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At least 73 records · Page 4

Oxidation of metals and alloys in controlled atmospheres using in situ transmission electron microscopy and Auger spectrography

Single-crystalline thin films of copper were oxidized at an isothermal temperature of 425 C and at an oxygen partial pressure of .005 Torr in situ in a high-resolution electron microscope. The specimens were prepared by epitaxial vapor deposition onto polished 100 and 110 faces of rocksalt and mounted in a hot stage inside an ultra-high-vacuum specimen chamber of the microscope. Large amounts of sulfur, carbon, and oxygen were detected by Auger electron spectroscopy on the surface of the as-received films and were removed in situ by ion-sputter etching immediately prior to the oxidation. The nucleation and growth characteristics of Cu2O on Cu were studied. Results show that neither stacking faults nor dislocations are associated with the Cu2O nucleation sites. The growth of Cu2O nuclei is linear with time. The experimental findings, including results from oxygen dissolution experiments and from repetitive oxidation-reduction-oxidation sequences, fit well into the framework of an oxidation process involving (a) the formation of a surface-charge layer, (b) oxygen saturation in the metal and (c) nucleation, followed by surface diffusion of oxygen and bulk diffusion of copper for lateral and vertical oxide growth, respectively.

Rao, D. B.↗

Immunohistochemical myofiber typing and high-resolution myofibrillar lesion detection in LR white embedded muscle

We have developed a method of fixing, embedding, sectioning, and staining that allows high-resolution detection of myofibrillar structure and myosin immunocytochemical muscle fiber typing in serial semithin sections of LR White plastic embedded muscle at the light microscopic level. Traditional approaches, such as cryostat sections, permit fiber typing, but small myofibrillar lesions (1-3 sarcomeres) are difficult to detect because of section thickness. Semithin sections of hydrophobic resins do not stain well either histochemically or immunocytochemically. Electron microscopy can resolve lesions and discriminate fiber types based on morphology, but the sampling area is small. Our goal was to develop a rapid method for defining both fiber type and high-resolution primary myofibrillar lesion damage. Mild fixation (1-4% paraformaldehyde, 0. 05-0.1% glutaraldehyde) and embedment in a hydrophilic resin (LR White) were used. Myofibrillar structure was extremely well preserved at the light microscopic (LM) level, and lesions could be readily resolved in Toluidine blue stained 500-nm sections. Fiber type was defined by LM immunomyosin staining of serial plastic semithin sections, which demonstrated reciprocal staining patterns for "fast (Sigma M4276) and "total" (skeletal muscle) myosins (Sigma M7523). Copyright 2000 Wiley-Liss, Inc.

NASA Program Fundamental Space Biology↗

Orion Artemis-1 Post-Flight Characterization

This abstract discusses the post-flight characterization of the heatshield used in the Orion Artemis-1 mission, which is a significant milestone in human space exploration. The Artemis-1 heatshield is a crucial component designed to protect the spacecraft during re-entry into Earth's atmosphere. It experiences extreme temperatures and forces as it encounters the intense heat generated by the friction between the spacecraft and the atmospheric gases. The post-flight characterization of the Artemis-1 heatshield involves analyzing its surface morphology and elemental composition. This analysis provides valuable insights into the performance and durability of the heatshield during the mission. By utilizing techniques such as Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Spectroscopy (EDX), a detailed examination of the heatshield’s surface features, and elemental composition can be conducted. The SEM analysis offers high-resolution imaging capabilities, enabling detailed observations of the heatshield’s surface morphology. EDX analysis provides elemental analysis, allowing for an assessment of any compositional changes induced by the thermal and environmental conditions experienced during the mission. This information is crucial for understanding the material's response to the extreme conditions and identifying any potential issues or degradation. Furthermore, density profiling analysis is performed to measure density variations across the depth of the heatshield material. This analysis offers insights into the effects of the mission on the heatshield, such as potential ablation, or changes in material porosity. Understanding these density variations helps to evaluate the heatshield's structural integrity and its ability to withstand future missions. This knowledge contributes to the ongoing development of advanced heatshield designs, enhancing their thermal protection capabilities and ensuring the safety of future manned missions to the Moon and beyond.

