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NASA NTRS2010

Economical Fabrication of Thick-Section Ceramic Matrix Composites

A method was developed for producing thick-section [>2 in. (approx.5 cm)], continuous fiber-reinforced ceramic matrix composites (CMCs). Ultramet-modified fiber interface coating and melt infiltration processing, developed previously for thin-section components, were used for the fabrication of CMCs that were an order of magnitude greater in thickness [up to 2.5 in. (approx.6.4 cm)]. Melt processing first involves infiltration of a fiber preform with the desired interface coating, and then with carbon to partially densify the preform. A molten refractory metal is then infiltrated and reacts with the excess carbon to form the carbide matrix without damaging the fiber reinforcement. Infiltration occurs from the inside out as the molten metal fills virtually all the available void space. Densification to <5 vol% porosity is a one-step process requiring no intermediate machining steps. The melt infiltration method requires no external pressure. This prevents over-infiltration of the outer surface plies, which can lead to excessive residual porosity in the center of the part. However, processing of thick-section components required modification of the conventional process conditions, and the means by which the large amount of molten metal is introduced into the fiber preform. Modification of the low-temperature, ultraviolet-enhanced chemical vapor deposition process used to apply interface coatings to the fiber preform was also required to accommodate the high preform thickness. The thick-section CMC processing developed in this work proved to be invaluable for component development, fabrication, and testing in two complementary efforts. In a project for the Army, involving SiC/SiC blisk development, nominally 0.8 in. thick x 8 in. diameter (approx. 2 cm thick x 20 cm diameter) components were successfully infiltrated. Blisk hubs were machined using diamond-embedded cutting tools and successfully spin-tested. Good ply uniformity and extremely low residual porosity (<2 percent) were achieved, the latter being far lower than that achieved with SiC matrix composites fabricated via CVI or PIP. The pyrolytic carbon/zirconium nitride interface coating optimized in this work for use on carbon fibers was incorporated in the SiC/SiC composites and yielded a >41 ksi (approx. 283 MPa) flexural strength.

Babcock, Jason↗
NASA NTRS1994

Rare earth garnet selective emitter

Thin film Ho-YAG and Er-YAG emitters with a platinum substrate exhibit high spectral emittance in the emission band (epsilon(sub lambda) approximately equal to 0.74, ((4)l(sub 15/2)) - ( (4)l(sub13/2)), for Er-YAG and epsilon(sub lambda) approximately equal to 0.65, ((5)l(sub 7))-((5)l(sub 8)) for Ho-YAG) at excellent candidates for high efficiency selective emitters in the thermophotovoltaics (TPV) systems operating at moderate temperatures (1200-1500K). Spectral emittance measurements of the thin films were made (1.2 less than lambda less than 3.0 microns) and compared to the theoretical emittances calculated using measured values of the spectral extinction coefficient. In this paper we present the results for a new class of rare earth ion selective emitters. These emitters are thin sections (less than 1 mm) of yttrium aluminum garnet (YAG) single crystal with a rare earth substitutional impurity. This paper presents normal spectral emittance, epsilon(sub lambda), measurements of holmium (Ho), and erbium (Er) doped YAG thin film selective emitters at 1500 K, and compares those results with the theoretical spectral emittance.

Lowe, Roland A.↗
NASA NTRS1978

Apollo 14 rock samples

Petrographic descriptions of all Apollo 14 samples larger than 1 cm in any dimension are presented. The sample description format consists of: (1) an introductory section which includes information on lunar sample location, orientation, and return containers, (2) a section on physical characteristics, which contains the sample mass, dimensions, and a brief description; (3) surface features, including zap pits, cavities, and fractures as seen in binocular view; (4) petrographic description, consisting of a binocular description and, if possible, a thin section description; and (5) a discussion of literature relevant to sample petrology is included for samples which have previously been examined by the scientific community.

