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At least 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
NASA NTRS2017

Oxidative Alteration of Ferrous Smectites: A Formation Pathway for Martian Nontronite?

Ferric (Fe3+-bearing) smectites, including nontronite, constitute the majority of hydrous mineral exposures observed on Mars. These smectite exposures are commonly interpreted as weathering products of Martian basaltic crust. However, ferrous (Fe2+-dominated) smectites, not ferric, are the thermo-dynamically predicted products of weathering in anoxic conditions, as predicted for early Mars. Earth was anoxic until the Proterozoic Great Oxidation Event; Mars likely experienced an analogous oxidative evolution to its present oxidized state, but the timing of this evolution is unresolved. We hypothesize that Fe3+-smectites observed by orbital spectroscopy are not the initial products of Noachian-era chemical weathering, but are instead the oxidative products of primary Fe2+-smectites. To test this hypothesis experimentally, we synthesized ferrous smectites and exposed them to Mars-relevant oxidants.

Chemtob, S. M.↗
NASA NTRS2020

Enhanced Groundwater Flow on and Below Vera Rubin Ridge, the Murray Formation, Gale Crater: Evidence from Thermochemical Modeling.

NASA’s Mars Science Laboratory Curiosity rover has been exploring Vera Rubin ridge (VRR), part of the Murray formation in Gale crater, Mars, between sol 1809 and 2302. Evidence for Fe-oxides and phyllosilicates in mineralogical and geochemical data for this region was returned by Curiosity [1-5]. We applied thermochemical modeling to con-strain the formation conditions of the phyllosilicate-hematite assemblage identified on and below VRR. Average alteration compositions for the Murray formation on and below VRR were derived using CheMin and APXS data. These compositions were reacted with Gale Portage Water (GPW) between 25–100 °C and for 10% and 50% Fe3+/Fetot of the host rock [6]. Here we summarize models run at 50 °C and 10% Fe3+/Fetot for alteration compositions derived from Murray host rock compositions.

Turner, S. M. R.↗
DOE OSTI2025

Quantification of Oxygen Vacancies in SrFe0.5Cr0.5O3−δ Thin Films: Correlating Lattice Expansion with Oxidation State Variability

Oxygen vacancies (VO), even in the dilute regime, can significantly impact the physical and chemical properties of complex oxides. It is however challenging to reliably detect and adequately quantify such defects in thin film samples where the VO concentration and distribution may further vary in response to interfacial strain. Here, we present a method to quantify VO concentrations in SrFe0.5Cr0.5O3−δ (SFCO) epitaxial thin films. Through coherent Bragg rod analysis, X-ray absorption spectroscopy, and theoretical modeling, we systematically correlate the c-axis lattice expansion detected in SFCO films with a VO concentration gradient. Our results reveal a nearly linear relationship between oxygen off-stoichiometry and out-of-plane lattice expansion in coherently strained SFCO films, with δ increasing from 0.32 to 0.52 and the lattice expanding by ∼1.0%. Moreover, a significant decrease in Cr oxidation state (from Cr5+ to Cr3+) is observed as the VO concentration increases, while the Fe oxidation state remains fixed at Fe3+. Our findings provide a reliable way to quantify oxygen stoichiometry in complex oxides, offering a pathway to design materials with precisely tailored structure–property relationships.

Hossain, Mohammad Delower↗
DOE OSTI2025

Spin dynamics in natural multiferroic pyroxene NaFeSi 2 ⁢O 6

Spin dynamics in the natural mineral aegirine, NaFeSi 2⁢ O 6 , a member of the pyroxene family, was studied by elastic and inelastic neutron scattering. Magnetization and specific-heat measurements as well as single-crystal neutron diffraction maps, taken in the temperature range 2–20 K, confirm two successive magnetic transitions at 8.8 and 5.8 K, consistent with previous studies. The observed spin-wave excitations emerge from the incommensurate magnetic Bragg peaks corresponding to the propagation vector 𝑘 ICM = (0,0.77,0), and extend up to energies of about 1.5 meV. In the low-temperature helical phase, the spin dynamics of the Fe3+ ions is well described by a simple linear spin-wave model. The observed excitations can be modeled using a spin Hamiltonian that includes three primary exchange interactions—intrachain coupling 𝐽 = 0.142⁢(2) ⁢meV, and interchain couplings 𝐽 1 = 0.083⁢(1) ⁢meV and 𝐽 2 = 0.186⁢(1) meV—and an easy-plane anisotropy 𝐷 = 0.020⁢(6)⁢ meV. Furthermore, our results show that no single exchange interaction dominates the spin dynamics. The similar strengths of the intrachain and interchain couplings point to the fact that the magnetic interactions in aegirine are three dimensional rather than confined along one direction. As a result, the system cannot be considered quasi one dimensional, as previously suggested, and calls for further investigations.

