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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Synthesis and Functionalization of Coal Fly Ash-Derived Zeolites for Boron Removal From Wastewater

There are hundreds of both active and unused surface impoundments in the United States containing coal combustion residuals (CCRs) produced by coal-fired power plants which can leach toxic elements into surface and groundwater. Therefore, the development of efficient means for both the clean-up of surface impoundments and for deriving economically viable products from CCRs are urgent tasks for researchers. Herein, a microwave-assisted strategy is presented for converting a common coal combustion residual, coal fly ash (CFA), into zeolite-based sorbents for boron (B) removal from wastewater. Specifically, CFA constitutes the main source of Si and Al ions to produce zeolite type-A and the resulting sorbent subsequently undergoes simple cation exchange with Ca to enhance its B adsorption capacity. Structure and composition of the sorbents were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), inductively coupled plasma (ICP)-mass spectrometry (MS), and ICP-optical emission spectroscopy (OES). The Ca-modified zeolite sorbent derived from CFA exhibits comparable B removal capacity with similar commercial zeolites.

Muldoon, Patrick↗
DOE OSTI2020

Application of electrodialysis pretreatment to enhance boron removal and reduce fouling during desalination by nanofiltration/reverse osmosis

we report membranes have emerged as promising technologies for treatment of non-traditional waters, but fouling and poor rejection of small, neutral solutes (e.g., boric acid) impede their further implementation for water purification. Boron rejection is increased by raising the pH to convert boric acid to borate ion, but this change often leads to calcite supersaturation. This study investigated the use of a hybrid electrodialysis-nanofiltration/reverse osmosis (ED-NF/RO) system to reduce fouling from calcite precipitation and calcium-polysaccharide sorption to NF/RO membranes. Also, the study examined the potential of the hybrid process to increase permeate flux and boron rejection during NF/RO of synthetic saline water. ED pretreatment reduced calcite oversaturation and reduced flux decline during NF/RO. Low alginate concentrations (25 mg/L) limited NF/RO fouling, but high concentrations (100 mg/L) appeared to promote calcite scaling. ED pretreatment reduced the osmotic pressure of the NF/RO feed water, enabling lower operating pressures or greater permeate water fluxes. Boron rejection during NF/RO increased with ED pretreatment, probably due to stronger electrostatic repulsion and an increase in the fraction of total boron present as B(OH)4- following ED. This hybrid ED-NF/RO system shows promise as a novel approach to enhancing the performance of current membrane systems for treating complex feed waters.

alginate↗
DOE OSTI2024

Synthesis and characterization of zeolite sorbents from coal fly ash by a microwave-assisted hydrothermal method for removal of boron leachate from coal impoundments

This study developed promoted zeolite-based sorbents derived from coal fly ash to remove leachates (like boron) from ash impoundment or landfill to protect the environment and reuse legacy coal ash. The sorbents were synthesized using machine learning model results as guide to accelerate the sorbent development.

Wang, Ping↗
DOE OSTI2021

Boric acid removal with polyol-functionalized polyether membranes

Poor selectivity of conventional desalination membranes for boron often necessitates multi-stage treatment trains to achieve desired boron removal for end uses such as irrigation. One approach to membrane design for improved single-pass boric acid removal is via incorporation of chelating ligands that selectively sorb boron. In this study, membranes based on epoxy-amine cross-linked poly(glycidyl glycidyl ether) (PGGE) were synthesized and functionalized with N-methyl-d-glucamine (NMDG), a polyol known to interact selectively with boron. PGGE and PGGE-NMDG membranes exhibited boron sorption isotherms that were well-described by dual mode isotherms. PGGE-NMDG sorbed 2.5 mmol B/g dry polymer from a neutral aqueous solution containing 100 mmol B/L, which was almost three times the adsorption density of a commercial boron selective resin, Amberlite IRA743. Further, the membranes were regenerated in acid without a significant loss of boron sorption capacity over four cycles. Interactions between boron and NMDG and PGGE sites (e.g., epoxides) impacted boron diffusion in both membranes. The use of ligand functionalized membranes to capture target solutes such as boron requires high loading of interacting sites to maximize uptake capacity. Establishing fundamental structure/property rules for boron selectivity could lead to new material designs with improved boron separation properties for water purification.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Computational screening of fly ash zeolite sorbents for boric acid removal

