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DOE OSTI2017

Field characterization of the PM 2:5 Aerosol Chemical Speciation Monitor: insights into the composition, sources, and processes of fine particles in eastern China

A PM 2.5 -capable aerosol chemical speciation monitor (Q-ACSM) was deployed in urban Nanjing, China, for the first time to measure in situ non-refractory fine particle (NR-PM 2.5 ) composition from 20 October to 19 November 2015, along with parallel measurements of submicron aerosol (PM 1 ) species by a standard Q-ACSM. Our results show that the NR-PM 2.5 species (organics, sulfate, nitrate, and ammonium) measured by the PM 2.5 -Q-ACSM are highly correlated ( r 2 > 0.9) with those measured by a Sunset Lab OC / EC analyzer and a Monitor for AeRosols and GAses (MARGA). The comparisons between the two Q-ACSMs illustrated similar temporal variations in all NR species between PM 1 and PM 2.5 , yet substantial mass fractions of aerosol species were observed in the size range of 1–2.5 µm. On average, NR-PM 1-2.5 contributed 53 % of the total NR-PM 2.5 , with sulfate and secondary organic aerosols (SOAs) being the two largest contributors (26 and 27 %, respectively). Positive matrix factorization of organic aerosol showed similar temporal variations in both primary and secondary OAs between PM 1 and PM 2.5 , although the mass spectra were slightly different due to more thermal decomposition on the capture vaporizer of the PM 2.5 -Q-ACSM. We observed an enhancement of SOA under high relative humidity conditions, which is associated with simultaneous increases in aerosol pH, gas-phase species (NO 2 , SO 2 , and NH 3 ) concentrations and aerosol water content driven by secondary inorganic aerosols. These results likely indicate an enhanced reactive uptake of SOA precursors upon aqueous particles. Therefore, reducing anthropogenic NO x , SO 2 , and NH 3 emissions might not only reduce secondary inorganic aerosols but also the SOA burden during haze episodes in China.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2018

Demonstration of LOTUS multiphysics BEPU analysis framework for LB-LOCA simulations

The LOCA Toolkit for U.S. light water reactors (LOTUS) currently under development at Idaho National Labs (INL) is a plug and play, multiphysics environment to be used in support of system level plant transient analysis. New proposed rule changes in LOCA safety regulations (10 CFR 50.46c) require the inclusion of cladding hydrogen content in the evaluation of equivalent cladding reacted (ECR) and peak cladding temperature (PCT). The potential for a future implementation of said rule change motivates the current development of a unique union of core design, system analysis, and fuel performance codes within a framework allowing for uncertainty quantification (UQ). A demonstration of LOTUS capabilities to address this potential need is performed with an integration of the core design code PHISICS, the fuel performance code FRAPCON, and the system analysis code RELAP5-3D. UQ is performed via Wilks’ method to compute the one sided 95/95 confidence values of the aforementioned safety metrics. Results demonstrate the benefits of the Multiphysics Best Estimate Plus Uncertainty (MP-BEPU) methodology and provide useful visualization of the limiting cases.

10CFR50.46c↗

DOE OSTI2023

A cryogenically cooled 200 kV DC photoemission electron gun for ultralow emittance photocathodes

Novel photocathode materials like ordered surfaces of single crystal metals, epitaxially grown high quantum efficiency thin films, and topologically non-trivial materials with dirac cones show great promise for generating brighter electron beams for various accelerator and ultrafast electron scattering applications. Despite several materials being identified as brighter photocathodes, none of them have been tested in electron guns to extract electron beams due to technical and logistical challenges. In this paper, we present the design and commissioning of a cryocooled 200 kV DC electron gun that is capable of testing a wide variety of novel photocathode materials over a broad range of temperatures from 298 to 35 K for bright electron beam generation. This gun is designed to enable easy transfer of the photocathode to various standard ultra-high-vacuum surface diagnostics and preparation techniques, allowing a full characterization of the dependence of beam brightness on the photocathode material and surface properties. We demonstrate the development of such a high-voltage, high-gradient gun using materials and equipment that are easily available in any standard university lab, making the development of such 200 kV electron guns more accessible.