Magnetic coupling↗
DOE OSTI2024

Iron Carbonyl Complexes of [2.2.2]Hericene as a Rigid Tris(1,3-diene) Ligand

Hericene is an unusual hexaolefin consisting of three 1,3-diene units located on a rigid bicyclo [2.2.2]octane framework that restricts the geometrical relationships of metal atoms bonded to these olefinic units. In order to explore possible effects of this rigidity limiting metal–metal interaction in polynuclear derivatives possibly stabilizing coordinatively unsaturated species, the structures and energetics of the hericene iron carbonyl complexes (hericene)Fem(CO)n (m = 1, n = 3; m = 2, n = 6, 5; m = 3, n = 9, 8) have been investigated by density functional theory. The lowest-energy (hericene)Fem(CO)3m (m = 1, 2, 3) structures have the cavities of the hericene ligand filled with a single Fe(CO)3 moiety bonded to a 1,3-diolefin unit. Such species have been synthesized by the reaction of Fe2(CO)9 with hericene. For the (hericene)Fe2(CO)5 system, the lowest energy structures are singlet structures with an Fe(CO)3 unit bonded to a 1,3-diene unit in one hericene cavity and an Fe(CO)2 unit in another hericene cavity bonded to three C=C double bonds from two 1,3-diene units. Higher energy (hericene)Fe2(CO)5 structures include a structure in which a single hericene cavity contains a Fe2(CO)4(µ-CO) moiety with each iron atom bonded to a 1,3-diene unit. In addition, both singlet and triplet (hericene)Fe2(CO)5 structures are found in which an Fe(CO)3 moiety and an Fe(CO)2 moiety located in separate hericene cavities are each bonded to a 1,3-diene unit. The lowest-energy (hericene)Fe3(CO)8 structures have two hericene cavities containing Fe(CO)3 moieties fully bonded to 1,3-diene units and a third hericene cavity containing an Fe(CO)2 moiety fully bonded to a 1,3-diene unit.

Luo, Jinfeng↗
DOE OSTI2024

Effects of Al Substitution for Fe in Na₅FeSi₄O₁₂ (5.1.8) Glasses: Structure and Crystallization

In this study, the effects of substituting Al for Fe in 5Na2O∙(Al2O3)x∙(Fe2O3)1-x∙8SiO2 glass, x=0 to 1, and Na5AlxFe1-xSi4O12 (5.1.8) crystal, were investigated using thermal analysis, Fe K-edge X-ray absorption, X-ray diffraction, Raman spectroscopy, and Electron Probe Microanalysis. In both glass and crystallized glass, nearly all the Fe was tetrahedrally coordinated Fe3+, as expected from the high concentration of Na2O. The substitution of Al for Fe in the glasses caused the glass transition temperature to increase as polymerization increased, as evidenced by Raman, likely due to both field strength differences of Al vs Fe and a small amount of Fe2+ network modifier present with Fe. After heat treatment at 700 °C for 24 hours, the glasses had crystallized, forming Na2SiO3 and NaAlSiO4 in compositions with high Al concentrations and the 5.1.8 crystal in compositions with high Fe concentrations. Through electron microprobe, it was determined that <0.04 formula unit Al incorporated into the 5.1.8 crystal, i.e. Na5Fe0.96Al0.04Si4O12. The 5.1.8 crystal only formed when Fe concentration was higher than Al in the starting glass.

