SEARCH · Engineering Papers

Results for “microscopy analysis”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

SourceResearch connectionFrom yearThrough year

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 361 records · Page 20

All sources NASA NTRS DOE OSTI

DOE OSTI2022

Synthesis and Characterization of Copolymers and Nanocomposites from Limonene, Styrene and Organomodified-Clay Using Ultrasonic Assisted Method

In the present work, we report a simple synthesis method for preparation of copolymers and nanocomposites from limonene and styrene using clay as a catalyst. The copolymerization reaction is carried out by using a proton exchanged clay as a catalyst called Mag-H+. The effect of temperature, reaction time and amount of catalyst were studied, and the obtained copolymer structure (lim-co-sty) is characterized by Fourier transform infrared spectroscopy (FT-IR), nuclear magnetic resonance spectroscopy (1H-NMR) and differential scanning calorimetry (DSC). The molecular weight of the obtained copolymer is determined by gel permeation chromatography (GPC) and is about 4500 g·mol−1. The (lim-co-sty/Mag 1%, 3%, 7% and 10% by weight of clay) nanocomposites were prepared through polymer/clay mixture in solution method using ultrasonic irradiation, in the presence of Mag-CTA+ as green nano-reinforcing filler. The Mag-CTA+ is organophilic silicate clay prepared through a direct exchange process, using cetyltrimethylammonuim bromide (CTAB). The prepared lim-co-sty/Mag nanocomposites have been extensively characterized by FT-IR spectroscopy, X-ray diffraction (XRD), scanning electronic microscopy (SEM) and transmission electronic microscopy (TEM). TEM analysis confirms the results obtained by XRD and clearly show that the obtained nanocomposites are partially exfoliated for the lower amount of clay (1% and 3% wt) and intercalated for higher amounts of clay (7% and 10% wt). Moreover, thermogravimetric analysis (TGA) indicated an enhancement of thermal stability of nanocomposites compared with the pure copolymer.

Derdar, Hodhaifa↗

DOE OSTI2023

Geogenic, Anthropogenic, and Authigenic Minerals Hosting Arsenic and Antimony in Yellowknife Bay Sediments

Abstract Yellowknife Bay (Great Slave Lake, Northwest Territories, Canada) is a water body valued by surrounding communities for its subsistence, recreational, and cultural use. Located directly downstream of the former Giant Mine and Con Mine, Yellowknife Bay has received inputs from mine waste streams enriched in arsenic (As), antimony (Sb), and metals since the late 1930s. Lake sediments in Yellowknife Bay provide a record of metal(loid) contamination from aerially deposited roaster stack emissions, mine effluent, and Giant Mine tailings. A sediment sampling program was conducted in Yellowknife Bay to characterize As and Sb mineralogy using scanning electron microscopy-mineral liberation analysis. Mineralogical analysis of As- and Sb-hosted minerals in nine sediment cores suggests that arsenic trioxide (As2O3), originally deposited during the period of peak-mining emissions, has since been transformed into authigenic sulfides (interpreted to be realgar) down core from peak-mining emissions. Arsenic has also been attenuated by iron (Fe)-oxyhydroxides and roaster-generated iron oxides up-core from peak-mining emissions, near the sediment–water interface. The Sb-bearing minerals appear to be stable in Yellowknife Bay sediments, with no conclusive evidence of post-depositional mobility having been identified. The observed prevalence of arsenic trioxide in surface sediments proximal to Giant Mine suggests that As and Sb contamination is ongoing, likely from terrestrial weathering of contaminated soils and shoreline outcrops. Arsenic-bearing oxide minerals prevalent in surface sediments may become unstable should redox conditions in the hypolimnion change; prolonged anoxia could destabilize the As hosting minerals and release As to bottom waters. Therefore, long-term monitoring of the water column, including hypolimnion conditions, in Yellowknife Bay is recommended.

Mineralogy↗

NASA NTRS1973

Application of diffusion bonding to electronic interconnection of flatpack leads

Diffusion-bonded joints between gold-plated Kovar leads and indium-plated copper circuit pads offer some advantages for electronic circuit packaging. Test results show that consistent high strength bonds stronger than the copper circuit foil are achieved by parallel-gap bonding at relatively low power settings. The bonds are basically formed by the alloying of the gold, indium and copper at the bond interface. Other low melting metals such as tin can also be used; however, tin does not offer the ease of bonding that results in consistent separation of the copper foil during pull testing. The investigation was conducted in three parts consisting of: (1) an evaluation of the physical strength of resulting bonds at ambient and elevated temperature, (2) a metallurgical analysis of bonds using scanning electron microscopy and nondispersive X-ray analysis, and (3) evaluation and development of various schemes for multiple lead flatpack bonding.

