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All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

R&D Outcomes of Surrogate Environmental Swipe Manufacturing Technique Method Development for Arms Control and Treaty Verification Applications

The analysis of environmental samples is a critical component of nuclear compliance verification and safeguards activities. While the associated particle analyses have benefitted from recent advances in the production of actinide-bearing particulates with uniform and well-characterized particle size, material phase, and isotopic ratios to serve as reference materials for calibration and interlaboratory comparisons, there is an outstanding need for surrogate environmental samples, which resemble field-collected samples, with the aforementioned reference particulates to support future nuclear compliance verification exercises and method development. This effort seeks to leverage the recent advances in tailored reference particle production to generate surrogate environmental swipe samples via parallel production techniques (direct and indirect) which are uniquely suited to the hydrothermal and aerosol-based synthesis routes developed at PNNL and SRNL, respectively. PNNL’s hydrothermal particle production method was used to generate surrogate reference particles for the indirect production of test swipes.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2022

On the characterization of biases arising from methods and approximations used for sensitivity analyses

The preliminary assessment of the performance and safety of advanced reactors, as well as the identification of research and development needs, rely on computer simulations due to the lack of operational experience. Those simulations should be based on verified and validated computational tools, calculation schemes, and nuclear data libraries, and should be accompanied of a proper characterization of the involved uncertainties, providing confidence in the computational-based predictions. Thus, sensitivity and uncertainty studies, together with integral experiments, play an essential role in that process. Sensitivities are then a critical element and guidelines about how to produce accurate enough sensitivities depending on the subsequent analyses to be performed are of interest. The present study addresses the sensitivities biases arising from the use of different nuclear data libraries, computational methods and the assumption of modelling simplifications. Not only sensitivities for multiplication factor but also for safety-relevant reactivity responses have been analyzed. In the study, propagated uncertainties are also included for the considered parameters to illustrate the impact of the sensitivity profiles obtained for each case on the final uncertainty. Then, relevant recommendations are given for sensitivity analyses of highly complex systems. (authors)

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
DOE OSTI2025

Advancing the Representation of Human Actions in Large‐Scale Hydrological Models: Challenges and Future Research Directions

Characterizing the impact of human actions on terrestrial water fluxes and storages at multi-basin, continental, and global scales has long been on the agenda of scientists engaged in climate science, hydrology, and water resources systems analysis. This need has resulted in a variety of modeling efforts focused on the representation of water infrastructure operations. Yet, the representation of human-water interactions in large-scale hydrological models is still relatively crude, fragmented across models, and often achieved at coarse resolutions (~10–100 km) that cannot capture local water management decisions. In this commentary, we argue that the concomitance of four drivers and innovations is poised to change the status quo: “hyper-resolution” hydrological models (~0.1–1 km), multi-sector modeling, satellite missions able to monitor the outcome of human actions, and machine learning are creating a fertile environment for human-water research to flourish. We then outline four challenges that chart future research in hydrological modeling: (a) creating hyper-resolution global data sets of water management practices, (b) improving the characterization of anthropogenic interventions on water quantity, stream temperature, and sediment transport, (c) improving model calibration and diagnostic evaluation, and (d) reducing the computational requirements associated with the successful exploration of these challenges. Overcoming them will require addressing modeling, computational, and data development needs that cut across the hydrology community, thereby requiring a major communal effort.

catchment hydrology↗
DOE OSTI2016

Materials Characterization using the Facilities of the Center for Synchrotron Radiation Research and Instrumentation (CSRRI), a NSUF Partner Facility

Advanced nuclear energy systems are envisioned to operate at high temperatures, high burn-up, harsh neutron irradiation, and corrosive environments. New materials and nuclear fuels with improved performance, safety and reliability are needed for the increasingly demanding operating conditions. The fundamental challenge in developing new materials with improved irradiation, temperature, and corrosion resistance is to understand and control chemical and physical phenomena in complex systems over multiple time and length scales. Solving these scientific and technical challenges will require an integrated approach of all available computational and experimental capabilities. This talk will focus on the application of synchrotron radiation techniques to characterize materials of interest to nuclear material science at the facilities operated by the Center For Synchrotron Radiation Research and Instrumentation (CSRRI) at the Illinois Institute of Technology. The CSRRI is a partner facility with the U. S. Department of Energy's Nuclear Science User Facility (NSUF). Using the CSRRI facilities, such as the Materials Research Collaborative Access Team (MRCAT) beamline, we can study the materials science of irradiated and model materials to improve the understanding of the performance of materials in nuclear reactors. (author)

