Silicon nitride powder
The characteristics and preparation methods of Si3N4 are reviewed. Special emphasis is placed on the correlation between impurities and strength of sintered Si3N4.
Mori, M.↗
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Study of the pore structure of ceramics prepared by the slip casting method
The porosity of the slip cast Si3N4 is similar to that of pressed Si3N4 formed at 2500 kg/sq cm. The porosity of cast Si oxynitride is equivalent to that of samples stressed at 10,000 kg/sq cm. Crucibles formed from these materials by slip casting have high thermal shock and corrosion resistance.
Guzman, I. Y.↗
Radiographic detectability limits for seeded voids in sintered silicon carbide and silicon nitride
Conventional and microfocus X-radiographic techniques were compared to determine relative detectability limits for voids in green and sintered SiC and Si3N4. The relative sensitivity of the techniques was evaluated by comparing their ability to detect voids that were artificially introduced by a seeding process. For projection microfocus radiography the sensitivity of void detection at a 90/95 probability of detection/confidence level is 1.5% of specimen thickness in sintered SiC and Si3N4. For conventional contact radiography the sensitivity is 2.5% of specimen thickness. It appears that microfocus projection radiography is preferable to conventional contact radiography in cases where increased sensitivity is required and where the additional complexity of the technique can be tolerated.
Baaklini, G. Y.↗
Preparation of silicon carbide-silicon nitride fibers by the pyrolysis of polycarbosilazane precursors
The development of silicon carbide-silicon nitride fibers (SiC-Si3N4) by the pyrolysis of polycarbosilazane precursors is reviewed. Precursor resin, which was prepared by heating tris(N-methylamino)methylsilane or tris(N-methylamino)phenylsilane to about 520 C, was drawn into fibers from the melt and then made unmeltable by humidity conditioning at 100 C and 95 percent relative humidity. The humidity treated precursor fibers were pyrolyzed to ceramic fibers with good mechanical properties and electrical resistivity. For example, SiC-Si3N4 fibers derived from tris(N-methylamino)methylsilane had a tensile rupture modulus of 29 million psi and electrical resistivity of 6.9 x ten to the 8th power omega-cm, which is ten to the twelfth power times greater than that obtained for graphite fibers.
Penn, B. G.↗
Oxidation of silicon nitride sintered with rare-earth oxide additions
The effects of rare-earth oxide additions on the oxidation of sintered Si3N4 were examined. Insignificant oxidation occurred at 700 and 1000 C, with no evidence of phase instability. At 1370 C, the oxidation rate was lowest for Y2O3 and increased for additions of La2O3, Sm2O3, and CeO2, in that order. Data obtained from X-ray diffraction, electron microprobe analysis, and scanning electron microscopy indicate that oxidation occurs via diffusion of cationic species from Si3N4 grain boundaries.
Mieskowski, D. M.↗
Microstructure of reaction-bonded silicon nitride consolidated by isostatic hot-pressing
A microstructural examination and chemical analysis are conducted for reaction-bonded Si3N4 specimens that were isostatically hot pressed at 1850, 1950, and 2050 C. The present observations indicate that the previously reported increase in the 1200 C bend strength of reaction-bonded Si3N4, after pressing at 2050 C exclusively, is due to the relative oxygen levels of the isostatically hot pressed specimens; calculations show that an SiO2 content of less than about 2.2 vol pct is needed to yield the 1200 C strength increase.
Mieskowski, D. M.↗
Hot isostatic pressing of ceramics
A mixture containing glass 70 to 95 and BN or B4C powder (0.1-10 microns) 5 to 30 vol. % is used as a secondary pressure medium in hot isostatic pressing of ceramics. Thus, Pyrex beads were mixed with 15% vol. BN powder (average diameter 2 microns), fused at 1400 deg for 2 h, cooled, crushed, and put into a graphite crucible. A Si3N4 sintered body was embedded in the powder, heated in vacuum at 1200 deg for 2 h, treated in a hot isostatic press furnace at 1700 deg and 1000 atm. for 1 h, and cooled to give a Si3N4 ceramic. It was easily separated from the crucible.
Honma, K.↗
Correlation of processing and sintering variables with the strength and radiography of silicon nitride
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 over 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 long, 10 to 30 microns wide, and with an aspect ratio of 5:1.
