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All sourcesNASA NTRSDOE OSTI
NASA NTRSDate not supplied

The Influence of Yttria Content on the Thermal Stability of Yttria-Stabilized Zirconia Aerogels

Aerogels demonstrate extraordinarily low thermal conductivity and low density, presenting a promising form of lightweight insulation for aerospace applications. The primary challenge is stabilization of the highly porous structure at temperatures to 1200 °C. Upon collapse of the pore structure, the favorable thermal properties and low density are diminished. Yttria-stabilized zirconia (YSZ) aerogels are synthesized to investigate the effect of composition on morphology, phase behavior, and thermal stability (specific surface area, pore size distribution). This work demonstrates the improvement in thermal stability of zirconia aerogels with increased yttria content. To develop insight on the influence of structure on thermal stability, the effects of water content and solids loading are studied and in elucidation of the mechanism by which yttria stabilizes the pore structure. With an improved understanding of aerogel structure and performance, metal oxide aerogels can be developed to withstand the extreme environments of space exploration.

Nathaniel Olson↗
DOE OSTI2021

Material transfers detection with seismic observations

We are exploring the use of data from a seismic network around a research nuclear reactor and isotope production facility at Oak Ridge National Laboratory to study activity patterns related to the transfer of nuclear material. A sensor network with eight seismometers was installed around the High Flux Isotope Reactor and the Radiochemical Engineering Development Center and started operating in October 2019. These data are used to detect and characterize operational events around facility. We are using those data to extract signals related to the movement of vehicles involved in the transport of nuclear materials (e.g., transportation of reactor fuel, targets, and product isotopes). Large vehicles produce mechanical energy that can be observed as seismic signals, either as the result of sound emanating from the vehicle engine or by the generation of surface waves as a response of the ground to the load of the vehicles. In particular, the station located near the entrance gate of the facility displays a clear seismic signature as vehicles cross a metal platform on the ground. This signal is characterized by sharp energy bursts that correspond to the number of axles on the vehicle. We developed and are testing an algorithm to identify sequences of energy bursts to count and characterize vehicles of different sizes. We are also exploring the use of seismic polarization analysis to measure the degree of polarization of the observed signals. These two techniques for detection and characterization of vehicles used for nuclear material transfers will be validated with seismic data from a targeted collection using different vehicles and routes similar to the ones used in real-life scenarios at the High Flux Isotope Reactor.

Marcillo, Omar↗
NASA NTRS2001

Creep-Fatigue Interaction Testing

Fatigue fives in metals are nominally time independent below 0.5 T(sub Melt). At higher temperatures, fatigue lives are altered due to time-dependent, thermally activated creep. Conversely, creep rates are altered by super. imposed fatigue loading. Creep and fatigue generally interact synergistically to reduce material lifetime. Their interaction, therefore, is of importance to structural durability of high-temperature structures such as nuclear reactors, reusable rocket engines, gas turbine engines, terrestrial steam turbines, pressure vessel and piping components, casting dies, molds for plastics, and pollution control devices. Safety and lifecycle costs force designers to quantify these interactions. Analytical and experimental approaches to creep-fatigue began in the era following World War II. In this article experimental and life prediction approaches are reviewed for assessing creep-fatigue interactions of metallic materials. Mechanistic models are also discussed briefly.

Halford, Gary R.↗
DOE OSTI2020

Role of the metal-support interface in the hydrodeoxygenation reaction of phenol

In this paper, the effect of interfacial sites between Pd particles and Nb 2 O 5 species is investigated by testing a series of Pd-Nb 2 O 5 /SiO 2 catalysts with different niobium loadings for the HDO reaction of phenol in the gas phase. Important differences in the selectivity to deoxygenated product were observed depending on the presence of niobium oxide close to Pd particles, which reveals the key role of the type of active phase in the control of reaction steps. It was found that Pd/SiO 2 catalyst promotes hydrogenation pathways, producing cyclohexanone as the major product. For Pd-Nb 2 O 5 /SiO 2 catalyst containing a Nb/Pd molar ratio of 0.5, a sharp increase in the selectivity to benzene is observed (7.5-fold). Increasing the Nb/Pd molar ratio, the formation of benzene is enhanced. The results showed that the Pd-Nb 2 O 5 interface, composed by an oxophilic oxide in the perimeter of the metal particle, is responsible for the activation of the Csingle bondO bond, promoting the deoxygenation reaction.