Carlson, I. C.↗
NASA NTRS2013

Transmission Electron Microscopy of Itokawa Regolith Grains

Introduction: In a remarkable engineering achievement, the JAXA space agency successfully recovered the Hayabusa space-craft in June 2010, following a non-optimal encounter and sur-face sampling mission to asteroid 25143 Itokawa. These are the first direct samples ever obtained and returned from the surface of an asteroid. The Hayabusa samples thus present a special op-portunity to directly investigate the evolution of asteroidal sur-faces, from the development of the regolith to the study of the effects of space weathering. Here we report on our preliminary TEM measurements on two Itokawa samples. Methods: We were allocated particles RA-QD02-0125 and RA-QD02-0211. Both particles were embedded in low viscosity epoxy and thin sections were prepared using ultramicrotomy. High resolution images and electron diffraction data were ob-tained using a JEOL 2500SE 200 kV field-emission scanning-transmission electron microscope. Quantitative maps and anal-yses were obtained using a Thermo thin-window energy-dispersive x-ray (EDX) spectrometer. Results: Both particles are olivine-rich (Fo70) with μm-sized inclusions of FeS and have microstructurally complex rims. Par-ticle RA-QD02-0125 is rounded and has numerous sub-μm grains attached to its surface including FeS, albite, olivine, and rare melt droplets. Solar flare tracks have not been observed, but the particle is surrounded by a continuous ~50 nm thick, stuctur-ally disordered rim that is compositionally similar to the core of the grain. One of the surface adhering grains is pyrrhotite show-ing a S-depleted rim (~8-10 nm thick) with nanophase Fe metal grains (<5 nm) decorating the outermost surface. The pyrrhotite displays a complex superstructure in its core that is absent in the S-depleted rim. Particle RA-QD02-0211 contains solar flare particle tracks (~2x109 cm-2) and shows a structurally disordered rim ~100 nm thick. The track density corresponds to a surface exposure of ~103-104 years based on the track production rate of [1]. The dis-ordered rim is nanocrystalline with minor amorphous material between crystalline domains. Quantitative element maps show the outermost ~10 nm of the disordered rim is Si-rich. Discussion and Conclusions: Both particles record the ef-fects of space weathering processes on Itokawa. Noguchi et al. [2] proposed that the disordered rims they observed on Itokawa particles largely result from solar wind radiation damage and we arrive at a similar conclusion for the two particles we analyzed. The microstructure of the S-depleted layer on the pyrrhotite grain in RA-QD02-0125 is similar to that observed in troilite irradiated with ~1018 4 kV He+ [3, 4]. Prolonged irradiation has also been shown to disorder pyrrhotite such that the superstructure reflec-tions are lost [5].

Keller, Lindsay P.↗
NASA NTRS2014

Space Weathering of Olivine in Lunar Soils: A Comparison to Itokawa Regolith Samples

Regolith particles from airless bodies preserve a record of the space weathering processes that occurred during their surface exposure history. These processes have major implications for interpreting remote-sensing data from airless bodies. Solar wind irradiation effects occur in the rims of exposed grains, and impact processes result in the accumulation of vapordeposited elements and other surface-adhering materials. The grains returned from the surface of Itokawa by the Hayabusa mission allow the space weathering "style" of a chondritic, asteroidal "soil" to be compared to the lunar case. Here, we present new studies of space-weathered olivine grains from lunar soils, and compare these results to olivine grains from Itokawa. Samples and Methods: We analyzed microtome thin sections of olivine grains from the 20-45 micron fractions of three lunar soils: 71061, 71501 and 10084 (immature, submature and mature, respectively). Imaging and analytical data were obtained using a JEOL 2500SE 200kV field-emission scanning-transmission electron microscope equipped with a thin-window energy-dispersive x-ray spectrometer. Similar analyses were obtained from three Hayabusa olivine grains. Results and Discussion: We observed lunar grains showing a range of solar flare track densities (from <10(exp 9) to approx.10(exp 12)/sq cm). The lunar olivines all show disordered, highly strained, nanocrystalline rims up to 150-nm thick. The disordered rim thickness is positively correlated with solar flare track density. All of the disordered rims are overlain by a Si-rich amorphous layer, ranging up to 50-nm thick, enriched in elements that are not derived from the host olivine (e.g., Ca, Al, and Ti). The outmost layer represents impact-generated vapor deposits typically observed on other lunar soil grains. The Hayabusa olivine grains show track densities <10(exp 10)/sq cm and display disordered rims 50- to 100-nm thick. The track densities are intermediate to those observed in olivines in immature and submature lunar soils and indicate surface exposures of approx. 10(exp 5) years. The outermost few nanometers of the disordered rims on Hayabusa olivines are more Si-rich and Mg- and Fe-depleted relative to the cores of the grains and likely represent a minor accumulation of impact-generated vapors or sputter deposits. Nanophase Fe metal particles are less abundant in the Hayabusa rims compared to the rims on lunar grains. Conclusions: The Hayabusa and lunar olivine grain rims have widths and microstructures consistent with formation from atomic displacement damage from solar wind ions. The space weathering features in the Hayabusa grains are similar to those observed in olivines from immature to submature lunar soils. A major difference, however, is that the Hayabusa grains appear to lack the hypervelocity impact products (melt spherules, thick vapor deposits, and abundant nanophase Fe metal particles) that are common in lunar soil grains with a similar exposure history.