Instruments & Instrumentation↗

DOE OSTI2026

Cold compressor performance and energy consumption improvements at Jefferson Lab’s Central Helium Liquefiers

Abstract Jefferson Lab operates two central helium liquefiers (CHLs) which both utilize full cold compression from the saturation pressure at operating temperature (approximately 2.1 K) to just over atmospheric pressure. The original plant, CHL1, was recently outfitted with a replacement subatmospheric cold box (SC1R) containing state-of-the-art cold compressor technology, while the newer plant, CHL2, uses an older cold compressor system. In both cases, the heat of compression is absorbed at low temperature at the expense of electrical power consumed by the warm compressors. Due to the superior efficiency and turndown capabilities of SC1R, a new operating mode has been identified for CHL1 in which the required number of operating warm compressors is reduced by one. A cost-based method for optimizing cold compressor stability and efficiency has been developed and applied to CHL2, improving its turndown and lowering the warm compressor discharge pressure. As a result of these efforts, power consumption of the combined CHLs during normal operations has been reduced by nearly 10%, or a total of 650 kW. The observed performance of CHL1 with SC1R, as well as the cold compressor optimization method, leading to this improved energy consumption rate will be discussed in detail.

Mastracci, B [Thomas Jefferson National Accelerato↗

DOE OSTI2021

Request for Proposal: MSI Workforce Program Funding Opportunity

Los Alamos National Laboratory is a multidisciplinary research institution engaged in strategic science on behalf of national security. The Laboratory strives to enhance national security and make the world safer through research and advances in innovative science and technology. The Lab inspires the talent of its workforce and the region to solve problems related to defense, energy, environment, infrastructure, health, and global security concerns. LANL currently employs 11,700 and anticipates hiring 1000 plus people this year. The LANL mission is critical to meeting military requirements to ensure the U.S. nuclear deterrent is modern, responsive, and resilient. LANL is designated by NNSA as the nation’s Plutonium Center of Excellence. LANL has an experienced and skilled workforce, high-hazard nuclear facilities and associated infrastructure, and unique plutonium processing, fabrication, and experimental capabilities.

96 KNOWLEDGE MANAGEMENT AND PRESERVATION↗

DOE OSTI2019

Embedded Optical Sensing Systems For Distribution Transformer Monitoring

Traditional utility monitoring systems do not provide real-time visibility into the condition of transformers or accurate performance measurements. This has resulted in the use of lagging indicators, such as oil sample analysis, typically requiring expensive field visits, grid outages, and laboratory sample testing. This presentation reviews the use of optical sensing systems for managing transformers and improving grid resiliency and safety. The sensing systems allow direct internal monitoring of critical transformer components. Versatility covering different monitoring parameters of interest in embedded configurations for new transformers and a retrofittable configuration for older transformers is achieved by applying hair-thin multiplexed fiber-optic and other low-profile optical sensors in combination with a high-resolution optical readout and advanced analytics. Under an initiative funded by the DOE Office of Electricity, PARC, GE and Con Edison built, tested, and qualified commercial network transformers with embedded optical sensing systems. The parameters monitored were validated across a range of scenarios with lab instruments typically used for qualification testing. An ongoing field trial to demonstrate the robustness of the technology for remote monitoring through the industrial internet under demanding grid deployment conditions in New York City is showing promise toward scale-up of the technology. This presentation will provide an overview of the typical pain points in managing transformers and parameters for monitoring. It will also cover the requirements for highly constrained installations that need to have a larger capacity and flexible rating but that must fit into a tight space. The unique capabilities of optical sensing systems and a low-cost approach to interpreting the signals from sensors in transformers for predictive maintenance will be covered. The presentation will discuss the compatibility of the sensors in the transformer environment. It will discuss the validation testing per IEEE standards that enabled the solution to be implemented in field-deployable commercial transformers. The initial results from the field deployment and the potential for the technology to provide systematic alerts for unsafe/unexpected events will be discussed. The technology could enable utility professionals to gain information they can use to better plan for maintenance/management, and improve grid performance. This would in turn accommodate DERs and other evolving grid market dynamics.

