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All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Gallionellaceae in rice root plaque: metabolic roles in iron oxidation, nutrient cycling, and plant interactions

On the roots of wetland plants such as rice, Fe(II) oxidation forms Fe(III) oxyhydroxide-rich plaques that modulate plant nutrient and metal uptake. The microbial roles in catalyzing this oxidation have been debated and it is unclear if these iron-oxidizers mediate other important biogeochemical and plant interactions. To investigate this, we studied the microbial communities, metagenomes, and geochemistry of iron plaque on field-grown rice, plus the surrounding rhizosphere and bulk soil. Plaque iron content (per mass root) increased over the growing season, showing continuous deposition. Analysis of 16S rRNA genes showed abundant Fe(II)-oxidizing and Fe(III)-reducing bacteria (FeOB and FeRB) in plaque, rhizosphere, and bulk soil. FeOB were enriched in relative abundance in plaque, suggesting FeOB affinity for the root surface. Gallionellaceae FeOB Sideroxydans were enriched during vegetative and early reproductive rice growth stages, while a Gallionella was enriched during reproduction through grain maturity, suggesting distinct FeOB niches over the rice life cycle. FeRB Anaeromyxobacter and Geobacter increased in plaque later, during reproduction and grain ripening, corresponding to increased plaque iron. Metagenome-assembled genomes revealed that Gallionellaceae may grow mixotrophically using both Fe(II) and organics. The Sideroxydans are facultative, able to use non-Fe substrates, which may allow colonization of rice roots early in the season. FeOB genomes suggest adaptations for interacting with plants, including colonization, plant immunity defense, utilization of plant organics, and nitrogen fixation. Taken together, our results strongly suggest that rhizoplane and rhizosphere FeOB can specifically associate with rice roots, catalyzing iron plaque formation, with the potential to contribute to plant growth.

59 BASIC BIOLOGICAL SCIENCES↗
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↗
DOE OSTI2021

Effects of Superparamagnetic Iron Nanoparticles on Electrocatalysts for the Reduction of Oxygen

It is of great research interest to understand the nanostructures contributing to the activity observed in the reduction of oxygen by non-platinum group metal (PGM) electrocatalysts in acidic media. Iron- and nitrogen-containing carbon networks are often the most studied structures, among which single-atom iron-coordinated nitrogen (FeNx) moieties have often been proposed to be the structures leading to the high activity in these non-PGM electrocatalysts. Iron nanoparticles embedded within a carbon support are also formed under certain conditions as a result of the synthetic processes in making non-PGM electrocatalysts. In this study, we present a study to understand the oxygen reduction reaction (ORR) activity of prepared iron- and nitrogen-containing non-PGM electrocatalysts obtained through the pyrolysis of metal–organic framework (MOF) precursors. We studied the structure–property relationship among nanostructures made from the MOF precursor ZIF-8 under different pyrolysis conditions. Density functional theory calculations were used to explain the effect of structural moieties on the ORR activity. Our results suggest that iron-coordinated C–N structures and iron nanoparticles act synergistically to catalyze the ORR.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Low quantum efficiency of μ-oxo iron bisporphyrin photocatalysts explained with femtosecond M-edge XANES

Bridged μ-oxo iron porphyrins serve as photocatalysts for oxidative organic transformations, but suffer from low photon-to-product efficiency. This low photochemical quantum yield is most commonly attributed to the short lifetime of a disproportionated TPPFe(II)/TPPFe(IV)=O state, but an alternate hypothesis suggests that the majority photoproduct is a catalytically inactive ligand-centered TPPFe(III)+/TPPFe(III)–O – ion pair. We use femtosecond optical and extreme ultraviolet (XUV) spectroscopy to investigate the early photodynamics of the μ-oxo iron bisporphyrin (TPPFe) 2 O and identify the primary loss mechanism. XUV spectroscopy probes 3p → 3d transitions, corresponding to M 2,3 -edge XANES spectra, and is a distinctive probe of the metal oxidation state. Excitation of the mixed π–π*/ligand-to-metal charge transfer (LMCT) band results in the formation of an iron(II)/iron(III) LMCT state in tens of femtoseconds. This state decays on a subpicosecond timescale to the ligand-centred iron(III) ion pair state, and no TPPFe(IV)=O species is observed within the sensitivity of the measurement. Finally, the lack of an iron(II)/iron(IV) XANES spectrum suggests that preferential formation of the inactive iron(III) ion pair state is a main cause of the low quantum yield of this and similar bisporphyrins.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Unlocking iron metal as a cathode for sustainable Li-ion batteries by an anion solid solution

Traditional cathode chemistry of Li-ion batteries relies on the transport of Li-ions within the solid structures, with the transition metal ions and anions acting as the static components. Here, we demonstrate that a solid solution of F – and PO 4 3– facilitates the reversible conversion of a fine mixture of iron powder, LiF, and Li 3 PO 4 into iron salts. Notably, in its fully lithiated state, we use commercial iron metal powder in this cathode, departing from electrodes that begin with iron salts, such as FeF 3 . Our results show that Fe-cations and anions of F – and PO 4 3– act as charge carriers in addition to Li-ions during the conversion from iron metal to a solid solution of iron salts. This composite electrode delivers a reversible capacity of up to 368 mAh/g and a specific energy of 940 Wh/kg. Our study underscores the potential of amorphous composites comprising lithium salts as high-energy battery electrodes.

