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At least 1,693 records · Page 94

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DOE OSTI2020

Microbially mediated iron redox cycling of subsurface sediments from Hanford Site, Washington State, USA

Iron-bearing clay minerals are predominant in soils and sediments, and they undergo oxidation-reduction cycles as a result of natural processes such as wetting/drying cycles and plant root respiration. However, the kinetics and mechanisms of multiple redox cycles of iron in clay-rich sediments and consequences of such cycling on sediment properties are poorly understood. The objective of this study was to understand how multiple redox cycles of Fe in clay-rich sediment affect the rate and extent of Fe bioreduction and the physicochemical properties of the sediment. A natural sediment sample containing Fe-bearing montmorillonite from Hanford, Washington, USA was size-fractionated [2.0 to 0.5 μm (Hanford-C) and 0.5 to 0.02 μm (Hanford-F)] and redox-cycled for four times. Bioreduction was achieved utilizing Geobacter sulfurreducens and re-oxidization was performed with sparged air. Time-course change of total Fe (II) was monitored to measure the rate and extent of Fe (III) bioreduction. Redox-cycled sediments were characterized to determine the physicochemical changes. Both the initial rate and extent of bioreduction fluctuated across the four redox cycles, but they ultimately decreased from 5.3 μmol g -1 h -1 and 22.9% to nearly zero by the fourth cycle. These fluctuation patterns were likely due to a combined effect of reductive dissolution of small/poorly crystalline clay particles (by 3–5%) and clay mineral structural changes, as evidenced by redox induced changes of aqueous chemistry, surface area, cation exchange capacity, mineralogy, and Mössbauer parameters. Once these small/poorly crystalline clay particles were dissolved, structural Fe in residual larger and more crystalline clay particles was largely reversible across additional redox cycles, as revealed by Mössbauer spectroscopy through the first three cycles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1992

An acetate precursor process for BSCCO (2223) thin films and coprecipitated powders

Since the discovery of high temperature superconducting oxides much attention has been paid to finding better and useful ways to take advantage of the special properties exhibited by these materials. One such process is the development of thin films for engineering applications. Another such process is the coprecipitation route to producing superconducting powders. An acetate precursor process for use in thin film fabrication and a chemical coprecipitation route to Bismuth based superconducting materials has been developed. Data obtained from the thin film process were inconclusive to date and require more study. The chemical coprecipitation method of producing bulk material is a viable method, and is preferred over the previously used solid state route. This method of powder production appears to be an excellent route to producing thin section tape cast material and screen printed devices, as it requires less calcines than the oxide route to produce quality powders.

Haertling, Gene H.↗

DOE OSTI2022

High Performance SOFCs with a Superior Stability for Reliable and Durable Power Systems

Next generation of fuel cells, electrolyzers, and batteries requires higher power, faster kinetics, and larger energy density, which necessitate the use of compositionally complex oxides to achieve multifunctionalities and activity. These compositionally complex oxides may change their phases and structures during an electrochemical process – a so-called “electrochemically driven phase transformation”. The origin for such a phase change has remained obscure. More importantly, there is a need to develop high performance solid oxide fuel cells with an enhanced stability. In this work, the La 0.6 Sr 0.4 Co 0.2 Fe 0.8 O 3 (LSCF) cathode surface is modified by infiltration of Pr 6 O 11 and the power density at 0.8V and 750 °C is improved by 21%. In addition, by replacing the traditional barrier layer Gd 0.2 Ce 0.8 O 1.9 with mixed conducting Pr 0.1 Gd 0.1 Ce 0.8 O 1.9 , the power density increases by 38%. The different mechanism of promotions was investigated by electrochemical impedance spectroscopy. The ohmic resistance is dramatically reduced by applying the PGCO interlayer, and the distribution of relaxation time was used to analyze the mechanism for which the polarization resistance was decreased attributing to the mixed conduction nature in PrO x . An increase of power density at 0.8 V of 0.358 W/cm 2 (71%) is achieved with the implementation of both surface modification and buffer layer engineering. An experimental study and a theoretical analysis were then carried out on phase evolution in praseodymium nickelates. Nickelate-based electrodes show up to 60× greater phase transformation during operation when compared to thermally annealed ones. Theoretical analysis suggests that the presence of a reduced oxygen partial pressure at the interface between the oxygen electrode and the electrolyte is the origin for the phase change in an oxygen electrode. Guided by the theory, an addition of the electronic conduction in the interface layer leads to the significant suppression of phase change, while improving cell performance and performance stability. When an oxygen electrode is under polarization, the oxygen partial pressure at the interface between the oxygen electrode and the electrolyte is lower than that of incoming oxidant. Under a high polarization, the environment at the aforementioned interface may lead to phase transformation of the oxygen electrode. The local oxygen partial pressure is determined by the transport properties at the interfaces. An addition of the electronic conduction in the interface layer, for instance using (Pr,Gd)-doped ceria to replace Gd-doped ceria, results in improved cell performance and performance stability, while the phase transformation is significantly suppressed. This work provides a fundamental understanding of the origin for phase transformation in oxygen electrodes during operation and use this knowledge to develop a high-performance electrode that exhibits improved performance stability.

