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At least 19 records

The effect of preparation conditions on the structure and mechanical properties of reaction-sintered silicon nitride

The microstructure of reaction sintered silicon nitride (RSSN) was changed over a wide range by varying the grain density, grain size of the silicon starting powder, nitriding conditions, and by introducing artificial pores. The influence of single microstructural parameters on mechanical properties like room temperature strength, creep behavior, and resistance to thermal shock was investigated. The essential factors influencing these properties were found to be total porosity, pore size distribution, and the fractions of alpha and beta Si3N4. In view of high temperature engineering applications of RSSN, potentials for optimizing the material's properties by controlled processing are discussed.

Heinrich, J.↗

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.↗

Development of energy-absorbing reaction-sintered Si3N4 surface layers on hot-pressed Si3N4

Energy-absorbing Si3N4 surface layers on dense Si3N4 substrates were formed by in-place nitridation of fine-grained silicon powder. Ballistic impact tests performed on samples with 1-mm thick layers at room temperature and 1370 C showed up to an eightfold increase in the energy necessary to fracture the substrate. For maximum impact resistance, a small amount (about 20 vol %) of residual Si must be present in the reaction-sintered Si3N4 surface layer. Thermal cycling to 1370 C did not affect impact resistance, even though a considerable amount of SiO2 formed within the reaction-sintered Si3N4 layer during cycling. Erosion testing of samples in a Mach 0.8 burner rig at 1370 C resulted in minimal surface recession of the surface layer. Chemically vapor-deposited SiC-coated material similarly tested exhibited no surface recession.

Brennan, J. J.↗

Improved reaction sintered silicon nitride

Processing treatments were applied to as-nitrided reaction sintered silicon nitride (RSSN) with the purposes of improving strength after processing to above 350 MN/m2 and improving strength after oxidation exposure. The experimental approaches are divided into three broad classifications: sintering of surface-applied powders; impregnation of solution followed by further thermal processing; and infiltration of molten silicon and subsequent carburization or nitridation of the silicon. The impregnation of RSSN with solutions of aluminum nitrate and zirconyl chloride, followed by heating at 1400-1500 C in a nitrogen atmosphere containing silicon monoxide, improved RSSN strength and oxidation resistance. The room temperature bend strength of RSSN was increased nearly fifty percent above the untreated strength with mean absolute strengths up to 420 MN/m2. Strengths of treated samples that were measured after a 12 hour oxidation exposure in air were up to 90 percent of the original as-nitrided strength, as compared to retained strengths in the range of 35 to 60 percent for untreated RSSN after the same oxidation exposure.

Baumgartner, H. R.↗

Effect of attrition milling on the reaction sintering of silicon nitride

Silicon powder was ground in a steel attrition mill under nitrogen. Air exposed powder was compacted, prefired in helium, and reaction sintered in nitrogen-4 v/o hydrogen. For longer grinding times, oxygen content, surface area and compactability of the powder increased; and both alpha/beta ratio and degreee of nitridation during sintering increased. Iron content remained constant.

Herbell, T. P.↗

Effect of attrition milling on the reaction sintering of silicon nitride

Silicon powder was ground in a steel attrition mill under nitrogen. Air-exposed powder was compacted, prefired in helium, and reaction-sintered in nitrogen-4 v/o hydrogen. For longer grinding times, oxygen content, surface area and compactability of the powder increased; and both alpha/beta ratio and degree of nitridation during sintering increased. Iron content remained constant.

Herbell, T. P.↗

Strength of hot isostatically pressed and sintered reaction bonded silicon nitrides containing Y2O3

The hot isostatic pressing of reaction bonded Si3N4 containing Y2O3 produced specimens with greater room temperature strengths than those by high pressure nitrogen sintering of the same material. Average room temperature bend strengths for hot isostatically pressed reaction bonded silicon nitride and high pressure nitrogen sintered reaction bonded silicon nitride were 767 and 670 MPa, respectively. Values of 472 and 495 MPa were observed at 1370 C. For specimens of similar but lower Y2O3 content produced from Si3N4 powder using the same high pressure nitrogen sintering conditions, the room temperature strength was 664 MPa and the 1370 C strength was 402 MPa. The greater strengths of the reaction bonded silicon nitride materials in comparison to the sintered silicon nitride powder material are attributed to the combined effect of processing method and higher Y2O3 content.

William A Sanders↗

Ceramics in gas turbine: Powder and process characterization

Some of the intrinsic properties of various forms of Si3N4 and SiC are listed and limitations of such materials' availability are pointed out. The essential features/parameters to characterize a batch of powder are 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. 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.↗

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.↗

Sintering of reaction bonded silicon nitride

A process to produce sintered reaction-bonded Si3N4 (SRBSN) articles has been developed. This process consists of the addition of an appropriate sintering aid to reaction-bonded Si3N4 followed by sintering between 1780 and 2000 C, using an over pressure of nitrogen. The principal advantage of this process is the low sintering shrinkages of 5 to 10 percent. The properties and microstructure of two SRBSN systems sintered with MgO and Y2O3 additives are described and were found to be comparable to corresponding hot-pressed Si3N4 systems. Examples of applications of both systems are illustrated, demonstrating near net shape fabrication capability of the process.

