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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

From Quantum to Classical: Sensing Materials, Methods, and Platforms for Energy

This presentation covers several ongoing sensors projects at NETL, including the use of quantum sensors for energy sector applications (e.g. infrastructure monitoring, critical metal detection, grid modernization) as well as NETL-developed materials and platforms for detecting economically critical metals including rare earth elements, cobalt, and aluminum. Taken together, these projects demonstrate NETL's leadership in unleashing American energy through the development of high performance sensors for reliable energy production and consumption.

critical minerals↗
DOE OSTI2025

Development of Luminescent Materials and Instrumentation for Critical Mineral Discovery and Monitoring

Presentation discussing career paths in chemistry as well as how chemical research is applied to address real-world problems. Here, a variety of different materials (metal-organic frameworks, carbon dots, thin films, etc.) are used as luminescent sensors to detect trace quantities of economically critical metals, which are used in applications ranging from renewable energy to national defense. In an application particularly relevant to Western Pennsylvania, the sensor technologies are deployed in coal utilization byproducts including fly ash leachates and acid mine drainage. Taken together, this research presents an exciting path towards reducing the characterization costs associated with metals prospecting and process monitoring, facilitating domestic production of these metals.

analytical chemistry↗
DOE OSTI2025

Chelation ion chromatography as an automated, and cost-effective analytical technique for REE determination: method development and applications

Rare earth elements (REEs), as critical minerals, have important uses in modern energy and technologies, yet are vulnerable to potential supply chain disruptions. To establish domestic REE supply chain, efficient REE detection methods for resource characterization and mineral processing will be needed to accelerate innovations for domestic REE recovery. This study developed a rapid, novel, and cost-effective for REE detection method using ion chromatography (IC) for aqueous samples. Various REE-targeted eluent gradients and post-column agent compositions were tested on the chelation ion chromatography (CIC) with UV-vis detector for optimal separation and quantification of REEs within approximately 20 min. The single-channel pump to deliver the post-column solution to UV-vis detector was replaced with a 4-channel gradient pump, to increase operation and maintenance efficiencies. After method optimization, resulting calibration curves for more than ten REEs achieved high coefficients of determination (R2>0.999) and low relatively standard deviations (below 3.24%), demonstrating sub-ppm level detection limits (0.0897 to 0.1149 mg/L). The reliability of the CIC method was validated through comparison with inductively coupled plasma mass spectrometry (ICP-MS), showing strong agreement in REE recovery from certified standards. The impact of metal ions and salts on REE recovery using CIC was also systematically investigated. CIC consistently exhibited reliable performance in the presence of salt solutions such as NaCl and Na₂SO₄ (up to 10,000 mg/L). Our study also found the presence of high concentrations of Al ions (at 10,000 mg/L) significantly influenced REE determination, and elevated concentrations of Ca ions affected the recovery of specific REEs, including La, Ce, and Pr. The CIC method was further tested on REE-containing eluents from solvent extraction tests out of fly ash leachates. REE detection from these real processing fluids were reported to achieve 90% to 100% recovery rate from our IC method, compared to ICP-MS results. This study underscores the potential of CIC as a reliable and efficient alternative for REE determination in complex matrices. It also highlights the importance of minimizing select interfering metal ions in solutions to ensure accurate results. The REE CIC method presents a promising, low-maintenance, salt-tolerant, and cost-effective alternative to traditional analytical methods for REE analysis.

detection of rare earth elements (REE)↗
DOE OSTI2021

Influence of the Anionic Zinc-Adeninate Metal–Organic Framework Structure on the Luminescent Detection of Rare Earth Ions in Aqueous Streams

