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Helium Saturation of Liquid Propellants

The research is in three areas which are: (1) techniques were devised for achieving the required levels of helium (He) saturation in liquid propellants (limited to monomethylhydrazine (MMH) and nitrogen tetroxide (NTO)); (2) the values were evaluated for equilibrium solubilities of He in liquid propellants as currently used in the industry; and (3) the He dissolved in liquid propellants were accurately measured. Conclusions drawn from these studies include: (1) Techniques for dissolving He in liquid propellants depending upon the capabilities of the testing facility (Verification of the quantity of gas dissolved is essential); (2) Until greater accuracy is obtained, the equilibrium solubility values of He in MMH and NTO as cited in the Air Force Propellant Handbooks should be accepted as standard (There are still enough uncertainties in the He saturation values to warrant further basic experimental studies); and (3) The manometric measurement of gas volume from a frozen sample of propellant should be the accepted method for gas analysis.

Yavrouian, A. H.↗

Preliminary Measurements of Partial Discharge Inception Voltage Degradation with Constant Temperature Aging of Magnet Wire Twisted Pairs for Electric Aircraft Motors

Electric aircraft require high reliability electric motors to meet the stringent safety standards of the aviation industry. Motor winding insulation lifetime and reliability models for electric aircraft applications are needed to enable design of high reliability and high-performance electric motors for aviation applications. Three primary stresses effect the lifetime of motor winding insulation: thermochemical, mechanical, and electrical. This paper presents preliminary experiments on twisted pairs of magnet wire targeting understanding the thermo-chemical degradation of motor winding insulation through constant temperature thermal aging. Three types of magnet wire twisted pairs where tested: polyimide insulated magnet wire, epoxy coated polyimide insulated magnet wire, and epoxy potted polyimide magnet wire. The degradation of the samples over time at temperature was tracked using partial discharge inception voltage measurements. These initial experiments were used for development of procedures and expertise in partial discharge testing and thermo-chemical aging to inform future testing. The preliminary nature of these experiments should be noted when viewing the results. Lessons learned from the experiments are documented.

Thomas Tallerico↗

Hybrid Chemo-Mechanical Plastics Recycling: Solvent-free, High-speed Reactive Extrusion of Low-Density Polyethylene

Low-Density Polyethylene (LDPE) is ubiquitous in the packaging industry due to its flexibility, toughness, and low cost. However, it is typically contaminated with other materials, seriously limiting options for mechanical recycling. Interest in chemical recycling techniques such as pyrolysis and hydrothermal liquefaction is growing, but most of these processes face technoeconomic challenges that have limited commercial deployment. We present a hybrid chemo-mechanical approach using reactive twin-screw extrusion (TSE) for tailoring the molecular weight and chain structure of reclaimed LDPE. Two types of zeolite catalysts at several loading levels were evaluated over a range of processing conditions. Structural, thermal, and rheological properties of the extruded samples were investigated and compared to virgin LDPE and LDPE extruded without the catalyst. A nuclear magnetic resonance spectroscopic technique was used to investigate changes in the structure of the polymer. LDPE extruded with microporous y-zeolite showed lower degradation temperature and increased short chain branching. Mesoporous MCM-41 also induced increased branching but had no effect on degradation temperature. The theoretical mechanical energy input for the chemical modification was calculated using process modeling. The demonstrated hybrid reactive extrusion process provides a potential low-cost, simple approach for repurposing LDPE-based flexible packaging as coatings and adhesives.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Geochemical Changes in Response to CO 2 Injection in a CO 2 -EOR Complex in Northern Michigan (Volume II.1)

