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DOE OSTI2022

Functionalized Mesoporous Carbon and Silica for Effective Recovery of Rare Earth Elements from Magnet Scrap

The dependence on international supplies of rare earth elements (REEs) have prompted the US to explore alternative sources and sustainable technologies for domestic REE production. One potential source is the secondary electronic and industrial wastes at the Department of Defense (DoD) complexes and across the US. These hazardous wastes require high costs for the maintenance and remediation, while their high-REE contents offer unique opportunities for REE recovery. However, current hydrometallurgical technologies for REE extraction are energy intensive and costly, with low REE recovery rate and the generation of toxic wastes. Thus, it is beneficial to develop environmentally friendly technologies for REE extraction and processing from the secondary wastes. This project aims to develop novel functionalized mesoporous carbon fiber (MCF) and silica for effective recovery of REEs from end-of-life NdFeB magnet scrap.

36 MATERIALS SCIENCE↗

DOE OSTI2020

GIS-Based Modeling of Contaminated Soil Volumes at Multiple Sites in the Formerly Utilized Sites Remedial Action Program - 20149

The remediation of hazardous, toxic, and radioactive waste (HTRW) sites produces cost-related risks associated with the estimation of contaminated soil or debris volumes. Historical risk-management techniques include cost contingencies to cover volume uncertainties that affect project budgeting and decision-making. The Buffalo District teamed with project partners to lessen volume uncertainty and reduce project risks at multiple HTRW sites managed under the Formerly Utilized Sites Remedial Action Program (FUSRAP). Historical remedial investigations under FUSRAP commonly identified the presence of radiological material in site media, the associated human health risk, and then areas of remediation. To manage remedial execution and reduce risk, pre-design or remediation-phase sampling essentially 'chased' contamination, which was not conducive to efficient predictive budgeting derived from Feasibility Study (FS) cost analyses. The Buffalo District first optimized their approach to better understand volume uncertainty by utilizing the Argonne National Laboratory's Bayesian Approaches for Adaptive Spatial Sampling (BAASS) software [1]. BAASS processed soft data (e.g., gamma walk-over data) and spatial sampling data to estimate the lateral extent of contaminated soil irrespective of depth (i.e., gross contamination extent) and define areas of contaminant uncertainty. The software performed a binary transformation of contaminant concentrations at all sampling points based upon remedial action goals or a sum of ratios approach (i.e., clean, impacted, or range of impacts in soil). The model produced two-dimensional (horizontal) contaminant probability contours and statistical uncertainty in the sampling coverage and resulting contaminant extents. This method was translated vertically by partitioning the sampling data into depth brackets that produced a stacked representation of contaminant extents and uncertainty in the subsurface (i.e., similar to construction lifts). The results commonly led to a better understanding of project uncertainty and the need for sampling strategies that produce high-confidence soil volumes, which control costs. The BAASS-based delineations were eventually replaced by Empirical Bayesian Kriging (EBK) methods available in ArcGIS Spatial or 3D Analysts [2]. The EBK method calculates contaminant probability zones derived from user-controlled semivariograms of the spatial datasets. The resulting probability zones (e.g., 50% or 80% of contaminant probability) represent the two-dimensional surface delineation of the overall horizontal remedial area, similarly to BAASS. However, unlike BAASS, the vertical sampling data within these probability zones became vertical control points to contour a subterranean surface that connects subsurface points to the land-surface delineations of contamination. The resulting representation of horizontal and vertical impacts within an enclosed envelop (volume) of soil included uncertainty distributions that are used to plan uncertainty-reduction sampling. These data-driven and math-based models of three-dimensional sampling results produced well-bounded remedial volumes for project planning and better uncertainty predictions during project budgeting. The EBK method was applied to several FUSRAP sites managed by the Buffalo District and compared to less rigorously modeled sites previously remediated by the District. The comparison of modeled to actual remediated volumes provide a basis for validating the volume-estimation method. This comparison is important to ensure modeled volumes match physical boundaries of site remediation. FUSRAP sites with denser investigative sampling and lesser volume uncertainty proved useful in remedial planning and contracting. The Buffalo District noted that historical sites with sparser sampling arrays had greater disparity between estimated volumes and final remedial volumes. The benefit achieved over the cost of detailed soil sampling appears positive for FUSRAP projects, especially where impacts vary widely and appear unbounded by investigation-phase sampling. The subsequent Empirical Bayesian Kriging of contamination coupled with vertical contouring for soil estimations reduces uncertainty in soil volumes or indicates where sampling is required to reduce uncertainty, which together optimize remedial planning and budgeting. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2023