Korb, R. W.↗

NASA NTRS1975

Characteristics of microcracks in lunar samples

Differential strain analysis and petrographic microscopy are discussed, and lunar rock studies which use these techniques are reported. Many cracks are present that were produced by nonshock processes in addition to the abundant shock-induced cracks. The crack spectra of lunar samples differ significantly from the spectra for shocked terrestrial rocks in that the lunar samples have very broad distributions of crack closure pressures while shocked terrestrial rocks have sharply peaked distributions with most cracks closing at pressures below 0.5 kbar. The difference may be attributed to either the effects of multiple shock events or the effects of confinement on the response of the rock to shock.

Simmons, G.↗

NASA NTRS1979

Adsorption of hydrogen chloride on microcrystalline silica

The interaction of hydrogen chloride with quartz was studied to determine the extent to which silica can irreversibly remove hydrogen chloride from the atmosphere. Adsorption isotherms were measured at 30 C for hydrogen chloride on silica outgassed between 100 C and 400 C. Readsorption isotherms were also measured. The silica surface was characterized further by infrared spectroscopy, electron spectroscopy for chemical analysis, scanning electron microscopy, and immersional calorimetry. Ground debris samples obtained from the Kennedy Space Center, were likewise examined.

Kang, Y.↗

NASA NTRS1979

Mechanical property degradation and chemical interactions in Borsic/titanium composite

A study was undertaken to identify the mechanisms of mechanical property degradation in a Borsic (silicon-carbide coated boron) fiber reinforced Ti-3Al-2.5V composite exposed to elevated temperature. Samples containing 0.45 volume fraction of fibers were exposed, in vacuum, to temperatures from 700 K to 1255 K for times up to 240 hours. Room temperature tensile properties of unidirectional material were determined in both the longitudinal and transverse directions, before and after high-temperature exposure. Electron micro-probe analysis, scanning electron microscopy, and X-ray diffraction were used to determine the compounds formed and the extent of interaction between the boron, SiC coating, and matrix materials.

Brewer, W. D.↗

NASA NTRS1982

Surface chemistry, microstructure and friction properties of some ferrous-base metallic glasses at temperatures to 750 C

X-ray photoelectron spectroscopy analysis, transmission electron microscopy, diffraction studies, and sliding friction experiments were conducted with ferrous-base metallic glasses in sliding contact with aluminum oxide at temperatures from room to 750 C in a vacuum of 30 nPa. The results indicate that there is a significant temperature influence on the friction properties, surface chemistry, and microstructure of metallic glasses. The relative concentrations of the various constituents at the surface of the sputtered specimens were very different from the normal bulk compositions. Contaminants can come from the bulk of the material to the surface upon heating and impart boric oxide and silicon oxide at 350 C and boron nitride above 500 C. The coefficient of friction increased with increasing temperature to 350 C. Above 500 C the coefficient of friction decreased rapidly. The segregation of contaminants may be responsible for the friction behavior.

Miyoshi, K.↗

NASA NTRS1983

Friction and wear of some ferrous-base metallic glasses

Sliding friction experiments, X-ray photoelectron spectroscopy (XPS) analysis, and electron microscopy and diffraction studies were conducted with ferrous base metallic glasses (amorphous alloys) in contact with aluminum oxide at temperatures to 750 C in a vacuum. Sliding friction experiments were also conducted in argon and air atmospheres. The results of the investigation indicate that the coefficient of friction increases with increasing temperature to 350 C in vacuum. The increase in friction is due to an increase in adhesion resulting from surface segregation of boric oxide and/or silicon oxide to the surface of the foil. Above 500 C the coefficient of friction decreased rapidly. The decrease correlates with the segregation of boron nitride to the surface. Contaminants can come from the bulk of the material to the surface upon heating and impart boric oxide and/or silicon oxide at 350 C and boron nitride above 500 C. The segregation of contaminants is responsible for the friction behavior. The amorphous alloys have superior wear resistance to crystalline 304 stainless steel. The relative concentrations of the various constituents at the surfaces of the amorphous alloys are very different from the nominal bulk compositions.