The Midwest Regional Carbon Sequestration Partnership (MRCSP) was founded in 2003 as part of the U.S. Department of Energy’s (DOE’s) Regional Carbon Sequestration Partnership initiative. Since its founding, MRCSP has made significant strides toward making CCUS a viable option for states in the region. The public/private consortium, funded through the DOE Regional Carbon Sequestration Initiative, brings together nearly 40 industry partners and 10 states. Battelle, as the project lead, oversees research, development and operations and coordinates activities among the partners. The incremental, phased approach has built a valuable knowledge base for the industry and paved the way for commercial-scale adoption of CCUS technologies. From 2008 to 2020, MRCSP Phase III focused on the development of large-scale injection projects. This report is part of a series of reports prepared under the Midwestern Regional Carbon Sequestration Partnership (MRCSP) Phase III (Development Phase). These reports summarize and detail the findings of the work conducted under the Phase III project. The report describes the geochemical monitoring program under MRCSP to use stable and radiogenic isotope geochemistry in concert with analysis of general geochemical parameters of fluids and gases and analysis of core samples to determine geochemical processes occurring in the reef structure because of CO 2 injection. Specifically, brine and gas samples were collected and analyzed to determine changes occurring between reefs prior to and following CO 2 injection. The analytical results for general geochemical parameters were modeled with chemical equilibrium models to determine if the injection of CO 2 resulted in the mineral dissolution or precipitation. Finally, core samples were collected and analyzed to determine if there was evidence of dissolution features or mineral precipitation.

01 COAL, LIGNITE, AND PEAT↗

Rare Earth Element (REE) and Critical Mineral Fractions of Central Appalachian Coal-Related Strata Determined by 7-Step Sequential Extraction

Rare earth elements (REEs) and critical minerals (CMs) are used in many modern industries, including the automotive sector, generation and storage, clean energy, and defense. The demand for REEs is increasing, and the REE supply chain is unpredictable. The US has driven to assess non-conventional sources of REE (such as coal underclay) to identify domestic resources to stabilize this uncertainty in supply. Knowledge of the minerology, distribution, and modes of occurrence of REEs is integral to the assessment of non-conventional sources. Additionally, extraction techniques can be optimized and targeted when REE distribution in different solid fractions from source material is understood. In this study, four bituminous coal-related samples associated with the Lower and Middle Kittanning coal seams in the Appalachian Basin (US) underwent a seven-step sequential extraction procedure, primarily targeting the water-soluble, exchangeable, acid soluble, mildly reducible, moderately reducible, strongly reducible, and oxidizable fractions. The REE and other elements of interest from each extraction step were analyzed, and the percentages of element extracted from raw solids were calculated. REEs extracted from the total seven steps were reported as the extractable fraction, whereas the fractions in the residual solids were reported as the non-extractable fraction. Less than 6% of REE were extracted from three samples. Twenty-one percent of REE was extracted from the fourth sample, mainly from the steps targeting oxidizable and exchangeable phases. Co-extraction of critical metals (Co, Ni, Cu, and Zn) occurred during the oxidizable, exchangeable, acid soluble, and water-soluble steps for the four samples. In the extracted fractions, the four samples all exhibited a middle and heavy REE enrichment relative to light REE. The mobility of major cation (e.g., Ca, Fe, and P) and REE is associated with exchangeable, oxidizable, and acid soluble fractions. Non-extractable REE is likely held in refractory apatitic phases, and/or primary REE-phosphates (e.g., monazite and xenotime).

58 GEOSCIENCES↗

A fundamental approach to the sticking of insect residues to aircraft wings

The aircraft industry is concerned with the increase of drag on planes due to the sticking of insects on critical airfoil areas. The objectives of the present study were to investigate the effects of surface energy and elasticity on the number of insects sticking onto the polymer coatings on a modified aircraft wing and to determine the mechanism by which insects stick onto surfaces during high velocity impact. Analyses including scanning electron microscopy, electron spectroscopy for chemical analysis and contact angle measurements of uncoated and polymer coated aluminum surfaces were performed. A direct relation between the number of insects sticking on a sample and its surface energy was obtained. Since the sticky liquid from a burst open insect will not spread on the low energy surface, it will ball up providing poor adhesion between the insect debris and the surface. The incoming air flow can easily blow off the insect debris and thus reducing the number of insects that remain stuck on the surface. Also a direct relation between the number of insect sticking onto a surface and their modulus of elasticity was obtained.

