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NASA NTRS1971

Oxidation/vaporization of silicide coated columbium base alloys

Mass spectrometric and target collection experiments were made at 1600 K to elucidate the mode of oxidative vaporization of two columbium alloys, fused-slurry-coated with a complex silicide former (Si-20Cr-Fe). At oxygen pressures up to 0.0005 torr the major vapor component detected by mass spectrometry for oxidized samples was gaseous silicon monoxide. Analysis of condensates collected at oxygen pressures of 0.1, 1.0 and 10 torr revealed that chromium-, silicon-, iron- and tungsten- containing species were the major products of vaporization. Equilibrium thermochemical diagrams were constructed for the metal-oxygen system corresponding to each constituent metal in both the coating and base alloy. The major vaporizing species are expected to be the gaseous oxides of chromium, silicon, iron and tungsten. Plots of vapor phase composition and maximum vaporization rate versus oxygen pressure were calculated for each coating constituent. The major contribution to weight loss by vaporization at oxygen pressures above 1 torr was shown to be the chromium-containing species.

Kohl, F. J.↗

DOE OSTI2020

Interfacial and Activation Energies of Environmentally Abundant Heterogeneously Nucleated Iron(III) (Hydr)oxide on Quartz

Poorly crystalline iron(III) (hydr)oxide nanoparticles are ubiquitous in environmental systems and play a crucial role in controlling the fate and transport of contaminants. Yet, the thermodynamic and kinetic parameters, e.g., the effective interfacial (α^') and apparent activation (E a ) energies, of iron(III) (hydr)oxide nucleation on earth-abundant mineral surfaces have not been determined, which hinders an accurate prediction of iron(III) (hydr)oxide formation and its interactions with other toxic or reactive ions. Here, for the first time, we report experimentally obtained α^' and E a for iron(III) (hydr)oxide nucleation on quartz mineral surfaces, by employing a flow-through, time-resolved grazing incidence small angle X-ray scattering (GISAXS). GISAXS enabled the in situ detection of iron(III) (hydr)oxide nucleation rates under different supersaturations (σ, achieved by varying pH 3.3-3.6) and temperatures (12-35ºC). By quantitative analyses based on classical nucleation theory, α^' was obtained to be 34.6 mJ/m 2 and E a was quantified as 32.8 kJ/mol. The fundamental thermodynamic and kinetic parameters obtained here will advance our fundamental understanding of the surface chemistry and nucleation behavior of iron(III) (hydr)oxides in subsurface and water treatment systems, as well as their effects on the fate and transport of pollutants in natural and engineered water systems. The in situ flow-through GISAXS method can also be adapted to quantify thermodynamic and kinetic parameters at interfaces for many important solid–liquid environmental systems.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2014

Verification of Dosimetry Measurements with Timepix Pixel Detectors for Space Applications

The current capabilities of modern pixel-detector technology has provided the possibility to design a new generation of radiation monitors. Timepix detectors are semiconductor pixel detectors based on a hybrid configuration. As such, the read-out chip can be used with different types and thicknesses of sensors. For space radiation dosimetry applications, Timepix devices with 300 and 500 microns thick silicon sensors have been used by a collaboration between NASA and University of Houston to explore their performance. For that purpose, an extensive evaluation of the response of Timepix for such applications has been performed. Timepix-based devices were tested in many different environments both at ground-based accelerator facilities such as HIMAC (Heavy Ion Medical Accelerator in Chiba, Japan), and at NSRL (NASA Space Radiation Laboratory at Brookhaven National Laboratory in Upton, NY), as well as in space on board of the International Space Station (ISS). These tests have included a wide range of the particle types and energies, from protons through iron nuclei. The results have been compared both with other devices and theoretical values. This effort has demonstrated that Timepix-based detectors are exceptionally capable at providing accurate dosimetry measurements in this application as verified by the confirming correspondence with the other accepted techniques.

Kroupa, M.↗

DOE OSTI2012

Theoretical analysis of two-gap superconductivity of magnesium diborades and iron pnictides in the generalized {alpha} model

A generalized {alpha} model for computing the superconducting parameters of real two-band superconductors is proposed based on an analysis of the properties of two-band equations in the theory of superconductivity. Using this model, we calculate the heat capacity and optical properties of Ba(Fe{sub 1-x}Co{sub x}){sub 2}As{sub 2} superconducting compound and obtain the temperature dependences of the gaps and energies of the Leggett modes in the Mg{sub 1-x}Al{sub x}B{sub 2} superconducting system. Good quantitative coincidence of the calculated data and experimental results is demonstrated.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2018