25 ENERGY STORAGE↗
DOE OSTI2020

A Low-Cost Iron-Based Current Collector for Alkaline Battery Electrodes

The use of three-dimensional porous nickel foam as the current collector of the nickel hydroxide electrode adds significantly to the cost of the nickel-based alkaline rechargeable batteries. Although iron is considerably less expensive than nickel, iron corrodes at the operating potential of the nickel hydroxide electrode. We have found that a 70–100 nm thick thermal coating of cobalt ferrite spinel protects the iron from corrosion. Such a coated iron substrate was found to be stable against corrosion even when polarized anodically at 10 mA cm -2 in 30% potassium hydroxide electrolyte for 1000 h. While the thermal coating of cobalt ferrite protected iron against corrosion, incorporation of lithium ions into the coating was found to enhance the electrical conductivity of the coating. XPS and EXAFS studies confirmed that the enhanced conductivity resulted from an increase in the population of Co 3+ in the ferrite spinel lattice. An inexpensive iron (steel) substrate protected by such a coating when used as a nickel hydroxide battery electrode exhibited a specific capacity of 0.25 Ah g -1 at C/5 discharge rate, comparable to a nickel hydroxide electrode based on a relatively expensive nickel foam substrate. The steel-based electrode also exhibited no noticeable degradation over 150 cycles at C/2 rate. This demonstration of a robust and economical steel substrate presents a unique opportunity for reducing the cost of the nickel hydroxide battery electrode in alkaline batteries

25 ENERGY STORAGE↗
DOE OSTI2021

Oxygen Evolution on Iron Oxide Nanoparticles: The Impact of Crystallinity and Size on the Overpotential

The oxygen evolution reaction (OER) is a critical reaction in electrolysis and photoelectrolysis of water to generate and store clean energy. Therefore, the development of low-cost and efficient electrocatalysts for the OER is of great scientific and technological importance. Although promising iron oxide-based electrocatalysts have been recently developed for the OER, an in-depth experimental and theoretical analysis of the OER mechanism on iron oxide-based electrocatalysts is still needed to provide guidelines to optimize the performance of iron oxide-based electrocatalysts further. To address this need, we synthesized a series of monodisperse iron oxide nanoparticles to analyze their intrinsic OER activities. Using nanoparticles of the same size but different crystallinity, we show that amorphous iron oxide nanoparticles have better OER activity than crystalline ones. The size effect studies further revealed that the edge/defect sites are the active sites for the OER. Density functional theory calculations demonstrated that the edge/defect sites provide bridge sites to adsorb OER intermediates, resulting in low OER overpotential. These calculations confirm that the high OER activity of amorphous nanoparticles results from a high concentration of defect sites on their surface. These results provide novel strategies to increase the performance of iron oxide-based and likely other oxide-based OER electrocatalysts.

Electrochemistry↗
DOE OSTI2026

Experimental Benchmarking for High-Reproducibility, Cross-Institutional Evaluation of Iron Redox Electrochemistry

We present a practical case study standardizing experimental protocols between collaborators with the goal of understanding ferrous iron (Fe 2+ ) chemistry and improving the iron deposition reaction for energy-efficient, electrochemical iron production. The study of iron reactions can be difficult, as aqueous iron electrolytes exhibit complex behaviors that can lead to differing interpretation of ostensibly similar experiments. The question we want to answer: are we studying the same chemistry? Our protocols address inherent challenges such as the tendency for Fe 2+ to spontaneously oxidize to ferric iron (Fe 3+ ) and the production of hydrogen at the potentials of interest. Our standardized protocol, executed by four collaborators in different labs and institutions, yields high-reproducibility results, and identified glassy carbon electrode surface quality and Fe 3+ impurities in the salt as key factors with outsized effects on cyclic voltammetry measurements. The process of developing the protocols helped to troubleshoot underlying issues that created poorer reversibility and reproducibility. This study highlights the fact that even nominally straightforward electrochemical systems can yield vastly different outcomes due to small differences in experimental preparation and serves as a useful example for creating transparent and achievable standards for the generation of reliable datasets that can be widely used and shared.