Yi, O.↗

Aerodynamic Analysis of Multistage Turbomachinery Flows in Support of Aerodynamic Design

This paper summarizes the state of 3D CFD based models of the time average flow field within axial flow multistage turbomachines. Emphasis is placed on models which are compatible with the industrial design environment and those models which offer the potential of providing credible results at both design and off-design operating conditions. The need to develop models which are free of aerodynamic input from semi-empirical design systems is stressed. The accuracy of such models is shown to be dependent upon their ability to account for the unsteady flow environment in multistage turbomachinery. The relevant flow physics associated with some of the unsteady flow processes present in axial flow multistage machinery are presented along with procedures which can be used to account for them in 3D CFD simulations. Sample results are presented for both axial flow compressors and axial flow turbines which help to illustrate the enhanced predictive capabilities afforded by including these procedures in 3D CFD simulations. Finally, suggestions are given for future work on the development of time average flow models.

Adamczyk, John J.↗

Lay and Expert Perceptions of Planetary Protection

As space scientists and engineers plan new missions to Mars and other planets in our solar system, they will face critical questions about the potential for biological contamination of planetary surfaces. In a society that places ever-increasing importance on the role of public involvement in science and technology policy, questions about risks of biological contamination will be examined and debated in the media, and will lead to the formation of public perceptions of planetary-contamination risks. These perceptions will, over time, form an important input to the development of space policy. Previous research in public and expert perceptions of technological risks and hazards has shown that many of the problems faced by risk-management organizations are the result of differing perceptions of risk (and risk management) between the general public and scientific and technical experts. These differences manifest themselves both as disagreements about the definition (and level) of risk associated with a scientific, technological or industrial enterprise, and as distrust about the ability of risk-management organizations (both public and private) to adequately protect people's health and safety. This report presents the results of a set of survey studies designed to reveal perceptions of planetary exploration and protection from a wide range of respondents, including both members of the general public and experts in the life sciences. The potential value of this research lies in what it reveals about perceptions of risk and benefit that could improve risk-management policies and practices. For example, efforts to communicate with the public about Mars sample return missions could benefit from an understanding of the specific concerns that nonscientists have about such a mission by suggesting areas of potential improvement in public education and information. Assessment of both public and expert perceptions of risk can also be used to provide an advanced signal of aspects of planetary exploration and protection that may be particularly sensitive or controversial and that could prove problematic from a risk-management standpoint, perhaps warranting a more stringent risk-management approach than would otherwise be the case based on technical considerations alone. The design of the study compares perceptions and attitudes about space exploration relevant to a Mars sample return mission between three respondent groups: (1) members of The Planetary Society, a group representing individuals with a strong interest in space-related issues, (2) a group of university-aged students, representing a population relatively sensitive to environmental hazards, and (3) a group of life scientists outside of the space research community. Members of The Planetary Society received the survey as part of a special issue of The Planetary Report on planetary protection, which contained a number of background articles on planetary protection and related topics. A synopsis of the issue was prepared as an introduction to the survey for the other two groups.

Race, Margaret S.↗

Degradation of Organics in a Glow Discharge Under Martian Conditions

The primary objective of this project is to understand the consequences of glow electrical discharges on the chemistry and biology of Mars. The possibility was raised some time ago that the absence of organic material and carbonaceous matter in the Martian soil samples studied by the VikinG Landers might be due in part to an intrinsic atmospheric mechanism such as glow discharge. The high probability for dust interactions during Martian dust storms and dust devils, combined with the cold, dry climate of Mars most likely results in airborne dust that is highly charged. Such high electrostatic potentials generated during dust storms on Earth are not permitted in the low-pressure CO2 environment on Mars; therefore electrostatic energy released in the form of glow discharges is a highly likely phenomenon. Since glow discharge methods are used for cleaning and sterilizing surfaces throughout industry, the idea that dust in the Martian atmosphere undergoes a cleaning action many times over geologic time scales appears to be a plausible one.

