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At least 19 records
All sourcesNASA NTRSDOE OSTI
NASA NTRS1990

Properties of RBSN and RBSN-SiC composites

Strengths, fracture toughnesses, hardnesses, and dimensional changes have been measured for RBSN and RBSN/SiC composites. Samples were made from mixtures of Si and either Si- or C-rich SiC powders. For pure, 75 pct dense RBSN dispersed with octanol, strengths up to 858 MPa have been achieved. Improved strengths result from a combination of microstructural perfection and increased fracture toughness. The mechanical properties of the composites were approximately equal to those of methanol processed RBSN but not quite equal to those of the octanol-processed RBSN. Results are discussed in terms of observed microstructural features.

Lightfoot, A.↗
NASA NTRS1992

Effect of HIPing on the effective thermal conductivity/diffusivity and the interfacial thermal conductance of uniaxial SiC fibre-reinforced RBSN

Hot isostatic pressing (HIPing) was found to increase the thermal diffusivity/conductivity of uniaxial silicon carbide fiber-reinforced reaction-bonded silicon nitride (RBSN) matrix composites, as the result of the densification of the matrix, the increase in the grain size of the silicon carbide and the improved thermal contact between the fibers and the matrix. Transverse to the fiber direction the thermal diffusivity/conductivity was found to be a function of the surrounding gaseous atmosphere due to the access of the gas phase to the fiber-matrix interface, which was facilitated by the existence of an interfacial gap due to the thermal expansion mismatch between the fibers and the matrix. The interfacial conductance was found to exhibit a strong positive temperature dependence as the result of the closure of the interfacial gap with increasing temperature.

Bhatt, H.↗
NASA NTRS1980

Development of moldable, high density reaction bonded silicon nitride

It is noted that currently available reaction bonded silicon nitride (RBSN) materials are limited by relatively low strength (up to 300 MPa) and oxidation resistance, primarily due to open porosity. Attention is given to technology that was developed and used to produce an improved grade of injection molded RBSN having a density of 2.8 g/cc, with significantly decreased open porosity and a strength exceeding 350 MPa. It is shown that these results are primarily due to advances in two areas: silicon powder processing, and nitriding technique. A comparison of room temperature strength and oxidation resistance of the new material with that of state-of-the-art RBSN, showed significant improvements. It is concluded that turbine stator vanes were produced to show that this improved RBSN technology has been reduced to engineering practice.

Mangels, J. A.↗
NASA NTRS1994

Oxidation Protection of Porous Reaction-Bonded Silicon Nitride

Oxidation kinetics of both as-fabricated and coated reaction-bonded silicon nitride (RBSN) were studied at 900 and 1000 C with thermogravimetry. Uncoated RBSN exhibited internal oxidation and parabolic kinetics. An amorphous Si-C-O coating provided the greatest degree of protection to oxygen, with a small linear weight loss observed. Linear weight gains were measured on samples with an amorphous Si-N-C coating. Chemically vapor deposited (CVD) Si3N4 coated RBSN exhibited parabolic kinetics, and the coating cracked severely. A continuous-SiC-fiber-reinforced RBSN composite was also coated with the Si-C-O material, but no substantial oxidation protection was observed.

Fox, D. S.↗
NASA NTRS1991

Processing and properties of SiC whisker- and particulate-reinforced reaction bonded Si3N4

The microstructure and mechanical properties of reaction bonded Si3N4 (RBSN) reinforced with SiC whiskers of particles were investigated using RBSN composites made from colloidally pressed octanol dispersions of high-purity Si powders mixed with either SiC whiskers or alpha-SiC particles. Results of investigations, revealing high conversions of Si to Si3N4, specific surface areas, and constant relative densities and strengths, showed that the uniform microstructure and small flaw size of the matrix were maintained in the composites and that no degradation of the reinforcements was taking place. Neither the monolithic nor the composite materials exhibited R-curve behavior. A modest increase in fracture toughness was observed only in the RBSN containing 33 vol pct SiC(p).

