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NASA NTRS1979

The impact of rare earth cobalt permanent magnets on electromechanical device design

Specific motor designs which employ rare earth cobalt magnets are discussed with special emphasis on their unique properties and magnetic field geometry. In addition to performance improvements and power savings, high reliability devices are attainable. Both the mechanism and systems engineering should be aware of the new performance levels which are currently becoming available as a result of the rare earth cobalt magnets.

Fisher, R. L.↗

DOE OSTI2023

Effects of rare-earth magnetism on the superconducting upper critical field in infinite-layer nickelates

The search for superconductivity in infinite-layer nickelates was motivated by analogy to the cuprates, and this perspective has framed much of the initial consideration of this material. However, a growing number of studies have highlighted the involvement of rare-earth orbitals; in that context, the consequences of varying the rare-earth element in the superconducting nickelates have been much debated. Here, we show notable differences in the magnitude and anisotropy of the superconducting upper critical field across the La-, Pr-, and Nd-nickelates. These distinctions originate from the 4f electron characteristics of the rare-earth ions in the lattice: They are absent for La 3+ , nonmagnetic for the Pr 3+ singlet ground state, and magnetic for the Nd 3+ Kramer’s doublet. The unique polar and azimuthal angle-dependent magnetoresistance found in the Nd-nickelates can be understood to arise from the magnetic contribution of the Nd 3+ 4f moments. Such robust and tunable superconductivity suggests potential in future high-field applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2026

Thermal Management for a Novel Non-Heavy Rare-Earth Interior Permanent Magnet Machine

The work presents a thermal management solution for a novel non-heavy rare-earth permanent magnet machine being developed at Oak Ridge National Laboratory. The motor has been designed to minimize losses while maximizing performance for a range of speeds and power ratings. The novel motor design reduces rare-earth magnet usage, thereby avoiding supply chain issues. The motor component heat losses are established for operating windows and desired performance. These heat losses, along with windage losses, are being used to develop cooling solutions for different components of this machine. A novel thermal management solution for stators and rotors has been developed, and progress is presented in this paper. The stator cooling is achieved with the help of water-ethylene glycol flowing over the finned aluminum stator jacket, and rotor cooling with automatic transmission fluid passing through novel channels designed in the rotor laminations. The attempt is to establish effective cooling of the stator winding, laminations, and rotor magnets. A 3D conjugate heat transfer model has been developed for overall thermal analysis to establish a down- selected thermal management solution for the machine. The model, in addition to estimated component heat losses, includes windage losses and its impact on rotor and stator cooling. Overall, the work presents a workable thermal solution for the interior permanent magnet machine with potential for further improvements. Future work will involve establishing end winding and refinement of other end parts of the machine with the aim of establishing a robust thermal management solution. The work will also focus on different shapes (e.g., round, non-round, presence of wedges) of rotor-stator gaps and investigate windage losses and their impact on thermal management for higher rotational speeds for the machine.

30 DIRECT ENERGY CONVERSION↗

DOE OSTI2024

Development of Leaching Processes for the Recovery of Rare Earth Elements from Acid Mine Drainage Precipitates

Acid mine drainage (AMD) has been a challenge for mine operators to address and has had significant environmental impacts when there is a failure to address it. Fortunately, there is a regulation in the US that requires the treatment of AMD before water can be discharged into the environment. AMD is generated when sulfide minerals are exposed to water and air from mining. The acidic water then leaches metals from the surrounding rock, creating the potential for environmental contamination of this acidic water containing dissolved metals. AMD can contain high concentrations of metals like iron, aluminum, and manganese and also have been shown to contain trace concentrations of critical minerals, including rare earth elements (REEs). This environmental waste stream is now being researched as a potential source for REEs. There is a patented process for processing and extracting REEs from AMD which produces rare earth oxide preconcentrate (REOP) from AMD treatment precipitates and a final stage mixed rare earth oxide (MREO) product. This body of research examines a selective leaching process for each of these products and determines the activation energy associated with the leaching processes. Acid leaching with HCl was examined to selectively leach REEs from REOP while contaminant metals remained in the solid residue. The maximum leaching recovery of the REEs from the REOP was approximately 90% and an activation energy of 6.4 kJ/mol at pH 3.0. Ammonium chloride leaching was examined to selectively remove contaminant metals from a MREO product. The ammonium chloride process successfully leached major contaminant metals in excess of 85% recovery and had a maximum activation energy of 40.0 kJ/mol.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2022

