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DOE OSTI2023

Extending Magnetic Core Shell Nanoparticle Extraction Technology to Cesium and Antimony Removal from Geothermal Brines in New Zealand

Our industrial client (Geo40) has developed and deployed a process to remove silica from geothermal fluids and produce a high-margin specialty colloidal silica product comparable to those of market leaders. Geo40 now wishes to explore opportunities to extend their mineral extraction operations to other elements that are present in these brines. Geo40 has identified cesium (Cs) that is present in Ohaaki brines (pH ~8–8.5) at parts per million levels and could be sold to customers if it could be produced at an attractive price. With support from the Department of Energy’s (DOE’s) Geothermal Technologies Office, a simple and highly cost-effective magnetic nanofluid method for extraction of rare earth elements (REEs) from geothermal brine solutions has been developed and demonstrated at the laboratory bench scale at Pacific Northwest National Laboratory (PNNL). Core shell sorbent particles are produced using an iron oxide core particle, which is used to anchor and grow a surrounding adsorbent shell functionalized with a chelating ligand that selectively binds REEs. We extended PNNL’s work by exploring new sorbent shells that are highly selective for Cs. Uptake of Cs was measured as a function of exposure time by analyzing solution samples extracted from batch sorption tests.

15 GEOTHERMAL ENERGY↗

DOE OSTI2022

A machine learning approach for clinker quality prediction and nonlinear model predictive control design for a rotary cement kiln

Abstract Cement manufacturing is energy‐intensive (5Gj/t) and comprises a significant portion of the energy footprint of concrete systems. Incorporating modern monitoring, simulation and control systems will allow lower energy use, lower environmental impact, and lower costs of this widely used construction material. One of the goals of the CESMII roadmap project on the Smart Manufacturing of Cement included developing an analytical process model for clinker quality that includes the chemistry of the kiln feed and accounts for critical process variables. This predictive model will be used in nonlinear model predictive control system designed to significantly reduce process energy use while maintaining or improving product quality. In the cement manufacturing plant used in this study, the kiln feed (meal) is tested every 12 h and used to estimate the mineral composition of the cement kiln output (clinker) using the stoichiometry‐based Bogue's model and the expertise of the plant operators. During kiln operation, kiln output (clinker) is sampled and tested every 2 h to measure its chemical and mineral composition. The predicted and measured values of the clinker composition are used by the plant operators to adjust the kiln input stream and the production process characteristics to maintain stable operation and uniform product quality. However, the time delay between prediction and testing, along with inaccuracies inherent in the Bogue's model have made any process changes designed to minimize energy use problematic, especially in‐light of potential clinker quality issues that process changes often pose. A new analytical model that integrates quality information and process operation information has been developed from data collected from 2 years of production from an operating cement facility. To make the model fuel‐type‐independent, consumed heat energy was computed in the model instead of fuel type and amount. A Feedforward Network was trained and tailored from collected data. Many data‐based simulations were conducted to quantitatively evaluate the proposed model and the 5‐fold cross‐validation procedure was used to test the models. The resulting predictive model was shown to have a low root mean square error (MSE) with respect to the estimated clinker mineral composition compared to that using the industry standard “Bogue’ model”. The end goal of this work was to develop a single machine learning tool that allows the use of quality control data and process control variables to improve energy efficiency of the process in a continuous fashion. The proposed nonlinear model predictive control system (NMPC) can generate predicted kiln production characteristics based on manipulated variables in manner that accurately follows the target product quality values. Simulation results also show that the proposed model produced accurate predictions of kiln outputs that fell within the required constraints, while manipulating control variables within typical operational ranges.

Ali, Asem M.↗

DOE OSTI2023

Metagenomic Methods for Addressing NASA's Planetary Protection Policy Requirements on Future Missions: A Workshop Report

Molecular biology methods and technologies have advanced substantially over the past decade. These new molecular methods should be incorporated among the standard tools of planetary protection (PP) and could be validated for incorporation by 2026. To address the feasibility of applying modern molecular techniques to such an application, NASA conducted a technology workshop with private industry partners, academics, and government agency stakeholders, along with NASA staff and contractors. The technical discussions and presentations of the Multi-Mission Metagenomics Technology Development Workshop focused on modernizing and supplementing the current PP assays. The goals of the workshop were to assess the state of metagenomics and other advanced molecular techniques in the context of providing a validated framework to supplement the bacterial endospore-based NASA Standard Assay and to identify knowledge and technology gaps. In particular, workshop participants were tasked with discussing metagenomics as a stand-alone technology to provide rapid and comprehensive analysis of total nucleic acids and viable microorganisms on spacecraft surfaces, thereby allowing for the development of tailored and cost-effective microbial reduction plans for each hardware item on a spacecraft. Workshop participants recommended metagenomics approaches as the only data source that can adequately feed into quantitative microbial risk assessment models for evaluating the risk of forward (exploring extraterrestrial planet) and back (Earth harmful biological) contamination. Participants were unanimous that a metagenomics workflow, in tandem with rapid targeted quantitative (digital) PCR, represents a revolutionary advance over existing methods for the assessment of microbial bioburden on spacecraft surfaces. The workshop highlighted low biomass sampling, reagent contamination, and inconsistent bioinformatics data analysis as key areas for technology development. Finally, it was concluded that implementing metagenomics as an additional workflow for addressing concerns of NASA's robotic mission will represent a dramatic improvement in technology advancement for PP and will benefit future missions where mission success is affected by backward and forward contamination.

