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1.
Koji Watari Kiyoshi Hirao Motohiro Toriyama Kozo Ishizaki 《Journal of the American Ceramic Society》1999,82(3):777-779
Polycrystalline Si3 N4 samples with different grain-size distributions and a nearly constant volume content of grain-boundary phase (6.3 vol%) were fabricated by hot-pressing at 1800°C and subsequent HIP sintering at 2400°C. The HIP treatment of hot-pressed Si3 N4 resulted in the formation of a large amount of ß-Si3 N4 grains ∼10 µm in diameter and ∼50 µm long, and the elimination of smaller matrix grains. The room-temperature thermal conductivities of the HIPed Si3 N4 materials were 80 and 102 Wm−1 K−1 , respectively, in the directions parallel and perpendicular to the hot-pressing axis. These values are slightly higher than those obtained for hot-pressed samples (78 and 93 Wm−1 K−1 ). The calculated phonon mean free path of sintered Si3 N4 was ∼20 nm at room temperature, which is very small as compared to the grain size. Experimental observations and theoretical calculations showed that the thermal conductivity of Si3 N4 at room temperature is independent of grain size, but is controlled by the internal defect structure of the grains such as point defects and dislocations. 相似文献
2.
Thermal decomposition of silicon diimide, Si(NH)2 , in vacuum resulted in very-high-purity, fine-particle-size, amorphous Si3 N4 powders. The amorphous powder was isothermally aged at 50° to 100° intervals from 1000° to 1500°C for phase identification. Examination of ir spectra and X-ray diffraction patterns indicated a slow and gradual transition from an amorphous material to a crystalline α-phase occurring at 1200°C for >4 h and/or 1300° to 1400°C for 2 h. As the temperature was increased to ≥1450°C for 2 h, the crystalline β-phase was observed. Phase nucleation and crystallite morphology in this system were studied by electron microscopy and electron diffraction combined with TG as functions of temperature for the inorganic polymer starting materials. Powders prepared in this manner with 4 wt% Mg3 N2 added as a sintering aid were hot-pressed to high-density fine-grained bodies with uniform microstructures. The optimum hot-pressing condition was 1650°C for 1 h. Silicon concentration steadily increased as the hot-pressing temperature or time was increased. A method for chemical etching for high-density fine-grained Si3 N4 is described. Electrical measurements between room temperature and ∼500°C indicated dielectric constant and tan δ values of 8.3±0.03 and 0.65±0.05×10−2 , respectively. 相似文献
3.
C. Greskovich 《Journal of the American Ceramic Society》1981,64(2):31-C-
The development of microstructure in hot-pressed Sia N4 was studiehd for a typical Si3 N4 powder with and without BeSiN2 as a densification aid. The effect of hot-pressing temperature on density, α- to β-Si3 N4 conversion and specific surface area showed that BeSiN2 appears to increase the mobility of the system by enhancing densification, α- to β-Si3 N4 transformation, and grain growth at temperatures between 1450° and 1800°. These processes appear to occur in the presence of a liquid phase. 相似文献
4.
IRVIN C. HUSEBY† HANS L. LUKAS GÜNTER PETZOW 《Journal of the American Ceramic Society》1975,58(9-10):377-380
The 1780°C isothermal section of the reciprocal quasiternary system Si3 N4 -SiO2 -BeO-Be3 N2 was investigated by the X-ray analysis of hot-pressed samples. The equilibrium relations shown involve previously known compounds and 8 newly found compounds: Be6 Si3 N8 , Be11 Si5 N14 , Be5 Si2 N6 , Be9 Si3 N10 , Be8 SiO4 N4 , Be6 O3 N2 , Be8 O5 N2 , and Be9 O6 N2 . Large solid solubility occurs in β-Si3 N4 , BeSiN2 , Be9 Si3 N10 , Be4 SiN4 , and β-Be3 N2 . Solid solubility in β-Si3 N4 extends toward Be2 SiO4 and decreases with increasing temperature from 19 mol% at 1770°C to 11.5 mol% Be2 SiO4 at 1880°C. A 4-phase isotherm, liquid +β-Si3 N4 ( ss )Si2 ON2 + BeO, exists at 1770°C. 相似文献
5.