SCALED-PRODUCTION OF RARE EARTH OXIDES AND CRITICAL MATERIALS FROM COAL-BASED SOURCES

A projected exponential increase in the production of electric vehicles and high-end advanced technologies including those used in the defense industrial is expected to require nearly double the amount of rare earth elements (REEs) and critical elements currently available worldwide. As such, recovery from secondary sources such as coal and coal byproducts may be needed to meet the increased demand. A project has been initiated to evaluate methods and technologies integrated in an existing rare earth pilot plant that have the potential to improve the economics of extracting rare earths and critical materials from coal-based materials. This presentation will provide details about the technologies and results from pilot plant testing.

Honaker, Rick Q↗

DOE OSTI2022

A Hybrid Experimental and Theoretical Approach to Optimize Recovery of Rare Earth Elements from Acid Mine Drainage Precipitates by Oxalic Acid Precipitation

The development of processing techniques for the extraction of rare earth elements and critical minerals (REE/CM) from acid mine drainage precipitates (AMDp) has attracted increased interest in recent years. Processes under development often utilize a standard hydrometallurgical approach that includes leaching and solvent extraction followed by oxalic acid precipitation and calcination to produce a final rare earth oxide product. Impurities such as Ca, Al, Mn, Fe and Mg can be detrimental in the oxalate precipitation step and a survey of the literature showed limited data pertaining to the REE precipitation efficiency in solutions with high impurity concentrations. As such, a systematic laboratory-scale precipitation study was performed on a strip solution generated by the acid leaching and solvent extraction of an AMDp feedstock to identify the optimal processing conditions that maximize REE precipitation efficiency and product purity while minimizing the oxalic acid dosage. Given the unique chemical characteristics of AMDp, the feed solution utilized in this study contained a moderate concentration of REEs (440 mg/L) as well a significant concentration (>7000 mg/L total) of non-REE contaminants such as Ca, Al, Mn, Fe and Mg. Initially, a theoretical basis for the required oxalic acid dose, optimal pH and predicted precipitation efficiency was established by solution equilibrium calculations. Following the solution chemistry calculations, bench-scale precipitation experiments were conducted and these test results indicate that a pH of 1.5 to 2, a reaction time of more than 2 h and an oxalic acid dosage of 30 to 40 g/L optimized the REEs recovery of at ~95% to nearly 100% for individual REE species. The test results validated the optimal pH predicted by the solution chemistry calculations (1.5 to 5); however, the predicted dosage needed for complete REE recovery (10 g/L) was significantly lower than the experimentally-determined dosage of 30 to 40 g/L. The reason for this discrepancy was determined to be due to the large concentration of impurities and large number of potential metal complexes that cause inaccuracies in the solution equilibrium calculations. Based on these findings, a hybrid experimental and theoretical approach is proposed for future oxalic acid precipitation optimization studies.

oxalic acid precipitation↗

NASA NTRS1972

Rare earths and other trace elements in Luna 16 soil.

An analysis has been made of four small samples of material brought to earth by the Luna 16 mission, with the aim to determine rare earths and other trace elements in these samples. The analytical results are tabulated, and the rare earth abundances are compared with the average for chondrites. A comparison is also made with the results of similar analyses of Apollo samples.

