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All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Accelerating Discovery of Solid‐State Thin‐Film Metal Dealloying for 3D Nanoarchitecture Materials Design through Laser Thermal Gradient Treatment

Thin‐film solid‐state metal dealloying (thin‐film SSMD) is a promising method for fabricating nanostructures with controlled morphology and efficiency, offering advantages over conventional bulk materials processing methods for integration into practical applications. Although machine learning (ML) has facilitated the design of dealloying systems, the selection of key thermal treatment parameters for nanostructure formation remains largely unknown and dependent on experimental trial and error. To overcome this challenge, a workflow enabling high‐throughput characterization of thermal treatment parameters is demonstrated using a laser‐based thermal treatment to create temperature gradients on single thin‐film samples of Nb‐Al/Sc and Nb‐Al/Cu. This continuous thermal space enables observation of dealloying transitions and the resulting nanostructures of interest. Through synchrotron X‐ray multimodal and high‐throughput characterization, critical transitions and nanostructures can be rapidly captured and subsequently verified using electron microscopy. The key temperatures driving chemical reactions and morphological evolutions are clearly identified. While the oxidation may influence nanostructure formation during thin‐film treatment, the dealloying process at the dealloying front involves interactions solely between the dealloying elements, highlighting the availability and viability of the selected systems. Further, this approach enables efficient exploration of the dealloying process and validation of ML predictions, thereby accelerating the discovery of thin‐film SSMD systems with targeted nanostructures.

36 MATERIALS SCIENCE↗
NASA NTRS2010

Acoustic Performance of Novel Fan Noise Reduction Technologies for a High Bypass Model Turbofan at Simulated Flights Conditions

Two novel fan noise reduction technologies, over the rotor acoustic treatment and soft stator vane technologies, were tested in an ultra-high bypass ratio turbofan model in the NASA Glenn Research Center s 9- by 15-Foot Low-Speed Wind Tunnel. The performance of these technologies was compared to that of the baseline fan configuration, which did not have these technologies. Sideline acoustic data and hot film flow data were acquired and are used to determine the effectiveness of the various treatments. The material used for the over the rotor treatment was foam metal and two different types were used. The soft stator vanes had several internal cavities tuned to target certain frequencies. In order to accommodate the cavities it was necessary to use a cut-on stator to demonstrate the soft vane concept.

Elliott, David M.↗
NASA NTRS2017

Diamond-Dispersed Fiber-Reinforced Composite for Superior Friction and Wear Properties in Extreme Environments and Method for Fabricating the Same

Systems, methods, and articles of manufacture related to composite materials are discussed herein. These materials can be based on a mixture of diamond particles with a matrix and fibers or fabrics. The matrix can be formed into the composite material through optional pressurization and via heat treatment. These materials display exceptionally low friction coefficient and superior wear resistance in extreme environments.

Street, Kenneth↗
NASA NTRS1998

Vapor-Phase Stoichiometry and Heat Treatment of CdTe Starting Material for Physical Vapor Transport

Six batches of CdTe, having total amounts of material from 99 to 203 g and gross mole fraction of Te, X(sub Te), 0.499954-0.500138, were synthesized from pure Cd and Te elements. The vapor-phase stoichiometry of the assynthesized CdTe batches was determined from the partial pressure of Te2, P(sub Te2) using an optical absorption technique. The measured vapor compositions at 870 C were Te-rich for all of the batches with partial pressure ratios of Cd to Te2, P(sub Cd)/P(sub Te2), ranging from 0.00742 to 1.92. After the heat treatment of baking under dynamic vacuum at 870 C for 8 min, the vapor-phase compositions moved toward that of the congruent sublimation, i.e. P(sub Cd)/P(sub Te2) = 2.0, with the measured P(sub Cd)/P(sub Te2) varying from 1.84 to 3.47. The partial pressure measurements on one of the heat-treated samples also showed that the sample remained close to the congruent sublimation condition over the temperature range 800-880 C.