Tane Boghozian↗

Analytical electron microscopy of extraterrestrial materials - Results from microtome sections of carbonaceous chondrites and interplanetary dust particles

The paper describes a method for embedding, sectioning, and observing two types of extraterrestrial materials, including hydrated interplanetary dust particles (IDPs) and carbonaceous chondrite meteorites. The technique, which produces large thin areas suitable for both high-resolution imaging and thin-film microanalysis, was applied to study the petrology of the IDP Ames-DE C86-11, the Murchison carbonaceous chondrite matrix, and the Allende dark inclusion. The technique makes it possible to maintain delicate interfaces, boundaries, and phase relationships between grains. Because phases are held in place, layer lattice silicates and other minerals with strong preferred orientations can be viewed in any orientation, including the orientation normal to their basal planes.

Blake, D. F.↗

Physical and Chemical Characterization of Particles in the Upper Troposphere and Lower Stratosphere: Microanalysis of Aerosol Impactor Samples

Herein is reported activities to support the characterization of the aerosol in the upper troposphere (UT) and lower stratosphere (LS) collected during the Airborne Southern Hemisphere Ozone Experiment/Measurements for Assessing the Effects of Stratospheric Aircraft (ASHOE/MAESA) missions in 1994. Through a companion proposal, another group was to measure the size distribution of aerosols in the 0.008 to 2 micrometer diameter range and to collect for us impactor samples of particles larger than about 0.02 gm. In the first year, we conducted laboratory studies related to particulate deposition patterns on our collection substrates, and have performed the analysis of many ASHOE/MAESA aerosol samples from 1994 using analytical electron microscopy (AEM). We have been building an "aerosol climatology" with these data that documents the types and relative abundances of particles observed at different latitudes and altitudes. The second year (and non-funded extension periods) saw continued analyses of impactor aerosol samples, including more ASHOE/MAESA samples, some northern hemisphere samples from the NASA Stratospheric Photochemistry Aerosols and Dynamics Expedition (SPADE) program for comparison, and a few aerosol samples from the NASA Stratospheric TRacers of Atmospheric Transport (STRAT) program. A high-resolution field emission microscope was used for the analysis and re-analysis of a number of samples to determine if this instrument was superior in performance to our conventional electron microscope. In addition, some basic laboratory studies were conducted to determine the minimum detectable and analyzable particle size for different types of aerosols. In all, 61 aerosol samples were analyzed, with a total of over 30,000 individual particle analyses. In all analyzed samples, sulfate particles comprised the major aerosol number fraction. It must be stressed that particles composed of more than one species, for example sulfate and organic carbon, were classified according to the major fraction. Thus, many of the particles classified as sulfate may have contained significant mass fractions of carbonaceous or other material. These particles for the most part did not show two physical phases, however. Nonsulfate particles were classified according to the physical and chemical characteristics of each particle, and were grouped into the major nonsulfate particle classes, including C-rich, crustal, metallic, and salts. Our UT and LS sample analyses indicate a maximum for crustal and C-rich particle abundance in the Northern Hemisphere upper troposphere, and a salt particle maximum in the Southern Hemisphere upper troposphere. Metallic particles are clearly more prevalent in the troposphere than in the stratosphere, but interhemispheric differences appear small.

Sheridan, Patrick J.↗

Transmission electron microscopy of composites

Since interphase-interfaces are often both the structurally weakest and chemically least stable regions of a composite material, they are critical determinants of such macrostructural characteristics as tensile strength and fracture toughness. Attention is presently given to the use of TEM for the study of interfaces between dissimilar materials; electron-diffraction, analytical, and high-resolution forms of TEM are employed, for the cases of both structural and semiconductor composites. The materials studied are SiC/Si, GaP/Si, and SiC fiber- and whisker-reinforced Si3N4.

Pirouz, P.↗

Vapor Growth and Characterization of Cr-Doped ZnSe Crystals

Cr-doped ZnSe single crystals were grown by a self-seeded physical vapor transport technique in both vertical (stabilized) and horizontal configurations. The source materials were mixtures of ZnSe and CrSe. Growth temperatures were in the range of 1140-1150 C and the furnace translation rates were 1.9-2.2 mm/day. The surface morphology of the as-grown crystals was examined by scanning electron microscopy (SEM) and atomic force microscopy (AFM). Different features of the as-grown surface of the vertically and horizontally grown crystals suggest that different growth mechanisms were involved in the two growth configurations. The [Cr] doping levels were determined to be in the range of 1.8-8.3 x 10 (exp 19) cm (exp -3) from optical absorption measurements. The crystalline quality of the grown crystals were examined by high-resolution triple-crystal X-ray diffraction (HRTXD) analysis.