24 POWER TRANSMISSION AND DISTRIBUTION↗

DOE OSTI2015

Hard disk drive based microsecond x-ray chopper for characterization of ionization chambers and photodiodes

A fast X-ray chopper capable of producing ms long X-ray pulses with a typical rise time of few μs was realized. It is ideally suited to investigate the temporal response of X-ray detectors with response times of the order of μs to ms, in particular, any kind of ionization chambers and large area photo diodes. The drive mechanism consists of a brushless DC motor and driver electronics from a common hard disk drive, keeping the cost at an absolute minimum. Due to its simple construction and small dimensions, this chopper operates at home lab based X-ray tubes and synchrotron radiation sources as well. The dynamics of the most important detectors used in time resolved X-ray absorption spectroscopy, namely, ionization chambers and Passivated Implanted Planar Silicon photodiodes, were investigated in detail. The results emphasize the applicability of this X-ray chopper.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2015

A Public-Private-Academic Partnership to Advance Solar Power Forecasting

Executive Summary NOAA is making major contributions to the solar forecasting project in three areas. First, it is improving its forecasts of solar irradiance, clouds, and aerosols in its numerical weather prediction models. Second, it is providing advanced satellite products for DOE's FOA awardees to use in their forecast systems. Third, it is using high-quality ground-based measurements from SURFRAD and ISIS stations to verify and validate forecast model output. This reports covers results from all three areas for the period May 1, 2014 - April 30, 2015. Modeling In its modeling effort, NOAA continues work to improve the skill of solar forecasts from the Earth System Research Lab (ESRL) research versions of the 13-km Rapid Refresh (RAP) and the 3-km High-Resolution Rapid Refresh (HRRR) models, which are in turn transitioned into operations at the National Centers for Environmental Prediction (NCEP). A major milestone was achieved in September 2014 with the initial operational implementation of the HRRR at NCEP. In the ESRL research versions of the models, testing and development, in both real-time runs and retrospective experiments, is guided by an extensive in-house verification system. Early in the SFIP project, we developed the capability to verify our model forecasts against the high-quality surface radiation measurements from the SURFRAD and ISIS networks. This highlighted some shortcomings with the RAP and HRRR forecasts of incoming shortwave radiation. Most of our effort during Phase 1 of SFIP was focused on addressing these problems with a variety of model system improvements. The RAP and HRRR models during the warm season of 2014 had a noticeable warm and dry bias in near-surface conditions over most of the central and eastern United States, and our new SURFRAD/ISIS verification revealed that there was also a large excess of incoming global horizontal irradiance in the models. We hypothesized that a lack of cloud cover (particularly low-level cloud cover) in the models was resulting in too much heating of the land surface. This, in turn, caused unrealistically strong surface heat fluxes and turbulent mixing in the planetary boundary layer (PBL), which further reduced the already deficient cloud cover. We addressed these issues with a combination of data assimilation system modifications and model physics improvements. Many of our data assimilation changes were made with a view towards improving the near-term representation of clouds and precipitation. One of these changes involved better accounting for regions of weak reflectivity in the RAP cloud / hydrometeor assimilation system, in order to improve the representation of light precipitation in the RAP initial conditions and provide more realistic initial cloud cover. Additional modifications more accurately accounted for radar beam blockage and data gaps (particularly in the western United States), which improves shorter lead times forecasts of clouds and precipitation. We have also tested the assimilation of new data sources within the RAP and the HRRR, including radar radial velocity data and surface mesonet observations. Within the HRRR, we have tested the cycling of the 3-km land surface fields to allow a higher-resolution treatment of land surface processes. In terms of model physics development for SFIP, we have implemented a shallow cumulus scheme within the RAP, and have made numerous improvements to the Mellor-Yamada-Nakanishi-Niino (MYNN) PBL scheme to address insufficient low-level cloud cover in the models. We have conducted tests incorporating the radiation effects of (parameterized) boundary-layer clouds within the modified MYNN PBL scheme (independent of the convective schemes). The Grell-Freitas-Olson shallow cumulus scheme has also been tested within the 3-km HRRR. Finally, we have also modified the RUC land surface model (LSM) treatment of the vegetation wilting point, reducing it to increase evapotranspiration and increase cloud cover in the boundary layer. All of these changes work in tandem to significantly improve the model forecasts of cloud cover, incoming shortwave radiation, and near-surface temperature and moisture. Satellite The role of NOAA/NESDIS in the Solar Forecasting Improvement Project is to provide Advanced Satellite Products (ASPs) for the two forecasting teams at NCAR and IBM. The ASPs are cloud, surface, and atmosphere products derived from geostationary satellite imagery at the highest possible spatial and temporal resolution - such quantities as cloud mask, cloud probability, cloud transmission, cloud top height, cloud top temperature, cloud effective particle size, etc. Ancillary data, such as elevation and numerical weather prediction fields are provided in the files at the same resolution as well. There are at this time 147 different variables in the ASP output, including quality flags and processing information. The main goals for Year 1 of the project were to implement an Advanced Satellite Products system for the use of the IBM and NCAR teams, begin validation, and make any needed changes based on feedback from the teams. ASP files are being produced every GOES Imager acquisition, which occur on a 15-30 minute schedule. Processing is done on a dedicated computer, with a turn-around time of 8-21 minutes from image acquisition to results available on ftp. Several helpful visualizations of the data are also created for users on web pages. Users have been provided with a document titled "User's Guide for 1km Cloud Products Derived from GOES Imager Data using CLAVR-x", which discusses the basics of the source imagery, the process by which it is turned into Advanced Satellite Products, and considerations users should make when using the data. Validation of selected variables from the older 4km version of the products was also included. Future work will concentrate on validation of the 1km products and improving the turn-around time, product variety, and product quality as needed. Ground Observations In the ground-based measurement effort, NOAA's main objectives are to provide high quality radiation products for validation and verification of short-term to day-ahead solar forecasts. More specifically for the three year project, our goals include (1) Maintaining and providing data from our 7 SURFRAD and 7 ISIS; (2) Update ISIS radiation measurements from 3 min to 1 min data: (3) Purchase and install new pyrheliometers for direct solar irradiance measurements at the 7 SURFRAD sites; (4) Building, testing, and deploying two mobile SURFRAD stations at two utility plants in collaboration with DOE sponsored partners, and includes ongoing maintenance and processing of the data at the mobile sites; (5) Upgrading the data acquisition and communications at 7 SURFRAD sites and 7 ISIS sites; (6) Providing radiation data at the 7 SURFRAD sites in near real-time; (7) Develop and provide aerosol optical depth and cloud images and cloud fraction at our two mobile sites; (8) Provide data recovery rates each year; (9) Provide temporally and spatially averaged radiation products for comparison to HRRR and RAP solar forecasts and advanced satellite products; (10) Provide a data-set for analysis of conversion of direct and diffuse to sloped surfaces; (11) and as time permits develop and provide spectral solar irradiance, cloud optical depth and spectral albedo from the mobile sites. Milestones this year include working with the DOE sponsored teams to find locations to deploy two mobile SURFRAD stations. One existing unit was deployed at a 30MW PV facility in the San Luis Valley in collaboration with Xcel and the NCAR team in August, 2014. The second unit was built and tested at our facilities in Boulder, CO and deployed near Green Mountain Power's Education Center in Rutland, VT in collaboration with Green Mountain Power and the IBM Team in October, 2014. Data processing was implemented and the radiation data from these two mobile sites have been made available on our ftp server in near real-time. We also are providing images and cloud fraction from the TSI cameras for these two mobile sites on our ftp site. Another milestone was upgrading our data acquisition and communication systems at 7 SURFRAD and 7 ISIS sites. We accelerated our schedule for these upgrades to provide timely radiation products. These upgrades allow more reliable and near-real time radiation data delivery to the DOE sponsored teams to meet their goals. Lastly, we changed the data rate at the ISIS sites from 3 min to 1 min.

