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At least 55 records · Page 3

New generation of plasma-sprayed mullite coatings on silicon carbide

Mullite is promising as a protective coating for silicon-based ceramics in aggressive high-temperature environments. Conventionally plasma-sprayed mullite on SiC tends to crack and debond on thermal cycling. It is shown that this behavior is due to the presence of amorphous mullite in the conventionally sprayed mullite. Heating the SiC substrate during the plasma spraying eliminated the amorphous phase and produced coatings with dramatically improved properties. The new coating exhibits excellent adherence and crack resistance under thermal cycling between room temperature and 1000 to 1400 C. Preliminary tests showed good resistance to Na2CO3-induced hot corrosion.

Lee, Kang N.↗

Shape-memory alloy micro-actuator

A method of producing an integral piece of thermo-sensitive material, which is responsive to a shift in temperature from below to above a phase transformation temperature range to alter the material's condition to a shape-memory condition and move from one position to another. The method is characterized by depositing a thin film of shape-memory material, such as Nickel titanium (Ni-Ti) onto a substrate by vacuum deposition process such that the alloy exhibits an amorphous non-crystalline structure. The coated substrate is then annealed in a vacuum or in the presence of an inert atmosphere at a selected temperature, time and cool down rate to produce an ordered, partially disordered or fully disordered BCC structure such that the alloy undergoes thermoelastic, martinsetic phase transformation in response to alteration in temperature to pass from a martinsetic phase when at a temperature below a phase transformation range and capable of a high level of recoverable strain to a parent austenitic phase in a memory shape when at a temperature above the phase transformation range. Also disclosed are actuator devices employing shape-memory material actuators that deform from a set shape toward an original shape when subjected to a critical temperature level after having been initially deformed from the original shape into the set shape while at a lower temperature. The actuators are mechanically coupled to one or more movable elements such that the temperature-induce deformation of the actuators exerts a force or generates a motion of the mechanical element(s).

Busch, John D.↗

Structural and compositional characterization of RF sputter-deposited Ni-Cr + Cr2O3 films

An RF-sputtered chrome oxide coating with metallic binders was developed. The chrome oxide coating has high-temperature capabilities and is wear resistant, and has some self-lubricating properties. A nichrome metallic binder was added in the coating to improve its ductility without significant loss in the hardness. The sputtering parameters were optimized to obtain a smooth coating with the maximum adherence. The coatings were applied using bias-sputter and sputter-deposit modes on the heat treated and annealed foil substrates. The coating applied on annealed foils using the sputter-deposit mode was smooth and had the best adherence. Metallurgical examinations showed that the coating was Ni-Cr + Cr2O3. The coating as applied was amorphous and it crystallized during substrate heat treatment.

Bhushan, B.↗

Properties of vacuum-evaporated boron films

The work on the properties of thin boron films made by vacuum evaporation of elemental boron using an electron beam as the energy source is reported. The program aimed at characterizing the properties of vacuum evaporated films. The work was directed toward those variables considered to be important in affecting the tensile strength of the boron films. In general, the thickness of the films was less than 0.002 in. The temperature of the substrate on which the boron was condensed was found to be most important. Three distinctly different forms of boron deposit were produced. Although the transition temperature was not sharply defined, at substrate temperatures of less than approximately 600 deg C the boron deposits were amorphous to X-ray. If the substrate were highly polished, the deposits were black and mirror-like. For substrates with coefficients of thermal expansion close to that of boron, the deposits were then continuous and uncracked. The studies suggest that the potential continues to exist for film-type composites to have both high strength and high modulus.

Feakes, F.↗

Corrosion-resistant amorphous metallic films of Mo49Cr33B18 alloy

Corrosion-resistant amorphous metallic alloy films of Mo49Cr33B18 with a crystallization temperature of 590 C were deposited onto glass and quartz substrates by magnetron sputter-quench technique. The amorphous nature of the films was confirmed by their diffuse X-ray diffraction patterns. The deposited films are densely packed (zone T) and exhibit low stress and good adhesion to the substrate. Corrosion current of as-deposited coating of MoCrB amorphous metallic alloy is approximately three orders of magnitude less than the corrosion current of 304 stainless steel in 1N H2SO4 solution.

Ramesham, R.↗

High-resolution electron microscope observation of voids in amorphous Ge.