59 BASIC BIOLOGICAL SCIENCES↗

NASA NTRSDate not supplied

Identifying Indicators of Harmful Algal Blooms in Coastal Atacama Using Satellite Image Processing Techniques to Improve Industry and Authority Response

Over the past decade, Chile has experienced a significant rise in both the frequency and intensity of coastal Harmful Algal Blooms (HABs). These bloom events are a growing concern for the Atacama Region especially, with potential impacts on human health, aquaculture, and the environment. HABs are caused by an excess proliferation of microalgae, with certain algae species commonly found in Chilean HABs capable of producing toxins which can poison fish, toxify shellfish, and cause illness or death when ingested by humans. Collaborating with the Ministry of Health of Chile, Centro de Información de Recursos Naturales, the University of Atacama, and the Embassy of Chile’s Agricultural Office, this study identifies potential indicators of HABs in the Coastal Atacama Region using NASA Earth observations. Satellite imagery from the Moderate Resolution Imaging Spectroradiometer (MODIS) instrument onboard NASA’s Aqua satellite was used for the identification of chlorophyll-a which provides direct estimates of the algae pigment’s concentration in water bodies. In addition, the spatiotemporal patterns of several other parameters were examined to identify correlations with occurrences of HABs, including sea surface temperature and normalized fluorescence line height using Aqua MODIS, Normalized Difference Turbidity Index (NDTI) using Landsat 8, and ocean wind speed measurements from the NOAA Joint Polar Satellite System. Analysis of these patterns revealed hotspots of high chlorophyll-a concentrations from the years 2014 to 2022, the most major of which occurring in the coastal zones of Chañaral, Bahía Inglesa, and Huasco. Also, through the use of a similarity search conducted, the seasonal variation of these indicators was mapped to highlight areas with great likelihood of experiencing HABs in the future. The results can guide future efforts for in-situ water sampling, toxin analysis and assessment, and HAB monitoring and prevention.

Cody O'Ferrall↗

DOE OSTI2020

Analysis of Respirator Cartridge Performance Testing on Hanford Tank A-101

Washington River Protection Solutions (WRPS) conducted tests on two types of chemical cartridges for use in air purifying respirators (APR) to determine the period of time that the cartridges would provide adequate performance1 to protect workers when exposed to a mixture of Chemicals of Potential Concern (COPCs) from vapors emanating from the headspace of tank A-101 on the Hanford Site. The Occupational Safety and Health Administration (OSHA) identifies cartridge testing as a valid approach for establishing a cartridge change schedules.[3] Testing is commonly applied in situations where mixtures of COPCs exist, and where other approaches, such as manufacturer recommendations and modeling, are less reliable. The tests were designed and conducted to ensure measurement and/or control of the key variables OSHA identified as important to estimate cartridge service life, including temperature, humidity, COPC concentration, breathing rate, and cartridge adsorption capacity. Testing was conducted over a period from July 22-24, 2016, using headspace vapors from Hanford tank A-101 under static conditions2 fed to a respirator cartridge test stand developed by WRPS in collaboration with HiLine Engineering (Richland, Washington). Multipurpose respirator cartridges, SCOTT 7422-SD1 and 7422-SC1 (SCOTT Safety, Monroe, North Carolina) were assessed on separate days with A-101 headspace vapors. Sample media (sorbent tubes) were used to collect samples of the vapor stream entering and exiting the respirator cartridge, and were subsequently analyzed for COPC concentrations. Pacific Northwest National Laboratory was tasked with conducting an independent analysis of the analytical results and making recommendations based on the results for respiratory cartridge performance and service life. Key conclusions from the assessment of the 59 COPCs in this study are described below: • Based on d measured cartridge inlet vapor concentrations from tank A-101 headspace, both ammonia and N-Nitrosodimethylamine (NDMA) exceeded their Occupational Exposure Limits (OEL).3 These measurements were generally consistent with maximum A-101 headspace measurements previously obtained for these two compounds. • Ammonia had respirator cartridge outlet concentrations that exceeded 10% of the OEL for both cartridges tested, indicating breakthrough for each. For the SCOTT 7422-SD1 cartridge, ammonia appeared to breakthrough above 10% of its OEL after 2 hours. For the SCOTT 7422-SC1 cartridge, ammonia breakthrough appeared to occur after 8 hours. 1 “Adequate performance” refers to the breakthrough criteria used in this analysis—that is, sustained cartridge outlet concentrations above 10% of the OEL. For some COPCs, an alternate threshold has been applied when necessary due to higher detection limit (DL)/reporting limit (RL) values for specific compounds. Ultimately, Industrial Hygiene professionals will use these results along with specific hazard assessments to determine service life and cartridge use that provides the necessary performance. 2 These tests were conducted under static conditions absent waste-disturbing activities in the subject tank or tank farm. 3 Occupational Exposure Limits accepted for Hanford Tank Farm use are based on OELs established by a U.S. governmental agency or national professional organization (e.g., OSHA, National Institute for Occupational Safety and Health, American Conference of Governmental Industrial Hygienists), or if no U.S. OEL exists, standard toxicological practices are applied to develop OELs using non-U.S. exposure limits, other established OELs for chemical surrogates when available, or other standard procedures. The OEL for NDMA was established in 2005 based on the MAK (Maximale Arbeitsplatzkonzentration) Commission standard adopted in Europe. iv • Despite respirator inlet measurements for NDMA that were in excess of its OEL, all corresponding outlet measurements, from both respirator cartridges, were below analytical DL 1 for the

