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At least 55 records · Page 3

Improved processing of Si3N4

A sintered Si3N4-SiO2-Y2O3 composition, NASA 6Y, was developed that reached four-point flexural average strength/standard deviation values of 857/36, 544/33, and 462/59 MPa at room temperature, 1200, and 1370 C, respectively. These strengths represented improvements of 56, 38, and 21 percent over baseline properties at the three test temperatures. At room temperature the standard deviation was reduced by more than a factor of three. These accomplishments were realized by the iterative utilization of conventional X-radiography to characterize structural (density) uniformity as affected by systematic changes in powder processing and sintering parameters. Accompanying the improvement in mechanical properties was a change in the type of flaw causing failure from a pore to a large columnar beta-Si3N4 grain typically 40 to 80 microns, 10 to 30 microns wide, and with an aspect ratio of 5:1.

Sanders, William A.↗

SiC fiber reinforced reaction-bonded Si3N4 composites

A technique for fabricating strong and tough SiC fiber reinforced reaction bonded Si3N4 matrix composites (SiC/RBSN) was developed. Using this technique, composites containing approximately 23, 30, and 40 volume fractions of aligned 140 micron diameter, chemically vapor deposited SiC fibers were fabricated. The room temperature physical and mechanical properties were evaluated. The results for composite tensile strength, bend strength, and fracture strain indicate that the composite displays excellent properties when compared with the unreinforced matrix of comparable porosity. The composite stress at which the matrix first cracks and the ultimate composite fracture strength increase with increasing volume fraction of fibers, and the composite fails gracefully. The mechanical property data of this ceramic composite are compared with similar data for unreinforced commercially available Si3N4 materials and for SEP SiC/SiC composites.

Bhatt, Ramakrishna T.↗

Microstructural evolution on crystallizing the glassy phase in a 6 weight percent Y2O3-Si3N4 ceramic

X-ray diffraction and analytical electron microscopy have been used to study the crystallization of the grain-boundary glass in a 6 wt pct Y2O3-Si3N4 ceramic. Upon crystallization, high densities of dislocations formed in the Si3N4 grains and remained after 5 h at temperature. However, prolonged holds at the crystallization temperature effectively annealed out the dislocations. Other features present in the microstructure are characterized.

Lee, W. E.↗

High-temperature deformation and microstructural analysis for Si3N4-Sc2O3

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 triple 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↗

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.↗

Mullite fiber reinforced reaction bonded Si3N4 composites

Fracture toughnesses of brittle ceramic materials have been improved by introducing reinforcements and carefully tailored interface layers. Silicon carbide and Si3N4 have been emphasized as matrices of structural composites intended for high temperature service because they combine excellent mechanical, chemical, thermal and physical properties. Both matrices have been successfully toughened with SiC fibers, whiskers and particles for ceramic matrix composite (CMC) parts made by sintering, hot pressing or reaction forming processes. These SiC reinforced CMCs have exhibited significantly improved toughnesses at low and intermediate temperature levels, as well as retention of properties at high temperatures for selected exposures; however, they are vulnerable to attack from elevated temperature dry and wet oxidizing atmospheres after the matrix has cracked. Property degradation results from oxidation of interface layers and/or reinforcements. The problem is particularly acute for small diameter (-20 tim) polymer derived SiC fibers used for weavable toes. This research explored opportunities for reinforcing Si3N4 matrices with fibers having improved environmental stability; the findings should also be applicable to SiC matrix CMCs.

Saleh, T.↗

The Improvement of Ion Plated Ag and Au Film Adherence to Si3N4 and SiC Surfaces for Increased Tribological Performance

A modified dc-diode plating system, utilizing a metallic screen cage as a cathode and referred as SCREEN CAGE ION PLATING (SCIP), is used to deposit Ag and Au lubricating films on Si3N4 and SiC surfaces. When deposition is performed in Ar or N2, glow discharge, the surface displays poor adhesive strength (less than 5 MPa). A dramatic increase in adhesive strength (less than 80 MPa) is achieved when plating is performed in a reactive 50% 02 + 50% Ar glow discharge. The excited/ionized oxygen species (O2(+)/O(+) in the glow discharge contribute to the oxidation of the Si3N4 or SiC surfaces as determined by X-ray Photoelectron Spectroscopy (XTS) depth profiling. The reactively sputter-oxidized S3N4 or SiC surfaces and the activated-oxidized-metastable Ag or Au species formed in the plasma cooperatively contribute to the increased adherence. As a result, the linear thermal expansion coefficient mismatch at the interface is reduced. These lubricating Ag and Au films under sliding conditions reduce the friction coefficient by a factor of 2-1/2 to 4.

Spalvins, Talivaldis↗

Development and Characterization of SiC)/ MoSi2-Si3N4(p) Hybrid Composites

Intermetallic compound MoSi2 has long been known as a high temperature material that has excellent oxidation resistance and electrical/thermal conductivity. Also its low cost, high melting point (2023 C), relatively low density (6.2 g/cu cm versus 9 g/cu cm for current engine materials), and ease of machining, make it an attractive structural material. However, the use of MoSi2 has been hindered due to its poor toughness at low temperatures, poor creep resistance at high temperatures, and accelerated oxidation (also known as 'pest' oxidation) at temperatures between approximately 450 and 550 C. Continuous fiber reinforcing is very effective means of improving both toughness and strength. Unfortunately, MoSi2 has a relatively high coefficient of thermal expansion (CTE) compared to potential reinforcing fibers such as SiC. The large CTE mismatch between the fiber and the matrix resulted in severe matrix cracking during thermal cycling. Addition of about 30 to 50 vol % of Si3N4 particulate to MoSi2 improved resistance to low temperature accelerated oxidation by forming a Si2ON2 protective scale and thereby eliminating catastrophic 'pest failure'. The Si3N4 addition also improved the high temperature creep strength by nearly five orders of magnitude, doubled the room temperature toughness and significantly lowered the CTE of the MoSi2 and eliminated matrix cracking in SCS-6 reinforced composites even after thermal cycling. The SCS-6 fiber reinforcement improved the room temperature fracture toughness by seven times and impact resistance by five times. The composite exhibited excellent strength and toughness improvement up to 1400 C. More recently, tape casting was adopted as the preferred processing of MoSi2-base composites for improved fiber spacing, ability to use small diameter fibers, and for lower cost. Good strength and toughness values were also obtained with fine diameter Hi-Nicalon tow fibers. This hybrid composite remains competitive with ceramic matrix composites as a replacement for Ni-base superalloys in aircraft engine applications.

