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NASA NTRS2012

Sources of Sulfate Found in Mounds and Lakes at the Lewis Cliffs Ice Tongue, Transantarctic

Massive but highly localized Na-sulfate mounds (mirabilite, Na2SO4.10H2O) have been found at the terminal moraine of the Lewis Cliffs Ice Tongue (LCIT), Antarctica. (Sigma)34S and (Sigma)18O values of LCIT mirabilite range from +48.8 to +49.3% (CDT), and -16.6 to -17.1% (V-SMOW), respectively, while (Delta)17O average -0.37% (V-SMOW). LCIT mirabilite mounds are isotopically different from other mirabilite mounds found in coastal regions of Antarctica, which have isotope values close to seawater compositions. (Sigma)18O and (Delta)17O values suggest the incorporation of isotopically light glacial water. Data point to initial sulfate formation in an anoxic water body, either as a stratified anoxic deep lake on the surface, a sub-glacial water reservoir, or a sub-glacial lake. Several surface lakes of varying size are also present within this region of the LCIT, and in some cases are adjacent to the mirabilite mounds. O and D isotope compositions of surface lakes confirm they are derived from a mixture of glacial ice and snow that underwent moderate evaporation. (Sigma)18O and (Sigma)D (V-SMOW) values of snow, ice, and lake water range from -64.2 to -29.7%, and -456.0 to -231.7%, respectively. However, the isotope chemistry of these surface lakes is extremely different from the mounds. Dissolved SO4-2 (Sigma)34S and (Sigma)18O values range from +12.0 to +20.0% and -12.8 to -22.2% (the most negative (Sigma)18O of terrestrial sulfate ever reported), respectively, with sulfate (Delta)17O ranging from +0.93 to 2.24%. Ion chromatography data show that lake water is fresh to brackish in origin, with TDS less than 1500 ppm, and sulfate concentration less than 431 ppm. Isotope and chemical data suggest that these lakes are unlikely the source of the mirabilite mounds. We suggest that lake water sulfate is potentially composed of a mixture of atmospheric sulfate and minor components of sulfate of weathering origin, much like the sulfate in the polar plateau soils of the McMurdo Dry Valleys. A simple model explains mirabilite mound formation at the LCIT. Sulfur redox processes could occur sub-glacially as a result of liquid-water-based glacial conditions (Alpine style glacier), most likely formed by pressure melting of overlying ice (Aharon, GCA, 52, 2321-2331). We suggest that the aqueous base of the LCIT contains dissolved SO42- and is anoxic where sulfate reduction to H2S, HS-, or native sulfur takes place. Sulfide is removed by either precipitation as sulfide minerals or by escape of H2S (neither of which have been observed). Mirabilite precipitation is likely the result of evaporation or freezing of sulfate-rich brines as they reach the surface where they manifest themselves as mounds. Pressure from the overlying ice contributing to a pressure-melting scenario that creates the sub-glacial aqueous environment also contributes to the mechanism of upward transport of the sulfate-rich fluids. Further evidence to support this upward transport model comes from the nature of ice motion at the LCIT. Cassidy et al (Meteoritics, 27, 490-525, 1992) pointed out that it is the vertical ice motion in this area that creates the meteorite-stranding surface that could also account for upward transport of sulfate-rich fluids. Alternatively, mirabilite was deposited in a similar condition as present-day coastal Antarctica when the LCIT was wetter and warmer

Socki, Richard↗

NASA NTRS2013

30-kW SEP Spacecraft as Secondary Payloads for Low-Cost Deep Space Science Missions