In the United States, many impoundments at coal-fired power plants contain elevated contaminants like arsenic, boron, barium, and selenium. Zeolites synthesized from fly ash show promise as sorbents for these contaminants. However, optimizing sorption capacity is challenging due to numerous possible topologies, silicon to aluminum (Si/Al) ratios, and cation types. In this study, molecular simulations are used to design cationic zeolites for boric acid adsorption. Force field models based on quantum mechanical calculations (PBE + D2) for Na-, Ca-, Mn-, and Fe-exchanged chabazite and LTA are presented. The new D2FF force fields reproduce DFT energies with about half the error of UFF. Zeolite performance depends on Si/Al ratio and cation type, with low Si/Al ratio chabazite (CHA) and phillipsite (PHI) zeolite frameworks exchanged with Ca 2+ or Na + /Ca 2+ mixtures showing the highest adsorption. In conclusion, these findings suggest tailored fly ash-derived zeolites could provide effective boron removal from leachate ponds.

CCR impoundment↗
DOE OSTI2021

Sustainable Functional Epoxies through Boric Acid Templating

Thermoset polymers (e.g. epoxies, vulcanizable rubbers, polyurethanes, etc.) are crosslinked materials with excellent thermal, chemical, and mechanical stability; these properties make thermoset materials attractive for use in harsh applications and environments. Unfortunately, material robustness means that these materials persist in the environment with very slow degradation over long periods of time. Balancing the benefits of material performance with sustainability is a challenge in need of novel solutions. Here, we aimed to address this challenge by incorporating boronic acid-amine complexes into epoxy thermoset chemistries, facilitating degradation of the material under pH neutral to alkaline conditions; in this scenario, water acts as an initiator to remove boron species, creating a porous structure with an enhanced surface area that makes the material more amenable to environmental degradation. Furthermore, the expulsion of the boron leaves the residual pores rich in amines which can be exploited for CO 2 absorption or other functionalization. We demonstrated the formation of novel boron species from neat mixing of amine compounds with boric acid, including one complex that appears highly stable under nitrogen atmosphere up to 600 °C. While degradation of the materials under static, alkaline conditions (our “trigger”) was inconclusive at the time of this writing, dynamic conditions appeared more promising. Additionally, we showed that increasing boronic acid content created materials more resistant to thermal degradation, thus improving performance under typical high temperature use conditions.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Tracking Active Phase Behavior on Boron Nitride during the Oxidative Dehydrogenation of Propane Using Operando X-ray Raman Spectroscopy

Hexagonal boron nitride (hBN) is a highly selective catalyst for the oxidative dehydrogenation of propane (ODHP) to propylene. Using a variety of ex situ characterization techniques, the activity of the catalyst has been attributed to the formation of an amorphous boron oxyhydroxide surface layer. The ODHP reaction mechanism proceeds via a combination of surface mediated and gas phase propagated radical reactions with the relative importance of both depending on the surface-to-void-volume ratio. Here we demonstrate the unique capability of operando X-ray Raman spectroscopy (XRS) to investigate the oxyfunctionalization of the catalyst under reaction conditions (1 mm outer diameter reactor, 500 to 550 °C, P = 30 kPa C 3 H 8 , 15 kPa O 2 , 56 kPa He). We probe the effect of a water cofeed on the surface of the activated catalyst and find that water removes boron oxyhydroxide from the surface, resulting in a lower reaction rate when the surface reaction dominates and an enhanced reaction rate when the gas phase contribution dominates. Computational description of the surface transformations at an atomic-level combined with high precision XRS spectra simulations with the OCEAN code rationalize the experimental observations. Finally, this work establishes XRS as a powerful technique for the investigation of light element-containing catalysts under working conditions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2004

High-Performance SiC/SiC Ceramic Composite Systems Developed for 1315 C (2400 F) Engine Components