Helmke, P. A.↗

DOE OSTI2024

Technoeconomic Assessment of Phosphoric Acid and Rare Earth Element Recovery from Phosphoric Acid Sludge

Sustainability faces many challenges, including the availability of materials necessary for technological advancement. Rare earth elements (REEs), for example, are key materials for several manufacturing industries that can unlock renewable energy and sustainable development. In this study, a decanter centrifuge has been employed to successfully separated phosphoric acid and REE-containing particles from phosphoric acid sludge with concentrations ranging from 1000 to 2200 ppm REEs. Operating efficiently with up to 35 wt.% solids, the centrifuge was demonstrated to achieve approximately 95% phosphoric acid recovery and 90% REE recovery in a single pass, eliminating the need for additional processing steps. This breakthrough supports a proposed rare earth oxide (REO) recovery process integrating phosphoric acid (PA), elemental phosphorus (P4), and REO into two potential pathways: PA-REO and PA-P4-REO. These processes aim to reintroduce recovered phosphoric acid into the main product to significantly increase output and revenue. Post-separation, phosphorus-rich particles can be converted to P4, while REE-containing solids undergo further treatment including acid leaching, extraction/stripping, precipitation, and calcination to produce a marketable REO material. Technoeconomic analysis indicates promising profitability, with the PA-REO process showing a delta net present value (ΔNPV) of USD 441.8 million over a 12-year period and expected return within a year of construction, while the PA-P4-REO process yields a ΔNPV of USD 178.7 million over a 12-year return period. Both pathways offer robust financial prospects and demonstrate the feasibility of commercial-scale REO recovery from phosphoric acid sludge, offering an economically feasible approach to produce REEs for future sustainable development challenges related to sustainability.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Global rare earth element resources: A concise review

Deposits enriched in rare earth elements (REEs) are abundant and diverse in mineralogy, but those of current economic value have extremely limited geographic distribution. Due to rapidly increasing demand and concerns about supply chain security, new and improved methods of prospecting, beneficiation, separation, purification, and recycling are needed. By overviewing the types and geographic distribution of REE reserves globally, their petrogenesis and major mineralogic assemblages, this review aims to provide a foundation for posing new directions for research and development in these areas. In conclusion, our review also seeks to provide a concise summary of important background information that is accessible to researchers from a variety of disciplines who are seeking to engage in this rapidly expanding field.

58 GEOSCIENCES↗

DOE OSTI2026

A Comparative Study of Ethanol Upgrading to Butadiene Over Rare Earth Elements Incorporated in Dealuminated Beta Zeolites

Copper and rare earth element-containing dealuminated Beta zeolites (CuREE/deAlBeta) are promising catalysts for the conversion of ethanol to C 3+ olefins en route to sustainable aviation fuel. Product selectivities over CuREE/deAlBeta depend on the identity of the REE. Here, in this study, a suite of La/deAlBeta catalysts of varied La loading are prepared, and their reactivities, selectivities, and apparent C-C coupling kinetics in the cascade reaction between ethanol and acetaldehyde are reported. Ex situ and in situ titrations to quantify Lewis acidic La sites quantify distinct numbers of sites, suggesting a distribution of site types. Across a series of REE/deAlBeta catalysts (REE = Y, La, Lu, Yb, Gd), the selectivity to secondary products correlates with the pyridine heats of adsorption at REE Lewis acid sites. The turnover frequency (per Lewis acid site) for C–C coupling was similar across the series of REE/deAlBeta catalysts. Y/deAlBeta and La/deAlBeta, which have the most disparate secondary product selectivities, had similar kinetics for C–C coupling. These findings demonstrate the complexity of quantifying active sites in REE/deAlBeta zeolites, and the sensitivity of the selectivity, but not the reactivity for C–C coupling, to the identity of the REE atom in REE/deAlBeta zeolites.

