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At least 37 records · Page 2

Mechanisms of devitrification of grain boundary glassy phases in Si3N4 materials

Changes in the grain boundary (g.b.) phases of Si3N4 are analyzed, the effects of composition and thermal history on devitrification of the g.b. phases are determined, devitrification of the g.b. phases of Si3N are related to mechanical behavior and oxidation sensitivity of the material. The phase relationships that occur within the grain boundaries of Si3N4 containing various densification aids are reviewed. Comparisons of the effects of MgO, Y2O3, CeO2, and Y2O3 + AL2O3 are made in terms of the phase equilibria of the Si3N4 + SiO2 + additive compositional system. Two new equilibrium phase diagrams for the Si3N4-SiO2 and Y2O3 and Si3N4-SiO2-Ce2O3 systems are preented. The effects of Y2O3 vs CeO2 densification aids on the fracture surfaces of Si3N4 are compared. Auger electron spectroscopy shows that both oxides are concentrated within the fracture surface. Scanning electron microscopy shows evidence that Si3N4 with CeO2 formed an intergranular structure of fine grained oxynitride reaction products, as predicted by phase quilibria, whereas the Y2O3 containing sample shows evidence of an intergranular glassy phase.

Hench, L. L.↗

Effect of Y2O3 and Al2O3 on the oxidation resistance of Si3N4

Oxidation of cold-pressed and sintered Si3N4 containing 15 wt% Y2O3 and 2, 4, 6, and 8% Al2O3 is observed at temperatures as low as 1000 C with IR reflection spectroscopy. Concentrations of Al2O3 in excess of 4% greatly retard the rate of oxidation and alter the mechanism of surface attack by promoting formation of a glassy layer on the surface containing mixed oxynitride bonds. The glassy layer retards heterogeneous attack and reduces the effect of an oxidation transition temperature between 1000 and 1100 C for these materials.

Hench, L. L.↗

Hot-pressed silicon nitride with various lanthanide oxides as sintering additives

The effects of addition of various lanthanide oxides and their mixture with Y2O3 on the sintering of Si3N4 were investigated. The addition of simple and mixed lanthanide oxides promoted the densification of Si3N4 in hot-pressing at 1800 C under 300-400kg/ centimeters squared for 60 min. The crystallization of yttrium and lanthanide-silicon oxynitrides which was observed inn the sintered body containing yttrium-lanthanide mixed oxides as additives led to the formation of a highly refractory Si3N4 ceramic having a bending strength of 82 and 84 kg/millimeters squared at room temperature and 1300 C respectively. In a Y2O3+La2O3 system, a higher molar ratio of La2O3 to Y2O3 gave a higher hardness and strength at high temperatures. It was found that 90 min was an optimum sintering time for the highest strength.

Ueno, K.↗

Grain-boundary phases in hot-pressed silicon nitride containing Y2O3 and CeO2 additives

Auger electron spectroscopy in conjunction with X-ray powder diffraction and scanning electron microscopy is used to analyze the grain-boundary phases of Y2O3- and CeO2-doped Si3N4 hot-pressed materials in order to demonstrate that the additives concentrate predominantly in the grain boundaries of Si3N4 in the form of various oxynitride phases. A high oxygen content observed in sample fracture surfaces was found to be consistent with the existence of an oxygen-enriched phase in the grain boundaries. The presence of yttrium and cerium in the fracture surfaces and an overall increase in the O/N ratio imply that the additive oxides are predominantly concentrated in the intergranular phases.

Guha, J. P.↗

Annual Conference on Nuclear and Space Radiation Effects, Gatlinburg, TN, July 18-21, 1983, Proceedings

Topics discussed include radiation effects in devices; the basic mechanisms of radiation effects in structures and materials; radiation effects in integrated circuits; spacecraft charging and space radiation effects; hardness assurance for devices and systems; and radiation transport, energy deposition and charge collection. Papers are presented on the mechanisms of small instabilities in irradiated MOS transistors, on the radiation effects on oxynitride gate dielectrics, on the discharge characteristics of a simulated solar cell array, and on latchup in CMOS devices from heavy ions. Attention is also given to proton upsets in orbit, to the modeling of single-event upset in bipolar integrated circuits, to high-resolution studies of the electrical breakdown of soil, and to a finite-difference solution of Maxwell's equations in generalized nonorthogonal coordinates.