Keller, L. P.↗
NASA NTRS1994

Phosphate microaggregates in Archean sediments

Light microscopy conducted on samples of Archean sediments reveals phosphate microaggregates which are suggestive of a biotic origin (Arrhenius et al., 1993). These aggregates, typically 15 micrometers wide and 50 micrometers long, are thought to be the mineral remains of colonies of microorganisms that lived during the late Archean Eon (greater than or equal to 2.5 Ga). Confocal microscopy was used to study the structures of these microaggregates in three dimensions. Samples used in this study are from the lowermost section of drill core taken from the Dales Gorge Member of the Brockman Iron-Formation (Hamersley Basin) in Western Australia. These sediments are well-preserved and escaped extensive metamorphism typically experienced by older rocks of this type. Two types of samples were prepared for study under the microscope: thin sections (30 micrometers) for transmitted light microscopy to study the general rock texture and to locate the grains of interest, and thick sections (3mm) for confocal microscopy to determine the 3-D structure of the aggregates in situ. The samples have been carefully polished so that they may be directly placed on the oil-immersion lens without the use of a cover slip. No chemical treatments of the surfaces have been performed. The aggregates often form clusters, although isolated aggregates have also been found. The clusters tend to distribute along microbands in the rocks. Electron microprobe analyses show that the phosphate grains and their inclusions, besides calcium and phosphorus, contain no major elements heavier than sodium. The proportions of calcium to phosphorus, the absence of stoichiometric amounts of other cations such as magnesium and iron, as well as optical properties suggest apatite as the mineral form.

Mojzsis, S.↗
NASA NTRS1997

Raman Spectroscopy for Mineral Identification and Quantification for in situ Planetary Surface Analysis: A Point Count Method

Quantification of mineral proportions in rocks and soils by Raman spectroscopy on a planetary surface is best done by taking many narrow-beam spectra from different locations on the rock or soil, with each spectrum yielding peaks from only one or two minerals. The proportion of each mineral in the rock or soil can then be determined from the fraction of the spectra that contain its peaks, in analogy with the standard petrographic technique of point counting. The method can also be used for nondestructive laboratory characterization of rock samples. Although Raman peaks for different minerals seldom overlap each other, it is impractical to obtain proportions of constituent minerals by Raman spectroscopy through analysis of peak intensities in a spectrum obtained by broad-beam sensing of a representative area of the target material. That is because the Raman signal strength produced by a mineral in a rock or soil is not related in a simple way through the Raman scattering cross section of that mineral to its proportion in the rock, and the signal-to-noise ratio of a Raman spectrum is poor when a sample is stimulated by a low-power laser beam of broad diameter. Results obtained by the Raman point-count method are demonstrated for a lunar thin section (14161,7062) and a rock fragment (15273,7039). Major minerals (plagioclase and pyroxene), minor minerals (cristobalite and K-feldspar), and accessory minerals (whitlockite, apatite, and baddeleyite) were easily identified. Identification of the rock types, KREEP basalt or melt rock, from the 100-location spectra was straightforward.

Haskin, Larry A.↗
NASA NTRS2003

Morphology of the Vestibular Utricule in Toadfish, Opsanus Tau

The uticle is an otolith organ in the vertebrate inner ear that provides gravitoinertial acceleration information into the vestibular reflex pathways. The aim of the present study was to provide an anatomical description of this structure in the adult oyster toadfish, and establish a morphological basis for interpretation of subsequent functional studies. Light, scanning electron and transmission electron microscopy were applied to visualize the sensory epithelium and its neural innervation. Electrophysiological techniques were used to identify utricular afferents by their response to translation stimuli. Similar to nerve afferents supplying the semicircular canals and lagena, utricular afferents commonly exhibit a short-latency increase of firing rate in response to electrical activation of the central efferent pathway. Afferents were labeled with biocytin either intraaxonally or with extracellular bulk deposits. Light microscope images of serial thick sections were used to make three-dimensional reconstructions of individual labeled afferents to identify the dendritic morphology with respect to epithelial location. Scanning electron microscopy was used to visualize the surface of the otolith mass facing the otolith membrane, and the hair cell polarization patterns of strioler and extrastriolar regions. Transmission electron micrographs of serial thin sections were compiled to create a three-dimensional reconstruction of the labeled afferent over a segment of its dendritic field and to examine the hair cell-afferent synaptic contacts.

Bass, L.↗
NASA NTRS2015

Are the Clast Lithologies Contained in Lunar Breccia 64435 Mixtures of Anorthositic Magmas

The anorthositic crust of the Moon is often used as the archtypical example of a primary planetary crust. The abundance and purity of anorthosite in the Apollo sample collection and remote sensing data are generally attributed to an early global magma ocean which produced widespread floating plagioclase cumulates (the ferroan anorthosites; FANs. Recent geochronology studies report evidence of young (less than 4.4 Ga) FAN ages, which suggest that either some may not be directly produced from the magma ocean or that the final solidification age of the magma ocean was younger than previous estimates. A greater diversity of anorthositic rocks have been identified among lunar meteorites as compared to returned lunar samples. Granted that these lithologies are often based on small clasts in lunar breccias and therefore may not represent their actual whole rock composition. Nevertheless, as suggested by the abundance of anorthositic clasts with Mg# [Mg/(Mg+Fe)] less than 0.80 and the difficulty of producing the extremely high plagioclase contents observed in Apollo samples and the remote sensing data, modification of the standard Lunar Magma Ocean (LMO) model may be in order. To ground truth mission science and to further test the LMO and other hypotheses for the formation of the lunar crust, additional coordinated petrology and geochronology studies of lunar anorthosites would be informative. Here we report new mineral chemistry and trace element geochemistry studies of thick sections of a composite of FAN-suite igneous clasts contained in the lunar breccia 64435 in order to assess the significance of this type of sample for petrogenetic studies of the Moon. This work follows recent isotopic studies of the lithologies in 64435 focusing on the same sample materials and expands on previous petrology studies who identified three lithologies in this sample and worked on thin sections.