Jow-Lay Huang Hung-Liang Chiu Ming-Tung Lee 《Journal of the American Ceramic Society》1994,77(3):705-710
The effects of TiC addition to Si3 N4 on microstructure and the chemical aspects of Si3 N4 –TiC interphase reaction were investigated in samples hot-pressed at 1800°C in Ar and N2 . Composition of a TiC1–x Nx solid solution was predicted based on thermodynamic calculation, with titanium carbonitride taken to be an ideal solid solution. The predicted value of x = 0.7 is slightly higher than that derived from the measured lattice parameter and Vegard's law (x = 0.67). Four distinguishable areas were observed in samples hot-pressed in nitrogen atmosphere. They were identified as β-Si3 N4 , mixtures of TiC and titanium carbonitride solid solution, SiC with twins, and iron silicide. As the duration of hot-pressing increased, more titanium carbonitride was formed, while less TiC phase remained. Thermodymanic calculations indicate one source of nitrogen gas came from the decomposition of Si3 N4 . The TiC particles also became more irregular, and reactants were found inside or between TiC as the hot-pressing time was extended. Silicon carbide was not detected in samples which were hot-pressed in argon atmosphere; however, numerous pores were found around TiC. 相似文献
6.
Full-density Si3 N4 -SiO2 -Ce2 O3 compositions were prepared by sintering with 2.5 MPa nitrogen pressure at temperatures of 1900° and 2090°C. Room-temperature flexural strengths near 700 MPa for sintered material compared favorably with the strength of hot-pressed material. At 1370°C, where flexural strengths as high as 363 MPa were obtained, it was observed that the coarsest structure was the strongest and the finest structure was the weakest. One of the compositions tested, Si3 N4 -8.7 wt% SiO2 -8.3 wt%-Ce2 O3 , was found to have excellent 200-h oxidation resistance at 700°, 1000°, and 1370°C, without incidence of 700° to 1000°C phase instability and cracking. 相似文献
7.
Cha-Yang Chu Jitendra P. Singh Jules L. Routbort 《Journal of the American Ceramic Society》1993,76(5):1349-1353
The high-temperature flexural strength of hot-pressed silicon nitride (Si3 N4 ) and Si3 N4 -whisker-reinforced Si3 N4 -matrix composites has been measured at a crosshead speed of 1.27 mm/min and temperatures up to 1400°C in a nitrogen atmosphere. Load–displacement curves for whisker-reinforced composites showed nonelastic fracture behavior at 1400°C. In contrast, such behavior was not observed for monolithic Si3 N4 . Microstructures of both materials have been examined by scanning and transmission electron microscopy. The results indicate that grain-boundary sliding could be responsible for strength degradation in both monolithic Si3 N4 and its whisker composites. The origin of the nonelastic failure behavior of Si3 N4 -whisker composite at 1400°C was not positively identified but several possibilities are discussed. 相似文献
8.
Hot-pressed Si3 N4 doped with 10 wt% zvttrite as a sinterine aid was studied. An equiaxed, fine-grainid microstructure was predominant, with no apparent porosity. Bend strengths were determined at room temperature and high temperatures (up to 1370°C/2500°F). Oxidation was measured by weight gain at 1370°C in air. The resulting material exhibited very good room-temperature strength (755 MPa/110 ksi). The work showed that room-temperature strength can be improved significantly by using controlled Si3 N4 powder with 10 wt% zyttrite. High-temperature strength (514 MPd75 ksi) at 1370°C was nearly double that of hot-pressed Si3 N4 (NC-132). The oxidation resistance at 1370°C was also higher than that of NC-132. 相似文献
9.
Subsolidus phase relations were established in the system Si3 N4 -SiO2 -Y2 O3 . Four ternary compounds were confirmed, with compositions of Y4 Si2 O7 N2 , Y2 Si3 O3 N4 , YSiO2 N, and Y10 (SiO4 )6 N2 . The eutectic in the triangle Si3 N4 -Y2 Si2 O7 -Y10 (SiO4 )6 N2 melts at 1500°C and that in the triangle Si2 N2 O-SiO2 -Y2 Si2 O7 at 1550°C. The eutectic temperature of the Si3 N4 -Y2 Si2 O7 join was ∼ 1520°C. 相似文献
10.