30 DIRECT ENERGY CONVERSION↗

NASA NTRS1990

Catalytic Destruction Of Toxic Organic Compounds

Proposed process disposes of toxic organic compounds in contaminated soil or carbon beds safely and efficiently. Oxidizes toxic materials without producing such other contaminants as nitrogen oxides. Using air, fuel, catalysts, and steam, system consumes less fuel and energy than decontamination processes currently in use. Similar process regenerates carbon beds used in water-treatment plants.

Voecks, Gerald E.↗

NASA NTRS2004

Recent Advances in the Development of Thick-Section Melt-Infiltrated C/SiC Composites

Using a pressureless melt infiltration and in situ reaction process to form the silicon carbide (SiC) matrix, Ultramet has been developing a means to rapidly fabricate ceramic matrix composites (CMCs) targeting thicker sections. The process also employs a unique route for the application of oxide fiber interface coatings designed to protect the fiber and impart fiber-matrix debond. Working toward a 12 inch diameter, 2.5 inch thick demonstrator component, the effect of various processing parameters on room temperature flexure strength is being studied with plans for more extensive elevated temperature mechanical strength evaluation to follow this initial optimization process.

Babcock, Jason R.↗

NASA NTRS2024

Modeling Evolvable Water Recovery Systems for Short and Long-Duration Missions in Partial Gravity

Water recovery technologies on the International Space Station (ISS) are designed and optimized for microgravity environments, thus creating a need for innovative systems optimized for mission operations in the presence of gravity. Alternative water recovery technologies under research by the Life Support Systems division were compiled into a series of Partial Gravity Water Recovery System (PGWRS) architectures. Individual unit processes were modeled via fundamental physical-chemical process equations to simulate their method of treatment, including chemical or biological oxidation, flash evaporation, filtration, or adsorption and ion exchange. Dimension and sizing data were then utilized to scale each architecture. Modeling was completed on an assortment of architectures assuming three scenarios in which treatment methods could take advantage of partial gravity: a short-duration mission with a temporary surface habitat, a longer duration mission with a more permanent habitat, and a long duration mission with minimal resupply. Total system mass was estimated to quantitatively compare architectures within scenarios, but qualitative observations were also made regarding system robustness, flexibility, and capacity to meet more stringent demands. Technologies that traded most favorably between the scenarios were those that included a pre-oxidation stage to minimize mass loading to downstream absorption and ion exchange beds, exploited gravity in liquid-vapor separation processes, and reconstituted wastewater components into recyclable material streams.