Su, Ching-Hua↗
DOE OSTI2020

Hydropower Geotechnical Foundations: Current Practice and Innovation Opportunities for Low-Head Applications

Hydropower is a renewable energy resource that produces electricity from flowing water under pressure. Engineered hydropower structures, such as dams, are used to create a hydraulic head, enabling a turbinegenerator unit to convert pressurized flow into electricity. While hydropower has been a source of renewable energy since antiquity, new development in the United States has slowed in recent decades. Based on recent resource assessments, the largest opportunity to expand hydropower in the United States is from new stream-reach development (i.e., new hydropower development along stream-reaches that do not currently have hydroelectric facilities or other forms of infrastructure, such as dams). Roughly 75% of identified new stream-reach development potential is from low-head sites (less than 30 ft of head), which typically suffer from smaller power densities and higher normalized costs, given economies of scale. Hydropower developers and other stakeholders are thus interested in strategies to reduce initial capital costs while practicing sustainable development to maximize environmental compatibility with minimal disruption to natural aquatic life, sediment, and water flows. Historically, civil works have represented a significant cost driver for new hydropower development, with the foundation system representing a major cost component and source of uncertainty. The foundation system is the collection of engineered structural features (e.g. cutoff trenches, walls, grouting, anchors) constructed at or below the preconstruction ground surface that interfaces between the overlying structures (superstructures) and the bed material below (subsurface). Development of a hydropower foundation system must consider the various characteristics of the surrounding stream environment and subsurface while adhering to the engineering requirements of the superstructure that it supports. The care of water, excavation, and other construction activities are important features of foundation design and construction. The design and construction cost of the foundation system is largely dependent on the site geology and riverbed composition and is influenced by the level of geotechnical assessment required and conducted. Thus, a hydropower facility’s geotechnical foundation is often highly site-specific, with proper site selection and assessment being important to project success. The foundation system is designed to provide structural stability (of the foundation and dam), limit seepage, ensure public safety, and maintain functionality for the project life, during both construction and facility operations. Inadequate foundation or dam design can result in dam failure and the uncontrolled release of significant volumes of water, which could cause a high number of casualties and extensive property damage downstream of the failure. According to the Association of State Dam Safety Officials, approximately 30% of all historical dam failures in the United States are attributed to foundation or abutment defects, and another 20% are attributed to piping or seepage through the embankment, foundation, or abutment. To ameliorate these safety considerations, foundations often require massive amounts of construction material (e.g., grout, concrete, engineered dam fill) and long construction times. Foundation design also requires significant analysis prior to construction because the initial in-stream and abutment subsurface conditions are site-specific, and sufficient data for them often are lacking. Current practice requires on-site assessment, using expensive drilling and invasive and non-invasive investigation methods, to determine the expected cost of foundation material and treatment. Additionally, foundation construction often requires site dewatering (and other care of water activities), which involves constructing temporary diversion structures upstream and often downstream, called cofferdams, and water diversion systems that route water around the construction site. Cofferdams and water diversion systems can drastically increase construction costs and contribute to environmental disruption, including modification of flow patterns and benthic habitats. Given the technical, economic, and environmental challenges associated with hydropower foundations, opportunities exist to improve the current state of practice and to develop new and innovative solutions to Hydropower is a renewable energy resource that produces electricity from flowing water under pressure. Engineered hydropower structures, such as dams, are used to create a hydraulic head, enabling a turbinegenerator unit to convert pressurized flow into electricity. While hydropower has been a source of renewable energy since antiquity, new development in the United States has slowed in recent decades. Based on recent resource assessments, the largest opportunity to expand hydropower in the United States is from new stream-reach development (i.e., new hydropower development along stream-reaches that do not currently have hydroelectric facilities or other forms of infrastructure, such as dams). Roughly 75% of identified new stream-reach development potential is from low-head sites (less than 30 ft of head), which typically suffer from smaller power densities and higher normalized costs, given economies of scale. Hydropower developers and other stakeholders are thus interested in strategies to reduce initial capital costs while practicing sustainable development to maximize environmental compatibility with minimal disruption to natural aquatic life, sediment, and water flows. Historically, civil works have represented a significant cost driver for new hydropower development, with the foundation system representing a