36 MATERIALS SCIENCE↗
DOE OSTI2025

Operando XPS in reactive plasmas: The importance of the wall reactions

In this article, advancements in differential pumping and electron optics over the past few decades have enabled x-ray photoelectron spectroscopy (XPS) measurements at (near-)ambient pressures, bridging the pressure gap for characterizing realistic sample chemistries. Recently, we have demonstrated the capabilities of an ambient pressure XPS setup for in situ plasma environment measurements, allowing plasma-surface interactions to be studied in operando rather than using the traditional before-and-after analysis approach. This new “plasma-XPS” technique facilitates the identification of reaction intermediates critical for understanding plasma-assisted surface processes relevant to semiconductor nanomanufacturing, such as physical vapor deposition, etching, atomic layer deposition, and many other plasma applications. In this paper, we apply the plasma-XPS approach to monitor real-time surface chemical changes on a model Ag(111) single crystal exposed to oxidizing and reducing plasmas. We correlate surface-sensitive data with concurrent gas-phase XPS measurements and residual gas mass-spectrum analysis of species generated during plasma exposure, highlighting the significant role of plasma-induced chamber wall reactions. Ultimately, we demonstrate that plasma-XPS provides comprehensive insights into both surface and gas-phase chemistry, establishing it as a versatile and dynamic characterization tool with broad applications in microelectronics research. Finally, we outline potential enhancements and future metrology directions to advance plasma-XPS investigations further.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Developing Enzyme Immobilization with Fibrous Membranes: Longevity and Characterization Considerations

Fibrous membranes offer broad opportunities to deploy immobilized enzymes in new reactor and application designs, including multiphase continuous flow-through reactions. Enzyme immobilization is a technology strategy that simplifies the separation of otherwise soluble catalytic proteins from liquid reaction media and imparts stabilization and performance enhancement. Flexible immobilization matrices made from fibers have versatile physical attributes, such as high surface area, light weight, and controllable porosity, which give them membrane-like characteristics, while simultaneously providing good mechanical properties for creating functional filters, sensors, scaffolds, and other interface-active biocatalytic materials. This review examines immobilization strategies for enzymes on fibrous membrane-like polymeric supports involving all three fundamental mechanisms of post-immobilization, incorporation, and coating. Post-immobilization offers an infinite selection of matrix materials, but may encounter loading and durability issues, while incorporation offers longevity but has more limited material options and may present mass transfer obstacles. Coating techniques on fibrous materials at different geometric scales are a growing trend in making membranes that integrate biocatalytic functionality with versatile physical supports. Biocatalytic performance parameters and characterization techniques for immobilized enzymes are described, including several emerging techniques of special relevance for fibrous immobilized enzymes. Diverse application examples from the literature, focusing on fibrous matrices, are summarized, and biocatalyst longevity is emphasized as a critical performance parameter that needs increased attention to advance concepts from lab scale to broader utilization. This consolidation of fabrication, performance measurement, and characterization techniques, with guiding examples highlighted, is intended to inspire future innovations in enzyme immobilization with fibrous membranes and expand their uses in novel reactors and processes.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2013

Low Dimensional System Hybrids for Advanced Electronics/Optoelectronics [Slides]

Interacting quantum wells: Type II InAs/GaSb superlattice for high performance infrared detection and imaging – CQD, Northwestern University 2005-2011: – Physics of interacting quantum wells: InAs/GaSb superlattice; – M-structure superlattice; – Materials growth and characterization; – Infrared detector operation and optimization strategies; – Infrared Focal Plane Array (aka. infrared camera). Cylindrical quantum Well In a Nanowire (CWIN): Heterostructuring core/multi-shell nanowires for advanced electronic/optoelectronic devices – CINT,LANL 2012-present: – Si-based Nanowire research overview; – Device physics of NWFETs: Diameter dependence performance; – CWIN design for high performance FET; – Growth and characterization of Si/Ge/Si core/multi-shell NWs; – Towards ultra-short channel length NWFETs.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructure and Fission Product Distribution Examination in the UCO kernel of TRISO Fuel Particles