Hybrid Iodide Perovskites of Divalent Alkaline Earth and Lanthanide Elements

Hybrid halide perovskites AM II X 3 (A = ammonium cation, M II = divalent cation, X = Cl, Br, I) have been extensively studied but have only previously been reported for the divalent carbon group elements Ge, Sn, and Pb. While they have displayed an impressive range of optoelectronic properties, the instability of Ge II and Sn II and the toxicity of Pb have stimulated significant interest in finding alternatives to these carbon group-based perovskites. Here, we describe the low-temperature solid-state synthesis of five new hybrid iodide perovskites centered around divalent alkaline earth and lanthanide elements, with the general formula AM II I 3 (A = methylammonium, MA; M II = Sr, Sm, Eu, and A = formamidinium, FA; M II = Sr, Eu). Structural, calorimetric, optical, photoluminescence, and magnetic properties of these materials are reported.

36 MATERIALS SCIENCE↗

NASA NTRS1983

Development of aircraft lavatory compartments with improved fire resistance characteristics. Phase 4: Sandwich panel decorative ink development

Five chemically different resin systems with improved fire resistance properties were studied for a possible screenprinting ink application. Fire resistance is hereby defined as the cured ink possessing improvements in flammability, smoke emission, and thermal stability. The developed ink is for application to polyvinyl fluoride film. Only clear inks without pigments were considered. Five formulations were evaluated compared with KC4900 clear acrylic ink, which was used as a baseline. The tests used in the screening evaluation included viscosity, smoke and toxic gas emission, limiting oxygen index (LOI), and polyvinyl fluoride film (PVF) printability. A chlorofluorocarbon resin (FPC461) was selected for optimization studies. The parameters for optimization included screenprinting process performance, quality of coating, and flammability of screenprinted 0.051-mm (0.002-in.) white Tedlar. The quality of the screenprinted coating on Tedlar is dependent on viscosity, curing time, adhesion to polyvinyl fluoride film, drying time (both inscreen and as an applied film), and silk screen mesh material and porosity.

Jayarajan, A.↗

NASA NTRS2015

Proof-of-Concept Experiments on a Gallium-Based Ignitron for Pulsed Power Applications