Simon, J. I.↗
NASA NTRS2014

Search for Fluid Inclusions in a Carbonaceous Chondrite Using a New X-Ray Micro-Tomography Technique Combined with FIB Sampling

Early solar system aqueous fluids are preserved in some H chondrites as aqueous fluid inclusions in halite (e.g., [1]). Although potential fluid inclusions are also expected in carbonaceous chondrites [2], they have not been surely confirmed. In order to search for these fluid inclusions, we have developped a new X-ray micro-tomography technique combined with FIB sampling and applied this techniqu to a carbanaceous chondrite. Experimental: A polished thin section of Sutter's Mill meteorite (CM) was observed with an optical microscope and FE-SEM (JEOL 7001F) for chosing mineral grains of carbonates (mainly calcite) and sulfides (FeS and ZnS) 20-50 microns in typical size, which may have aqueous fluid inclusions. Then, a "house" similar to a cube with a roof (20-30 microns in size) is sampled from the mineral grain by using FIB (FEI Quanta 200 3DS). Then, the house was atached to a thin W-needle by FIB and imaged by a SR-based imaging microtomography system with a Fresnel zone plate at beamline BL47XU, SPring-8, Japan. One sample was imaged at two X-ray energies, 7 and 8 keV, to identify mineral phases (dual-enegy microtomography: [3]). The size of voxel (pixel in 3D) was 50-80 nm, which gave the effective spatial resolution of approx. 200 nm. A terrestrial quartz sample with an aqueous fluid inclusion with a bubble was also examined as a test sample by the same method. Results and discussion: A fluid inclusion of 5-8 microns in quartz was clearly identified in a CT image. A bubble of approx. 4 microns was also identified as refraction contrast although the X-ray absorption difference between fluid and bubble is small. Volumes of the fluid and bubble were obtained from the 3D CT images. Fourteen grains of calcite, two grains of iron sulfide and one grain of (Zn,Fe)S were examined. Ten calcite, one iron sulfide and one (Zn,Fe)S grains have inclusions >1 micron in size (the maximum: approx. 5 microns). The shapes are spherical or irregular. Tiny inclusions (<1 micron) are also present in all the grains examined. These results show that mineral grains have more inclusions than expected from 2D observations. The X-ray absorption of the inclusions shows that they are not solid inclusions. No bubbles were observed inside, indicating that we cannot determine whether they are really aqueous fluids or merely voids. One calcite grain has an inclusion approx. 2 microns in size, which seems to have a bubble and a tiny solid daughter crystal inside (three-phase inclusion). As we know the exact 3D position of the inclusion, we will anlyze the inclusion by SIMS after freezing the sample as has been done for a halite sample [3]. The present technique is useful for finding small inclusions not only in carbonaceous chondrites but also for terrestrial materials.

Tsuchiyama, A.↗
NASA NTRS1983

Removal of histological sections from glass for electron microscopy - Use of Quetol 651 resin and heat

A number of approaches have been used to separate stained conventional histological sections from glass slides in preparation for a study with the electron microscope. However, in each reported case some problems were encountered with respect to the separation process. The present investigation is concerned with the use of the epoxy resin Quetol 651 as an embedding medium for this procedure, taking into account the simple application of heat (62-64 C) for performing the separation step. After the tissue has been removed from the glass by the considered technique, it is thin sectioned, and stained with uranyl acetate-lead citrate.

Kraft, L. M.↗
NASA NTRS2014

A Coordinated Focused Ion Beam/Ultramicrotomy Technique for Serial Sectioning of Hayabusa Particles and Other Returned Samples

Recent sample return missions, such as NASA's Stardust mission to comet 81P/Wild 2 and JAXA's Hayabusa mission to asteroid 25143 Itokawa, have returned particulate samples (typically ~5-50 μm) that pose tremendous challenges to coordinated analysis using a variety of nano- and micro-beam techniques. The ability to glean maximal information from individual particles has become increasingly important and depends critically on how the samples are prepared for analysis. This also holds true for other extraterrestrial materials, including interplanetary dust particles, micrometeorites and lunar regolith grains. Traditionally, particulate samples have been prepared using microtomy techniques (e.g., [1]). However, for hard mineral particles ≳20 μm, microtome thin sections are compromised by severe chatter and sample loss. For these difficult samples, we have developed a hybrid technique that combines traditional ultramicrotomy with focused ion beam (FIB) techniques, allowing for the in situ investigation of grain surfaces and interiors. Using this method, we have increased the number of FIB-SEM prepared sections that can be recovered from a particle with dimensions on the order of tens of μms. These sections can be subsequently analyzed using a variety of electron beam techniques. Here, we demonstrate this sample preparation technique on individual lunar regolith grains in order to study their space-weathered surfaces. We plan to extend these efforts to analyses of individual Hayabusa samples.