major cost component and source of uncertainty. The foundation system is the collection of engineered structural features (e.g. cutoff trenches, walls, grouting, anchors) constructed at or below the preconstruction ground surface that interfaces between the overlying structures (superstructures) and the bed material below (subsurface). Development of a hydropower foundation system must consider the various characteristics of the surrounding stream environment and subsurface while adhering to the engineering requirements of the superstructure that it supports. The care of water, excavation, and other construction activities are important features of foundation design and construction. The design and construction cost of the foundation system is largely dependent on the site geology and riverbed composition and is influenced by the level of geotechnical assessment required and conducted. Thus, a hydropower facility’s geotechnical foundation is often highly site-specific, with proper site selection and assessment being important to project success. The foundation system is designed to provide structural stability (of the foundation and dam), limit seepage, ensure public safety, and maintain functionality for the project life, during both construction and facility operations. Inadequate foundation or dam design can result in dam failure and the uncontrolled release of significant volumes of water, which could cause a high number of casualties and extensive property damage downstream of the failure. According to the Association of State Dam Safety Officials, approximately 30% of all historical dam failures in the United States are attributed to foundation or abutment defects, and another 20% are attributed to piping or seepage through the embankment, foundation, or abutment. To ameliorate these safety considerations, foundations often require massive amounts of construction material (e.g., grout, concrete, engineered dam fill) and long construction times. Foundation design also requires significant analysis prior to construction because the initial in-stream and abutment subsurface conditions are site-specific, and sufficient data for them often are lacking. Current practice requires on-site assessment, using expensive drilling and invasive and non-invasive investigation methods, to determine the expected cost of foundation material and treatment. Additionally, foundation construction often requires site dewatering (and other care of water activities), which involves constructing temporary diversion structures upstream and often downstream, called cofferdams, and water diversion systems that route water around the construction site. Cofferdams and water diversion systems can drastically increase construction costs and contribute to environmental disruption, including modification of flow patterns and benthic habitats. Given the technical, economic, and environmental challenges associated with hydropower foundations, opportunities exist to improve the current state of practice and to develop new and innovative solutions to challenges frequently encountered with traditional approaches. With this understanding, it is critically important to understand and document the current state of practice for hydropower geotechnical foundations, identify key challenges, and define opportunities for innovative solutions. To this end, this report documents the current state of practice across the three main phases of geotechnical foundation development: (1) geotechnical site assessment, (2) design, and (3) construction for hydropower systems. It also describes the major challenges with conventional approaches and identifies opportunities for innovation to reduce hydropower foundations costs, timelines, and risks. Key takeaways from this report include the following: Approximately 80% of available low-head sites are expected to have foundations on soil beds rather than rock beds, suggesting that rockfill and earthfill dams may be the most cost-effective conventional dam type for new projects.; Geotechnical and geologic investigation activities are time-consuming and expensive but are essential to define the parameters and criteria needed for foundation design.; Certain riverbed soil and bedrock types present significant technical challenges or require expensive foundation construction, which can prove financially prohibitive for low-head project development.; Modular hydropower design and prefabricated modular foundations represent a promising but unproven paradigm for new hydropower development. Design and construction approaches using optimized and highly repeatable, reliable components would benefit project cost, time, and risk but require additional research and development.; Temporary construction features for foundations, including cofferdams, water diversion, and water control systems, can prove costly and have inherent construction risk.; For economically viable development, hydropower geotechnical foundations should be limited to 4 to 15% of the project’s total initial capital costs. Many proposed projects have experienced cost overruns attributable to foundation difficulties or surprises during construction. These overruns may have been due to inadequate investigations, lack of adequate engineering effort to tailor the structures to site geology and topography, and/or contractual terms, among other considerations.; Challenges for hydropower foundations and opportunities for innovative technology solutions are identified in the following areas (consistent with the three main phases of foundation development): Geotechnical site assessment, Foundation design and materials, Construction methods and technology. Ultimately, this report aims to provide information about geotechnical foundations for low-head hydropower and to motivate transformative technologies to support hydropower growth.