Avery L. Carlson↗

NASA NTRSDate not supplied

Modeling Evolvable Water Recovery Systems for Short and Long-Duration Missions in Partial Gravity

Avery Carlson↗

NASA NTRS1997

Single Crystal Fibers of Yttria-Stabilized Cubic Zirconia with Ternary Oxide Additions

Single crystal fibers of yttria (Y2O3)-stabilized cubic zirconia, (ZrO2) with ternary oxide additions were grown using the laser float zone fiber processing technique. Ternary additions to the ZrO2-Y2O3 binary system were studied aimed at increasing strength while maintaining the high coefficient of thermal expansion of the binary system. Statistical methods aided in identifying the most promising ternary oxide candidate (Ta2O5, Sc2O3, and HfO2) and optimum composition. The yttria, range investigated was 14 to 24 mol % and the ternary oxide component ranged from 1 to 5 mol %. Hafnium oxide was the most promising ternary oxide component based on 816 C tensile strength results and ease of fabrication. The optimum composition for development was 81 ZrO2-14 Y203-5 HfO2 based upon the same elevated temperature strength tests. Preliminary results indicate process improvements could improve the fiber performance. We also investigated the effect of crystal orientation on strength.

Ritzert, F. J.↗

DOE OSTI2022

Process Model-Based Validation of the Intensification of Biomass Fast Pyrolysis in a Fluidized Bed via Autothermal Operation

A model for the fluidized-bed pyrolysis of biomass is extended to enable the simulation of intensified autothermal operation. In this system, partial oxidation of char and pyrolysate species replaces an external heat source to supply the enthalpy of pyrolysis, greatly increasing the throughput of a given fast pyrolysis reactor. Oxidation reactions are compiled from CRECK and other literature sources and extended to cover the species found in pyrolysis products, including a derivation of the catalytic effect of ash on char combustion from experimental studies at Iowa State University (ISU). Results indicate a roughly 3-fold increase in biomass throughput for a given reactor volume at the pilot scale with minimal loss of valuable products, in agreement with published data from the 3 × 10 -2 m 3 reactor operated by ISU. Additionally, a proposal for a 250 ton/day commercial-scale biomass pyrolysis reactor is analyzed, showing that the same size reactor operated by heating the fluidizing gas externally would have only one-tenth the capacity; if operated by heating the sand externally, the sand would need to circulate at an impractical 0.7 bed volume per minute rate to maintain a 250 ton/day biomass throughput.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Low-Temperature Processing of Pyrolysis Bio-Oil for Sustainable Biographite Production

Catalytic graphitization of pyrolysis bio-oil with iron (Fe) can produce an anode material for lithium-ion batteries (LIBs) at a moderate temperature. The key challenge to scaling up the process is foaming, which occurs due to the oxidation of Fe by the organic acids present in bio-oil. This study explored five different pathways to control foaming in bio-oil upon Fe addition, including (i) defoamers use, (ii) use of iron oxide (Fe2O3) as graphitization catalyst, (iii) pH adjustment of bio-oil, (iv) bio-oil coking (300-500 degrees C), and (v) low-temperature pretreatment of bio-oil (150-200 degrees C). The low-temperature pretreatment successfully avoided foaming by removing the volatile acids in bio-oil. The bio-oil was solidified and powdered for even mixing with the Fe catalyst. The biographite catalytically prepared at 1500 degrees C following this pathway demonstrated nearly theoretical specific gravimetric capacity (~370 mAh/g), high initial Coulombic efficiency (90.03%), and minimal capacity fading after 50 cycles in LIB half-cells. The low-temperature pretreatment pathway also addressed the viscosity, swelling, and aging issues associated with bio-oil processing and will make scale-up endeavors more attainable.

09 BIOMASS FUELS↗

DOE OSTI2023

Pretreatment of Bituminous Coal By-Products for the Hydrometallurgical Extraction of Rare Earth Elements