61 RADIATION PROTECTION AND DOSIMETRY↗

NASA NTRS2006

Development and Characterization of Improved NiTiPd High-Temperature Shape-Memory Alloys by Solid-Solution Strengthening and Thermomechanical Processing

The need for compact, solid-state actuation systems for use in the aerospace, automotive, and other transportation industries is currently motivating research in high-temperature shape-memory alloys (HTSMA) with transformation temperatures greater than 100 C. One of the basic high-temperature alloys investigated to fill this need is Ni(19.5)Ti(50.5)Pd30. Initial testing has indicated that this alloy, while having acceptable work characteristics, suffers from significant permanent deformation (or ratcheting) during thermal cycling under load. In an effort to overcome this deficiency, various solid-solution alloying and thermomechanical processing schemes were investigated. Solid-solution strengthening was achieved by substituting 5at% gold or platinum for palladium in Ni(19.5)Ti(50.5)Pd30, the so-called baseline alloy, to strengthen the martensite and austenite phases against slip processes and improve thermomechanical behavior. Tensile properties, work behavior, and dimensional stability during repeated thermal cycling under load for the ternary and quaternary alloys were compared. The relative difference in yield strength between the martensite and austenite phases and the dimensional stability of the alloy were improved by the quaternary additions, while work output was only minimally impacted. The three alloys were also thermomechanically processed by cycling repeatedly through the transformation range under a constant stress. This so-called training process dramatically improved the dimensional stability in these samples and also recovered the slight decrease in work output caused by quaternary alloying. An added benefit of the solid-solution strengthening was maintenance of enhanced dimensional stability of the trained material to higher temperatures compared to the baseline alloy, providing a greater measure of over-temperature capability.

Bigelow, Glen↗

DOE OSTI2022

All-Inorganic Open-Framework Chalcogenides, A 3 Ga 5 S 9 · x H 2 O ( A = Rb and Cs), Exhibiting Ultrafast Uranyl Remediation and Illustrating a Novel Post-Synthetic Preparation of Open-Framework Oxychalcogenides

Fast and effective uranyl sequestration is of interest to the nuclear industry. Recently layered chalcogenide materials have demonstrated fast, selective, and efficient sorption properties towards uranyl cations and the development and investigation of new types of chalcogenide materials continues to be of interest and represents an intriguing option for uranyl remediation. Three new all-inorganic A 3 Ga 5 S 9 ·xH 2 O (A = Rb, Rb/Cs, and Cs) open-framework chalcogenides were obtained via an in-situ alkali carbonate to alkali sulfide conversion process achieved under mild hydrothermal conditions. The structures of the all-inorganic open framework chalcogenides consist of a 2-fold interpenetrated diamond-like 3D framework containing pseudo-T 3 [Ga 10 S 20 ] 10– supertetrahedra. 48% of the structural volume is occupied by A + cations and water species, as established by single-crystal X-ray diffraction (SCXRD), infrared (IR) and energy-dispersive (EDS) spectroscopies. The dynamic nature of the A + cations and water molecules within the pores was investigated via single crystal X-ray diffraction as well as by IR spectroscopy monitored H 2 O to D 2 O exchange experiments. Framework stability was probed with post-synthetic treatment of A 3 Ga 5 S 9 ·xH 2 O (A = Rb and Cs) samples in acidic solutions that resulted in the formation of the oxysulfide (A/H) 3 Ga 5 S 9–y O y ·xH 2 O (A = Rb and Cs; y = 0–1), as shown by SCXRD and IR. Ion-exchange studies on A 3 Ga 5 S 9 ·xH 2 O (A = Rb and Cs) samples were carried out utilizing a uranyl acetate solution. The presence of the UO 2 2+ species in the ion-exchanged product was supported by IR and EDS spectroscopies. Batch method ion-exchange experiments on Cs 3 Ga 5 S 9 ·xH 2 O powder demonstrated fast kinetics with 95% uranyl removal from the uranyl acetate solution during the first minute, a maximum uranyl uptake capacity of 15mg/g, and the subsequent elution of uranyl species with KCl solution. Furthermore, the porous and dynamic nature of the A 3 Ga 5 S 9 ·xH 2 O framework coupled with effective UO 2 2+ ···S 2– bonding interactions makes it a good potential sorbent for uranyl remediation from aqueous media.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Key environmental and production factors for understanding variation in switchgrass chemical attributes