As structural materials for hot-section components in advanced aerospace and land-based gas turbine engines, silicon carbide (SiC) ceramic matrix composites reinforced by high performance SiC fibers offer a variety of performance advantages over current bill-of-materials, such as nickel-based superalloys. These advantages are based on the SiC/SiC composites displaying higher temperature capability for a given structural load, lower density (approximately 30- to 50-percent metal density), and lower thermal expansion. These properties should, in turn, result in many important engine benefits, such as reduced component cooling air requirements, simpler component design, reduced support structure weight, improved fuel efficiency, reduced emissions, higher blade frequencies, reduced blade clearances, and higher thrust. Under the NASA Ultra-Efficient Engine Technology (UEET) Project, much progress has been made at the NASA Glenn Research Center in identifying and optimizing two highperformance SiC/SiC composite systems. The table compares typical properties of oxide/oxide panels and SiC/SiC panels formed by the random stacking of balanced 0 degrees/90 degrees fabric pieces reinforced by the indicated fiber types. The Glenn SiC/SiC systems A and B (shaded area of the table) were reinforced by the Sylramic-iBN SiC fiber, which was produced at Glenn by thermal treatment of the commercial Sylramic SiC fiber (Dow Corning, Midland, MI; ref. 2). The treatment process (1) removes boron from the Sylramic fiber, thereby improving fiber creep, rupture, and oxidation resistance and (2) allows the boron to react with nitrogen to form a thin in situ grown BN coating on the fiber surface, thereby providing an oxidation-resistant buffer layer between contacting fibers in the fabric and the final composite. The fabric stacks for all SiC/SiC panels were provided to GE Power Systems Composites for chemical vapor infiltration of Glenn designed BN fiber coatings and conventional SiC matrices. Composite panels with system B were heat treated at Glenn, and the pores that remained open were filled by silicon melt infiltration (MI). Panels with system A and the other SiC/SiC systems were not heat treated, and remaining open pores in these systems were filled with SiC slurry and silicon MI.

DiCarlo, James A.↗
DOE OSTI2026

Removal of deuterium retained in boron powder by oxygen or high-temperature bakeout

Fuel retention in dust accumulated in fusion devices is a potential operational hazard. Boronization is one of the leading wall-conditioning candidates for future fusion devices. Fuel retention characteristics of boron dust must be studied to accurately understand the potential hazards of boron dust in fusion devices. We evaluated the retention of deuterium (D) in commercially available boron powder as a proxy for tritium retention in boron dust. Diffuse reflectance infrared Fourier transform spectroscopy revealed that boron powder between 300 and 500 K exposed to neutral hydrogen (H 2 ) gas retains H via B-H bonding. We utilized D 2 exposures of 17,400 L on the boron powder, which led to retention on the order of 0.5 g D per 100 kg B or 1.2 g D per m 2 B, as estimated from temperature programmed desorption measurements. We evaluated how powder bakeouts under ultra-high vacuum (UHV), or in an oxygen (O 2 ) or H 2 gas backfilled environment can remove the retained fuel. Bakeouts below 523 K under UHV exhibited poor D removal, promoting recapture of D 2 present as background gas in the chamber. Higher temperature bakeouts led to the removal of over 80% of the retained D within 3 days (623 K) or 1 h (723 K). Bakeouts at 423 K under an O 2 gas environment removed ∼150% more retained D from the boron powder, when compared to bakeouts conducted under UHV. These results suggest that efficient fuel removal from boron dust can be achieved by high-temperature bakeout (>623 K) or by bakeouts at lower temperature (423 K) under an O 2 environment.

Bakeout↗
NASA NTRS2002

New High-Performance SiC Fiber Developed for Ceramic Composites

Sylramic-iBN fiber is a new type of small-diameter (10-mm) SiC fiber that was developed at the NASA Glenn Research Center and was recently given an R&D 100 Award for 2001. It is produced by subjecting commercially available Sylramic (Dow Corning, Midland, MI) SiC fibers, fabrics, or preforms to a specially designed high-temperature treatment in a controlled nitrogen environment for a specific time. It can be used in a variety of applications, but it currently has the greatest advantage as a reinforcement for SiC/SiC ceramic composites that are targeted for long-term structural applications at temperatures higher than the capability of metallic superalloys. The commercial Sylramic SiC fiber, which is the precursor for the Sylramic-iBN fiber, is produced by Dow Corning, Midland, Michigan. It is derived from polymers at low temperatures and then pyrolyzed and sintered at high temperatures using boron-containing sintering aids (ref. 1). The sintering process results in very strong fibers (>3 GPa) that are dense, oxygen-free, and nearly stoichiometric. They also display an optimum grain size that is beneficial for high tensile strength, good creep resistance, and good thermal conductivity (ref. 2). The NASA-developed treatment allows the excess boron in the bulk to diffuse to the fiber surface where it reacts with nitrogen to form an in situ boron nitride (BN) coating on the fiber surface (thus the product name of Sylramic-iBN fiber). The removal of boron from the fiber bulk allows the retention of high tensile strength while significantly improving creep resistance and electrical conductivity, and probably thermal conductivity since the grains are slightly larger and the grain boundaries cleaner (ref. 2). Also, as shown in the graph, these improvements allow the fiber to display the best rupture strength at high temperatures in air for any available SiC fiber. In addition, for CMC applications under oxidizing conditions, the formation of an in situ BN surface layer creates a more environmentally durable fiber surface not only because a more oxidation-resistant BN is formed, but also because this layer provides a physical barrier between contacting fibers with oxidation-prone SiC surface layers (refs. 3 and 4). This year, Glenn demonstrated that the in situ BN treatment can be applied simply to Sylramic fibers located within continuous multifiber tows, within woven fabric pieces, or even assembled into complex product shapes (preforms). SiC/SiC ceramic composite panels have been fabricated from Sylramic-iBN fabric and then tested at Glenn within the Ultra-Efficient Engine Technology Program. The test conditions were selected to simulate those experienced by hot-section components in advanced gas turbine engines. The results from testing at Glenn demonstrate all the benefits expected for the Sylramic-iBN fibers. That is, the composites displayed the best thermostructural performance in comparison to composites reinforced by Sylramic fibers and by all other currently available high-performance SiC fiber types (refs. 3 and 5). For these reasons, the Ultra-Efficient Engine Technology Program has selected the Sylramic-iBN fiber for ongoing efforts aimed at SiC/SiC engine component development.

