Pressure-induced structural transformations and new polymorphs in BiVO[subscript 4]
Abstract not provided
Cheng, Xuerui↗
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Site Disorder as a Predictor for Compositionally Complex 5RE 2 Zr 2 O 7 Ceramic Phase Stability
Here, phase formation and stability of five component compositionally complex rare earth zirconates (5RE 2 Zr 2 O 7 ) were investigated by X-ray diffraction and electron microprobe analysis. Zirconates with different rare earth compositions (LaNdSmEuDy, LaNdSmEuYb, LaNdEuErYb, LaNdDyErYb, SmEuDyYHo, LaYHoErYb, and DyYHoErYb) were synthesized at 1700°C and 2000°C by the solid-state method to investigate the effect of A-site site disorder (δ A ) on phase stability. Increased site disorder results from mixed cation occupancy with localized crystallographic strain and bond disorder. Compositions LaNdSmEuDy (δ A = 4.6) and LaNdSmEuYb (δ A = 6.0) produced a single pyrochlore phase and compositions SmDyYHoErYb (δ A = 2.8), LaYHoErYb (δ A = 6.2), and DyYHoErYb (δ A = 1.7) produced a single fluorite phase. High δ A compositions LaNdEuErYb (δ A = 6.9) and LaNdDyErYb (δ A = 7.2) produced a pyrochlore and fluorite phase mixture at 1700°C. Single phase was obtained for the latter composition at 2000°C. Of the single phase compositions calcined at 1700°C, LaNdSmEuYb and LaYHoErYb (both with largest δ A ) showed decomposition to mixed fluorite and pyrochlore phases during lower temperature anneals, indicating entropic stabilization. Comparison with prior work shows a temperature dependence of the critical δ A for phase stability, and compositions near it are expected to be entropy stabilized.
36 MATERIALS SCIENCE↗
Proton-Conducting Solid Oxide Electrolysis Cells for Large-scale Hydrogen Production at Intermediate Temperatures
Proton-conducting electrolyte based SOECs offer potential for operation at low to intermediate temperatures. Although yttrium-doped barium zirconate (BZY) and ceria-doped barium zirconate (BCY) have conductivity of 0.01 and 0.017 S.cm -1 respectively at 650C in comparison to the conductivity of 0.015 S.cm -1 for 8-YSZ at 850°C, there remains technology gaps and research needs related to understanding of chemical and structural stability in oxidizing and/or reducing atmospheres at intermediate temperatures, material processing and densification techniques, high polarization losses, and electrode poisoning due to intrinsic and extrinsic gas phase contaminants. Synthesis methods have produced proton-conducting materials and cells that met degradation rate targets, showcasing stable hydrogen production. Improved performance was evident in the HSOEC cell, achieving higher hydrogen production at a lower operating temperature compared to standard cells. Collaborations with multiple research facilities ensured scaling up of synthesis processes and milestone achievements for large-scale manufacturing. Assessment of contaminants revealed their adverse effects on electrode performance and structural stability. Contaminants like Cr and Si compounds, in high humidity, degraded electrodes by forming stable silicate and chromates, inhibiting active surface reactions. Getter materials showed promise in capturing contaminants, suggesting potential for mitigation.
08 HYDROGEN↗
U-Pb ages for sphene in a contact metamorphic zone.
U-Pb ages have been determined on sphene concentrates from the 2700 my old Giants Range Granite at varying distances from the contact with the 1100 my old Duluth gabbro. As the contact is approached the sphene ages become more discordant and plot along a chord between 1100 and 2700 my on a concordia diagram. The U-Pb ages for sphene in the contact aureole are more resistant to thermal metamorphism than are K-Ar ages for hornblende and biotite. The resistance relative to U-Pb ages for zircon is more difficult to interpret because the zircon U-Pb ages may have become discordant prior to or after 1100 my ago, whereas the U-Pb ages for sphene appear to have had episodic discordance only at 1100 my ago.
