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NASA NTRS1978

Conductivity of materials made of aluminum nitride and silicon nitride mixtures

To establish the possible mechanism for conductivity in aluminum nitride a study was made of the electric conductivity of pure AlN and its mixtures with silicon nitride at different temperatures and partial pressures of nitrogen in the gas phase. The thermoelectromotive force was also measured. The experiments used polycrystalline samples of cylindrical shape 18 mm in diameter made of powders by hot pressing in graphite press molds at a temperature of 1973-2273 K and pressure 1,470,000 n/sqm. The items obtained by this method had porosity not over 5%. After pressing, the samples were machined to remove carbon from the surface, and were annealed in a stream of dry ammonia for 10 h at a temperature of 1273-1373 K. Electric conductivity was measured according to the bridge scheme on an alternating current of frequency 10 kHz. In order to guarantee close contact of the platinum electrodes with the surface of the samples, a thin layer of platinum was sprayed on them. Experiments were conducted in the temperature interval 1273-1573 K with a half hour delay at each assigned temperature with heating and cooling.

Gorbatov, A. G.↗

NASA NTRS1977

Effect of microstructure on Na/+/ diffusion in beta alumina

The effect of microstructural features, such as grain size and orientation, on sodium ion diffusion in polycrystalline beta alumina is investigated; the ionic solid is suitable for use in high-energy and power density batteries. Two types of hot-pressed polycrystalline samples are studied, one with grains highly oriented in the direction normal to the pressing direction, the other with significantly less preferred orientation normal to the pressing direction. Results of the experimental assessments indicate that grain size and diffusion path tortuosity have little effect on diffusion kinetics, while grain boundary type and grain aspect ratio are important factors in determining the diffusion rate.

Sarian, S.↗

NASA NTRS1977

Improved performance of silicon nitride-based high temperature ceramics

Results are presented regarding experiments intended for improving the strength and toughness of hot-pressed Si3N4 (HPSN), improving the strength and oxidation resistance of reaction-sintered Si3N4 (RSSN), and improving the strength and oxidation resistance of sinterable Si-Al-O-N compositions. It is shown that the use of ZrO2 instead of MgO as a sintering aid improved the room-temperature and high-temperature flexural strength of HPSN, in addition to enhancing the rupture strength and Charpy impact resistance. The use of crushable energy absorbing layers increased the impact resistance of HPSN. Impregnation of RSSN with solutions that oxidize to Al2O3 or ZrO2 resulted in increased bending strength at room temperature. Beta-prime Si-Al-O-N sintered to full density by means of the sintering aids CeO2, Y2O3, and ZrO2 yielded the greatest strength with Y2O3 and the greatest oxidation resistance with ZrO2.

Ashbrook, R. L.↗

NASA NTRS1977

Ceramics in gas turbines - Powder and process characterization

The role of powder and process characterization in producing high quality silicon nitride and silicon carbide components, for gas turbine applications, is described. Some of the intrinsic properties of various forms of Si3N4 and SiC are listed and limitations of such materials' availability have been pointed out. The essential features/parameters to characterize a batch of powder have been discussed including the standard techniques for such characterization. In process characterization, parameters in sintering, reaction sintering, and hot pressing processes are discussed including the factors responsible for strength limitations in ceramic bodies. It is inevitable that significant improvements in material properties can be achieved by reducing or eliminating the strength limiting factors with consistent powder and process characterization along with process control.

Dutta, S.↗

NASA NTRS1977

Pressureless sintered beta-prime-Si3N4 solid solution - Fabrication, microstructure, and strength

Pressureless sintering of beta-prime-Si3N4 solid solution was studied as a function of temperature using Si3N4, A1N, and Al2O3 as basic constituents. Y2O3-SiO2 additions were used to promote liquid-phase sintering. The sintered specimens were characterized with respect to density, microstructure, strength, oxidation, and thermal shock resistance. Density greater than 98 percent of theoretical was achieved by pressureless sintering at 1750 C. The microstructure consisted essentially of fine-grained beta-prime-Si3N4 solid solution as the major phase. Modulus of rupture strengths up to 483 M Pa were achieved at moderate temperature (1000 C), but decreased to 228 M Pa at 1380 C. This substantial strength loss was attributed to a 'glassy' grain boundary phase formed during cooling from the sintering temperature. The best oxidation resistance was exhibited by a composition containing 3 mol % Y2O3-SiO2 additives. Water quench thermal shock resistance was equivalent to that of reaction sintered silicon nitride but lower than hot-pressed silicon nitride.

