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1.
Beta-type CVD-Si3 N4 plates (up to 1.1 mm thick) have been prepared by adding TiCl4 vapor to the system SiCl4 -NH3 -H2 at deposition temperatures of 1350° to 1450°C, while α-type or amorphous CVD-Si3 N4 was obtained without TiCl4 vapor at the same deposition temperature. Three to four wt % 777V was included in the β-type CVD-Si3 N4 matrix. The density, preferred orientation, and lattice parameters of β-type CVD-Si3 N4 were examined. 相似文献
2.
The development of crystalline phases in lithium oxynitride glass-ceramics was examined, with particular emphasis placed on the effect of the nitrogen source (AlN or Si3 N4 ) on the formation and stability of a β-quartz solid-solution ( ss ) phase. Oxynitride glasses derived from the Li-Si-Al-O-N system were heat-treated at temperatures up to 1200°C to yield glass-ceramics in which β-quartz( ss ) and β-spodumene( ss ) of approximate composition Li2 OAl2 O3 4SiO2 formed as major phases and in which X-phase (Si3 Al6 O12 N2 ) and silicon oxynitride (Si2 N2 O) were present as minor phases. The nitrogen-containing β-quartz( ss ) phase that was prepared with AlN was stable at 1200°C; however, the use of Si3 N4 as the nitrogen source was significantly less effective in promoting such thermal stabilization. Lattice parameter measurements revealed that AlN and Si3 N4 had different effects on the crystalline structures, and it was proposed that the enhanced thermal stability of the β-quartz( ss ) phase that was prepared with AlN was due to both the replacement of oxygen by nitrogen and the positioning of excess Al3+ ions into interstitial sites within the β-quartz( ss ) crystal lattice. 相似文献
3.
β-Si3 N4 ceramics sintered with Yb2 O3 and ZrO2 were fabricated by gas-pressure sintering at 1950°C for 16 h changing the ratio of "fine" and "coarse" high-purity β-Si3 N4 raw powders, and their microstructures were quantitatively evaluated. It was found that the amount of large grains (greater than a few tens of micrometers) could be drastically reduced by mixing a small amount of "coarse" powder with a "fine" one, while maintaining high thermal conductivity (>140 W·(m·K)−1 ). Thus, this work demonstrates that it is possible for β-Si3 N4 ceramics to achieve high thermal conductivity and high strength simultaneously by optimizing the particle size distribution of raw powder. 相似文献
4.
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
5.
Novel Two-Step Sintering Process to Obtain a Bimodal Microstructure in Silicon Nitride 总被引:5,自引:0,他引:5
Hai-Doo Kim Byung-Dong Han Dong-Soo Park Byong-Taek Lee Paul F. Becher 《Journal of the American Ceramic Society》2002,85(1):245-252
A two-step sintering process is described in which the first step suppresses densification while allowing the α-to-β phase transformation to proceed, and the second step, at higher temperatures, promotes densification and grain growth. This process allows one to obtain a bimodal microstructure in Si3 N4 without using β-Si3 N4 seed crystals. A carbothermal reduction process was used in the first step to modify the densification and transformation rates of the compacts consisting of Si3 N4 , Y2 O3 , Al2 O3 , and a carbon mixture. The carbothermal reduction process reduces the oxygen:nitrogen ratio of the Y-Si-Al-O-N glass that forms, which leads to the precipitation of crystalline oxynitride phases, in particular, the apatite phase. Precipitation of the apatite phase reduces the amount of liquid phase and retards the densification process up to 1750°C; however, the α-to-β phase transformation is not hindered. This results in the distribution of large β-nuclei in a porous fine-grained β-Si3 N4 matrix. Above 1750°C, liquid formed by the melting of apatite resulted in a rapid increase in densification rates, and the larger β-nuclei also grew rapidly, which promoted the development of a bimodal microstructure. 相似文献
6.