Sanders, W. A.↗
Radiographic detectability limits for seeded voids in sintered silicon carbide and silicon nitride
Conventional and microfocus X-radiographic techniques were compared to determine relative detectability limits for voids in green and sintered SiC and Si3N4. The relative sensitivity of the techniques was evaluated by comparing their ability to detect voids that were artificially introduced by a seeding process. For projection microfocus radiography the sensitivity of void detection at a 90/95 probability of detection/confidence level is 1.5 percent of specimen thickness in sintered SiC and Si3N4. For conventional contact radiography the sensitivity is 2.5 percent of specimen thickness. It appears that microfocus projection radiography is preferable to conventional contact radiography in cases where increased sensitivity is required and where the additional complexity of the technique can be tolerated.
Baaklini, G. Y.↗
Effect of grain-boundary crystallization on the high-temperature strength of silicon nitride
Si3N4 specimens having the composition 88.7 wt pct Si3N4-4.9 wt pct SiO2-6.4 wt pct Y2O3 were sintered at 2140 C under 25 atm N2 for 1 h and then subjected to a 5 h anneal at 1500 C. Crystallization of an amorphous grain-boundary phase resulted in the formation of Y2Si2O7. The short-time 1370 C strength of this material was compared with that of material of the same composition having no annealing treatment. No change in strength was noted. This is attributed to the refractory nature of the yttrium-rich grain-boundary phase (apparently identical in both glassy and crystalline phases) and the subsequent domination of the failure process by common processing flaws.
Pierce, L. A.↗
NDE reliability and process control for structural ceramics
The reliability of microfocus x-radiography and scanning laser acoustic microscopy for detecting microvoids in silicon nitride and silicon carbide was statistically evaluated. Materials- and process-related parameters that influenced the statistical findings in research samples are discussed. The use of conventional x-radiography in controlling and optimizing the processing and sintering of an Si3N4-Si02-Y203 composition designated NASA 6Y is described. Radiographic evaluation and guidance helped develop uniform high-density Si3N4 modulus-of-rupture bars with improved four-point flexural strength (857, 544, and 462 MPa at room temperature, 1200 C, and 1370 C, respectively) and reduced strength scatter.
Baaklini, G. Y.↗
Correlation of processing and sintering variables with the strength and radiography of silicon nitride
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 over 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 40-80 micron long, 10-30 micron wide, and with an aspect ratio of 5:1.
Sanders, W. A.↗
Preparation of silicon carbide-silicon nitride fibers by the pyrolysis of polycarbosilazane precursors - A review
The development of silicon carbide-silicon nitride fibers (SiC-Si3N4) by the pyrolysis of polycarbosilazane precursors is reviewed. Precursor resin, which was prepared by heating tris(N-methylamino)methylsilane or tris(N-methylamino)phenylsilane to about 520 C, was drawn into fibers from the melt and then made unmeltable by humidity conditioning at 100 C and 95 percent relative humidity. The humidity treated precursor fibers were pyrolyzed to ceramic fibers with good mechanical properties and electrical resistivity. For example, SiC-Si3N4 fibers derived from tris(N-methylamino)methylsilane had a tensile rupture modulus of 29 million psi and electrical resistivity of 6.9 x ten to the 8th power omega-cm, which is ten to the twelfth power times greater than that obtained for graphite fibers.
Penn, B. G.↗
NDE reliability and process control for structural ceramics
The reliability of microfocus X-radiography and scanning laser acoustic microscopy for detecting microvoids in silicon nitride and silicon carbide was statistically evaluated. Materials- and process-related parameters that influenced the statistical findings in research samples are discussed. The use of conventional X-radiography in controlling and optimizing the processing and sintering of an Si3N4-SiO2-Y2O3 composition designated NASA 6Y is described. Radiographic evaluation and guidance helped develop uniform high-density Si3N4 modulus-of-rupture bars with improved four-point flexural strength (857, 544, and 462 MPa at room temperature, 1200 C, and 1370 C, respectively) and reduced strength scatter.
Baaklini, G. Y.↗
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.↗
A sintering model for SiC(sub)w/Si3N4 composites
Presented is a model which suggests that it should be possible to pressureless sinter a SiC(sub w)/ Si3N4 composite to theoretical density. Prior failure to achieve complete densification by sintering is attributed to the use of compositions which result in a glass deficit. There is one basic premise for this model. The ratio of glass amount to surface area of nonglass constituents must be the same for both composite and sinterable monolithic Si3N4. This model suggests that whisker and grain sizes and whisker loading influence the glass amount necessary for successful sintering of composites. According to the model, a large glass amount will be necessary for successful sintering of these composites. However, grain boundary thicknesses in the composite will be less than those in the analogous monolithic materials. This suggests that good high temperature strength may still be attained. A recent report supports the predictions of the model.
Freedman, Marc R.↗
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.↗
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↗