Ketter, Benjamin [Argonne National Laboratory (ANL↗
NASA NTRS1972

A Study of Heavy Trans-Iron Primary Cosmic Rays (Z More than or Equal to 55) with a Fast Film Cerenkov Detector

The detection and measurement of the cosmic ray charge spectrum for nuclei heavier than iron (Fe, Z = 26) are discussed. These trans-iron nuclei are of great interest for several reasons. They promise to be one of the more sensitive clocks for use in determining the age of cosmic rays. The discovery of radioactive nuclides and their decay products in the primary flux, will allow an estimation of the elapsed time since these cosmic rays were synthesized. In addition, the relatively short interaction length of the very heavy trans-iron particles makes their relative abundance a source of information regarding the amount of interstellar matter that they had to traverse to reach the earth. A study of the trans-iron cosmic rays may provide clues as to the very processes of nucleosyntheses by which the bulk of the trans-iron nuclei in the universe are produced. This in turn may shed light on the mechanics of the supernova, which is postulated to be the major source of all cosmic rays. Finally, trans-iron cosmic ray experiments may demonstrate the existence of the recently postulated super-heavy nuclei.

Pinsky, L. S.↗
NASA NTRS1973

Iron abundance in the moon from magnetometer measurements

Apollo 12 and 15 lunar surface magnetometer data with simultaneous lunar orbiting Explorer 35 data are used to plot hysteresis curves for the whole moon. From these curves a whole-moon permeability mu = 1.029 + 0.024 or - 0.019 is calculated. This result implies that the moon is not composed entirely of paramagnetic material, but that ferromagnetic material such as free iron exists in sufficient amounts to dominate the bulk lunar susceptibility. From the magnetic data the ferromagnetic free iron abundance is calculated. Then for assumed compositional models of the moon the additional paramagnetic iron is determined, yielding total lunar iron content. The calculated abundances are as follows: ferromagnetic free iron = 5 + or - 4 wt. percent, and total iron in the moon = 9 + or - 4 wt. percent.

Parkin, C. W.↗
NASA NTRS1974

Iron abundance and magnetic permeability of the moon

A set of simultaneous data from the Apollo 12 lunar surface magnetometer and the Explorer 35 Ames magnetometer are used to construct a whole-moon hysteresis curve, from which a new value of global lunar permeability is determined to be mu = 1.012 + or - 0.006. The corresponding global induced dipole moment is 2.1 x 10 to the 18th power gauss-cucm for typical inducing fields of .1000 gauss in the lunar environment. From the permeability measurement, lunar free iron abundance is determined to be 2.5 + or - 2.0 wt. %. Total iron abundance is calculated for two assumed compositional models of the lunar interior: a free iron/orthopyroxene lunar composition and a free iron/olivine composition. The overall lunar total iron abundance is determined to be 9.0 + or - 4.7 wt. %. Other lunar models with a small iron core and with a shallow iron-rich layer are discussed in light of the measured global permeability. Effects on permeability and iron content calculations due to a possible lunar ionosphere are also considered.

Parkin, C. W.↗
NASA NTRS1974

Iron abundance and magnetic permeability of the moon

A larger set of simultaneous data from the Apollo 12 lunar surface magnetometer and the Explorer 35 Ames magnetometer are used to construct a whole-moon hysteresis curve, from which a new value of global lunar permeability is determined to be mu = 1.012 + or - 0.006. The corresponding global induced dipole moment is 2.1 x 10 to the 18th power gauss-cu cm for typical inducing fields of .0001 gauss in the lunar environment. From the permeability measurement, lunar free iron abundance is determined to be 2.5 + or - 2.0 wt. %. Total iron abundance (sum of iron in the ferromagnetic and paramagnetic states) is calculated for two assumed compositional models of the lunar interior: a free iron/orthopyroxene lunar composition and a free iron/olivine composition. The overall lunar total iron abundance is determined to be 9.0 + or - 4.7 wt. %. Other lunar models with a small iron core and with a shallow iron-rich layer are discussed in light of the measured global permeability.

Parkin, C. W.↗
NASA NTRS1973

Iron abundance in the moon from magnetometer measurements

Apollo 12 and 15 lunar surface magnetometer data with simultaneous lunar orbiting Explorer 35 data are used to plot hysteresis curves for the whole moon. From these curves a whole-moon permeability of 1.029 (+0.024 or -0.019) is calculated. This result implies that the moon is not composed entirely of paramagnetic material, but that ferromagnetic material such as free iron exists in sufficient amounts to dominate the bulk lunar susceptibility. From the magnetic data the ferromagnetic free iron abundance is calculated. Then for assumed compositional models of the moon the additional paramagnetic iron is determined, yielding total lunar iron content. The calculated abundances are as follows: ferromagnetic free iron, 5 plus or minus 4 wt %; total iron in the moon, 9 plus or minus 4 wt %.

