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At least 145 records · Page 8

FE-SEM, FIB and TEM Study of Surface Deposits of Apollo 15 Green Glass Volcanic Spherules

Surface deposits on lunar pyroclastic green (Apollo 15) and orange (Apollo 17) glass spherules have been attributed to condensation from the gas clouds that accompanied fire-fountain eruptions. The fire fountains cast molten lava high above the lunar surface and the silicate melt droplets quenched before landing producing the glass beads. Early investigations showed that these deposits are rich in sulfur and zinc. The deposits are extremely fine-grained and thin, so that it was never possible to determine their chemical compositions cleanly by SEM/EDX or electron probe x-ray analysis because most of the excited volume was in the under-lying silicate glass. We are investigating the surface deposits by TEM, using focused ion beam (FIB) microscopy to extract and thin the surface deposits. Here we report on chemical mapping of a FIB section of surface deposits of an Apollo green glass bead 15401using the ultra-high resolution JEOL 2500 STEM located at NASA Johnson Space Center.

Ross, Daniel K.↗

Experimental Space Weathering of Ordinary Chondrites by Nanopulse Laser: TEM Results

A set of ordinary chondrite meteorites has been subjected to artificial space weathering by nanopulse laser to simulate the effects of micrometeorite bombardment. Three meteorites, an H (Ehole), L (Chateau Renard - CR), and LL (Appley Bridge - AB) were lasered following the method of Sasaki et al [1]. Near IR spectra were taken before and after exposure to examine the optical changes induced and the samples were examined by scanning and transmission electron microscopy (SEM and TEM) to understand the physical changes.

Noble, S. K.↗

SEM and TEM Observation of the Surfaces of the Fine-Grained Particles Retrieved from the Muses-C Regio on the Asteroid 25413 Itokawa

Surface materials on airless solar system bodies exposed to interplanetary space are gradually changed their visible to near-infrared reflectance spectra by the process called "space weathering", which makes the spectra darker and redder. Hapke et al. proposed a model of space weathering: vapor deposition of nanophase reduced iron (npFe(sup 0)) on the surfaces of the grains within the very surface of lunar regolith. This model has been proved by detailed observation of the surfaces of the lunar soil grains by transmission electron microscope (TEM). They demonstrated that npFe(sup 0) was formed by a combination of vapor deposition and irradiation effects. In other words, both micrometeorite impacts and irradiation by solar wind and galactic cosmic ray play roles on the space weathering on the Moon. Because there is a continuum of reflectance spectra from those of Q-type asteroids (almost the same as those of ordinary chondrites) to those of S-type asteroids, it is strongly suggested that reflectance spectra of asteroids composed of ordinary chondrite-like materials were modified over time to those of S-type asteroids due to space weathering. It is predicted that a small amount of npFe(sup 0) on the surface of grains in the asteroidal regolith composed of ordinary chondrite-like materials is the main agent of asteroidal space weathering.

Noguchi, T.↗

In-Situ TEM-STM Observations of SWCNT Ropes/Tubular Transformations

Single-walled carbon nanotubes (SWCNTs) prepared by the HiPco process were purified using a modified gas phase purification technique. A TEM-STM holder was used to study the morphological changes of SWCNT ropes as a function of applied voltage. Kink formation, buckling behavior, tubular transformation and eventual breakdown of the system were observed. The tubular formation was attributed to a transformation from SWCNT ropes to multi-walled carbon nanotube (MWCNT) structures. It is likely mediated by the patching and tearing mechanism which is promoted primarily by the mobile vacancies generated due to current-induced heating and, to some extent, by electron irradiation.

Sola, F.↗

High-Resolution and Analytical TEM Investigation of Space Radiation Processing Effects in Primitive Solar System Materials and Airless Planetary Surface Environments

Energetic ions present in the diverse plasma conditions in space play a significant role in the formation and modification of solid phases found in environments ranging from the interstellar medium (ISM) to the surfaces of airless bodies such as asteroids and the Moon. These effects are often referred to as space radiation processing, a term that encompasses changes induced in natural space-exposed materials that may be only structural, such as in radiation-induced amorphization, or may involve ion-induced nanoscale to microscale chemical changes, as occurs in preferential sputtering and ion-beam mixing. Ion sputtering in general may also be responsible for partial or complete erosion of space exposed materials, in some instances possibly bringing about the complete destruction of free-floating solid grains in the ISM or in circumstellar nebular dust clouds. We report here on two examples of the application of high-resolution and analytical transmission electron microscopy (TEM) to problems in space radiation processing. The first problem concerns the role of space radiation processing in controlling the overall fate of Fe sulfides as hosts for sulfur in the ISM. The second problem concerns the known, but as yet poorly quantified, role of space radiation processing in lunar space weathering.

