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At least 163 records · Page 9

NDE of structural ceramics

Radiographic, ultrasonic, scanning laser acoustic microscopy (SLAM), and thermo-acoustic microscopy techniques were used to characterize silicon nitride and silicon carbide modulus-of-rupture test specimens in various stages of fabrication. Conventional and microfocus X-ray techniques were found capable of detecting minute high density inclusions in as-received powders, green compacts, and fully densified specimens. Significant density gradients in sintered bars were observed by radiography, ultrasonic velocity, and SLAM. Ultrasonic attenuation was found sensitive to microstructural variations due to grain and void morphology and distribution. SLAM was also capable of detecting voids, inclusions and cracks in finished test bars. Consideration is given to the potential for applying thermo-acoustic microscopy techniques to green and densified ceramics. The detection probability statistics and some limitations of radiography and SLAM also are discussed.

Klima, S. J.↗

Study program to develop and evaluate die and container materials for the growth of silicon ribbons

The development and evaluation of proprietary coatings of pure silicon carbide, silicon nitride, and aluminum nitride on less pure hot pressed substrates of the respective ceramic materials, is described. Silicon sessile drop experiments were performed on coated test specimens under controlled oxygen partial pressure. Prior to testing, X-ray diffraction and SEM characterization was performed. The reaction interfaces were characterized after testing with optical and scanning electron microscopy and Auger electron spectroscopy. Increasing the oxygen partial pressure was found to increase the molten silicon contact angle, apparently because adsorbed oxygen lowers the solid-vapor interfacial free energy. It was also found that adsorbed oxygen increased the degree of attack of molten silicon upon the chemical vapor deposited coatings. Cost projections show that reasonably priced, coated, molten silicon resistant refractory material shapes are obtainable.

Addington, L. A.↗

NDE of advanced ceramics

Radiographic, ultrasonic, and scanning laser acoustic microscopy (SLAM) techniques were used to characterize silicon nitride and silicon carbide modulus-of-rupture test specimens in various stages of fabrication. Conventional and microfocus X-ray techniques were found capable of detecting minute high-density inclusions in as-received powders, green compacts, and fully densified specimens. Significant density gradients in sintered bars were observed by radiography, ultrasonic velocity, and SLAM. Ultrasonic attenuation was found sensitive to microstructural variations due to grain and void morphology and distribution. SLAM was capable also of detecting voids, inclusions, and cracks in finished test bars. Consideration is given to the potential for applying thermoacoustic microscopy techniques to green and densified ceramics. Some limitations and the detection probability statistics of the aforementioned nondestructive evaluation (NDE) processes are also discussed.

Klima, S. J.↗

Surface topographical effects on the structural growth of thick sputtered metal and alloy coatings

Thick sputtered S-Monel, silver, and 304 stainless steel coatings were deposited on mica and metal substrates with various surface finishes to investigate the structural growth of the coating by scanning electron microscopy. The geometry and the surface structure of the nodules are characterized. Compositional changes within the coating were analyzed by X-ray dispersion miscroscopy. Defects in the surface finish act as preferential nucleation sites and form isolated and complex nodules and various surface overgrowths in the coating. The nodule boundaries are very vulnerable to chemical etching, and these nodules do not disappear after full annealing. Further, they have undesirable effects on mechanical properties; cracks are initiated at the nodules when the coating is stressed by mechanical forces.

Spalvins, T.↗

Surface characterization in composite and titanium bonding: Carbon fiber surface treatments for improved adhesion to thermoplastic polymers

The effect of anodization in NaOH, H2SO4, and amine salts on the surface chemistry of carbon fibers was examined by X-ray photoelectron spectroscopy (XPS). The surfaces of carbon fibers after anodization in NaOH and H2SO4 were examined by scanning transmission electron microscopy (STEM), angular dependent XPS, UV absorption spectroscopy of the anodization bath, secondary ion mass spectrometry, and polar/dispersive surface energy analysis. Hercules AS-4, Dexter Hysol XAS, and Union Carbide T-300 fibers were examined by STEM, angular dependent XPS, and breaking strength measurement before and after commercial surface treatment. Oxygen and nitrogen were added to the fiber surfaces by anodization in amine salts. Analysis of the plasmon peak in the carbon 1s signal indicated that H2SO4 anodization affected the morphological structure of the carbon fiber surface. The work of adhesion of carbon fibers to thermoplastic resins was calculated using the geometric mean relationship. A correlation was observed between the dispersive component of the work of adhesion and the interfacial adhesion.

