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1.
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
2.
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
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.
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
5.
Gui-hua Peng Guo-jian Jiang Wen-lan Li Bao-lin Zhang Li-dong Chen 《Journal of the American Ceramic Society》2006,89(12):3824-3826
α/β-Si3 N4 composites with various α/β phase ratios were prepared by hot pressing at 1600°–1650°C with MgSiN2 as sintering additives. An excellent combination of mechanical properties (Vickers indentation hardness of 23.1 GPa, fracture strength of about 1000MPa, and toughness of 6.3 MPa·m1/2 ) could be obtained. Compared with conventional Si3 N4 -based ceramics, this new material has obvious advantages. It is as hard as typical in-situ-reinforced α-Sialon, but much stronger than the latter (700 MPa). It has comparable fracture strength and toughness, but is much harder than β-Si3 N4 ceramics (16 GPa). The microstructures and mechanical properties can be tailored by choosing the additive and controlling the heating schedule. 相似文献
6.
L. J. BOWEN T. G. CARRUTHERS R. J. BROOK 《Journal of the American Ceramic Society》1978,61(7-8):335-359
The rates of densification and phase transformation undergone by α-Si3 N4 during hot-pressing in the presence of Y2 O3 , Y2 O3 −2SiO2 , and Li2 0−2Si02 as additives were studied. Although these systems behave less simply than MgO-doped Si3 N4 , the data can be interpreted during the early stages of hot-pressing as resulting from a solution-diffusion-reprecipitation mechanism, where the diffusion step is rate controlling and where the reprecipitation step invariably results in the formation of the β-Si3 N4 phase. 相似文献
7.
Youren Xu Chao M. Huang Waltraud M. Kriven Avigdor Zangvil 《Journal of the American Ceramic Society》1994,77(8):2213-2216
The microstructure of a pressureless sintered (1605°C, 90 min) O'+β' SiAlON ceramic with CeO2 doping has been investigated. It is duplex in nature, consisting of very large, slablike elongated O' grains (20–30 μm long), and a continuous matrix of small rodlike β' grains (< 1.0 μm in length). Many α-Si3 N4 inclusions (0.1–0.5 μm in size) were found in the large O' grains. CeO2 -doping and its high doping level as well as the high Al2 O3 concentration were thought to be the main reasons for accelerating the reaction between the α-Si3 N4 and the Si-Al-O-N liquid to precipitate O'–SiAlON. This caused the supergrowth of O' grains. The rapid growth of O' crystals isolated the remnant α–Si3 N4 from the reacting liquid, resulting in a delay in the α→β-Si3 N4 transformation. The large O' grains and the α-Si3 N4 inclusions have a pronounced effect on the strength degradation of O'+β' ceramics. 相似文献
8.
Martin Krämer 《Journal of the American Ceramic Society》1993,76(6):1627-1629
α-Si3 N4 core structures within β-Si3 N4 grains have been studied by transmission electron microscopy. The grains were dispersed in an oxynitride glass which was previously melted at 1600°C. The cores were topotactically related to the as-grown β-Si3 N4 crystallites and are related to epitactical nucleation during heat treatment as the most probable mechanism. 相似文献
9.
Jun-Qi Li Fa Luo Dong-Mei Zhu Wan-Cheng Zhou 《Journal of the American Ceramic Society》2007,90(6):1950-1952
The influence of phase formation on the dielectric properties of silicon nitride (Si3 N4 ) ceramics, which were produced by pressureless sintering with additives in MgO–Al2 O3 –SiO2 system, was investigated. It seems that the difference in the dielectric properties of Si3 N4 ceramics sintered at different temperatures was mainly due to the difference of the relative content of α-Si3 N4 , β-Si3 N4 , and the intermediate product (Si2 N2 O) in the samples. Compared with α-Si3 N4 and Si2 N2 O, β-Si3 N4 is believed to be a major factor influencing the dielectric constant. The high-dielectric constant of β-Si3 N4 could be attributed to the ionic relaxation polarization. 相似文献
10.
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
11.
The subsolidus phase diagram of the quasiternary system Si3 N4 -AlN-Y2 O3 was established. In this system α-Si3 N4 forms a solid solution with 0.1Y2 O3 : 0.9 AIN. The solubility limits are represented by Y0.33 Si10.5 Al1.5 O0.5 N15.5 and Y0.67 Si9 A13 ON15 . At 1700°C an equilibrium exists between β-Si3 N4 and this solid solution. 相似文献
12.