Christoffersen, R.↗

TEM Observation of the Ti Interlayer Between SiC Substrates During Diffusion Bonding

Diffusion bonding was carried out to join SiC to SiC substrates using titanium interlayers. In this study, 10 m and 20 m thick physical vapor deposited (PVD) Ti surface coatings, and 10 and 20 m thick Ti foils were used. Diffusion bonding was performed at 1250 C for PVD Ti coatings and 1200 C for Ti foil. This study investigates the microstructures of the phases formed during diffusion bonding through TEM and selected-area diffraction analysis of a sample prepared with an FIB, which allows samples to be taken from the reacted area. In all samples, Ti3SiC2, Ti5Si3Cx and TiSi2 phases were identified. In addition, TiC and unknown phases also appeared in the samples in which Ti foils were used as interlayers. Furthermore, Ti3SiC2 phases show high concentration and Ti5Si3Cx formed less when samples were processed at a higher temperature and thinner interlayer samples were used. It appears that the formation of microcracks is caused by the presence of intermediate phase Ti5Si3Cx, which has anisotropic thermal expansion, and by the presence of an unidentified Ti-Si-C ternary phase with relatively low Si content.

Tsuda, Hiroshi↗

Solar Ion Processing of Major Element Surface Compositions of Mature Mare Soils: Insights from Combined XPS and Analytical TEM Observations

Solar wind ions are capable of altering the sur-face chemistry of the lunar regolith by a number of mechanisms including preferential sputtering, radiation-enhanced diffusion and sputter erosion of space weathered surfaces containing pre-existing compositional profiles. We have previously reported in-situ ion irradiation experiments supported by X-ray photoelectron spectroscopy (XPS) and analytical TEM that show how solar ions potentially drive Fe and Ti reduction at the monolayer scale as well as the 10-100 nm depth scale in lunar soils [1]. Here we report experimental data on the effect of ion irradiation on the major element surface composition in a mature mare soil.

Christoffersen, R.↗

A Microanalytical (TEM) Study of Fine-grained Chondrule Rims in NWA 5717

Northwest Africa (NWA) 5717 is a highly primitive ordinary chondrite of petrologic type 3.05 with ubiquitous fine-grained chondrule rims [1, 2]. Rims appear around approximately 60% of chondrules and are comprised of micron-sized mineral and lithic fragments and microchondrules that are embdedded in an FeO-rich submicron groundmass that compositionally resembles fayalitic olivine. Some rim clasts appear overprinted with FeO-rich material, suggesting secondary alteration that postdates rim formation. Here we present a microanalytical (TEM) study of the submicron component (i.e. the groundmass) of the rims in order to determine the crystal structures and compositions of their constituent phases and decipher the accretion and alteration history recorded in rims.

Bigolski, J. N.↗

A Survey of Jet Aircraft PM by TEM in APEX III

Based upon field testing during the NASA led APEX III campaign conducted in November 2005 at the NASA Glenn Research Center in coordination with Continental Airlines and Cleveland Hopkins International Airport. This paper reports observations of particulate emissions collected from a suite of jet engine aircraft to assess differences and similarities in soot macro- micro- and nanostructure using transmission electron microscopy (TEM). Aggregates are compact, primary particle sizes varied and nanostructure mixed. Comparisons are made to more familiar laboratory flame-generated soot as a well-studied point of reference. Results are interpreted in terms of turbulence interacting with the different stages of particle formation and growth.

soot↗

A TEM Investigation of the Fine-Grained Matrix of the Martian Basaltic Breccia NWA 7034

