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At least 145 records · Page 8

Continuous Fiberization of Silicon-Carbide-Nitride Precursor Resin

The objective of this project is to design and build a laboratory scale extruder and with it to fiberize 5000 continuous feet of silicon-carbide-nitride precursor resin. Subsequently the objective is extended to include the cross-linking and pyrolysis of approximately 100 feet of the resin fiber. The extruder is designed to accommodate approximately 1 cubic centimeter samples at accurately controllable rates corresponding to take-up from a single orifice of a 25 micron fiber at speeds in the 1000 feet/minute region. Positive feed delivery is achieved with a cylinder and piston driven by a geared down electric motor. Gear reduction is achieved primarily with off-the-shelf parts. Over 5000 feet of fiber, 20 to 30 micron diameter, are spun from precursor resin samples. The formation of continuous silicon carbide/silicon nitride fiber appears to be feasible.

Dunn, S. A.↗

Manufacture of sintered silicon nitrides

Sintered silicon nitrides are manufactured by sintering Si3N powder containing 2 to 15% in wt of a powder mixture composed of nitride powder of lanthanide or Y 100 parts and AIN powder less than 100 parts at 1500 to 1900 deg. temperature under a pressure of less than 200 Kg/sq. cm. The sintered Si3N has high mechanical strength in high temperature. Thus, Si3N4 93.0, Y 5.0 and AlN 2.0% in weight were wet mixed in acetone in N atom, molded and sintered at 1750 deg. and 1000 Kg/sq. cm. to give a sintered body having high hardness.

Iwai, T.↗

Processing study of injection molding of silicon nitride for engine applications

The high hardness of silicon nitride, which is currently under consideration as a structural material for such hot engine components as turbine blades, renders machining of the material prohibitively costly; the near net shape forming technique of injection molding is accordingly favored as a means for component fabrication. Attention is presently given to the relationships between injection molding processing parameters and the resulting microstructural and mechanical properties of the resulting engine parts. An experimental program has been conducted under NASA sponsorship which tests the quality of injection molded bars of silicon nitride at various stages of processing.

Rorabaugh, M. E.↗

Boron nitride: Composition, optical properties and mechanical behavior

A low energy ion beam deposition technique was used to grow boron nitride films on quartz, germanium, silicon, gallium arsenide, and indium phosphate. The film structure was amorphous with evidence of a hexagonal phase. The peak boron concentration was 82 at %. The carbon and oxygen impurities were in the 5 to 8 at % range. Boron-nitrogen and boron-boron bonds were revealed by X-ray photoelectron spectroscopy. The index of refraction varied from 1.65 to 1.67 for films deposited on III-V compound semiconductors. The coefficient of friction for boron nitride in sliding contact with diamond was less than 0.1. The substrate was silicon.

Pouch, John J.↗

Ion-beam nitriding of steels

A surface of a steel substrate is nitrided without external heating by exposing it to a beam of nitrogen ions under low pressure, a pressure much lower than that employed for ion-nitriding. An ion source is used instead of a glow discharge. Both of these features reduce the introduction of impurities into the substrate surface.

Salik, Joshua↗

Devitrification and delayed crazing of SiO2 on single-crystal silicon and chemically vapor-deposited silicon nitride

The linear growth rate of cristobalite was measured in thin SiO2 films on silicon and chemically vapor-deposited silicon nitride. The presence of trace impurities from alumina furnace tubes greatly increased the crystal growth rate. Under clean conditions, the growth rate was still 1 order-of-magnitude greater than that for internally nucleated crystals in bulk silica. Crystallized films cracked and lifted from the surface after exposure to atmospheric water vapor. The crystallization and subsequent crazing and lifting of protective SiO2 films on silicon nitride should be considered in long-term applications.

Choi, Doo Jin↗

Boron nitride - Composition, optical properties, and mechanical behavior

A low energy ion beam deposition technique was used to grow boron nitride films on quartz, germanium, silicon, gallium arsenide, and indium phosphate. The film structure was amorphous with evidence of a hexagonal phase. The peak boron concentration was 82 at. percent. The carbon and oxygen impurities were in the 5 to 8 at. percent range. Boron-nitrogen and boron-boron bonds were revealed by X-ray photoelectron spectroscopy. The index of refraction varied from 1.65 to 1.67 for films deposited on III-V compound semiconductors. The coefficient of friction for boron nitride in sliding contact with diamond was less than 0.1. The substrate was silicon.

Pouch, John J.↗

Plasma deposited silicon nitride for indium phosphide encapsulation

The composition and the annealing characteristics of plasma-deposited silicon-nitride encapsulating films on the ion-implanted InP substrates were investigated, using two different substrate-cleaning procedures (organic solvents and HF or HIO3 solutions) prior to encapsulation. The effect of plasma deposition of silicon nitride on the InP substrates was assessed through the current-voltage characteristics of Schottky diodes. Results of XPS analyses showed that the cleaning procedure that employed HF solution left less oxygen on the InP surface than the procedure involving HIO3. No chemical interaction between the film and the substrate was observed before or after annealing.