Parkin, C. W.↗
NASA NTRS1978

Segregation of acid plume pixels from background water pixels, signatures of background water and dispersed acid plumes, and implications for calculation of iron concentration in dense plumes

Two files of data, obtained with a modular multiband scanner, for an acid waste dump into ocean water, were analyzed intensively. Signatures were derived for background water at different levels of effective sunlight intensity, and for different iron concentrations in the dispersed plume from the dump. The effect of increased sunlight intensity on the calculated iron concentration was found to be relatively important at low iron concentrations and relatively unimportant at high values of iron concentration in dispersed plumes. It was concluded that the basic equation for iron concentration is not applicable to dense plumes, particularly because lower values are indicated at the very core of the plume, than in the surrounding sheath, whereas radiances increase consistently from background water to dispersed plume to inner sheath to innermost core. It was likewise concluded that in the dense plume the iron concentration would probably best be measured by the higher wave length radiances, although the suitable relationship remains unknown.

Bahn, G. S.↗
NASA NTRS1980

Materials processing threshold report: 2. Use of low gravity for cast iron process development

Potential applications of a low gravity environment of interest to the commercial producers of cast iron were assessed to determine whether low gravity conditions offer potential opportunities to producers for improving cast iron properties and expanding the use of cast irons. The assessment is limited to the gray and nodular types of iron, however, the findings are applicable to all cast irons. The potential advantages accrued through low gravity experiments with cast irons are described.

Frankhouser, W. L.↗
NASA NTRS1985

Iron impurities in Si3N4 processing

The atomic environment of iron impurities is investigated during the processing cycle of reaction-bonding silicon nitride (RBSN). Several analysis techniques are utilized, including X-ray photoelectron spectroscopy (XPS), extended X-ray absorption fine structure (EXAFS), and electron spin resonance (ESR), to examine iron impurities in the starting silicon powder, in sintered silicon compacts, and in RBSN materials. Results indicate that iron impurities in as-received metallurgical grade silicon powder are incorporated in the silicon bulk as a highly distorted FeSi2 compound. No surface iron or iron-based particulate is observed in the starting material. Upon sintering, the iron environment becomes an ordered FeSi2 structure. In the RBNS material, the FeSi2 structure is again distorted, as observed by both EXAFS and ESR.

Bouldin, C. E.↗
NASA NTRS1986

Isotopic, petrologic and biogeochemical investigations of banded iron-formations

It is recognized that the first occurrence of banded iron-formations (BIFs) clearly predates biological oxygenation of the atmosphere-hydrosphere system and that their last occurrences extend beyond plausible dates of pervasive biological oxygenation. For this reason, and because enormous quantities of oxidizing power have been sequestered in them, it is widely thought that these massive, but enigmatic, sediments must encode information about the mechanism and timing of the rise of atmospheric O2. By coupling isotopic analyses of iron-formation carbonates with biogeochemical and petrologic investigations, we are studying (1) the mechanism of initial sedimentation of iron; (2) the role of iron in microbially mediated diagenetic processes in fresh iron-formation sediments; and (3) the logical integration of mechanisms of deposition with observed levels of banding. Thus far, it has been shown that (1) carbonates in BIFs of the Hamersley Group of Western Australia are isotopically inhomogenous; (2) the nature and pattern of isotopic ordering is not consistent with a metamorphic origin for the overall depletion of C-13 observed in the carbonates; (3) if biological, the origin of the C-13 depleted carbonate could be either respiratory or fermentative; (4) iron may have been precipitate d as Fe(3+), then reduced to Fe(2+) within the sediment; and (5) sedimentary biogeochemical systems may have been at least partially closed to mass transport of carbonate species.

Hayes, J. M.↗
NASA NTRS1990

Melting relations in the iron-sulfur system at ultra-high pressures - Implications for the thermal state of the earth

The melting temperatures of FeS-troilite and of a 10-wt-pct sulfur iron alloy have been measured to pressures of 120 and 90 GPa, respectively. The results document that FeS melts at a temperature of 4100 (+ or - 300) K at the pressure of the core-mantle boundary. Eutecticlike behavior persists in the iron-sulfur system to the highest pressures of measurements, in marked contrast to the solid-solutionlike behavior observed at high pressures in the iron-iron oxide system. Iron with 10-wt-pct sulfur melts at a similar temperature as FeS at core-mantle boundary conditions. If the sole alloying elements of iron within the core are sulfur and oxygen and the outer core is entirely liquid, the minimum temperature at the top of the outer core is 4900 (+ or - 400) K. Calculations of mantle geotherms dictate that there must be a temperature increase of between 1000 and 2000 K across thermal boundary layers within the mantle. If D-double-prime is compositionally stratified, it could accommodate the bulk of this temperature jump.

Williams, Quentin↗