The martian basaltic breccia NWA 7034 is characterized by fine-grained groundmass containing several different types of mineral grains and lithologic clasts. The matrix composition closely resembles Martian crustal rock and soil composition measured by recent rover and orbiter missions. The first results of NWA 7034 suggest that the brecciation of this martian meteorite may have formed due to eruptive volcanic processes; however, impact related brecciation processes have been proposed for paired meteorites NWA 7533 and NWA 7475]. Due to the very fine grain size of matrix, its textural details are difficult to resolve by optical and microprobe observations. In order to examine the potential nature of brecciation, transmission electron microscopy (TEM) studies combined with focused ion-beam technique (FIB) has been undertaken. Here we present the preliminary observations of fine-grained groundmass of NWA 7034 from different matrix areas by describing its textural and mineralogical variations and micro-structural characteristics.

Muttik, N.↗

Problems at the Leading Edge of Space Weathering as Revealed by TEM Combined with Surface Science Techniques

Both transmission electron micros-copy (TEM) and surface analysis techniques such as X-ray photoelectron spectroscopy (XPS) were instrumen-tal in making the first characterizations of material generated by space weathering in lunar samples [1,2]. Without them, the nature of nanophase metallic Fe (npFe0) correlated with the surface of lunar regolith grains would have taken much longer to become rec-ognized and understood. Our groups at JSC and UVa have been using both techniques in a cross-correlated way to investigate how the solar wind contributes to space weathering [e.g., 3]. These efforts have identified a number of ongoing problems and knowledge gaps. Key insights made by UVa group leader Raul Barag-iola during this work are gratefully remembered.

Christoffersen, R.↗

Compositional and Microstructural Evolution of Olivine Under Multiple-Cycle Pulsed Laser Irradiation as Revealed by FIB/Field-Emission TEM

The use of pulsed laser irradiation to simulate the short duration, high-energy conditions characteristic of micrometeorite impacts is now an established approach in experimental space weathering studies. The laser generates both melt and vapor deposits that contain nanophase metallic Fe (npFe(sup 0)) grains with size distributions and optical properties similar to those in natural impact-generated melt and vapor deposits. There remains uncertainty, however, about how well lasers simulate the mechanical work and internal (thermal) energy partitioning that occurs in actual impacts. We are currently engaged in making a direct comparison between the products of laser irradiation and experimental/natural hypervelocity impacts. An initial step reported here is to use analytical SEM and TEM is to attain a better understanding of how the microstructure and composition of laser deposits evolve over multiple cycles of pulsed laser irradiation.

Christoffersen, R.↗

TEM Analyses of Itokawa Regolith Grains and Lunar Soil Grains to Directly Determine Space Weathering Rates on Airless Bodies