Devilbiss, T. A.↗

Nodular growth in thick-sputtered metallic coatings

Thick-sputtered S-Monel, silver, and 304 stainless steel coatings were deposited on mica and metal substrates with various surface finishes to investigate the nodular growth in the coating by scanning electron microscopy. The geometry and the surface structure of the nodules are characterized. Compositional changes within the coating were analyzed by energy dispersive X-ray analysis. Defects in the surface finish (i.e., scratches, inclusions, etc.), act as preferential nucleation sites and form isolated and complex nodules and various surface overgrowths in the coating. The nodule boundaries are very vulnerable to chemical etching and these nodules do not disappear after full annealing. Further, they have undesirable effects on mechanical properties; cracks are initiated at the nodules when the coating is stressed by mechanical forces. These effects are illustrated by micrographs. Nodular growth within a coating can be minimized or eliminated by increasing the surface smoothness.

Spalvins, T.↗

Scanning electron microscope investigation of the structural growth in thick sputtered coatings

Sputtered S-Monel, silver, and 304 stainless steel coatings and molybdenum disulfide coatings were deposited on mica and metal substrates with various surface finishes to investigate the structural growth of the coating by scanning electron microscopy. The geometry and the surface morphology of the nodules are characterized. Compositional changes within the coating were analyzed by energy dispersive X-ray analysis. Defects in the surface finish act as preferential nucleation sites and form isolated overlapping and complex nodules and various unusual surface overgrowths on the coating. The nodule boundaries are very vulnerable to chemical etching and these nodules do not disappear after full annealing. Further, they have undesirable effects on mechanical properties; cracks are initiated at the nodules when the coating is stressed by mechanical forces.

Spalvins, T.↗

A fundamental study of the sticking of insect residues to aircraft wings

The aircraft industry has long been concerned with the increase of drag on airplanes due to fouling of the wings by insects. The present research studied the effects of surface energy and surface roughness on the phenomenon of insect sticking. Aluminum plates of different roughnesses were coated with thin films of polymers with varying surface energies. The coated plates were attached to a custom jig and mounted on top of an automobile for insect collection. Contact angle measurements, X-ray photoelectron spectroscopy and specular reflectance infrared spectroscopy were used to characterize the surface before and after the insect impact experiments. Scanning electron microscopy showed the topography of insect residues on the exposed plates. Moments were calculated in order to find a correlation between the parameters studied and the amount of bugs collected on the plates. An effect of surface energy on the sticking of insect residues was demonstrated.

Eiss, N. S., Jr.↗

Effects of high energy radiation on the mechanical properties of epoxy/graphite fiber composites

Studies on the effects of high energy radiation on graphite fiber reinforced composites are summarized. Studies of T300/5208 and C6000/PMR15 composites, T300 fibers and the resin system MY720/DDS (tetraglycidyl-4,4'-diaminodiphenyl methane cured with diaminodiphenyl sulfone) are included. Radiation dose levels up to 8000 Mrads were obtained with no deleterious effects on the breaking stress or modulus. The effects on the structure and morphology were investigated using mechanical tests, electron spin resonance, X-ray diffraction, and electron spectroscopy for chemical analysis (ESCA or X-ray photoelectron spectroscopy). Details of the experiments and results are given. Studies of the fracture surfaces of irradiated samples were studied with scanning electron microscopy; current results indicate no differences in the morphology of irradiated and control samples.