Hintze, P. E.↗

Electrostatic Levitation for Studies of Additive Manufactured Materials

The electrostatic levitation (ESL) laboratory at NASA's Marshall Space Flight Center is a unique facility for investigators studying high temperature materials. The laboratory boasts two levitators in which samples can be levitated, heated, melted, undercooled, and resolidified. Electrostatic levitation minimizes gravitational effects and allows materials to be studied without contact with a container or instrumentation. The lab also has a high temperature emissivity measurement system, which provides normal spectral and normal total emissivity measurements at use temperature. The ESL lab has been instrumental in many pioneering materials investigations of thermophysical properties, e.g., creep measurements, solidification, triggered nucleation, and emissivity at high temperatures. Research in the ESL lab has already led to the development of advanced high temperature materials for aerospace applications, coatings for rocket nozzles, improved medical and industrial optics, metallic glasses, ablatives for reentry vehicles, and materials with memory. Modeling of additive manufacturing materials processing is necessary for the study of their resulting materials properties. In addition, the modeling of the selective laser melting processes and its materials property predictions are also underway. Unfortunately, there is very little data for the properties of these materials, especially of the materials in the liquid state. Some method to measure thermophysical properties of additive manufacturing materials is necessary. The ESL lab is ideal for these studies. The lab can provide surface tension and viscosity of molten materials, density measurements, emissivity measurements, and even creep strength measurements. The ESL lab can also determine melting temperature, surface temperatures, and phase transition temperatures of additive manufactured materials. This presentation will provide background on the ESL lab and its capabilities, provide an approach to using the ESL in supporting the development and modeling of the selective laser melting process for metals, and provide an overview of the results to date.

SanSoucie, Michael P.↗

Spray-Coated Silver as Backside Metal for III–V Photovoltaic Devices on GaAs and Ge Substrates

The accelerated increase in demand for III-V space photovoltaics on GaAs and Ge substrates, as well as growing interests in terrestrial applications, motivate the development of cost-effective, high-throughput processing routes of these materials. Here, in this study, we assess spray-coated silver (Ag) back contact metallization as a substitute for electron-beam-evaporated metals currently used in industry. We find that the spray-coated Ag films are dense and continuous. By means of quantum efficiency, dark current-voltage, and illuminated current-voltage characterizations, we show that spray-coated GaAs and Ge solar cells perform similarly to baseline devices with electroplated Au, including under high current densities. We estimate that the thresholds for specific contact resistance below which back contacts do not significantly contribute to resistive loss are 2.1 x 10 -1 Ω•cm 2 for GaAs and 4.7 x 10 -2 Ω•cm 2 for Ge. We experimentally confirm that our spray-coated samples meet these requirements. Peel tests show that the adhesion of plain spray-coated Ag films to the back of p-type Ge substrates used in III-V solar cells is currently insufficient, whereas adhesion to p-type GaAs substrates is outstanding and requires no further optimization.

14 SOLAR ENERGY↗

On the design and performance of InGaN/Si double-junction photocathodes

Via a combined theoretical and experimental study, we have investigated the synthesis and performance characteristics of InGaN/Si double-junction photoelectrochemical (PEC) water splitting devices, which promise a theoretical solar-to-hydrogen conversion efficiency ~30% under AM 1.5G one-sun illumination. The double-junction photocathodes consist of a p + -InGaN top light absorber and a Si bottom p-n junction, which are connected through a nanowire tunnel junction. The effect of indium composition of the top light absorber as well as the impact of p-type Mg dopant incorporation on the PEC performance was studied. Experimentally, the sample with 32% indium composition showed a maximum photocurrent density of ~9 mA/cm 2 at 0.4 mV vs reverse hydrogen electrode (RHE) with applied bias photon-to-current efficiency (ABPE) of ~9.5%. An optimum p-type doping level ~1 × 10 17 cm -3 was also identified, which results in the best device performance as a result of optimum surface band bending as well as vertical charge carrier (hole) transport. These results also show a good agreement with our theoretical analysis. This work provides significant insights in advancing the design and development of high efficiency PEC devices for artificial photosynthesis using industry ready materials, e.g., Si and GaN, to achieve large-scale, low-cost onsite hydrogen fuel production.