Ignitrons are electrical switching devices that operate at switching times that are on the order of microseconds, can conduct high currents of thousands of amps, and are capable of holding off tens of thousands of volts between pulses. They consist of a liquid metal pool within an evacuated tube that serves both the cathode and the source of atoms and electrons for an arc discharge. Facing the liquid metal pool is an anode suspended above the cathode, with a smaller ignitor electrode tip located just above the surface of the cathode. The ignitron can be charged to significant voltages, with a potential difference of thousands of volts between anode and cathode. When an ignition pulse is delivered from the ignitor electrode to the cathode, a small amount of the liquid metal is vaporized and subsequently ionized, with the high voltage between the anode and cathode causing the gas to bridge the gap between the two electrodes. The electrons and ions move rapidly towards the anode and cathode, respectively, with the ions liberating still more atoms from the liquid metal cathode surface as a high-current plasma arc discharge is rapidly established. This arc continues in a self-sustaining fashion until the potential difference between the anode and cathode drops below some critical value. Ignitrons have been used in a variety of pulsed power applications, including the railroad industry, industrial chemical processing, and high-power arc welding. In addition, they might prove useful in terrestrial power grid applications, serving as high-current fault switches, quickly shunting dangerous high-current or high-voltage spikes safely to ground. The motivation for this work stemmed from the fact that high-power, high-reliability, pulsed power devices like the ignitron have been used for ground testing in-space pulsed electric thruster technologies, and the continued use of ignitrons could prove advantageous to the future development and testing of such thrusters. Previous ignitron designs have used mercury as the liquid metal cathode, owing to its presence as a liquid at room temperatures and a vapor pressure of 10 Pa (75 mtorr) at room temperature. While these are favorable properties, there are obvious environmental and personal safety concerns with the storage, handling, and use of mercury and its compounds. The purpose of the present work was to fabricate and test an ignitron that used as its cathode an alternate liquid metal that was safe to handle and store. To that end, an ignitron test article that used liquid gallium as the cathode material was developed and tested. Gallium is a metal that has a melting temperature of 29.76 C, which is slightly above room temperature, and a boiling point of over 2,300 C at atmospheric pressure. This property makes gallium the element with the largest relative difference between melting and boiling points. Gallium has a limited role in biology, and when ingested, it will be subsequently processed by the body and expelled rather than accumulating to toxic levels. The next section of this Technical Memorandum (TM) provides background information on the development of mercury-based ignitrons, which serves as the starting point for the development of the gallium-based variant. Afterwards, the experimental hardware and setup used in proof-of-concept testing of a basic gallium ignitron are presented. Experimental data, consisting of discharge voltage and current waveforms as well as high-speed imaging of the gallium arc discharge in the gallium ignitron test article, are presented to demonstrate the efficacy of the concept. Discussion of the data and suggestions on improvements for future iterations of the design are presented in the final two sections of this TM.

Ali, H. K.↗

NASA NTRS2018

Method of Making Dye-Doped Polystyre Microparticles

Various embodiments provide dye-doped polystyrene microspheres generated using dispersion polymerization. Polystyrene microspheres may be doped with fluorescent dyes, such as xanthene derivatives including kiton red 620 (KR620), using dispersion polymerization. Certain functionalities, such as sodium styrene sulfonate, may be used to shift the equilibrium distribution of dye molecules to favor incorporation of the dye into the particles. Polyelectrolyte materials, such as poly(diallyldimethyl ammonium chloride), PolyDADMAC, may be used to electrostatically trap and bind dye molecules within the particles. A buffer may be used to stabilize the pH change of the solution during dye-doped polystyrene microsphere generation and the buffer may be selected depending on the pKa of the dye being incorporated. The various embodiments may provide dye-doped polystyrene microspheres, such as KR620-doped polystyrene microspheres that are non-toxic and non-carcinogenic. These non-toxic and non-carcinogenic dye-doped polystyrene microspheres may be suitable for use in wind tunnel testing.

Wohl, Jr., Christopher J.↗

DOE OSTI2023

On the Durability of Tin‐Containing Perovskite Solar Cells

Abstract Tin (Sn)‐containing perovskite solar cells (PSCs) have gained significant attention in the field of perovskite optoelectronics due to lower toxicity than their lead‐based counterparts and their potential for tandem applications. However, the lack of stability is a major concern that hampers their development. To achieve the long‐term stability of Sn‐containing PSCs, it is crucial to have a clear and comprehensive understanding of the degradation mechanisms of Sn‐containing perovskites and develop mitigation strategies. This review provides a compendious overview of degradation pathways observed in Sn‐containing perovskites, attributing to intrinsic factors related to the materials themselves and environmental factors such as light, heat, moisture, oxygen, and their combined effects. The impact of interface and electrode materials on the stability of Sn‐containing PSCs is also discussed. Additionally, various strategies to mitigate the instability issue of Sn‐containing PSCs are summarized. Lastly, the challenges and prospects for achieving durable Sn‐containing PSCs are presented.