Low-temperature plasma (LTP) oxidation has been widely used to study the mineralogy of the mineral matter existing in coal sources. The current study investigated the potential of LTP oxidation as a pre-treatment method to improve rare earth element (REE) leachability from coal and its by-products. Representative density-fractionated samples of Baker and Fire Clay coarse refuse seam materials were ground to a top size of 180 µm and subjected to low-temperature plasma oxidation. Subsequently, the treated samples were leached at 1% w/v solids concentration and 75 °C for 5 h using (i) de-ionized (DI) water, (ii) 0.1 mol/L of ammonium sulfate, and (iii) 1.2 mol/L of sulfuric acid. It was determined that LTP treatment improved REE leaching characteristics, especially the leaching of heavy REEs (HREE), existing in the lighter density fractions of the Baker seam coarse refuse material. For instance, the HREE recovery for the 1.6 specific gravity (SG) float fraction increased from 8% to 33% using 0.1 mol/L of ammonium sulfate solution after 32 h of LTP treatment. This finding indicated that HREEs associated with the organic matter were released by the LTP treatment and adsorbed onto the surfaces of highly negative charged mineral matter and was exchanged with ammonium to allow their recovery. Similarly, when using 1.2 mol/L of sulfuric acid, the HREE recovery increased from 23% to 53% for the 1.6 SG float fraction. Interestingly, LTP oxidation did not provide significant improvement in REE recovery from the 2.2 sink density fractions, which was likely due to its lower organic content. No significant benefits were observed when treating the Fire Clay coarse refuse material, which was likely due to the lack of organic affinity and the difficult-to-leach REE minerals associated with the coal source such as monazite, xenotime, and zircon. Conversely, high-temperature oxidation within a temperature range of 600–750 °C significantly improved REE leaching characteristics for both coal sources. Improvement in REE recovery was due to decarbonization of the material, clay dehydroxylation and subsequent conversion of liberated REE-bearing minerals into a more leachable form. However, increasing the temperature above 800 °C decreased REE recovery due to the conversion of meta-kaolinite into mullite, which is chemically stable.

58 GEOSCIENCES↗

DOE OSTI2020

Manganese: The overlooked contaminant in the world largest mine tailings dam collapse

Manganese (Mn) is an abundant element in terrestrial and coastal ecosystems and an essential micronutrient in the metabolic processes of plants and animals. Mn is generally not considered a potentially toxic element due to its low content in both soil and water. However, in coastal ecosystems, the Mn dynamic (commonly associated with the Fe cycle) is mostly controlled by redox processes. Here, we assessed the potential contamination of the Rio Doce estuary (SE Brazil) by Mn after the world’s largest mine tailings dam collapse, potentially resulting in chronic exposure to local wildlife and humans. Estuarine soils, water, and fish were collected and analyzed seven days after the arrival of the tailings in 2015 and again two years after the dam collapse in 2017. Using a suite of solid-phase analyses including X-ray absorption spectroscopy and sequential extractions, our results indicated that a large quantity of Mn II arrived in the estuary in 2015 bound to Fe oxyhydroxides. Over time, dissolved Mn and Fe were released from soils when Fe III oxyhydroxides underwent reductive dissolution. Due to seasonal redox oscillations, both Fe and Mn were then re-oxidized to Fe III , Mn III , and Mn IV and re-precipitated as poorly crystalline Fe oxyhydroxides and poorly crystalline Mn oxides. In 2017, redox conditions (Eh: -47 ± 83 mV; pH: 6.7 ± 0.5) favorable to both Fe and Mn reduction led to an increase (~880%) of dissolved Mn (average for 2015: 66 ± 130 μg L -1 ; 2017: 582 ± 626 μg L -1 ) in water and a decrease (~75%, 2015: 547 ± 498 mg kg -1 ; 2017: 135 ± 80 mg kg -1 ) in the total Mn content in soils. The crystalline Fe oxyhydroxides content significantly decreased while the fraction of poorly ordered Fe oxides increased in the soils limiting the role of Fe in Mn retention. The high concentration of dissolved Mn found within the estuary two years after the arrival of mine tailings indicates a possible chronic contamination scenario, which is supported by the high levels of Mn in two species of fish living in the estuary. Our work suggests a high risk to estuarine biota and human health due to the rapid Fe and Mn biogeochemical dynamic within the impacted estuary.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS2007