Su, Ching-Hua↗

Ballistic-Electron-Emission Microscope

Ballistic-electron-emission microscope (BEEM) employs scanning tunneling-microscopy (STM) methods for nondestructive, direct electrical investigation of buried interfaces, such as interface between semiconductor and thin metal film. In BEEM, there are at least three electrodes: emitting tip, biasing electrode, and collecting electrode, receiving current crossing interface under investigation. Signal-processing device amplifies electrode signals and converts them into form usable by computer. Produces spatial images of surface by scanning tip; in addition, provides high-resolution images of buried interface under investigation. Spectroscopic information extracted by measuring collecting-electrode current as function of one of interelectrode voltages.

Kaiser, William J.↗

Microstructural Constraints on the Formation of Diamond in Ureilites, the Case from the Kenna Meteorite

The origin of diamonds in ureilitic meteorites, a major family of ultramafic achondrites, has long been debated, with various formation mechanisms inferred, including: 1) shock conversion of preexisting graphite due to a hypervelocity impact on the ureilite parent body; 2) vapor deposition during condensation of the solar nebula; or 3) static transformation in the mantle of a large planetesimal (>1000 km in diameter). The Kenna ureilite is a 10.9 kg stone that was found in Kansas in 1972 and is dominantly composed of olivine and pigeonite (68% and 22% modal abundance, respectively), together with minor metal and carbon-rich regions. Within the carbon-rich domains researchers have identified microdiamonds up to ~10 µm in size. Due to the proximity of the extremely hard microdiamonds with soft graphite and moderately hard silicates, achieving an appropriately flat surface for electron backscatter diffraction (EBSD) analysis has proved challenging. We have, therefore, employed a Hitachi ArBlade 5000 broad beam Ar ion milling system to prepare a sample with an adequate surface uniformity. The ion milling dramatically improved indexing of the EBSD patterns and facilitated high-resolution microstructural analysis of the carbon-rich domains. The carbon-bearing regions occur as tabular domains between polygonal olivine and pigeonite, and are composed of aggregates of micrometer-scale diamond with intermediate graphite, oxides and metal grains. Within the microdiamonds, {111} twins are abundant, many of which form ragged lamellae consistent with mechanical twinning. The microdiamond assemblages appear to pseudomorph tabular graphite habits, which together with the abundant deformation twins, supports a shock transformation mechanism for microdiamond formation within the Kenna meteorite. To compliment the EBSD microstructural analyses, coordinated laser Raman, focused ion beam/transmission electron microscopy imaging and diffraction data, and NanoSIMS N and C tomographic isotopic imaging will be collected. These data will provide further constraints on the formation of diamonds within ureilites.

Timmons M Erickson↗

Mud Volcanoes - Analogs to Martian Cones and Domes (by the Thousands!)