14 SOLAR ENERGY↗

DOE OSTI2022

A Blockchain Based Co-Simulation Framework for Integrating DERs into Wholesale Electricity Markets

As the number of distributed energy resources (DERs) continue to increase across energy-delivery systems, there remains a need for integrating their capabilities into traditional grid operations. In this paper, a blockchain-based solution is proposed to facilitate FERC's Order No. 2222 implementations. The presented use-case enables small-scale DERs to participate in wholesale market operations through DER aggregators, while also enabling local distribution system operators to enforce distribution system constraints in a secure and traceable manner. The presented use case is built around the Unified Testing Platform (UTP) being developed as a part of the Blockchain for Optimized Security and Energy Management (BLOSEM) project. This is a multi-lab effort intended to simplify the deployment of blockchain-powered grid solutions by enabling the integration of simulation tools, and blockchain technologies through the use of system-agnostic interfaces that provide a modular, interoperable, and reusable connectivity layer.

blockchain testing↗

DOE OSTI2022

A Blockchain Based Co-Simulation Framework for Integrating DERs to Wholesale Electricity Markets: Preprint

blockchain testing↗

DOE OSTI2021

Advancements of On-Line Monitoring and Real-Time Characterization of Actual Low-Level Hanford Tank-Waste Samples

Waste and process stream characterization is essential to the safe, efficient, and cost-effective processing of Hanford Site materials. The demand for materials characterization including chemical, radionuclide, and physical attributes during waste management, transfer, and staging operations in the Hanford tank farms is expected to significantly increase as the U.S. Department of Energy River Protection Project progresses toward Hanford waste treatment and immobilization. Our past work has applied Raman on-line monitoring and chemometric modeling to the supernate of Hanford tank 241-AP-105 and has demonstrated the quantitative measurement of nine analytes within this waste. To demonstrate broader applicability, this method has now been expanded to waste from two additional Hanford tanks, AW-102 and AP-107, and the offgas condensate from lab-scale melter runs of actual-tank waste feeds. To enhance the performance of the Raman method, instruments with various excitation wavelengths were compared, since it is known that the Raman response is enhanced by shorter wavelength excitation. The laser excitations for the three systems tested were 404 nm, 532 nm, and 671 nm. In addition to laser wavelength selection, the laser power, measurement integration times, and signal averaging techniques were also investigated to determine their effect on detection limits for oxy-anion analytes within tank wastes. These advancements in Raman capability are compared with past standards and will be presented.

Bryan, Samuel A.↗

DOE OSTI2021

Transportation Energy Analytics Dashboard (TEAD)

The investment decisions within the nation’s transportation sector have traditionally been prioritized and measured against safety and travel efficiency goals. Increasingly, federal, state, and local policies are requiring consideration of energy use and emissions in the design of our transportation infrastructure. Yet the processes, analytics, and knowledge to include these new metrics into transportation decisions are lacking. Although targeted studies and before and after analysis are performed from time to time, no comprehensive real-time monitoring systems provide energy and emissions to the same level as congestion and safety. To address this gap, the Center for Advanced Transportation Technology (CATT Lab) and the Maryland Transportation Institute (MTI) at the University of Maryland (UMD), in partnership with the National Renewable Energy Laboratory (NREL), have developed a Transportation Energy Analytics Dashboard, or TEAD, to raise awareness of the energy and emission impacts to the same level of observability as that of safety and mobility concerns. The overall goal of this project was to develop and demonstrate an online tool to monitor transportation energy use and emissions in real-time and to archive this data for retrospective analysis. By combining surface transportation energy and emissions evaluation capability with more traditional safety, mobility and reliability system evaluation, our goal is for TEAD to create a dynamic new paradigm in transportation systems management and performance analyses, for both real-time traffic operations, and longer-term planning for project and program investment decision-making.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

