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At least 217 records · Page 12

Characterization of ceramics and intermetallics fabricated by self-propagating high-temperature synthesis

Three efforts aimed at investigating the process of self-propagating high temperature synthesis (SHS) for the fabrication of structural ceramics and intermetallics are summarized. Of special interest was the influence of processing variables such as exothermic dopants, gravity, and green state morphology in materials produced by SHS. In the first effort directed toward the fabrication of SiC, exothermic dopants of yttrium and zirconium were added to SiO2 or SiO2 + NiO plus carbon powder mix and processed by SHS. This approach was unsuccessful since it did not produce the desired product of crystalline SiC. In the second effort, the influence of gravity was investigated by examining Ni-Al microstructures which were produced by SHS combustion waves traveling with and opposite the gravity direction. Although final composition and total porosities of the combusted Ni-Al compounds were found to be gravity independent, larger pores were created in those specimens which were combusted opposite to the gravity force direction. Finally, it was found that green microstructure has a significant effect on the appearance of the combusted piece. Severe pressing laminations were observed to arrest the combustion front for TiC samples.

Hurst, Janet B.↗

Measurements of complex permittivity of microwave substrates in the 20 to 300 K temperature range from 26.5 to 40.0 GHz

A knowledge of the dielectric properties of microwave substrates at low temperatures is useful in the design of superconducting microwave circuits. Results are reported for a study of the complex permittivity of sapphire (Al2O3), magnesium oxide (MgO), silicon oxide (SiO2), lanthanum aluminate (LaAlO3), and zirconium oxide (ZrO2), in the 20 to 300 Kelvin temperature range, at frequencies from 26.5 to 40.0 GHz. The values of the real and imaginary parts of the complex permittivity were obtained from the scattering parameters, which were measured using a HP-8510 automatic network analyzer. For these measurements, the samples were mounted on the cold head of a helium gas closed cycle refrigerator, in a specially designed vacuum chamber. An arrangement of wave guides, with mica windows, was used to connect the cooling system to the network analyzer. A decrease in the value of the real part of the complex permittivity of these substrates, with decreasing temperature, was observed. For MgO and Al2O3, the decrease from room temperature to 20 K was of 7 and 15 percent, respectively. For LaAlO3, it decreased by 14 percent, for ZrO2 by 15 percent, and for SiO2 by 2 percent, in the above mentioned temperature range.

Miranda, Felix A.↗

The effect of metal surface passivation on the Au-InP interaction

The effect of SiO2 encapsulation on reaction rates in the Au-InP system was studied. Scanning electron microscopy and x-ray photoelectron spectroscopy were used to investigate surface and/or interface morphologies and in-depth compositional profiles. It was found that the rate of dissolution of InP into Au and subsequent phase transformations are largely dependent on the condition of the free surface of the metalization. SiO2 capping of Au is reported for the first time to suppress the Au-InP reaction rate. The Au-InP interaction is shown to be quite similar to the Au-GaAs interaction despite differences in behavior of the group-V elements.

Fatemi, Navid S.↗

Thermal infrared (2.5-13.5-micron) spectroscopic remote sensing of igneous rock types on particulate planetary surfaces

The compositional significance of outstanding spectral features in the reflectance spectra of particulate igneous rocks was investigated by analyzing directional reflectance spectra, obtained with an FTIR spectrophotometer at 2.17-13.5 microns, of a suite of well-characterized igneous rocks ground to fine particle size. It was found that, using spectral features associated with the principal Christiansen frequency and with a region of relative transparency between the Si-O stretching and bending bands, it is possible to identify general rock type using the Walter and Salisbury (1989) SCFM chemical index, SCFM, defined as SCFM = SiO2/(SiO2 + CaO + FeO + MgO). It is emphasized, however, that the appearance and the wavelength of these features may be affected by environmental factors.

Salisbury, John W.↗

Spectral characterization of igneous rocks in the 8- to 12-micron region

This paper investigates the crystal-chemistry basis for the variation in spectral behavior of ingneous rocks, with the purpose of developing relationships useful for applications in the lithologic characterization of terrestrial and extraterrestrial surfaces. A new parameter is proposed for characterizing general rock and mineral type. The parameter, SCFM, defined as the ratio SiO2/(SiO2 + CaO + FeO + MgO), reflects the degree of depolymerization of the silica tetrahedra in both fine-grained and coarse-grained igneous rocks, and is a good descriptor of the composition of these rocks. Using spectra obtained in the laboratory on coarse-particulate mineral and solid-rock samples, the SCFM parameter was used to assess the effects of variations in the rock composition on the location, number, and width of spectral bands. A regression analysis of bands varying in width from 0.2 micron to 1.4 microns versus the SCFM value resulted in correlation coefficients ranging from 0.88 to 0.97.

