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At least 37 records · Page 2

Enhancing cold spray coatings: Microstructural dynamics and performance attributes of Inconel 625 with chromium carbide incorporation for hydropower applications

The incorporation of chromium carbide (CrC) particles into the cold spray (CS) process is known to mitigate nozzle clogging, although at the expense of deposition efficiency. This study explores the intricate microstructural changes induced by varying amounts of CrC powder (12.5 % and 6 %) in conjunction with Inconel-625 (Inc-625) powder. The deposition was carried out onto A27 cast steel under different CS parameters. Microstructural characterization, including detailed electron microscopy studies, reveals a complex yet structurally stable coating. Noteworthy features include grain fragmentation and a cellular structure enriched with Nb and Mo, with minimal plastic deformation of CrC in the matrix. The cold-sprayed coatings exhibit a significant (~4 times) increase in microhardness compared to the A27 substrate. Mechanical and cavitation erosion properties were systematically investigated. Coatings subjected to higher particle energy conditions with a gas pressure of 600 psi and gas temperature of 650 °C, demonstrated superior resistance to cavitation erosion. This resistance is attributed to a combination of factors, including microstructural characteristics and porosity. Altogether, the study provides valuable insights into the structural dynamics and performance of CS coatings enriched with CrC particles.

A27 cast steel

Critically evaluated/distributed database of IRAS LRS spectra

Accomplishments under this grant effort include: successful scientific utilization of the IRAS Low Resolution Spectrometer (LRS) database of over 150,000 scans of 7-23 micron spectra for over 50,000 celestial sources; publication in refereed journal of an additional 486 critically evaluated spectra of sources brighter than 20 Jy, completing the LRS ATLAS (Olnon and Raimond 1986 A&A) uniformly to that level, and production of an additional 1,830 critically evaluated spectra of sources brighter than 10 Jy; creation and maintenance of on-line, remotely accessible LRS spectra of over 7500 sources; cooperation with Astrophysics Data System personnel for transitioning this LRS database to the ADS access system after funding for this project expires; and publication of research highlights, which include a systematic variation of the shapes of LRS silicate features among stars of differing IRAS broad-band colors, maser characteristics and light curve asymmetries, all correlated with the chemical and physical development and processing of solid phase materials, and preliminary evidence for silicate profile variations in individual stars as a function of visual light curve phase.

Stencel, R. E.

Fluid dynamics of the unsteady two phase processes leading to DDT in granular solid propellants

Deflagration to Detonation (DDT) was predicted to occur in porous beds of high-energy solid propellants by solving the unsteady fluid mechanical convective heat transfer from hot gas products, obtained from the rapid burning at high pressures, provides the impetus to develop a narrow combustion zone and a resulting strong shock. A parametric study clearly indicates that DDT occurs only when a combination of the solids loading fraction, the burning rate constants, the propellant chemical energy, and the particle size provide for critical energy and gas release to support a detonation wave. Predictions for the run-up length to detonation as a function of these parameters are presented.

Krier, H.

Aqua Factorem: Ultra Low Energy Lunar Water Extraction

We propose a new method we call Aqua Factorem to extract lunar water. It will drastically reduce energy and complexity of lunar mining operations helping to establish this industry. Other methods to extract water from the regolith are based on phase change, pumping energy into the regolith to sublimate the ice into vapor, then capturing the vapor, re-freezing it, and hauling the solid ice to a chemical processor where it is converted again into vapor for purification then electrolysis. This requires transporting high power into the permanently shadowed regions (PSRs) not only to vaporize the ice in situ in the soil but to heat the surrounding soil itself, which is wasted energy. Still other methods are based on strip mining and hauling the resource along with slag (the unwanted silicates, which constitutes about 95% of the mass), to a processing unit that is located outside the PSRs. That may be a simpler architecture but is generally not favored because hauling 49,000 t of regolith over many kilometers yearly to produce the projected demand of 2,450 t of propellant would be terribly difficult and expensive with high risk that the vehicles will get stuck driving with such loads across the unprepared regolith. We propose an alternative to both of these approaches, taking advantage of the processing that the unique lunar geology has already performed. Micrometeoroid bombardment has already broken most solid material in the upper part of the regolith into fine grains. This includes solid material of all compositions, including the ice, which is as hard as granite at PSR temperatures and is therefore essentially another type of rock. These ice grains are intermixed with all the other minerals, so a simple, ultra-low-energy grain-sorting process can extract the ice without phase change. As another benefit it can extract the 1 wt% free metal known to be in lunar soil, again with very little energy. The ice can then be hauled to the chemical processing unit in solid phase and converted into rocket propellant. We estimate the 800 kW power needed for thermal extraction can be reduced to less than 100 watts using the new method. This affects the entire architecture of the mining operation producing extensive economic benefit, which we will quantify in this study. We will study it in the context of a mission to mine propellants commercially for space tugs that boost commercial communication satellites from Geosynchronous Transfer Orbit (GTO) to Geostationary Orbit (GEO) then return to the lunar surface for refueling. This simple architecture requires the minimum number of in-space elements, and notably does not require an in-space propellant depot, so it provides the lowest cost and lowest risk startup for a commercial operation. The study will also test the innovative Aqua Factorem process through laboratory experiments, and this will produce basic insights into the handling of lunar resources.