The Solar Array System contracts awarded by NASA's Space Technology Mission Directorate are developing solar arrays in the 30 kW to 50 kW power range (beginning of life at 1 AU) that have significantly higher specific powers (W/kg) and much smaller stowed volumes than conventional rigid-panel arrays. The successful development of these solar array technologies has the potential to enable new types of solar electric propulsion (SEP) vehicles and missions. This paper describes a 30-kW electric propulsion vehicle built into an EELV Secondary Payload Adapter (ESPA) ring. The system uses an ESPA ring as the primary structure and packages two 15-kW Megaflex solar array wings, two 14-kW Hall thrusters, a hydrazine Reaction Control Subsystem (RCS), 220 kg of xenon, 26 kg of hydrazine, and an avionics module that contains all of the rest of the spacecraft bus functions and the instrument suite. Direct-drive is used to maximize the propulsion subsystem efficiency and minimize the resulting waste heat and required radiator area. This is critical for packaging a high-power spacecraft into a very small volume. The fully-margined system dry mass would be approximately 1120 kg. This is not a small dry mass for a Discovery-class spacecraft, for example, the Dawn spacecraft dry mass was only about 750 kg. But the Dawn electric propulsion subsystem could process a maximum input power of 2.5 kW, and this spacecraft would process 28 kW, an increase of more than a factor of ten. With direct-drive the specific impulse would be limited to about 2,000 s assuming a nominal solar array output voltage of 300 V. The resulting spacecraft would have a beginning of life acceleration that is more than an order of magnitude greater than the Dawn spacecraft. Since the spacecraft would be built into an ESPA ring it could be launched as a secondary payload to a geosynchronous transfer orbit significantly reducing the launch costs for a planetary spacecraft. The SEP system would perform the escape from Earth and then the heliocentric transfer to the science target.

Dawn spacecraft↗

NASA NTRS2019

Evidence for Dry Carbonatite Metasomatism in the Oceanic Lithosphere from Peridotite Xenoliths of Samoa and Lanzarote

Water in Earth’s mantle affects processes like magmatism and plate tectonics. Experiments show that CO2-rich fluids lower the water solubility in olivine, implying that CO2-rich melts/fluids may dehydrate the lithosphere during metasomatism. To test this hypothesis, we report water concentrations (by polarized FTIR) of olivines, orthopyroxenes (OPX) and clinopyroxenes (CPX) from Savai’i (Samoa) and Lanzarote (Canary Islands) peridotite xenoliths with evidence of carbonatite metasomatism. Savai’i peridotites are highly depleted harzburgites and dunites with spinel Cr# (Cr/(Cr+Al)) ranging from 0.4 to 0.76 (estimated degree of melting: 191.5%). Strong Light Rare Earth Element (LREE) enrichments with Ti and Zr depletions in OPX and CO2-rich fluid inclusions (via Raman spectroscopy) are consistent with carbonatite metasomatism. Olivine, OPX and reconstructed bulk rock water concentrations (0.67-3.8, 17-89 and 4-26 ppm H2O, respectively) are low and show no apparent relationship with extent of carbonatite metasomatism. Calculated water concentrations of melts in equilibrium with Savai’i OPX (OPX/melt partitioning of water 0.0063 to 0.011) are, on average (0.540.32 wt% H2O), lower than host Samoan lavas (0.63 to 1.5 wt% H2O), despite the LREE enrichments in OPX. Lanzarote peridotites are also highly depleted (degree of melting from spinel Cr#: 171.8%).Water concentrations are low in olivines (1.7-5.3 ppm H2O) and variable in pyroxenes (OPX: 42-103 ppm H2O; CPX: 105-301 ppm H2O), and show no apparent correlation with indicators of carbonatite metasomatism. Both Savai’i and Lanzarote peridotites show negative correlations between water and degree of melting (i.e. Mg/(Mg+Fe), Cr#), suggesting melt depletion rather than metasomatism may have influenced their water concentrations. Calculated water concentrations of melts in equilibrium with Lanzarote CPX (average 1.90.75 wt% H2O; CPX/melt partitioning of water 0.011 to 0.012) are similar to those for Western Canaries lavas (average 1.80.31 wt%; CPX/melt partitioning of water 0.016 to 0.021) inferred from their CPX phenocrysts. However, calculated Ce concentrations in such melts (352 to 378 ppm; CPX/melt partitioning of Ce 0.07) are an order of magnitude greater than the lavas, and similar to carbonatites. This leads to H2O/Ce to be an order of magnitude lower in the inferred melts (26 to 57) than estimates for Western Canary lavas (280150). These low H2O/Ce ratios may suggest H2O loss from CPX during ascent, but the lack of strong water diffusion gradients in Lanzarote minerals does not support this. Instead we hypothesize that carbonatite metasomatism resulted in greater enrichment of Ce over H2O. Assuming carbonatite magmas are water rich, this implies a lower partitioning of water between minerals and melts during metasomatism, as suggested by experiments. Our data suggests carbonatite metasomatism does not result in significant re-hydration of the lithosphere, in contrast to silicate metasomatism as previously observed in Hawaiian peridotites.