Source record↗

X-ray photoelectron spectroscopy study of the chemical structure of thermally nitrided SiO2

X-ray photoelectron spectroscopy has been used to study the composition of 100-A thermally grown SiO2 films that have been thermally nitrided in ammonia. The SiO(x)N(y)/Si interface was studied both by chemical depth profiling of the oxynitride and by removal of the Si substrate with XeF2. It is found that N is distributed throughout the film, but with the concentration higher at the surface and in a region centered 25 A from the film/substrate interface. The interface region itself is found to be oxygen-rich relative to the rest of the film. Possible models which can explain these results are discussed.

Vasquez, R. P.↗

Study of the pore structure of ceramics prepared by the slip casting method

The porosity of the slip cast Si3N4 is similar to that of pressed Si3N4 formed at 2500 kg/sq cm. The porosity of cast Si oxynitride is equivalent to that of samples stressed at 10,000 kg/sq cm. Crucibles formed from these materials by slip casting have high thermal shock and corrosion resistance.

Guzman, I. Y.↗

Chemical structure of interfaces

The interfacial structure of silicon/dielectric and silicon/metal systems is particularly amenable to analysis using a combination of surface spectroscopies together with a variety of chemical structures of Si/SiO2, Si/SiO2Si3N4, Si/Si2N2O, Si/SiO2/Al, and Si/Native Oxide interfaces using high resolution (0.350 eV FWHM) X ray photoelectron spectroscopy. The general structure of these dielectric interfaces entails a monolayer chemical transition layer at the Si/dielectric boundary. Amorphous Si substrates show a wide variety of hydrogenated Si and Si(OH) sub x states that are not observed in thermal oxidation of single crystal material. Extended SiO2 layers greater than 8 A in thickness are shown to be stoichiometric SiO2, but to exhibit a wide variety of local network structures. In the nitrogen containing systems, an approach to stoichiometric oxynitride compounds with interesting impurity and electron trapping properties are seen. In native oxides, substantial topographical nonuniformity in oxide thickness and composition are found. Analysis of metal/oxide interfacial layers is accomplished by analytical removal of the Si substrate by UHV XeF2 dry etching methods.

Grunthaner, F. J.↗

Study of the kinetics and mechanism of the thermal nitridation of SiO2

X-ray photoelectron spectroscopy (XPS) has been used to study the nitridation time and temperature dependence of the nitrogen distribution in thermally nitrided SiO2 films. The XPS data show that the maximum nitrogen concentration near the (SiO(x)N(y)/Si interface is initially at the interface, but moves 20-25 A away from the interface with increasing nitridation time. Computer modeling of the kinetic processes involved is carried out and reveals a mechanism in which diffusing species, initially consisting primarily of nitrogen, react with the substrate, followed by formation of the oxygen-rich oxynitride due to reaction of the diffusing oxygen displaced by the slower nitridation of the SiO2. The data are consistent with this mechanism provided the influence of the interfacial strain on the nitridation and oxidation kinetics is explicitly accounted for.

Vasquez, R. P.↗

Submillimeter-wave antennas on thin membranes

Submillimeter-wave antennas have been fabricated on 1-micron thick silicon-oxynitride membranes. This approach results in better patterns than previous lens-coupled antennas, and eliminates the dielectric loss associated with the substrate lens. Measurements on a wideband log-periodic antenna at 700 GHz, 370 GHz and 167 GHz show no sidelobes and 3-dB beamwidths between 40 and 60 deg. A linear imaging array has similar patterns at 700 GHz. Possible applications for membrane antennas include wideband superconducting tunnel-junction receivers for radio astronomy and imaging arrays for radiometry and plasma diagnostics.