The effect of irradiation and fabrication process on the UCO fuel kernel, kernel-buffer interlayer and fission products, has not been fully studied for UCO fuel kernels of TRISO coated particles. Specifically, the potential correlation(s) with fission product retention, composition and distribution within these structures for the tristructural isotropic (TRISO) fuel performance at normal and accident conditions, are not well reported in literature. Structural and chemical information in the irradiated UCO fuel kernel, e.g., the stoichiometry variations, may further contribute to fuel performance modeling under the Nuclear Energy Advanced Modeling and Simulation (NEAMS) program. The microstructural and micro-chemical evolution of selected irradiated UCO fuel kernels, kernel buffer interfaces and recoil zones were characterized using Scanning Transmission Electron Microscopy (STEM) and Energy Dispersive Spectroscopy (EDS) elemental mapping. The fuel kernel of particles from Advanced Gas Reactor (AGR)-2 irradiated to 10.8% fissions per initial metal atom (FIMA), were examined with the following main findings: (1) large fission gas bubbles were mainly identified in the zirconium and molybdenum enriched but oxygen depleted phases in the center of fuel kernel, (2) significant inter-diffusion between the UCO fuel kernel and pyro-carbon buffer layer was observed as a high density of sub-micron sized carbon inclusions was identified at near the interface in the kernel side and some isolated UCO particles were located in the buffer layer, (3) pores filled with free carbon were also observed in the recoil zone specimen. Fuel kernels from two AGR-1 compacts irradiated to 11.4 and 17.4% FIMA respectively, were examined with the following main findings: (1) two primary phases consisting of a “high-Z (atomic mass)” UC(O) phase (rocksalt; a=0.496 nm) that also contained Zr, Mo, and/or Ru and a “low-Z” UO2(C) phase (fluorite structure; a = 0.547nm) in which trace amounts of I, Nd, Pr, and/or Er could be detected. This latter phase contained many precipitates of the “high-Z” phase. Conversely, this latter phase did not contain precipitates of the UO2-type material, (2) Xe bubbles were found almost exclusively in the “high-Z” phase and in the particular example shown, the Zr-containing variant. Further work in this area should address whether this potential Xe preference for just one of the high-Z phases is indeed a real effect.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

High-energy micrometre-scale pixel direct conversion X-ray detector

The objective of this work was to fabricate and characterize a new X-ray imaging detector with micrometre-scale pixel dimensions (7.8 µm) and high detection efficiency for hard X-ray energies above 20 keV. A key technology component consists of a monolithic hybrid detector built by direct deposition of an amorphous selenium film on a custom designed CMOS readout integrated circuit. Characterization was carried out at the synchrotron beamline 1-BM-B at the Advanced Photon Source of Argonne National Laboratory. The direct conversion detector demonstrated micrometre-scale spatial resolution with a 63 keV modulation transfer function of 10% at Nyquist frequency. In addition, spatial resolving power down to 8 µm was determined by imaging a transmission bar target at 21 keV. X-ray signal linearity, responsivity and lag were also characterized in the same energy range. Finally, phase contrast edge enhancement was observed in a phase object placed in the beam path. This amorphous selenium/CMOS detector technology can address gaps in commercially available X-ray detectors which limit their usefulness for existing synchrotron applications at energies greater than 50 keV; for example, phase contrast tomography and high-resolution imaging of nanoscale lattice distortions in bulk crystalline materials using Bragg coherent diffraction imaging. Here, the technology will also facilitate the creation of novel synchrotron imaging applications for X-ray energies at or above 20 keV.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Design of a first-of-A-kind instrumented advanced test reactor irradiation Capsule experiment for In situ thermal conductivity measurements of metallic fuel

Metallic fuel undergoes dramatic microstructural changes early in life due to fission gas swelling until ~2–3 at% burnup which affects the conductivity of the material, however the evolution of metallic fuel thermal conductivity during this early phase burnup has never been successfully measured in situ. The Irradiated Material Properties Accelerated Characterization Test (IMPACT) experiment will be the first in a series of experiments to irradiate advanced nuclear metallic fuel specimens with novel embedded thermal conductivity probes in ATR. In the current work the IMPACT experiment final design and supporting analysis is reported in detail. Results are evaluated for various reactor operational conditions to meet the functional requirements of the experiment. Finally, the first iteration of this IMPACT experiment will provide data regarding thermal properties evolution in uranium-zirconium (U10Zr) fuel, but this experiment vehicle is envisioned for future advanced fuels and structural materials irradiations in ATR.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2014

Characterizing diamylamylphosphonate (DAAP) as an Americium Ligand for nuclear fuel cycle applications