Dynamics of interaction between dislocations and point defects in bcc iron

The interaction between dislocations and point defects is crucial for many physical properties and phenomena in materials, such as strengthening mechanisms, dislocation bias and void swelling, creep, and impurity segregation around dislocations. Conventional dislocation-point defect interaction models use approximations based on elasticity theory and/or based on assumptions that transition states energies can be deduced from the binding energies of the defects. In this paper, we present the transport properties of point defects near dislocations based on the actual saddle-point configuration of vacancies and self-interstitial atoms as a function of position with respect to screw and edge dislocations in a model system (bcc iron) using the self-evolving atomistic kinetic Monte Carlo. Here, KMC simulations reveal defect dynamics near dislocations are highly anisotropic and correlated, particularly for dumbbells in the compressive field of the edge dislocation, which could result in zones near dislocation cores where dumbbells are less efficiently absorbed compared with vacancies. This study provides accurate saddle-point configurations and energies required to properly describe the dynamics of point defects around dislocations, allowing fundamental insights on the transport mechanisms which are essential for understanding microstructural evolution and mechanical properties of metallic materials.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Coupled Kinetics of Ferrihydrite Transformation and As(V) Sequestration under the Effect of Humic Acids: A Mechanistic and Quantitative Study

In natural environments, kinetics of As(V) sequestration/release is usually coupled with the dynamic iron mineral transformation, which is further influenced by the presence of the natural organic matter (NOM). However, both quantitative and mechanistic understanding of this process is still lacking. In this study, we investigated the effect of humic acids (HA), a major component of NOM, on the coupled kinetics of ferrihydrite transformation into hematite/goethite and sequestration of As(V) in iron minerals. Time-resolved As(V) and HA interactions with iron minerals were studied in stirred-flow kinetic experiments, using aberration-corrected scanning transmission electron microscopy (STEM), and X-ray adsorption spectroscopy. Based on the experimental results, we developed a mechanistic kinetics model for As(V) reactions with iron minerals with varying iron mineral compositions and solution chemistry. Our results showed that HA slowed ferrihydrite transformation and the rates of As(V) speciation changes within iron minerals, while HA did not incorporate into iron minerals. Our kinetics model is able to account for the variations of iron mineral compositions, solution chemistry, and As(V) speciation, which has significant environmental implications on predicting the As(V) behavior in the environment.

ferrihydrite, humic acid↗

DOE OSTI2023

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

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

01 COAL, LIGNITE, AND PEAT↗

NASA NTRS2024

Evaluation of Vertical Patterns in Chlorophyll-A Derived From A Data Assimilating Model of Satellite-Based Ocean Color

Satellite-based sensors of ocean color have become the primary tool to infer changes in surface chlorophyll, while BGC-Argo floats are now filling the information gap at depth. Here we use BGC-Argo data to assess depth-resolved information on chlorophyll-a derived from an ocean biogeochemical model constrained by the assimilation of surface ocean color remote sensing. The data-assimilating model replicates well the general seasonality and meridional gradients in surface and depth-resolved chlorophyll-a inferred from the float array in the Southern Ocean. On average, the model tends to overestimate float-based chlorophyll, particularly at times and locations of high productivity such as the beginning of the spring bloom, subtropical deep chlorophyll maxima, and non-iron limited regions of the Southern Ocean. The highest model RMSE in the upper 50 m with respect to the float array is of 0.6 mg Chl m −3 , which should allow the detection of seasonal changes in float-based biomass (varying between 0.01 and >1 mg Chl m −3 ) but might hinder the identification of subtle changes in chlorophyll at narrow local scales. Both model and float profiling data show good agreement with in situ data from station ALOHA, with model estimates showing a slight accuracy edge in inferring depth-resolved observations. Uncertainties in float bio-optical estimates impede their use as a reliable benchmark for validation, but the general qualitative agreement between model and float data provides confidence in the ability of model to replicate biogeochemical features below the surface, where data is not directly constrained by the assimilation of satellite ocean color.

Lionel A Quintero↗

DOE OSTI2015

An Aqueous Redox Flow Battery Based on Neutral Alkali Metal Ferri/ferrocyanide and Polysulfide Electrolytes

Aiming to explore low-cost redox flow battery systems, a novel iron-polysulfide (Fe/S) flow battery has been demonstrated in a laboratory cell. This system employs alkali metal ferri/ferrocyanide and alkali metal polysulfides as the redox electrolytes. When proper electrodes, such as pretreated graphite felts, are used, 78% energy efficiency and 99% columbic efficiency are achieved. The remarkable advantages of this system over current state-of-the-art redox flow batteries include: 1) less corrosive and relatively environmentally benign redox solutions used; 2) excellent energy and utilization efficiencies; 3) low cost for redox electrolytes and cell components. These attributes can lead to significantly reduced capital cost and make the Fe/S flow battery system a promising low-cost energy storage technology. The major drawbacks of the present cell design are relatively low power density and possible sulfur species crossover. Further work is underway to address these concerns.

