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At least 217 records · Page 12
All sourcesNASA NTRSDOE OSTI
NASA NTRS1987

Improved silicon nitride for advanced heat engines

The technology base required to fabricate silicon nitride components with the strength, reliability, and reproducibility necessary for actual heat engine applications is presented. Task 2 was set up to develop test bars with high Weibull slope and greater high temperature strength, and to conduct an initial net shape component fabrication evaluation. Screening experiments were performed in Task 7 on advanced materials and processing for input to Task 2. The technical efforts performed in the second year of a 5-yr program are covered. The first iteration of Task 2 was completed as planned. Two half-replicated, fractional factorial (2 sup 5), statistically designed matrix experiments were conducted. These experiments have identified Denka 9FW Si3N4 as an alternate raw material to GTE SN502 Si3N4 for subsequent process evaluation. A detailed statistical analysis was conducted to correlate processing conditions with as-processed test bar properties. One processing condition produced a material with a 97 ksi average room temperature MOR (100 percent of goal) with 13.2 Weibull slope (83 percent of goal); another condition produced 86 ksi (6 percent over baseline) room temperature strength with a Weibull slope of 20 (125 percent of goal).

Yeh, Hun C.↗
NASA NTRS1988

Reactions of silicon-based ceramics in mixed oxidation chlorination environments

The reaction of silicon-based ceramics with 2 percent Cl2/Ar and 1 percent Cl2/1 percent to 20 percent O2/Ar at 950 C was studied with thermogravimetric analysis and high-pressure mass spectrometry. Pure Si, SiO2, several types of SiC, and Si3N4 were examined. The primary corrosion products were SiCl4(g) and SiO2(s) with smaller amounts of volatile silicon oxychlorides. The reactions appear to occur by chlorine penetration of the SiO2 layer, and gas-phase diffusion of the silicon chlorides away from the sample appears to be rate limiting. Pure SiO2 shows very little reaction with Cl2, SiC with excess Si is more reactive than the other materials with Cl2, whereas SiC with excess carbon is more reactive than the other materials with Cl2/O2. Si3N4 shows very little reaction with Cl2. These differences are explained on the basis of thermodynamic and microstructural factors.

Marra, John E.↗
NASA NTRS1988

Auger analysis of a fiber/matrix interface in a ceramic matrix composite

Auger electron spectroscopy (AES) depth profiling was used to characterize the fiber/matrix interface of an SiC fiber, reaction bonded Si3N4 matrix composite. Depth profiles of the as received double coated fiber revealed concentration oscillations which disappeared after annealing the fiber in the environment used to fabricate the composite. After the composite was fractured, the Auger depth profiles showed that failure occurred in neither the Beta-SiC fiber body nor in the Si3N4 matrix but, concurrently, at the fiber coating/matrix interface and within the fiber coating itself.

Honecy, Frank S.↗
NASA NTRS1990

Matrix density effects on the mechanical properties of SiC/RBSN composites

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.↗
NASA NTRS1990

Studies on the use of supercritical ammonia for ceramic nitride synthesis and fabrication

The extractability of ammonia halides (including ammonium thiocyanate) formed as byproducts from the synthesis of Si(NH)2 via ammonolysis of the corresponding silicon tetrahalides using supercritical NH3 as the extraction medium was investigated. It was found that the NH4SCN byproduct of ammonolysis of Si(SCN)4 can be almost completely extracted from the insoluble Si(NH)2 forming a promising system for the synthesis of pure Si(NH)2, one of the best precursors for Si3N4. In addition it was found that Si3N4, AlN, BN, and Si(NH)2 are insoluble in SC ammonia. Also discussed are design considerations for a supercritical ammonia extraction unit.

Cornell, Linda↗
NASA NTRS1989

Microstructural changes in beta-silicon nitride grains upon crystallizing the grain-boundary glass

Crystallizing the grain-boundary glass of a liquid-phase-sintered Si3N4 ceramic for 2 h or less at 1500 C led to formation of delta-Y2Si2O7. After 5 h at 1500 C, the delta-Y2Si2O7 had transformed to beta-Y2Si2O7 with a concurrent dramatic increase in dislocation density within beta-Si3N4 grains. Reasons for the increased dislocation density are discussed. Annealing for 20 h at 1500 C reduced dislocation densities to the levels found in as-sintered material.