Electron micrographs have been obtained which clearly show the existence of a void network in amorphous Ge films formed at substrate temperatures of 25 and 150 C, and the absence of a void network in films formed at higher substrate temperatures of 200 and 250 C. These results correlate quite well with density measurements and predictions of void densities by indirect methods.

Donovan, T. M.↗

Nature and origin of interstellar diamond from the Allende CV3 meteorite

Data and experimental evidence which support the contention that the C delta diamonds may result from grain-grain collisions in supernova shocks in the interstellar medium are presented. Fragments of the Allende CV3 chondrite were acid-treated. A whitish powder was obtained. For the Analytical Electron Microscopy (AEM) a small drop of ethanol suspension was transferred onto holey carbon support films on 3 mm EM grids. The AEM was performed on transmission-thin fragments of the material which overlay holes in the film, to eliminate interference from the substrate. Electron Spectroscopy for Chemical Analysis (ESCA) was performed on a large aliquot of C. Diamond was identified by selected area electron diffraction. Scanning Transmission Electron Microscope / Energy Dispersive X-ray (STEM-EDS) microanalyses of the C delta diamond, using a light-element detector, show that oxygen and possibly nitrogen are the only impurities consistently present. ESCA spectra from bulk C delta material confirm the presence of N at a level of 0.35 percent or less. Under UV irradiation a yellow-red fluorescence is observed, consistent with that of natural diamonds containing substitutional N. Electron Energy Loss Spectra (EELS) were recorded at 2 eV resolution from the C delta diamond, high pressure synthetic diamond, a diamond film produced in a low pressure plasma by chemical vapor deposition (CVD) on a heated silicon substrate (Roy, 1987), graphite, and amorphous arc sputtered carbon. Comparison of the carbon K edge shape and fine structure shows the Allende C delta phase to be largely diamond, but with a significant pre-edge absorption feature indicative of transitions of C 1s electrons into pi asterisk orbitals which are absent in the purely sp(3)-bonded diamond but present in graphite and amorphous carbon.

Blake, David↗

Diamond Composite Films for Protective Coatings on Metals and Method of Formation

Composite films consisting of diamond crystallites and hard amorphous films such as diamond-like carbon, titanium nitride, and titanium oxide are provided as protective coatings for metal substrates against extremely harsh environments. A composite layer having diamond crystallites and a hard amorphous film is affixed to a metal substrate via an interlayer including a bottom metal silicide film and a top silicon carbide film. The interlayer is formed either by depositing metal silicide and silicon carbide directly onto the metal substrate, or by first depositing an amorphous silicon film, then allowing top and bottom portions of the amorphous silicon to react during deposition of the diamond crystallites, to yield the desired interlayer structure.

Ong, Tiong P.↗

The growth of cubic silicon carbide on a compliant substrate

Research has shown that silicon carbide grown on silicon and 6H silicon carbide has problems associated with these substrates. This is because silicon and silicon carbide has a 20% lattice mismatch and cubic silicon carbide has not been successfully achieved on 6H silicon carbide. We are investigating the growth of silicon carbide on a compliant substrate in order to grow defect free silicon carbide. This compliant substrate consists of silicon/silicon dioxide with 1200 A of single crystal silicon on the top layer. We are using this compliant substrate because there is a possibility that the silicon dioxide layer and the carbonized layer will allow the silicon lattice to shrink or expand to match the lattice of the silicon carbide. This would improve the electrical properties of the film for the use of device fabrication. When trying to grow silicon carbide, we observed amorphous film. To investigate, we examined the process step by step using RHEED. RHEED data showed that each step was amorphous. We found that just by heating the substrate in the presence of hydrogen it changed the crystal structure. When heated to 1000 C for 2 minutes, RHEED showed that there was an amorphous layer on the surface. We also heated the substrate to 900 C for 2 minutes and RHEED data showed that there was a deterioration of the single crystalline structure. We assumed that the presence of oxygen was coming from the sides of the silicon dioxide layer. Therefore, we evaporated 2500 A of silicon to all four edges of the wafer to try to enclose the oxygen. When heating the evaporated wafer to 900 C the RHEED data showed single crystalline structure however at 1000 C the RHEED data showed deterioration of the single crystalline structure. We conclude that the substrate itself is temperature dependent and that the oxygen was coming from the sides of the silicon dioxide layer. We propose to evaporate more silicon on the edges of the wafer to eliminate the escape of oxygen. this will allow us to grow single crystal cubic silicon carbide.