14 SOLAR ENERGY↗

DOE OSTI2022

CRISPR–Cas9-mediated nuclear transport and genomic integration of nanostructured genes in human primary cells

DNA nanostructures are a promising tool to deliver molecular payloads to cells. DNA origami structures, where long single-stranded DNA is folded into a compact nanostructure, present an attractive approach to package genes; however, effective delivery of genetic material into cell nuclei has remained a critical challenge. Here, we describe the use of DNA nanostructures encoding an intact human gene and a fluorescent protein encoding gene as compact templates for gene integration by CRISPR-mediated homology-directed repair (HDR). Our design includes CRISPR–Cas9 ribonucleoprotein binding sites on DNA nanostructures to increase shuttling into the nucleus. We demonstrate efficient shuttling and genomic integration of DNA nanostructures using transfection and electroporation. These nanostructured templates display lower toxicity and higher insertion efficiency compared to unstructured double-stranded DNA templates in human primary cells. Furthermore, our study validates virus-like particles as an efficient method of DNA nanostructure delivery, opening the possibility of delivering nanostructures in vivo to specific cell types. Together, these results provide new approaches to gene delivery with DNA nanostructures and establish their use as HDR templates, exploiting both their design features and their ability to encode genetic information. This work also opens a door to translate other DNA nanodevice functions, such as biosensing, into cell nuclei.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2022

Templated synthesis enhances the cobalt adsorption capacity of a porous organic polymer

Divalent transition metals such as Co(II) are important targets for removal from water sources, due to their potential toxicity as well as their high value. In this study, we found that a series of porous organic polymers based on amide-linked tetraphenylmethane units are effective Co(II) ion adsorbents in aqueous solution. To increase the density of Co(II) binding sites, we then developed a templated synthesis in which the branched, rigid monomers are pre-assembled around Co(II) ions prior to polymerization. Furthermore, after polymer formation, the Co(II) template ions are removed to yield a material rich in Co(II) binding sites. Ion adsorption isotherms show that the Co(II)-templated material has an ion adsorption capacity significantly greater than those of the non-templated materials, highlighting the utility of a templated synthetic route. SEM and TEM images show the morphology of the templated polymer to be dramatically different from the non-templated polymers and to be similar in size and shape to the Co(II)–monomer precursors, emphasizing the role of the template ions in directing the formation of the resulting polymer. This guest-templated approach requires no functionalization of the generic monomer and represents a promising synthetic route to high-capacity ion adsorbents for water purification and aqueous separations.

36 MATERIALS SCIENCE↗

DOE OSTI2020

DOE Investments in Environmentally Acceptable Lubricants for Hydropower Applications Fact Sheet

Environmentally acceptable lubricants (EALs) are defined as lubricants that meet U.S. Environmental Protection Agency (EPA) standards for “biodegradability, toxicity, and bioaccumulation potential that minimize their likely adverse consequences in the aquatic environment, compared to conventional lubricants.” Restrictions from state, local, and federal agencies, as well as a growing awareness of the environmental risks associated with petroleumbased lubricants, have shifted government and industry to seek out high-performing EALs. The U.S. Department of Energy (DOE) is working to reduce the environmental impacts of hydropower development and operation by investing in tools and methods to develop, demonstrate, and validate EAL materials.

water, environment, hydropower, EALs↗

NASA NTRS1982

Surface flow visualization using indicators

Surface flow visualization using indicators in the cryogenic wind tunnel which requires a fresh look at materials and procedures to accommodate the new test conditions is described. Potential liquid and gaseous indicators are identified. The particular materials illustrate the various requirements an indicator must fulfill. The indicator must respond properly to the flow phenomenon of interest and must be observable. Boundary layer transition is the most important phenomenon for which flow visualization indicators may be employed. The visibility of a particular indicator depends on utilizing various optical or chemical reactions. Gaseous indicators are more difficult to utilize, but because of their diversity may present unusual and useful opportunities. Factors to be considered in selecting an indicator include handling safety, toxicity, potential for contamination of the tunnel, and cost.