09 BIOMASS FUELS↗
DOE OSTI2019

A Reactive Element Approach to Improve Fracture Healing in Metallic Systems

Self-healing materials demonstrate the ability to close fractures and regain mechanical integrity after a catastrophic failure. However, self-healing in metals can be inhibited by the natural tendency for technologically-relevant metallic systems to oxidize on the crack surface. This study seeks to provide a thermodynamically-based mechanism to enhance healing capability at a solid/liquid interface through alloys designed with a reactive element alloying addition possessing a lower free energy of oxide formation than the parent element. In this study, model Sb-Cu and Sb-Zn systems enable comparisons between mechanistic behaviors based only on thermodynamic reactivity. Mechanical and microstructural investigation demonstrated that the more reactive alloying addition resulted in more effective bonding through increasing bond area and load-bearing capacity of the system. The improved bonding was attributed to improved wetting and reduction of the passivating surface oxide across an interface. The work has potential to advance self-healing capabilities in metallic systems through more appropriate alloy selection to enable improved healing.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Anion exchange and extraction chromatography tandem column isolation of zirconium-89 ( 89 Zr) from cyclotron bombarded targets using an automated fluidic platform

The long-lived positron emitter 89 Zr is a highly promising nuclide employed in diagnostic Positron Emission Tomography (PET) imaging. Methods of radiochemical processing to obtain 89 Zr for clinical use are traditionally performed with a single hydroxamate resin column. In this work, we present a tandem column purification method for the preparation of high-purity 89 Zr from cyclotron bombarded Y metal foils. The primary column is a macroporous, strongly basic anion exchange resin on styrene divinylbenzene co-polymer. The secondary microcolumn, with an internal volume of 33 µL, is packed with an extraction chromatography resin (ExCR) loaded with HDEHP. A condition of “inverted selectivity” is presented, wherein the 89 Zr elution from the primary column is synonymous with the load condition on the secondary column. The ability to transfer 89 Zr from one column to the next allows two sequential column clean-up methods to be performed prior to the final elution of the 89 Zr product. This approach assures delivery of very high purity 89 Zr . The tandem column purification process has been implemented into a prototype automated fluidic system. Optimization of the method is presented, followed by evaluation of the process using seven cyclotron bombarded Y metal foil targets. Once optimized, we found that 93.7±2.3% of the 89 Zr present in the foils was recovered in the secondary column elution fraction (0.8 M oxalic acid). Radiochromatograms of the product elution peaks enabled determination of full width at half-maximum (FWHM) and 89 Zr collection yields as a function of volume. Because of the small size of the secondary microcolumn, a 89 Zr product volume of ~0.28 mL is reported, which provides a substantially increased nuclide concentration over traditional methods. Finally, we evaluated the transchelation of the resulting 89 Zr oxalate product to deferoxamine mesylate (DFOM) salt. We observed effective specific activities (ESA) and bindable metals concentrations ([M B ]) that exceed those reported by the traditional single hydroxamate column method.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2017

Development of advanced high porosity wicks for the high temperature heat pipes of concentrating solar power