Successful deployment of the currently-envisioned advanced nuclear fuel cycle requires the development of a partitioning scheme to separate Am from the lanthanides. The Am/lanthanide separation is challenging since all the metals are normally trivalent and have similar ionic radii. Oxidation of Am to higher oxidation states is one option to achieve such a separation. Hexavalent Am has now been routinely prepared in our laboratory in strongly acidic solution using sodium bismuthate as the oxidant, and then extracted into diamylamylphosphonate/dodecane solution. Here, we have characterized this phosphonate-containing solvent with regard to the extraction of Am, the lanthanides, Cm, other fission product, and/or inert constituents expected in dissolved nuclear fuel. Additionally, the effects of irradiation on dispersion numbers and the phosphonate concentration were investigated.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2020

Assessment of Potential Future Demands for Hydrogen in the United States

H2@Scale is a U.S. Department of Energy (DOE) initiative that brings together stakeholders to advance the affordable production, transport, storage, and utilization of hydrogen (H2) as an energy carrier to increase revenue opportunities in multiple energy sectors. The focus of the current work is to characterize the growth potential of diverse hydrogen industries in the United States, given research and development (R&D) advancements in hydrogen technologies. Current and emerging hydrogen production technologies utilize diverse energy sources, including natural gas (NG) reforming, as well as renewable and nuclear power for low-temperature and high-temperature water splitting. The produced hydrogen also enables emerging domestic industries that value conventional and renewable hydrogen as an energy carrier for intermediate and end use. The success of H2@Scale (Figure ES.1) depends not only on hydrogen demand from growing existing markets such as petroleum refining and ammonia (NH 3 ) production, but also on the development of new markets such as metals refining, synthetic fuel (synfuel) and chemical production, biofuels, light-duty (LD) and heavy-duty (HD) hydrogen fuel cell (FC) electric vehicles (FCEVs), and injection into NG pipelines, all of which can significantly increase hydrogen demand relative to current levels of approximately10 million metric tons [MMT] annually. This study focused primarily on five demand sectors — synfuels, upgrading of oil/biomass, NH 3 /fertilizer, metals refining, and hydrogen vehicles (transportation) — along with gas infrastructure. For each sector, a hydrogen demand potential was quantified, along with a “threshold price.” The hydrogen demand potential reflects a practical amount of hydrogen that could be used in that sector, barring economic considerations. The threshold price reflects the price at which the consumer would utilize hydrogen in lieu of an alternative that could supply the same performance.

08 HYDROGEN↗
DOE OSTI2025

Machine learning approaches for intentional materials engineering

In this article, the development of nanoporous metals and metallic composites through dealloying processes presents significant opportunities in materials engineering. However, designing multicomponent precursor alloys and establishing corresponding processing methods that yield predictable compositions and nanostructures remain a complex challenge. This article explores how machine learning (ML)-augmented computational and experimental methodologies can tackle these challenges by predicting precursor alloy compositions, final nanoporous structures, and mechanical properties, while integrating ML-enabled autonomous experimentation for material design and quantification. We highlight recent advancements in applying ML to nanostructured materials design via dealloying and discuss how techniques from other nanomaterial designs can be adapted for improved control over morphological and compositional outcomes in nanoporous and nanocomposite materials. Furthermore, we explore the role of ML in autonomous synchrotron x-ray experimentation, enabling real-time feedback between modeling and experimental setups. ML-driven approaches to microstructure characterization and mechanical property prediction are also examined, with a focus on modeling and advanced imaging techniques such as three-dimensional nanotomography. Finally, this article outlines future directions for ML-enhanced materials science, emphasizing the exploration of high-dimensional parameter spaces and the incorporation of materials kinetics into processing and property evaluation, ultimately advancing the design of nanoporous structures and materials science.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Materials Characterization using the Center For Synchrotron Radiation Research and Instrumentation (CSRRI), a NSUF Partner Facility

Demanding operating conditions for advanced nuclear energy systems have called for a push in the development of new materials and nuclear fuels with improved performance, safety, and reliability. The development of new materials with improved irradiation, temperature, and corrosion resistance requires significant study of chemical and physical phenomena over multiple time and length scales. To do so, an integrated approach utilizing both computational and experimental capabilities will be required to overcome these scientific and technical challenges. This talk will focus on the application of synchrotron radiation techniques available for characterization of nuclear materials at the Center For Synchrotron Radiation Research and Instrumentation (CSRRI) at the Illinois Institute of Technology. The CSRRI is a partner facility with the U.S. Department of Energy's Nuclear Science User Facility (NSUF), and includes the Materials Research Collaborative Access Team (MRCAT) beam line at Argonne National Laboratory. Using the capabilities of CSRRI, we can study the materials science of irradiated and model materials to improve our understanding of the performance of materials used in nuclear reactors. Current examples of each technique will be discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2014