42 ENGINEERING↗

Williston Basin Carbon Ore, Rare Earths, and Critical Minerals (CORE-CM) Program

The U.S. Department of Energy’s Office of Fossil Energy awarded 13 CORE-CM programs as part of the CORE-CM Initiative, designed to develop the technology and upstream and midstream supply chains to extract rare-earth elements (REEs) and critical minerals (CMs) from the nation’s coal supplies. The intent is to catalyze regional economic growth and job creation while strengthening the use of domestic resources. The Williston Basin CORE-CM Program aims to drive the expansion and transformation of coal and coal-based resource usage within the Williston Basin to produce REEs, CMs, and nonfuel carbon-based products (CBPs). A coalition team of nearly 30 private industry, university, and state, local, and federal government partners was formed for this task. Partners include the University of North Dakota’s Energy & Environmental Research Center, College of Engineering and Mines Research Institute, and Nistler College; North Dakota State University; Montana Tech University; Pacific Northwest National Laboratory; Critical Materials Institute; North Dakota Geological Survey; South Dakota Geological Survey; U.S. Geological Survey; North American Coal Corporation; BNI Energy; Basin Electric Power Cooperative; Minnkota Power Cooperative; and many more. This presentation will focus on the current status and results to date of the Williston Basin CORE-CM Program, with a focus on core sample characterization for REE and CM content.

Folkedahl, Bruce C.↗

Concentration and Recovery of Rare Earth Elements from Eastern US Coal Refuse

Recent studies funded by the US Department of energy have shown that coal and coal byproducts contain elevated contents of Rare Earth Elements (REEs), making them a potential resource for these critical materials. The approach employed in this research focused on the concentration and extraction of REEs from fine coal refuse derived from various preparation plants in the Appalachian coal basin of the United States. Initial efforts in this research focused on the identification and characterization of REEs in various fine coal refuse streams from nine distinct industrial preparation plants in Appalachia. The average REE content in these materials was determined to be approximately 200 ppm, but the REE content showed a strong correlation to the aluminum content, suggesting that the REEs are closely associated with the clay minerals present in the refuse. Given the relatively low REE concentrations, initial efforts sought to concentrate the REEs through decarbonization and dispersive liberation steps. In these tests, high-shear agitation in the presence of a polyelectrolyte, followed by sedimentation was able to isolate the REE-enriched fine clay particles from siliceous gangue minerals. Following the dispersive liberation step, all samples were found to have an REE content greater than 300 ppm, a benchmark used for many initial exploratory studies. In one case, the REE content was increased by more than 125%. Subsequent extraction tests initially utilized a direct ion-exchange leaching approach with ammonium sulfate as lixiviant. In all cases, the simple ion-exchange leaching process failed to recover significant quantities of rare earth elements, ultimately suggesting that the REEs in fine coal waste may be passivated or bound in a colloidal phase. To access this colloidal phase, several alternative approaches were evaluated, including leaching with alternative ion-exchange lixiviants, reductive leaching, gas-purged leaching, and others. The approach that showed the most promise was strong alkaline pretreatment, followed by ion-exchange leaching with ammonium sulfate at pH 4. A combination of strong alkali and high-temperatures treatment successfully liberated the REEs, converting them to a form amenable to ion-exchange leaching. The highest REE recovery achieved with this method was determined to be 39%. Lastly, bench-scale solvent extraction tests were used to further concentrate REEs in the leach solution and demonstrate that mixed rare earth concentrates can be successfully produced from fine coal refuse.

01 COAL, LIGNITE, AND PEAT↗

Stability and molecular pathways to the formation of spin defects in silicon carbide

Abstract Spin defects in wide-bandgap semiconductors provide a promising platform to create qubits for quantum technologies. Their synthesis, however, presents considerable challenges, and the mechanisms responsible for their generation or annihilation are poorly understood. Here, we elucidate spin defect formation processes in a binary crystal for a key qubit candidate—the divacancy complex (VV) in silicon carbide (SiC). Using atomistic models, enhanced sampling simulations, and density functional theory calculations, we find that VV formation is a thermally activated process that competes with the conversion of silicon (V Si ) to carbon monovacancies (V C ), and that VV reorientation can occur without dissociation. We also find that increasing the concentration of V Si relative to V C favors the formation of divacancies. Moreover, we identify pathways to create spin defects consisting of antisite-double vacancy complexes and determine their electronic properties. The detailed view of the mechanisms that underpin the formation and dynamics of spin defects presented here may facilitate the realization of qubits in an industrially relevant material.

