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At least 19 records

Structural characterization and gas reactions of small metal particles by high resolution in-situ TEM (Transmission Electron Microscopy) and TED (Transmission Electron Diffraction)

The detection and size analysis of small metal particles supported on amorphous substrates becomes increasingly difficult when the particle size approaches that of the phase contrast background structures of the support. An approach of digital image analysis, involving Fourier transformation of the original image, filtering, and image reconstruction was studied with respect to the likelihood of unambiguously detecting particles of less than 1 nm diameter on amorphous substrates from a single electron micrograph.

Heinemann, K.

Transmission Electron Microscopy of Carbonaceous Matter in Bennu Aggregate Samples

Preliminary analyses of regolith samples from asteroid Bennu show high bulk carbon abundances (~4.7 wt.%). The organic matter is readily apparent in scanning electron microscopy (SEM), transmission electron microscopy (TEM), and NanoSIMS observations. A major objective of the OSIRIS-REx mission is to understand the nature and origin of the pre-biotic organic matter inventory in Bennu samples. Here we report on TEM studies of indigenous organic matter in Bennu aggregate samples.

L P Keller

In Situ Observation of Carbonaceous Material in the Matrices of CV and CM Carbonaceous Chondrites: Preliminary Results from Energy Filtered Transmission Electron Microscopy

Energy filtered transmission electron microscopy shows that organic matter can be detected in situ in the matrices of carbonaceous chondrites at a spatial resolution of at least 1 nm. In CM chondrites, carbon is often associated with sulfide particles. Additional information is contained in the original extended abstract.

Brearley, A. J.

A parametric study of single-wall carbon nanotube growth by laser ablation

Results of a parametric study of carbon nanotube production by the double-pulse laser oven process are presented. The effect of various operating parameters on the production of single-wall carbon nanotubes (SWCNTs) is estimated by characterizing the nanotube material using analytical techniques, including scanning electron microscopy, transmission electron microscopy, thermo gravimetric analysis and Raman spectroscopy. The study included changing the sequence of the laser pulses, laser energy, pulse separation, type of buffer gas used, operating pressure, flow rate, inner tube diameter, as well as its material, and oven temperature. It was found that the material quality and quantity improve with deviation from normal operation parameters such as laser energy density higher than 1.5 J/cm2, pressure lower than 67 kPa, and flow rates higher than 100 sccm. Use of helium produced mainly small diameter tubes and a lower yield. The diameter of SWCNTs decreases with decreasing oven temperature and lower flow rates.

Nanotubes, Carbon/chemistry

Heterogeneous Distribution of Carbonaceous Material in Murchison Matrix: In Situ Observations Using Energy Filtered Transmission Electron Microscopy

Energy filtered TEM (Transmission Electron Microscopy) has been used to study the location of carbonaceous material in situ in Murchison matrix. Carbon occurs frequently as narrow rims around sulfide grains, but is rare in regions of matrix that are dominated by phyllosilicates. Additional information is contained in the original extended abstract.

Brearley, Adrian J.

The Correlation of Structural, Chemical, and Electronic Properties of Small Metal Particles and Their Alloys

The low pressure interaction of CO with small Ru particles supported on ultrahigh vacuum (UHV) cleaved mica was studied using flash thermal desorption, Auger electron microscopy, transmission electron microscopy, and transmission electron diffraction. Average particle sizes for these experiments varied between 1.2 and 16 nm. A careful search for CO decomposition on the Ru particles revealed no evidence of dissociaiton over a temperature range and pressure range of 300 to 550 C and 10 to the minus 11th power to 10 to the minus 6th millibar, respectively. Cas and heat treatments caused significant morphological changes and dispersion in the Ru particles, which affected CO desorptiom These effects were dependent on the particle size.

Source record

An ultrahigh vacuum multipurpose specimen chamber with sample introduction system for in situ transmission electron microscopy investigations

A commercial transmission electron microscope (TEM), with flat-plate upper pole piece configuration of the objective lens, and top-entry specimen introduction was modified by introducing an ultrahigh vacuum (UHV) specimen chamber for in situ TEM experimentation. The pumping and design principles and special features of this UHV chamber, which makes it possible to obtain 5 x 10 to the -10th mbar pressure at the site of the specimen, while maintaining the airlock system that allows operation in the 10 to the -10th mbar range within 15 min after specimen change, are described. Design operating pressures and image quality (resolution of metal particles smaller than 1 nm in size) were achieved. Schematic drawings and design dimensions are included.

Heinemann, K.

Transmission electron microscopy of the 'LOW-CA' hydrated interplanetary dust particle

Transmission electron microscopy of a hydrated interplanetary dust particle indicates that it consists largely of a poorly crystalline phyllosilicate containing Fe, Mg and Al with an interlayer spacing of 10 to 12 A and so is distinct from the major phyllosilicate in CI and CM carbonaceous chondrites. The silicate is probably an Fe- and Mg-rich smectite or mica. Submicron, spherical to euhedral pyrrhotite and pentlandite are prominent. Unusual, low-Ni pentlandite is also common and typically occurs as rectangular platelets. Unlike many chondritic interplanetary dust particles, olivine is rare and pyroxene was not observed. Other less abundant phases are magnetite, chromite, and an unidentified phase containing Fe, Mg, Si, Ca, and Mn. This particle differs from a hydrated micrometeorite described previously by Brownlee (1978), indicating there are mineralogically different subsets of hydrated interplanetary dust particles. Despite gross similarities in mineralogy between the particle and the carbonaceous chondrites, they show appreciable differences in detail.