Mitchell, Sharanda↗

Jet Fuel Thermal Stability Investigations Using Ellipsometry

Jet fuels are typically used for endothermic cooling in practical engines where their thermal stability is very important. In this work the thermal stability of Sasol IPK (a synthetic jet fuel) with varying levels of naphthalene has been studied on stainless steel substrates using spectroscopic ellipsometry in the temperature range 385-400 K. Ellipsometry is an optical technique that measures the changes in a light beam’s polarization and intensity after it reflects off of a thin film to determine the film’s thickness and optical properties. All of the tubes used were rated as thermally unstable by the color standard portion of the Jet Fuel Thermal Oxidation Test, and this was confirmed by the deposit thicknesses observed using ellipsometry. A new amorphous model on a stainless steel substrate was used to model the data and obtain the results. It was observed that, as would be expected, increasing the temperature of the tube increased the overall deposit amount for a constant concentration of naphthalene. The repeatability of these measurements was assessed using multiple trials of the same fuel at 385 K. Lastly, the effect of increasing the naphthalene concentration in the fuel at a constant temperature was found to increase the deposit thickness.In conclusion, ellipsometry was used to investigate the thermal stability of jet fuels on stainless steel substrate. The effects of increasing temperature and addition of naphthalene on stainless steel tubes with Sasol IPK fuel were investigated. It was found, as expected, that increasing temperature lead to an increase in deposit thickness. It wasAmerican Institute of Aeronautics and Astronautics6also found that increasing amounts of naphthalene increased the maximum deposit thickness. The repeatability of these measurements was investigated using multiple tests at the same conditions. The present work provides as a better quantitative tool compared to the widely used JFTOT technique. Future work will expand on the fuel types, temperature, and substrate materials.

thermal stability↗

Catalytic crystallization of ices by small silicate smokes at temperatures less than 20K

Samples of methanol and water ices condensed from the vapor onto aluminum substrates at low temperatures (below approximately 80 K) form amorphous ices; annealing at temperatures in excess of 140-155 K is usually required to convert such amorphous samples to crystalline ices. However, we have found that when either methanol or water vapor is deposited on to aluminum substrates that have been coated with a thin (0.1-0.5 mm) layer of amorphous silicate smoke, the ices condense in crystalline form. We believe that crystalline ice forms as the result of energy liberated at the ice/silicate interface perhaps due to weak bonding of the ice at defect sites on the grains and the very high surface to volume ratio and defect density of these smokes. Annealing of amorphous water ice mixed with more volatile components such as methane, carbon monoxide, etc., has been suggested as an efficient way to produce clatherates in the outer solar nebula and thus explain the volatile content of comets and icy satellites of the outer planets. This hypothesis may need to be re-examined if amorphous ice does not form on cold silicate grains.

Moore, M.↗

Infrared spectra of crystalline phase ices condensed on silicate smokes at T less than 20 K

Infrared spectra of H2O, CH3OH, and NH3 condensed at T less than 20 K on amorphous silicate smokes reveal that predominantly crystalline phase ice forms directly on deposit. Spectra of these molecules condensed on aluminum substrates at T less than 20 K indicate that amorphous phase ice forms. On aluminum, crystalline phase H2O and CH3OH are formed by annealing amorphous deposits to 155 K and 130 K, respectively (or by direct deposit at these temperatures); crystalline NH3 is formed by direct deposit at 88 K. Silicate smokes are deposited onto aluminum substrates by evaporation of SiO solid or by combustion of SiH4 with O2 in flowing H2 followed by vapor phase nucleation and growth. Silicate smokes which are oxygen-deficient may contain active surface sites which facilitate the amorphous-to-crystalline phase transition during condensation. Detailed experiments to understand the mechanism are currently in progress. The assumption that amorphous phase ice forms routinely on grains at T less than 80 K is often used in models describing the volatile content of comets or in interpretations of interstellar cloud temperatures. This assumption needs to be reexamined in view of these results.