Lightfoot, A.↗
NASA NTRS1994

Effects of Thermal Cycling on Thermal Expansion and Mechanical Properties of Sic Fiber-reinforced Reaction-bonded Si3n4 Composites

Thermal expansion curves for SiC fiber-reinforced reaction-bonded Si3N4 matrix composites (SiC/RBSN) and unreinforced RBSN were measured from 25 to 1400 C in nitrogen and in oxygen. The effects of fiber/matrix bonding and cycling on the thermal expansion curves and room-temperature tensile properties of unidirectional composites were determined. The measured thermal expansion curves were compared with those predicted from composite theory. Predicted thermal expansion curves parallel to the fiber direction for both bonding cases were similar to that of the weakly bonded composites, but those normal to the fiber direction for both bonding cases resulted in no net dimensional changes at room temperature, and no loss in tensile properties from the as-fabricated condition. In contrast, thermal cycling in oxygen for both composites caused volume expansion primarily due to internal oxidation of RBSN. Cyclic oxidation affected the mechanical properties of the weakly bonded SiC/RBSN composites the most, resulting in loss of strain capability beyond matrix fracture and catastrophic, brittle fracture. Increased bonding between the SiC fiber and RBSN matrix due to oxidation of the carbon-rich fiber surface coating and an altered residual stress pattern in the composite due to internal oxidation of the matrix are the main reasons for the poor mechanical performance of these composites.

Bhatt, R. T.↗
NASA NTRS1995

Heat Treatment Effects on the Tensile Properties and Microstructures of a SiC/RBSN Composite in Nitrogen

The room-temperature tensile properties and constituent microstructures of a unidirectionally reinforced SiC/reaction bonded silicon nitride (RBSN) composite have been investigated after heat treatments at 1400, 1600, or 1800 C in nitrogen for up to 100 hr. The composite consisted of approximately 24 vol% of aligned 140 micron diameter, continuous length, chemically vapor deposited SiC fibers in an approximately 40% porous silicon nitride matrix. The composites heat treated at 1400 C for up to 100 hr showed elastic modulus, first matrix cracking strength, and ultimate tensile strength values similar to those of the as-fabricated composites, but those heat treated for 1 hr beyond this temperature displayed losses in all three properties. Recrystallization of the SiC fibers, reaction between the carbon-rich interface coating on the fibers and the RBSN matrix, and dissociation of the RBSN matrix are the reasons for the loss of mechanical properties.

Bhatt, R. T.↗
NASA NTRS2000

Effects of Interface Coating and Nitride Enhancing Additive on Properties of Hi-Nicalon SiC Fiber Reinforced Reaction-Bonded Silicon Nitride Composites

Strong and tough Hi-Nicalon SiC fiber reinforced reaction-bonded silicon nitride matrix composites (SiC/ RBSN) have been fabricated by the fiber lay-up approach. Commercially available uncoated and PBN, PBN/Si-rich PBN, and BN/SiC coated SiC Hi-Nicalon fiber tows were used as reinforcement. The composites contained approximately 24 vol % of aligned 14 micron diameter SiC fibers in a porous RBSN matrix. Both one- and two-dimensional composites were characterized. The effects of interface coating composition, and the nitridation enhancing additive, NiO, on the room temperature physical, tensile, and interfacial shear strength properties of SiC/RBSN matrix composites were evaluated. Results indicate that for all three coated fibers, the thickness of the coatings decreased from the outer periphery to the interior of the tows, and that from 10 to 30 percent of the fibers were not covered with the interface coating. In the uncoated regions, chemical reaction between the NiO additive and the SiC fiber occurs causing degradation of tensile properties of the composites. Among the three interface coating combinations investigated, the BN/SiC coated Hi-Nicalon SiC fiber reinforced RBSN matrix composite showed the least amount of uncoated regions and reasonably uniform interface coating thickness. The matrix cracking stress in SiC/RBSN composites was predicted using a fracture mechanics based crack bridging model.

Bhatt, Ramakrishana T.↗
NASA NTRS1979

Variations in pore structure of reaction-bonded silicon nitride /RBSN/

A discussion is presented relating the observed pore structures (sizes) to the reaction mechanisms in reaction-bonded silicon nitride (alpha- and beta-Si3N4) on the basis of information available from the literature. While the techniques for reducing the residual macroporosity are quite well-developed for reaction-bonded Si3N4 (RBSN), it is important to be aware of three other orders of magnitude for porosity present in RBSN as a result of the nitriding process itself, and how these types of nitridation-induced porosity can be controlled. For ease of description, these types of nitridation-induced porosity are called micropores, nanopores, and picopores in order of their decreasing size. A scanning electron micrograph is presented, showing nanopores isolated in the unreacted Si and picopores in the alpha-matte Si3N4. The assumption that an alpha-matte growth mechanism is active explains the occurrence of nanopores and their partial filling with alpha-Si3N4, leaving behind very fine-grained alpha-matte and picopores.