Hanson, G. N.↗
Development of Si3N4 and SiC of improved toughness
The application of energy absorbing surface layers to Si3N4 and SiC was investigated. Among the layers studied were microcracked materials such as iron titanate and a silica-zircon mixture and porous materials such as reaction sintered Si3N4. Energy absorption due to microcrack extension upon impact was found not to be an important mechanism. Instead, the fivefold improvement in Charpy and ballistic impact at elevated temperature (1250 C and 1370 C) found for Fe2TiO5 was due to plastic deformation while similar improvement found for silica-zircon mixtures at RT was due to crushing of the porous material. Due to thermal expansion mismatch, these two materials could not withstand thermal cycling when used as energy absorbing surface layers on Si3N4. Reaction sintered Si3N4 layers on dense Si3N4 were found to give up to a sevenfold increase in ballistic impact resistance due to crushing of the layer upon impact. High porosity (45%), large particle size R.S. Si3N4 layers fabricated from -100, +200 mesh Si powder gave better impact improvement than less porous (30%), small particle size layers fabricated from -325 mesh Si powder.
Brennan, J. J.↗
Lu-Hf total-rock age for the Amitsoq gneisses, West Greenland
Lu-Hf total-rock data for the Amitsoq gneisses of West Greenland yield an age of 3.55 + or - 0.22 billion years, based on the decay constant for Lu-176 of 1.96 x 10 to the -11th/year, and an initial Hf-176/Hf-177 ratio of 0.280482 + or - 33. The result is in good agreement with Rb-Sr total-rock and U-Pb zircon ages. In spite of severe metamorphism of the area at 2.9 billion years, zircons from two of the samples have remained on the total-rock line, and define points close to the initial Hf ratio. The initial Hf-176/Hf-177 lies close to a chondritic Hf isotopic evolution curve from 4.55 billion years to present. This is consistent with the igneous precursors to the Amitsoq gneisses having been derived from the mantle at or shortly before 3.6 billion years. Anomalous relationships between Hf concentration and the Lu-176/Hf-177 ratio may suggest that trace element abundances in the Amitsoq gneisses are partly controlled by processes related to metamorphism.
Pettingill, H. S.↗
Trace element abundances in megacrysts and their host basalts - Constraints on partition coefficients and megacryst genesis
Rare earth and other trace element abundances are determined in megacrysts of clinopyroxene, orthopyroxene, amphibole, mica, anorthoclase, apatite and zircon, as well as their host basalts, in an effort to gather data on mineral/melt trace element partitioning during the high pressure petrogenesis of basic rocks. Phase equilibria, major element partitioning and isotopic ratio considerations indicate that while most of the pyroxene and amphibole megacrysts may have been in equilibrium with their host magmas at high pressures, mica, anorthoclase, apatite, and zircon megacrysts are unlikely to have formed in equilibrium with their host basalts. It is instead concluded that they were precipitated from more evolved magmas, and have been mixed into their present hosts.
Irving, A. J.↗
Evolution of basin and range structure in the Ruby Mountains and vicinity, Nevada
Results from various age dating techniques, seismic reflection profiling hydrocarbon maturation studies, and structural analysis were used to evaluate the Cenozoic deformation in the Ruby Mountains and adjoining ranges (pinyon Range and Cortez Range) in Elko and Eureka Counties, Nevada. Age dating techniques used include potassium-argon ages of biotites from granites published by Kistler et al. (1981) and fission track ages from apatite and zircon. Fission track ages from apatite reflect a closing temperature of 100 plus or minus 20 deg C. Zircon fission track ages reflect a closing temperature of 175 plus or minus 25 deg C and potassium-argon ages from brotite reflect a closing temperature of 250 plus or minus 30 deg C. Thus these results allow a reasonably precise tracking of the evolution of the ranges during the Cenozoic. Seismic reflection data are available from Huntington Valley. Access to seismic reflection data directly to the west of the Harrison Pass Pluton in the central Ruby Mountains was obtained. In addition results are available from several deep exploration holes in Huntington Valley.