Valco, G. J.↗

Chemical profiling of silicon nitride structures

X ray photoelectron spectroscopy (XPS), spectroscopic ellipsometry (SE), and scanning electron microscopy (SEM) were used to study structural and chemical inhomogeneities in several electronic materials and device structures of relevance to radiation hard electronics. The systems studied include metal nitride oxide semiconductor (MNOS) structures, silicon oxynitride (SiO(x)N(y)) formed by the thermal nitridation of SiO2, and semiconductor on insulator (SOI) structures. Studies of MNOS structures suggest that the effect of H2 annealing is to make the Si3N4/SiO2 interface less abrupt by causing interdiffusion of silanol and silamine groups with subsequent oxynitride formation. Another effect of the annealing appears to be to relieve the strain at the SiO2/Si interface.

Vasquez, R. P.↗

Matrix density effects on the mechanical properties of SiC fiber-reinforced silicon nitride matrix properties

The room temperature mechanical properties were measured for SiC fiber reinforced reaction-bonded silicon nitride composites (SiC/RBSN) of different densities. The composites consisted of approx. 30 vol percent uniaxially aligned 142 micron diameter SiC fibers (Textron SCS-6) in a reaction-bonded Si3N4 matrix. The composite density was varied by changing the consolidation pressure during RBSN processing and by hot isostatically pressing the SiC/RBSN composites. Results indicate that as the consolidation pressure was increased from 27 to 138 MPa, the average pore size of the nitrided composites decreased from 0.04 to 0.02 microns and the composite density increased from 2.07 to 2.45 gm/cc. Nonetheless, these improvements resulted in only small increases in the first matrix cracking stress, primary elastic modulus, and ultimate tensile strength values of the composites. In contrast, HIP consolidation of SiC/RBSN resulted in a fully dense material whose first matrix cracking stress and elastic modulus were approx. 15 and 50 percent higher, respectively, and ultimate tensile strength values were approx. 40 percent lower than those for unHIPed SiC/RBSN composites. The modulus behavior for all specimens can be explained by simple rule-of-mixture theory. Also, the loss in ultimate strength for the HIPed composites appears to be related to a degradation in fiber strength at the HIP temperature. However, the density effect on matrix fracture strength was much less than would be expected based on typical monolithic Si3N4 behavior, suggesting that composite theory is indeed operating. Possible practical implications of these observations are discussed.

Bhatt, Ramakrishna T.↗

An evaluation of bearings operating in a cryogenic environment with silicon nitride rolling elements

The bearings used in the space shuttle main engine (SSME) high pressure oxidizer turbopump (HPOTP) do not meet the expected life goals that were set for them. In an effort to improve their performance, many solutions are being studied. New bearing materials are being developed, better manufacturing techniques are being investigated, and improved cage materials for better lubrication are being tested. The focus is on the replacement of steel balls with ones made of silicon nitride in 57-mm HPOTP bearings. The bearings were then installed in a test rig and run at near turbopump operating conditions. The results from this test series are encouraging, with silicon nitride showing good wear resistance and thermal stability.

Gibson, H. G.↗

Comparison of dynamic fatigue behavior between SiC whisker-reinforced composite and monolithic silicon nitrides

The dynamic fatigue behavior of 30 vol percent silicon nitride whisker-reinforced composite and monolithic silicon nitrides were determined as a function of temperature from 1100 to 1300 C in ambient air. The fatigue susceptibility parameter, n, decreased from 88.1 to 20.1 for the composite material, and from 50.8 to 40.4 for the monolithic, with increasing temperature from 1100 to 1300 C. A transition in the dynamic fatigue curve occurred for the composite material at a low stressing rate of 2 MPa/min at 1300 C, resulting in a very low value of n equals 5.8. Fractographic analysis showed that glassy phases in the slow crack growth region were more pronounced in the composite compared to the monolithic material, implying that SiC whisker addition promotes the formation of glass rich phases at the grain boundaries, thereby enhancing fatigue. These results indicate that SiC whisker addition to Si3 N4 matrix substantially deteriorates fatigue resistance inherent to the matrix base material for this selected material system.

Choi, Sung R.↗

Plasma-deposited germanium nitride gate insulators for indium phosphide metal-insulator-semiconductor field-effect transistors

Plasma-deposited germanium nitride was investigated for the first time as a possible gate insulator for InP compound semiconductor metal-insulator-semiconductor FET (MISFET) technology. The germanium nitride films were successfully deposited in a capacitively coupled parallel plate reactor at 13.56 MHz operation using GeH4/N2/NH3 and GeH4/N2 mixtures as reactant gases. The former process produced better quality films with enhanced uniformity, increased deposition rates, and increased resistivity. The breakdown field strength of the films was greater than 10 to the 6th V/cm. Auger electron spectroscopy did not indicate significant chemical composition differences between the two processes. For MISFETs with 2-micron channel lengths fabricated on InP, the device transconductance and threshold voltage for the GeH4/N2/NH3 process were 17 mS/mm and -3.6 V, respectively. The drain-source breakdown voltages were greater than 10 V.