Rare earth elements (REEs) are critical to numerous technologies; however, a combination of increasing demand, environmental concerns, and monopolistic marketplace conditions has spurred interest in boosting the domestic REE production from sources such as coal utilization byproducts. The economic viability of this approach requires rapid, inexpensive, and sensitive analytical techniques capable of characterizing the REE content during resource exploration and downstream REE processing (e.g., analyzing REE separation, concentration, and purification production steps). Luminescence-based sensors are attractive because many REEs may be sensitized to produce element-specific emission. Hence, a single material may simultaneously detect and distinguish multiple REEs. Metal–organic frameworks (MOFs) can sensitize multiple REEs, but their viability has been hindered by sensitivity and selectivity challenges. Understanding how the MOF structure impacts the REE sensing efficacy is critical to the rational design of new sensors. Here, we evaluate the sensing performance of seven different anionic zinc-adeninate MOFs with different organic linkers and/or structures for the visible-emitting REEs Tb, Dy, Sm, and Eu. The choice of a linker determines which REEs are sensitized and significantly influences their sensitivity and selectivity against competing species (here, Fe(II) and HCl). For a given linker, structural changes to the MOF can further fine-tune the performance. The MOFs produce some of the lowest detection limits (sub-10 ppb for Tb) reported for the aqueous sensitization-based REE detection. Importantly, the most selective MOFs demonstrated the ability to sensitize the REE signal at sub-ppm levels in a REE-spiked acid mine drainage matrix, highlighting their potential for use in real-world sensing applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Quantum Sensing for Energy Applications

Quantum sensing is creating potentially transformative opportunities to exploit intricate quantum mechanical phenomena in new ways to make ultrasensitive measurements of multiple parameters. A growing interest in quantum sensing has created opportunities for its deployment to improve processes pertaining to energy production, distribution, and consumption. NETL is leveraging experimental and computational quantum tools to enhance sensitivity of hybrid quantum-classical ultrasensitive sensors for the detection of hydrocarbons and rare earth elements (REEs).

Paudel, Hari P.↗
DOE OSTI2026

Advanced Characterization of Wastewaters with a Focus on the Environment & Economics (Final Technical Progress Report)

This project, funded by the U.S. Department of Energy under award DE-FE0032457 and conducted at the University of Illinois at Urbana-Champaign, focused on advancing the characterization of coal combustion residual (CCR) effluents. The primary objectives were to develop analytical methods for detecting major cations, anions, trace metals, and rare earth elements (REEs) in CCR wastewater, assess environmental impacts, and explore opportunities for resource recovery. The project advanced the development of a "One-Shot" analysis system designed to simultaneously analyze multiple analytes in CCR effluents.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2024

Materials for the Photoluminescence-Based Detection of Economically Critical Metals

Critical metals, such as rare earth elements (REEs), cobalt, lithium, aluminum, nickel, and others, are essential to advanced technologies and renewable energy in particular. Widespread global adoption of renewable energy technologies has spurred dramatic demand increases for these metals; however, the global supply of these metals is highly monopolistic and conventional mining poses economic and environmental challenges. As a result, there is increasing interest in domestic production from alternative resources such as coal and its utilization byproducts. Slow and expensive characterization costs remain a significant barrier for domestic production. Here, luminescent sensing materials and platforms are presented that provide an alternative to the current state-of-the-art characterization methods; highly sensitive and selective sensing materials for cobalt, aluminum, and rare earth elements are presented, as well as compact, inexpensive platforms capable of analyzing signal from these materials for rapid characterization of critical metal content.

Crawford, Scott↗
DOE OSTI2024

Materials for the Photoluminescence-Based Detection of Economically Critical Metals

Critical metals, such as rare earth elements (REEs), cobalt, lithium, aluminum, nickel, and others, are essential to advanced technologies and renewable energy in particular. Widespread global adoption of renewable energy technologies has spurred dramatic demand increases for these metals; however, the global supply of these metals is highly monopolistic and conventional mining poses economic and environmental challenges. As a result, there is increasing interest in domestic production from alternative resources such as coal and its utilization byproducts. Slow and expensive characterization costs remain a significant barrier for domestic production. Here, luminescent sensing materials and platforms are presented that provide an alternative to the current state-of-the-art characterization methods; highly sensitive and selective sensing materials for cobalt, aluminum, and rare earth elements are presented, as well as compact, inexpensive platforms capable of analyzing signal from these materials for rapid characterization of critical metal content.