Ashley, Aaron↗

NASA NTRS2024

Pull-off Behavior of Stitched Composite T-Joints

T-joints are key structural elements that connect opposing surfaces, thereby providing the load path between flat or curved panels (i.e., upper and lower wing skins) and transverse components (i.e., stiffeners). Due to the low interlaminar strength of polymer matrix composites and their geometrical discontinuities, these joints are vulnerable to pull-off loads. To address these issues, through-thickness reinforcements can be employed to enhance the interlaminar capability of these type of joints. In this study, T-joints were manufactured using through-thickness stitching in dry carbon preforms and cured using the vacuum-assisted resin transfer molding (VARTM) process. Stitched and unstitched T-joints were tested under pull-off loading conditions, and surface strain fields were obtained using a 3D digital image correlation system. The ultimate load, displacement, and absorbed energy of the stitched T-joints were greater than their unstitched counterparts by approximately 16%, 34%, and 58%, respectively. Failure mechanisms were identified by examining fracture surfaces using optical microscopy. Results demonstrate that through-thickness stitching significantly improves the damage tolerance of T-joints, which highlights the effectiveness of stitching to enhance the structural integrity of large aerospace components.

VARTM↗

DOE OSTI2021

Biomass Size Reduction, Drying, and Densification

The overall objective is to solve the particle attrition issue during biomass grinding and pelleting and to enable pelleting as a viable option for production of on-spec material or conversion-ready cellulosic feedstocks.

09 BIOMASS FUELS↗

DOE OSTI2020

Petrophysical and geomechanical properties of gas hydrate-bearing sediments recovered from Alaska North Slope 2018 Hydrate-01 Stratigraphic Test Well

Knowledge of petrophysical and geomechanical properties of gas hydrate-bearing sediments are essential for predicting reservoir response due to gas production from gas hydrate reservoirs. That information will be critical parameters for designing production well completion such as specification of depressurization pump, water storage tank, and mesh size of sand screen. In December 2018, Stratigraphic Test Well Hydrate-01 was drilled in the western part of the Prudhoe Bay Unit, Alaska North Slope as part of the technical planning effort for a future long-term production test by collaborative team of DOE/NETL, USGS, and MH21-S (Boswell et al., 2020, Collett et al., 2020, Okinaka et al., 2020). Data set of logging-while-drilling (LWD) were acquired (Haines et al., 2020, Suzuki et al., 2019) and core sampling depth was determined on-site.Side-wall pressure coring was conducted to recover gas hydrate-bearing sediments from two reservoir sections named Unit-B and Unit-D. A total of 34 cores were successfully recovered by 5 runs of a wire-line deployed pressure corer (CoreVault® System - Halliburton). Core analysis scheme of this project are shown in Figure 1. All cores were quenched in liquid nitrogen while at high pressure in the laboratory of Stratum Reservoir, LLC. at Anchorage (Figure 1, a)). And the cores were removed from the pressure corer autoclave with temperature support of dry ice and stored under liquid nitrogen at atmospheric pressure. 19 damaged cores were processed to index property measurements directly such as grain size, grain density. 4 of another 17 cores were depressurized and trimmed for making a plug to analyze petrophysical properties of host sediments. Unsteady-state permeability test was conducted to obtain relative water permeability to gas and core scale NMR T2 distribution measurement was performed for evaluating pore size distribution at Houston (Figure 1, b)). Remained high quality 13 cores were preserved with gas hydrate for advanced laboratory analysis. National Institute of Advanced Industrial Science and Technology, as a part of the Japanese National Hydrate Research Program (MH21-S, funded by Ministry of Economy, Trade and Industry), received the samples at Sapporo, Japan for advanced core analysis. High-resolution X-ray CT was used to analyze the quality of the samples, which showed undisturbed lithological layers. Cores were lathed into cylindrical shape and distributed for multi property measurements (Figure 1, c)).<p>As a result, sediment from Unit-D is categorized as silty sand at ~37% porosity with ~80% gas hydrate saturation. An average hydration number n = 6.16 was measured by Raman spectroscopy. An average intrinsic permeability of ~400 mD and in situ effective permeability (with hydrate) on the order of ~10 mD. The Unit B recovered cores consisted of well sorted sand at ~40% porosity with ~95% gas hydrate saturation. An average intrinsic permeability of ~1 Darcy and in situ effective permeability on the order of ~30 mD was measured for the Unit B cores. There was a small permeability reduction due to porosity loss with increasing effective stress that simulated consolidation behavior along with depressurization in the highly permeable sandy sediment. The apparent minimum change in porosity and permeability may be caused by the low compressibility of quartz sand grains in the recovered cores. XRD and thermal conductivity analysis also suggested high quartz content. Triaxial compression tests established internal friction angles based on the Mohr-Coulomb's failure criterion, which are 40° for hydrate-bearing sediment and 29.8° for hydrate free sediment.</p>