Walter, Louis S.↗

Polysiloxanes derived from the controlled hydrolysis of tetraethoxysilane as precursors to silica for use in ceramic processing

Synthesis, properties, and potential applications in ceramic processing for two polysiloxane silica precursors derived from the controlled hydrolysis of tetraethoxysilane (TEOS) are presented. The higher molecular weight TEOS-A is a thick adhesive liquid of viscosity 8000 to 12,000 c.p. having a SiO2 char yield of about 55 percent. The lower molecular weight TEOS-B is a more fluid liquid of viscosity 150 to 200 c.p. having a SiO2 char yield of about 52 percent. The acid catalyzed hydrolysis of TEOS to hydrated silica gel goes through a series of polysiloxane intermediates. The rate of this transition increases with the quantity of water added to the TEOS; thus, for ease of polymer isolation, the amount of water added must be carefully determined so as to produce the desired polymer in a reasonable time. The water to TEOS mole ratio falls in the narrow range of 1.05 for TEOS-A and 0.99 for TEOS-B. Further polymerization or gelation is prevented by storing at -5 C in a freezer. Both polysiloxanes thermoset to a glassy solid at 115 C. The liquid polymers are organic in nature in that they are miscible with toluene and ethanol, slightly souble in heptane, but immiscible with water. For both polymers, results on viscosity versus time are given at several temperatures and water additions. Based on these results, some examples of practical utilization of the precursors for ceramic fabrication are given.

Philipp, Warren H.↗

'Nose method' of calculating critical cooling rates for glass formation

The use of the so-called 'nose method' for computing critical cooling rates for glass formation is examined and compared with other methods, presenting data for the glass-forming systems SiO2, GeO2, and P2O5. It is shown that, for homogeneous crystallization, the nose-method will give an overestimate of Rc, a conclusion which was drawn after assessing the enfluence of a range of values for the parameters which control crystal growth and nucleation. The paper also proposes an alternative simple procedure (termed the 'cutoff method') for computing critical cooling rates from T-T-T diagrams, which was shown in the SiO2 and GeO2 systems to be superior to the nose method.

Weinberg, Michael C.↗

Tracer versus trace element diffusion - Diffusional decoupling of Sr concentration from Sr isotope composition

Chemical diffusivities for nonalkali major, minor, and selected trace elements have been measured at 10 kbar, 1300 C during interdiffusion of dacitic and rhyolitic melts. Sr tracer diffusivities were measured at the same conditions in melts of dacitic and rhyolitic composition and in a diffusion couple of these two melts undergoing simultaneous chemical diffusion. Chemical diffusivities of all elements studied are functions of the silica content of the melt, but at any one silica content the chemical diffusivities of all elements studied are within a factor of five of the Si and Al diffusivities. Si diffusivity varies from 2.8 x 10 to the -9th sq cm/s at 65 percent SiO2 to 5.1 x 10 to the -10th sq cm/s at 75 percent SiO2. The diffusivities of minor and trace elements are proposed to be controlled by the ability of the local melt structure to accommodate these elements while maintaining LTE. The measured Sr tracer diffusivities are an order of magnitude above Sr chemical diffusivities.

Baker, Don R.↗

Ellipsometric study of Al2O3/Ag/Si and SiO2/Ag/quartz ashed in an oxygen plasma

The growth of silver oxide (proposed as a potentially useful protective coating for space environment) on a silver mirror coated with an Al2O3 or a SiO2 protective layer was investigated using the monolayer-sensitive variable angle of incidence spectroscopic ellipsometry technique. The samples were exposed to a pure oxygen plasma in a plasma asher, and the silver oxide growth was monitored as a function of the exposure time. It was found that atomic oxygen in the asher penetrated through the SiO2 or Al2O3 coatings to convert the silver underneath to silver oxide, and that the quantity of the silver oxide formed was proportional to the ashing time. The band gap of silver oxide was determined to be 1.3 eV. A schematic diagram of the variable angle of incidence spectroscopic ellipsometer is included.

De, Bhola N.↗

Flexible fluoropolymer filled protective coatings

Metal oxide films such as SiO2 are known to provide an effective barrier to the transport of moisture as well as gaseous species through polymeric films. Such thin film coatings have a tendency to crack upon flexure of the polymeric substrate. Sputter co-deposition of SiO2 with 4 to 15 percent fluoropolymers was demonstrated to produce thin films with glass-like barrier properties that have significant increases in strain to failure over pure glass films which improves their tolerance to flexure on polymeric substrates. Deposition techniques capable of producing these films on polymeric substrates are suitable for durable food packaging and oxidation/corrosion protection applications.