Miyoshi, K.↗

NASA NTRS1983

Interaction of hydrogen chloride and water with oxide surfaces. III - Titanium dioxide

The adsorption of hydrogen chloride and water vapors on five TiO2 powders in both the anatase and rutile crystalline forms was studied as a function of temperature, pressure, and outgas conditions. The adsorbents were characterized utilizing X-ray powder diffraction, scanning electron microscopy, surface area analysis, indicator method, microelectrophoresis, XPS, and infrared spectroscopy. It was found that both outgas temperature and adsorption temperature influenced the adsorption of water vapor on TiO2, while water vapor adsorption on TiO2 was completely reversible. It is argued that the number of hydroxyl groups present on the surface determines the adsorption capacity of water on the different titanium dioxides. It was found that heats of immersion in water were affected significantly by outgas temperature. Hydrogen chloride adsorption isotherms at 30 C measured on TiO2 after outgassing at 100-400 C showed that a part of the total HCl adsorbed was irreversibly adsorbed. The highest HCl adsorption capacity per unit area was exhibited by anatase, while pure rutile exhibited the lowest adsorption capacity.

Siriwardane, R. V.↗

NASA NTRS1983

Erosion of mylar and protection by thin metal films

Mylar strips, 2.5 microns thick, uncoated and coated with 50A, 100A and 200A of Al, Pd, and Au/Pd were exposed on STS-5 in order to measure the erosion of mylar and to test means of protecting thin plastic foils commonly used for space experiments in low earth orbit. Analysis by optical microscopy, SEM and STEM investigation, EDX measurements, FTIR spectroscopy and weight loss measurements showed that while up to 75 percent of the uncoated mylar was eroded during exposure, thin coatings of the above metals can protect mylar for integrated oxygen-fluxes of at least 10 to the 21st atoms/sq cm.

Fraundorf, P.↗

NASA NTRS1984

Influence of aluminum oxide film on thermocompression bonding of gold wire to evaporated aluminum film

The influence of Al surface condition on the thermocompression bonding of Au wires to Al electrodes for integrated electric circuits was studied. Au wires were connected to Al electrodes by nail-head bonding after various Al surface treatments. Bonding was evaluated by measuring the wire pull strength and fraction of the number of failures at Au-Al bonds to the total number of failures. Dependence of the fraction on applied load was derived theoretically with a parameter named critical load to take into consideration the differences in Al surface condition. The relation also held explicately for various surface treatments. Characterization of the Al surface was carried out by electron microscopy for chemical analysis.

Iwata, S.↗

NASA NTRS1984

Friction and wear of some ferrous-base metallic glasses

Sliding friction experiments, X-ray photoelectron spectroscopy (XPS) analysis, and electron microscopy and diffraction studies were conducted with ferrous base metallic glasses (amorphous alloys) in contact with aluminium oxide at temperatures to 750 C in a vacuum. Sliding friction experiments were also conducted in argon and air atmospheres. The results of the investigation indicate that the coefficient of friction increases with increasing temperature to 350 C in vacuum. The increase in friction is due to an increase in adhesion resulting from surface segregation of boric oxide and/or silicon oxide to the surface of the foil. Above 500 C the coefficient of friction decreased rapidly. The decrease correlates with the segregation of boron nitride to the surface. Contaminants can come from the bulk of the material to the surface upon heating and impart boric oxide and/or silicon oxide at 350 C and boron nitride above 500 C. The segregation of contaminants is responsible for the friction behavior. The amorphous alloys have superior wear resistance to crystalline 304 stainless steel. The relative concentrations of the various constituents at the surfaces of the amorphous alloys are very different from the nominal bulk compositions.

Miyoshi, K.↗

NASA NTRS1986

Dislocations in extruded Co-49.3 at. pct Al

Polycrystalline Co-49.3 at. pct Al, which had been extruded at 1505 K, was examined using transmission electron microscopy. Diffraction contrast analysis showed that b = 100 as well as b = 111 line dislocations contribute to elevated temperature deformation in CoAl. Therefore, it was concluded that sufficient slip systems exist in CoAl to allow for general plasticity in the absence of diffusional mechanisms. Line dislocations of the type b = 001 were observed on both 110 and 100 planes while b = 111 line dislocations were observed on 1 -1 0 planes.

Yaney, D. L.↗

NASA NTRS1987

Effect of an oxygen plasma on uncoated thin aluminum reflecting films

Thin aluminum films were considered for use as a reflective surface for solar collectors on orbiting solar dynamic power systems. A matter of concern is the durability of such reflective coatings against oxidative attack by highly reactive neutral atomic oxygen, which is the predominate chemical specie in low Earth orbit. Research to date was aimed at evaluating the protective merit of thin dielectric coatings over the aluminum or other reflective metals. However, an uncoated aluminum reflector may self-protect by virtue of the oxide formed from its exposed surface, which constitutes a physical barrier to further oxidation. This possibility was investigated, and an attempt was made to characterize the effects of atomic oxygen on thin Al films using photomicrographs, scanning electron microscopy, spectrophotometry, Auger analysis, and mass measurements. Data collected in a parallel effort is discussed for its comparative value. The results of the investigation of uncoated aluminum supported the self-protection hypothesis, and importantly, it was found that long term specular reflectance for uncoated aluminum exceeded that of Al and Ag reflectors with dielectric coatings.