Tomeoka, K.

Lunar sample analysis

A wide variety of lunar sample and meteorite studies were performed. Abstracts of the most recent reports are also attached. Experimental techniques employed have included scanning electron microscopy, transmission electron microscopy, Mossbauer spectroscopy, atomic absorption analysis and a variety of simulation studies.

Housley, R. M.

Surface Diagnostics in Tribology Technology and Advanced Coatings Development

This paper discusses the methodologies used for surface property measurement of thin films and coatings, lubricants, and materials in the field of tribology. Surface diagnostic techniques include scanning electron microscopy, transmission electron microscopy, atomic force microscopy, stylus profilometry, x-ray diffraction, electron diffraction, Raman spectroscopy, Rutherford backscattering, elastic recoil spectroscopy, and tribology examination. Each diagnostic technique provides specific measurement results in its own unique way. In due course it should be possible to coordinate the different pieces of information provided by these diagnostic techniques into a coherent self-consistent description of the surface properties. Examples are given on the nature and character of thin diamond films.

Miyoshi, Kazuhisa

Mechanical, Chemical and Microstructural Characterization of Monazite-Coated Silicon Carbide Fibers

Tensile strengths of as-received Hi-Nicalon and Sylramic fibers and those having monazite surface coatings, deposited by atmospheric pressure chemical vapor deposition, were measured at room temperature and the Weibull statistical parameters determined. The average tensile strengths of uncoated Hi-Nicalon and Sylramic fibers were 3.19 +/- 0.73 and 2.78 +/- 0.53 GPa with a Weibull modulus of 5.41 and 5.52, respectively. The monazite-coated Hi-Nicalon and Sylramic fibers showed strength loss of approx. 10 and 15 percent, respectively, compared with the as-received fibers. The elemental compositions of the fibers and the coatings were analyzed using scanning Auger microprobe and energy dispersive X-ray spectroscopy. The LaPO4 coating on Hi-Nicalon fibers was approximately stoichiometric and about 50 nm thick. The coating on the Sylramic fibers extended to a depth of about 100 to 150 nm. The coating may have been stoichiometric LaPO4 in the first 30 to 40 nm of the layer. However, the surface roughness of Sylramic fiber made this profile somewhat difficult to interpret. Microstructural analyses of the fibers and the coatings were done by scanning electron microscopy, transmission electron microscopy, and selected area electron diffraction. Hi-Nicalon fiber consists of fine beta-SiC nanocrystals ranging in size from 1 to 30 mn embedded in an amorphous matrix. Sylramic is a polycrystalline stoichiometric silicon carbide fiber consisting of submicron beta-SiC crystallites ranging from 100 to 300 nm. Small amount of TiB2 nanocrystallites (approx. 50 nm) are also present. The LaPO4 coating on Hi-Nicalon fibers consisted of a chain of peanut shape particles having monazite-(La) structure. The coating on Sylramic fibers consisted of two layers. The inner layer was a chain of peanut shape particles having monazite-(La) structure. The outer layer was comprised of much smaller particles with a microcrystalline structure.

Bansal, N. P.

Measurements and Diagnostics of Diamond Films and Coatings

The commercial potential of chemical-vapor-deposited (CVD) diamond films has been established and a number of applications have been identified through university, industry, and government research studies. This paper discusses the methodologies used for property measurement and diagnostic of CVD diamond films and coatings. Measurement and diagnostic techniques studied include scanning electron microscopy, transmission electron microscopy, atomic force microscopy, stylus profilometry, x-ray diffraction, electron diffraction, Raman spectroscopy, Rutherford backscattering, elastic recoil spectroscopy, and friction examination. Each measurement and diagnostic technique provides unique information. A combination of techniques can provide the technical information required to understand the quality and properties of CVD diamond films, which are important to their application in specific component systems and environments. In this study the combination of measurement and diagnostic techniques was successfully applied to correlate deposition parameters and resultant diamond film composition, crystallinity, grain size, surface roughness, and coefficient of friction.

Miyoshi, Kazuhisa

Growth of Multi-Walled Carbon Nanotubes by Injection CVD Using Cyclopentadienyliron Dicarbonyl Dimer and Cyclooctatetraene Iron Tricarbonyl

Preferential oriented multiwalled carbon nanotubes were prepared by the injection chemical vapor deposition (CVD) method using either cyclopentadienyliron dicarbonyl dimer or cycloctatetraene iron tricarbonyl as the iron catalyst source. The catalyst precursors were dissolved in toluene as the carrier solvent for the injections. The concentration of the catalyst was found to influence both the growth of the nanotubes as well as the amount of iron in the deposited material. As deposited the multiwalled carbon nanotubes contained as little as 2.8% iron by weight. The material was deposited onto tantalum foil and fused silica substrates. The nanotubes were characterized by scanning electron microscopy, transmission electron microscopy, Raman spectroscopy and thermogravimetric analysis. This synthetic route provides a simple and scalable method to deposit MWNTs with a low defect density, low metal content and preferred orientation.