Banks, Bruce A.↗

Oxygen production by electrolysis of molten lunar regolith

The goal of this study was threefold. First, the theoretical energy requirements of the process were to be defined. This includes studies of the relevant oxidation-reduction reactions in the melt, their kinetics and energies of reaction, and experimental determination of production efficiencies and melt resistivities as functions of melt composition and applied potential. Second, the product(s) of silicate electrolysis were to be characterized. This includes: (1) evaluating the phase relationships in the systems SiO2-TiO2-Al2O3-MgO-FeO-CaO and Fe-Si; (2) estimating the compositions of the metal products as a function of applied potential and feedstock composition based on phase equilibria in the Fe-Si system and free energy values for SiO2 and FeO reported in the literature; (3) definition of compositions of products in actual experiments; and (4) definition of the form the product takes (whether phases separate or remain fixed, whether crystals settle or float in the remaining melt, and how large crystals form). Third, materials for these highly corrosive high-temperature silicate melts were to be identified. This includes identifing materials that may be either inert or thermodynamically stable in these melts, and experimental testing of the materials to confirm that they do not deteriorate. The results are discussed within this framework.

Haskin, Larry A.↗

Magma Electrolysis: An update

Electrolytic extraction of O2 from molten lunar soil is conceptually simple and thus a candidate process for producing O2 on the Moon. Possible container and electrode materials are being tested for durability in corrosive high-temperature silicate melts and looking for complications that might increase energy requirements. Gaseous oxygen is being produced by electrolysis of 1-2 gram quantities of silicate melts in spinel (MgAl2O4) crucibles; in these melts, spinel is a stable phase. The concentration of FeO was kept low because FeO decrease O2 production efficiency. Platinum electrodes were placed about 0.5 cm apart in the melt. The spinel crucible was still intact after 40 minutes of electrolysis, when the experiment was halted for examination. The Pt anode was also intact; its Pt was maintained in a dynamci state in which the anode was continuously oxidized but quickly reduced again by the silicate melt, inhibiting migration of Pt away from the anode. In melts with low concentrations of Al2O3 + SiO2 (2 wt percent), the energy of resistance heating was only approximately equal to 10 to 20 percent of the theoretical amount required to produce O2. In melts substantially more concentrated in Al2O3 + SiO2, higher melt viscosity resulted in frothing that, in the worst case, caused high enough melt resistivities to raise the energy requirements to nearly 10 times theoretical. Both Fe and Si are produced at the cathode; in iron-rich melts, a- and c-iron and molten ferrosilicon were observed. Production was also observed at the cathode of a previously unrecognized gas; which is not yet identified. The solubility of metallic species was measured in silicate melts. They are too low to reduce significantly the efficiency of O2 production.

Colson, Russell O.↗

Undercutting of defects in thin film protective coatings on polymer surfaces exposed to atomic oxygen

Protection for polymeric surfaces is needed to make them durable in the low earth orbital environment. Thin film coatings of oxides such as SiO2 are viable candidates to provide this protection, but concern has been voiced over the ability of these coatings to protect when defects are present in the coating due to surface anomalies. When a defected coating protecting a polymer substrate is exposed to atomic oxygen, the defect provides a pathway to the underlying polymer allowing oxidation and subsequent undercutting to occur. Defect undercutting was studied for sputter deposited coatings of SiO2 on polyimide Kapton. Preliminary results indicate that undercutting may be limited as long as the coating remains intact with the substrate. Therefore, coatings may not need to be defect free to give protection to the underlying surface.

Rutledge, Sharon K.↗

Evolution of optical coatings in earth orbit

High-resolution medium-energy backscattering analyses have been performed on SiO and SiO2 optical coatings that were exposed to the space environment aboard the NASA long-duration experiment module flight. The data show an increase in areal density of 1 percent (resolved at the 10 sigma level) in the SiO film as a result of this exposure. It appears that this effect has been produced by the incorporation of atomic oxygen from the ambient environment. Data on the SiO2 film are less compelling but are consistent with some loss of material from the surface. These analyses set a new standard for profiling film thicknesses by ion backscattering.