High efficiency turbine blade coatings

The development of advanced thermal barrier coatings (TBCs) of yttria stabilized zirconia (YSZ) that exhibit lower thermal conductivity through better control of electron beam - physical vapor deposition (EB-PVD) processing is of prime interest to both the aerospace and power industries. This report summarizes the work performed under a two-year Lab-Directed Research and Development (LDRD) project (38664) to produce lower thermal conductivity, graded-layer thermal barrier coatings for turbine blades in an effort to increase the efficiency of high temperature gas turbines. This project was sponsored by the Nuclear Fuel Cycle Investment Area. Therefore, particular importance was given to the processing of the large blades required for industrial gas turbines proposed for use in the Brayton cycle of nuclear plants powered by high temperature gas-cooled reactors (HTGRs). During this modest (~1 full-time equivalent (FTE)) project, the processing technology was developed to create graded TBCs by coupling ion beam-assisted deposition (IBAD) with substrate pivoting in the alumina-YSZ system. The Electron Beam - 1200 kW (EB-1200) PVD system was used to deposit a variety of TBC coatings with micron layered microstructures and reduced thermal conductivity below 1.5 W/m.K. The use of IBAD produced fully stoichiometric coatings at a reduced substrate temperature of 600°C and a reduced oxygen background pressure of 0.1 Pa. IBAD was also used to successfully demonstrate the transitioning of amorphous PVD-deposited alumina to the -phase alumina required as an oxygen diffusion barrier and for good adhesion to the substrate Ni 2 Al 3 bondcoat. This process replaces the time consuming thermally grown oxide formation required before the YSZ deposition. In addition to the process technology, Direct Simulation Monte Carlo plume modeling and spectroscopic characterization of the PVD plumes were performed. The project consisted of five tasks. These included the production of layered periodic microstructures in the coating, the Direct Simulation Monte Carlo (DSMC) modeling of particle transport in the PVD plume, functional graded layer development, the deposition of all layers to form a complete coating, and materials characterization including thermal testing. Ion beam-assisted deposition, beam sharing through advanced digital rastering, substrate pivoting, hearth calorimetry, infrared imaging, fiber optic-enabled optical emission spectroscopy and careful thermal management were used to achieve all the milestones outlined in the FY 02 LDRD proposal.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Reducing Uncertainty in Hydrodynamic Modeling of ATR Experiments Via Flow Testing, Validation, and Optimization

The development, characterization, and qualification testing of nuclear fuel at Idaho National Laboratory’s Advanced Test Reactor (ATR) requires extensive design and analysis activities prior to the insertion of an irradiation experiment in-pile. Significant effort is made in the design and development phase of all in-pile experiments to ensure that the maximum feasible impacts of all necessary experimental requirements are satisfied. The advancement of fuel, cladding, and in-reactor materials technology in recent years has introduced complexities associated with the design and construct of in-pile experiments necessitating deeper understanding of boundary conditions and increasingly comprehensive observations resulting from the experiment. Each unique experiment must be assessed for neutronics response, thermal/hydraulic/hydrodynamic performance, and structural integrity. This is accomplished either analytically, computationally, or experimentally, or some combination thereof, prior to insertion into the ATR. The various effects are interrelated to various degrees, such as the case with the experiment temperature affecting the thermal cross section of the fuel or the increased temperature of the experiment’s materials reducing the mechanical strength of the assemblies. Additionally, the feedback between the experiment’s response to a reactor transient could alter the neutron flux profile of the reactor during the transient. Each experiment must therefore undergo a barrage of analyses to assure the ATR operational safety review committee that the insertion and irradiation of the experiment will not detrimentally affect the safe operational envelope of the reactor. In many cases, the nuclear fuel being tested can be double-encapsulated to ensure safety margins are adequately addressed, whereas failed fuel would be encased in a protective capsule. In other cases, the experiments can be inserted in a self-contained loop that passes through the reactor core, remaining isolated from the primary coolant. In the case of research reactor fuel, however, the fuel plates must be tested in direct contact with the reactor coolant, and being fuel designed for high neutron fluxes, they are inherently power-dense plates. The combination of plate geometry, high-power density, and direct contact with primary coolant creates a scenario where the neutronic/thermomechanic/hydrodynamic characteristics of the fuel plates are tightly coupled, necessitating as complete characterization as possible to support the safety and programmatic assessments, thus enabling a successful experiment. This paper explores the efforts of the U.S. High-Performance Research Reactor program to thermomechanically/hydromechanically characterize the program’s wide variety of experiments, which range from stacks of miniplate capsules to full-sized, geometrically representative curved plates. Special attention is given to instances where the combination of experimental characterization and analytical assessment has reduced uncertainties of the safety margins, allowing experiments to be irradiated that would otherwise not have passed the rigorous qualification process for irradiation in the ATR. In some cases, the combined processes have exposed flow and heat transfer characteristics that would have been missed using historical methods, which allows for more accurate and representative postirradiation assessments.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2017