Blackwell, D. D.↗
U-Pb ages and Sr, Pb and Nd isotope data for gneisses near the Kolar Schist Belt: Evidence for the juxtaposition of discrete Archean terranes
Uranium-lead ages and Sr, Pb, and Nd isotopic data for gneisses near the Kolar Schist Belt and their interpretation as evidence for the juxtaposition of discrete Archean terranes were presented. The granodioritic Kambha gneiss east of the schist belt has a zircon age of 2532 + or - 3 Ma and mantle-like initial Sr, Pb, and Nd isotopic ratios. Therefore these gneisses are thought to represent new crust added to the craton in the latest Archean. By contrast, more mafic Dod gneisses and leucocratic Dosa gneisses west of the schist belt (2632 + or - 7 and 2610 + or - 10 Ma) show evidence for contamination of their magmatic precursors (LREE-enriched mantle-derived for the Dod gneisses) by older (greater than 3.2 Ga) continental crust. Fragments of this older crust may be present as granitic and tonalitic inclusions in the 2.6-Ga gneisses and in shear zones. The antiquity of these fragments is supported by their Nd, Sr, and Pb isotopic compositions and by 2.8 to greater than 3.2 Ga zircon cores.
Krogstad, E. J.↗
Neodymium and lead isotope evidence for enriched early Archean crust in North America
Neodymium and lead isotope measurements and uranium-lead zircon geochronology from Archaean gneisses of the Slave Province in the Northwest Territories of Canada are reported. The gneisses contain zircons with cores older than 3.842 Gyr and an epsilon(Nd) (3.7 Gyr) of - 4.8. This is the oldest reported chondritic model age for a terrestrial sample and provides evidence for strongly enriched pre-3.8-Gyr crust, a reservoir complementary to the depleted mantle already in existence by 3.8 Gyr before the present.
Bowring, Samuel A.↗
Chronology of lunar granite 12033,576: Resetting of Rb-Sr and K-Ca isochrons
Lunar granite 12033,576 is a subsample of the 'large' (approximately 1 g) felsite 12033,507 which was identified from a collection of 4-10 mm particles from the 12033 soil sampled from the north rim of Head Crater in the eastern part of Oceanus Procellarum. Discordant ages of approximately 3.6, approximately 0.8, approximately 3.9, and approximately 2.2 Ga for this lunar granite were obtained, respectively, by the K-Ca, Ar-39/Ar-40, and U-Pb zircon methods in previous studies and by the Rb-Sr method is this study. Assuming the granite crystallized approximately 3.9 Ga ago (zircon age) and was shocked by meteoritic impacts at 0.8 Ga ago (Ar-39-Ar-40 age), the intermediate apparent ages by the Rb-Sr and K-Ca methods can be interpreted as reset by diffusion of the parent and daughter nuclides. The Rb-Sr age is less resistant to resetting than the K-Ca age, but more resistant that the Ar-39/Ar-40 age.
Shih, C.-Y.↗
Calibrating rates of early Cambrian evolution
An explosive episode of biological diversification occurred near the beginning of the Cambrian period. Evolutionary rates in the Cambrian have been difficult to quantify accurately because of a lack of high-precision ages. Currently, uranium-lead zircon geochronology is the most powerful method for dating rocks of Cambrian age. Uranium-lead zircon data from lower Cambrian rocks located in northeast Siberia indicate that the Cambrian period began about 544 million years ago and that its oldest (Manykaian) stage lasted no less than 10 million years. Other data indicate that the Tommotian and Atdabanian stages together lasted only 5 to 10 million years. The resulting compression of Early Cambrian time accentuates the rapidity of both the faunal diversification and subsequent Cambrian turnover.