Samples returned from the moon and Asteroid Itokawa by NASA's Apollo Missions and JAXA's Hayabusa Mission, respectively, provide a unique record of their interaction with the space environment. Space weathering effects result from micrometeorite impact activity and interactions with the solar wind. While the effects of solar wind interactions, ion implantation and solar flare particle track accumulation, have been studied extensively, the rate at which these effects accumulate in samples on airless bodies has not been conclusively determined. Results of numerical modeling and experimental simulations do not converge with observations from natural samples. We measured track densities and rim thicknesses of three olivine grains from Itokawa and multiple olivine and anorthite grains from lunar soils of varying exposure ages. Samples were prepared for analysis using a Leica EM UC6 ultramicrotome and an FEI Quanta 3D dual beam focused ion beam scanning electron microscope (FIB-SEM). Transmission electron microscope (TEM) analyses were performed on the JEOL 2500SE 200kV field emission STEM. The solar wind damaged rims on lunar anorthite grains are amorphous, lack inclusions, and are compositionally similar to the host grain. The rim width increases as a smooth function of exposure age until it levels off at approximately 180 nm after approximately 20 My (Fig. 1). While solar wind ion damage can only accumulate while the grain is in a direct line of sight to the Sun, solar flare particles can penetrate to mm-depths. To assess whether the track density accurately predicts surface exposure, we measured the rim width and track density in olivine and anorthite from the surface of rock 64455, which was never buried and has a surface exposure age of 2 My based on isotopic measurements. The rim width from 64455 (60-70nm) plots within error of the well-defined trend for solar wind amorphized rims in Fig. 1. Measured solar flare track densities are accurately reflecting the surface exposure of the grains. Track densities correlate with the amorphous rim thicknesses. While the space-weathered rims of anorthite grains are amorphous, the space-weathered rims on both Itokawa and lunar olivine grains show solar wind damaged rims that are not amorphous. Instead, the rims are nanocrystalline with high dislocation densities and sparse inclusions of nanophase Fe metal. The rim thicknesses on the olivine grains also correlate with track density. The Itokawa olivine grains have track densities that indicate surface exposures of approximately 10(exp 5) years. Longer exposures (up to approximately 10(exp 7) years) do not amorphize the rims, as evidenced by lunar soil olivines with high track densities (approximately 10(exp 11) cm(exp -2)). From the combined data, shown in Fig. 1, it is clear that olivine is damaged (but not amorphized) more rapidly by the solar wind compared to anorthite. The olivine damaged rim forms quickly (in approximately 10(exp 6) y) and saturates at approximately 120nm with longer exposure time. The anorthite damaged rims form more slowly, amorphize, and grow thicker than the olivine rims. This is in agreement with numerical modeling data which predicts that solar wind damaged rims on anorthite will be thicker than olivine. However, the models predict that both olivine and anorthite rims will amorphize and reach equilibrium widths in less than 10(exp 3) y, in contrast to what is observed for natural samples. Laboratory irradiation experiments, which show rapid formation of fully amorphous and blistered surfaces from simulated solar wind exposures are also in contrast to observations of natural samples. These results suggest that there is a flux dependence on the type and extent of irradiation damage that develops in olivine. This flux dependence suggests that great caution be used in extrapolating between high-flux laboratory experiments and the natural case, as demonstrated by. We constrain the space weathering rate through analysis of returned samples. Provided that the track densities and the solar wind damaged rim widths exhibited by the Itokawa grains are typical of the fine-grained regions of Itokawa, then the space weathering rate is on the order of 10(exp 5) y. Space weathering effects in lunar soils saturate within a few My of exposure while those in Itokawa regolith grains formed in approximately 10(exp 5) y. Olivine and anorthite respond differently to solar wind irradiation. The space weathering effects in olivine are particularly difficult to reconcile with laboratory irradiation studies and numerical models. Additional measurements, experiments, and modeling are required to resolve the discrepancies among the observations and calculations involving solar wind amorphization of different minerals on airless bodies.

Berger, Eve L.↗

Visualizing time-dependent microstructural and chemical evolution during molten salt corrosion of Ni-20Cr model alloy using correlative quasi in situ TEM and in situ synchrotron X-ray nano-tomography

In situ monitoring of corrosion processes is important to fundamentally understand the kinetics and evolution of materials in harsh environments. A quasi in situ transmission electron microscopy technique was utilized to study microstructural and chemical evolution of a Ni-20Cr disc sample 6 exposed to molten KCl-MgCl 2 salt for 60 s in consecutive 20 s iterations. In situ synchrotron X-ray nano-tomography was performed to characterize the morphological evolution of a Ni-20Cr microwire exposed to molten KCl-MgCl 2 . Here, both techniques captured key corrosion events and revealed mechanisms at different time and length scales, potentially bringing greater insights and 10 deeper understanding beyond conventional analysis.

36 MATERIALS SCIENCE↗

Microstructure and phase evolution in the U-10Zr fuel investigated by in situ TEM heating experiments

The development of U-Zr metallic nuclear fuel for fast spectrum reactors is impacted by a lack of mechanistic understanding of the fuel behavior evolution under thermal irradiation conditions, despite previous works providing substantial fuel performance data. This work uses in-situ transmission electron microscopy heating experiments to study phase and microstructural evolution in several unirradiated U-10Zr specimens during rapid heating ramps (from room temperature to 1000 °C). The starting a-U + bcc-(Zr, U) eutectic microstructure began to decompose above 600 °C. The decomposition initiated from the bcc (U,Zr) phase. Similar results were observed for all specimens even when fabricated by different routes (e.g., cold rolled or annealed). As a result, the impact of observed microstructure and phase evolutions at high temperatures on fuel fabrication and in-pile fuel transient test was also discussed.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