Yoneda, Jun↗

DOE OSTI2024

Drop Analysis of a Department of Energy Standard Canister Containing Fort Saint Vrain SNF– 24138

DOE manages over 300 types of SNF, many of which are located at the INL site. Managing this large variety of SNF for storage, transportation, and disposal poses a challenge to DOE. The Idaho Cleanup Project and INL are collaborating on the DOE SNF Road-Ready Demonstration (“Road-Ready Demonstration”), which will develop and demonstrate the designs, technology, processes, and regulatory framework for packaging DOE-managed SNF for “road-ready dry storage.” Road-ready dry storage (RRDS) is an SNF management concept in which SNF is packaged into dry, sealed canisters that are then placed in on-site storage in anticipation of later transport and disposition. The forward-looking goal of the Road-Ready Demonstration is to establish the foundation for a large-scale RRDS program at the INL site. One critical aspect of RRDS is the ability to certify the DOE Standard Canister and its associated transportation package in accordance with 10 CFR 71 for offsite transportation. Depending on the SNF type and transportation strategy, DOE Standard Canisters may be required to maintain structural integrity under hypothetical accident scenarios (e.g., drop events). The DOE Standard Canisters have been tested and analyzed under various SNF loading configurations and accident drop events in support of the Idaho Spent Fuel Facility and other DOE programs; however, no analysis has yet been completed in support of the recently initiated Road-Ready Demonstration. This paper presents preliminary results from a finite element analysis of the Ø45.7 cm × 4.6 m (Ø18 in. × 15 ft) DOE Standard Canister under the 9 m drop at 80 degrees off-vertical drop scenario considered in previous INL tests and analyses. It considers the Fort St. Vrain spent nuclear fuel loading configuration proposed for the Road-Ready Demonstration, uses updated material properties, and applies the strain-based acceptance criteria established in ASME Boiler and Pressure Vessel Code’s Section III, Division 3 rules for storage and transportation spent nuclear fuel containments. This updated analysis is compared to previous DOE Standard Canister drop analyses. Preliminary results from the updated analysis show that certain regions of the containment exceed the allowable limits during the accidental drop event. However, these regions are limited to components performing a non-structural function. While further work on this analysis will be pursued, this analysis serves as the foundation for formal calculations used to support applicable certification efforts of the RRDS system at INL.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2024

Drop Analysis of a Department of Energy Standard Canister Containing Fort Saint Vrain SNF

42 ENGINEERING↗

NASA NTRS2007

United Space Alliance LLC Parachute Refurbishment Facility Model

The Parachute Refurbishment Facility Model was created to reflect the flow of hardware through the facility using anticipated start and delivery times from a project level IV schedule. Distributions for task times were built using historical build data for SFOC work and new data generated for CLV/ARES task times. The model currently processes 633 line items from 14 SFOC builds for flight readiness, 16 SFOC builds returning from flight for defoul, wash, and dry operations, 12 builds for CLV manufacturing operations, and 1 ARES 1X build. Modeling the planned workflow through the PRF is providing a reliable way to predict the capability of the facility as well as the manpower resource need. Creating a real world process allows for real world problems to be identified and potential workarounds to be implemented in a safe, simulated world before taking it to the next step, implementation in the real world.