Bowring, Samuel A.↗
Materials Selection and Their Characteristics as Used in Rapid Prototyping
NASA's Marshall Space Flight Center (MSFC) conducted a program to evaluate six technologies used in Rapid Prototyping (RP) to produce investment casting patterns. In this paper, RP refers to the collective additive fabrication technologies known as Solid Free-Form Fabrication. Such technologies are being used with increasing frequency in manufacturing applications, due in part to their rapidly expanding capabilities to fabricate models from many types of materials. This study used ABS plastic, polycarbonate, TrueForm PM6, epoxy resin, paper, starch, and wax. The baseline model was a semi-complex prototype fuel pump housing, intended for use in the X-33 reusable launch vehicle. All models were shelled in a production- grade colloidal silica ceramic. Primary coats were zircon-base flour with zircon backup, while secondary coats were silica grains with a tabular alumina backup. Each model was shelled in an identical manner, using the same atmospheric conditions and drying times, as well as the same number of layers. Bake-outs and firing cycles were consistent with the leach ability of each material. Preheat and bath temperatures were also kept consistent. All molds were cast in vacuum using a hydrogen-resistant superalloy (NASA- 23) that was developed in-house. The final technical evaluation included detailed measurements of the model and the final casting, in order to determine any dimensional changes caused by different pattern materials, as well as documentation of all defects and any obvious refractory/model reactions. Prototype production costs were estimated for each method and taken into consideration during trade-off analysis.
Cooper, K.↗
Recognition of > or = 3850 Ma water-lain sediments in West Greenland and their significance for the early Archaean Earth
A layered body of amphibolite, banded iron formation (BIF), and ultramafic rocks from the island of Akilia, southern West Greenland, is cut by a quartz-dioritic sheet from which SHRIMP zircon 206Pb/207Pb weighted mean ages of 3865 +/- 11 Ma and 3840 +/- 8 Ma (2 sigma) can be calculated by different approaches. Three other methods of assessing the zircon data yield ages of >3830 Ma. The BIFs are interpreted as water-lain sediments, which with a minimum age of approximately 3850 Ma, are the oldest sediments yet documented. These rocks provide proof that by approximately 3850 Ma (1) there was a hydrosphere, supporting the chemical sedimentation of BIF, and that not all water was stored in hydrous minerals, and (2) that conditions satisfying the stability of liquid water imply surface temperatures were similar to present. Carbon isotope data of graphitic microdomains in apatite from the Akilia island BIF are consistent with a bio-organic origin (Mojzsis et al. 1996), extending the record of life on Earth to >3850 Ma. Life and surface water by approximately 3850 Ma provide constraints on either the energetics or termination of the late meteoritic bombardment event (suggested from the lunar cratering record) on Earth.
NASA Discipline Exobiology↗
The Life and Times of Supervolcanoes: Inferences from Long Valley Caldera
Cataclysmic eruptions of silicic magma from "supervolcanoes" are among the most awe-inspiring natural phenomena found in the geologic record, in terms of size, power, and potential hazard. Based on the repose intervals between eruptions of this magnitude, the magmas responsible for them could accumulate gradually in the shallow crust over time scales that may be in excess of a million years (Smith, 1979; Spera and Crisp, 1981; Shaw, 1985). Pre-eruption magma residence time scales can also be inferred from the age difference between eruption (i.e., using 40Ar/39Ar dating to determine the time when hot erupted material cools to below its Ar closure temperature, 200 to 600 degC) and early pre-eruption crystallization (i.e., zircon saturation temperatures; Reid et al., 1997). I will discuss observations from Long Valley a Quaternary volcanic center in California. Long Valley is a voluminous, dominantly silicic caldera system. Based on extensive dating of accessory minerals (e.g., U-Th-Pb dating of zircon and allanite) along with geochemical and isotopic data we find that silicic magmas begin to crystallize 10's to 100's of thousands of years prior to their eruption and that rhyolites record episodes of punctuated and independent evolution rather than the periodic tapping of a long-lived magma. The more punctuated versus more gradual magma accumulation rates required by the absolute and model ages, respectively, imply important differences in the mass and heat fluxes associated with the generation, differentiation, and storage of voluminous rhyolites and emphasize the need to reconcile the magmatic age differences.