Moore, Marla H.↗

Laser Techniques in Photovoltaic Research

High-power laser pulses were used to replace the conventional high temperature furnace processing for the p-n junction formation step in high speed, low cost solar cell fabrication. Three different approaches to junction formation were tested: (1) laser annealing of ion-implanted Si in which laser radiation is used to remove the radiation damage and to recover the electrical activity in the implanted layer; (2) a process in which a thin film of dopant is first deposited on the substrate and then incorporated into the near-surface region by laser-induced diffusion; and (3) a process in which a heavily doped amorphous silicon layer is deposited on the Si substrate and epitaxially regrown from the melted substrate layer by laser radiation. All three methods were found to provide suitable candidates for high efficiency Si solar cells.

Young, R. T.↗

Structural characterization and gas reactions of small metal particles by high-resolution TEM and TED

The interaction of 100 and 200 keV electron beams with amorphous alumina, titania, and aluminum nitride substrates and nanometer-size palladium particulate deposits was investigated for the two extreme cases of (1) large-area electron-beam flash-heating and (2) small-area high-intensity electron-beam irradiation. The former simulates a short-term heating effect with minimum electron irradiation exposure, the latter simulates high-dosage irradiation with minimum heating effect. All alumina and titania samples responded to the flash-heating treatment with significant recrystallization. However, the size, crystal structure, shape, and orientation of the grains depended on the type and thickness of the films and the thickness of the Pd deposit. High-dosage electron irradiation also readily crystallized the alumina substrate films but did not affect the titania films. The alumina recrystallization products were usually either all in the alpha phase, or they were a mixture of small grains in a number of low-temperature phases including gamma, delta, kappa, beta, theta-alumina. Palladium deposits reacted heavily with the alumina substrates during either treatment, but they were very little effected when supported on titania. Both treatments had the same, less prominent localized crystallization effect on aluminum nitride films.

Heinemann, K.↗

Preparation and analysis of particulate metal deposits

Small particles and clusters of palladium were grown by deposition from the vapor phase under ultrahigh vacuum conditions. Amorphous and crystalline support films of Al2O3 and ultrathin amorphous carbon films were used as substrate materials. The growth of the metal deposit was monitored in situ by scanning transmission diffraction of energy-filtered 100 kV electrons and high resolution transmission electron microscopy (TEM) analysis was performed in a separate instrument. It was established by in situ TEM, however, that the transfer of specimens in this case did not unduly affect the size and distribution of deposit particles. It was found that the cleanness, stoichiometry, crystallinity and structural perfection of the support surface play an essential role in determining the crystalline perfection and structure of the particles. The smallest palladium clusters reproducibly prepared contained not more than six atoms but size determinations below 1 nm average particle diameter are very problematic with conventional TEM. Palladium particles grown on carbon supports feature an impurity-stabilized mosaic structure.

Poppa, H.↗

Internal stresses in wear and corrosion resistant amorphous metallic coatings of (W/0.6/Re/0.4/)76B24 and (Mo/0.6/Ru/0.4/)82B18

Hard protective coatings in the W-Re-B and Mo-Ru-B alloy systems have been deposited by magnetron sputtering onto soda-lime glass and heat-treated AISI 52100 steel substrates. X-ray diffraction has confirmed the amorphous nature of the as-deposited coatings, and their crystallization temperatures were determined by differential thermal analysis to be 1000 and 790 C for W-Re-B and Mo-Ru-B coatings, respectively. Both coatings exhibit high microhardness; Mo-Ru-B, in addition, has excellent corrosion resistance by comparison with pure Mo at high anodic potentials. Attention is given to the influence of internal stresses on the protective properties of the coatings deposited under different conditions.

Thakoor, A. P.↗

Hydrogenated amorphous silicon deposited by ion-beam sputtering

Hydrogenated amorphous silicon films 1/2 to 1 micron thick were deposited on metal and glass substrates using ion-beam sputtering techniques. The 800 eV, 2 mA/sq cm beam was a mixture of argon and hydrogen ions. The argon sputtered silicon from a pure (7.6 cm) single crystal wafer, while the hydrogen combined with the sputtered material during the deposition. Hydrogen to argon pressure ratios and substrate temperatures were varied to minimize the defect state density in the amorphous silicon. Characterization was done by electrical resistivity, index of refraction and optical absorption of the films.

Lowe, V. E.↗