Crawford, Scott↗
DOE OSTI2025

Rare Earth Element Detection and Quantification in Coal and Rock Mineral Matrices

As global demand for rare earth elements (REEs) increases, maintaining the production and supply chain is critical. Technologies capable of being used in the field and in situ in the subsurface for rapid REE detection and quantification facilitates the efficient mining of known resources and exploration of new and unconventional resources. Laser-induced breakdown spectroscopy (LIBS) is a promising technique for rapid elemental analysis both in the laboratory and in the field. Multiple articles have been published evaluating LIBS for detection and quantification of REEs; however, REEs in their natural deposits have not been adequately studied. In this work, detection and quantification of two REEs, La and Nd, have been studied in both synthetic and natural mineral matrices at concentrations relevant to REE extraction. Measurements were performed on REE-containing rock and coal samples (natural and synthetic) utilizing different LIBS instruments and techniques, specifically a commercial benchtop instrument, a custom benchtop instrument (single- and double-pulse modes), and a custom LIBS probe currently being developed for in situ, subsurface, borehole wall detection and quantification of REEs. Plasma expansion, emission intensity, detection limits, and double-pulse signal enhancement were studied. The limits of detection (LOD) were found to be 10/14 ppm for La and 15/25 ppm for Nd in simulated coal/rock matrices in single-pulse mode. Signal enhancement of 3.5 to 6-fold was obtained with double-pulse mode as compared to single-pulse operation.

La detection↗
DOE OSTI2026

Fluorescence Signatures of Rare Earth Metals during Precipitation in Various Conditions

Fluorescence spectroscopy is a widely used sensor methodology that analyzes light emitted from a compound or element as it decays from an excited state. This technique is very sensitive and selective, which is ideal to characterize analytes at lower limits of detection. Key example targets of significant industry and research interest include rare earth elements (REEs) such as dysprosium (Dy) and europium (Eu). These are widely used in advanced technologies including semiconductors, electric vehicle motors, lasers, and permanent magnets. Identifying new sources and responsible reutilization of REEs is essential, and new approaches to extract and recycle REEs could be notably enhanced through the integration of on-line sensors. The sensors can support faster process design, informed scale-up, and cost-effective deployment. This study covers the initial exploration of applying fluorescence-based on-line monitoring to REEs within a precipitation process. This study demonstrates the successful scale-up of a fluorescence -based sensing approach, from stationary cuvettes and small-volume microfluidic devices to continuous flow systems operating at the bench scale (10-25mL). This work also provides initial insight into the challenges of signal’s effects and utility within a turbid environment. Using a modular design for monitoring flowing solutions in a flow tube, fluorescence can be characterized for a variety of analytical targets. In this study, detection performance parameters between the cuvette and flow tube system were compared. Additionally, the response of Dy during precipitation by sodium bicarbonate in the two measurement designs was explored. This letter represents a starting point to bridge the gap between traditional fluorescence sensor measurements in a cuvette to future developments that explore the ability to integrate fluorescence sensors into extraction and separation processes at industrially relevant scales.

fluorescence↗
NASA NTRS1992

AVIRIS as a tool for carbonatite exploration: Comparison of SPAM and Mbandmap data analysis methods

Data acquired with the Airborne Visible/Infrared Imaging Spectrometer (AVIRIS) of the Mountain Pass, San Bernadino County, California, area were analyzed to evaluate the use of narrow-band imaging data for carbonatite exploration. Carbonatites are igneous carbonate-rich rocks that are economically important in part because they are the major source for rare-earth minerals. Because the 224 AVIRIS spectral channels have a nominal spectral resolution of 10 nm, narrow absorption features such as those displayed by the rare-earth elements neodymium (Nd) and samarium (Sm) may be detected. The Mountain Pass region encompasses a well-exposed sequence of sedimentary, metamorphic, and igneous rocks, including an alkalic carbonatite intrusion. The carbonatite was emplaced in Precambrian granitic rocks that are fault bounded by a thick suite of Paleozoic, sedimentary rock, predominantly dolomite. The carbonatite stock, the major source of light rare-earth elements (REE) in the United States, affords the opportunity to test AVIRIS capabilities for detecting REE absorption features. Nd-bearing minerals display narrow, sharp and distinctive spectral features at 580, 740, 800, and 870 nm. Minerals bearing Sm display similarly sharp features near 1090, 1250, 1410, and 1550 nm. The more common REE, lanthanum and cerium, do not display absorption features in the visible/near-infrared region in their natural oxidation states.