Antonio, Raine (ORCID:0009000634297975)↗
NASA NTRS1976

Fe-57 Moessbauer study of tektites

Moessbauer measurements were made on selected moldavite, australite, philippinite, and Georgia tektites. The spectra consist of two apparent lines, but at least two quadrupole doublets can be fitted to these spectra. The Moessbauer parameters for these doublets indicate that they arise from Fe2+ ions with local environments, which are relatively rich and relatively poor in calcium, respectively, similar to those in clinopyroxenes. No evidence for Fe3+/Fe2+ ratios above 0.01 (estimated detection limit) have been found in any tektite. Tektites are considerably more reduced than previously believed, and the extent of the reduction shows little or no variation among different types of tektites. These results limit the source materials of tektites to minerals in which the iron is uniformly highly reduced and in which the iron is contained clinopyroxene-like phases.

Evans, B. J.↗
NASA NTRS1978

Reflection spectra and magnetochemistry of iron oxides and natural surfaces

The magnetic properties and spectral characteristics of iron oxides are distinctive. Diagnostic features in reflectance spectra (0.5 to 2.4 micron) for alpha Fe2O3, gamma Fe2O3, and FeOOH include location of Fe3(+) absorption features, intensity ratios at various wavelengths, and the curve shape between 1.2 micron and 2.4 micron. The reflection spectrum of natural rock surfaces are seldom those of the bulk rock because of weathering effects. Coatings are found to be dominated by iron oxides and clay. A simple macroscopic model of rock spectra (based on concepts of stains and coatings) is considered adequate for interpretation of LANDSAT data. The magnetic properties of materials associated with specific spectral types and systematic changes in both spectra and magnetic properties are considered.

Wasilewski, P.↗
NASA NTRS1988

Compositional studies of primitive asteroids

The composition of primitive asteroids and their relationship to satellites in the solar system will be studied by analyzing existing narrowband charge coupled device (CCD) reflectance spectra, acquiring additional spectra of asteroids and small satellites in the 0.5 to 1.0 micrometer spectral range, and exploring possibilities for obtaining compositional information in the blue-UV spectral region. Comparison with laboratory spectra of terrestrial chlorites and serpentines (phyllosilicates) and the clay minerals found in carbonaceous chondrite meteorites will continue. During 1987, narrowband CCD reflectance spectra of 17 additional asteroids were acquired. These spectra and spectra of 34 other asteroids have been used primarily for two studies: weak absorption features similar to those due to Fe2(+) and Fe2(+) - Fe3(+) transitions in iron oxides f ound in terrestrial chlorites and serpentines and carbonaceous chondrites have been identified in some primitive asteroid spectra. There is a first indication that asteroids grouped by heliocentric distance show similar weak absorption features. Nonparametric statistics are being applied to test the hypothesis of discrete remnants of a gradation in composition of outer-belt asteroids.

Vilas, F.↗
NASA NTRS1989

Growth of a mat-forming photograph in the presence of UV radiation

Knowledge of the survival and growth of microorganisms in the presence of ultraviolet radiation is important for understanding the potential for life to exist in environments exposed to high fluxes of UV radiation. The growth of a mat-forming phototrophic prokaryote, Chloroflexus aurantiacus, was examined in the presence of continuous high UV irradiation under otherwise optimal growth conditions. Evidence was sought for an intrinsic ability to grow in the presence of UV radiation in a carefully chosen organism known to be unusually resistant to UV radiation, of ancient lineage among the phototrophs, to resemble ancient microfossils from the Precambrian, and to be a mat-former. It was assumed that even a high intrinsic UV resistance would be inadequate for survival and growth in the presence of very high UV fluxes, and iron (Fe3+) was selected as a common, abundant UV-absorbing substance that might protest microorganisms growing in or under iron-bearing sediments. The effectiveness of Fe(3+) was tested as a UV protective agent at low concentrations in thin layers. It was concluded that intrinsic UV resistance in some organisms may account for growth, not just survival, of these organisms when exposed to high UV fluxes under otherwise optimal growth conditions in an anoxic environment. It was also concluded that Fe(3+) bearing sediments of 1 mm or less in thickness may provide an adequate shield against high UV fluxes permitting the growth of microorganisms just below their surface. As long as growth conditions were met, then the evolution and development of microorganisms would not be hampered by high UV fluxes impinging upon the surface of iron-bearing sediments.