The compressive creep behavior and oxidation resistance of an Si3 N4 /Y2 Si2 O7 material (0.85Si3 N4 +0.10SiO2 +0.05Y2 O3 ) were determined at 1400°C. Creep re sistance was superior to that of other Si3 N4 materials and was significantly in creased by a preoxidation treatment (1600°C /120 h). An apparent parabolic rate constant of 4.2 × 10−11 kg2 ·m-4 ·s−1 indicates excellent oxidation resistance. 相似文献
11.
Linus U. J. T. Ogbuji 《Journal of the American Ceramic Society》1992,75(11):2995-3000
The results of two-step oxidation experiments on chemically-vapor-deposited Si3 N4 and SiC at 1350°C show that a correlation exists between the presence of a Si2 N2 O interphase and the strong oxidation resistance of Si3 N4 . During normal oxidation, k p for SiC was 15 times higher than that for Si3 N4 , and the oxide scale on Si3 N4 was found by SEM and TEM to contain a prominent Si2 N2 O inner layer. However, when oxidized samples are annealed in Ar for 1.5 h at 1500°C and reoxidized at 1350°C as before, three things happen: the oxidation k p increases over 55-fold for Si3 N4 , and 3.5-fold for SiC; the Si3 N4 and SiC oxidize with nearly equal k p 's; and, most significant, the oxide scale on Si3 N4 is found to be lacking an inner Si2 N2 O layer. The implications of this correlation for the competing models of Si3 N4 oxidation are discussed. 相似文献
12.
Jae-Yuk Kim Takayoshi Iseki Toyohiko Yano 《Journal of the American Ceramic Society》1996,79(10):2744-2746
The effect of aluminum and yttrium nitrate additives on the densification of monolithic Si3 N4 and a Si3 N4 /SiC composite by pressureless sintering was compared with that of oxide additives. The surfaces of Si3 N4 particles milled with aluminum and yttrium nitrates, which were added as methanol solutions, were coated with a different layer containing Al and Y from that of Si3 N4 particles milled with oxide additives. Monolithic Si3 N4 could be sintered to 94% of theoretical density (TD) at 1500°C with nitrate additives. The sintering temperature was about 100°C lower than the case with oxide additives. After pressureless sintering at 1750°C for 2 h in N2 , the bulk density of a Si3 N4 /20 wt% SiC composite reached 95% TD with nitrate additives. 相似文献
13.
Shigeyuki Smiya Masahiro Yoshimura Shutaro Fujiwara Ken-Ichi Kondo Akira Sawaoka Takeo Haitori Jun-Ichi Mohri Masatada Araki 《Journal of the American Ceramic Society》1984,67(3):51-C-
To enhance the sinter ability of Si3 N4 , powders mixed with 0, 2, and 5 wt% Y2 O3 were explosively shock-treated. Compacts of these powders were encapsulated in 96% silica glass containers and isostatically hot-pressed. The shocked Si3 N4 with 5 wt% Y2 O3 was pressed to a density of 3.09 g/cm3 (95.4% of theoretical) at 1400°C under 430 MPa for 3 h, whereas the unshocked material attained only 82.4% of theoretical density under the same hot isostatic pressing conditions. 相似文献
14.
A. J. KIEHLE L. K. HEUNG P. J. GIELISSE T. J. ROCKETT 《Journal of the American Ceramic Society》1975,58(1-2):17-20
The high-temperature chemical stability of hot-pressed Si3 N4 was studied between 600° and 1450°C. Reactions were followed by X-ray diffraction and scanning electron microscopy. In air, this material begins to oxidize at 700° to 750°C; a distinct amorphous siO2 surface layer results after 24 h at 750°C-Concomitant formation of cristobalite occurs, depending on exposure time, and is enhanced as temperature is Increased. Magnesium and calcium magnesium silicates form above 1000°C. The data suggest that impurities, e.g. Mg, Ca, and Fe, greatly lower the oxidation resistance of Si3 N4 in air. 相似文献
15.