DOE OSTI2025

HiTEM

SAND2025-03438O HiTEM3d v1.0 is a user-friendly software designed to simulate how electromagnetic signals move through large geological environments, particularly around wellbores. It helps geophysicists and resource explorers understand subsurface conditions more effectively and affordably. By simplifying complex geological models, HiTEM3d allows users to visualize and analyze electromagnetic fields, making it easier to identify valuable resources like minerals or water. Its efficient processing capabilities ensure quick results, making it an essential tool for anyone involved in geophysical research or exploration. Sandia National Laboratories is a multimission laboratory managed and operated by National Technology & Engineering Solutions of Sandia, LLC, a wholly owned subsidiary of Honeywell International Inc., for the U.S. Department of Energy’s National Nuclear Security Administration under contract DE-NA0003525.

Weiss, Chester [Sandia National Lab. (SNL-CA), Liv↗

DOE OSTI2025

Cardinal: Seismic and Geoacoustic Array Processing

Data collected via seismic and infrasound array deployments are leveraged in the geosciences to detect and characterize a myriad of natural and anthropogenic sources. These deployments consist of numerous sensors placed in a predetermined configuration to amplify signal strength and improve the efficacy of array processing techniques used to measure signal directionality and waveform coherence. High‐fidelity feature extraction is often predicated on interstation distance as well as the frequency content and wavelength of an incident signal. Numerous array processing softwares analyze data in sequential frequency bands to obtain a more detailed characterization of a signal. However, current algorithms are limited in their ability to determine optimal array configuration for each band. We introduce an open‐source Python code, called Cardinal, to process seismic and infrasound array data in discretized time–frequency space with the option of applying an adaptive array design to determine optimal subarray configuration for each frequency band. To reduce computational time, the array processing step can be run in parallel using multithreading. Furthermore, the software has the capability to aggregate array processing results from different time–frequency pixels to produce separate sets of detections, or families, with added utility via the application of an adaptive semblance threshold, which aids in isolating signals‐of‐interest from coherent background noise. Upon appropriate configuration, Cardinal exhibits the potential to combine distinct seismic and infrasound phases into separate families.

Adaptive Array↗

DOE OSTI2022

Reactivity initiated accident uncertainty quantification for fuel assembly with subchannel code

UNIST CORE lab has developed a multiphysics coupling framework (MPCORE) consisting of Neutronics, Thermal Hydraulics and Fuel Performance modules. It can accommodate one-dimensional as well as sub-channel code Thermal Hydraulics (TH) module. Generally, running a transient requires more computational power due to the convergence of modules with each other. The difference between one-dimensional and sub-channel TH modules is studied in this research for a Reactivity Initiated Accident (RIA). Both TH modules are compared for a RIA uncertainty propagation in a single VERA fuel assembly with 2.11% enrichment. MPCORE is capable of analyzing the transient at any burnup point but for current work, only fresh fuel has been considered. The results have been obtained using dynamic gap heat conductance in FRAPTRAN. Peak centerline temperature, fuel enthalpy and DNBR are compared for both the approaches. The results indicate that the use of sub-channel code lead to greater safety margin for critical parameters. Computation time comparison is also presented for both the cases. (authors)