alcohol upgrading↗

NASA NTRS2011

Improved Rare-Earth Emitter Hollow Cathode

An improvement has been made to the design of the hollow cathode geometry that was created for the rare-earth electron emitter described in Compact Rare Earth Emitter Hollow Cathode (NPO-44923), NASA Tech Briefs, Vol. 34, No. 3 (March 2010), p. 52. The original interior assembly was made entirely of graphite in order to be compatible with the LaB6 material, which cannot be touched by metals during operation due to boron diffusion causing embrittlement issues in high-temperature refractory materials. Also, the graphite tube was difficult to machine and was subject to vibration-induced fracturing. This innovation replaces the graphite tube with one made out of refractory metal that is relatively easy to manufacture. The cathode support tube is made of molybdenum or molybdenum-rhenium. This material is easily gun-bored to near the tolerances required, and finish machined with steps at each end that capture the orifice plate and the mounting flange. This provides the manufacturability and robustness needed for flight applications, and eliminates the need for expensive e-beam welding used in prior cathodes. The LaB6 insert is protected from direct contact with the refractory metal tube by thin, graphite sleeves in a cup-arrangement around the ends of the insert. The sleeves, insert, and orifice plate are held in place by a ceramic spacer and tungsten spring inserted inside the tube. To heat the cathode, an insulating tube is slipped around the refractory metal hollow tube, which can be made of high-temperature materials like boron nitride or aluminum nitride. A screw-shaped slot, or series of slots, is machined in the outside of the ceramic tube to constrain a refractory metal wire wound inside the slot that is used as the heater. The screw slot can hold a single heater wire that is then connected to the front of the cathode tube by tack-welding to complete the electrical circuit, or it can be a double slot that takes a bifilar wound heater with both leads coming out the back. This configuration replaces the previous sheathed heater design that limited the cycling-life of the cathode.

Goebel, Dan M.↗

DOE OSTI2020

Leaching Kinetics of Rare Earth Elements from Fire Clay Seam Coal

Recovery of rare earth elements (REEs) from coal samples collected from the Fire Clay coal seam using diluted mineral acid solutions was investigated. The initial processing step was coal recovery using conventional froth flotation which concentrated the REEs in tailing material resulting in an upgrade to values around 700 ppm on a dry whole mass basis. Leaching experiments were performed on the flotation tailings material using a 1.2 M sulfuric acid solution adjusted to a temperature of 75 °C to study the extractability of REEs from coal material. The effect of particle size, leaching time, leaching temperature, and solid concentration on REE leaching recovery were evaluated. The kinetic data obtained from leaching over a range of temperatures suggested that the leaching process follows the shrinking core model with possibly a mixed control mechanism that may be a result of several heterogenous materials leaching simultaneously. Leaching recovery increased rapidly at the beginning of the reaction then slowed as the system reached equilibrium. The apparent activation energy determined from test data obtained over a range of temperatures using 1 M sulfuric acid was 36 kJ/mol for the first 20 min of reaction time and 27 kJ/mol for the leaching period between 20 and 120 min. The leaching of light REEs during the initial stage was determined to be driven by a chemical reaction, followed by the formation of a product layer, which required lower activation energy in the later stage of leaching. In regards to the heavy REEs, the major mechanism for leaching is desorption and the product layer formation does not affect the heavy REEs significantly.

58 GEOSCIENCES↗

DOE OSTI2025

X-ray absorption spectroscopy of lanmodulin-derived peptides bound to rare earth elements

A sustainable and robust supply chain of rare earth elements (REEs) is necessary to meet our consumer, national security and clean energy goals. However, current intra-REE separation technologies (e.g. solvent extraction) are costly and carry a heavy environmental burden. Therefore, the development of new aqueous based ligands that are selective for individual REEs will be integral in future REE production systems. To develop these ligands, an understanding of how ligand coordination structure relates to selectivity is imperative. We used X-ray absorption spectroscopy (XAS) to observe the local structure around four lanthanide (Ln) ions (La, Ce, Pr and Nd) complexed by water and several relevant chelating ligands [lanmodulin EF-hand 1 peptides (LanM1), ethylenediaminetetraacetic acid (EDTA), aminotris(methylenephosphonic acid) (ATMP) and citric acid]. To collect these liquid-phase XAS spectra, we developed a new flow cell that prevents bubble interference and beam damage to the samples. In the X-ray absorption near-edge structure (XANES), we observed energy shifts in the white line, white line broadening and differences in the white line intensity of different Ln–ligand complexes between ligands. In the extended X-ray absorption fine structure (EXAFS), we distinguished differences in peak intensity and distance between coordinating ligands. Differences in the local coordination structure between Ln–LanM1 peptide complexes were more subtle compared with the other ligands (La–water, La–EDTA, La–ATMP and La–citric acid complexes). Further XANES and EXAFS studies, in combination with modelling and other techniques, could greatly improve our structural knowledge of how these aqueous ligands bind Ln ions and how they can be used to design more selective ligands for more efficient and sustainable REE separations.

