Administration is exploring lightweight alternatives to the metal containment structures that currently encase commercial jet engines. Epoxy reinforced with braided carbon fibers is a candidate structural material which may be suitable for an engine case. This paper reports flat-coupon mechanical-property experiments performed to compliment previously reported subcomponent impact testing and analytical simulation of containment structures. Triaxial-braid T700/5208 epoxy and triaxial-braid T700h436 toughened epoxy composites were evaluated. Also, two triaxial-braid architectures (0 degrees plus or minus 60 degrees, and 0 degrees plus or minus 45 degrees) with the M36 resin were evaluated through tension, compression, and shear testing. Tensile behavior was compared between standard straight-sided specimens (ASTM D3039) and bow-tie specimens. Both double-notch shear (ASTM D3846) and Iosepescu (ASTM D5379) tests were performed as well. The M36/O degrees plus or minus 45 degrees configuration yield the best response when measurements were made parallel to the axial tows. Conversely, the M36/0 degrees plus or minus 60 degrees configuration was best when measurements were made perpendicular to the axial tows. The results were used to identify critical properties and to augment the analysis of impact experiments.

Bowman, C. L.↗

NASA NTRS2003

Mechanical Properties of Triaxial Braided Carbon/Epoxy Composites

In an on-going effort to increase the safety and efficiency of turbine engines, the National Aeronautics and Space Administration is exploring lightweight alternatives to the metal containment structures that currently encase commercial jet engines. Epoxy reinforced with braided carbon fibers is a candidate structural material which may be suitable for an engine case. This paper reports flat-coupon mechanical-property experiments performed to compliment previously reported subcomponent impact testing and analytical simulation of containment structures. Triaxial-braid T700/5208 epoxy and triaxial-braid T700/M36 toughened epoxy composites were evaluated. Also, two triaxial-braid architectures (0 +/- 60 deg., 0 +/- 45 deg.) with the M36 resin were evaluated through tension, compression, and shear testing. Tensile behavior was compared between standard straight-sided specimens (ASTM D3039) and bowtie specimens. Both double-notch shear (ASTM D3846) and Iosepescu (ASTM D5379) tests were performed as well. The M36/0 +/- 45 deg. configuration yield the best response when measurements were made parallel to the axial tows. Conversely, the M36/0 +/- 60 deg. configuration was best when measurements were made perpendicular to the axial tows. The results were used to identify critical properties and to augment the analysis of impact experiments.

Bowman, C. L.↗