Rebeiz, Gabriel M.↗

Production of Ultrafine, High-purity Ceramic Powders Using the US Bureau of Mines Developed Turbomill

Turbomilling, an innovative grinding technology developed by the U.S. Bureau of Mines in the early 1960's for delaminating filler-grade kaolinitic clays, has been expanded into the areas of particle size reduction, material mixing, and process reaction kinetics. The turbomill, originally called an attrition grinder, has been used for particle size reduction of many minerals, including natural and synthetic mica, pyrophyllite, talc, and marble. In recent years, an all-polymer version of the turbomill has been used to produce ultrafine, high-purity, advanced ceramic powders such as SiC, Si3N4, TiB2, and ZrO2. In addition to particle size reduction, the turbomill has been used to produce intimate mixtures of high surface area powders and whiskers. Raw materials, TiN, AlN, and Al2O3, used to produce a titanium nitride/aluminum oxynitride (TiN/AlON) composite, were mixed in the turbomill, resulting in strength increases over samples prepared by dry ball milling. Using the turbomill as a leach vessel, it was found that 90.4 pct of the copper was extracted from the chalcopyrite during a 4-hour leach test in ferric sulfate versus conventional processing which involves either roasting of the ore for Cu recovery or leaching of the ore for several days.

Hoyer, Jesse L.↗

Quasi-optical antenna-mixer-array design for terahertz frequencies

A new quasi-optical antenna-mixer-array design for terahertz frequencies is presented. In the design, antenna and mixer are combined into an entity, based on the technology in which millimeter-wave horn antenna arrays have been fabricated in silicon wafers. It consists of a set of forward- and backward-looking horns made with a set of silicon wafers. The front side is used to receive incoming signal, and the back side is used to feed local oscillator signal. Intermediate frequency is led out from the side of the array. Signal received by the horn array is picked up by antenna probes suspended on thin silicon-oxynitride membranes inside the horns. Mixer diodes will be located on the membranes inside the horns. Modeling of such an antenna-mixer-array design is done on a scaled model at microwave frequencies. The impedance matching, RF and LO isolation, and patterns of the array have been tested and analyzed.

Guo, Yong↗

Micromachined electron tunneling infrared sensors

The development of an improved Golay cell is reported. This new sensor is constructed entirely from micromachined silicon components. A silicon oxynitride (SiO(x)N(y)) membrane is deflected by the thermal expansion of a small volume of trapped gas. To detect the motion of the membrane, an electron tunneling transducer is used. This sensor detects electrons which tunnel through the classically forbidden barrier between a tip and a surface; the electron current is exponentially dependent on the separation between the tip and the surface. The sensitivity of tunneling transducers constructed was typically better than 10(exp -3) A/square root of Hz. Through use of the electron tunneling transducer, the scaling laws which have prevented the miniaturization of the Golay cell are avoided. This detector potentially offers low cost fabrication, compatibility with silicon readout electronics, and operation without cooling. Most importantly, this detector may offer better sensitivity than any other uncooled infrared sensor, with the exception of the original Golay cell.

Kenny, T. W.↗

Integrated Optical Interferometers with Micromachined Diaphragms for Pressure Sensing

Optical pressure sensors have been fabricated which use an integrated optical channel waveguide that is part of an interferometer to measure the pressure-induced strain in a micromachined silicon diaphragm. A silicon substrate is etched from the back of the wafer leaving a rectangular diaphragm. On the opposite side of the wafer, ring resonator and Mach-Zehnder interferometers are formed with optical channel waveguides made from a low pressure chemical vapor deposited film of silicon oxynitride. The interferometer's phase is altered by pressure-induced stress in a channel segment positioned over the long edge of the diaphragm. The phase change in the ring resonator is monitored using a link-insensitive swept frequency laser diode, while in the Mach-Zehnder it is determined using a broad band super luminescent diode with subsequent wavelength separation. The ring resonator was found to be highly temperature sensitive, while the Mach-Zehnder, which had a smaller optical path length difference, was proportionally less so. The quasi-TM mode was more sensitive to pressure, in accord with calculations. Waveguide and sensor theory, sensitivity calculations, a fabrication sequence, and experimental results are presented.

DeBrabander, Gregory N.↗

Preceramic Polymers for Use as Fiber Coatings

Polymeric precursors to Si-C-O, SI-B-N and Si-C were evaluated for use as ceramic interfaces in ceramic matrix composites. Use of the preceramic polymers allows for easy dip coating of fibers from dilute solutions of a polymer, which are then pyrolyzed to obtain the ceramic. SCS-0 fibers (Textron Specialty Materials, Lowell, MA) were coated with polymers from three systems: polysilsesquioxanes, polyborosilazanes and polycarbosilanes. The polysilsesquioxane systems were shown to produce either silicon oxycarbide or silicon oxynitride, depending on the pyrolysis conditions, and demonstrated some promise in an RBSN (reaction-bonded silicon nitride) matrix model system. Polyborosilazanes were shown, in studies of bulk polymers, to give rise to oxidation resistant Si-B-N ceramics which remain amorphous to temperatures of 1600 C, and should therefore provide a low modulus interface. Polycarbosilanes produce amorphous carbon-rich Si-C materials which have demonstrated oxidation resistance.