Mangels, J. A.↗

Fracture of yttria-doped, sintered reaction-bonded silicon nitride

Flexural strength of an yttria-doped, slip-cast, sintered reaction-bonded silicon nitride was evaluated as a function of temperature (20 to 1400 C in air), applied stress, and time. Static oxidation at 700 to 1400 C was investigated in detail; in tests at 1000 C in air, the material showed anomalous weight gain. Flexural stress-rupture testing at 800 to 1200 C in air indicated that the material is susceptible to stress-enhanced oxidation and early failure. Fractographic evidence for time-dependent and -independent failures is presented.

Govila, R. K.↗

Fracture of flash oxidized, yttria-doped sintered reaction-bonded silicon nitride

The oxidation behavior of a slip cast, yttria-doped, sintered reaction-bonded silicon nitride after 'flash oxidation' was investigated. It was found that both the static oxidation resistance and flexural stress rupture life (creep deformation) were improved at 1000 C in air compared to those of the same material without flash oxidation. Stress rupture data at high temperatures (1000 to 1200 C) are presented to indicate applied stress levels for oxidation-dependent and independent failures.

Govila, R. K.↗

Silicon nitride: A ceramic material with outstanding resistance to thermal shock and corrosion

The known physical, mechanical and chemical properties of reaction-sintered silicon nitride are summarized. This material deserves interest especially because of its unusually good resistance to thermal shock and corrosion at high temperatures. Two types are distinguished: reaction-sintered (porous) and hot-pressed (dense) Si3N4. Only the reaction-sintered material which is being produced today in large scale as crucibles, pipes, nozzles and tiles is considered.

Huebner, K. H.↗

Improved performance of silicon nitride-based high temperature ceramics

Recent progress in the production of Si3N4 based ceramics is reviewed: (1) high temperature strength and toughness of hot pressed Si3N4 were improved by using high purity powder and a stabilized ZrO2 additive, (2) impact resistance of hot pressed Si3N4 was increased by the use of a crushable energy absorbing layer, (3) the oxidation resistance and strength of reaction sintered Si3N4 were increased by impregnating reaction sintered silicon nitride with solutions that oxidize to Al2O3 or ZrO2, (4) beta prime SiA1ON compositions and sintering aids were developed for improved oxidation resistance or improved high temperature strength.

Ashbrook, R. L.↗

Development of silicon nitride of improved toughness

The application of reaction sintered Si2N4 energy absorbing surface layers to hot-pressed Si3N4 was investigated. The surface layer was formed by in-place nitridation of silicon powder. It was found that reaction sintered Si3N4 layers of 1 mm thickness, fabricated from either -100, +200, -200, or -325 mesh Si powder and nitrided in 96% N2/4% H2 so that approximately 20-25 vol % unnitrided Si remained in the layer, resulted in a sevenfold increase in ballistic impact resistance of a 0.64 cm thick hot-pressed SI3N4 substrate from RT 1370 C. Both NC-132 SI3N4, with MgO additive, and NCX-34 Si3N4, with Y2O3 additive, were evaluated as substrate material. The finer grain size -200 and -325 mesh nitrided Si layers were for their smoothness and relatively high density. It was found that nitriding in N2/H2 mixtures, rather than pure N2, resulted in a microstructure that did not substantially degrade the strength of the hot-pressed Si3N4 substrate. Thermal cycling tests on the RSSN/HPSN combinations from 200 C to 1370 C for 75 cycles in air did not degrade the impact resistance nor the interfacial bonding, although a large amount of internal silica formation occurred within the RSSN layer. Mach 0.8, 5 hr, hot gas erosion tests showed no surface recession of RSSN layers at 1200 C and slight surface recession at 1370 C.

Brennan, J. J.↗

Development of Si3N4 and SiC of improved toughness

The application of energy absorbing surface layers to Si3N4 and SiC was investigated. Among the layers studied were microcracked materials such as iron titanate and a silica-zircon mixture and porous materials such as reaction sintered Si3N4. Energy absorption due to microcrack extension upon impact was found not to be an important mechanism. Instead, the fivefold improvement in Charpy and ballistic impact at elevated temperature (1250 C and 1370 C) found for Fe2TiO5 was due to plastic deformation while similar improvement found for silica-zircon mixtures at RT was due to crushing of the porous material. Due to thermal expansion mismatch, these two materials could not withstand thermal cycling when used as energy absorbing surface layers on Si3N4. Reaction sintered Si3N4 layers on dense Si3N4 were found to give up to a sevenfold increase in ballistic impact resistance due to crushing of the layer upon impact. High porosity (45%), large particle size R.S. Si3N4 layers fabricated from -100, +200 mesh Si powder gave better impact improvement than less porous (30%), small particle size layers fabricated from -325 mesh Si powder.

Brennan, J. J.↗

Phenomenological study of the behavior of some silica formers in a high velocity jet fuel burner

Samples of four silica formers: single crystal SiC, sintered alpha-SiC, reaction sintered Si3N4 and polycrystalline MoSi2, were subjected to a Mach 1 jet fuel burner for 1 hr, at a sample temperature of 1375 deg C (2500 deg F). Two phenomena were identified which may be deleterious to a gas turbine application of these materials. The glass layer formed on the MoSi2 deformed appreciably under the aerodynamic load. A scale developed on the samples of the other materials which consisted of particular matter from the gas stream entrapped in a SiO2 matrix.

Cawley, J. D.↗