Sandia National Laboratories and Heat Pipes Laboratory of National Technical University of Ukraine «KPI» have developed several methods of improving robustness of the high-temperature heat pipe wick for their application to concentrating solar power systems with Stirling engine. In this case the wick structures must retain high heat pipe performance with robustness for long-term operation. Recent modeling indicates that wicks based on various fiber combinations could provide the robustness combined with sufficient performance. Results of the development, characterization, modeling, and testing of advanced felt metal wicks that addresses durability issues while maintaining sufficient performance are showed in this paper. The project resulted in an ongoing durability bench-scale heat pipe that simulates wick load conditions required for 80kWth throughput solar receiver, including periodic non-destructive evaluation of the wick durability. Two mock-ups of high-temperature heat pipes were made for long life and performance tests: the first sample with wick based on 12 μm fibers; and the second with hybrid wick based on 30 μm fibers and 6.5 μm fibers. Finally, the second heat pipe operation has continued unattended at 775 °C vapor temperature for nearly 13,600 h, with no observable loss of performance or change in startup characteristics.

42 ENGINEERING↗
NASA NTRS1943

Some Investigations of the General Instability of Stiffened Metal Cylinders IV : Continuation of Tests of Sheet-covered Specimens and Studies of the Buckling Phenomena of Unstiffened Circular Cylinders

This is the fourth of a series of reports covering an investigation of the general instability problem by the California Institute of Technology. The first five reports of this series cover investigations of the general instability problem under the loading conditions of pure bending and were prepared under the sponsorship of the Civil Aeronautics Administration. The succeeding reports of this series cover the work done on other loading conditions under the sponsorship of the National Advisory Committee for Aeronautics. This report is to deal primarily with the continuation of tests of sheet-covered specimens and studies of the buckling phenomena of unstiffened circular cylinders.

CYLINDERS, STEEL↗
DOE OSTI2016

Performance assessment of dilute-acid leaching to improve corn stover quality for thermochemical conversion

Lignocellulosic biomass is a sustainable energy source that can help meet the increasing demand for biofuels in the United States. However, the quality and availability of such feedstocks greatly affects their suitability for downstream conversion. This work reports the effects of dilute-acid leaching at various solid loadings, temperatures and acid loadings on the quality of a traditional biochemical feedstock, corn stover, as a potential feedstock for thermochemical conversions. At 5 wt% solids, dilute-acid leaching was observed to effectively remove 97.3% of the alkali metals and alkaline earth metals that can negatively affect degradation pathways during pyrolysis and result in greater yield of non-condensable gases. In addition, up to 98.4% of the chlorine and 88.8% of the phosphorus, which can cause equipment corrosion and foul upgrading catalysts, respectively, were removed. At 25°C in the absence of acid, only 6.8% of the alkali metals and alkaline earth metals were removed; however 88.0% of chloride was still removed. The ratio of alkaline/acidic ash species has been suggested to proportionately relate to slagging in biopower applications. The initial alkali/acid ratio of the ash species present in the untreated corn stover was 0.38 (significant slagging risk). At 5 wt% solids, this ratio was decreased to 0.18 (moderate slagging risk) at 0 wt% acid and 90°C, and was decreased to 0.07, 0.08 and 0.06 at 0.5 wt% acid at 25°C, 50°C and 90°C, respectively (little or no slagging risk). Increasing the acid loading to 1.0% only slightly decreased the measured alkali/acid ratio of remaining ash species. Lastly, the results presented here show that a water wash or dilute-acid preprocessing step can improve corn stover quality for pyrolysis, hydrothermal liquefaction and biopower.

09 BIOMASS FUELS↗
DOE OSTI2020

A Hybrid AI/ML and Computational Mechanics Based Approach for Time-Series State and Fatigue Life Estimation of Nuclear Reactor Components