13 HYDRO ENERGY↗
NASA NTRS1993

A numerical treatment of geodynamic viscous flow problems involving the advection of material interfaces

Effective numerical treatment of multicomponent viscous flow problems involving the advection of sharp interfaces between materials of differing physical properties requires correction techniques to prevent spurious diffusion and dispersion. We develop a particular algorithm, based on modern shock-capture techniques, employing a two-step nonlinear method. The first step involves the global application of a high-order upwind scheme to a hyperbolic advection equation used to model the distribution of distinct material components in a flow field. The second step is corrective and involves the application of a global filter designed to remove dispersion errors that result from the advection of discontinuities (e.g., material interfaces) by high-order, minimally dissipative schemes. The filter introduces no additional diffusion error. Nonuniform viscosity across a material interface is allowed for by the implementation of a compositionally weighted-inverse interface viscosity scheme. The combined method approaches the optimal accuracy of modern shock-capture techniques with a minimal increase in computational time and memory. A key advantage of this method is its simplicity to incorporate into preexisting codes be they finite difference, element, or volume of two or three dimensions.

Lenardic, A.↗
DOE OSTI2023

Improved treatment of multi-material cells in thermal radiation transport codes

High-energy-density physics simulations with non-conformal meshes of materials require a multi-material (MM) closure that affects the thermal radiation transport (TRT). We propose a set of novel closures that work for an arbitrary number of materials, both grey and multigroup energy discretizations, and any angular discretization (such as Sn, IMC, or diffusion). For each spatial cell, our closures let each species (ion and electron) of each material have its own temperature, density, and internal energy, but use a single radiation distribution that interacts with all materials within the cell. Our closures maintain energy conservation, do not incur increased computational cost in the TRT solve itself, are compatible with single-material TRT solvers, and do not make any temperature-equilibrium assumptions. Here we test our closures on a wide range of increasingly realistic problems and find them to be robust.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
NASA NTRS1992

Ion beam treatment of potential space materials at the NASA Lewis Research Center

Ion source systems in different configurations, have been used to generate unique morphologies for several NASA space applications. The discharge chamber of a 30 cm ion source was successfully used to texture potential space radiator materials for the purpose of obtaining values of thermal emittance greater than 0.85 at 700 and 900 K. High absorptance surfaces were obtained using ion beam seed texturing, for space radiator materials that were flown on the Long Duration Exposure Facility (LDEF) for 5.8 years in space. An ion source discharge chamber was also used to develop electrode surfaces with suppressed secondary electron emission characteristics for use in collectors in microwave amplifier traveling wave tubes. This was accomplished by sputtering textured carbon onto copper as well as texturing copper using tantalum and molybdenum as sacrificial texture inducing seeding materials. In a third configuration, a dual ion beam system was used to generate high transmittance diamondlike carbon (DLC) films.

Kussmaul, Michael↗
NASA NTRS1992

Effect of heat treatment on stiffness and damping of Sic/Ti-15-3

The effect of heat treatment on material properties of Sic/Ti-15-3 was measured by vibration tests. Heat treatment changes the microstructure, which stiffens the matrix and reduces its damping capacity. Test results illustrate how the changes in matrix material affect the stiffness and damping properties of the composite. Damping was found to be more sensitive than stiffness to microstructural changes in the matrix. Effects of heat treatment temperature and exposure time are presented.

Grady, Joseph E.↗
DOE OSTI2023

Solutionization via Severe Plastic Deformation: Effect on Natural Aging in an Al-Mg-Si-(Mn) Alloy

Shear Assisted Processing and Extrusion (ShAPE), a severe plastic deformation technique that is fast and scalable, was used to produce thin-wall tubing from alloy 6082 (Al-0.8Mg-0.9Si-0.7Mn) with in-situ solutionization during processing quickly followed by quenching. Quench medium and input material heat treatment were varied and natural aging behavior (T1 heat treatment) was evaluated using tensile testing. As-cast input material was found to have higher strength early in post-ShAPE natural aging and homogenized input material was found to have strengthening during natural aging. Compared to air quenching, water quenching gave greater strength both early in and after natural aging. These observations along with microscopy suggest that: 1. air quenching was too slow; 2. as-cast material was not fully solutionized but plastic deformation broke up the coarse intermetallic particles, which provided strengthening; and 3. homogenized material was solutionized well, which led to good natural aging behavior.

Milligan, Brian K.↗
NASA NTRS1992

Effect of heat treatment on stiffness and damping of SiC/Ti-15-3

The effect of heat treatment on material properties of SiC/Ti-15-3 was measured by vibration tests. Heat treatment changes the microstructure, which was found to stiffen the matrix and reduce its damping capacity. Test results indicate how these changes in the matrix affect the corresponding properties of the composite. Measurements show that heat treatment affects damping properties of the composite to a greater extent than stiffness properties. The extent of change in mechanical properties is shown to depend on heat treatment temperature and exposure time.