Berger, E. L.↗
NASA NTRS1994

Rare Earth Garnet Selective Emitter

Thin film Ho-YAG and Er-YAG emitters with a platinum substrate exhibit high spectral emittance in the emission band (epsilon(sub lambda) approx. = 0.75, sup 4)|(sub 15/2) - (sup 4)|(sub 13/2),for Er-YAG and epsilon(sub lambda) approx. = 0.65, (sup 5)|(sub 7) - (sup 5)|(sub 8) for Ho-YAG) at 1500 K. In addition, low out-of-band spectral emittance, epsilon(sub lambda) less than 0.2, suggest these materials would be excellent candidates for high efficiency selective emitters in thermophotovoltaic (TPV) systems operating at moderate temperatures (1200-1500 K). Spectral emittance measurements of the thin films were made (1.2 less than lambda less than 3.0 microns) and compared to the theoretical emittances calculated using measured values of the spectral extinction coefficient. In this paper we present the results for a new class of rare earth ion selective emitters. These emitters are thin sections (less than 1 mm) of yttrium aluminum garnet (YAG) single crystal with a rare earth substitutional impurity. Selective emitters in the near IR are of special interest for thermophotovoltaic (TPV) energy conversion. The most promising solid selective emitters for use in a TPV system are rare earth oxides. Early spectral emittance work on rare earth oxides showed strong emission bands in the infrared (0.9 - 3 microns). However, the emittance outside the emission band was also significant and the efficiency of these emitters was low. Recent improvements in efficiency have been made with emitters fabricated from fine (5 - 10 microns) rare earth oxide fibers similar to the Welsbach mantle used in gas lanterns. However, the rare earth garnet emitters are more rugged than the mantle type emitters. A thin film selective emitter on a low emissivity substrate such as gold, platinum etc., is rugged and easily adapted to a wide variety of thermal sources. The garnet structure and its many subgroups have been successfully used as hosts for rare earth ions, introduced as substitutional impurities, in the development of solid state laser crystals. Doping, dependent on the particular ion and crystal structure, may be as high as 100 at. % (complete substitution of yttrium ion with the rare earth ion). These materials have high melting points, 1940 C for YAG (Yttrium Aluminum Garnet), and low emissivity in the near infrared making them excellent candidates for a thin film selective emitter. As previously stated, the spectral emittance of a rare earth emitter is characterized by one or more well defined emission bands. Outside the emission band the emittance(absorptance) is much lower. Therefore, it is expected that emission outside the band for a thin film selective emitter will be dominated by the emitter substrate. For an efficient emitter (power in the emission band/total emitted power) the substrate must have low emittance, epsilon(sub S). This paper presents normal spectral emittance, epsilon(sub lambda), measurements of holmium(Ho) and erbium (Er) doped YAG thin film selective emitters at (1500 K), and compares those results with the theoretical spectral emittance.

Lowe, Roland A.↗
NASA NTRS2018

Novel Applications of Focused Ion Beam Technique for Planetary Sample Analyses

We are using innovative FIB techniques to prepare samples of planetary materials for different types of coordinated analyses using ion microprobes, synchrotron beamlines, and specialized transmission electron microscopy (TEM) techniques. In these cases, the FIB sample preparation is the critical step in enabling these specialized analyses. We discuss several examples below utilizing the FEI Quanta3D instrument at the NASA Johnson Space Center. Trace element analyses utilizing synchrotron x-ray fluorescence. The trace element content of mineral grains in comet dust provides important clues on their formation and processing in the early solar system. We preformed coordinated analyses of a comet dust particle that had been prepared using ultramicrotomy for TEM analysis. Following the TEM analyses, we extracted a 70 nm thick section from a region of the carbon (C) film of the TEM grid, for additional analyses. A carbon ring ~2-3 μm thick was deposited on top of the C film using the FIB. The C film on the outer rim of the ring was milled away using various patterns to uniformly release the stresses on the film, preventing rupture and collapse, and was attached to the micromanipulator needle. We then isolated the ring completely and transferred the section to a silicon sample holder for analysis using the HXN (hard X-ray nanoprobe) beamline at NSLSII at Brookhaven National Lab. Coordinated Analyses of Presolar Grains. Rare sub-m presolar grains that originate in evolved stars and supernovae, occur in primitive astromaterials and are identified by their exotic isotopic compositions. Coordinated analyses of these grains using NanoSIMS, TEM, and other techniques on the same grain is enabled by innovative FIB sample preparation. In order to obtain subsequent isotopic analyses of Mg and Fe, contributions from surrounding grains were minimized. We precisely deposited a protective cap of Pt on top of the grain to preserve the grain of interest and then milled away about 5 μm diameter of the surrounding material. Following the isotopic analyses, the spindle was extracted and thinned to electron transparency for TEM microstructural analyses. In situ heating TEM experiments on lunar samples. We extracted a FIB thin section from Apollo 17 lunar rock 76015. To avoid ion-beam damage, e-beam deposition was used to deposit the first 500 nm of the C strap, followed by ion beam-assisted deposition of ~3 μm carbon. We performed an ex situ lift-out of the section and placed the section on one of the elements of a microelectromechanical systems (MEMS) - specialized heating substrate and attached the section to the substrate by depositing small C straps with the FIB. The heating chips utilize silicon nitride windows to support the samples and provide uniform heating while enabling TEM imaging. The heating chip was loaded into a Hitachi “Blaze” heating holder and analyzed using a Hitachi HF5000 at the University of Arizona.