lunar

Thermo-Mechanical Processing in Friction Stir Welds

Friction stir welding is a solid-phase joining, or welding process that was invented in 1991 at The Welding Institute (TWI). The process is potentially capable of joining a wide variety of aluminum alloys that are traditionally difficult to fusion weld. The friction stir welding (FSW) process produces welds by moving a non-consumable rotating pin tool along a seam between work pieces that are firmly clamped to an anvil. At the start of the process, the rotating pin is plunged into the material to a pre-determined load. The required heat is produced by a combination of frictional and deformation heating. The shape of the tool shoulder and supporting anvil promotes a high hydrostatic pressure along the joint line as the tool shears and literally stirs the metal together. To produce a defect free weld, process variables (RPM, transverse speed, and downward force) and tool pin design must be chosen carefully. An accurate model of the material flow during the process is necessary to guide process variable selection. At MSFC a plastic slip line model of the process has been synthesized based on macroscopic images of the resulting weld material. Although this model appears to have captured the main features of the process, material specific interactions are not understood. The objective of the present research was to develop a basic understanding of the evolution of the microstructure to be able to relate it to the deformation process variables of strain, strain rate, and temperature.

Schneider, Judy

Laboratory Investigations of the Complex Refractory Organic Material Produced from Irradiation of Pluto Ice Analogs

Much of Pluto's surface consists of N2 ice with smaller amounts of CH4 and CO ices. Despite the low temperature (approximately 45K), chemistry can be driven in the surface ices by radiation processing such as cosmic ray bombardment. When cosmic rays strike the surface, much of their energy is dispersed in the form of secondary electrons, which in turn drive much of the resulting chemical reactions. Laboratory experiments designed to simulate the conditions on these icy bodies may provide insight into this chemistry. Significant progress has been made in the laboratory toward understanding the smaller, simple compounds produced in the solid phase by radiation processing of (N2, CH4, CO) ices (Bohn et al. 1994; Moore & Hudson 2003; Hodyss et al. 2011; Kim and Kaiser 2012). Recently Materese et al. (2014) used a variety of techniques to better characterize the refractory materials produced from the UV photo-irradiation of N2:CH4:CO ices. However, because Pluto's atmosphere is optically thick to Lyman-alpha UV radiation it is important to re-examine the results using an alternate radiation source. Our latest work has consisted of the analysis of refractory materials produced from the electron bombardment of low temperature N2(‐), CH4(‐), and CO(‐)containing ices (100:1:1). The ice mixture was chosen to be analogous to the known surface ices on Pluto and the radiation source was chosen to mimic the secondary electrons produced by cosmic rays bombardment. The residues were studied using multiple chemical techniques including, infrared (IR) spectroscopy, X‐ray absorption near‐edge structure (XANES) spectroscopy, and gas chromatography coupled with mass spectrometry (GC‐MS). The organic residues produced in these experiments can be seen as an analog for the refractory component of the surface of Pluto, and are compared with the residues previously obtained from UV photo‐irradiation. UV and near‐ IR spectroscopy of the surfaces of Pluto and Charon during the encounter with NASA's New Horizons spacecraft in 2015, will give the first close‐up measurements of ices and their photoproducts. Laboratory measurements and experiments will provide a better context for the data returned by the spacecraft.