Characterization of Rare Earth Element Minerals in Coal Utilization Byproducts

The United States currently produces over 100 million tons of coal utilization byproducts (CUB) per year in the form of fly ash, bottom ash, slag, and flue gas (American Coal Ash Association (ACCA), 2015). But this “waste material” also contains potentially useful levels of rare earth elements (REE). Rare earth elements are crucial for many existing and emerging technologies, but the U.S. lacks a domestic, sustainable REE source. Our project explored the possibility of developing a supply of REEs for U.S. technologies by extracting REEs from CUBs. This work offers the potential to reduce our dependence on other countries for supply of these critical elements (NETL, REE 2016 Project Portfolio). Geologic and diagenetic history, industrial preparation methods, and the specific combustion process all play major roles in the composition of CUB. During combustion, inorganic mineral phases of coal particles are fluidized at temperatures higher than 1400oC, so inorganic mineral materials are oxidized, fused, disintegrated, or agglomerated into larger spherical and amorphous (non-crystalline) particles. The original mineralogy of the coal-containing rock and heating/cooling of the material significantly affects the composition and morphology of the particles in the combustion byproduct (Kutchko and Kim, 2006). Thus, different types of coal/refuse/ash must be characterized to better understand mineral evolution during the combustion process. Our research focused on developing a working model to address how REE minerals behave during the combustion process: this research should help determine the most effective engineering methods for extracting REEs from CUBs. We used multimodal imaging and image processing techniques to characterize six rock and ash samples from different coal power plants with respect to morphology, grain size, presence of mineral phases, and elemental composition. The results of these characterization activities provided thresholds for realizing the occurrence of REE mineral phases in CUB and allowed us to calculate structural and volumetric estimates of REE. Collectively, the rock and coal ash samples contained minerals such as quartz, kaolinite, muscovite/illite, iron oxide (as hematite or magnetite), mullite, and clinochlore. Trace minerals included pyrite, zircon, siderite, rutile, diopside, foresterite, gypsum, and barite. We identified REE phosphate minerals monazite (Ce,La,Nd,Th)(PO 4 ,SiO 4 ), xenotime (YPO 4 ,SiO 4 ), and apatite (Ca 5 (PO 4 ) 3 (F,Cl,OH) via SEM and electron microprobe analysis: these materials generally occurred as 1-10 μm-long crystals in the rock and ash samples. As has been shown in other studies, amorphous material-aluminosilicate glass or iron oxyhydroxide-are the major components of coal fly and bottom ash. Trace amounts of amorphous calcium oxide and mixed element (e.g., Al-Si-Ca-Fe) slag are also present. Quartz, mullite, hematite, and magnetite are the crystalline phases present. We found that REEs are present as monomineralic grains dispersed within the ash, as well as fused to or encapsulated by amorphous aluminosilicate glass particles. Monazite and xenotime have relatively high melting points (>1800 °C) compared to typical combustion temperatures; our observations indicate that the REE-phosphates, which presumably contribute a large percentage of REE to the bulk ash REE pool, as measured by mass spectroscopy, are largely unaltered by the combustion. Our study shows that conventional coal combustion processes sequester REE minerals into aluminosilicate glass phases, which presents a new engineering challenge for extracting REE from coal ash. The characterization work summarized in this report provides a semi-quantitative assessments of REE in coal-containing rock and CUB. The data we obtained from 2- and 3-D imaging, elemental mapping, volumetric estimates, and advanced high-resolution pixel classification successfully identified the different mineral phases present in CUB. Further, our characterization results can guide techniques for extracting REEs from CUB, or other geologic and engineered materials. Whilst, interpretations will inform future REE separation and extraction techniques and technologies practical for commercial utilization of combustion byproducts generated by power plants.

01 COAL, LIGNITE, AND PEAT↗