Hebsur, Mohan G.↗

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.↗

Mechanical behavior of polycrystalline ceramics: Brittle fracture of SiC-Si3N4 materials

Research on the fracture behavior of silicon nitride and silicon carbide is reported along with the role of anion impurities in the fabrication and behavior of magnesium oxide. The results of a survey of crack propagation in SiC and Si3N4 are presented. Studies in the following areas are reported: development of a fracture toughness testing technique, constant moment beam, microcrack examination, and etching techniques.

Ceipold, M. H.↗

Microstructure of hot-pressed Al2O3-Si3N4 mixtures as a function of holding temperature

Powder mixtures of 40 m/o Si3N4-60 m/o Al2O3 were hot-pressed at 4000 psi at various holding temperatures from 1100 C to 1700 C. Scanning Electron Microscopy and Transmission Electro Microscopy results were correlated to X-ray phase analysis and density measurements. The progressively developed microstructure was used to interpret the densification behavior of SiAlON. Photomicrographs of microstructures are shown.

Yeh, H. C.↗

Pressure sintering of Si3N4-Al2O3 /Sialon/

Essentially pore-free Sialon bodies were obtained by pressure sintering for three blends (mol ratios of 4:1, 2:3, and 3:2) of Si3N4 and Al2O3 powders under the conditions of 27.6 MN/sq m and a temperature of 1700 C for 2 h. These dense bodies consist mainly of a Sialon solid solution with a minor amount of a particular second phase. The higher the Al2O3 content (20 to 60 mol% range) in Sialon, the higher the densification rate. Fully dense bodies can be obtained at temperatures as low as 1500 C at 27.6 MN/sq m for 2 h with no second phase detectable by X-ray diffraction. A 100% dense body can be obtained by heating at 1700 C at 27.6 MN/sq m without a holding time.

Yeh, H. C.↗

Microstructure of hot-pressed Al2O3-Si3N4 mixtures as a function of holding temperature

Powder mixtures of 40 m/o Si3N4-60 m/o Al2O3 were hot-pressed at 4000 psi at various holding temperatures from 1100 C to 1700 C. Scanning and transmission electron microscopy results were correlated to X-ray phase analysis and density measurements. The progressively developed microstructure was used to interpret the densification behavior of SiAlON.

Yeh, H. C.↗

Effect of CeO2, MgO and Y2O3 additions on the sinterability of a milled Si3N4 with 14.5 wt% SiO2

The sinterability of alpha Si3N4 with 0-5.07 equivalent per cent of CeO2, MgO, or Y2O3 has been studied in the temperature range 1650-1820 C by density measurements and X-ray diffraction analysis. Maximum densities were obtained in the range 1765-1820 C and were 99.6% of theoretical with 2.5% CeO2; 98.5% of theoretical with 1.24 to 1.87% MgO, and 99.2% of theoretical with 2.5% Y2O3. Densities 94% or more of theoretical value were obtained with as little as 0.62 equivalent per cent additive.

Arias, A.↗

Sintered reaction bonded Si3N4 for the AGT 101 turbine rotor

The sintered reaction reaction bonded Si3N4 (SRBSN) process, with Y2O3 as a sintering aid, was selected for the fabrication of the AGT 101 turbine rotor. Experiments to determine the optimum Y2O3 composition of this system are discussed. The room temperature strength of the optimum material (RM-1) exceeds 700 MPa while the 1200 C strength exceeds 550 MPa. The slip casting fabrication technique employed for the AGT 101 simulated rotor is described. Rotors have been cast, nitrided and sintered. Densities exceeding 97% of theoretical (3.26 g/cc) have been obtained. Problems relating to sintering reproducibility, and the overall quality of the simulated rotors have been identified.

Mangels, J. A.↗

Effects of oxidation and oxidation under load on strength distributions of Si3N4

The room-temperature strength distributions of a sintered and a hot-pressed Si3N4 were examined in the as-machined condition, after oxidation at 1370 C and after oxidation under load at 1370 C. The strength-controlling flaw populations were highly transient in nature. Both the duration of oxidation and the magnitude of the applied load were observed to effect changes in strength. This dynamic situation is related to both strengthening and weakening processes, which at times may occur simultaneously in the same strength distribution.

Easler, T. E.↗

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.↗

Strength and fracture toughness of reaction-bonded Si3N4

Fracture strength and fracture toughness measurements were made on reaction-bonded Si3N4 materials with a range of alpha/beta ratios. The results do not indicate any clear relation between the modulus of rupture and the alpha/beta ratio over the range 1.5-9. Values for the modulus of rupture range from 219 to 290 MN per sq m, with an overall average of 238 MN per sq m. The notched beam fracture toughness is found to be constant over the range of microstructures produced, indicating that of the various microstructural features (e.g., alpha/beta ratio and pore size and distribution) no single element has a controlling influence over fracture toughness and the fracture surface energy.

Danforth, S. C.↗