Grady, Joseph E.↗
NASA NTRS1993

Crystal growth of ZnSe and related ternary compound semiconductors by physical vapor transport

The materials to be investigated are ZnSe and related ternary semiconducting alloys (e.g., ZnS(x)Se(1-x), ZnTe(x)Se(1-x), and Zn(1-x)Cd(x)Se). These materials are useful for opto-electronic applications such as high efficient light emitting diodes and low power threshold and high temperature lasers in the blue-green region of the visible spectrum. The recent demonstration of its optical bistable properties also makes ZnSe a possible candidate material for digital optical computers. The investigation consists of an extensive ground-based study followed by flight experimentation, and involves both experimental and theoretical work. The objectives of the ground-based work are to establish the characteristics of the crystals grown on Earth as a basis for subsequent comparative evaluations of the crystals grown in a low gravity environment and to obtain the experimental data and perform the analyses required to define the optimum parameters for the flight experiments. During the six months of the Preliminary Definition Phase, the research efforts were concentrated on the binary compound ZnSe - the purification of starting materials of Se by zone refining, the synthesis of ZnSe starting materials, the heat treatments of the starting materials, the vapor transport rate measurements, the vapor partial pressure measurements of ZnSe, the crystal growth of ZnSe by physical vapor transport, and various characterization on the grown ZnSe crystals.

Su, Ching-Hua↗
NASA NTRSDate not supplied

Development of Directed Energy Deposited NASA HR-1 to Optimize Properties for Liquid Rocket Engine Applications

Metal additive manufacturing (AM) processes have been demonstrated to be effective at reducing costs and lead times associated with fabrication of complex propulsion component designs. Laser powder directed energy deposition (LP-DED) and laser powder bed fusion (L-PBF) are metal AM technologies that have effectively been used to produce a variety of parts for space applications. These technologies have enabled new designs and materials for these applications. The National Aeronautics and Space Administration (NASA) has identified the need to develop and advance new materials in unique space applications such as high-pressure hydrogen environments. One such metal alloy being developed for these applications is NASA HR-1. A high-strength Fe-Ni based superalloy, NASA HR-1 was designed to resist high pressure hydrogen environment embrittlement, oxidation, and corrosion. AM technologies have enabled the manufacturing of NASA HR-1 to be a feasible material for components in hydrogen environments. Development efforts for NASA HR-1 have completed build and heat treatment optimization, material characterization, thermophysical property testing, and mechanical testing in air and hydrogen environments to mature the understanding of the material. This poster will summarize the development of NASA HR-1 for AM including composition and heat treatment optimization, microstructure characterization, and results of mechanical testing in air and high pressure hydrogen.

NASA HR-1↗
NASA NTRSDate not supplied

Development and Optimization of Additively Manufactured NASA HR-1 for Space Applications

Metal additive manufacturing (AM) processes have been demonstrated to be effective at reducing costs and lead times associated with fabrication of complex propulsion component designs. Laser powder directed energy deposition (LP-DED) and laser powder bed fusion (L-PBF) are metal AM technologies that have effectively been used to produce a variety of parts for space applications. These technologies have enabled new designs and materials for these applications. The National Aeronautics and Space Administration (NASA) has identified the need to develop and advance new materials in unique space applications such as high-pressure hydrogen environments. One such metal alloy being developed for these applications is NASA HR-1. A high-strength Fe-Ni based superalloy, NASA HR-1 was designed to resist high pressure hydrogen environment embrittlement, oxidation, and corrosion. AM technologies have enabled the manufacturing of NASA HR-1 to be a feasible material for components in hydrogen environments. Development efforts for NASA HR-1 have completed build and heat treatment optimization, material characterization, thermophysical property testing, and mechanical testing in air and hydrogen environments to mature the understanding of the material. This presentation will summarize the development of NASA HR-1 for AM including composition and heat treatment optimization, microstructure characterization, and results of mechanical testing in air and high pressure hydrogen.

Additive Manufacturing↗
DOE OSTI2020

Enduring Transuranic Liquid Waste Volume Forecast and Constituent Evaluation (FY20)

The “FY11 Radioactive Liquid Waste (RLW) Influent Boundary Condition Assessment and Forecast” report provided influent volume forecasts that were critical in establishing the design capacity for the new Radioactive Liquid Waste Transuranic (RLW-TRU) capability. The design for the new RLW-TRU capability was paused as the final design was being completed and prior to the transition of the new management and operations contract for Los Alamos National Laboratory (LANL). Recently, NNSA has directed the project to restart and complete the design effort. As part of the restart process, LANL was asked to validate or document any material changes in the influent volumes or constituents that formed the design basis for the new capability. This analysis updates the transuranic liquid waste influents volumes, incorporating the changes in the LANL program of record since the FY11 assessment, and includes a cursory validation of influent constituents. The results of the FY19 update to influent volume forecasts shows: 1) the influent volume of 29,000 L should continue to be used as the project design-basis; 2) There have been no material changes in the operational processes that would change the constituents of concern from either a treatment or material compatibility perspective.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2021