Pierson, Beverly K.↗
NASA NTRS1991

Transformation products of submicron-sized aluminum-substituted magnetite: Color and reductant solubility

Magnetite, when present as fine particles, is soluble in acid ammonium oxalate (pH equals 3). However, the commonly used extractant for free iron oxides (i.e., citrate dithionite-bicarbonate (CDB) is not very effective in dissolving magnetite in soils and geologic materials. Upon oxidation, magnetite transforms to maghemite; at elevated temperatures, maghemite inverts to hematite. This transformation causes a change in color from black to red and may affect the reductant solubility as well. The objectives here were to examine the color and reflectance spectral characteristics of products during the transformation of magnetite to maghemite to hematite and to study the effect of Al-substitution in magnetite on the above process. Reductant solubility of Al-substituted magnetite, maghemite, and hematite was also studied. In summary, the transformation of magnetite to maghemite was accompanied by a change in color from black to red because of the oxidation of Fe2(+) to Fe3(+). The phase change maghemite to hematite had a relatively minor effect on the color and the reflectance spectra.

Golden, D. C.↗
NASA NTRS1991

Degradation of Fe-Mg silicates in hot CO2 atmospheres: Applications to Venus

Experiments demonstrated that oxidation of ferromagnesian silicates and magnetite occurs when these minerals are heated at 800 C in 1 atmosphere of CO2, under which conditions hematite is thermodynamically stable. The 30 ppm oxygen impurity in CO2 presumably facilitates the oxidation of some of the ferrous iron initially present in the crystal structures of the minerals. Mossbauer spectral measurements reveal, however, that only CO2 degraded olivine and pigeonite is hematite formed as a magnetically ordered phase at ambient temperatures. In orthopyroxene, some of the ferric iron produced by oxidation is present as nanophase hematite which, because it remains superparamagnetic until 4.2 K, must exist as particles less than or equal to 4 nm in diameter. In the calcic pyroxenes much of the oxidized ferrous iron may still remain as structural Fe3(+) in the host silicates. Some ferric iron may also be present as unit cell sized Fe2O3 inclusions in the pyroxenes, or be segregated along cleavage planes, or be coating mineral grains. In these states of aggregation, the Fe2O3 is unidentifiable by x ray diffraction and in low temperature Mossbauer spectra. Applications of this research to the surface of Venus are discussed.

Straub, Darcy W.↗
NASA NTRS1992

Survival of microorganisms in smectite clays - Implications for Martian exobiology

The survival of Baccillus subtilis, Azotobacter chroococcum, and the enteric bacteriophage MS2 has been examined in clays representing terrestrial (Wyoming type montmorillonite) and Martian (Fe3+ montmorillonite) soils exposed to terrestrial and Martian environmental conditions of temperature and atmospheric composition and pressure. An important finding is that MS2 survived simulated Mars conditions better than the terrestrial environment, probably owing to stabilization of the virus caused by the cold and dry conditions of the simulated Mars environment. This finding, the first published indication that viruses may be able to survive in Mars-type soils, may have important implications for future missions to Mars.

Moll, Deborah M.↗
NASA NTRS1993

Tambo Quemado: Extraordinary concentrations of REE and refractory trace elements caused by artificial heating

Buchwald examined samples of the IIIB iron Tambo Quemado (TAMQ) cut from the 130 kg main mass. He determined it had been artificially heated, at some time prior to being reported, in an attempt to obtain metal from it. Although the Widmanstatten structure appears relatively unaffected under macroscopic examination, microscopic study of etched sections reveals the effect of the heating. Taenite and plessite area boundaries are indistinct due to high temperature diffusion. Schreibersite, once present in significant amounts, has been melted. Schreibersites in the interior have resolidified in fine-grained eutectic textures surrounded by dark-etching metal rims supersaturated with phosphorus. Buchwald states that phosphate minerals were probably present originally, because graftonite, and its polymorph sarcopside (both essentially Fe3(PO4)2), are common in irons of the IIIB groups. Based on his metallographic study Buchwald estimates TAMQ was heated to 1000 C for about one hour. An interior sample from TAMQ was examined in order to determine what effect this unintended heating 'experiment' had upon the phosphate phases.