Abstract Switchgrass ( Panicum virgatum L.) is a promising feedstock for bioenergy and bioproducts; however, its inherent variability in chemical attributes creates challenges for uniform conversion efficiencies and product quality. It is necessary to understand the range of variation and factors (i.e., field management, environmental) influencing chemical attributes for process improvement and risk assessment. The objectives of this study were to (1) examine the impact of nitrogen fertilizer application rate, year, and location on switchgrass chemical attributes, (2) examine the relationships among chemical attributes, weather and soil data, and (3) develop models to predict chemical attributes using environmental factors. Switchgrass samples from a field study spanning four locations including upland cultivars, one location including a lowland cultivar, and between three and six harvest years were assessed for glucan, xylan, lignin, volatiles, carbon, nitrogen, and ash concentrations. Using variance estimation, location/cultivar, nitrogen application rate, and year explained 65%–96% of the variation for switchgrass chemical attributes. Location/cultivar × year interaction was a significant factor for all chemical attributes indicating environmental‐based influences. Nitrogen rate was less influential. Production variables and environmental conditions occurring during the switchgrass field trials were used to successfully predict chemical attributes using linear regression models. Upland switchgrass results highlight the complexity in plant responses to growing conditions because all production and environmental variables had strong relationships with one or more chemical attributes. Lowland switchgrass was limited to observations of year‐to‐year environmental variability and nitrogen application rate. All explanatory variable categories were important for lowland switchgrass models but stand age and precipitation relationships were particularly strong. The relationships found in this study can be used to understand spatial and temporal variation in switchgrass chemical attributes. The ability to predict chemical attributes critical for conversion processes in a geospatial/temporal manner would provide state‐of‐the‐art knowledge for risk assessment in the bioenergy and bioproducts industry.

09 BIOMASS FUELS↗

DOE OSTI2022

Tuscaloosa Marine Shale Laboratory

The Tuscaloosa Marine Shale (TMS) in Louisiana and Mississippi is an Upper Cretaceous source rock formation sandwiched between the sands of the upper and lower Tuscaloosa sections. The TMS is believed to be the source rock for underlying prolific Tuscaloosa sand formation. The TMS has an unproven estimate of 7,000,000,000 bbls of recoverable oil while its current total average production is about 3,000 bbls of oil per day in 2017. In 2013 and 2014, more than 80 wells were drilled horizontally into the TMS that were fractured using multi-stage fracturing technology. The results from this have been mixed, but recent production for several wells show an appealing initial oil production rate of more than 1000 bbl/day. The preliminary core analysis by industry partners and a few literature studies shows that the TMS is one of the most clay-rich and sensitive shales to water. Due to these and other technical problems, there is high risk for the economic development of TMS compared to other shale plays. The experiences of major industrial players in the TMS show the necessity of open and collaborative efforts to better understand the critical gaps in the development of this challenging and potentially highly economic shale play to enable more cost-efficient and environmentally-sound recovery from this unconventional liquid-rich shale play. The overall objective of this project is to form a consortium of science and industry partners to address the following six major objectives using scientific and technical approaches: 1. To improve wellbore integrity by better understanding the sources of the wellbore instability issues, proposing innovative mud and cement design for the TMS. 2. To improve formation evaluation using laboratory techniques for the evaluation of mineralogical composition, organic content, and produced-water chemistry as well as well log and geophysical analysis. 3. To determine the role of geologic discontinuities on fracture growth and shale creep behavior using digital image correlation technique. 4. To investigate the application of stable CO 2 foam and super-hydrophobic proppants for improved reservoir stimulation. 5. To better understand the nature of water/hydrocarbon/CO 2 flow in clay and organic-rich formation and the role of water/fluid interaction on recovery. 6. To prepare better socio-economic environment for TMS development by community engagement. Subsequently, the TMS virtual laboratory conducted testing and analysis of various properties of rock and formation fluids from the TMS, including but not limited to the following: Analyzing reports and logs to better understand the source of wellbore instability in TMS wells; Experiments to design a customized cement based on TMS requirements; Experiments to obtain the mineralogical and geochemical composition of TMS samples; Seismic analysis of TMS geophysical data to better predict total organic carbon (TOC) content and brittleness in TMS; Well log analysis to better estimate the TOC and geo-mechanical properties of TMS; Experiments on formation water to understand the chemistry of produced water; Experiments to determine the role of lamination and natural fractures on fracture propagation or rock deformation using digital image correlation technique in in-direct tensile tests, semi-circular bend test and creep tests Experiments to determine the stability and rheological properties of nanoparticle-stabilized CO 2 foam in TMS rock samples; Experiments to determine fluid dynamics in un-propped TMS fractures and the role of nano-coating of proppants on fluid dynamics in fractures with proppants; Micro-fluidics experiments to enhance the understanding of fluid dynamics in tight liquidrich pores with high clay content; Socio-economic studies to better engage communities in TMS development.