Johnson, Gregory A.↗

Crack healing behavior of hot pressed silicon nitride due to oxidation

It is shown that limited oxidation of an MgO-containing, hot-pressed silicon nitride ceramic at 800 deg C and above results in increased strength due to crack healing. Slight oxidation of the surface produces enstatite and cristobalite which fills in cracks. More extensive oxidation leads to strength degradation due to the formation of new flaws by the evolution of N2 gas at the surface. The apparent fracture toughness also increased at 800 deg C and above due to oxidation. Bonds formed between the two surfaces of the crack during oxidation leads to a reduction in stress intensity at the crack tip, suggesting that valid high-temperature toughness values cannot be obtained in an air environment. The increase in strength due to crack healing by oxidation can be achieved without compromising the fatigue properties of the silicon nitride ceramic.

Choi, S. R.↗

Friction and wear of plasma-deposited amorphous hydrogenated films on silicon nitride

An investigation was conducted to examine the friction and wear behavior of amorphous hydrogenated carbon (a-C:H) films in sliding contact with silicon nitride pins in both dry nitrogen and humid air environments. Amorphous hydrogenated carbon films approximately 0.06 micron thick were deposited on silicon nitride flat substrates by using the 30 kHz ac glow discharge of a planar plasma reactor. The results indicate that an increase in plasma deposition power gives an increase in film density and hardness. The high-density a-C:H films deposited behaved tribologically much like bulk diamond. In the dry nitrogen environment, a tribochemical reaction produced a substance, probably a hydrocarbon-rich layer, that decreased the coefficient of friction. In the humid air environment, tribochemical interactions drastically reduced the wear life of a-C:H films and water vapor greatly increased the friction. Even in humid air, effective lubrication is possible with vacuum-annealed a-C:H films. The vacuum-annealed high-density a-C:H film formed an outermost superficial graphitic layer, which behaved like graphite, on the bulk a-C:H film. Like graphite, the annealed a-C:H film with the superficial graphitic layer showed low friction when adsorbed water vapor was present.

Miyoshi, Kazuhisa↗

Damage Mechanisms and Controlled Crack Propagation in a Hot Pressed Silicon Nitride Ceramic

The subcritical growth of cracks from pre-existing flaws in ceramics can severely affect the structural reliability of a material. The ability to directly observe subcritical crack growth and rigorously analyze its influence on fracture behavior is important for an accurate assessment of material performance. A Mode I fracture specimen and loading method has been developed which permits the observation of stable, subcritical crack extension in monolithic and toughened ceramics. The test specimen and procedure has demonstrated its ability to generate and stably propagate sharp, through-thickness cracks in brittle high modulus materials. Crack growth for an aluminum oxide ceramic was observed to be continuously stable throughout testing. Conversely, the fracture behavior of a silicon nitride ceramic exhibited crack growth as a series of subcritical extensions which are interrupted by dynamic propagation. Dynamic initiation and arrest fracture resistance measurements for the silicon nitride averaged 67 and 48 J/sq m, respectively. The dynamic initiation event was observed to be sudden and explosive. Increments of subcritical crack growth contributed to a 40 percent increase in fracture resistance before dynamic initiation. Subcritical crack growth visibly marked the fracture surface with an increase in surface roughness. Increments of subcritical crack growth loosen ceramic material near the fracture surface and the fracture debris is easily removed by a replication technique. Fracture debris is viewed as evidence that both crack bridging and subsurface microcracking may be some of the mechanisms contributing to the increase in fracture resistance. A Statistical Fracture Mechanics model specifically developed to address subcritical crack growth and fracture reliability is used together with a damaged zone of material at the crack tip to model experimental results. A Monte Carlo simulation of the actual experiments was used to establish a set of modeling input parameters. It was demonstrated that a single critical parameter does not characterize the conditions required for dynamic initiation. Experimental measurements for critical crack lengths, and the energy release rates exhibit significant scatter. The resulting output of the model produces good agreement with both the average values and scatter of experimental measurements.

Calomino, Anthony Martin↗

Isotopic Enrichment of Boron in the Sputtering of Boron Nitride with Xenon Ions

An experimental study is described to measure the isotopic enrichment of boron. Xenon ions from 100 eV to 1.5 keV were used to sputter a boron nitride target. An ion gun was used to generate the ion beam. The ion current density at the target surface was approximately 30 microA/sq cm. Xenon ions impinged on the target surface at 50 deg angle to the surface normal. Since boron nitride is an insulator, a flood electron gun was used in our experiments to neutralize the positive charge buildup on the target surface. The sputtered secondary ions of boron were detected by a quadrupole mass spectrometer. The spectrometer entrance aperture was located perpendicular to the ion beam direction and 10 mm away from the target surface. The secondary ion flux was observed to be enriched in the heavy isotopes at lower ion energies. The proportion of heavy isotopes in the sputtered secondary ion flux was found to decrease with increasing primary ion energy from 100 to 350 eV. Beyond 350 eV, light isotopes were sputtered preferentially. The light isotope enrichment factor was observed to reach an asymptotic value of 1.27 at 1.5 keV. This trend is similar to that of the isotopic enrichment observed earlier when copper was sputtered with xenon ions in the same energy range.

Ray, P. K.↗