Heimann, P. J.↗

Joining of Silicon Carbide-Based Ceramics by Reaction Forming Method

Recently, there has been a surge of interest in the development and testing of silicon-based ceramics and composite components for a number of aerospace and ground based systems. The designs often require fabrication of complex shaped parts which can be quite expensive. One attractive way of achieving this goal is to build up complex shapes by joining together geometrically simple shapes. However, the joints should have good mechanical strength and environmental stability comparable to the bulk materials. These joints should also be able to maintain their structural integrity at high temperatures. In addition, the joining technique should be practical, reliable, and affordable. Thus, joining has been recognized as one of the enabling technologies for the successful utilization of silicon carbide based ceramic components in high temperature applications. Overviews of various joining techniques, i.e., mechanical fastening, adhesive bonding, welding, brazing, and soldering have been provided in recent publications. The majority of the techniques used today are based on the joining of monolithic ceramics with metals either by diffusion bonding, metal brazing, brazing with oxides and oxynitrides, or diffusion welding. These techniques need either very high temperatures for processing or hot pressing (high pressures). The joints produced by these techniques have different thermal expansion coefficients than the ceramic materials, which creates a stress concentration in the joint area. The use temperatures for these joints are around 700 C. Ceramic joint interlayers have been developed as a means of obtaining high temperature joints. These joint interlayers have been produced via pre-ceramic polymers, in-situ displacement reactions, and reaction bonding techniques. Joints produced by the pre-ceramic polymer approach exhibit a large amounts of porosity and poor mechanical properties. On the other hand, hot pressing or high pressures are needed for in-situ displacement reactions and reaction bonding techniques. Due to the equipment required, these techniques are impractical for joining large or complex shaped components.

Singh, M.↗

Fundamentals of Passive Oxidation In SiC and Si3N4

The very slow oxidation kinetics of silicon carbide and silicon nitride, which derive from their adherent and passivating oxide films, has been explored at length in a broad series of studies utilizing thermogravimetric analysis, electron and optical micrography, energy dispersive spectrometry, x-ray diffractometry, micro-analytical depth profiling, etc. Some interesting microstructural phenomena accompanying the process of oxidation in the two materials will be presented. In Si3N4 the oxide is stratified, with an SiO2 topscale (which is relatively impervious to O2)underlain by a coherent subscale of silicon oxynitride which is even less permeable to O2- Such "defence in depth" endows Si3N4 with what is perhaps the highest oxidation resistance of any material, and results in a unique set of oxidation processes. In SiC the oxidation reactions are much simpler, yet new issues still emerge; for instance, studies involving controlled devitrification of the amorphous silica scale confirmed that the oxidation rate of SiC drops by more than an order of magnitude when the oxide scale fully crystallizes.

Thomas-Ogbuji, Linus U.↗

Thin Film Ceramic Strain Sensor Development for High Temperature Environments

The need for sensors to operate in harsh environments is illustrated by the need for measurements in the turbine engine hot section. The degradation and damage that develops over time in hot section components can lead to catastrophic failure. At present, the degradation processes that occur in the harsh hot section environment are poorly characterized, which hinders development of more durable components, and since it is so difficult to model turbine blade temperatures, strains, etc, actual measurements are needed. The need to consider ceramic sensing elements is brought about by the temperature limits of metal thin film sensors in harsh environments. The effort at the NASA Glenn Research Center (GRC) to develop high temperature thin film ceramic static strain gauges for application in turbine engines is described, first in the fan and compressor modules, and then in the hot section. The near-term goal of this research effort was to identify candidate thin film ceramic sensor materials and provide a list of possible thin film ceramic sensor materials and corresponding properties to test for viability. A thorough literature search was conducted for ceramics that have the potential for application as high temperature thin film strain gauges chemically and physically compatible with the NASA GRCs microfabrication procedures and substrate materials. Test results are given for tantalum, titanium and zirconium-based nitride and oxynitride ceramic films.

Wrbanek, John D.↗