Environmental fatigue modeling is a complex problem due to multiple failure modes and their intermixing. The failure modes are function of various underlying causes in addition to the corrosive effect of reactor coolant environment. Some of the major causes are time-dependence of material associated with cyclic loading, load sequence effect associated with random/variable amplitude loading, effect of strain amplitude and rates, effect of varying temperature (along both temporal and spatial directions) and the effect of mean strain and stress. The nonlinear intermixing of failure modes associated with above mentioned causing parameters makes the environmental fatigue modeling is a challenging task. Because of this challenge, fatigue is traditionally being modeled based on experimental data. However, test based empirical approach often requires hundreds of fatigue tests to model the above-mentioned intermixing failure causes even for a single material system. The problem is further exaggerated for reactor component made from multi-material systems such as made from both carbon and stainless-steel base metals and their similar and dissimilar metal welds. With the difficulty of conducting hundreds of fatigue tests to capture the above-mentioned intermixing failure causes, fatigue modeling approaches often depends on empirical models based on limited available test data such as available through ASME code and NUREG 6909. However, these limited test-data-based models may not be enough to accurately predict the life of reactor components. Accurate prediction of life of reactor component would become a necessity, particularly when the license of the reactors to be extended for long-term-operation (LTO) that is for well beyond its original design life of 40 years. The requirement of extending the license of reactor under LTO requires hundreds of fatigue tests to be conducted to understand the mechanism associated with the above-mentioned interdependent failure causes. However, conducting large number of fatigue tests is not a feasibility due to the cost involved. To address this issues Argonne National Laboratory (ANL) with the sponsorship of DOE Light Water Reactor Sustainability (LWRS) program trying to develop a hybrid predictive modeling approach. This is based on limited experiment-data, Artificial-intelligence (AI) – Machine-Learning (ML) - Deep-Learning (DL) based techniques and Multiphysics-computational-mechanics based modeling tools. The hybrid approach not-only can improve the accuracy of the existing stress analysis and fatigue modeling approach but also can reduce the over-dependency on test-based approach. Towards this goal following are some of the major contributions based on ANL’s FY-20 environmental fatigue modeling activities: 1) A cyclic plasticity material model database for 82/182 dissimilar metal weld, which can be readily shared with US nuclear industry and regulatory agency on request. 2) A well validated analytical modeling methodology to perform cycle-by-cycle stress prediction under both constant amplitude fatigue loading and variable amplitude fatigue loading (with load-sequence effect). 3) An AI/ML/DL based methodology to predict unmeasurable cyclic strain based on other available sensor signals. This type of approach can be used for estimating strain in real reactor components from other sensor readings. 4) An AI/ML based approach to improve the US capability on environmental fatigue testing. This is by improving ANL’s existing environmental fatigue testing capacity to conduct ASME required strain-controlled tests (by controlling strain amplitudes and its rate), while not measuring the strain (due to the difficulty of placing an extensometer in a narrow autoclave in a PWR-water-test system). 5) A simulation and experiment based probabilistic modeling methodology for time-series fatigue state and life estimation of reactor metal such as dissimilar metal weld.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2021

Nanoparticle O–H Bond Dissociation Free Energies from Equilibrium Measurements of Cerium Oxide Colloids

A novel equilibrium strategy for measuring the hydrogen atom affinity of colloidal metal oxide nanoparticles is presented. Reactions between oleate-capped cerium oxide nanoparticle colloids (nanoceria) and organic proton-coupled electron transfer (PCET) reagents are used as a model system. Nanoceria redox changes, or hydrogen loadings, and overall reaction stoichiometries were followed by both 1 H NMR and X-ray absorption near-edge spectroscopies. Furthermore, these investigations revealed that, in many cases, reactions between nanoceria and PCET reagents reach equilibrium states with good mass balance. Each equilibrium state is a direct measure of the bond strength, or bond dissociation free energy (BDFE), between nanoceria and hydrogen. Further studies, including those with larger nanoceria, indicated that the relevant bond is a surface O–H. Thus, we have measured surface O–H BDFEs for nanoceria—the first experimental BDFEs for any nanoscale metal oxide. Remarkably, the measured CeO–H BDFEs span 13 kcal mol –1 (0.56 eV) with changes in the average redox state of the nanoceria colloid. Possible chemical models for this strong dependence are discussed. We propose that the tunability of ceria BDFEs may be important in explaining its effectiveness in catalysis. More generally, metal oxide BDFEs have been used as predictors of catalyst efficacy that, traditionally, have only been accessible by computational methods. These results provide important experimental benchmarks for metal oxide BDFEs and demonstrate that the concepts of molecular bond strength thermochemistry can be applied to nanoscale materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1973

