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At least 199 records · Page 11

Effects of oxide additions and temperature on sinterability of milled silicon nitride

Specimens of milled alpha-Si3N4 with 0 to 5.07 equivalent percent of oxide additions were pressureless sintered at 1650 to 1820 C for 4 hours in nitrogen while covered with powdered Si3N4 + SiO2. Densities of less than or equal to 97.5 percent resulted with approximately 2.5 equivalent percent of MgO, CeO2, Y2O3, and three mixtures involving these oxides. Densities of greater than or equal to 94 percent were obtained with approximately 0.62 equivalent percent of the same additives. At most temperatures, best sinterability (density maxima) was obtained with 1.2 to 2.5 equivalent percent additive.

Arias, A.↗

Effect of W and WC on the oxidation resistance of yttria-doped silicon nitride

The effect of W and WC contamination on the oxidation and cracking in air of sintered Si3N4 - 8 w/o Y2O3 ceramics at 500, 750, and 1350 C is examined. A mixture of Si3N4 - 8Y2O3, milled with alumina balls, was divided into four portions. Three portions were doped with 2 w/o WC W, and 4 w/o W respectively, in order to simulate contamination during milling. The fourth portion was undoped and used on a control. The addition of W or WC did not affect the phase relationships in the system, as all bars with or without additions contained melilite as the major Si-Y-O-N phase after sintering. At 750 C, instability (rapid oxidation and cracking) of W-doped bars appears to have occurred as a result of oxidation of the tungsten containing melilite phase. No intermediate temperature instability was observed in bars containing 2 w/o WC or in bars with no additive. Specimens exposed at 1350 C had good oxidation resistance due to the formation of a protective siliceous oxide layer. A specimen containing 4 w/o W which was preoxidized at 1350 C had improved oxidation resistance at 750 C. The tendency towards oxidation and cracking of Si3N4 - 8 Y2O3 at 750 C is concluded to be related to tungsten content of the sintered bars.

Schuon, S.↗

Effect of Yttria additives on properties of pressureless-sintered silicon nitride

Si3N4-base ceramics were made from milled Si3N4 containing 11.1 wt% SiO2 and oxide additives by pressureless sintering at 1760 C. The four-point-average moduli of rupture were 460, 515, and 515 MPa at room temperature and 270, 256, and 227 MPa at 1400 C for compositions with 3.67, 7.22, and 14.0 wt% Y2O3, respectively. The oxidation resistance of these compositions decreased with increasing Y2O3 in the 600 to 1400 C range, and no surface oxide cracking or spalling was noted. Partial substitution of Al2O3 for Y2O3 reduced both strength and oxidation resistance.

Arias, A.↗

Thermodynamics of silicon nitridation - Effect of hydrogen

Equilibrium compositions for the nitridization of Si were calculated to detect the effectiveness of H2 in removal of the oxide film and in increasing the concentration of SiO and reducing the proportions of O2. Gibbs free energy for the formation of SiN2O was computed above 1685 K, and at lower temperatures. The thermodynamic properties of SiN2O2 were then considered from 1000-3000 K, taking into account the known thermodynamic data for 39 molecular combinations of the Si, Ni, and O. The gases formed were assumed ideal mixtures with pure phase condensed species. The mole fractions were obtained for a system of SiO2 with each Si particle covered with a thin layer of SiO2 before nitridation, and a system in which the nitriding atmosphere had access to the Si. The presence of H2 was determined to enhance the removal of NiO2 in the first system, decrease the partial pressure of O2, increase the partial pressures of SiO, Si, H2O, NH3, and SiH4, while its effects were negligible in the Si system.

Shaw, N. J.↗

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.↗

Grain-boundary phases in hot-pressed silicon nitride containing Y2O3 and CeO2 additives

Auger electron spectroscopy in conjunction with X-ray powder diffraction and scanning electron microscopy is used to analyze the grain-boundary phases of Y2O3- and CeO2-doped Si3N4 hot-pressed materials in order to demonstrate that the additives concentrate predominantly in the grain boundaries of Si3N4 in the form of various oxynitride phases. A high oxygen content observed in sample fracture surfaces was found to be consistent with the existence of an oxygen-enriched phase in the grain boundaries. The presence of yttrium and cerium in the fracture surfaces and an overall increase in the O/N ratio imply that the additive oxides are predominantly concentrated in the intergranular phases.

Guha, J. P.↗

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.↗

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.↗

Silicon carbide-silicon nitride fibers: Preparation and characterization of polycarbosilazane precursors

This study examines the effect of modifications of the chemical structure of the monomers on the properties of the polymeric precursor and and ceramic fibers. A group of silaneamines, R'-Si (NH-R) sub 3, taken from the series where R' is methyl or phenyl and R is n-propyl, n-butyl, phenyl or allyl, are converted to polycarbosilazanes by heating in excess of 500 C. Resins obtained from this polymerization are characterized by NMR and IR spectroscopy and GPC. Each resin is tested for fiber-forming properties. Resin samples and fibers are hydrolytically cured. Thermogravimetric analyses are conducted on the cured resins to compare the relative thermal stability and examine the pyrolysis process. Cured fibers are tested for tensil strength.

Crouse, D. J.↗

Method for measuring surface activity of silicon nitride powder

Amorphous, alpha-, and beta-Si3N4 powders were activated by vibration ball milling in purified MeOH, and the surface activity of ground powders was determined by the temperature programmed desorption (TPD) method using NH3 gas. The concentration of active sites with a potential energy equivalent to the peak temperature in the spectrum increased was markedly by ball milling the amorphous Si3N4. The alpha- and beta-Si3N4 also had active sites produced by ball milling. The concentration of active site increased with increased ball milling time. A method for measuring surface activity of ceramic raw materials by TPD is proposed.

Kanno, Y.↗

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.↗

Manufacture of dense sintered bodies containing silicon nitride

Sintered bodies containing 1-32.5 Si oxide and 1.5 wt.% SiC (Si oxide/SiC wt. ratio 3/2) are prepared and kept in a 10-3000 kg/2 sq. cm. N (g) atmosphere at 1500-2300 degrees, while simultaneously maintaining the CO (g) partial pressure around the body lower than the nitrogenation equil. pressure to give a dense sintered body. The prepared dense sintered body has high strength at high temperatures. Thus, SiC 40, oxide 30 and Si3N4 30 wt% were fired to a body which was kept in 1500 kg/sq. cm. N (g) for 20 h at 2000 degrees to give a dense sintered body having high bending strength at high temperatures.

Hirota, K.↗