Lee, William E.↗
NASA NTRS1989

Slurry-pressing consolidation of silicon nitride

A baseline slurry-pressing method for a silicon nitride material is developed. The Si3N4 composition contained 5.8 wt percent SiO2 and 6.4 wt percent Y2O3. Slurry-pressing variables included volume percent solids, application of ultrasonic energy, and pH. Twenty vol percent slurry-pressed material was approximately 11 percent stronger than both 30 vol percent slurry-pressed and dry-pressed materials. The Student's t-test showed the difference to be significant at the 99 percent confidence level. Twenty volume percent (300 h) slurry-pressed test bars exhibited strengths as high as 980 MPa. Large, columnar beta-Si3N4 grains caused failure in the highest strength specimens. The improved strength correlated with better structural uniformity as determined by radiography, optical microscopy, and image analysis.

Sanders, William A.↗
NASA NTRS1990

Active-to-passive transition in the oxidation of silicon carbide and silicon nitride in air

The active-to-passive transition in the oxidation of SiC and Si3N4 was determined in a flowing air environment as a function of temperature and total pressure. The experimentally observed transition temperatures ranged from a low of 1347 C to a high of 1543 C for partial pressures of oxygen of 2.5 and 123.2 Pa, respectively. The SiC and Si3N4 samples had approximately the same transition point for a given pressure. In general, the higher the flow rate, the higher the transition temperature for a given pressure. The transitions for SiC measured in this study agree with previous data for the transition of SiC measured in pure oxygen at reduced pressures and in oxygen inert gas mixtures.

Vaughn, Wallace L.↗
NASA NTRS1990

Development of impact design methods for ceramic gas turbine components

Impact damage prediction methods are being developed to aid in the design of ceramic gas turbine engine components with improved impact resistance. Two impact damage modes were characterized: local, near the impact site, and structural, usually fast fracture away from the impact site. Local damage to Si3N4 impacted by Si3N4 spherical projectiles consists of ring and/or radial cracks around the impact point. In a mechanistic model being developed, impact damage is characterized as microcrack nucleation and propagation. The extent of damage is measured as volume fraction of microcracks. Model capability is demonstrated by simulating late impact tests. Structural failure is caused by tensile stress during impact exceeding material strength. The EPIC3 code was successfully used to predict blade structural failures in different size particle impacts on radial and axial blades.

Song, J.↗
NASA NTRS1990

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.↗
NASA NTRS1991

Microstructural changes in Beta-silicon nitride grains upon crystallizing the grain-boundary glass

Crystallizing the grain boundary glass of a liquid phase sintered Si3N4 ceramic for 2 h or less at 1500 C led to formation of gamma Y2Si2O7. After 5 h at 1500 C, the gamma Y2Si2O7 had transformed to beta Y2Si2O7 with a concurrent dramatic increase in dislocation density within beta Si3N4 grains. Reasons for the increased dislocation density is discussed. Annealing for 20 h at 1500 C reduced dislocation densities to the levels found in as-sintered materials.

Lee, William E.↗
NASA NTRS1991

Precautions toward XTEM of Si3N4/SiO2

Severe difficulties are encountered in the preparation of oxidized Si3N4 specimens for XTEM transmission electromicroscopic inspection, in virtue of the extreme difference between Si3N4 and SiO2 mechanical properties. Attention is presently given to a preparation method in which an overlayer of the nitride is always occluded; this protects the oxide through most of the thinning that specimen preparation entails. An XTEM image of the oxide/nitride interface is presented.

Ogbuji, Linus U. J. T.↗
NASA NTRS1992

Fiber coating/matrix reactions in silicon-base ceramic matrix composites

The Knudsen cell technique and coupons of carbon coated Si3N4 and BN coated SiC were employed to study the possible reactions at the SiC/C/Si3N4 and SiC/BN/SiC interface. Carbon reacts with Si3N4 to form gaseous N2 and solid SiC. Solid SiC acts as a physical barrier to the reaction, which prevents the generation of high N2 pressure predicted from thermochemical calculations. Thus, deleterious effects of the reaction to the composite are limited. Limited reactions between BN and C-rich SiC was observed. However, the vapor pressure was so low that it is not likely to cause any interfacial instability. The predicted formation of a BN-C solid solution was not observed.

Lee, K. N.↗
NASA NTRS1992

Environmental durability of ceramics and ceramic composites

An account is given of the current understanding of the environmental durability of both monolithic ceramics and ceramic-matrix composites, with a view to the prospective development of methods for the characterization, prediction, and improvement of ceramics' environmental durability. Attention is given to the environmental degradation behaviors of SiC, Si3N4, Al2O3, and glass-ceramic matrix compositions. The focus of corrosion prevention in Si-based ceramics such as SiC and Si3N4 is on the high and low sulfur fuel combustion-product effects encountered in heat engine applications of these ceramics; sintering additives and raw material impurities are noted to play a decisive role in ceramics' high temperature environmental response.