organics

Efficient Low-Temperature Direct Lithium Extraction from Chloride Brines Enabled by High-Capacity Sorbent

The demand for lithium, a key component in rechargeable batteries for electric vehicles and renewable energy storage systems, has surged in recent years. Meeting this demand requires efficient extraction methods that are both environmentally friendly and economically viable. This study investigates the utilization of the high-capacity sorbent amorphous aluminum hydroxide for enabling efficient direct lithium extraction at low temperatures. Traditional extraction methods often involve acid-leaching and energy-intensive processes that are not only expensive but also environmentally taxing. In contrast, our approach leverages the exceptional sorption properties of amorphous aluminum hydroxide to facilitate lithium extraction directly from brine, achieving extraction efficiencies of 94.4% in case 1 and 96.2% in case 2 at low temperatures. Kinetic modeling using the Avrami–Erofe’ev framework reveals a nucleation-growth mechanism ( n = 0.71, k = 0.131 h –1 ), providing quantitative insights into the solid-state phase transformation process. This method significantly reduces energy consumption and minimizes the environmental footprint. Through systematic experimentation and optimization, we demonstrate the effectiveness and scalability of our approach, highlighting its potential to revolutionize lithium extraction processes. Our findings highlight the potential of high-capacity sorbents, particularly amorphous aluminum hydroxide toward sustainable lithium production, contributing to the advancement of clean-energy technologies.

anions

[Corrected Title: Solid-Phase Extraction of Polar Compounds from Water] Automated Electrostatics Environmental Chamber

A solid-phase extraction (SPE) process has been developed for removing alcohols, carboxylic acids, aldehydes, ketones, amines, and other polar organic compounds from water. This process can be either a subprocess of a water-reclamation process or a means of extracting organic compounds from water samples for gas-chromatographic analysis. This SPE process is an attractive alternative to an Environmental Protection Administration liquid-liquid extraction process that generates some pollution and does not work in a microgravitational environment. In this SPE process, one forces a water sample through a resin bed by use of positive pressure on the upstream side and/or suction on the downstream side, thereby causing organic compounds from the water to be adsorbed onto the resin. If gas-chromatographic analysis is to be done, the resin is dried by use of a suitable gas, then the adsorbed compounds are extracted from the resin by use of a solvent. Unlike the liquid-liquid process, the SPE process works in both microgravity and Earth gravity. In comparison with the liquid-liquid process, the SPE process is more efficient, extracts a wider range of organic compounds, generates less pollution, and costs less.

Sauer, Richard

Solid Waste Processing: An Essential Technology for the Early Phases of Mars Exploration and Colonization

Terraforming of Mars is the long-term goal of colonization of Mars. However, this process is likely to be a very slow process and conservative estimates involving a synergic, technocentric approach estimate that it may take around 10,000 years before the planet can be parallel to that of Earth and where humans can live in open systems. Hence, any early missions will require the presence of a closed life support system where all wastes, both solids and liquids, will need to be recycled or where all consumables will need to be supplied. The economics of both are often a matter of speculation and conjecture, but some attempt is made here to evaluate the choice. If a choice is made to completely resupply and eject the waste mass, a number of unknown issues are at hand. On the other hand, processing of the wastes, will enable predictability and reliability of the ecosystem. Solid wastes though smaller in volume and mass than the liquid wastes contains more than 90% of the essential elements required by humans and plants. Further, if left unprocessed they present a serious risk to human health. This paper presents the use of well established technology in processing solid wastes, ensuring that the biogeochemical cycles of ecosystems are maintained, reliability of the closed life support system maintained and the establishment of the early processes necessary for the permanent presence of humans on Mars.