Esser, Valerie↗

DOE OSTI2023

Viral but not bacterial community successional patterns reflect extreme turnover shortly after rewetting dry soils

As central members of soil trophic networks, viruses have the potential to drive substantial microbial mortality and nutrient turnover. Pinpointing viral contributions to terrestrial ecosystem processes remains a challenge, as temporal dynamics are difficult to unravel in the spatially and physicochemically heterogeneous soil environment. In Mediterranean grasslands, the first rainfall after seasonal drought provides an ecosystem reset, triggering microbial activity during a tractable window for capturing short-term dynamics. In this report we simulated precipitation in microcosms from four distinct dry grassland soils and generated 144 viromes, 84 metagenomes and 84 16S ribosomal RNA gene amplicon datasets to characterize viral, prokaryotic and relic DNA dynamics over 10 days. Vastly different viral communities in each soil followed remarkably similar successional trajectories. Wet-up triggered a significant increase in viral richness, followed by extensive compositional turnover. Temporal succession in prokaryotic communities was much less pronounced, perhaps suggesting differences in the scales of activity captured by viromes (representing recently produced, ephemeral viral particles) and total DNA. Still, differences in the relative abundances of Actinobacteria (enriched in dry soils) and Proteobacteria (enriched in wetted soils) matched those of their predicted phages, indicating viral predation of dominant bacterial taxa. Rewetting also rapidly depleted relic DNA, which subsequently reaccumulated, indicating substantial new microbial mortality in the days after wet-up, particularly of the taxa putatively under phage predation. Production of abundant, diverse viral particles via microbial host cell lysis appears to be a conserved feature of the early response to soil rewetting, and results suggest the potential for ‘Cull-the-Winner’ dynamics, whereby viruses infect and cull but do not decimate dominant host populations.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS2016

Torrefaction Processing for Human Solid Waste Management

This study involved a torrefaction (mild pyrolysis) processing approach that could be used to sterilize feces and produce a stable, odor-free solid product that can be stored or recycled, and also to simultaneously recover moisture. It was demonstrated that mild heating (200-250 C) in nitrogen or air was adequate for torrefaction of a fecal simulant and an analog of human solid waste (canine feces). The net result was a nearly undetectable odor (for the canine feces), complete recovery of moisture, some additional water production, a modest reduction of the dry solid mass, and the production of small amounts of gas and liquid. The liquid product is mainly water, with a small Total Organic Carbon content. The amount of solid vs gas plus liquid products can be controlled by adjusting the torrefaction conditions (final temperature, holding time), and the current work has shown that the benefits of torrefaction could be achieved in a low temperature range (< 250 C). These temperatures are compatible with the PTFE bag materials historically used by NASA for fecal waste containment and will reduce the energy consumption of the process. The solid product was a dry material that did not support bacterial growth and was hydrophobic relative to the starting material. In the case of canine feces, the solid product was a mechanically friable material that could be easily compacted to a significantly smaller volume (approx. 50%). The proposed Torrefaction Processing Unit (TPU) would be designed to be compatible with the Universal Waste Management System (UWMS), now under development by NASA. A stand-alone TPU could be used to treat the canister from the UWMS, along with other types of wet solid wastes, with either conventional or microwave heating. Over time, a more complete integration of the TPU and the UWMS could be achieved, but will require design changes in both units.

Serio, Michael A.↗

DOE OSTI2023

Tuning Organic Semiconductor Packing and Morphology through Non-equilibrium Solution Processing (Final Report)