Ultrahigh-Temperature Ceramics

Ultrahigh temperature ceramics (UHTCs) are a class of materials that include the diborides of metals such as hafnium and zirconium. The materials are of interest to NASA for their potential utility as sharp leading edges for hypersonic vehicles. Such an application requires that the materials be capable of operating at temperatures, often in excess of 2,000 C. UHTCs are highly refractory and have high thermal conductivity, an advantage for this application. UHTCs are potentially applicable for other high-temperature processing applications, such as crucibles for molten-metal processing and high-temperature electrodes. UHTCs were first studied in the 1960 s by the U.S. Air Force. NASA s Ames Research Center concentrated on developing materials in the HfB2/SiC family for a leading-edge application. The work focused on developing a process to make uniform monolithic (2-phase) materials, and on the testing and design of these materials. Figure 1 shows arc-jet models made from UHTC materials fabricated at Ames. Figure 2 shows a cone being tested in the arc-jet. Other variations of these materials being investigated elsewhere include zirconium based materials and fiber-reinforced composites. Current UHTC work at Ames covers four broad topics: monoliths, coatings, composites, and processing. The goals include improving the fracture toughness, thermal conductivity and oxidation resistance of monolithic UHTCs and developing oxidation-resistant UHTC coatings for thermal-protection-system substrates through novel coating methods. As part of this effort, researchers are exploring compositions and processing changes that have yielded improvements in properties. Computational materials science and nanotechnology are being explored as approaches to reduce materials development time and improve and tailor properties.

Johnson, Sylvia M.↗

DOE OSTI2022

A Review on Application of Poly(3,4-ethylenedioxythiophene) (PEDOT) in Rechargeable Batteries

Since the very first patent on poly(3,4-ethylenedioxythiophene) (PEDOT) that was filed in 1988, this polymer has been widely utilized and has achieved great success owing to its high electrical conductivity and excellent stability. The application of the conducting polymer, PEDOT, in renewable energy devices, especially rechargeable batteries, is attracting increasing attention due to its potential to solve the energy and climate crisis. In this review, we summarize the research over the past few decades directed toward the application of PEDOT in rechargeable batteries aimed at improving their electrochemical performance. We focus on PEDOT synthesized via oxidative chemical vapor deposition (oCVD), a relatively new process known for its ability to grow conducting polymer thin films with uniform, pinhole-free properties, and controllable thickness and conformality. For a comparison purpose, PEDOT synthesized via solution-based methods is also briefly summarized. Finally, future research directions for applying oCVD PEDOT in rechargeable batteries are discussed. Introduction PEDOT Synthesis Methods Application of oCVD PEDOT in Rechargeable Batteries Applications of Solution-Based PEDOT in Rechargeable Batteries Conclusions and Outlook

25 ENERGY STORAGE↗

NASA NTRS1984

Occurrence of oxidized components in Qingzhen enstatite chondrite

It is shown that the most unequilibrated enstatite chondrite, Qingzhen, contains a population of enstatite grains which appear to have formed under more oxidizing nebular conditions than the bulk of the meteorite, which is highly reduced. These grains are black in transmitted light because of the presence of micron-sized inclusions of Ni-poor, Cr-rich metal, and occur either isolated within the matrix or in chondrule interiors. The textural occurrence of these grains argues against their having been introduced during collision of Qingzhen with an oxidized meteorite. Most likely, they originated in the same general nebular neighborhood of the reduced bulk Qingzhen material and were subsequently transported into the reducing environment either before or during the process of chondrule formation. The discovery of this once-oxidized material in Qingzhen posed significant constraints on existing models of formation of reduced matter in the solar system.