58 GEOSCIENCES↗

DOE OSTI2025

Application of Raman Spectroscopy to Determine Uranium Content in ADUN Solution

The work presented in this report is part of the ongoing efforts to address the nuclear material control and accounting needs for advanced reactor fuel fabrication facilities. This work was supported by the Materials Protection, Accounting, and Control Technologies (MPACT) program under the US Department of Energy Office of Nuclear Energy‘s Nuclear Fuel Cycle and Supply Chain program. The activities and engagements under the MPACT program are designed to support a robust US civilian nuclear energy enterprise. In the work described in this report, we supported MPACT objectives by developing measurement techniques that could be used for material accounting and process monitoring and by working with industry partners to identify existing gaps and areas for improvement. Oak Ridge National Laboratory has been working with commercial tristructural isotropic (TRISO) fuel fabricators such as Standard Nuclear to develop technology for rapid and cost-effective uranium content assessment. This work has focused on demonstrating advanced measurement techniques (e.g., Raman spectroscopy) that can be used for rapid, reliable, and cost-effective routine measurements of uranium content in feed solutions and liquid waste streams as well as for monitoring in-line process measurements and product streams. Specifically, this report explores techniques for accurately determining uranium content in acid-deficient uranyl nitrate (ADUN) solutions and detecting low uranium concentrations in ammonia solutions. Developing such measurement techniques will benefit TRISO fuel fabrication facilities, facilities involved in other parts of the fuel cycle that require online monitoring of aqueous solutions, and potentially molten salt fuel reactors. This work supports developing Raman spectroscopy procedures to determine uranium concentrations in ADUN solutions, which are used as feedstock in the sol–gel process for creating TRISO fuel. Some additional benefits of using Raman spectroscopy for uranium quantification in fabrication facilities include enabling online monitoring of the chemical process, which would provide near real-time feedback; eliminating the need for sample transfers, preparation, or dilution; providing nondestructive measurements; and user friendliness. In this fiscal year, FY25, we determined the identity of the unknown Raman band at approximately 853 cm−1 that was discovered in ADUN Raman spectra in FY24, created calibration curves and determined uranium concentrations of two ADUN solutions, and compared the Raman results to results obtained from inductively coupled plasma mass spectrometry and Davies–Gray titration. Furthermore, we have identified focus areas for experimentation in future fiscal years. A key result is that the accuracy of using Raman can provide accuracy comparable to destructive analysist techniques, With a well-developed calibration curve, using standards and a large number of samples (more than five samples), uncertainty on the order of 1%–3% is achievable. Given that the uncertainties achieved by Raman spectroscopy were on the order of the uncertainties achieved using ICP-MS, we conclude that with a well-developed procedure Raman spectroscopy can be used to determine uranium concentrations in ADUN solutions for NMC&A applications. The benefits of such an approach are that the time and effort will be less than that of comparable destructive analysis techniques, with approximately the same level of technical expertise. This will be attractive to operators of fuel fabrication facilities as it will lower costs and improve efficiencies.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2020

Decreasing wind speed extrapolation error via domain-specific feature extraction and selection

Abstract. Model uncertainty is a significant challenge in the wind energy industry and can lead to mischaracterization of millions of dollars' worth of wind resources. Machine learning methods, notably deep artificial neural networks (ANNs), are capable of modeling turbulent and chaotic systems and offer a promising tool to produce high-accuracy wind speed forecasts and extrapolations. This paper uses data collected by profiling Doppler lidars over three field campaigns to investigate the efficacy of using ANNs for wind speed vertical extrapolation in a variety of terrains, and it quantifies the role of domain knowledge in ANN extrapolation accuracy. A series of 11 meteorological parameters (features) are used as ANN inputs, and the resulting output accuracy is compared with that of both standard log-law and power-law extrapolations. It is found that extracted nondimensional inputs, namely turbulence intensity, current wind speed, and previous wind speed, are the features that most reliably improve the ANN's accuracy, providing up to a 65 % and 52 % increase in extrapolation accuracy over log-law and power-law predictions, respectively. The volume of input data is also deemed important for achieving robust results. One test case is analyzed in depth using dimensional and nondimensional features, showing that the feature nondimensionalization drastically improves network accuracy and robustness for sparsely sampled atmospheric cases.