Wei, Xiaoliang↗

NASA NTRS2001

BNL accelerator-based radiobiology facilities

For the past several years, the Alternating Gradient Synchrotron (AGS) at Brookhaven National Laboratory (USA) has provided ions of iron, silicon and gold, at energies from 600 MeV/nucleon to 10 GeV/nucleon, for the US National Aeronautics and Space Administration (NASA) radiobiology research program. NASA has recently funded the construction of a new dedicated ion facility, the Booster Applications Facility (BAF). The Booster synchrotron will supply ion beams ranging from protons to gold, in an energy range from 40-3000 MeV/nucleon with maximum beam intensities of 10(10) to 10(11) ions per pulse. The BAF Project will be described and the future AGS and BAF operation plans will be presented.

NASA Discipline Radiation Health↗

DOE OSTI2013

SWIFT AND RXTE OBSERVATIONS OF THE BLACK HOLE TRANSIENT GX 339-4 IN THE HARD STATE BETWEEN OUTBURSTS

We use simultaneous Swift and RXTE observations of the black hole binary GX 339-4 to measure the inner radius of its accretion disk in the hard state down to 0.4% L{sub Edd} via modeling of the thermal disk emission and the relativistically broadened iron line. For the luminosity range covered in this work, our results rule out a significantly truncated disk at 100-1000 R{sub g} as predicted by the advection-dominated accretion flow paradigm. The measurements depend strongly on the assumed emission geometry, with most results providing no clear picture of radius evolution. If the inclination is constrained to roughly 20 Degree-Sign , however, the measurements based on the thermal disk emission suggest a mildly receding disk at a luminosity of 0.4% L{sub Edd}. The iron abundance varies between {approx}1 and 2 solar abundances, with the i = 20 Degree-Sign results indicating a negative correlation with luminosity, though this is likely due to a change in disk illumination geometry.

79 ASTRONOMY AND ASTROPHYSICS↗

DOE OSTI2016

Effect of alloying elements, cold work, and hydrogen on the irradiation-induced growth behavior of zirconium alloy variants - 2016-0040

In-reactor dimensional changes in zirconium-based alloys result from a complex interplay of many factors, such as (1) alloy type and composition, including the addition of elements such as niobium, iron, and tin; (2) fabrication process, including cold work, texture, and residual stresses; (3) irradiation temperature; and (4) hydrogen levels. In many cases, the observed dimensional changes in light water reactor fuel-assembly components-especially at high exposures-cannot be fully explained based on current growth and creep models. Therefore, a systematic approach was taken in this multi-year (2005-2011) Nuclear Fuel Industry Research Program investigation. The objective was to measure stress-free irradiation-induced growth (IIG) of specially fabricated alloys through irradiation under controlled conditions in the BOR-60 fast-flux test reactor up to a high fluence of approximately 2X10{sup 26} m{sup -2} (E>1 MeV)-equivalent to maximum of approximately 37 dpa exposure-followed by postirradiation examinations (PIEs). Irradiation temperature was within a narrow temperature range (320±10 deg. C). The PIEs included dimensional-change and microhardness measurements, metallography and hydride etching, and scanning transmission electron microscopy (STEM) or transmission electron microscopy (TEM). All irradiation samples (typically flat rectangular coupons or curvilinear cutouts of cladding tubes sized 35 by 6.5 by 0.8 mm) were pre-filmed to avoid the uptake of impurity hydrogen from sodium-cooled BOR-60. A wide variety of samples representing standard LWR cladding alloys with and without pre-hydriding (approximately 116 to approximately 718 ppm) as well as special compositions with iron contents (100 to 4,000 ppm) were irradiated. The irradiation in BOR-60 was done in five different stages (eight micro-cycles) and lasted approximately 18 months with interim and final growth measurements made using a high precision-length measurement device. Results of the extensive investigation include: significant effects of Fe, Nb, and hydrogen additions; quantification of growth rates from low to very high fluences (dpas); measurement of volume changes; and correlation of growth with -component dislocation densities. (authors)

36 MATERIALS SCIENCE↗

NASA NTRS1974

The vapor pressure of iron pentacarbonyl

Vapor pressure measurements have been made on pure iron pentacarbonyl between +31 and -19 C. The experimental results may be expressed by the logarithm of pressure (mm Hg) to the base 10 equals -(2096.7 K/T) + 8.4959, which corresponds to a heat of vaporization for the liquid carbonyl of delta H ? (9.588 plus or minus 0.12) kcal/mole. This result confirms and extends the earlier measurements made by Trautz and Badstuebner between 0 and 140 C. The need for careful purification of commercially available iron pentacarbonyl is emphasized, particularly for establishing the correct vapor pressure below 45 C.