Rambaldi, E. R.↗

NASA NTRS1995

Sub-ppb Oxygen Contaminant Detection in Semi-Conductor Processing

Gaseous contaminants such as oxygen, water vapor, nitrogen and hydrocarbons are often present in the processing environment in semiconductor device fabrication and in containerless materials processing. The contaminants arise as a result of outgassing from hot surfaces or they may be part of the impurities in commercial ultra-high purity gases. Among these gaseous contaminants, oxygen is the most reactive and, therefore, has the most adverse effects on the end product. There has been an intense effort at the Jet Propulsion Laboratory to develop different types of oxygen sorbents to reduce oxygen concentration in a microgravity processing environment to sub-ppb (parts-per-billion) levels. Higher concentrations can lead to rapid surface oxide formation, hence reducing the quality of semiconductor devices. If the concentration of oxygen in a processing chamber at 1000oC is in the ppb level, it will only take approximately 10 seconds for an oxide layer to form on the surface of a sample. The interaction of oxygen with the water surface can lead to the formation of localized defects in semi-conductor devices, hence decreasing the manufacturing yield. For example, efficient production of 64 Mb RAM chips requires contaminations below ppb levels. This paper describes a technique for measuring trace quantities of oxygen contaminants by recording the monoatomic negative ions, O-, using mass spectrometry. The O- formation from the e--O2 interaction utilizes the electron dissociative attachment method that is greatly enhanced at the resonant energy (6.8 eV). The device combines a small gridded electron ionizer with a compact mass spectrometer. The concentrations of oxygen have been measured using the method of standard additions by diluting O2 in N2. The lowest detection limit obtained was 1.2 kHz (O- count rate) at a concentration of 10-10, corresponding to 0.1 ppb.

Sub-ppb Contaminant↗

NASA NTRS2010

Parallel Processing of Broad-Band PPM Signals

A parallel-processing algorithm and a hardware architecture to implement the algorithm have been devised for timeslot synchronization in the reception of pulse-position-modulated (PPM) optical or radio signals. As in the cases of some prior algorithms and architectures for parallel, discrete-time, digital processing of signals other than PPM, an incoming broadband signal is divided into multiple parallel narrower-band signals by means of sub-sampling and filtering. The number of parallel streams is chosen so that the frequency content of the narrower-band signals is low enough to enable processing by relatively-low speed complementary metal oxide semiconductor (CMOS) electronic circuitry. The algorithm and architecture are intended to satisfy requirements for time-varying time-slot synchronization and post-detection filtering, with correction of timing errors independent of estimation of timing errors. They are also intended to afford flexibility for dynamic reconfiguration and upgrading. The architecture is implemented in a reconfigurable CMOS processor in the form of a field-programmable gate array. The algorithm and its hardware implementation incorporate three separate time-varying filter banks for three distinct functions: correction of sub-sample timing errors, post-detection filtering, and post-detection estimation of timing errors. The design of the filter bank for correction of timing errors, the method of estimating timing errors, and the design of a feedback-loop filter are governed by a host of parameters, the most critical one, with regard to processing very broadband signals with CMOS hardware, being the number of parallel streams (equivalently, the rate-reduction parameter).

Gray, Andrew↗

DOE OSTI2026

Elucidating the role of surface species in CO oxidation catalyzed by boron nitride nanotube supported transition metal oxides

Boron nitride nanotube (BNNT) is considered a highly promising catalyst support due to its outstanding thermal stability and chemical inertness. These characteristics make BNNT an attractive alternative for high-temperature applications. However, most studies to date have focused on incorporating platinum group metals (PGMs) to achieve high activity. Although BNNT-supported PGM catalysts are highly effective, their scarcity and high cost hinder widespread use in industrial processes. In this study, BNNT-supported transition metal oxides (TMO x /BNNT; TM = Fe, Co, Ni, and Cu) catalysts were investigated, and CO oxidation was applied as a model reaction to evaluate their catalytic performance. Several characterization techniques, including SEM-EDX, TEM, SXRD, H 2 -TPR, and XPS, were employed to examine their physicochemical properties. Notably, the particle size of the metal oxides differed significantly depending on the metal type. This variation is primarily attributed to the inherent metal–support interactions and the thermodynamic stability of each oxide during synthesis. These properties also affected catalytic activity, and various parameters, such as oxygen mobility and redox behavior, played important roles in determining performance. Finally, in situ DRIFTS, CO-TPSR, reaction-order analysis, and 18 O 2 isotope-labeling experiment were used to investigate the reaction mechanism. In conclusion, the findings provide insights into the design of cost-effective BNNT-supported catalysts and highlight their potential applicability in oxidation reactions.

36 MATERIALS SCIENCE↗