17 WIND ENERGY↗

NASA NTRS2018

Radar Measurements of the LEO Orbital Debris Environment

Access to space and the preservation of the near-Earth space environment is of critical significance. Increased interest in issues surrounding space traffic management and the continued assessment and discussion of orbital debris at the United Nations Committee on the Peaceful Uses of Outer Space (COPUOS) illustrates the significance of the topic of orbital debris. There are currently over 20,000 tracked objects in the publicly available satellite catalog on Space-Track.org. The catalog is maintained by the US Air Force Space Command using a network of optical and radar ground-based sensors and is believed to be complete for a characteristic size of 10 cm or larger in low Earth orbit (LEO). Based on the work of the NASA Orbital Debris Program Office (ODPO) over approximately the past 40 years it is understood that the small debris population (< 10 cm) increases by orders of magnitude as characteristic size decreases. With population estimates ranging from 500,000 to 1,000,000 small debris objects (> 5 mm) in orbit, it is currently not practical to track and maintain precision orbits on every object. Instead the NASA ODPO uses powerful ground-based radars to sample the low Earth Orbit (LEO) environment and assign approximate orbits to each detection. This poses an interesting signal processing challenge as we are trying to detect the smallest objects possible on the edge of the radar's sensitivity. For approximately the last 30 years, NASA ODPO has partnered with the Massachusetts Institute of Technology Lincoln Laboratory (MIT/LL) to utilize the Haystack Ultra-wideband Satellite Imaging Radar (HUSIR - formerly the Long-Range Imaging Radar or simply Haystack) and the Haystack Auxiliary (HAX) radar to collect orbital debris radar data. Additionally, the ODPO collaborates with the NASA Jet Propulsion Laboratory (JPL) to use the Goldstone Solar System Radar. The orbital debris detections from these radars serve as inputs for statistical risk models used by the human spaceflight and satellite communities to assess risk to spacecraft posed by orbital debris. In this paper, we will describe the history of orbital debris radar measurements conducted by NASA, provide an overview of current radar measurements techniques and facilities, discuss the signal processing software used for orbital debris measurements and the inference of debris size and orbital parameters from these measurements, and discuss how orbital debris radar measurements are validated for use in models that are used throughout the aerospace industry.

Blackwell, Chris↗

DOE OSTI2024

Experimental Examination of Additively Manufactured Patterns on Structural Nuclear Materials for Digital Image Correlation Strain Measurements

Abstract Background There are a limited number of commercially available sensors for monitoring the deformation of materials in-situ during harsh environment applications, such as those found in the nuclear and aerospace industries. Such sensing devices, including weldable strain gauges, extensometers, and linear variable differential transformers, can be destructive to material surfaces being investigated and typically require relatively large surface areas to attach (> 10 mm in length). Digital image correlation (DIC) is a viable, non-contact alternative to in-situ strain deformation. However, it often requires implementing artificial patterns using splattering techniques, which are difficult to reproduce. Objective Additive manufacturing capabilities offer consistent patterns using programmable fabrication methods. Methods In this work, a variety of small-scale periodic patterns with different geometries were printed directly on structural nuclear materials (i.e., stainless steel and aluminum tensile specimens) using an aerosol jet printer (AJP). Unlike other additive manufacturing techniques, AJP offers the advantage of materials selection. DIC was used to track and correlate strain to alternative measurement methods during cyclic loading, and tensile tests (up to 1100 µɛ) at room temperature. Results The results confirmed AJP has better control of pattern parameters for small fields of view and facilitate the ability of DIC algorithms to adequately process patterns with periodicity. More specifically, the printed 100 μm spaced dot and 150 μm spaced line patterns provided accurate measurements with a maximum error of less than 2% and 4% on aluminum samples when compared to an extensometer and commercially available strain gauges. Conclusion Our results highlight a new pattern fabrication technique that is form factor friendly for digital image correlation in nuclear applications.