Rahman, Z.↗
NASA NTRS2013

Allochthonous Addition of Meteoritic Organics to the Lunar Regolith

Preparation of lunar samples 74220,861 was discussed in detail in [3, 4]. Our analysis sequence was as follows: optical microscopy, UV fluorescence imaging, -Raman, FESEM-EDX imaging and mapping, FETEMEDX imaging and mapping of a Focused Ion Beam (FIB) extracted section, and NanoSIMs analysis. We observed fluffytextured C-rich regions of interest (ROI) on three different volcanic glass beads. Each ROI was several m2 in size and fluoresced when exposed to UV. Using FESEM/EDX, the largest ROI measured ~36 m and was located on an edge of a plateau located on the uppermost surface of the bead. The ROI was covered on one edge by a siliceous filament emanating from the plateau surface indicating it was attached to the bead while on the Moon. EDX mapping of the ROI shows it is composed primarily of heterogeneously distributed C. Embedded with the carbonaceous phase are localized concentrations of Si, Fe, Al and Ti indicating the presence of glass and/or minerals grains. -Raman showed strong D- and G-bands and their associated second order bands; intensity and location of these bands indicates the carbonaceous matter is structurally disorganized. A TEM thin section was extracted from the surface of a glass bead using FIB microscopy. High resolution TEM imaging and selected area electron diffraction demonstrate the carbonaceous layer to be amorphous; it lacked any long or short range order characteristic of micro- or nanocrystalline graphite. Additionally TEM imaging also revealed the presence of submicron mineral grains, typically < 50 nm in size, dispersed within the carbonaceous layer. NanoSIMs data will be presented and discussed at the meeting. Given the noted similarities between the carbonaceous matter present on 74220 glass beads and meteoritic kerogen, we suggest the allochthonous addition of meteoritic organics as the most probable source for the C-rich ROIs.

Thomas-Keprta, K. L.↗
NASA NTRS2016

Precision Oxygen Isotope Measurements of Two C-Rich Hydrated Interplanetary Dust Particles