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2024

Foldy: An open-source web application for interactive protein structure analysis

Foldy is a cloud-based application that allows non-computational biologists to easily utilize advanced AI-based structural biology tools, including AlphaFold and DiffDock. With many deployment options, it can be employed by individuals, labs, universities, and companies in the cloud without requiring hardware resources, but it can also be configured to utilize locally available computers. Foldy enables scientists to predict the structure of proteins and complexes up to 6000 amino acids with AlphaFold, visualize Pfam annotations, and dock ligands with AutoDock Vina and DiffDock. In our manuscript, we detail Foldy’s interface design, deployment strategies, and optimization for various user scenarios. We demonstrate its application through case studies including rational enzyme design and analyzing proteins with domains of unknown function. Furthermore, we compare Foldy’s interface and management capabilities with other open and closed source tools in the field, illustrating its practicality in managing complex data and computation tasks. Our manuscript underlines the benefits of Foldy as a day-to-day tool for life science researchers, and shows how Foldy can make modern tools more accessible and efficient.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2018

SRNL 2017 LDRD Annual Report

Fiscal Year (FY) 2017 marked the twelfth year of Savannah River National Laboratory’s (SRNL’s) Laboratory Directed Research and Development (LDRD) program and the largest year to date. When the program began in FY06, just two years after SRNL becoming the DOE’s 17th national lab, it began with a modest authorized collection rate of just under 1.5%. It grew from there each year, reaching 4% in FY11. FY17 marked the first increase in the authorized collection rate since FY11, increasing from 4% to 5%. This increase highlights the value placed on this important program, which provides the discretionary funding needed to develop ideas for future programmatic growth in our key business areas of environmental stewardship, national security, nuclear materials management, and secure energy manufacturing, as well as develop and maintain our core competencies. The LDRD program leverages the unique capabilities of SRNL to yield foundational scientific research and development (R&D) essential to our core business areas, while aligning optimally and continuously with SRNL’s Strategic Plan and providing long-term benefits to DOE and the National Nuclear Security Administration (NNSA), other customers, and stakeholders. As can be seen in the “By the Numbers” summary, this program also plays an important role in sustaining staff excellence with high participation by students, post-docs, and early-career staff. Over 75% of the projects in FY17 included contributions from early-career or post-doctoral staff.

99 GENERAL AND MISCELLANEOUS↗

DOE OSTI2023

Demonstration of Scaled-Production of Rare Earth Oxides and Critical Materials from U. S. Coal-Based Sources (Final Report)