Wignarajah, Kanapathipillai

Use of Frit‐Disc Crucible Sets to Make Solution Growth More Quantitative and Versatile

The recent availability of step‐edge, frit‐disc crucible sets (generally sold as Canfield Crucible Sets or CCS) has led to multiple innovations associated with the group's use of solution growth. The use of CCS allows for the clean separation of liquid from solid phases during the growth process. This clean separation enables the reuse of the decanted liquid, either allowing for simple, economic, savings associated with recycling expensive precursor elements or allowing for the fractionation of a growth into multiple, small steps, revealing the progression of multiple solidifications. Clean separation of liquid from solid phases also allows for the determination of the liquidus line (or surface) and the creation, or correction, of composition–temperature phase diagrams. The reuse of clean decanted liquid has also allowed to prepare liquids ideally suited for the growth of large single crystals of specific phases by tuning the composition of the melt to the optimal composition for growth of the desired phase, often with reduced nucleation sites. Finally, it is discussed how solution growth and CCS use can be harnessed to provide a plethora of composition–temperature data points defining liquidus lines or surfaces with differing degrees of precision to either test or anchor artificial intelligence and/or machine‐learning‐based attempts to augment and extend the limited experimentally determined database.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH

Effect of gravity on liquid phase sintering

The unique conditions offered by the earth orbital environment in material processing involving both solid and liquid phases, such as liquid phase sintering, were studied. An experimental development program involving both test and theoretical work was initiated. Experimental work using material combinations selected such that maximum information about the effect of gravity can be derived has been conducted. Wetting of the solid phase by the liquid during sintering is an important phenomenon in liquid phase sintering, and gravity has influence on both capillary phenomenon and density segregation; hence, material combinations were selected such that these two effects can be suitably studies. The experimental work is meant to form the basis for similar comparative work done under low-g conditions. The part of the model dealing with the capillary phenomenon, as related to liquid phase sintering and the effect of gravity on it, suggest that gravity will have negligible effect on the Bond number and that the cohesive force is dependent on both the amount of liquid phase and the angle of contact.

Mookherji, T.

Separation of Carbon Monoxide and Carbon Dioxide for Mars ISRU-Concepts

Solid oxide electrolyzers, such as electrolysis cells utilizing yttria-stabilized zirconia, can produce oxygen from Mars atmospheric carbon dioxide and reject carbon monoxide and unreacted carbon dioxide in a separate stream. The oxygen-production process has been shown to be far more efficient if the high-pressure, unreacted carbon dioxide can be separated and recycled back into the feed stream. Additionally, the mass of the adsorption compressor can be reduced. Also, the carbon monoxide by-product is a valuable fuel for space exploration and habitation, with applications from fuel cells to production of hydrocarbons and plastics. In our research, we will design, construct, and test an innovative, robust, low mass, low power separation device that can recover carbon dioxide and carbon monoxide for Mars ISRU. Such fundamental process technology, involving gas-solid phase separation in a reduced gravitational environment, will help to enable Human Exploration and Development of Space. The separation device will be scaled to operate with a CO2 sorption compressor and a zirconia electrolysis device built at the NASA Ames Research Center and the University of Arizona, respectively. In our research, we will design, construct, and test an innovative, robust, low mass, low power separation device that can recover carbon dioxide and carbon monoxide for Mars ISRU, Such fundamental process technology, involving gas-solid phase separation in a reduced gravitational environment, will help to enable Human Exploration and Development of Space. The separation device will be scaled to operate with a CO2 sorption compressor and a zirconia electrolysis device built at the NASA Ames Research Center and the University of Arizona, The separation device will be scaled to operate with a CO2 sorption compressor and a zirconia electrolysis device built at the NASA Ames Research Center and the University of Arizona, Research needs for the design shown are as follows: (1) The best adsorbent for the process must be determined. (2) Adsorption isotherms must be measured, both for pure components and mixtures. (3) Mathematical modeling must be performed to provide a solid framework for design. (4) The separation system must be constructed and tested. (5) System integration must be studied.

LeVan, M. Douglas

Chemically Driven Multistep Crystallization in the Synthesis of Sodium Yttrium Fluoride Via a Porous, Electrochemically Active Intermediate