Olsen, E.↗
NASA NTRS2001

Spectroscopic and Geochemical Analyses of Ferrihydrite from Hydrothermal Springs in Iceland and Applications to Mars

Ferrihydrite samples were collected from a thermal spring and a cold stream in the Landmannalaugar region of Iceland. Chemical and spectroscopic analyses have been performed on the air-dried and fine-grained fractions of these samples. The ferrihydrite from the cold stream is a pure sample, containing small amounts of Ca, P and Si, which do not form minerals detectable with X-ray diffraction (XRD) or reflectance and transmittance spectroscopy. The ferrihydrite from the thermal pool is a less pure sample, containing larger amounts of amorphous Si and P. The XRD and spectral features for this sample are also consistent with a less crystalline structure. Some of the Si is incorporated in the structure of the ferrihydrite. The Ca, P and possibly some of the Si may be biogenic. The spectral character of these Icelandic ferrihydrites is compared with those of synthetic ferrihydrites and other iron oxide/oxyhydroxide minerals. Ferrihydrite is characterized by a broad Fe3+ excitation band near 0.92 microns (approx. 10900/cm) and a strong Fe-O absorption feature near 475/cm (approx. 21 microns) in transmittance spectra. Multiple bands due to H2O and OH are also present for ferrihydrite. Natural ferrihydrites frequently exhibit a band near 950-1050/cm (approx. 10 microns) that is typically not observed for synthetic ferrihydrites and may be due to some Si in the structure. An additional pair of spectral bands near 1400 and 1500/cm (approx. 7 microns) are characteristic of pure ferrihydrites from natural and synthetic sources. Hydrothermal springs may have been present at one time on Mars in association with volcanic activity. Ferrihydrite formation in such an environment may have contributed to the ferric oxide-rich surface material on Mars.

Bishop, Janice↗
NASA NTRS2003

Moessbauer Spectroscopy on the Martian Surface: Predictions

Moessbauer spectrometers will be used on the upcoming MER/Athena and Mars Express/ Beagle 2 landers to identify and quantify relative amounts of iron-bearing minerals and determine Fe3+/Fe2+ ratios, allowing more realistic modeling of Martian mineralogy and geochemistry. To properly interpret the spectra acquired by these instruments, we must understand the Mossbauer parameters of minerals that we might expect to find on Mars. We present here a summary of predicted Fe-bearing minerals that might be observed by the MER Moessbauer spectrometers, based upon previous and our own on-going work.

Schaefer, M. W.↗
NASA NTRS2003

Electron Energy-Loss Spectroscopy (EELS) of Fe-bearing Sheet Silicates in CM Chondrites

The primitive character and hydrated mineralogy of the CM chondrites offers insight into some of the earliest reactions between solids and water. Such reactions profoundly affected the matrices and fine-grained rims (FGRs) [1-4], two of the most significant components of these meteorites [5]. We are using EELS combined with a transmission electron microscope (TEM) to investigate the compositions of Fe-bearing minerals, with emphasis on determining oxidation states and quantification of oxidation-state ratios. Iron is among the most abundant elements in the solar system and it can occur naturally in three oxidation states: Fe0, Fe2+, and Fe3+. Determination of oxidation- state ratios is useful because they can be used to infer the redox conditions under which the minerals formed or were last equilibrated [6, 7]. We are particularly interested in understanding how the oxidation state of Fe was affected by the aqueous reactions of the CM chondrites.

Zega, Thomas J.↗
NASA NTRS2004

Lunar and Planetary Science XXXV: Special Session: Oxygen in the Solar System, II

The Special Session: Oxygen in the Solar System, II, included the following reports:Evolution of Oxygen Isotopes in the Solar Nebula; Disequilibrium Melting of Refractory Inclusions: A Mechanism for High-Temperature Oxygen; Isotope Exchange in the Solar Nebula; Oxygen Isotopic Compositions of the Al-rich Chondrules in the CR Carbonaceous Chondrites: Evidence for a Genetic Link to Ca-Al-rich Inclusions and for Oxygen Isotope Exchange During Chondrule Melting; Nebular Formation of Fayalitic Olivine: Ineffectiveness of Dust Enrichment; Water in Terrestrial Planets: Always an Oxidant?; Oxygen Barometry of Basaltic Glasses Based on Vanadium Valence Determination Using Synchrotron MicroXANES; A New Oxygen Barometer for Solar System Basaltic Glasses Based on Vanadium Valence; The Relationship Between Clinopyroxene Fe3+ Content and Oxygen Fugacity ; and Olivine-Silicate Melt Partitioning of Iridium.

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