Dutta, S.↗

NASA NTRS1978

Sialons as high temperature insulators

Sialons were evaluated for application as high temperature electrical insulators in contact with molybdenum and tungsten components in hard vacuum applications. Both D.C. and variable frequency A.C. resistivity data indicate the sialons to have electrical resistivity similar to common oxide in the 1000 C or higher range. Metallographic evaluations indicate good bonding of the type 15R ALN polytype to molybdenum and tungsten. The beta prime or modified silicon nitride phase was unacceptable in terms of vacuum stability. Additives effect on electrical resistivity. Similar resistivity decreases were produced by additions of molybdenum or tungsten to form cermets. The use of hot pressing at 1800 C with ALN, Al2 O3 and Si3N4 starting powders produced a better product than did a combination of SiO2 and AIN staring powders. It was indicated that sialons will be suitable insulators in the 1600K range in contact with molybdenum or tungsten if they are produced as a pure ceramic and subsequently bonded to the metal components at temperatures in the 1600K range.

Phillips, W. M.↗

NASA NTRS1978

Study program to develop and evaluate die and container materials for the growth of silicon ribbons

Initial sessile drop experiments on SiC, Si3N4 and A1N were conducted. Very promising results were achieved on both SiC and Si3N4 where minimal penetration of these CNTD coatings by molten silicon was observed. More detailed characterization of the CNTD microstructures was accomplished as well as X-ray characterization of the third and fourth candidate materials system sets (i.e. A1N and altered Si3N4). Polished sections of post sessile drop specimens were also prepared and evaluated. The techniques of full scale crucible hot pressing were developed and die grinding development was initiated. The apparatus for measurement of oxygen partial pressure was reconstructed and calibrated. The sessile drop temperature measurement procedure was calibrated for absorption by the pyrex view-port and additional Auger electron analysis was performed at the interface of molten silicon with CNTD Si3N4 and A1N.

Source record↗

NASA NTRS1979

Design, fabrication and spin testing of ceramic blade metal disk attachment

A ceramic turbine blade-metal disk attachment was designed for small, non man-rated turbine engine applications. The selected design consisted of a hot pressed silicon nitride blade having a skewed dovetail attachment with a compliant interlayer between the disk and the blade. Two-dimensional and three-dimensional analyses predicted that life goals could be achieved, considering both NDE limitations and crack growth rates for the ceramic material. Twenty ceramic blades were fabricated to closely-held manufacturing tolerances. New fracture mechanics data at elevated temperature are presented.

Calvert, G.↗

NASA NTRS1979

Study Program to Develop and Evaluate Die and Container Materials for the Growth of Silicon Ribbons

The completion of a major hardware delivery milestone was accomplished with the delivery of three CNTD Si3N4 coated hot pressed Si3N4 crucibles. A limited characterization of the coating was performed at MRL prior to delivery. The coatings were fine grained alpha - Si3N4. It was determined that a two piece die design is required. The importance of the role of oxygen in influencing the attack of the CNTD materials by molten silicon was demonstrated. The stability is greatly enhanced by maintaining the oxygen partial pressure near or below the Si + O2 = SiO2 equilibrium.

Ounby, P. D.↗

NASA NTRS1978

Diminiode thermionic energy conversion with lanthanum-hexaboride electrodes

This paper presents thermionic-conversion data obtained from a variable-gap cesium diminiode with a hot-pressed, sintered lanthanum-hexaboride emitter and an arc-melted lanthanum-hexaboride collector. Performance curves cover a range of temperatures: emitter 1500 to 1700 K, collector 750 to 1000 K, and cesium reservoir 370 to 510 K. Calculated values of emitter and collector work functions and barrier index are also given.

Kroeger, E. W.↗

NASA NTRS1978

Beta-to-alpha transformation in polycrystalline SiC. II - Interfacial energetics

A phenomenological analysis of the energetics of the beta-to-alpha transformation in polycrystalline SiC is presented. It is found that the extreme anisotropy of the interfacial energy between alpha- and beta-SiC can account for the rapid growth of composite grains into the beta matrix during conventional sintering or hot-pressing processes. The composite grains consist of alpha-SiC plates 'sandwiched' between well-oriented and recrystallized beta-SiC 'envelopes'. The interfaces involving the 111 plane type of beta and (0001) of alpha have much lower energies than random beta/alpha interfaces.

Mitchell, T. E.↗

NASA NTRS1979

Study program to develop and evaluate die and container materials for the growth of silicon ribbons

The development and evaluation of proprietary coatings of pure silicon carbide, silicon nitride, and aluminum nitride on less pure hot pressed substrates of the respective ceramic materials, is described. Silicon sessile drop experiments were performed on coated test specimens under controlled oxygen partial pressure. Prior to testing, X-ray diffraction and SEM characterization was performed. The reaction interfaces were characterized after testing with optical and scanning electron microscopy and Auger electron spectroscopy. Increasing the oxygen partial pressure was found to increase the molten silicon contact angle, apparently because adsorbed oxygen lowers the solid-vapor interfacial free energy. It was also found that adsorbed oxygen increased the degree of attack of molten silicon upon the chemical vapor deposited coatings. Cost projections show that reasonably priced, coated, molten silicon resistant refractory material shapes are obtainable.