Fengxia Li Li Fu Xiaojian Ma Changhui Sun LianCheng Wang Chunli Guo Yitai Qian Yitai Qian 《Journal of the American Ceramic Society》2009,92(2):517-519
Starting from Si powder, NaN3 and different additives such as N -aminothiourea, iodine, or both, Si3 N4 nanomaterials were synthesized through the nitridation of silicon powder in autoclaves at 60°–190°C. As the additive was only N -aminothiourea, β-Si3 N4 nanorods and α-Si3 N4 nanoparticles were prepared at 170°C. If the additive was only iodine, α-Si3 N4 dendrites with β-Si3 N4 nanorods were obtained at 190°C. However, when both N -aminothiourea and iodine were added to the system of Si and NaN3 , the products composed of β-Si3 N4 nanorods and α, β-Si3 N4 nanoparticles could be prepared at 60°C. 相似文献
7.
Electrical conductivity was measured from 850° to 1400°C for β-sialon and pure X phase as well as for the sintered system Si3 N4 -Al2 O3 , containing β-sialon, X phase, β-Si3 N4 , and glassy phase. Ionic conductivity was measured at >1000°C. The charge carriers were identified by electrolysis. The results showed that pure β-sialon is ionically conducting because of Si4+ migration for the temperature range studied. Pure X phase shows ionic conduction by Si4+ above 1000°; below 1000°C, it shows electronic conduction because of impurities. The conductivity of the sintered system Si3 N4 -Al2 O3 containing β-sialon, β-Si3 N4 X phase, and glassy phase changes as the relative quantities of β -sialon and X phase change. The apparent activation energies for the ionic and electronic conductivities are 45 and 20 kcal/mol, respectively. 相似文献
8.
Gui-hua Peng Min Liang Zhen-hua Liang Qing-yu Li Wen-lan Li Qian Liu 《Journal of the American Ceramic Society》2009,92(9):2122-2124
Silicon nitride ceramics were prepared by spark plasma sintering (SPS) at temperatures of 1450°–1600°C for 3–12 min, using α-Si3 N4 powders as raw materials and MgSiN2 as sintering additives. Almost full density of the sample was achieved after sintering at 1450°C for 6 min, while there was about 80 wt%α-Si3 N4 phase left in the sintered material. α-Si3 N4 was completely transformed to β-Si3 N4 after sintering at 1500°C for 12 min. The thermal conductivity of sintered materials increased with increasing sintering temperature or holding time. Thermal conductivity of 100 W·(m·K)−1 was achieved after sintering at 1600°C for 12 min. The results imply that SPS is an effective and fast method to fabricate β-Si3 N4 ceramics with high thermal conductivity when appropriate additives are used. 相似文献
9.
Chunli Guo Zheng Xing Xiaojian Ma Liqiang Xu Yitai Qian 《Journal of the American Ceramic Society》2008,91(5):1725-1728
Silicon nitride nanowires or nanorods have been synthesized from SiCl4 , NaN3 , and metallic Mg at temperatures ranging from 200° to 300°C. X-ray powder diffraction patterns indicated that the as-obtained products were mainly β-Si3 N4 . Scanning electron microscope and high-resolution transmission electronic microscopy showed that the samples mostly consisted of Si3 N4 nanowires or nanorods. As metallic iron powder was used, α-Si3 N4 was mainly formed at 250°C. 相似文献
10.
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
11.
Koichi Terao Yoshinari Miyamoto Mitsue Koizumi 《Journal of the American Ceramic Society》1988,71(3):167-C
Dense, ZrO2 -dispersed Si3 N4 composites without additives were fabricated at 180 MPa and ∼1850° to 1900°C for l h by hot isostatic pressing using a glass-encapsulation method; the densities reached >96% of theoretical. The dispersion of 20 wt% of 2.5YZrO2 (2.5 mol% Y2 O3 ) in Si3 N4 was advantageous to increase the room-temperature fracture toughness (∼7.5 MPa˙m1/2 ) without degradation of hardness (∼15 GPa) because of the high retention of tetragonal ZrO2 . The dependence of fracture toughness of Si3 N4 –2.5YZrO2 on ZrO2 content can be related to the formation of zirconium oxynitride because of the reaction between ZrO2 and Si3 N4 matrix in hot isostatic pressing. 相似文献
12.