Harris, Jerry D.

From Bench Top to Market: Growth of Multi-Walled Carbon Nanotubes by Injection CVD Using Fe Organometallics - Production of a Commercial Reactor

Preferential oriented multiwalled carbon nanotubes were prepared by the injection chemical vapor deposition (CVD) method using either cyclopentadienyliron dicarbonyl dimer or cyclooctatetraene iron tricarbonyl as the iron catalyst source. The catalyst precursors were dissolved in toluene as the carrier solvent for the injections. The concentration of the catalyst was found to influence both the growth (i.e., MWNT orientation) of the nanotubes, as well as the amount of iron in the deposited material. As deposited, the multiwalled carbon nanotubes contained as little as 2.8% iron by weight. The material was deposited onto tantalum foil and fused silica substrates. The nanotubes were characterized by scanning electron microscopy, transmission electron microscopy, Raman spectroscopy and thermogravimetric analysis. This synthetic route provides a simple and scalable method to deposit MWNTs with a low defect density, low metal content and a preferred orientation. Subsequently, a small start-up was founded to commercialize the deposition equipment. The contrast between the research and entrepreneurial environments will be discussed.

Rowsell, J.

Thermochemical Stability of Ca2Yb8(SiO4)6O2 Apatite in Presence of Molten Calcium-Magnesium-AluminoSilicate (CMAS)

Thermochemical stability of ytterbium silicon oxyapatite Ca 2 Yb 8 (SiO 4 ) 6 O 2 (CYbS) in the presence of molten calcium-magnesium aluminosilicate (CMAS) has been investigated at elevated temperatures. CYbS apatite powder was synthesized from the constituent oxides via solid state reaction method. Hot pressed apatite substrates were exposed to molten CMAS at 1200, 1300, and 1400 °C for 1, 10, and 50 h. Development of phases in the interaction region of the heat-treated specimens was monitored using scanning electron microscopy, transmission electron microscopy, high angle annular dark field imaging, selected area electron diffraction and energy dispersive X-ray spectroscopy. Monoclinic cyclosilicate Ca 3 Yb 2 (Si 3 O 9 ) 2 formed from interaction of CYbS apatite with CaO in the CMAS melt at the apatite-CMAS reaction front and continued to nucleate and grow within the residual CMAS in diffusion couples annealed for 1-50 h at 1200 °C and those heat treated at 1300 °C for 1 h. Residual CMAS was Ca-depleted when cyclosilicate was present. Dendritic wollastonite CaSiO 3 was observed within the residual CMAS in couples annealed at 1200 and 1300 °C. Ingress of molten CMAS, because of its exponential decrease in viscosity, occurred through open pores and along the grain boundaries of the apatite substrates without any detectable chemical reaction at 1300 and 1400 °C. Results of this study indicate that Ca 2 Yb 8 (SiO 4 ) 6 O 2 apatite has the potential to mitigate the CMAS corrosion up to about 1200 °C but not at higher temperatures.

X-ray diffraction

Thermochemical Stability of Ca2Yb8(SiO4)6O2 Apatite in Presence of Molten Calcium-Magnesium-Aluminosilicate (CMAS)

Thermochemical stability of ytterbium silicon oxyapatite Ca 2 Yb 8 (SiO 4 ) 6 O 2 (CYbS) in the presence of molten calcium-magnesium aluminosilicate (CMAS) has been investigated at elevated temperatures for consideration as a thermal and environmental barrier coating (T/EBC) material. CYbS apatite powder was synthesized from the constituent oxides via a solid-state reaction method. Hot-pressed apatite substrates were exposed to molten CMAS at 1200, 1300, and 1400 °C for 1, 10, and 50 h. Development of phases in the interaction region of the heat-treated specimens was monitored using scanning electron microscopy, transmission electron microscopy, high-angle annular dark-field imaging, selected area electron diffraction, and energy dispersive x-ray spectroscopy. Monoclinic cyclosilicate Ca 3 Yb 2 (Si 3 O 9 ) 2 formed from interaction of CYbS apatite with CaO in the CMAS melt at the apatite-CMAS reaction front and continued to nucleate and grow within the residual CMAS in diffusion couples annealed for 1 to 50 h at 1200 °C as well as in those heat treated at 1300 °C for 1 h. Residual CMAS was depleted of Ca when cyclosilicate was present. Dendritic wollastonite (CaSiO3) was observed within the residual CMAS in couples annealed at 1200 and 1300 °C. Ingress of molten CMAS, because of its exponential decrease in viscosity, occurred through open pores and along the grain boundaries of the apatite substrates without any detectable chemical reaction at 1300 and 1400 °C. Results of this study indicate that Ca 2 Yb 8 (SiO 4 ) 6 O 2 apatite has the potential to mitigate the CMAS corrosion up to about 1200 °C but not at higher temperatures.

Narottam P Bansal