Gilbert, A. G.↗

NASA NTRS1993

Wet inside and out? Constraints on water in the Martian mantle and on outgassed water, based on melt inclusions in SNC meteorites

Constraints on the volatile inventory and outgassing history of Mars are critical to understanding the origin of ancient valley systems and paleoclimates. Planetary accretion models for Mars allow either a volatile-rich or volatile-poor mantle, depending on whether the accreted materials were fully oxidized or whether accretion was homogeneous so that water was lost through reaction with metallic iron. The amount of water that has been outgassed from the interior is likewise a contentious subject, and estimates of globally distributed water based on various geochemical and geological measurements vary from a few meters to more than a thousand meters. New data on SNC meteorites, which are thought to be Martian igneous rocks, provide constraints on both mantle and outgassed water.

Mcsween, H. Y., Jr.↗

NASA NTRS1972

Plastic set of smooth large radii of curvature thermal conductance specimens at light loads

Thermal contact conductance test data at high vacuum were obtained from two Armco iron specimens having smooth, large radii of curvature, convex, one-half wave length surfaces. The data are compared with calculations based on two macroscopic elastic deformation theories and an empirical expression. Major disagreement with the theories and fair agreement with the empirical expression resulted. Plastic deformation of all the contacting surfaces was verified from surface analyzer statistics. These results indicate that the theoretical assumption of macroscopic elastic deformation is inadequate for accurate prediction of heat transfer with light loads for Armco iron specimens similar to those used in this investigation.

Mckinzie, D. J., Jr.↗

NASA NTRS1972

Plastic set of smooth large radii of curvature thermal conductance specimens at light loads.

Mckinzie, D. J., Jr.↗

DOE OSTI2015

Hybrid yttrium iron garnet-ferromagnet structures for spin-wave devices

We study coupled ferromagnetic layers, which could facilitate low loss, sub 100 nm wavelength spin-wave propagation and manipulation. One of the layers is a low-loss garnet film (such as yttrium iron garnet (YIG)) that enables long-distance, coherent spin-wave propagation. The other layer is made of metal-based (Permalloy, Co, and CoFe) magnetoelectronic structures that can be used to generate, manipulate, and detect the spin waves. Using micromagnetic simulations, we analyze the interactions between the spin waves in the YIG and the metallic nanomagnet structures and demonstrate the components of a scalable spin-wave based signal processing device. We argue that such hybrid-metallic ferromagnet structures can be the basis of potentially high-performance, ultra low-power computing devices.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2011

High Efficiency Generation of Hydrogen Fuels Using Solar Thermochemical Splitting of Water

The objective of this work is to identify economically feasible concepts for the production of hydrogen from water using solar energy. The ultimate project objective was to select one or more competitive concepts for pilot-scale demonstration using concentrated solar energy. Results of pilot scale plant performance would be used as foundation for seeking public and private resources for full-scale plant development and testing. Economical success in this venture would afford the public with a renewable and limitless source of energy carrier for use in electric power load-leveling and as a carbon-free transportation fuel. The Solar Hydrogen Generation Research (SHGR) project embraces technologies relevant to hydrogen research under the Office of Hydrogen Fuel Cells and Infrastructure Technology (HFCIT) as well as concentrated solar power under the Office of Solar Energy Technologies (SET). Although the photoelectrochemical work is aligned with HFCIT, some of the technologies in this effort are also consistent with the skills and technologies found in concentrated solar power and photovoltaic technology under the Office of Solar Energy Technologies (SET). Hydrogen production by thermo-chemical water-splitting is a chemical process that accomplishes the decomposition of water into hydrogen and oxygen using only heat or a combination of heat and electrolysis instead of pure electrolysis and meets the goals for hydrogen production using only water and renewable solar energy as feed-stocks. Photoelectrochemical hydrogen production also meets these goals by implementing photo-electrolysis at the surface of a semiconductor in contact with an electrolyte with bias provided by a photovoltaic source. Here, water splitting is a photo-electrolytic process in which hydrogen is produced using only solar photons and water as feed-stocks. The thermochemical hydrogen task engendered formal collaborations among two universities, three national laboratories and two private sector entities. The photoelectrochemical hydrogen task included formal collaborations with three universities and one national laboratory. The formal participants in these two tasks are listed above. Informal collaborations in both projects included one additional university (the University of Nevada, Reno) and two additional national laboratories (Lawrence Livermore National Laboratory and Lawrence Berkeley National Laboratory).

08 HYDROGEN↗