Kingston, Marguerite J.↗
DOE OSTI2022

Quantification of Rare Earth Elements in the Parts Per Million Range: A Novel Approach in the Application of Laser-Induced Breakdown Spectroscopy

This work extends a previous percentage level concentration study of the optical emission spectra for six rare earth elements, europium (Eu), gadolinium (Gd), lanthanum (La), praseodymium (Pr), neodymium (Nd), and samarium (Sm), along with the transition metal, yttrium (Y) using laser-induced breakdown spectroscopy (LIBS). The concentration of these six rare earth elements and yttrium has been attempted for the first time systematically down to parts per million (ppm) concentration levels ranging from 30 to 300 ppm. In this study, the authors have developed multivariate models for each element capable of predicting concentration with acceptable to excellent levels of accuracy. Additionally, partial least squares regression coefficients were used to identify key spectral features able to be used in this lower concentration regime. This study has demonstrated that it is conceivable to quantify the six rare earth elements along with yttrium at low concentrations in the parts per million levels.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2023

Development of a Low-Cost, Sensitivity-Optimized Fluorescence Sensor for Visible Spectrum Analysis

This paper presents an economically viable, sensitivity-optimized fluorescence sensor for detecting low concentrations of fluorophores in the visible spectrum range. The sensor employs a deep ultraviolet (DUV) 275-nm LED and a dichroic mirror to establish a co-axial optical path for excitation and emission. Instead of utilizing a general-purposed spectrometer optimized for high spectral resolution, the sensor strikes a balance between resolution and sensitivity by using an appropriate aperture size and optimized optical design tailored for the spectral characteristics of fluorophores. Here, the manuscript demonstrates measurements of ppb-level rare earth element (REE) samples containing terbium (Tb), europium (Eu), dysprosium (Dy), and samarium (Sm) in aqueous solutions. Through balanced design that optimizes collection of fluorescence emission without losing spectral information, this work shows the feasibility of developing a low-cost, compact, and highly sensitive fluorescence sensors with improved detection sensitivity when compared to bench-top commercial spectrofluorometers at far higher costs.

47 OTHER INSTRUMENTATION↗
DOE OSTI2020

Evaluation of analytical performance of double pulse laser-induced breakdown spectroscopy for the detection of rare earth elements

Double pulse laser-induced breakdown spectroscopy (DP-LIBS) in collinear configuration was demonstrated to enhance the signal intensity of three rare earth elements (REEs), Eu, Gd, Pr, and Y (Yttrium is included because of its similar chemical properties and occurrence in similar deposits as REE). Significant enhancement in spectral signals of all elements was observed with an aid of second laser. Two laser pulses of 1064 nm wavelength were employed in collinear geometry on the Pr 2 O 3 , Eu 2 O 3 , Gd 2 O 3 , and Y 2 O 3 pellets to obtain emission spectra. For selected strong emission lines of Eu and Gd signal enhancement was found to be 3 to 7-fold and that for Y and Pr lines was observed to be 3 to 13-fold compared to single-pulse laser-induced breakdown spectroscopy (SP-LIBS). Role of inter-pulse delay between two pulses in DP-LIBS was found to be very crucial. Furthermore, while comparing selected ionic and neutral lines, ionic lines were found to have larger signal enhancement in DP-LIBS at the experimental conditions used in this study.

47 OTHER INSTRUMENTATION↗
DOE OSTI2023

Magnetostrictive materials for enhanced sensors and electronic components

Magnetostriction is a property of magnetic materials that causes them to change their shape or dimensions proportional to their magnetization. Low-cost, mechanically robust magnetostrictive sensors would be valuable for a wide range of applications across the DOE and national security mission space, such as monitoring the internal conditions of pipelines, rapidly detecting high-impedance faults in power lines (e.g. trees touching power lines), or enhancing implantable systems for the human body. Dilute doping (<1 at.%) of rare earth elements (REE) has been shown to amplify the magnetostriction. Furthermore, alloy processing by rapid cooling from high temperature tends to result in texturing and therefore greater magnetostriction values, which bodes well for developing advanced manufacturing approaches significantly less expensive than single crystal growth. The goal of this effort was to develop robust, low-cost magnetostrictive materials compatible with advanced manufacturing techniques to exploit the rapid cooling of these approaches while retaining the ability to produce fully dense structures. To be useful as a sensor or actuator the coercivity of the material needs to be minimized so that there is minimal magnetic hysteresis. Employing a small scale laser powder bed fusion (L-PBF) system, specimens of Fe-Ga-Ce were built from alloy powder which had a magnetostriction of 289 ppm along the build direction and 197 ppm perpendicular to the build direction. These values are not far from the 310-350 ppm observed in single crystals of Fe-Ga. The results of the series of samples run suggest this is a very promising route for REE doping to higher levels, especially if the powders can be produced using far from equilibrium approaches such as ultrasonic atomization. The promising results from applying additive manufacturing techniques to these materials, particularly the inexpensive Fe-Al system, has potential for inexpensive high-performing magnetostrictive parts producible at large scales for low-cost sensors.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Developing Fluorescence-Based Sensors to Support Rare Earth Element Separation