Crowder, J. P.↗

NASA NTRS2010

DF-1, A Nontoxic Carbon Fullerene Based Antioxidant, is Effective as a Biomedical Countermeasure Against Radiation

A long-term goal of radiation research is the mitigation of inherent risks of radiation exposure. Thus the study and development of safe agents, whether biomedical or dietary, that act as effective radioprotectors is an important step in accomplishing this long-term goal. Some of the most effective agents to date have been aminothiols and their derivatives. Unfortunately, most of these agents have side effects such as nausea, vomiting, hypotension, weakness, and fatigability. For example, nausea and emesis occur in most patients treated with WR-2721 (Amifostine), requiring the use of effective antiemetics, with hypotension being the dose-limiting side effect in patients treated. Clearly, the need for a radioprotector that is both effective and safe still exists. Development of biocompatible nano-materials for radioprotection is a promising emerging technology that could be exploited to address the need to minimize biological effects when exposure is unavoidable. Testing free radical scavenging nanoparticles for potential use in radioprotection is exciting and highly relevant. Initial investigations presented here demonstrate the ability of a particular functionalized carbon fullerene nanoparticle, (DF-1), to act as an effective radioprotector. DF-1 was first identified as the most promising candidate in a screen of several functionalized carbon fullerenes based on lack of toxicity and antioxidant therapeutic potential against oxidative injuries (i.e. organ reperfusion and ionizing radiation). Subsequently, DF-1 has been shown to reduce chromosome aberration yield and cell death, as well as overall ROS levels in human lymphocytes and fibroblasts after exposure to gamma radiation and energetic protons while demonstrating no associated toxicity. The dose-reducing factor of DF-1 at LD50 is nearly 2.0 for gamma radiation. In addition, DF-1 treatment also significantly prevented cell cycle arrest after exposure. Finally, DF-1 markedly attenuated COX2 upregulation in cell culture after irradiation thus preventing an inflammatory response to irradiation. Taken together, these results suggest that DF-1 provides potent protection against several deleterious cellular consequences of irradiation in mammalian systems including oxidative stress, DNA damage, inflammation and cell death.

Theriot, Corey A.↗

NASA NTRS1994

Dual Use Space Technology Transfer Conference Paper

New textile fibers have been developed or modified to meet the complex and constraining criteria of space applications. The most common of these criteria are light weight, nonflammability or flame retardancy, and high strength and durability in both deep space environment and the oxygen enriched crew bay area of the spacecraft. The fibers which successfully pass the tests of flammability and toxicity, and display the desired mechanical properties are selected for space applications. Such advanced fibers developed for the Crew and Thermal Systems Division (CTSD) at the Johnson Space Center include 'Beta' fiber, heat stabilized polybenzimidazole and polyimide, as well as modified aramid Durette(TM), multi-fibrous Ortho(TM) fabric, and flame resistant cotton. The physical, mechanical, and chemical properties of these fibers are briefly discussed. The testing capabilities in the CTSD laboratory to ascertain some of the properties of these and other fibrous materials are also discussed. Most of these materials developed for spacecraft, space suit, and flight equipment applications have found other commercial applications. These advanced textile fibers are used mostly for aircraft, transportation, public buildings, hospitals, and protective clothing applications.

Orndoff, Evelyne↗

DOE OSTI2026

Will Nontoxic High‐Performance Perovskite Photovoltaics Ever Be Possible?