EDTA↗

NASA NTRS1999

Rare Earth Doped Yttrium Aluminum Garnet (YAG) Selective Emitters

As a result of their electron structure, rare earth ions in crystals at high temperature emit radiation in several narrow bands rather than in a continuous blackbody manner. This study presents a spectral emittance model for films and cylinders of rare earth doped yttrium aluminum garnets. Good agreement between experimental and theoretical film spectral emittances was found for erbium and holmium aluminum garnets. Spectral emittances of films are sensitive to temperature differences across the film. For operating conditions of interest, the film emitter experiences a linear temperature variation whereas the cylinder emitter has a more advantageous uniform temperature. Emitter efficiency is also a sensitive function of temperature. For holminum aluminum garnet film the efficiency is 0.35 at 1446K but only 0.27 at 1270 K.

Chubb, Donald L.↗

DOE OSTI2025

Extraction and Separation of Rare-Earth Elements from Coal Fly Ash and Leachate using a Recyclable Ionic Liquid

Coal fly ash (CFA) can be a promising source for recovering rare-earth elements (REEs), as it contains a broad range of REEs with average concentrations frequently exceeding those in traditional rare earth mines. Recent research from our group has demonstrated that REEs can be preferentially extracted from CFA solids using a recyclable ionic liquid (IL), betainium bis-(trifluoromethylsulfonyl)imide ([Hbet][Tf2N]). When CFA was heated with the mixture of IL and an aqueous solution above 65°C, most leached REEs partitioned into the IL phase and were separated from the bulk elements. Subsequent acid stripping of the REE-loaded IL removed the REEs and regenerated the IL for reuse in multiple extraction cycles. This IL-based REE-CFA recovery method has been applied to ten CFA samples derived from different coal sources, including ash recovered from disposal ponds. Analysis of 34 elements confirmed the process consistently achieved high REE recovery efficiency, with strong selectivity over bulk and trace elements across diverse CFA types. In addition to the IL-solid extraction, the performance of [Hbet][Tf2N] in extracting REEs from fly-ash leachates have been evaluated by four commonly used leaching reagents, including HCl, HNO3, H2SO4, and citrate. During the IL-leachate extraction, [Hbet][Tf2N] was mixed and heated with a Class C fly ash leachate generated from each leaching reagent, followed by an acid stripping. It was observed that the partitioning and recovery of REEs increased as the leachate pH increased from 3 to 11. Among the investigated leachates, HCl and citrate proved to be the most compatible with IL extraction, exhibiting a slightly higher REE recovery and a lower non-REE co-extraction compared to the IL-solid extraction. Sc, Y, Nd, Sm, Gd, Dy, and Yb consistently showed a high recovery rate from both CFA solids and leachates. Notably, Pr, Tb, and Ho, which were not previously leached from the CFA solids, were partially recovered from the leachates. Overall, our studies revealed the strong potential of [Hbet][Tf2N] for effectively recovering REEs from leachates, highlighting its applicability as a sustainable strategy for other aqueous REE feedstocks. Furthermore, a techno-economic analysis will be performed to quantify the economic viability of the IL-based REE recovery method and guide future process improvement.