Two-step crystallization mechanisms based on liquid–liquid phase separations followed by crystallization are commonly observed both in the laboratory and in nature. While this pathway quite often occurs as a result of a chemical reaction, the subsequent nucleation and growth are often considered as separate, discrete events from the reaction itself. We show this mechanism in the aqueous synthesis sodium yttrium fluoride, but by using a combination of experimental techniques and computational modeling, we show an additional step of solid-state chemical diffusion that is essential to the nucleation mechanism. In this system, we observe at least four distinct steps in the crystallization process, including (1) the segregation of aqueous ions into a dense liquid phase, (2) the formation of a metastable amorphous aggregate, (3) the continuous, gradual solid-state diffusion of sodium and fluoride ions into the amorphous aggregate toward a NaYF4 stoichiometry, and (4) the crystallization of a stable cubic sodium yttrium fluoride phase. Unlike previous descriptions of nucleation and growth, we find that the stoichiometry of the final solid phase evolves throughout the crystallization process rather than being determined at the time of the initial separation from solution. Further, this emphasizes that the chemical reaction cannot be assumed to be a separate event from the phase separation and growth, especially in compounds with variable stoichiometry. We also find that the amorphous aggregate that forms prior to the ion incorporation step adopts a porous, gel-like structure, which we isolated and showed to be electrochemically active, allowing for its potential use as a battery anode in lithium and sodium ion batteries, among other potential applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH

Laboratory Studies on the Formation of Carbon-Bearing Molecules in Extraterrestrial Environments: From the Gas Phase to the Solid State

A detailed knowledge of the formation of carbon-bearing molecules in interstellar ices and in the gas phase of the interstellar medium is of paramount interest to understand the astrochemical evolution of extraterrestrial environments (1). This research also holds strong implications to comprehend the chemical processing of Solar System environments such as icy planets and their moons together with the atmospheres of planets and their satellites (2). Since the present composition of each interstellar and Solar System environment reflects the matter from which it was formed and the processes which have changed the chemical nature since the origin (solar wind, planetary magnetospheres, cosmic ray exposure, photolysis, chemical reactions), a detailed investigation of the physicochemical mechanisms altering the pristine environment is of paramount importance to grasp the contemporary composition. Once these underlying processes have been unraveled, we can identify those molecules, which belonged to the nascent setting, distinguish molecular species synthesized in a later stage, and predict the imminent chemical evolution of, for instance, molecular clouds. Laboratory experiments under controlled physicochemical conditions (temperature, pressure, chemical composition, high energy components) present ideal tools for simulating the chemical evolution of interstellar and Solar System environments. Here, laboratory experiments can predict where and how (reaction mechanisms; chemicals necessary) in extraterrestrial environments and in the interstellar medium complex, carbon bearing molecules can be formed on interstellar grains and in the gas phase. This paper overviews the experimental setups utilized in our laboratory to mimic the chemical processing of gas phase and solid state (ices) environments. These are a crossed molecular beams machine (3) and a surface scattering setup (4). We also present typical results of each setup (formation of amino acids, aldehydes, epoxides; synthesis of hydrogen terminated carbon chains as precursors to complex PAHs and to carbonaceous dust grains in general; nitriles as precursor to amino acids).

Jamieson, C. S.

Modern insights into the mechanisms of neptunium oxalate decomposition

Neptunium oxalate (Np(C 2 O 4 ) 2 ·6H 2 O) is a historically relevant solid phase used in nuclear processing as a precursor for neptunium dioxide (NpO 2 ). Although Np oxalate has been synthesized and used for NpO 2 production for decades, the thermal decomposition mechanism of this phase remains poorly understood and has not been evaluated in over 30 years. Conflicting reports in historical literature suggest either a direct conversion from anhydrous oxalate to NpO 2 or a decomposition that includes the formation of Np carbonate or oxidized Np intermediate phases. In this work, we reexamine the decomposition pathway of Np(C 2 O 4 ) 2 ·6H 2 O using thermal analysis coupled with evolved gas analysis and temperature-dependent Raman spectroscopy to elucidate decomposition mechanisms and intermediate phases using modern analytical techniques. Thermal analysis revealed a three-stage decomposition process, including dehydration below 200 °C, oxalate breakdown between 170 and 370 °C, and NpO 2 formation by 500 °C. However, an unidentified plateau in the thermal data was observed during measurements. Raman spectroscopy confirmed the stages of decomposition, and in the analysis of potential intermediate phases, no carbonate phases or Np 2 O 5 were identified. Raman data suggest that residual oxalate or nonstoichiometric oxide are present during decomposition before pure NpO 2 is formed. These findings clarify aspects of the Np oxalate decomposition mechanism and address longstanding discrepancies in the literature, with a specific focus on Np-specific materials chemistry.

Lawson, Kathryn M. [Oak Ridge National Laboratory