DiCarlo, James A.↗
DOE OSTI2022

Interfacial interactions between polymers and selective adsorbents influence ion transport properties of boron scavenging ion-exchange membranes

The recent emergence of adsorptive ion-exchange membranes (IEMs), designed by the synergistic integration of highly selective porous aromatic frameworks (PAFs) with ion-exchange polymers, has enabled simultaneous desalination and targeted removal of specific solutes (e.g., mercury, iron, boron, etc.). While the addition of highly selective PAFs to IEMs yields membranes with entirely new functions, PAF-polymer interactions, and the effects of such interactions on ion transport properties of the membranes, are not well understood. In this study, we developed cross-linked adsorptive cation- and anion-exchange membranes (CEMs and AEMs) for simultaneous desalination and boron removal via in-situ formation of the cross-linked polymer network around the boron selective PAF particles. Here we systematically investigated the influence of PAF loading level on PAF-polymer interactions as well as the equilibrium and transport properties of the adsorptive IEMs. The interactions between the PAF and the ion-exchange polymer matrix differed for the CEMs and AEMs due to differences in the fixed charge group chemistry. Notably, the sulfonate groups of the CEMs can form hydrogen bonds with the hydroxyl groups of the PAF, while the quaternary ammonium groups in the AEMs cannot. These differences in interfacial interactions did not significantly impact counter-ion transport across the adsorptive IEMs but had a significant influence on co-ion transport, which affected the counter-ion/co-ion selectivity of the membranes. The selectivity of the adsorptive CEMs decreased while that of the adsorptive AEMs increased with PAF loading level. The results of this study underscore the importance of controlling interfacial interactions when designing adsorptive IEMs for simultaneous water desalination and solute capture and recovery.

36 MATERIALS SCIENCE↗
DOE OSTI2020

The Brachiopod δ 11 B Record Across the Carboniferous-Permian Climate Transition

In this work, we present the δ 11 B of well-preserved brachiopod fossils coupled with geochemical modeling to examine how seawater boron responded to abrupt and dynamic climate changes in the Late Paleozoic. The Late Carboniferous, a time of major coal formation and glacioeustatic sea level changes, is characterized by relatively stable brachiopod δ11B of 15–17‰, similar to values seen in modern brachiopods. Brachiopod δ 11 B dropped by ~5‰ in the early Permian and then restabilized at a new value of 10‰ within a few million years. Mass balance models of seawater δ 11 B reproduced the overall trends in our brachiopod data but failed to capture the large drop in δ11B in the early Permian. Published seawater 87 Sr/ 86 Sr and δ 44 / 40 Ca data based on brachiopod shells also shift to lower values in the early Permian, suggesting a common control on all three seawater isotope systems. The Permian terrestrial record of evaporites and eolian deposits suggests a prolonged reduced delivery of dissolved weathering products to the ocean, accounting for the change in seawater 87 Sr/ 86 Sr. This reduced weathering, in turn, led to increased atmospheric CO 2 and lowered seawater pH, which may have significantly decreased major removal mechanisms for seawater calcium and boron leading to declines in both isotope systems. We propose that boron removal via coprecipitation in carbonates and adsorption onto clay minerals was significantly diminished due to a reduction in the availability of the borate aqueous species caused by lowered seawater pH.