74 ATOMIC AND MOLECULAR PHYSICS↗

Community Extreme Tonnage User Service (CETUS): A 5000 Ton Open Research Facility in the United States

Large sample volume 5000 ton multi-anvil presses have contributed to the exploration of deep Earth and planetary interiors, synthesis of ultra-hard and other novel materials, and serve as a sample complement to pressure and temperature regimes already attainable by diamond anvil cell experiments. However, no such facility exists on the North American continent. We propose the establishment of an open user facility for COMPRES members and the entire research community, with the unique capability of a 5000 ton (or more) press, supported by a host of extant co-located experimental and analytical laboratories and research staff. We offer wide range of complementary and/or preparatory experimental options. Any required synthesis of materials or follow up experiments can be carried out controlled atmosphere furnaces, piston cylinders, multi-anvil, or experimental impact apparatus. Additionally, our division houses two machine shops that would facilitate any modification or custom work necessary for development of CETUS, one for general fabrication and one located specifically within our experimental facilities. We also have a general sample preparation laboratory, specifically for experimental samples, that allows users to quickly and easily prepare samples for ebeam analyses and more. A service we can offer to COMPRES community members in general, and CETUS visiting users specifically, is a multitude of analytical instrumentation literally steps away from the experimental laboratories. This year we will be pursuing site funding of our laboratories through NASA's Planetary Science Directorate, which should result in substantial cost savings to all visiting users, and supports our mission of interagency cooperation for the enhancement of science for all (see companion PSAMS abstract). The PI is in a unique position as an employee of Jacobs Technology to draw funding from multiple sources, including those from industry and commerce. We submitted a Planetary Major Equipment proposal to the NASA Emerging Worlds solicitation for the full cost of a press, with competitive bids submitted from Sumitomo, Rockland Research, and Voggenreiter. Additional funding is currently being sought from industry sources through the Strategic Partnerships Office at NASA JSC, External Pursuits Program Office on the JETS contract, and Jacobs corporate in the United States. Internal funding is available for JETS contract personnel to travel to large press locations worldwide to study set-up and operations. We also anticipate a fortuitous cost savings in installation of the large press because plans are already underway for major renovations to the entire experimental petrology suite within the next 2 years in order to accommodate our growing user base. Our focus as contract staff is on serving the scientific needs of our users and collaborators. We are seeking community expert input on multiple aspects of this proposed facility, such as the press type and design, access management, immediate projects, and future innovation initiatives.

Danielson, L.↗

Prioritizing Nuclear Materials for SAM-3 Neutron Irradiation Campaign: Structural and Cladding Materials Candidates

This report outlines a framework for selecting structural and cladding materials for the Nuclear Science User Facilities (NSUF) SAM-3 neutron irradiation campaign to support the advancement of nuclear energy technologies. The document begins with an introduction that provides background context, highlights the motivations for launching a new irradiation campaign, and defines the overall objectives. The core of the report describes the design considerations for the irradiation campaign, including capsule configurations, irradiation temperature ranges, and target dose levels (defined by displacements per atom, or dpa). The material recommendation was guided by the Specimen Identification and Prioritization (SIP) Working Group, a multidisciplinary team of experts representing national laboratories, academia, industry, federal government and agency. This group played a central role in identifying candidate materials, evaluating technical justifications, and ensuring alignment with boarder programmatic goals. A detailed set of criteria for material prioritization is then presented, taking into account reactor relevance, performance gaps, advanced manufacturing methods, and emerging material classes. Based on the input of SIP working group, specific materials were selected and justified for inclusion in the irradiation campaign by the NSUF leadership and its U.S. Department of Energy (DOE)-Office of Nuclear Energy (NE) management. The final section provides recommended capsule designs, summarizing critical parameters such as material type, fabrication method, sample geometry, irradiation conditions, and specimen quantities. This report serves as a foundation for executing a focused and high-impact neutron irradiation campaign aimed at addressing key materials challenges for both existing and advanced nuclear reactors.

36 - MATERIALS SCIENCE↗