Simon, Justin↗
Sphene Emotional: How Titanite Was Shocked When the Dinosaurs Died
Accessory mineral geochronometers such as zircon, monazite, baddeleyite, and xenotime are increasingly being recognized for their ability to preserve diagnostic microstructural evidence of hypervelocity processes. However, little is known about the response of titanite to shock metamorphism, even though it is a widespread accessory phase and U-Pb geochronometer. Here we report two new mechanical twin modes in titanite within shocked granitoids from the Chicxulub impact structure, Mexico. Titanite grains in the newly acquired International Ocean Discovery Program Site expedition 364 M0077A core preserve multiple sets of polysynthetic twins, most commonly with composition planes (K1), = ~{1̅11}, and shear direction (η1) = <110>, and less commonly with the mode K1 = {130}, η1 = ~<522>. In some grains, {130} deformation bands have formed concurrently with shock twins, indicating dislocation glide with Burgers vector b = [341] can be active at shock conditions. Twinning of titanite in these modes, the presence of planar deformation features in shocked quartz, and lack of diagnostic shock microstructures in zircon in the same samples highlights the utility of titanite as a shock indicator for a shock pressure range between ~12 and ~17 GPa. Given the challenges of identifying ancient impact evidence on Earth and other bodies, microstructural analysis of titanite is here demonstrated to be a new avenue for recognizing impact deformation in materials where other impact evidence may be erased, altered, or did not manifest due to low shock pressure.
Timms, Nicholas E.↗
Applicability of Micro X-Ray Fluorescence Spectroscopy to Astromaterials Curation and Research
Introduction: The Astromaterials Acquisition and Curation Office at NASA’s Johnson Space Center (JSC) curates NASA’s astromaterial sample collections which includes: Apollo samples, Luna samples, Ant-arctic meteorites, cosmic dust particles, microparticle impacts into space-flown materials, Genesis solar wind atoms, Stardust comet Wild-2 particles, Stardust inter-stellar particles, Hayabusa asteroid Itokawa particles, Hayabusa 2 asteroid Ryugu particles, and future OSIRIS-Rex asteroid Bennu particles (landing in Sep-tember, 2023) [1–3]. To enhance JSC’s advanced cu-ration capabilities, we have recently installed a high-performance micro-X-ray fluorescence (µXRF) spec-trometer to assist in sample characterization through rapid, non-destructive, in-situ elemental analyses that do not require the sample preparation protocols (i.e., polishing and carbon-coating) commonly needed for electron beam analyses. With this new instrument, we are capable of detecting all elements down to carbon in a variable-pressure or He-purged chamber for anal-ysis of a wide range of sample types. Here we describe the instrumental set-up, capabilities, and applicability of µXRF analysis to astromaterials curation and re-search. Instrumentation and Methodology: The X-ray fluorescence and computed tomography lab (X-FaCT) lab at JSC is now equipped with a Bruker M4 Tornado Plus µXRF (Fig. 1). This system is an energy-dispersive x-ray spectrometer equipped with two 60 mm2 silicon drift detectors (SDD) that are able to be used simulta-neously for output count rates ~500,000 cps. New light element windows allow detecting and analyzing the entire elemental range from carbon to americium. Two x-ray tubes (micro-focus Rh with polycapillary lenses and W with collimators of 0.5, 1.0, 2.0, and 4.5 mm) with max excitation parameters of 50 kV, 30 W and 50 kV, 40 W, respectively, allow for more flexibility of the analysis of high energy lines. The motorized X-Y-Z stage has a mapping range of 190 x 160 mm and can support samples up to 7 kg (~15.5 lbs) and a height of 120 mm [4]. Analytical modes include elemental analysis (down to ~20 µm spot size) via point, line, or area of bulk materials (rock surfaces, thin sections, thick sections, etc.) as well as coating analysis (determination of thickness and composition) of samples. This system has a variable vacuum chamber (1 mbar to 1 atm) that is also equipped with a He-purge system which accommodates vacuum sensitive samples while still allowing detection of light elements at atmospheric pressure. Utility and Applicability of µXRF in Astro-materials research and exploration science (ARES): Elemental analysis using µXRF is commonly em-ployed for both terrestrial and planetary geological science disciplines [5]. It is especially useful for analy-sis of astromaterials given the limited sample prepara-tion required, which is not feasible