42 ENGINEERING↗

DOE OSTI2023

Quasi-one-dimensional Ising-like antiferromagnetism in the rare-earth perovskite oxide TbScO 3

The rare-earth perovskite TbScO 3 has been widely used as a substrate for the growth of epitaxial ferroelectric and multiferroic thin films, while its detailed low-temperature magnetic properties were rarely reported. In this paper, we performed detailed magnetization, specific heat, and single crystal neutron scattering measurements, along with the crystalline electric field calculations to study the low-temperature magnetic properties of TbScO 3. All our results suggest the magnetic Tb 3+ has an Ising-like pseudo-doublet ground state at low temperatures. Due to the constrain of local point symmetry, these Tb 3+ Ising moments are confined in the ab plane with a tilt angle of φ=±48° to the a axis. In zero field, the system undergoes an antiferromagnetic phase transition at T N =2.53 K, and forms a G x A y noncollinear magnetic structure below T N . Here, we find the dipole-dipole interactions play an important role to determine the magnetic ground state, which are also responsible for the quasi-one-dimensional magnetism in TbScO 3 . The significant anisotropic diffuse scatterings further confirm the quasi-one-dimensional magnetism along the c axis. The magnetic phase diagram with the field along the easy b axis is well established. In addition to the G x A y antiferromagnetic state, there is an exotic field-induced phase emerged near the critical field B c ≃0.7 T, where three-dimensional magnetic order is suppressed but strong one-dimensional correlations may still exist.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Mediating Photochemical Reaction Rates at Lewis Acidic Rare Earths by Selective Energy Loss to 4f-Electron States

Manifesting chemical differences in individual rare earth (RE) element complexes is challenging due to the similar sizes of the tripositive cations and the corelike 4f shell. In this work, we disclose a new strategy for differentiating between similarly sized Dy 3+ and Y 3+ ions through a tailored photochemical reaction of their isostructural complexes in which the f-electron states of Dy 3+ act as an energy sink. Complexes RE(hfac) 3 (NMMO) 2 (RE = Dy (2-Dy) and Y (2-Y), hfac = hexafluoroacetylacetonate, and NMMO = N-methylmorpholine-N-oxide) showed variable rates of oxygen atom transfer (OAT) to triphenylphosphine under ultraviolet (UV) irradiation, as monitored by 1 H and 19 F NMR spectroscopies. Ultrafast transient absorption spectroscopy (TAS) identified the excited state(s) responsible for the photochemical OAT reaction or lack thereof. Competing sensitization pathways leading to excited-state deactivation in 2-Dy through energy transfer to the 4f electron manifold ultimately slows the OAT reaction at this metal cation. The measured rate differences between the open-shell Dy 3+ and closed-shell Y 3+ complexes demonstrate that using established principles of 4f ion sensitization may deliver new, selective modalities for differentiating the RE elements that do not depend on cation size.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Phase stability and tensorial thermal expansion properties of single to high-entropy rare-earth disilicates

Temperature limitations in nickel-base superalloys have resulted in the emergence of SiC-based ceramic matrix composites as a viable replacement for gas turbine components in aviation applications. Higher operating temperatures allow for reduced fuel consumption but present a materials design challenge related to environmental degradation. Rare-earth disilicates (RE 2 Si 2 O 7 ) have been identified as coatings that can function as environmental barriers and minimize hot component degradation. In this work, single- and multiple-component rare-earth disilicate powders were synthesized via a sol-gel method with compositions selected to exist in the monoclinic C 2/m phase (β phase). Phase stability in multiple cation compositions was shown to follow a rule of mixtures and the C 2/m phase could be realized for compositions that contained up to 25% dysprosium, which typically only exists in a triclinic, P $\bar1$, phase. All compositions exhibited phase stability from room temperature to 1200°C as assessed by X-ray diffraction. The thermal expansion tensors for each composition were determined from high-temperature synchrotron X-ray diffraction and accompanying Rietveld refinements. It was observed that ytterbium-containing compositions had larger changes in the α 31 shear component with increasing temperature that led to a rotation of the principal axes. Principal axes rotation of up to 47° were observed for ytterbium disilicate. The results suggest that microstructure design and crystallographic texture may be essential future avenues of investigation to ensure thermo-mechanical robustness of rare-earth disilicate environmental barrier coatings.

36 MATERIALS SCIENCE↗