Fox, Dennis S.↗
NASA NTRS1992

High-temperature deformation and microstructural analysis for silicon nitride-scandium(III) oxide

It was indicated that Si3N4 doped with Sc2O3 may exhibit high temperature mechanical properties superior to Si3N4 systems with various other oxide sintered additives. High temperature deformation of samples was studied by characterizing the microstructures before and after deformation. It was found that elements of the additive, such as Sc and O, exist in small amounts at very thin grain boundary layers and most of them stay in secondary phases at tripple and multiple grain boundary junctions. These secondary phases are devitrified as crystalline Sc2Si2O7. Deformation of the samples was dominated by cavitational processes rather than movements of dislocations. Thus the excellent deformation resistance of the samples at high temperature can be attributed to the very small thickness of the grain boundary layers and the crystalline secondary phase.

Cheong, Deock-Soo↗
NASA NTRS1992

Elevated-temperature fracture resistances of monolithic and composite ceramics using chevron-notched bend tests

The quasi-static fracture behaviors of monolithic ceramics (SiC, Si3N4, MgAl2O4), self-reinforced monoliths (acicular grained Si3N4, acicular grained mullite), and ceramic matrix composites (SiC whisker/Al2O3 matrix, TiB2 particulate/SiC matrix, SiC fiber/CVI SiC matrix, Al2O3 fiber/CVI SiC matrix) were measured over the temperature range of 20 to 1400 C. The chevron notched, bend bar test geometry was essential for characterizing the elevated temperature fracture resistances of this wide range of quasi-brittle materials during stable crack growth. Fractography revealed the differences in the fracture behavior of the different materials at the various temperatures. The fracture resistances of the self-reinforced monoliths were comparable to those of the composites and the fracture mechanisms were found to be similar at room temperature. However at elevated temperatures the differences of the fracture behavior became apparent where the superior fracture resistance of the self-reinforced monoliths were attributed to the minor amounts of glassy, intergranular phases which were often more abundant in the composites and affected the fracture behavior when softened by elevated temperatures.

Ghosh, Asish↗
NASA NTRS1994

The Effect of Polymer Char on Nitridation Kinetics of Silicon

Effects of polymer char on nitridation kinetics of attrition milled silicon powder have been investigated from 1200 to 1350 C. Results indicate that at and above 1250 C, the silicon compacts containing 3.5 wt percent polymer char were fully converted to Si3N4 after 24 hr exposure in nitrogen. In contrast, the silicon compacts without polymer char could not be fully converted to Si3N4 at 1350 C under similar exposure conditions. At 1250 and 1350 C, the silicon compacts with polymer char showed faster nitridation kinetics than those without the polymer char. As the polymer char content is increased, the amount of SiC in the nitrided material is also increased. By adding small amounts (approx. 2.5 wt percent) of NiO, the silicon compacts containing polymer char can be completely nitrided at 1200 C. The probable mechanism for the accelerated nitridation of silicon containing polymer char is discussed.

Chan, Rickmond C.↗
NASA NTRS1995

Enhancement of perfluoropolyether boundary lubrication performance: I. Preliminary results

A ball bearing simulator operating under starved conditions was used to evaluate the boundary lubrication performance of a perfluoropolyether (PFPE) Krytox 143 AB. Several approaches to enhance boundary lubrication were studied. These included: (1) soluble boundary additives, (2) bearing surface modifications, (3) 'run-in' surface films, and (4) ceramic bearing components. In addition, results were compared with two non-perfluorinated liquid lubricant formulations. Based on these preliminary tests, the following tentative conclusions can be made: (1) substantial improvements in boundary lubrication performance were observed with a beta-diketone boundary additive and a tricresyl phosphate (TCP) liquid surface pretreatment; (2) the use of rough Si3N4 balls (Ra = 40 micro-in) also provided substantial improvement but with concomitant abrasive wear; (3) marginal improvements were seen with two boundary additives (a phosphine and a phosphatriazine) and a neat (100%) fluid (a carboxylic acid terminated PFPE); and surface pretreatments with a synthetic hydrocarbon, a PTFE coating, and TiC coated 440C and smooth Si3N4 balls (R(sub a) less than 1 micro-in); and (4) two non-PFPE lubricant formulations (a PAO and a synthetic hydrocarbon) yielded substantial improvements.

Jones, W. R., Jr.↗