Pilot-Scale Testing of an Integrated Circuit for the Extraction of Rare Earth Minerals and Elements from Coal and Coal Byproducts Using Advanced Separation Technologies

The primary objective of this project was to develop and demonstrate an integrated pilot-scale circuitry for recovering high-value rare earth elements (REEs) from coal and coal byproducts. The target performance was to produce a mixed REE product with content of at least two percent by weight on a dry mass basis in a cost-effective and environmentally benign manner. During the first nine months of the project period (Phase 2 Budget Period 2), pilot plant construction was completed including all field site startup activities such as permitting, engineering design, procurement/bidding, unit fabrication, site construction, equipment installation, module assembly, safety training, and circuit shakedown. During the remaining 21 months of project period (Phase 2 Budget Period 3), detailed field-testing activities were performed including feedstock sample collection and preparation, exploratory testing, circuit modification, detailed parametric study, and performance optimization. A detailed techno-economic analysis was performed based on the pilot plant testing findings which provided various scenarios for REE production. The project successfully accomplished the proposed target performance by producing mixed rare earth oxide (REO) with greater than 90% purity by weight in a continuous pilot scale operation from two distinctly different coarse refuse materials (i.e., West Kentucky No. 13 and Fire Clay coal seams), and at least three secondary sources (i.e., heap leach process and naturally formed acid mine drainage system). Project partners included the University of Kentucky, Virginia Tech, West Virginia University, Alliance Coal, Blackhawk Mining, Mineral Refining Company, and Mineral Separation Technologies. The pilot scale test facility was constructed at a former mining complex owned by Alliance Natural Resource Partners (Alliance Coal). The site was rehabilitated to accommodate the equipment installation, construction and fabrication, electrical power requirement, water line management and containment. The process units constructed and installed included X-ray sorting unit, crushing and grinding unit, physical separation unit, acid leaching unit, solvent extraction unit, and wastewater management unit. A rare earth mineral concentration unit was constructed as a standalone unit for flexible operation. A detailed environmental assessment and control plan was carried out to identify and quantify any potential impacts of the pilot-scale processing circuitry on the human and eco-system health and well-being. Corresponding mitigation strategies and control measures were provided. A conceptual flowsheet was developed to effectively remove thorium and uranium from high purity rare earth oxide mix or any potential radionuclide enriched stream. The two distinct feedstock materials were secured from the Blackhawk Mining Complex in eastern Kentucky where the Fire Clay (Hazard No. 4) seam is processed. The West Kentucky No. 13 (Baker) coarse refuse material was collected from an active process stream at an Alliance coal preparation plant located in western Kentucky. Characterization analysis indicated that both of feed materials generated from the two sources contained >300 ppm of TREEs on a dry whole mass basis which met the requirements for a qualified feed stock. The two feedstocks were further upgraded using a dual x-ray sorter to prepare the feed material for hydrometallurgical circuit. Thermal treatment on feed material prior to leaching was found to: 1) improve the leaching recovery of REEs, 2) increase the leaching kinetics, and 3) allow the leaching reaction to occur at lower acidity. Roasting at 600°C was selected as the pre-treatment condition for both West Kentucky No. 13 and Fire Clay coarse refuse material. Over 40% of leaching recovery was achieved by roasting West Kentucky No. 13 material having a top particle size of 3 mm in the pilot scale operation using 1.2M sulfuric acid leaching at 75OC. Initial pilot scale testing involved continuous operation of the pilot plant for 94 hours. The leaching unit was operated at solid-to-liquid ratio of 1 to 10 (w/v) using 0.5M sulfuric acid solution at a temperature of 75°C. The continuous solvent extraction circuit utilized rougher and cleaner units with DEHPA and TBP as the extractants. An innovative stripping circuit was developed to accumulate the REE concentration in the stripping solution to a level above 600 ppm. A bleed stream from the recycled strip solution was treated using oxalic acid precipitation which produced a high grade rare earth oxalate. The oxalate product was roasted to remove the oxalate which produced a rare earth oxide product having a purity greater 90%. Due to high concentrations of contaminant ions in the pregnant leach solution (PLS), a modified flowsheet was developed that involved pre-concentration of the REEs using multiple stages of precipitation and redissolution. The advantage of this process was improved removal of contamination before the downstream purification process and a significant cost reduction relative to the circuit that utilized the solvent extraction process. The modified circuitry included processes