Parsons, Roger L.↗

NASA NTRS1987

Review of Low Earth Orbital (LEO) flight experiments

The atomic oxygen flux exposure experiments flown on Space Shuttle flights STS-5 and STS-8 are described along with the results of measurements made on hardware returned from the Solar Maximum repair mission (Space Shuttle flight 41-C). In general, these experiments have essentially provided for passive exposure of samples to oxygen fluences of approximately 1 to 3.5 x 10(20) atoms/sq cm. Atmospheric density is used to derive fluence and is dependent on solar activity, which has been on the decline side of the 11-year cycle. Thus, relatively low flight altitudes of less than 300 km were used to acquire these exposures. After exposure, the samples were analyzed using various methods ranging from mass loss to extensive scanning electron microscopy and surface analysis techniques. Results are summarized and implications for the space station are discussed.

Leger, L.↗

NASA NTRS1987

Laser induced OMCVD growth of AlGaAs on GaAs

A major factor limiting the efficiency of the GaAs-GaAlAs solar cell is the rate of recombination at the GaAs-AlGaAs interface. Evidence has been previously reported which indicates that recombination at this interface can be greatly reduced if the AlGaAs layer is grown at lower than normal temperatures. The authors examine the epitaxial growth of AlGaAs on GaAs using a horizontal OMCVD reactor and an excimer laser operating in the UV (lambda = 193 nm) region. The growth temperatures were 450 and 500 C. The laser beam was utilized in two orientations: 75 deg angle of incidence and parallel to the substrate. Film composition and structure were determined by Auger electron spectroscopy (AES) and transmission electron microscopy (TEM). Auger analysis of epilayers grown at 500 C with the laser impinging show no carbon or oxygen contamination of the epitaxial layers or interfaces. TEM diffraction patterns of these same epilayers exhibit single crystal (100) zone axis patterns.

Wilt, David M.↗

NASA NTRS1988

Slurry-pressing consolidation of silicon nitride

A baseline slurry-pressing method for a silicon nitride material is developed. The Si3N4 composition contained 5.8 wt percent SiO2 and 6.4 wt percent Y2O3. Slurry-pressing variables included volume percent solids, application of ultrasonic energy, and pH. Twenty vol percent slurry-pressed material was approximately 11 percent stronger than both 30 vol percent slurry-pressed and dry-pressed materials. The Student's t-test showed the difference to be significant at the 99 percent confidence level. Twenty volume percent (300 h) slurry-pressed test bars exhibited strengths as high as 980 MPa. Large, columnar beta-Si3N4 grains caused failure in the highest strength specimens. The improved strength correlated with better structural uniformity as determined by radiography, optical microscopy, and image analysis.

Sanders, William A.↗

NASA NTRS1990

Raman spectroscopic studies of carbon in extra-terrestrial materials

The measurements obtained here indicate ways in which micro-Raman spectroscopy can be used to elucidate structural characteristics and distribution of carbon in meteorites and interplanetary dust particles (IDPs). Existing information about structurally significant aspects of Raman measurements of graphite is combined with structurally relevant findings from the present micro-Raman studies of carbons prepared by carbonization of polyvinylidine chloride (PVDC) at various temperatures and natural material, as well as several acid residues from the Allende and Murchison meteorites in order to establish new spectra-structure relationships. Structural features of many of the materials in this study have been measured by x ray analysis and electron microscopy: thus, their structural differences can be directly correlated with differences in the Raman spectra. The spectral parameters consequently affirmed as indicators of structure are used as a measure of structure in materials that have unknown carbon structure, especially IDPs. The unique applicability of micro-Raman spectroscopy is realized not only in the ability to conveniently measure spectra of micron-size IDPs, but also micro-sized parts of an inhomogeneous material. Microcrystalline graphite is known to give Raman spectra that differ dependent on crystallite size (see e.g., Lespade, et. al., 1984, or Nemanich and Solin, 1979). The spectral changes that accompany decreasing particle size include increase in the ratio (R) of the intensity of the band near 1350 cm(-1) (D band) to that of the band near 1600 cm(-1) (G band) increase in the half width of the D band (wD) increase in the frequency maximum of the G band and increase in the half-width (wG) of the 2nd order band near 2700 cm(-1) (G) band.

Macklin, John↗