Introduction: Chondritic-smooth IDPs (Interplanetary Dust Particles) are low porosity objects whose mineralogy is dominated by aqueous alteration products such as Mg-rich phyllosilicates (smectite and serpentine group) and Mg-Fe carbonate minerals. Their hydrated mineralogy combined with low atmospheric entry velocities have been used to infer an origin largely from asteroidal sources. Spectroscopic studies show that the types and abundance of organic matter in CS IDPs is similar to that in CP IDPs. Although CS IDPs show broad similarities to primitive carbonaceous chondrites, only a few particles have been directly linked to specific meteorite groups such as CM and CI chondrites based on the presence of diagnostic minerals. Many CS IDPs however, have carbon contents that greatly exceed that of known meteorite groups suggesting that they either may derive from comets or represent samples of more primitive parent bodies than do meteorites. It is now recognized that many large, dark primitive asteroids in the outer main belt, as well as some trans-Neptunian objects, show spectroscopic evidence for aqueous alteration products on their surfaces. Some CS IDPs exhibit large bulk D enrichments similar to those observed in the cometary CP IDPs. While hydrated minerals in comets have not been unambiguously identified to date, the presence of the smectite group mineral nontronite has been inferred from infrared spectra obtained from the ejecta from comet 9P/Tempel 1 during the Deep Impact mission. Recent observations of low temperature sulfide minerals in Stardust mission samples suggest that limited aqueous activity occurred on comet Wild-2. All of these observations, taken together, suggest that the high-carbon hydrated IDPs are abundant and important samples of primitive solar system objects not represented in meteorite collections. Oxygen isotopic compositions of chondrites reflect mixing between a 16O-rich reservoir and a 17O,18O-rich reservoir produced via mass-independent fractionation. The composition of the 16O-rich reservoir is well constrained but material representing the 17O,18O-rich end-member is rare. Self-shielding models predict that cometary water, presumed to represent this reservoir, should be enriched in 17O and 18O by greater than 200 per mille. The high-carbon hydrated IDPs may be among the best materials available to search for preserved "cometary" H2O signatures. In order to better understand the origin and evolution of these particles, we have obtained 10 hydrated interplanetary dust particles for coordinated mineralogical, isotopic and organic analyses. We have previously reported the results of mineralogical and O isotopic measurements of two hydrated IDPs; here we present results of O isotopic measurements of three additional IDPs. Samples and Methods: Three interplanetary dust particles (L2079C35, L2083D46 and L2083E46) were embedded in S and partially ultramicrotomed into approximately 70 nanometer sections for analysis via transmission electron microscopy (TEM). The remainders of the unsliced particles were removed from S and pressed into high purity Au foil that was cleaned with HF acid and annealed at 800 degrees Centigrade. The pressed IDPs were analyzed via electron microprobe analysis (EPMA) for quantitative bulk chemical analysis. After EPMA analysis, the IDPs were subjected to precision O isotope analysis with the UCLA Cameca IMS-1270 ion probe. A 20 kiloelectronvolt, 0.5 nanoangstrom Cs+ primary beam of approximately 15 micrometers diameter was used for each measurement. Small particles of San Carlos olivine and Burma spinel were pressed into the Au foil for use as standards to correct for instrumental mass fractionation. The detection system was configured for multicollection, with 16O measured on a Faraday cup, and 17O and 18O measured on electron multipliers (EMs). Individual analyses consisted of 15 cycles of 10 seconds per cycle. Additionally, two microtome thin sections were measured for H isotopic compositions with the JSC NanoSIMS 50L ion probe. An 8 picoangstrom, 16 kiloelectronvolt Cs plus primary beam was used. Measurements consisted of H, C, 12C, 16O, and 18O collected with EMs in multicollection. Terrestrial biotite and kerogen were used for isotopic standards. A significant challenge in O isotope measurement of hydrated minerals is the interference from 16OH at mass 17O. We ensured that the 17O and 16OH peaks were fully resolved by using a mass resolution of greater than 7000 and by careful analyses of San Carlos olivine, Burma spinel and chlorite hydrated mineral standards. The hydride was further suppressed with a cold finger attached to an LN2 dewar to trap volatiles in the sample chamber. All sputtered ions were counted (i.e. presputtering was not used); after applying background, yield and deadtime corrections, we performed a change-point analysis on our data via R in order to determine when the sample reached sputtering equilibrium; data points collected prior to the change point were excluded. Change-point analysis was also used to determine whether the IDP had completely sputtered. Results: Mineralogy. IDPs C35 and E46 exhibited hydrated mineralogies, Fe-Ni sulfide grains, nanoglobules and occasional enstatite grains distributed throughout a fine-grained Mg-Fe saponite matrix. C35 also contained breunnerite (Mg,Fe)CO3; solar flare tracks were observed in enstatite, indicating minimal atmospheric entry heating. The mineralogy of D46 is dominated by a large FeS grain with a minor component of adhering silicate material. D46 was strongly heated during atmorpheric entry as evidenced by a well-developed magnetite rim. EPMA analyses show that both C35 and E46 have high carbon contents of 20 weight percentage (approximately 6X CI). D46 contains approximately 6 wt.weight percentage C. A significant amount of the carbon is present as carbon nanoglobules. Results: Hydrogen isotopes: Although the bulk delta D values of both sections of L2079C35 were within error of SMOW (minus 33 plus or minus 19 per mille, 1 plus or minus 14 per mille 1 sigma), several delta D-rich hotspots were also identified, reaching 2000 per mille. As shown in Fig. 1, these hotspots are clearly associated with discrete carbonaceous inclusions that are akin to nanoglobules found in many meteorites and other IDPs. Oxygen Isotopes. Results of the oxygen isotope measurements are shown in Figure 1. The oxygen isotope composition for L2079C35 was delta 18O equals plus11.6 plus or minus 1.9per mille, delta 17O equals plus 7.9 plus or minus 1.9per mille (2 standard errors). The oxygen isotope composition for L2083D46 was delta 18O equals minus 8.1 plus or minus 1.9 per mille, delta 17O equals minus 6.4 plus or minus 3.1 per mille (2 standard errors). The oxygen isotope composition for L2083E46 was delta 18O equals plus 12.0 plus or minus 1.9 per mille, delta 17O equals plus 9.2 plus or minus 2.0 per mille (2 standard errors). Discussion: Despite mineralogical similarities to highly aqueously altered carbonaceous chondrites, the hydrated IDPs we analyzed have oxygen isotopic compositions that are distinct from matrix materials in the CI, CM, and CR chondrites. The IDPs plot along the Young-Russell line, with delta 17O values for C35 and E46 suggestive of interaction with a 16O-poor reservoir. However, we have thus far not observed evidence of extreme 16O-poor reservoirs expected from self-shielding models and observed in Acfer 094 simplectite. The high carbon contents of the IDPs also set them apart from known meteoritic samples. The lack of atmospheric entry heating effects are consistent with low encounter velocities and suggest either an asteroidal source, or a low inclination, low eccentricity cometary origin. Conclusions: The unusual oxygen isotopic compositions, high carbon contents, and the abundance of Drich nanoglobules, together, suggest that the high-carbon, hydrated IDPs are derived from a primitive source that is not yet represented in meteorite collections.