involving leaching, multistage precipitation, redissolution, and oxalate precipitation followed by roasting of the oxalate product. The circuit produced a mixed REO that was 92.96% pure from the initial test. A detailed parametric test plan was carried out which involved varying key parameters including solids feed rate, acid flowrate, acid concentration, multistage precipitation pH, redissolution pH, oxalate precipitation dosage and pH. The response variables included REE recovery, contaminant recovery, REO product grade and overall chemical consumption. Test results indicated that the acid-to-solid ratio is the key parameter to leaching efficiency as performance deteriorated with an increase in solids concentration. The optimal pH determined for REE precipitation and redissolution was 6.5 and 2.5, respectively. Additional tests were conducted to further improve the flowsheet. Recirculating a portion of the PLS to the feed of the leach tanks improved the leaching performance by lowering the pH of the leaching system and reducing the contamination recovery by shortening the residence time. Moreover, the removal of Al prior to REE precipitation significantly reduced the oxalic acid consumption in the oxalate precipitation circuit. The modified circuit produced over 90% grade REO by weight from both West Kentucky No. 13 and Fire Clay coarse refuse material in pilot scale continuous test programs. A case analysis model was developed to project the REE and major contaminants concentration in each PLS stream based on the leaching condition, pH cut point, and oxalic acid dosage. A correlation was established using empirical and semi-empirical models. Using the models, chemical consumption required for each stage was predicted based on the projected performance of the hydrometallurgy circuit. After identifying the optimum conditions, validation tests were carried out for the treatment of both West Kentucky No. 13 and Fire Clay coarse refuse materials in the pilot plant. The actual circuit performance and chemical consumptions were very close to the model predictions. Other than the two coarse refuse sources, several secondary feedstocks were also tested in the pilot plant facility. A “heap leach” system was constructed using the coarse refuse material generated from cleaning the West Kentucky No. 13 seam coal. Using the two stage SX rougher and cleaner circuit, a concentrate with a grade >90% REO was produced while recovering >97% of the REEs from the heap leach PLS. Naturally generated acid mine drainage (AMD) from West Kentucky No.13 mine was processed using the multistage precipitation circuit in the pilot plant in a test conducted for a period of 32 hours. The final grade of the mix RE oxide produced from the AMD was 90.84% with an overall circuit recovery of 64%. The primary source of REE was the selective precipitation steps involving iron and aluminum rejection. The hydrophobic-hydrophilic separation (HHS) process was proven to effectively recover coal from fine waste materials. For REM recovery, the HHS process was able to produce concentrates at grades of approximately 1.8% REE on an ash basis; however, recovery values were typically low, <10%, under the optimal conditions determined in the laboratory-scale testing. Staged testing of the pilot-scale HHS process for coal recovery and semi-continuous laboratory testing for REM testing showed that a total concentration ratio of more than 15x was observed for the REM recovery process. A circuit simulation package was developed for REE extraction and purification using a spreadsheet-based platform (Microsoft Excel). The REESim circuit simulation package is configured to track the mass and volume flows of components passing through a series of unit operations specified and configured by the user. The mass rates can then be utilized by the user to determine important performance indicators such as product mass yields, concentrate purity levels, element-by-element recoveries, and so forth. The techno-economic analysis showed that the roasting and leaching operations were the most expensive capital items, each contributing approximately 30% to the total capital cost. One notable contributor to the high production costs was the low REE recovery observed in the pilot scale trials. The product basket price was shown to have a strong influence on the economic viability of the scenarios, with the scandium price being the most significant influencer. Operating cost was shown to be extremely sensitive to REE recovery, REE feed grade, and leaching acid consumption. An analysis of ten different scenarios for a 500 t/h commercial operation revealed that three were economically favorable, producing internal rates of return varying from 27.7% to 33.1% and payback periods of 4 to 5 years. The project successfully developed and demonstrated a process to recover REEs from coal and coal byproducts in a pilot-plant operation which consistently produced over 90% grade REO mix from varies types of feedstocks. Commercialization analysis showed that the technology readiness level successfully achieved TRL 6 at the end of the project and demonstrated the need and the potential for scaling the process to further advance the technologies toward the goal of providing a domestic supply of REEs at a commercial scale.

01 COAL, LIGNITE, AND PEAT↗