The project objective was to demonstrate scaled production of high purity rare earth oxides (REO), nominally exceeding 90% grade, from coal refuse sources using innovative technologies that reduce cost and improve environmental outcomes relative to traditional rare earth processing technologies. The project utilized a critical material pilot plant constructed and tested as part of a previous U.S. Department of Energy project. Target performance criteria was a 50% reduction in production cost based on previous optimum values, 150% increase in recovery and greater than 2% concentrates of rare earth oxides, cobalt and manganese. Concentrate production goals were to produce a rare earth mix oxide product at a rate of 200 grams per day having a minimum purity of 50% as well as products of cobalt and manganese having a minimum purity of 2%. A previous pilot plant investigation identified acid cost as the major contributor to an operating cost that made the recovery of rare earth and other critical metals from bituminous coal sources economically challenging. As such, acid cost reduction was a major target using bio-oxidation reactors to produce sulfuric acid from naturally occurring coal pyrite. Based on laboratory data, a bio-oxidation circuit was designed for the pilot plant to produce 7.5 l/min of acid using two 11-m3 (3000 gallon) reactors equipped with 40 hp aerators for air dispersion. The pilot-scale tests revealed that acid concentration equivalent to as high as 1.0 M sulfuric acid could be continuously produced. However, the bio-acid contained exceptionally high iron concentrations, which complicated downstream processing of the pregnant leach solution (PLS). A TEA of the bio-oxidation circuit showed that production cost was approximately $0.13 per kg acid equivalent if produced using a four-day retention time in the reactors. This value represents a 48% reduction from that of purchased bulk sulfuric acid. Calcination (or roasting) studies were conducted on coarse refuse from West Kentucky No. 13 and Fire Clay coal seam sources. The test results revealed the potential to increase recovery by nearly 100% using temperatures between 500°C to 700°C with light REE recovery value being the most improved. Acid baking of the calcined products using sulfuric acid at 250°C increased heavy rare earth recovery from around 40% to 80% while decreasing the acid requirements by over 50%. The existing pilot plant was upgraded for the pilot scale demonstration of REE and CM recovery. The primary feedstocks were West Kentucky No.13 and heap leach pregnant leach solution (PLS) while a secondary feedstock was a lignite waste material from a construction sand operation. The pilot scale operation started with PLS generation through leaching followed by iron and aluminum removal, nominally at 3.3 and 4.5 pH, respectively. Leaching lixiviants used for the test were industrial grade sulfuric acid or bio-acid generated at the pilot scale facility. For most of the tests, the solid feed rate was 200 lb/hr whereas lixiviant was added at 2 gpm to provide an optimal residence time of 45 minutes. Following the contaminant removal step, several different process schematics were tested with the goal of maximizing REE recovery and purity. In the first test, direct processing of aluminum precipitation raffinate for REE recovery using oxalic acid at pH 1.5 was investigated. Overall REE recovery was approximately 45%. Unfortunately, elevated calcium content in the PLS significantly impacted the RE-Oxide product grade. Similarly, high calcium content decreased both the product purity and grades of CM products. As such, a new flowsheet was tested with the same initial process schematic but different precipitation stages for REEs and CMs at pH 6.0 and 9.0, respectively. It was noted that the overlapping precipitation behavior of Co, Ni and Zn with REEs limited the applicability of this process schematic. While this change increased the RE-Oxide grade from 36% in the first test to 87%, the loss of critical metals to the REE cake and bypass of the REEs to the CM cake significantly impacted the recovery of both REEs and CMs. Therefore, the modified process flowsheet combined oxalic acid precipitation stage raffinate and redissolved CM cake filtrate to maximize both the recovery and purity of the products. Consequently, a RE-Oxide product with 85% purity and CM cakes with over 19% Co, 38% Ni, 14% Zn and 9% Mn content were generated with significantly higher recoveries. While the modified process flowsheet improved recoveries and grades, elemental losses observed in separate precipitation and redissolution losses inspired the adaptation of a single precipitation stage at pH 9.0 for both REEs and CMs. This change was anticipated to maximize the REE recovery while minimizing the costs associated with separated redissolution and processing stages. As expected, REE recovery in this new circuit arrangement was over 56% with a product grade of over 87% RE-Oxide content. Similarly, Co, Ni, Mn, and Zn recoveries of 54%, 40%, 67%, and 66%, respectively, were achieved. Unfortunately, the elevated calcium content present in the solution due to its precipitation at pH 9.0 caused a decrease in the CM cake quality. Therefore, the final process flowsheet involved the addition of calcium oxalate precipitation following the oxalic acid precipitation stage, which effectively eliminated calcium contamination of the CM products. Finally, the pilot scale experiments conducted using bio-acid achieved comparable REE leaching recoveries to the conventional sulfuric acid leaching. Elevated iron concentration in the solution caused the co-precipitation of REEs with the iron and aluminum cake, resulting in the REE losses. Furthermore, elevated iron content bypassing the iron and aluminum precipitation stages contaminated the metal sulfide and manganese cake, respectively. A techno-economic analysis was performed based on a commercial facility capable of treating 500 tph of coal-based material. The production cost for West Kentucky No. 13 coarse refuse material ranged from approximately $500-$700/kg of total rare earth oxide whereas the lignite source had significantly lower production cost of $100-$300/kg. The significant difference in cost was due to the easier leaching characteristics of the lignite material and the higher feed concentrations. All process scenarios resulted in a negative net present value (NPV). For the lignite feedstock, laboratory REE leach recovery values were about 30% higher than the pilot plant data. Using the lab leach results, a positive net present value was achieved and the production cost decreased from $100-$300 $/kg to less than $150/kg of total REO.

01 COAL, LIGNITE, AND PEAT↗