Mud volcanoes are mounds formed by low temperature slurries of gas, liquid, sediments and rock that erupt to the surface from depths of meters to kilometers. They are common on Earth, with estimates of thousands onshore and tens of thousands offshore. Mud volcanoes occur in basins with rapidly-deposited accumulations of fine-grained sediments. Such settings are ideal for concentration and preservation of organic materials, and mud volcanoes typically occur in sedimentary basins that are rich in organic biosignatures. Domes and cones, cited as possible mud volcanoes by previous authors, are common on the northern plains of Mars. Our analysis of selected regions in southern Acidalia Planitia has revealed over 18,000 such features, and we estimate that more than 40,000 occur across the area. These domes and cones strongly resemble terrestrial mud volcanoes in size, shape, morphology, associated flow structures and geologic setting. Geologic and mineralogic arguments rule out alternative formation mechanisms involving lava, ice and impacts. We are studying terrestrial mud volcanoes from onshore and submarine locations. The largest concentration of onshore features is in Azerbaijan, near the western edge of the Caspian Sea. These features are typically hundreds of meters to several kilometers in diameter, and tens to hundreds of meters in height. Satellite images show spatial densities of 20 to 40 eruptive centers per 1000 square km. Many of the features remain active, and fresh mud flows as long as several kilometers are common. A large field of submarine mud volcanoes is located in the Gulf of Cadiz, off the Atlantic coasts of Morocco and Spain. High-resolution sonar bathymetry reveals numerous km-scale mud volcanoes, hundreds of meters in height. Seismic profiles demonstrate that the mud erupts from depths of several hundred meters. These submarine mud volcanoes are the closest morphologic analogs yet found to the features in Acidalia Planitia. We are also conducting laboratory analyses of surface samples collected from mud volcanoes in Azerbaijan, Taiwan and Japan. X-ray diffraction, visible / near infrared reflectance spectroscopy and Raman spectroscopy show that the samples are dominated by mixed-layer smectite clays, along with quartz, calcite and pyrite. Thin section analysis by optical and scanning electron microscopy confirms the mineral identifications. These samples also contain chemical and morphological biosignatures, including common microfossils, with evidence of partial replacement by pyrite. The bulk samples contain approximately 1 wt% total organic carbon and 0.4 mg / gm volatile hydrocarbons. The thousands of features in Acidalia Planitia cited as analogous to terrestrial mud volcanoes clearly represent an important element in the sedimentary record of Mars. Their location, in the distal depocenter for massive Hesperian-age floods, suggests that they contain fine-grained sediments from a large catchment area in the martian highlands. We have proposed these features as a new class of exploration target that can provide access to minimally-altered material from significant depth. By analogy to terrestrial mud volcanoes, these features may also be excellent sites for the sampling martian organics and subsurface microbial life, if such exist or ever existed.

Allen, Carlton C.↗

Structural Characterization of Lateral-grown 6H-SiC am-plane Seed Crystals by Hot Wall CVD Epitaxy

The performance of commercially available silicon carbide (SiC) power devices is limited due to inherently high density of screw dislocations (SD), which are necessary for maintaining polytype during boule growth and commercially viable growth rates. The NASA Glenn Research Center (GRC) has recently proposed a new bulk growth process based on axial fiber growth (parallel to the c-axis) followed by lateral expansion (perpendicular to the c-axis) for producing multi-faceted m-plane SiC boules that can potentially produce wafers with as few as one SD per wafer. In order to implement this novel growth technique, the lateral homoepitaxial growth expansion of a SiC fiber without introducing a significant number of additional defects is critical. Lateral expansion is being investigated by hot wall chemical vapor deposition (HWCVD) growth of 6H-SiC am-plane seed crystals (0.8mm x 0.5mm x 15mm) designed to replicate axially grown SiC single crystal fibers. The post-growth crystals exhibit hexagonal morphology with approximately 1500 m (1.5 mm) of total lateral expansion. Preliminary analysis by synchrotron white beam x-ray topography (SWBXT) confirms that the growth was homoepitaxial, matching the polytype of the respective underlying region of the seed crystal. Axial and transverse sections from the as grown crystal samples were characterized in detail by a combination of SWBXT, transmission electron microscopy (TEM) and Raman spectroscopy to map defect types and distribution. X-ray diffraction analysis indicates the seed crystal contained stacking disorders and this appears to have been reproduced in the lateral growth sections. Analysis of the relative intensity for folded transverse acoustic (FTA) and optical (FTO) modes on the Raman spectra indicate the existence of stacking faults. Further, the density of stacking faults is higher in the seed than in the grown crystal. Bundles of dislocations are observed propagating from the seed in m-axis lateral directions. Contrast extinction analysis of these dislocation lines reveals they are edge type basal plane dislocations that track the growth direction. Polytype phase transition and stacking faults were observed by high-resolution TEM (HRTEM), in agreement with SWBXT and Raman scattering.