Addington, L. A.↗

NASA NTRS1980

Advanced ceramic material for high temperature turbine tip seals

Forty-one material systems were evaluated for potential use in turbine blade tip seal applications at 1370 C. Both ceramic blade tip inserts and abradable ceramic tip shoes were tested. Hot gas erosion, impact resistance, thermal stability, and dynamic rub performance were the criteria used in rating the various materials. Silicon carbide and silicon nitride were used, both as blade tips and abradables. The blade tip inserts were fabricated by hot pressing while low density and honeycomb abradables were sintered or reaction bonded.

Vogan, J. W.↗

NASA NTRS1980

Fracture toughness of brittle materials determined with chevron notch specimens

The use of chevron-notch specimens for determining the plane strain fracture toughness (K sub Ic) of brittle materials is discussed. Three chevron-notch specimens were investigated: short bar, short rod, and four-point-bend. The dimensionless stress intensity coefficient used in computing K sub Ic is derived for the short bar specimen from the superposition of ligament-dependent and ligament-independent solutions for the straight through crack, and also from experimental compliance calibrations. Coefficients for the four-point-bend specimen were developed by the same superposition procedure, and with additional refinement using the slice model of Bluhm. Short rod specimen stress intensity coefficients were determined only by experimental compliance calibration. Performance of the three chevron-notch specimens and their stress intensity factor relations were evaluated by tests on hot-pressed silicon nitride and sintered aluminum oxide. Results obtained with the short bar and the four-point-bend specimens on silicon nitride are in good agreement and relatively free of specimen geometry and size effects within the range investigated. Results on aluminum oxide were affected by specimen size and chevron-notch geometry, believed due to a rising crack growth resistance curve for the material. Only the results for the short bar specimen are presented in detail.

Shannon, J. L., Jr.↗

NASA NTRS1979

Effect of Si3N4 powder reactivity on the preparation of the Si2N2O-Al2O3 silicon aluminum oxynitride solid solution

Dense high-purity silicon aluminum oxynitride was prepared by reactive hot-pressing of an Si3N4-Al2O3-SiO2 mixture. The formation of a single-phase material was found to be critically dependent on the Si3N4 powder in the starting mixture. It is suggested that evolution of a chlorine- and nitrogen-containing species may enhance the reactivity of Si3N4 in this reaction. Densities of O prime sialons are very similar to that of Si2N2O, the widely quoted value in the ceramics literature of 3.1 g/cu cm for the density of Si2N2O being incorrect.

Sekercioglu, I.↗

NASA NTRS1980

3500-hour durability testing of ceramic materials for automotive gas turbine engines

A two-year durability program was performed by AiResearch Phoenix to evaluate four commercially available ceramic materials under simulated automotive gas turbine combustor discharge conditions. These conditions included extended cyclic thermal exposures up to 2500 F and 3500 hr. The four materials selected for evaluation were Norton NCX-34 hot pressed silicon nitride, AiResearch RBN 101 reaction bonded silicon nitride, Carborundum pressureless sintered alpha-SiC and Pure Carbon Co. (British Nuclear Fuels, Ltd.) Refel reaction sintered silicon carbide. These materials were initially exposed to 350 hr/1750 cycles at 1200 and 1370 C. Subsequent exposures to 1050, 2100 and 3500 hr were performed on those materials maintaining 50% of baseline strength after the initial exposure. Additional evaluations of exposed bars included dimensional and weight changes, dye penetrant, specific damping capacity changes, SEM fractography, and X-ray diffraction.

Carruthers, W. D.↗

NASA NTRS1979

Combustion rig durability testing of turbine ceramics

A test facility for cyclic exposure of ceramic test bars to 1370 C has been designed as a means of the evaluation of the material durability under high-temperature cycling, particularly in heat-engine applications. The principal features of the test rig and test procedures are briefly discussed, and test results are presented for several commercial ceramics, including hot-pressed silicon nitride, carborundum sintered alpha-SiC, siliconized SiC, and reaction-bonded silicon nitride.

Carruthers, W. D.↗

NASA NTRS1982

Graphite-Fiber-Reinforced Glass-Matrix Composite

G/GI structural composite material made of graphite fibers embedded in borosilicate glass exhibit excellent strength, fracture toughness, and dimensional stability at elevated temperatures. It is made by passing graphite-fiber yarn through slurry containing suspension of fine glass particles in carrier liquid and winding on drum to produce prepegged uniaxial tape. After drying, tapes are cut into appropriate lengths and laid up in graphite die in desired stacking scheme. Stack is consolidated by hot pressing in furnace.

Prewo, K. M.↗