Novich, K. A. (ORCID:0000000204466022)↗

NASA NTRS2010

Identifying Aerosol Type/Mixture from Aerosol Absorption Properties Using AERONET

Aerosols are generated in the atmosphere through anthropogenic and natural mechanisms. These sources have signatures in the aerosol optical and microphysical properties that can be used to identify the aerosol type/mixture. Spectral aerosol absorption information (absorption Angstrom exponent; AAE) used in conjunction with the particle size parameterization (extinction Angstrom exponent; EAE) can only identify the dominant absorbing aerosol type in the sample volume (e.g., black carbon vs. iron oxides in dust). This AAE/EAE relationship can be expanded to also identify non-absorbing aerosol types/mixtures by applying an absorption weighting. This new relationship provides improved aerosol type distinction when the magnitude of absorption is not equal (e.g, black carbon vs. sulfates). The Aerosol Robotic Network (AERONET) data provide spectral aerosol optical depth and single scattering albedo - key parameters used to determine EAE and AAE. The proposed aerosol type/mixture relationship is demonstrated using the long-term data archive acquired at AERONET sites within various source regions. The preliminary analysis has found that dust, sulfate, organic carbon, and black carbon aerosol types/mixtures can be determined from this AAE/EAE relationship when applying the absorption weighting for each available wavelength (Le., 440, 675, 870nm). Large, non-spherical dust particles absorb in the shorter wavelengths and the application of 440nm wavelength absorption weighting produced the best particle type definition. Sulfate particles scatter light efficiently and organic carbon particles are small near the source and aggregate over time to form larger less absorbing particles. Both sulfates and organic carbon showed generally better definition using the 870nm wavelength absorption weighting. Black carbon generation results from varying combustion rates from a number of sources including industrial processes and biomass burning. Cases with primarily black carbon showed improved definition in the 870nm wavelength absorption weighting due to the increased absorption in the near-infrared wavelengths, while the 440nm wavelength provided better definition when black carbon mixed with dust. Utilization of this particle type scheme provides necessary information for remote sensing applications, which needs a priori knowledge of aerosol type to model the retrieved properties especially over semi-bright surfaces. In fact, this analysis reveals that the aerosol types occurred in mixtures with varying magnitudes of absorption and requires the use of more than one assumed aerosol mixture model. Furthermore, this technique will provide the aerosol transport model community a data set for validating aerosol type.

Giles, D. M.↗

NASA NTRS2006

The Ability of AMSTAR Dechlorination Solution to Remove and Degrade PCBs from Contaminated Surfaces

Polychlorinated biphenyls (PCBs) are a group of synthetic aromatic compounds with the general formula C12H(10-x)Cl(-x) that were historically used in industrial paints, caulking material and adhesives, as their properties enhanced structural integrity, reduced flammability and boosted antifungal properties. Although the United States Environmental Protection Agency (USEPA) has banned the manufacture of PCBs since 1979, they have been found in at least 500 of the 1,598 National Priorities List (Superfund) sites identified by the USEPA. Prior to the US EPA's ban on PCB production, PCBs were commonly used as additives in paints and asphalt-based adhesives that were subsequently applied to a variety of structures. Government facilities constructed as early as 1930 utilized PCB-containing binders or PCB-containing paints, which are now leaching into the environment and posing ecological and worker health concerns. In 2006, a commercially available product known as AMSTAR Dechlorination Solution was tested at NASA's Kennedy Space Center for its ability to remove and degrade PCBs from structural materials. This evaluation was requested by the Environmental Security Technology Certification Program (ESTCP) evaluating the ability of NASA's Bimetallic Treatment System (BTS) to remove and degrade PCBs from structural materials. The results of the laboratory testing are to be used to determine if a side-by-side field-scale test comparing BTS to AMSTAR was warranted. A recommended sampling and analysis testing program was submitted to ESTCP that included triplicate screening of AMSTAR's PCB dechlorination capabilities on a variety of surfaces including glass, bare metal, and painted metal coupons. The test procedures, analytical techniques and results obtained are presented in this interim report to ESTCP.

Quinn, Jacqueline E.↗

DOE OSTI2022

Illuminating the Photophysics of Oxygen Atom Transfer in Rare Earth Metal-Organic Complexes