Organic semiconductors (OSCs) are a promising candidate to produce low-cost, large area, and flexible electronics. There has previously been successful development of organic field effect transistors (OFETs), photovoltaics (OPV), and bioelectronics using OSCs. Solution processing of these materials allows for the fabrication of large-area devices in the kinetic crystallization regime. The charge transport capabilities have been shown to depend on the morphology and molecular packing of the OSC within thin films. Our hypothesis is that solution processing conditions may significantly impact OSC morphology and as a result the charge transport. Therefore, this work has focused on obtaining a fundamental understanding of the morphology and molecular packing of OSCs for optimal device performance. Through our work, we have gained a better understanding of how these structural conditions were influenced by the solution processing conditions. Our studies have led to a more systematic understanding of the various parameters that impact OSC morphology. Solution processing leads to non-equilibrium films, thus allowing for the formation of diverse morphologies that are inaccessible by other fabrication methods. Previously, our group has focused on tuning the morphology of small-molecular OSCs [53, 55-57]. However, little work had been devoted to polymer OSCs. There was a lack of detailed studies characterizing the solution-state of polymer OSCs in terms of their conformation, degree of entanglement, polymer aggregation, and chain relaxation dynamics. The solution state properties are also likely to be influenced by the rigidity and molecular weight of the polymer OSCs investigated. Thus, we have focused our attention on gaining a better insight of polymer OSC films and solution processing methods. Through this proposal, our approach is to investigate the correlation between solution-state properties and the morphology of the resulting polymer OSC films. We worked three specific aims: investigate the effects of 1) polymer OSC solution-state properties on final film morphology; 2) molecular additives on the solution-state and final film properties; 3) controlled pre-aggregation in the solution-state in the final film morphology. More rigid and planar polymer backbones should promote interchain charge transport and more efficient interchain hopping between polymer chains. Through tailoring the polymer backbone, polymer sidechains, and molecular weight, we expected the altered solution-state properties to affect the final film morphology. In addition, reducing the entanglements and promoting chain alignment will likely prevent charge carrier trapping through conformation disorders. We thus studied different mechanisms, such as molecular additives, to reduce entanglements in solution. Devices fabricated from these solutions were expected to have improved charge transport abilities. In addition to tailoring the solution-state characteristics of the polymer OSCs, we investigated the effect of solution processing methods on the molecular packing and morphology of polymer OSC films. Two main solution processing techniques, e.g., spin-coating and solution shearing, were employed to fabricate OFETs. Spin coating was employed to prepare OSC films, which produce isotropic films. This technique creates several parameters to tune such as spin coating speed, acceleration, and time. Additionally, our research group developed the solution shearing method, which consists of the solution initially sandwiched between two plates. By sliding the top plate, the solution front is exposed and drying begins. This technique allows for the creation of aligned large crystalline domains. Solution shearing consists of different processing parameters which can affect the final morphology, such as shearing speed, substrate temperature and temperature gradient, distance between both plates, and the tilt angle of the top plate. Due to the complexity of the polymer systems investigated, numerous techniques were employed to characterize the polymer OSC solution state and films. All the materials were characterized using the DOE supported synchrotron X-ray scattering facilities at the Stanford Synchrotron Radiation Lightsource (SSRL). Using grazing incidence X-ray scattering (GIXS) and Near Edge X-ray Absorption Fine Structure (NEXAFS) techniques, the crystalline structure and molecular orientations of the thin films were measured. Optical absorption (UV-Vis) spectroscopy was employed to determine the aggregation state in solution and films of the polymer systems. Polarized UV-Vis also allowed for the determination of the relative degree of polymer chain alignment for solution sheared films. Additionally, various other techniques were used to investigate other properties within the film, such as atomic force microscopy (AFM) and solution rheology. Finally, the device performance is quantified through the fabrication and characterization of OFETs, which will highlight the effects of morphology on charge transport.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Pivotal role of organic adsorbates for the creation of catalytic sites during dry reforming of methane

Inadvertent factors can sometimes be crucial for synthesis of catalysts. The use of polyalcohols is common in the synthesis of heterogeneous catalysts. Interactions between alcohols and heterogeneous catalysts have been shown to induce surface reconstructions that greatly impact catalytic performance. Thus, traces of these alcohol functionalities on the as-synthesized catalysts, combined with heat treatment, could be critical in the generation of catalytic sites. Here, we show that during the synthesis of a Ni–Mo/MgO catalyst using a polyol process, residual ethylene glycol (EG) on the surface plays a significant role in the generation of catalytic sites for dry reforming of methane (DRM). The as-synthesized catalyst presents dispersed cationic Ni. Under DRM reaction conditions, the presence of EG, and H2 generated in situ, promote the generation of co-localized Ni–Mo nanoparticles (NPs). Greater amount of EG in the as-synthesized catalyst prevented sintering, leading to better catalyst stability and higher rates. If the residual EG remaining post-synthesis is removed through calcination, before conducting DRM, NiO NPs are formed and the material is completely inactive for catalyzing the reaction. When using a different support, denoted MgO*, EG also proved indispensable to generate active sites, although Ni–Mo co-localization was not evident, and a combination of DRM-related species was needed to activate the catalyst, not just H2. This work systematically uncovers how the interactions between organic adsorbates, the supported metals and the catalyst support dictate the creation of catalytic active sites.