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
13.
The kinetics of anisotropic β-Si3 N4 grain growth in silicon nitride ceramics were studied. Specimens were sintered at temperatures ranging from 1600° to 1900°C under 10 atm of nitrogen pressure for various lengths of time. The results demonstrate that the grain growth behavior of β-Si3 N4 grains follows the empirical growth law Dn – D0 n = kt , with the exponents equaling 3 and 5 for length [001] and width [210] directions, respectively. Activation energies for grain growth were 686 kJ/mol for length and 772 kJ/mol for width. These differences in growth rate constants and exponents for length and width directions are responsible for the anisotropy of β-Si3 N4 growth during isothermal grain growth. The resultant aspect ratio of these elongated grains increases with sintering temperature and time. 相似文献
14.
Silicon nitride (Si3 N4 ) ceramics, prepared with Y2 O3 and Al2 O3 sintering additives, have been densified in air at temperatures of up to 1750°C using a conventional MoSi2 element furnace. At the highest sintering temperatures, densities in excess of 98% of theoretical have been achieved for materials prepared with a combined sintering addition of 12 wt% Y2 O3 and 3 wt% Al2 O3 . Densification is accompanied by a small weight gain (typically <1–2 wt%), because of limited passive oxidation of the sample. Complete α- to β-Si3 N4 transformation can be achieved at temperatures above 1650°C, although a low volume fraction of Si2 N2 O is also observed to form below 1750°C. Partial crystallization of the residual grain-boundary glassy phase was also apparent, with β-Y2 Si2 O7 being noted in the majority of samples. The microstructures of the sintered materials exhibited typical β-Si3 N4 elongated grain morphologies, indicating potential for low-cost processing of in situ toughened Si3 N4 -based ceramics. 相似文献
15.
Tzer-Shin Sheu 《Journal of the American Ceramic Society》1994,77(9):2345-2353
The in situ β-Si3 N4 /α'-SiAlON composite was studied along the Si3 N4 –Y2 O3 : 9 AlN composition line. This two phase composite was fully densified at 1780°C by hot pressing Densification curves and phase developments of the β-Si3 N4 /α'-SiAlON composite were found to vary with composition. Because of the cooperative formation of α'-Si AlON and β-Si3 N4 during its phase development, this composite had equiaxed α'-SiAlON (∼0.2 μm) and elongated β-Si3 N4 fine grains. The optimum mechanical properties of this two-phase composite were in the sample with 30–40%α', which had a flexural strength of 1100 MPa at 25°C 800 MPa at 1400°C in air, and a fracture toughness 6 Mpa·m1/2 . α'-SiAlON grains were equiaxed under a sintering condition at 1780°C or lower temperatures. Morphologies of the α°-SiAlON grains were affected by the sintering conditions. 相似文献
16.
Elongated β'-SiAlON grains grown from several finegrained Ym/3 Si12(m+n) Alm+n On N16–r compositions with α-Si3 N4 , AlN, Al2 O3 , and Y2 O3 starting materials have been examined. These grains have large aspect ratios and are oriented along the [0001] axis. TEM structural and chemical analysis suggests that they are nucleated from various seed crystals, which can be α-Si3 N4 , β-Si3 N4 , or other β'-SiAlON. The β'-SiAlON seed and the initial precipitation on β-Si3 N4 show a higher content of Al and O, indicating that a large transient supersaturation of Al and O in the liquid is instrumental for β'-SiAlON formation, whereas subsequent growth proceeds under a much lower driving force. The misfit between phases is accommodated by interfacial dislocations ( c -type and a -type). Fully grown β'-SiAlON grains usually contain several variants independently nucleated from the same seed. In particular, the two alternative α/β phase-matching possibilities result in two [0001] growth habits separated by a twin boundary. 相似文献
17.