Si3 N4 /MoSi2 and Si3 N4 /WSi2 composites were prepared by reaction-bonding processes using as starting materials powder mixtures of Si-Mo and Si-W, respectively. A presintering step in an At-base atmosphere was used before nitriding for the formation of MoSi2 and WSi2 ; the nitridation in a N2 -base atmosphere was followed after presintering with the total stepwise cycle of 1350°C × 20 h +1400°C × 20 h +1450°C × 2 h. The final phases obtained in the two different composites were Si3 N4 and MoSi2 or WSi2 ; no free elemental Si and Mo or W were detected by X-ray diffraction. 相似文献
16.
The phase relations in the Si3 N4 -rich portion of the Si3 N4 –AlN–Y2 O3 rystem were investigated using hot-pressed bodies. The one-phase fields of β3 and α, the twophase fields of β+α, β+M (M=melilite), and α+M, and the three-phase fields of β+α+M were observed in the Si3 N4 -rich portion. The α- and β-sialons are not two different compounds but an allotropic transformation phase of the Si–Al–O–N system, and an α solid solution expands and stabilizes with increasing Y2 O3 content. Therefore, the formulas of the two sialons should be the same. 相似文献
17.
Composites containing 30 vol%β-Si3 N4 whiskers in a Si3 N4 matrix were fabricated by hot-pressing. The composites exhibited fracture toughness values between 7.6 and 8.6 MPa · m1/2 , compared to 4.0 MPa · m1/2 for unreinforced polycrystalline Si3 N4 . The improvements in fracture toughness were attributed to crack wake effects, i.e., whisker bridging and pullout mechanisms. 相似文献
18.
John J. Petrovic Maria I. Pena H. Harriett Kung 《Journal of the American Ceramic Society》1997,80(5):1111-1116
Details of the fabrication and microstructures of hot-pressed MoSi2 reinforced–Si3 N4 matrix composites were investigated as a function of MoSi2 phase size and volume fraction, and amount of MgO densification aid. No reactions were observed between MoSi2 and Si3 N4 at the fabrication temperature of 1750°C. Composite microstructures varied from particle–matrix to cermet morphologies with increasing MoSi2 phase content. The MgO densification aid was present only in the Si3 N4 phase. An amorphous glassy phase was observed at the MoSi2 –Si3 N4 phase boundaries, the extent of which decreased with decreased MgO level. No general microcracking was observed in the MoSi2 –Si3 N4 composites, despite the presence of a substantial thermal expansion mismatch between the MoSi2 and Si3 N4 phases. The critical MoSi2 particle diameter for microcracking was calculated to be 3 μm. MoSi2 particles as large as 20 μm resulted in no composite microcracking; this indicated that significant stress relief occurred in these composites, probably because of plastic deformation of the MoSi2 phase. 相似文献
19.
Young Sik Yoon Sang Woong Na Jaehyung Lee † Myeong-Woo Cho Eun-Sang Lee Won-Seung Cho 《Journal of the American Ceramic Society》2004,87(7):1374-1377
R -curve behavior of Si3 N4 –BN composites and monolithic Si3 N4 for comparison was investigated. Si3 N4 –BN composites showed a slowly rising R -curve behavior in contrast with a steep R -curve of monolithic Si3 N4 . BN platelets in the composites seem to decrease the crack bridging effects of rod-shaped Si3 N4 grains for small cracks, but enhanced the toughness for long cracks as they increased the crack bridging scale. Therefore, fracture toughness of the composites was relatively low for the small cracks, but it increased significantly to ∼8 MPa·m1/2 when the crack grew longer than 700 μm, becoming even higher than that of the monolithic Si3 N4 . 相似文献
20.
Composite ceramic materials based on Si3 N4 and ZrO2 stabilized by 3 mol% Y2 O3 have been formed using aluminum isopropoxide as a precursor for the Al2 O3 sintering aid. Densification was carred out by hot-pressing at temperatures in the range 1650° to 1800°C, and the resulting micro-structures were related to mechanical properties as well as to oxidation behavior at 1200°C. Densification at the higher temperatures resulted in a fibrous morphology of the Si3 N4 matrix with consequent high room-temperature toughness and strength. Decomposition of the ZrO2 grains below the oxidized surface during oxidation introduced radial stresses in the subscalar region, and from the oxidation experiments it is suggested that the ZrO2 incorporated some N during densification. 相似文献