Polo Garzon, Felipe [ORNL] (ORCID:0000000265076183↗

NASA NTRS2012

Composite Interstage Structural Concept Down Select Process and Results

NASA's Advanced Composites Technologies (ACT) project evaluated several composite construction options for the Ares V Interstage to support the Constellation Program's goal of reducing the mass of vehicle dry structures. In Phase 1 of the project, eight candidate construction concepts were evaluated for the Ares V Interstage design. Trade studies were performed using finite element analyses to determine weight estimates for the construction concepts. An evaluation process was then used to down select the construction concepts down to two concepts for further consideration in Phase 2 of the project. In Phase 2 of the project, additional trade studies were performed using detailed finite element analyses of the Interstage and a final down select process was used to choose the recommended Interstage construction concept. The results of the study showed that a honeycomb sandwich design was the most favorable Interstage construction concept based on advantages in manufacturing cost. Details of the Phase 1 and Phase 2 trade studies and down select process with final results are presented in the paper.

Sleight, David W.↗

DOE OSTI2021

Self-assembly of aramid amphiphiles into ultra-stable nanoribbons and aligned nanoribbon threads

Small molecule self-assembly is an established route for producing high surface area nanostructures with readily customizable chemistries and precise molecular organization. However, these structures are fragile, exhibiting molecular exchange, migration, and rearrangement - among other dynamic instabilities - and ultimately disassociate upon drying. Here we show a small molecule platform, the aramid amphiphile (AA), that overcomes these dynamic instabilities by incorporating a Kevlar-inspired domain into the molecular structure. Strong, anisotropic interactions between AAs suppress molecular exchange and elicit spontaneous self-assembly in water to form nanoribbons with lengths of up to 20 microns. The nanoribbons have a Young’s modulus of 1.7 GPa and tensile strength of 1.9 GPa. Here, we exploit this stability to extend small molecule self-assembly to hierarchically ordered macroscopic materials outside of solvated environments. Through an aqueous shear alignment process, we organize AA nanoribbons into arbitrarily long flexible threads that support 200 times their weight when dried. Tensile tests of the threads provide a benchmark for Young’s moduli (between ~400 and 600 MPa) and extensibilities (between ~0.6 and 1.1%) that depend on the counterion chemistry in solution. This bottom-up approach to macroscopic materials could benefit solid-state applications, historically inaccessible by self-assembled nanomaterials.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

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 OSTI2022

High-Quality Dry Etching of LiNbO3 Assisted by Proton Substitution through H2-Plasma Surface Treatment

The exceptional material properties of Lithium Niobate (LiNbO3) make it an excellent material platform for a wide range of RF, MEMS, phononic and photonic applications; however, nano-micro scale device concepts require high fidelity processing of LN films. Here, we reported a highly optimized processing methodology that achieves a deep etch with nearly vertical and smooth sidewalls. We demonstrated that Ti/Al/Cr stack works perfectly as a hard mask material during long plasma dry etching, where periodically pausing the etching and chemical cleaning between cycles were leveraged to avoid thermal effects and byproduct redeposition. To improve mask quality on X- and Y-cut substrates, a H2-plasma treatment was implemented to relieve surface tension by modifying the top surface atoms. Structures with etch depths as deep as 3.4 µm were obtained in our process across a range of crystallographic orientations with a smooth sidewall and perfect verticality on several crystallographic facets.

36 MATERIALS SCIENCE↗

NASA NTRS1998

Process for controlling morphology and improving thermal mechanical performance of high performance interpenetrating and semiinterpenetrating polymer networks

In the process of the present invention, a non-polar, aprotic solvent is removed from an oligomer/polymer solution by freeze-drying in order to produce IPNs and semi-IPNs. By thermally quenching the solution to a solid in a short length of time, the size of the minor constituent-rich regions is greatly reduced as they are excluded along with the major constituent from the regions of crystallizing solvent. The use of this process sequence of controlling phase morphology provides IPNs and semi-IPNs with improved fracture toughness, microcracking resistance, and other physical-mechanical properties as compared to IPNs and semi-IPNs formed when the solvent is evaporated rather than sublimed.

Pater, Ruth H.↗