54 ENVIRONMENTAL SCIENCES↗
NASA NTRS1976

Changes in boron fiber strength due to surface removal by chemical etching

The effects of chemical etching on the tensile strength of commercial boron/tungsten fibers were investigated. Fibers with as-received diameters of 203, 143, and 100 micrometers were etched to diameters as small as 43 micrometers. The etching generally resulted in increasing fiber tensile strength with decreasing fiber diameter. And for the 203 micrometer fibers there was an accompanying significant decrease in the coefficient of variation of the tensile strength for diameters down to 89 micrometers. Heat treating these fibers above 1,173 K in a vacuum caused a marked decrease in the average tensile strength of at least 80 percent. But after the fibers were etched, their strengths exceeded the as-received strengths. The tensile strength behavior is explained in terms of etching effects on surface flaws and the residual stress pattern of the as-received fibers.

Smith, R. J.↗
NASA NTRS1977

Thermal degradation of the tensile strength of unidirectional boron/aluminum composites

The variation of ultimate tensile strength with thermal treatment of B-Al composite materials and of boron fibers chemically removed from these composites in an attempt to determine the mechanism of the resulting strength degradation was studied. Findings indicate that thermally cycling B-Al represents a more severe condition than equivalent time at temperature. Degradation of composite tensile strength from about 1.3 GN/m squared to as low as 0.34 GN/m squared was observed after 3,000 cycles to 420 C for 203 micrometers B-1100 Al composite. In general, the 1100 Al matrix composites degraded somewhat more than the 6061 matrix material studied. Measurement of fiber strengths confirmed a composite strength loss due to the degradation of fiber strength. Microscopy indicated a highly flawed fiber surface.

Grimes, H. H.↗
NASA NTRS1977

Thermal degradation of the tensile strength of unidirectional boron/aluminum composites

The variation of ultimate tensile strength with thermal treatment of B-Al composite materials and of boron fibers chemically removed from these composites is studied systematically in an attempt to determine the mechanism of the resulting strength degradation. The results indicate that thermally cycling of B-Al represents a more severe condition than equivalent time at temperature. Degradation of composite tensile strength from about 1.3 GN/sq m to as low as 0.34 GN/sq m was observed after 3000 cycles to 420 C for 203-micron B-1100 Al composite. In general, the 1100 Al-matrix composites degraded somewhat more than the 6061 matrix material studied. Measurement of fiber strengths confirmed a composite strength loss due to the degradation of fiber strength. Microscopy indicated a highly flawed fiber surface. On the basis of various thermal-cycling studies and electron diffraction analysis, a mechanism is favored in which B reacts with Al, freshly exposed by cold working during cycling, to form AlB2. The nonuniform interface reaction leads to a highly flawed and weakened B fiber.

Grimes, H. H.↗
NASA NTRS1982

Low-Waste Purification of Silicon

Ultra-high-purity silicon required for solar cells, transistors and integrated circuits can be produced from metallurgical grade silicon by formation and pyrolysis of silane gas in continuous-flow process that maximizes product purity with minimum amount of equipment. Integrated process recycles unreacted and byproduct materials, minimizing material losses and simplifying waste disposal. Ensures effective removal of impurities, including boron.

Breneman, W. C.↗
DOE OSTI2025

Selective semihydrogenation of acetylene in ethylene using defect-rich boron nitride catalyst from flux reconstruction

Efficient removal of trace acetylene from ethylene streams is essential for producing polymer-grade ethylene, yet achieving highly selective semihydrogenation without over-hydrogenation remains a long-standing challenge. A key barrier is the lack of a simple, low-cost catalyst that can activate hydrogen effectively while preventing ethylene from reacting further. Here we show that defect-rich boron nitride, prepared through a straightforward flux reconstruction method, serves as a highly selective and metal-free catalyst for acetylene semihydrogenation. The catalyst contains abundant open boron and nitrogen sites that enable efficient hydrogen activation and rapid release of ethylene, thereby avoiding over-hydrogenation. Experiments combined with isotope labeling and theoretical analysis reveal that these defects lower the energy barrier for hydrogen activation while accelerating product desorption. Our findings demonstrate a scalable strategy for defect engineering in boron nitride and highlight its potential as a robust, sustainable alternative to metal-based catalysts in industrial ethylene purification.

Wang, Tao [Oak Ridge National Laboratory (ORNL), O↗