In-flight and laboratory vacuum-friction test results

Coefficient of friction measurements were made for six unlubricated metal couples exposed to the space environment aboard the OV-1-13 spacecraft and exposed to laboratory vacuum. Materials studied included mutually soluble, partially soluble, and insoluble metal combinations. Two samples of each material couple were tested in space and in the laboratory using the disk and rider technique. Linear velocity was 0.10 cm/s (2.5 in/min) and rider normal load was 4.45 N (1 lb) for the gold versus silver couples and 8.90 N (2lb) for the other combinations. Results showed that friction data obtained in a clean ion-pumped laboratory vacuum of 10 to the minus 10 power materials with low mutual solubility can be correlated to operation in the vicinity of a typical scientific spacecraft that is exposed to an ambient pressure as low as 10 to the minus 12 power torr. The expected increase in coefficient of friction with solubility was shown. Material couples with high mutual solubility present the hazard of unpredictable drastic friction increase in orbit which may not be evident in laboratory testing at levels down to 10 to the minus 10 power torr. It was also shown that gross cold welding of unlubricated metals exposed to a satellite environment does not occur.

Devine, E. J.↗
NASA NTRS2004

Integrity of Ceramic Parts Predicted When Loads and Temperatures Fluctuate Over Time

Brittle materials are being used, and being considered for use, for a wide variety of high performance applications that operate in harsh environments, including static and rotating turbine parts for unmanned aerial vehicles, auxiliary power units, and distributed power generation. Other applications include thermal protection systems, dental prosthetics, fuel cells, oxygen transport membranes, radomes, and microelectromechanical systems (MEMS). In order for these high-technology ceramics to be used successfully for structural applications that push the envelope of materials capabilities, design engineers must consider that brittle materials are designed and analyzed differently than metallic materials. Unlike ductile metals, brittle materials display a stochastic strength response because of the combination of low fracture toughness and the random nature of the size, orientation, and distribution of inherent microscopic flaws. This plus the fact that the strength of a component under load may degrade over time because of slow crack growth means that a probabilistic-based life-prediction methodology must be used when the tradeoffs of failure probability, performance, and useful life are being optimized. The CARES/Life code (which was developed at the NASA Glenn Research Center) predicts the probability of ceramic components failing from spontaneous catastrophic rupture when these components are subjected to multiaxial loading and slow crack growth conditions. Enhancements to CARES/Life now allow for the component survival probability to be calculated when loading and temperature vary over time.