Lead-based halide perovskite solar cells represent a significant advancement in photovoltaic technology, achieving certified power conversion efficiencies of over 27%. However, the toxicity of lead poses a major barrier to widespread commercialization. The demand for environmentally safe alternatives has driven extensive research into Pb-free perovskites. Current efforts include replacing Pb with Sn or Ge; forming double perovskites in which Pb is substituted by a monovalent–trivalent cation pair; and developing chalcogenide perovskites where the B site (ABX 3 ) adopts tetravalent cations (rather than Pb) to balance the charge. This concept examines the recent progress in developing Pb-free alternatives, revealing fundamental performance bottlenecks, inherent material limitations, and persistent development challenges. Through a comparative assessment of material properties and device performance limitations, this work highlights the underlying dilemma between environmental safety and efficiency in perovskite photovoltaics. The analysis identifies fundamental material constraints that create substantial barriers to simultaneously achieving both objectives.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Carbon Dioxide Conversion to Nanomaterials: Methods, Applications, and Challenges

Anthropogenic carbon dioxide (CO 2 ) emission is one of the biggest global threats that we are confronted with in the 21st century. A lack of prompt action to mitigate the atmospheric CO 2 level could lead to global catastrophic events. As a result of the significance of the aforementioned threat, multiple nations have agreed to enact carbon capture, storage, utilization, and sequestration (CCUS) technologies at academic and industrial scales with the aim of lowering the atmospheric CO 2 level. Although there are many reviews on CCUS technologies, there is a lack of comprehensive review on CO 2 conversion to more economically valuable products, such as nanomaterials. Carbon dioxide capture and conversion into nanomaterials is an interesting research topic in many ways because it contributes to our fundamental knowledge of material conversion, provides alternative ways to reduce atmospheric pollution, and yields lucrative products, which has not been explored broadly. Aside from the positive outcomes, we have a moral obligation to rectify a global threat caused by anthropogenic emission. Herein, we present current methods of converting CO 2 into organic and inorganic nanomaterials with a focus on operating conditions and challenges as well as the potential of nanomaterials in specifically biomedical applications as opposed to extensively reviewed energy-related uses. Furthermore, our review emphasizes the toxicity issues related to using such nanomaterials in biological settings based on literature and other comparable studies.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1984

Protective Coating

Inorganic Coatings, Inc.'s K-Zinc 531 protective coating is water-based non-toxic, non-flammable and has no organic emissions. High ratio silicate formula bonds to steel, and in 30 minutes, creates a very hard ceramic finish with superior adhesion and abrasion resistance. Improved technology allows application over a minimal commercial sandblast, fast drying in high humidity conditions and compatibility with both solvent and water-based topcoats. Coating is easy to apply and provides long term protection with a single application. Zinc rich coating with water-based potassium silicate binder offers cost advantages in materials, labor hours per application, and fewer applications over a given time span.

Source record↗

DOE OSTI2021

On-device lead absorbing tapes for sustainable perovskite solar cells

Perovskite solar cells are a promising technology that could facilitate and accelerate the energy transition to a sustainable future. However, the toxicity of Pb remains one of the obstacles impeding their commercialization. Here we apply on-device tapes to absorb leaked lead from damaged devices. Furthermore, our chemical approach can capture over 99.9% of leakage without compromising the performance and operation.

14 SOLAR ENERGY↗

NASA NTRS1977

The use of a behavioral response system in the USF/NASA toxicity screening test method

Relative toxicity data on the pyrolysis effluents from bisphenol A polycarbonate and wool fabric were obtained, based on visual observations of the behavior of free-moving mice and on an avoidance response behavioral paradigm of restrained rats monitored by an instrumented behavioral system. The initial experiments show an essentially 1:1 correlation between the two systems with regard to first signs of incapacitation, collapse, and death from pyrolysis effluents from polycarbonate. It is hypothesized that similarly good correlations between these two systems might exist for other materials exhibiting predominantly carbon monoxide mechanisms of intoxication. This hypothesis needs to be confirmed, however, by additional experiments. Data with wool fabric exhibited greater variability with both procedures, indicating possibly different mechanisms of intoxication for wool as compared with bisphenol A polycarbonate.

Hilado, C. J.↗