Single Crystal↗

Holographic Optical Data Storage

Although the basic idea may be traced back to the earlier X-ray diffraction studies of Sir W. L. Bragg, the holographic method as we know it was invented by D. Gabor in 1948 as a two-step lensless imaging technique to enhance the resolution of electron microscopy, for which he received the 1971 Nobel Prize in physics. The distinctive feature of holography is the recording of the object phase variations that carry the depth information, which is lost in conventional photography where only the intensity (= squared amplitude) distribution of an object is captured. Since all photosensitive media necessarily respond to the intensity incident upon them, an ingenious way had to be found to convert object phase into intensity variations, and Gabor achieved this by introducing a coherent reference wave along with the object wave during exposure. Gabor's in-line recording scheme, however, required the object in question to be largely transmissive, and could provide only marginal image quality due to unwanted terms simultaneously reconstructed along with the desired wavefront. Further handicapped by the lack of a strong coherent light source, optical holography thus seemed fated to remain just another scientific curiosity, until the field was revolutionized in the early 1960s by some major breakthroughs: the proposition and demonstration of the laser principle, the introduction of off-axis holography, and the invention of volume holography. Consequently, the remainder of that decade saw an exponential growth in research on theory, practice, and applications of holography. Today, holography not only boasts a wide variety of scientific and technical applications (e.g., holographic interferometry for strain, vibration, and flow analysis, microscopy and high-resolution imagery, imaging through distorting media, optical interconnects, holographic optical elements, optical neural networks, three-dimensional displays, data storage, etc.), but has become a prominent am advertising, and security medium as well. The evolution of holographic optical memories has followed a path not altogether different from holography itself, with several cycles of alternating interest over the past four decades. P. J. van Heerden is widely credited for being the first to elucidate the principles behind holographic data storage in a 1963 paper, predicting bit storage densities on the order of 1/lambda(sup 3) with source wavelength lambda - a fantastic capacity of nearly 1 TB/cu cm for visible light! The science and engineering of such a storage paradigm was heavily pursued thereafter, resulting in many novel hologram multiplexing techniques for dense data storage, as well as important advances in holographic recording materials. Ultimately, however, the lack of such enabling technologies as compact laser sources and high performance optical data I/O devices dampened the hopes for the development of a commercial product. After a period of relative dormancy, successful applications of holography in other arenas sparked a renewed interest in holographic data storage in the late 1980s and the early 1990s. Currently, with most of the critical optoelectronic device technologies in place and the quest for an ideal holographic recording medium intensified, holography is once again considered as one of several future data storage paradigms that may answer our constantly growing need for higher-capacity and faster-access memories.

Timucin, Dogan A.↗

High-Resolution Detector For X-Ray Diffraction

Proposed x-ray-sensitive imaging detector offers superior spatial resolution, counting-rate capacity, and dynamic range. Instrument based on laser-stimulated luminescence and reusable x-ray-sensitive film. Detector scans x-ray film line by line. Extracts latent image in film and simultaneously erases film for reuse. Used primarily for protein crystallography. Principle adapted to imaging detectors for electron microscopy and fluorescence spectroscopy and general use in astronomy, engineering, and medicine.

Carter, Daniel C.↗

In situ fatigue loading stage inside scanning electron microscope

A fatigue loading stage inside a scanning electron microscopy (SEM) was developed. The stage allows dynamic and static high-magnification and high-resolution viewing of the fatigue crack initiation and crack propagation processes. The loading stage is controlled by a closed-loop servohydraulic system. Maximum load is 1000 lb (4450 N) with test frequencies ranging up to 30 Hz. The stage accommodates specimens up to 2 inches (50 mm) in length and tolerates substantial specimen translation to view the propagating crack. At room temperature, acceptable working resolution is obtainable for magnifications ranging up to 10,000X. The system is equipped with a high-temperature setup designed for temperatures up to 2000 F (1100 C). The signal can be videotaped for further analysis of the pertinent fatigue damage mechanisms. The design allows for quick and easy interchange and conversion of the SEM from a loading stage configuration to its normal operational configuration and vice versa. Tests are performed entirely in the in-situ mode. In contrast to other designs, the NASA design has greatly extended the life of the loading stage by not exposing the bellows to cyclic loading. The loading stage was used to investigate the fatigue crack growth mechanisms in the (100)-oriented PWA 1480 single-crystal, nickel-based supperalloy. The high-magnification observations revealed the details of the crack growth processes.

Telesman, Jack↗

Dynamical diffraction imaging (topography) with X-ray synchrotron radiation

By contrast to electron microscopy, which yields information on the location of features in small regions of materials, X-ray diffraction imaging can portray minute deviations from perfect crystalline order over larger areas. Synchrotron radiation-based X-ray optics technology uses a highly parallel incident beam to eliminate ambiguities in the interpretation of image details; scattering phenomena previously unobserved are now readily detected. Synchrotron diffraction imaging renders high-resolution, real-time, in situ observations of materials under pertinent environmental conditions possible.