Nemeth, Noel N.↗
NASA NTRS2024

Hybrid Thermally Efficient Core (HyTEC) HyTEC Phase 1 – Combustor Final Report

The objective of the HyTEC – Combustor Technology project is to develop technology for a compact, low emissions, rich-burn combustor that maintains a high-level of durability. To accomplish this, the combustor will incorporate CMC liners and a CMC Dome to enable improved air utilization for mixing and NOx reduction. In particular, three technology areas were matured: metallic swirler attachment to the CMC dome, Nickel diffusion in CMC, and EBC advancements with improved durability. The maturation of these technology areas is critical to successfully designing a combustor for an engine intended to demonstrate increased thermal efficiency with integrated high-power density-core engine technologies. As part of the project, multiple swirler attachment architectures were matured through the design process, manufactured, and tested in simulated engine conditions. These architectures utilized two different approaches to attachment: a pressure loaded approach and a clamped approach. Each approach required testing at simulated engine conditions to mature the technology. These tests were developed to ensure that the probable failure mechanisms for each architecture were assessed relative to its long-term durability. After successfully testing both approaches, the pressure loaded approach was chosen based on its simplicity and its similarity to the attachment approach used on lean burn combustors. Finally, this successful testing resulted in the swirler attachment technology achieving TRL 4 status. Another aspect of concern with the metallic swirler attachment is the potential for nickel diffusion into the CMC to cause durability shortfalls. A series of tests were completed to understand both the amount of nickel that is expected to diffuse into the CMC and the effect this diffusion will have on mechanical properties of the CMC. After successfully completing this testing, the reduction in local mechanical properties was found to not have an impact on the overall durability of the CMC Dome. To further improve the overall durability, three different EBC coating architectures were also studied. One of these coatings being the current state of the art for CMC liners with the other two being proposed improvements. Coupons were produced using each coating and subjected to a series of laboratory testing. One coating was found to have an overall superior durability in laboratory testing and survived rig testing without indication of degradation. This successful testing resulted in the EBC technology achieving TRL 5 status. Overall, a design approach was successfully down-selected that achieves both the TPM requirements and the need for TRL 4+ status. This design incorporates a pressure loaded swirler attachment with an improved EBC coating (Architecture 1). This combination allows the continued use of a CMC dome and results in an improved durability for the proposed compact core combustor.

CMC↗
DOE OSTI2023

Boosting Hydrogen Evolution in Neutral Medium by Accelerating Water Dissociation with Ru Clusters Loaded on Mo 2 CTx MXene

Abstract Electrocatalytic hydrogen evolution reaction (HER) in mild neutral medium is a compelling goal for environmentally sustainable energy conversion, but its development is greatly limited by slow kinetics. Platinum group noble metals exhibit ultra‐high HER activities, but their scarcity and performance instability restrict wide application. Herein, taking advantage of excellent catalyst carrier properties of 2D‐layered transition metal carbides (MXenes), highly dispersed of Ru clusters anchored on Mo 2 CT x MXene are demonstrated as a superior HER electrocatalyst, which is prepared by a facile in situ reduction strategy. The as‐prepared Ru/Mo 2 CT x catalyst exhibits a very low overpotential of 73 mV to achieve a current density of −10 mA cm −2 and Tafel slope of 57 mV dec −1 in neutral medium, surpassing performance of most previously reported MXene‐based catalysts. In addition, Ru/Mo 2 CT x catalyst also presents superior stability compared to commercial Pt/C. Experimental results and theoretical calculations indicate that the interaction between Ru clusters modulates the electronic structure of active sites and promotes H 2 O dissociation and hydrogen desorption.

Wu, Yanze↗
NASA NTRS1979

Composite components under impact load and effects of defects on the loading capacity

Investigations were carried out on a horizontal tail assembly made of carbon fiber reinforced plastic for the Alpha Jet. The possibility of obtaining a leading edge nose design lighter but not more expensive than a metal version was studied. An important consideration was sufficient resistance of the leading edge against impact of stones and hailstones combined with high degree of stiffness. The improvement of energy reception characteristics of the materials through suitable laminate design was considered. Since certain defects occur in structural components, the effects of such defects on the characteristics of the parts were also studied.

Aoki, R.↗
NASA NTRS1981

Nonlinear laminate analysis for metal matrix fiber composites

A nonlinear laminate analysis is described for predicting the mechanical behavior (stress-strain relationships) of angleplied laminates in which the matrix is strained nonlinearly by both the residual stress and the mechanical load and in which additional nonlinearities are induced due to progressive fiber fractures and ply relative rotations. The nonlinear laminate analysis (NLA) is based on linear composite mechanics and a piece wise linear laminate analysis to handle the nonlinear responses. Results obtained by using this nonlinear analysis on boron fiber/aluminum matrix angleplied laminates agree well with experimental data. The results shown illustrate the in situ ply stress-strain behavior and synergistic strength enhancement.

Chamis, C. C.↗