Industrial separations of rare earth metals are reliant on selectivity based on ionic radii, which are time, energy, and resource consuming.1 The unique and discontinuous manifold of energy states associated with the f-electron configurations of the rare earth ions2 offer an opportunity to overcome some of these limitations by incorporating light into the separation process. Here, we use transient absorption spectroscopy to understand the differences in mechanism of light-initiated oxygen atom transfer (OAT) in yttrium (Y) and dysprosium (Dy) rare earth complexes. These metal-organic complexes are functionalized with hexfluoroacetyl-acetonate (hfac) and 4-methylmorpholine-N-oxide (NMMO). After light absorption in the presence of triphenyl phosphine (TPP), the NMMO in the Y-NMMO complex is replaced by the TPPO OAT reaction product. Because the Dy f-electron manifold is accessible to the ligand excited states, while there are no accessible states associated with f-electrons for Y, there are significant differences in reactivity. Transient absorption spectroscopy (TAS) was used to monitor changes after 340 nm photoexcitation of Dy/Y-NMMO or the product complex Dy/Y-TPPO. TAS is a pump-probe technique where a white light probe pulse is delayed relative to a visible pump pulse, which photoexcites a sample. Differences between the ground and excited states are monitored over time. With TAS, we access time scales from 100 fs-400 us to determine the photophysics of the complexes of interest. Photoexcitation of Y-NMMO (Fig. 1A) creates a broad photoinduced absorption (PIA) that evolves into a sharp positive feature over 4.2 ps centered at 450 nm. A secondary feature centered at 550 nm grows in with a 200 ps time constant and remains through the 5 ns time window of our experiment. Control experiments for Y-TPPO reveal that the feature at 450 nm is due to internal dynamics of the hfac ligand, while the 550 nm shoulder is due to the presence of the NMMO. Comparing kinetics at 550 nm for Y-NMMO and Dy-NMMO (Fig. 1B) shows that while Y exhibits a distinct growth in the NMMO feature, the Dy decays almost completely within 5 ns. Control experiments with Dy-TPPO prove that the ligand excited states centered on the hfac ligand are deactivated via energy transfer to the Dy manifold within 200 ps. This deactivation leads to significant differences in OAT reactivity between Y and Dy.

CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSICS↗

NASA NTRS2001

A Rover Deployed Ground Penetrating Radar on Mars

Radar is a fundamental tool capable of addressing a variety of geological problems on Mars via collection of data suitable for interpreting variations in surface morphology and reflectivity. Surface-deployed ground penetrating radar (GPR) can help further constrain the geology and structure of the near surface of Mars by directly measuring the range and character of in situ radar properties. In recognition of this potential, a miniaturized, easily modified GPR is being developed for possible deployment on a future Mars rover and will enable definition of radar stratigraphy at high spatial resolution to depths of 10-20 meters. Ongoing development of a Mars impulse GPR with industry partners at Geophysical Survey Systems, Inc., focuses on design and testing of a prototype transducer array (with both high frequency bistatic and low frequency monostatic components) in parallel with fabrication of a low power, mass, and volume control unit. The operational depth of 10-20 meters is geared towards definition of stratigraphy, subsurface blocks, and structure at the decimeter to meter scale that is critical for establishing the geologic setting of the rover. GPR data can also be used to infer the degree of any post-depositional pedogenic alteration or weathering that has subsequently taken place, thereby enabling assessment of pristine versus secondary morphology at the landing site. As is the case for most remote sensing instruments, a GPR may not detect water unambiguously. Nevertheless, any local, near-surface occurrence of liquid water will lead to large, easily detected dielectric contrasts. Moreover, definition of stratigraphy and setting will help in evaluating the history of aqueous activity and where any water might occur and be accessible. Most importantly perhaps, GPR can provide critical context for other rover and orbital instruments/data sets. Hence, GPR deployment along well positioned transects in the vicinity of a lander should enable 3-D mapping of stratigraphy and could serve to guide direct subsurface sampling. Additional information is contained in the original extended abstract.

Grant, J. A.↗

NASA NTRS2014

Fabrication of Turbine Disk Materials by Additive Manufacturing

Precipitation-strengthened, nickel-based superalloys are widely used in the aerospace and energy industries due to their excellent environmental resistance and outstanding mechanical properties under extreme conditions. Powder-bed additive manufacturing (AM) technologies offer the potential to revolutionize the processing of superalloy turbine components by eliminating the need for extensive inventory or expensive legacy tooling. Like selective laser melting (SLM), electron beam melting (EBM) constructs three-dimensional dense components layer-by-layer by melting and solidification of atomized, pre-alloyed powder feedstock within 50-200 micron layers. While SLM has been more widely used for AM of nickel alloys like 718, EBM offers several distinct advantages, such as less retained residual stress, lower risk of contamination, and faster build rates with multiple-electron-beam configurations. These advantages are particularly attractive for turbine disks, for which excessive residual stress and contamination can shorten disk life during high-temperature operation. In this presentation, we will discuss the feasibility of fabricating disk superalloy components using EBM AM. Originally developed using powder metallurgy forging processing, disk superalloys contain a higher refractory content and precipitate volume fraction than alloy 718, thus making them more prone to thermal cracking during AM. This and other challenges to produce homogeneous builds with desired properties will be presented. In particular, the quality of lab-scale samples fabricated via a design of experiments, in which the beam current, build temperature, and beam velocity were varied, will be summarized. The relationship between processing parameters, microstructure, grain orientation, and mechanical response will be discussed.

oxidation↗