Fornes, R. E.↗

Spheres of the metallic glass Au55 Pb22.5 Sb22.5 and their surface characteristics

Spheres of the metallic glass Au55 Pb22.5 Sb22.5 have been formed up to a size of approximately 1.5 mm in diameter. X-ray diffraction was used to establish the glassy nature of the samples and to provide evidence of two phase-separated glass regions. Scanning electron microscopy provided a direct visual observation of the two-phase amorphous network on the surface of the sphere. The physical dimensions of the phase-separated regions were observed to be cooling-rate sensitive. Energy dispersive spectroscopy indicated that the compositions of these two glassy phases were Au-rich and Pb-rich, respectively, confirming the results of Kim and Johnson (1981). In addition, the spheres exhibited an unusual surface smoothness of better than + or - 250 A

Lee, M. C.↗

Electron microscopy and diffraction of layered, superconducting intercalation complexes.

Several layered, transition metal dichalcogenide intercalation complexes with unique superconducting properties have been examined by high-resolution electron microscopy and electron diffraction. Details of the crystalline lattice and of the lattice imperfections have been directly resolved. The results can be correlated with the available X-ray diffraction and chemical data, and they confirm and extend the postulated models.

Fernandez-Moran, H.↗

An exploratory study of the microstructure of mullite fibers

Mullite fibers of three compositions, ranging from SiO2-rich to Al2O3-rich, were investigated by a number of transmission electron microscopy (TEM) techniques. The fibers were examined in the as-received condition and after subjecting them to thermal exposures as high as 142 C. The investigative techniques used included direct TEM of microtomed sections of mounted fibers and TEM of replicas of polished, chemically etched, and cathodically etched fibers. In addition, X-ray diffraction line broadening analyses was used for determining average crystallite size. A preliminary description of the microstructure of mullite fibers is given.

Santoro, G. J.↗

Fungi and bacteria involved in desert varnish formation

Desert varnish is a coating of ferromanganese oxides and clays that develops on rock surfaces in arid to semi-arid regions. Active respiration but not photosynthesis was detected on varnished rock surfaces from the Sonoran Desert. Light microscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) observations, and cultivation experiments indicate that both fungi, primarily dematiaceous hyphomycetes, and bacteria are found on and within desert varnish coatings from the arid regions studied. Some fungi grow as microcolonial fungi (MCF) on rocks, and microscopic observations suggest MCF become incorporated in the varnish coating. SEM-EDAX (energy dispersive X-ray systems) analyses indicate the MCF contain 3 of the characteristic elements of varnish: iron, aluminum, and silicon. In some locations, MCF are also enriched in manganese relative to the rock substratum. Furthermore, some of the dematiaceous hyphomycetes that have been cultivated are able to oxidize manganese under laboratory conditions. It is possible that manganese-oxidizing bacteria, which are found in varnish, also play an important role in varnish formation.

Taylor-George, S.↗

Airborne particle monitoring by electrostatic precipitation

For qualitative analysis of atmospheric particulates by microscopy, the sampling device should preserve the particles in the state existing at the moment of capture. A collector is described that uses electrostatic precipitation to capture and disperse specimens on various substrates for direct insertion into microscopes. Sampling runs in various atmospheres are described. Micrographs are presented to show particle morphology and distribution on the substrates. Chemical identification by X-ray energy probe and electron diffraction is illustrated.

Robinson, J. C.↗

Phase purity of NiCo2O4, a catalyst candidate for electrolysis of water

NiCo2O4 is shown to be difficult to obtain as a pure phase, and may never have been so obtained. High resolution x-ray diffractometry is required for its precise characterization. Film XRD is not likely to show the asymmetry in the spinel diffraction lines, caused by poorly crystallized NiO, as seen in diffractometer traces. The Co3O4 which is expected to accompany NiO as an impurity in NiCo2O4 syntheses has the same diffraction pattern as the binary oxide. Firings of the co-precipitated hydroxides at 300, 350, and 400 C, including one in pure O2, failed to produce single phase cobaltate. Scanning electron microscopy showed all the sintered products to range over several orders of magnitude in agglomerate/particle size. Surface areas by BET were all in the range 40 to 110 m sq/g, equivalent to particles of 200 to 100 Angstrom diameter. The spinel diffraction line breadths were compatible with those approximate dimensions.