Mendelhall, Marcus H.↗

Elemental analyses of hypervelocity micro-particle impact sites on interplanetary dust experiment sensor surfaces

The Interplanetary Dust Experiment (IDE) had over 450 electrically active ultra-high purity metal-oxide-silicon impact detectors located on the six primary sides of the Long Duration Exposure Facility (LDEF). Hypervelocity micro-particles that struck the active sensors with enough energy to breakdown the 0.4 to 1.0 micron thick SiO2 insulator layer separating the silicon base (the negative electrode), and the 1000 A thick surface layer of aluminum (the positive electrode) caused electrical discharges that were recorded for the first year of orbit. These discharge features, which include 50 micron diameter areas where the aluminum top layer has been vaporized, facilitate the location of the impacts. The high purity Al-SiO2-Si substrates allow detection of trace (ppm) amounts of hypervelocity impactor residues. After sputtering through a layer of surface contamination, secondary ion mass spectrometry (SIMS) is used to create two-dimensional elemental ion intensity maps of micro-particle impact sites on the IDE sensors. The element intensities in the central craters of the impacts are corrected for relative ion yields and instrumental conditions and then normalized to silicon. The results are used to classify the particles' origins as 'manmade', 'natural' or 'indeterminate'. The last classification results from the presence of too little impactor residue (a frequent occurrence on leading edge impacts), analytical interference from high background contamination, the lack of information on silicon residue, the limited usefulness of data on aluminum in the central craters, or a combination of these circumstances. Several analytical 'blank' discharges were induced on flight sensors by pressing down on the sensor surface with a pure silicon shard. Analyses of these blank discharges showed that the discharge energy blasts away the layer of surface contamination. Only Si and Al were detected inside the discharge zones, including the central craters, of these features. A total of 35 impacts on leading edge sensors and 22 impacts on trailing edge sensors were analyzed.

Simon, Charles G.↗

Measurements of complex permittivity of microwave substrates in the 20 to 300 K temperature range from 26.5 to 40.0 GHz

A knowledge of the dielectric properties of microwve substrates at low temperatures is useful in the design of superconducting microwave circuits. Results are reported for a study of the complex permittivity of sapphire (Al2O3), magnesium oxide (MgO), silicon oxide (SiO2), lanthanum aluminate (LaAlO3), and zirconium oxide (ZrO2), in the 20 to 300 Kelvin temperature range, at frequencies from 26.5 to 40.0 GHz. The values of the real and imaginary parts of the complex permittivity were obtained from the scattering parameters, which were measured using an HP-8510 automatic network analyzer. For these measurements, the samples were mounted on the cold head of a helium gas closed cycle refrigerator, in a specially designated vacuum chamber. An arrangement of wave guides, with mica windows, was used to connect the cooling system to the network analyzer. A decrease in the value of the real part of the complex permittivity of these substrates, with decreasing temperature, was observed. For MgO and Al2O3, the decrease from room temperature to 20 K was of 7 and 15 percent, respectively. For LaAlO3, it decreased by 14 percent, for ZrO2 by 15 percent, and for SiO2 by 2 percent, in the above mentioned temperature range.

Miranda, Felix A.↗

Neodymium and strontium isotopic study of Australasian tektites - New constraints on the provenance and age of target materials

The Nd and Sr isotopic compositions of Australasian tectites (including two flanged Australian tectites, two low-SiO2 Muong Nong-type tectites, and three high-SiO2 Muong Nong-type tectites) and the Nd, Sm, Sr, and Rb concentrations were investigated by isotope-dilution thermal ionization mass spectrometry, and the Sm-Nd and Rb-Sr isotope systematics were used to study the characteristics of the parental material. It is shown that the Nd and Sr isotopic data provide evidence that all Australasian tektites were derived from a single sedimentary formation with a narrow range of stratigraphic ages close to 170 Ma. It is suggested that all of the Australasian tektites were derived from a single impact event and that the australites represent the upper part of a melt sheet ejected at high velocity, whereas the indochinites represent melts formed at a lower level in the target material distributed closer to the area of the impact.

Blum, Joel D.↗

Adsorption of CO on oxide and water ice surfaces - Implications for the Martian atmosphere

The adsorption of carbon monoxide (CO) on water ice and on the oxides Fe2O3, Fe3O4, Al2O3, SiO2, CaO, MgO, and TiO2 (rutile and anatase) has been investigated in a flow reactor. A mass spectrometer was employed as a detector to monitor the temporal concentrations of CO. Adsorption coefficients as large as 1 x 10 exp -4 were measured for CO on TiO2 solids in helium at 196 K. The fractional surface coverage for CO on TiO2 solids in helium was also determined to be approximately 10 percent at 196 K. The upper limits of the fractional surface coverage for the other oxides (Fe2O3, Fe3O4, Al2O3, SiO2, CaO, and MgO) and water ice were also measured to be less than 1 percent. The implications for the stability of CO2 in the Martian atmosphere and the 'CO hole' observed by the Phobos/ISM experiment are discussed.

Leu, M.-T.↗