Danforth, S. C.↗
NASA NTRS1979

Formation of porous surface layers in reaction bonded silicon nitride during processing

Microstructural examination of reaction bonded silicon nitride (RBSN) has shown that there is often a region adjacent to the as-nitrided surfaces that is even more porous than the interior of this already quite porous material. Because this layer of large porosity is considered detrimental to both the strength and oxidation resistance of RBSN, a study was undertaken to determine if its formation could be prevented during processing. All test bars studied were made from a single batch of Si powder which was milled for 4 hours in heptane in a vibratory mill using high density alumina cylinders as the grinding media. After air drying the powder, bars were compacted in a single acting die and hydropressed.

Shaw, N. J.↗
NASA NTRS1982

Oxidation stability of advanced reaction-bonded Si3N4 materials

Four slip-cast, injection-molded and isostatically-pressed specimens of reaction-bonded silicon nitride (RBSN) were subjected to static oxidation tests at 900 C for 10 hours. Specimens containing 8-10% interconnected open porosity of size greater than one micron exhibited a 20-30% decrease in average room temperature four-point flexure strength, while those with 10% open porosity of magnitudes much smaller than one micron as well as those with 2-4% interconnected open porosity of about one micron did not decrease in strength after 900 C exposure. It was determined that preoxidation treatment at 1350 C prevents the 20-30% strength degradation due to internal oxidation, and evidence is presented which suggests that surface pit formation in some RBSN may result from contamination by the furnace environment rather than any intrinsic material properties.

Lindberg, L. J.↗
NASA NTRS1985

Iron impurities in Si3N4 processing

The atomic environment of iron impurities is investigated during the processing cycle of reaction-bonding silicon nitride (RBSN). Several analysis techniques are utilized, including X-ray photoelectron spectroscopy (XPS), extended X-ray absorption fine structure (EXAFS), and electron spin resonance (ESR), to examine iron impurities in the starting silicon powder, in sintered silicon compacts, and in RBSN materials. Results indicate that iron impurities in as-received metallurgical grade silicon powder are incorporated in the silicon bulk as a highly distorted FeSi2 compound. No surface iron or iron-based particulate is observed in the starting material. Upon sintering, the iron environment becomes an ordered FeSi2 structure. In the RBNS material, the FeSi2 structure is again distorted, as observed by both EXAFS and ESR.

Bouldin, C. E.↗
NASA NTRS1986

Effect of loading rate on dynamic fracture of reaction bonded silicon nitride

Wedge-loaded, modified tapered double cantilever beam (WL-MTDCB) specimens under impact loading were used to determine the room temperature dynamic fracture response of reaction bonded silicon nitride (RBSN). The crack extension history, with the exception of the terminal phase, was similar to that obtained under static loading. Like its static counterpart, a distinct crack acceleration phase, which was not observed in dynamic fracture of steel and brittle polymers, was noted. Unlike its static counterpart, the crack continued to propagate at nearly its terminal velocity under a low dynamic stress intensity factor during the terminal phase of crack propagation. These and previously obtained results for glass and RBSN show that dynamic crack arrest under a positive dynamic stress intensity factor is unlikely in static and impact loaded structural ceramics.

Liaw, B. M.↗
NASA NTRS1987

Durability characterization of ceramic materials for gas turbines

The strength retention of ceramic materials during extended high-temperature cyclic exposure is critical to their widespread application in gas turbine engines. During a continuing NASA funded program initated in 1979, reaction bonded silicon nitride (RBSN), sintered silicon carbide (SSC), reaction sintered silicon carbide (RSSC), and sintered silicon nitride (SSN) materials were evaluated following simulated gas turbine engine exposures. Exposures were performed by cycling specimens five times per hour between a high velocity burner discharge and a rapid air quench. The retained flexural strengths were determined following up to 3500 hours of exposure at temperatures up to 1370 C. Post-exposure strengths have been correlated with fractography and surface examination using SEM. Results illustrate excellent strength retention of SSC materials after 3500 hours of exposure to 1370 C. At 1200 C, RBSN and RSSC also demonstrate significant strength retention. Although SSN materials typically suffer significant strength losses during exposures at 1200 C, a new composition, which has improved high-temperature strength, also shows improved durability. In the majority of the materials, strength loss is typically associated with flaw formation in the protective SiO2 layer.