The subsolidus phase relations in the entire system ZrO2 -Y2 O3 were established using DTA, expansion measurements, and room- and high-temperature X-ray diffraction. Three eutectoid reactions were found in the system: ( a ) tetragonal zirconia solid solution→monoclinic zirconia solid solution+cubic zirconia solid solution at 4.5 mol% Y2 O3 and ∼490°C, ( b ) cubic zirconia solid solutiow→δ-phase Y4 Zr3 O12 +hexagonalphase Y6 ZrO11 at 45 mol% Y2 O3 and ∼1325°±25°C, and ( c ) yttria C -type solid solution→wcubic zirconia solid solution+ hexagonal phase Y6 ZrO11 at ∼72 mol% Y2 O3 and 1650°±50°C. Two ordered phases were also found in the system, one at 40 mol% Y2 O3 with ideal formula Y4 Zr3 O12 , and another, a new hexagonal phase, at 75 mol% Y2 O3 with formula Y6 ZrO11 . They decompose at 1375° and >1750°C into cubic zirconia solid solution and yttria C -type solid solution, respectively. The extent of the cubic zirconia and yttria C -type solid solution fields was also redetermined. By incorporating the known tetragonal-cubic zirconia transition temperature and the liquidus temperatures in the system, a new tentative phase diagram is given for the system ZrO2 -Y2 O3 . 相似文献
18.
Raju S. Parikh Annamarie Lightfoot John S. Haggerty Brian W. Sheldon 《Journal of the American Ceramic Society》1999,82(10):2626-2632
The effects of trace O2 levels on the nitridation of compacts made from silane-derived Si powders were studied in N2 atmospheres, with oxygen levels of either 5 ppm or 10 ppb (approximately). The nitriding kinetics were studied by thermogravimetric analysis as a function of temperature (1100–1200°C) and heating rate (5°C/min and 100°C/min). Reducing the O2 level in the nitriding gas enhanced conversion to Si3 N4 at lower temperatures, reduced the composition variations within the samples, and decreased the α/β ratios. The results suggest that nucleation and rapid growth of Si3 N4 at relatively low temperatures are possible only when the oxygen partial pressure in the system is below the threshold value for passive oxidation. 相似文献
19.
The existence of compounds between Si3 N4 -CeO2 and Si3 N4 -Ce2 O3 was investigated for firing temperatures of 1600° to 1700°C. The two new monoclinic compounds found were Ce2 O3 ·2Si3 N4 with lattice parameters a = 16.288, b = 4.848, and c =7.853 Å and β=91.54° and Ce4 Si2 O7 N2 with lattice parameters a = 10.360, b = 10.865, and c =3.974 Å and β=90.33°. Cerium orthosilicate (Ce 4.67 (SiO4 )3 O) is present during firing as a glassy intermediate phase which promotes sintering and densification and then reacts with silicon nitride to form cerium silicon oxynitrde (CeSiO2 N). 相似文献
20.
X-ray Diffraction Analysis of the Pyrolytic Conversion of Perhydropolysilazane into Silicon Nitride 总被引:1,自引:0,他引:1
A detailed investigation using X-ray diffraction and other supportive techniques was performed on a preceramic polysilazane to study its pyrolytic conversion to silicon nitride (Si3 N4 ). Analytical techniques were developed to determine the volumetric degree of crystallinity with respect to pyrolysis temperature. Quantitative data for crystallite size, phase composition, and degree of crystallinity versus pyrolysis temperature and atmosphere (nitrogen and ammonia) are presented. Pyrolytic products produced under nitrogen and ammonia atmospheres consist of microcrystals of silicon, α-Si3 N4 , and β-Si3 N4 . Under both atmospheres, a majority of the char is crystalline at ≅1270°C, and the entire char is crystallized at 1400°C. Pyrolysis under an ammonia atmosphere produces nearly stoichiometric Si3 N4 , while pyrolysis under nitrogen produces silicon-rich material. 相似文献