Snead, C. J.↗
NASA NTRS2004

Constraints on the Lithological Variation near the Surface of the HED Planetoid from the Petrology of 91 & 92 Series Antarctic Achondrites

The petrography of a suite of meteorite sections: PCA91006,14; PCA91078,9; PCA91083,6; PCA91159,4; PCA91179,9; PCA91245,9; EET92003,14; EET92004,12; EET92015,4; EET92022,7; EET92026,4; and EET92027,5 is used as an initial sample of the lithological variation on the surface of the HED planetoid (presumably asteroid 4 Vesta). These samples will be combined with much larger arrays of petrographic data for the many Antarctic basaltic achondrites to provide a random sample of the surface of the body. The full variety of the lithologies existing on the parent body is only accessible when the polymict achondrites are considered. The polymict samples contain lithologies that sample multiple provenances as well as those not seen as monolithologic meteorites like eucrites and diogenites. Comparison of lithological variation within individual meteorites provides a subset of variations at the site of last impact. In aggregate, the variations within the achondrites now available may be close to a random sample of the parent body. In combination of microanalytical and imaging techniques now available permit a mass balanced assessment of the distribution and abundance of lithologies to be made. These initial results provide a description of methodology to be tested. All samples were studied and photographed on a polarizing microscope to provide location information. Major mineral phases and randomly selected points (on lines and grids) were analyzed in each thin section. In addition backscattered electron and X-ray imaging of clasts and sections provide the basis for high precision modal analyses of the abundance and distribution of both lithic and mineral clasts. These data provide objective, area based comparisons with other Antarctic samples.

Bjonnes, Emily E.↗
NASA NTRS2003

Autotrophic Ecosystems on the Early Earth

Ophiolite sequences, sections of lower oceanic crust and upper mantle that have been thrust onto continental craton, are located in northern and central California and provide easily accessible areas that serve as good analogs for similar, more extensive areas of the early Earth. We have begun investigating and characterizing these sites in order to understand better the processes that may be responsible for the water chemistry, mineralogy and biology of similar environments on the early Earth. The geophysical and geochemical processes in these terranes provide niches for unique communities of extremeophiles and likely provide a good analog to the location that first gave rise to life on Earth. The ophiolites found in northern and central California include the Trinity, Josephine, Coast Range and Point Sal, all of which are approximately 160 million years old. Fluids from serpentinizing springs are generally alkaline with high pH and H2 contents, indicating that the mafic rock compositions control the fluid composition through water-rock reactions during relatively low-grade hydrothermal processes. There are significant amounts of primary mineralogy remaining in the rocks, meaning that substantial alteration processes are still occurring in these terranes. The general reaction for serpentinization of olivine is given by one of the authors. olivine + H2O = serpentine + brucite + magnetite + H2. We have analyzed the mineralogical composition of several rock samples collected from the Coast Range Ophiolite near Clear Lake, CA by electron microprobe. The remnant primary mineralogy is fairly urnform in composition, with an olivine composition of Fo(sub 90), and with pyroxene compositions of En(sub 90) for orthopyroxene and En(sub 49)Wo(sub 48)Fs(sub 03) for the clinopyroxene. Other primary phases observed include chromites and other spinels. Examination of petrographic thin sections reveals that serpentinization reactions have occurred in these locations. The serpentine resulting from aqueous alteration of olivine resides in veins that are see to cross cut the primary mineral grains. There are several generations of alteration products, comprised mostly of serpentines that are magnesium rich, with magnetite, brucite and carbonates observed as accessory minerals. The formation of carbonates can be taken to indicate the presence of CO2 in the altering fluids. We collected samples from a spring in the Coast Range Ophiolite in order to determine whether the geochemical environment serves as a habitat for chemotrophic microorganisms. DNA was extracted from the sediment samples and the 16s rRNA gene was PCR amplified using universal Archaeal primers. Denaturing gradient gel electrophoresis (DGGE) was used to determine the community of Archaea thriving in these samples. Our results indicate that there were 8 different genera of Archaea from a single sample. A sequence was obtained from one of these eight. The sequence is of an organism similar to Halorubrum tibetense, and alkalophilic Archaeon. This result suggests that these environments are likely hosts for communities of organisms that are adapted for the unique chemistry provided by the alkaline spring.

Schulte, M.↗