Rare earth elements (REEs) are essential to most renewable energy technologies. Unfortunately, as we transition to sustainable energy production, the demand for REEs is rapidly growing well beyond current rates of production. As a result, novel means of efficient, scalable, and easily adaptable methods for processing primary and recycle feedstocks are needed. Development and integration of sensors for highly selective in-line monitoring can support more efficient design and testing of such novel separation processes, as well as more cost-effective deployment of those separation flowsheets. Work here will explore the application of fluorescence spectroscopy, a highly sensitive and selective technique, to quantify multiple lanthanides in complex mixtures including known interferents or quenching agents. Results include identification of the optimal excitation wavelength and the limit of detection of various rare earth elements as well as the performance of data-science-based quantification approaches in streams where “unknowns” are present. Overall, the data science tools in conjunction with optical sensor data were able to quantify analytes in the presence of other lanthanides which can be anticipated in the actual industrial stream. Here we include characterization of lanthanides in a microfluidic device similar to those used in new process development. This study demonstrates the capability of utilizing fluorescence spectroscopy to quantify analytes in a complicated solution matrix, suggesting this is a successful approach for in-line monitoring to optimize the separation efficiency in an industrial stream.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Bioleaching ion-unexchangeable rare earth in ion-adsorption type rare earth waste tailing

Ion-adsorption type rare earth ores (IREO) in China serve as the primary source of medium and heavy rare earth globally. With the rapidly growing demand for rare earth elements (REEs) and the dwindling supply of premium IREO, enhancing the recovery of REEs, especially the ion-unexchangeable REEs with ultra-low content and ambiguous speciation from IREO or its tailing, has become a critical trend and challenge. Here, this study identified the occurrences of ion-unexchangeable REEs, primarily detected in Fe-enriched minerals, xenotime, and monazite of IREO using TESCAN integrated mineral analyzer (TIMA) and laser ablation inductively coupled plasma mass spectrometer (LA-ICP-MS) analysis. To extract these elusive REEs, a bioleaching technique utilizing Aspergillus niger (A. niger) metabolites was proposed, achieving a leaching yield of 31.4 wt%. Complementary sequential chemical extraction methods (SCEM), X-ray photoelectron spectroscopy (XPS), and density functional theory (DFT) calculations further elucidate the underlying mechanism, involving the carboxylic acid produced by the metabolic process of microbes that dissolves goethite by disrupting Fe—O bonds and liberating REEs, which complexed with carboxylate (R—COO—), to promote further dissolution. This work offers insight into enhancing the recovery of ion-unexchangeable REEs from IREO or its tailing, paving the way for sustainable and efficient rare earth mining practices.

42 ENGINEERING↗
DOE OSTI2024

Incorporation of rare earth elements $\text{Sc}$, $\text{Y}$ and $\text{La}$ into gibbsite

Rare earth elements (REE) are increasingly critical resources in technological applications, but the current understanding of their separation by uptake into minerals remains limited. We examined the adsorption and solubilization of scandium (Sc), yttrium (Y), and lanthanum (La) into aluminum hydroxide (gibbsite, Al(OH) 3 ). Based on spectroscopic investigations such as inductively coupled plasma-optical emission spectroscopy (ICP-OES) and time of flight-secondary ion mass spectrometry (ToF-SIMS), only Sc exhibited favorable incorporation and adsorption (0.66 and 0.06 atom%, respectively). Analysis of solid state 45 Sc magic angle spinning-nuclear magnetic resonance spectroscopy (MAS-NMR) indicated that Sc exhibits an octahedral coordination consistent with isolated substitutions for Al in the gibbsite structure, leading to a increase in lattice constants detectable by X-ray diffraction. Density functional theory (DFT) calculations reinforced this interpretation by reproducing the detected structural distortion as well as demonstrating the relatively favorable energetic basis for Sc incorporation into gibbsite by substitution.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