Nanocrystalline α-Si3 N4 powders have been prepared with a yield of 93% by the reaction of Mg2 Si with NH4 Cl in the temperature range of 450° to 600°C in an autoclave. X-ray diffraction patterns of the products can be indexed as the α-Si3 N4 with the lattice constants a = 7.770 and c = 5.627 Å. X-ray photoelectron spectroscopy analysis indicates that the composition of the α-Si3 N4 samples has a Si:N ratio of 0.756. Transmission electron microscopy images show that the α-Si3 N4 crystallites prepared at 450°, 500°, and 550°C are particles of about 20, 40, and 70 nm in average, respectively. 相似文献
13.
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
14.
Soo Young Lee 《Journal of the American Ceramic Society》1998,81(5):1262-1268
Si3 N4 /SiC composite materials have been fabricated by reaction-sintering and postsintering steps. The green body containing Si metal and SiC particles was reaction-sintered at 1370°C in a flowing N2 /H2 gas mixture. The initial reaction product was dominated by alpha-Si3 N4 . However, as the reaction processed there was a gradual increase in the proportion of β-Si3 N4 . The reaction-bonded composite consisting of alpha-Si3 N4 , β-Si3 N4 , and SiC was heat-treated again at 2000°C for 150 min under 7-MPa N2 gas pressure. The addition of SiC enhanced the reaction-sintering process and resulted in a fine microstructure, which in turn improved fracture strength to as high as 1220 MPa. The high value in flexural strength is attributed to the formation of uniformly elongated β-Si3 N4 grains as well as small size of the grains (length = 2 μm, thickness = 0.5 μm). The reaction mechanism of the reaction sintering and the mechanical properties of the composite are discussed in terms of the development of microstructures. 相似文献
15.
C. GRESKOVICH 《Journal of the American Ceramic Society》1981,64(12):725-730
Si3 N4 compacts, containing ≅7 wt% of both BeSiN2 and SiO2 as densification aids, can be reproducibly sintered to relative densities >99% by a gas-pressure sintering process. Nearly all densification takes place via liquid-phase sintering of transformed β-Si3 N4 grains at T =1800° to 2000°C. Compacts with high density are produced by first sintering to the closed-pore stage (≅92% relative density) in 2.1 MPa (20 atm) of N2 pressure at 2000°C and then increasing the N2 pressure to 7.1 MPa (70 atm) where rapid densification proceeds at T = 1800° to 2000°C. The experimental density results are interpreted in terms of theoretical arguments concerning the growth (coalescence) of gas-filled pores and gas solubility effects. Complex chemical reactions apparently occur at high temperatures and are probably responsible for incomplete understanding of some of the experimental data. 相似文献
16.
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
17.
Solid-liquid equilibria at 1750°C and subsolidus phase relations in the system Si3 N4 −AlN-SiO2 −Al2 O3 were determined for the composition region bounded by the β-Si3 N4 solid solution line and silica-alumina join X-ray diffraction and optical microscopy were used to determine the phases present in specimens cooled rapidly after equilibration. The extent of a single liquid-phase region and the tie lines for the βsolid solution + liquid field at 1750°C were established from quantitative X-ray diffractometry and lattice parameter measurements of βsolid solutions in equilibrium with liquid. The results were corroborated by optical microscopy and melting behavior observations. A new composition, Si12 Al18 O3 9N8 , is suggested for the x1 phase. The lowest melting temperature in the system is ≅ 1480°C and the corresponding composition is 10 eq% Al-90 eq%O. 相似文献
18.
The densification behavior of Si3 N4 containing MgO was studied in detail. It was concluded that MgO forms a liquid phase (most likely a magnesium silicate). This liquid wets and allows atomic transfer of Si3 N4 . Evidence of a second-phase material between the Si3 N4 grains was obtained through etching studies. Transformation of α- to β-Si3 N4 during hot-pressing is not necessary for densification. 相似文献
19.
L. K. V. LOU T. E. MITCHELL A. H. HEUER 《Journal of the American Ceramic Society》1978,61(9-10):392-396
Impurity phases in commercial hot-pressed Si3 N4 were investigated using transmission electron microscopy. In addition to the dominant, β-Si3 N4 phase, small amounts of Si2 N2 O, SiC, and WC were found. Significantly, a continuous grain-boundary phase was observed in the ∼ 25 high-angle boundaries examined. This film is ∼ 10 Å thick between, β-Si3 N4 grains and ∼ 30 Å thick between Si2 N2 O and β-Si3 N4 grains. 相似文献
20.
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