Carruthers, W. D.↗
NASA NTRS1988

Laminate behavior for SiC fiber-reinforced reaction-bonded silicon nitride matrix composites

The room temperature mechanical properties of SiC fiber reinforced reaction-bonded silicon nitride matrix composite laminates (SiC/RBSN) have been measured. The laminates contained approx 30 volume fraction of aligned 142-micron diameter SiC fiber in a porous RBSN matrix. Three types of laminate studied were unidirectional: (1) (0) sub 8, (2) (10) sub 8, and (3) (45) sub 8, and (90) sub 8; cross plied laminates (0 sub 2/90 sub 2); and angle plied laminates: (+45 sub 2/-45 sub 2). Each laminate contained eight fiber plies. Results of the unidirectionally reinforced composites tested at various angles to the reinforcement direction indicate large anisotropy in in-plane properties. In addition, strength properties of these composites along the fiber direction were independent of specimen gage length and were unaffected by notches normal to the fiber direction. Splitting parallel to the fiber at the notch tip appears to be the dominant crack blunting mechanism responsible for notch insensitive behavior of these composites. In-plane properties of the composites can be improved by 2-D laminate construction. Mechanical property results for (0 sub 2/90 sub 2)sub s and (+45/-45 sub 2) sub s laminates showed that their matrix failure strains were similar to that for (0) sub 8 laminates, but their primary elastic moduli, matrix cracking strengths, and ultimate composite strengths were lower. The elastic properties of unidirectional, cross-ply, and angle-ply composites can be predicted from modified constitutive equations and laminate theory. Further improvements in laminate properties may be achieved by reducing the matrix porosity and by optimizing the bond strength between the SiC fiber and RBSN matrix.

Rhatt, R. T.↗
NASA NTRS1988

Preparation and evaluation of silicon nitride matrices for silicon nitride-SiC fiber composites

Continuous silicon carbide (SiC) fiber was added to three types of silicon nitride (Si3N4) matrices. Efforts were aimed at producing a dense Si3N4 matrix from reaction-bonded silicon nitride (RBSN) by hot-isostatic-pressing (HIP) and pressureless sintering, and from Si3N4 powder by hot-pressing. The sintering additives utilized were chosen to allow for densification, while not causing severe degradation of the fiber. The ceramic microstructures were evaluated using scanning optical microscopy. Vickers indentation was used to determine the microhardness and fracture toughness values of the matrices. The RBSN matrices in this study did not reach more than 80 percent of theoretical density after sintering at various temperatures, pressures, and additive levels. Hot-pressing Si3N4 powder produced the highest density matrices; hardness and toughness values were within an order of magnitude of the best literature values. The best sintering aid composition chosen included Y2O3, SiO2, and Al2O3 or AlN. Photomicrographs demonstrate a significant reduction of fiber attack by this additive composition.

Axelson, Scott R.↗
NASA NTRS1990

Laminate behavior for SiC fiber-reinforced reaction-bonded silicon nitride matrix composites

The room temperature mechanical properties of SiC fiber reinforced reaction-bonded silicon nitride matrix composite laminates (SiC/RBSN) have been measured. The laminates contained approx 30 volume fraction of aligned 142-micron diameter SiC fiber in a porous RBSN matrix. Three types of laminate studied were unidirectional: (1) (0) sub 8, (2) (10) sub 8, and (3) (45) sub 8, and (90) sub 8; cross plied laminates (0 sub 2/90 sub 2); and angle plied laminates: (+45 sub 2/-45 sub 2). Each laminate contained eight fiber plies. Results of the unidirectionally reinforced composites tested at various angles to the reinforcement direction indicate large anisotropy in in-plane properties. In addition, strength properties of these composites along the fiber direction were independent of specimen gage length and were unaffected by notches normal to the fiber direction. Splitting parallel to the fiber at the notch tip appears to be the dominant crack blunting mechanism responsible for notch insensitive behavior of these composites. In-plane properties of the composites can be improved by 2-D laminate construction. Mechanical property results for (0 sub 2/90 sub 2) sub s and (+45/-45 sub 2) sub s laminates showed that their matrix failure strains were similar to that for (0) sub 8 laminates, but their primary elastic moduli, matrix cracking strengths, and ultimate composite strengths were lower. The elastic properties of unidirectional, cross-ply, and angle-ply composites can be predicted from modified constitutive equations and laminate theory. Further improvements in laminate properties may be achieved by reducing the matrix porosity and by optimizing the bond strength between the SiC fiber and RBSN matrix.

Bhatt, Ramakrishna T.↗
NASA NTRS1992

Relationships between toughness and microstructure of reaction bonded Si3N4

Fracture toughnesses of nominally identical batches of reaction bonded silicon nitride (RBSN) differed significantly (about 2.0 and about 2.7 MPa sq rt m). Detailed fractographic and microstructural characterizations investigated underlying factors. Subtile differences between high and low toughness RBSN and between constituent Si powders have been revealed through SEM/FEG, TEM, BET, Hg-porosimetry, and XRD. The results illustrate the need for behavioral models to guide microstructural design and to interpret properties of brittle materials with intermediate levels of porosity.

Lightfoot, Annamarie↗