Kuriyama, M.↗

Application of an alkylammonium method for characterization of phyllosilicates in CI chondrites

Many meteorites and interplanetary dust particles (IDP's) with primitive compositions contain significant amounts of phyllosilicates, which are generally interpreted as evidence of protoplanetary aqueous alteration at an early period in the solar system. These meteorites are chondrites of the carbonaceous and ordinary varieties. Characterization of phyllosilicates in these materials is important because of the important physico-chemical information they hold, e.g., from well characterized phyllosilicates, thermodynamic stability relations and hence the conditions of formation of phyllosilicates in the parent body of the meteorite can be predicted. Although we are at a rudimentary level of understanding of the minerals resulting from the aqueous alteration in the early solar nebula, we know that the most common phyllosilicates present in chondritic extraterrestrial materials are serpentines, smectites, chlorites, and micas. The characterization of fine grained minerals in meteorites and IDP's rely heavily on electron beam instruments, especially transmission electron microscopy (TEM). Typically, phyllosilicates are identified by a combination of high resolution imaging of basal spacings, electron diffraction analysis, and chemical analysis. Smectites can be difficult to differentiate from micas because the smectites loose their interlayer water and the interlayers collapse to the same basal spacing as mica in the high vacuum of the TEM. In high-resolution TEM (HRTEM) images, smectite basal spacings vary from 1 nm up to 1.5 nm, while micas show 1 or 2 nm basal spacings. Not only is it difficult to differentiate smectites from micas, but there is no way of identifying different classes of smectites in meteorites and IDP's. To differentiate smectites from micas and also to recognize the charge differences among smectites, an alkylammonium method can be employed because the basal spacings of alkylammonium saturated smectites expand as a function of alkylamine chain length and the layer-charge density of the 2:1 expanding phyllosilicate, and the final product is significantly more stable under electron beam examination. Such a method was tested on standard clays and several meteorite samples using four alkylammonium salts.

Golden, D. C.↗

Convective flow effects on protein crystal growth

A high-resolution microscopic interferometric setup for the monitoring of protein morphologies has been developed. Growth or dissolution of a crystal can be resolved with a long-term depth resolution of 200 A and a lateral resolution of 2 microns. This capability of simultaneously monitoring the interfacial displacement with high local depth resolution has yielded several novel results. We have found with lysozyme that (1) the normal growth rate is oscillatory, and (2) depending on the impurity content of the solution, the growth step density is either greater or lower at the periphery of a facet than in its center. The repartitioning of Na plus and Cl minus ions between lysozyme solutions and crystals was studied for a wide range of crystallization conditions. A nucleation-growth-repartitioning model was developed, to interpret the large body of data in unified way. The results strongly suggest that (1) the ion to lysozyne ratio in the crystal depends mostly on kinetic rather than crystallographic parameters, and (2) lysozyme crystals possess a salt-rich core with a diameter electron microscopy results appear to confirm this finding, which could have far-reaching consequences for x-ray diffraction studies. A computational model for diffusive-convective transport in protein crystallization has been applied to a realistic growth cell geometry, taking into account the findings of the above repartitioning studies and our kinetics data for the growth of lysozyme. The results show that even in the small cell employed, protein concentration nonuniformities and gravity-driven solutal convection can be significant. The calculated convection velocities are of the same order to magnitude as those found in earlier experiments. As expected, convective transport, i.e., at Og, lysozyme crystal growth remains kinetically limited. The salt distribution in the crystal is predicted to be non-uniform at both 1g and 0g, as a consequence of protein depletion in the solution. Static and dynamic light scattering studies in undersaturated and supersaturated solutions have been performed. Diffusivities in undersaturated solutions, were found to vary with lysozyme concentrations. Depending on the salt concentration, the diffusivities either increase or decrease. Interestingly, the corresponding static scattering intensities behave oppositely, Our current analysis indicates that these changes are inconsistent with aggregation in undersaturated solutions. However, the data are compatible with concentration-dependent changes of the interactions between protein and salt.

Rosenberger, Franz↗