Singer, J.↗

Soft x ray window encapsulant for HgI2 detectors

HgI2 is an excellent semiconductor material for a low energy, room temperature x-ray spectrometer. The high values of the atomic numbers for its constituent elements gives high x-ray and gamma ray stopping power. The band gap of HgI2 is significantly higher than other commonly used semiconductors. Owing to the large value band gap, the leakage current for HgI2 devices is smaller, thus allowing low noise performance. Devices fabricated from HgI2 crystals have demonstrated energy resolution sufficient to distinguish the x-ray emission from the neighboring elements on the periodic table. Also the power requirements of HgI2 are very low. These characteristics make a HgI2 spectrometer an ideal component in a satellite based detection system. Unfortunately, HgI2 crystals tend to deteriorate with time, even if protected by standard semiconductor encapsulants. This degradation ruins the performance of the device in terms of its energy resolution and pulse amplitude. The degrading mechanism is believed to be material loss occurring from below the electrodes, due to high vapor pressure of HgI2 at room temperature. To address this major obstacle to rapid expansion of HgI2 technology, a research program aimed at improving device stability by encapsulation with inert polymeric materials was carried out. The program focused specifically on optimizing the encapsulant materials and their deposition techniques. The principal objectives for this program were device encapsulation, device testing, and accelerated testing to ensure very long term stability of these high resolution sensors. A variety of encapsulants were investigated with the selection criteria based on their chemical diffusion barrier properties, mechanical stability, reactivity, and morphology of encapsulant films. The investigation covered different classes of encapsulants including solvent based encapsulants, vapor deposited encapsulants, and plasma polymerized encapsulants. A variety of characterization techniques were employed to examine their effectiveness in stabilizing HgI2 devices; these included permeability evaluation, vacuum and heat testing, scanning electron microscopy (SEM) as well as studying the detector performance of coated detectors. The plasma polymerized films appear to have entirely solved the HgI2 degradation problem. Another achievement of this program was the development of an accelerated testing technique which correlates extremely well with long term tesing.

Entine, G.↗

The locations and amounts of endogenous ions and elements in the cap and elongating zone of horizontally oriented roots of Zea mays L.: an electron-probe EDS study

We used quantitative electron-probe energy-dispersive x-ray microanalysis to localize endogenous Na, Cl, K, P, S, Mg and Ca in cryofixed and freeze-dried cryosections of the cap (i.e. the putative site of graviperception) and elongating zone (i.e. site of gravicurvature) of horizontally oriented roots of Zea mays. Ca, Na, Cl, K and Mg accumulate along the lower side of caps of horizontally oriented roots. The most dramatic asymmetries of these ions occur in the apoplast, especially the mucilage. We could not detect any significant differences in the concentrations of these ions in the central cytoplasm of columella cells along the upper and lower sides of caps of horizontally-oriented roots. However, the increased amounts of Na, Cl, K and Mg in the longitudinal walls of columella cells along the lower side of the cap suggest that these ions may move down through the columella tissue of horizontally-oriented roots. Ca also accumulates (largely in the mucilage) along the lower side of the elongating zone of horizontally-oriented roots, while Na, P, Cl and K tend to accumulate along the upper side of the elongating zone. Of these ions, only K increases in concentration in the cytoplasm and longitudinal walls of cortical cells in the upper vs lower sides of the elongating zone. These results indicate that (1) gravity-induced asymmetries of ions differ significantly in the cap and elongating zone of graviresponding roots, (2) Ca accumulates along the lower side of the cap and elongating zone of graviresponding roots, (3) increased growth of the upper side of the elongating zone of horizontally-oriented roots correlates positively with increased amounts of K in the cytoplasm and longitudinal walls of cortical cells, and (4) the apoplast (especially the mucilage) may be an important component of the pathway via which ions move in graviresponding rots of Zea mays. These results are discussed relative to mechanisms for graviperception and gravicurvature of roots.

NASA Program Space Biology↗