for certain materi-als. Here we show select applications of µXRF anal-yses of astromaterials that can, have, and will be done at JSC’s X-FaCT lab. Point analysis: In-situ spot analyses (~20 µm spot size) on a cut slab of Martian meteorite NWA 10922 allowed for the discovery, qualitative elemental analy-sis and determination of different feldspar minerals [6]. These point analyses served as an effective prelim-inary step for subsequent quantitative analyses. Ana-lytical standards can be employed for more accurate quantification of µXRF spot analyses. Area analysis: This analytical mode measures all detectable elements (from C to Am) at each pixel (>5 µm pixel size) in a user-defined area. The results are shown as elemental maps which can be extracted as 16-bit TIFF’s for further data processing. In Fig. 2. we show elemental distribution maps of the high-Ti basalt 73001,531 that have been processed using ImageJ software. From these maps you can accurately and quickly (this map took ~50 mins.) identify mineral components, such as pyroxene, plagioclase, oxides, and phosphates, compositional zoning, and mineral textures. Detection of high-Z phases: µXRF techniques are es-pecially effective at analyzing trace minerals with high-atomic-number (high-Z) elements because the high-energy characteristic X-rays used (relative to SEM EDS) allow for mapping of K lines in elements up to La (typically SEM maps use L X-ray lines for elements >Zn, and these can often have interferences). Thus, µXRF is especially suited for identifying minerals like zircon, baddeleyite, REE-rich phosphates, Fe-rich met-als, oxides, sulfides, and phosphides [4]. In Fig. 3 we show elemental distribution maps for 73001,530 where we are able to correlate the original video image with, Zr, Si, Y and Hf elemental maps together identi-fying the location of a zircon. In this location you would expect lower Si compared to surrounding mate-rial, as well as higher Zr, Y, and Hf content compared to surrounding material, all of which is confirmed by our XRF ele-mental distribution maps (Figure 2.) Conclusions: The new M4 Tornado Plus µXRF within the Astromaterials Acquisition and Curation office at NASA JSC allows for rapid and non-destructive elemental analysis of astromaterials with limited or no sample preparation. µXRF analyses pro-vide crucial compositional knowledge for the prelimi-nary examination and curation of astromaterials. This instrument enhances the advanced curation capabili-ties in the X-FaCT laboratory at JSC by allowing pro-ductive, cohesive, and non-destructive multi-modal x-ray analyses on astromaterial samples, which is neces-sary for the comprehensive curation and study of our current and future astromaterial collections. Addition-ally, µXRF can provide complimentary information to researchers for studies on astromaterials. References: [1] Allen, C. et al., (2011). Chemie De Erde Geochemistry, 71, 1-20. [2] McCubbin, F. M. et al., (2016) 47th LPSC, abstract #2668 [3] Zeigler, R. A. et al., (2017) 48th LPSC, abstract #2772 [4] Bruker User Manual [5] Young et al., (2016) Appl. Geochemistry, 72, 77-87 [6] Mor-ris, R. V. et al., (2023) 54th LPSC.
E W O'Neal↗
Evidence for a ~1 Ga Hypervelocity Impact Event Found in Northwest Greenland
There are likely many undiscovered impact structures on Earth, but several challenges prevent their detection, including possible concealment beneath large ice sheets. In recent years, geophysical, geochemical, and microphysical evidence has mounted for a ca. 58 Ma impact structure under the Hiawatha Glacier, northwest Greenland. Here, we report evidence for a second, much older hypervelocity impact event in this region, recorded in an impact melt rock sample collected from a glaciofluvial deposit in Inglefield Land. Secondary ion mass spectrometry U-Pb analyses of shock metamorphosed zircon grains yielded a previously unrecorded, Proterozoic best estimate impact age of 1039 ± 16 Ma (mean square of weighted deviates = 2.9). Based on Archean−Proterozoic target rock U-Pb ages obtained from unshocked zircon grains and the location of the melt rock sample along the ice margin, we suggest this sample was derived from a hypervelocity impact structure farther inland, concealed by the Greenland Ice Sheet. This study demonstrates the ability to uncover new impact events in some of the most inaccessible areas on Earth and the possibility of sampling multiple impact structures from one location when examining ex situ material. Our results have implications for current and future Martian and lunar returned samples that demonstrably bear complex impact histories.
William R. Hyde↗