Fabrication of Fine-Grained Si_3N_4-Si_2N_2O Composites by Sintering Amorphous Nano-sized Silicon Nitride Powders

Si3N4-Si2N2O composites were fabricated with amorphous nano-sized silicon nitride powders by the liquid phase sintering （ LPS ）. The Si2 N2O phase was generated by an in-situ reaction 2 Si3 N4 （ s ） ＋ 1.5 02 （ g ） = 3 Si2 N2O （ s ） ＋ N2 （ g ） . The content of Si2 N2 O phase up to 60% in the volume was obtained at a sintering temperature of 1 650℃ and reduced when the sintering temperature increased or decreased, indicating the reaction is reversible. The mass loss, relative density and average grain size increased with increasing the sintering temperature. The average grain size was less than 500 nm when the sintering temperature was below 1 700 ℃. The sintering procedure contains a complex crystallization and a phase transition ： amorphous silicon nitride→equiaxial α- Si3 N4→ equiaxial β- Si3 N4→ rod- like Si2 N2O→ needle- like β- Si3N4 . Small round-shaped β→ Si3 N4 particles were entrapped in the Si2 N2O grains and a high density of staking faults was situated in the middle of Si2 N2O grains at a sintering temperature of 1 650 ℃. The toughness inereased from 3.5 MPa·m^1/2 at 1 600 ℃ to 7.2 MPa· m^1/2 at 1 800 ℃ . The hardness was as high as 21.5 GPa （Vickers） at 1 600 ℃ .

Microstructure and Mechanical Properties of Si_3N_4 Composites Containing SiC Platelet

Hoppressed Si3N4/SiC platelet composites had been investigated with respect to their microstructure and mechanical properties. The results indicate that Vickers hardness, elastic modulus and fracture toughness of the composites were increased by the addition of SiC platelet until the content up to 20 vol pct. A slight decrease in flexural Strength was measured at room temperature with increasing SiC platelet content. The high temperature flexural strength tests at 1150, 1250, and 1350℃ were conducted. It was found that the flexural strength at elevated temperature was degraded with the rising temperature, and the downward trend of flexural strength for the composite containing 10 vol. pct SiC platelet was less. The results indicate that SiC platelet had a positive influence on the high temperature strength. Effects of SiC platelet reinforcement were presented

Study on Microstructures of Micron Si_3N_4 Composite Ceramic with Addition of Nano SiC and SiC Whisker

The microstructures and crack propagating characteristic of Si 3N 4 (μ)/SiC (n, w) composite ceramic were studied with AEM. The Si 3N 4 (μ)/SiC (n, w) composite ceramic consists of β Si 3N 4, β SiC, a small amount of α Si 3N 4 and α SiC, and amorphous phase. Most of Si 3N 4 grains were equiaxed crystal and also there were some bulky columnar ones. Most of SiC particles and SiC whiskers distributed at the Si 3N 4 grain boundaries and a few of smaller SiC particles in the Si 3N 4 grains. Most of amorphous structure was in the junction of several Si 3N 4 grains and thin amorphous layer was observed only at a few of Si 3N 4 boundaries. Failured cracks propagated mainly along the boundaries of the Si 3N 4 grains and partially passed through Si 3N 4 grains. The path of crack propagating might change, branching and twisting of the cracks might occur when the expanding crack meet the SiC particle and/or SiC whisker. Effect of the microstructure on strength and toughness of the composite ceramic was briefly discussed.

Mechanism of toughening and strengthening of Si_3N_4/SiC/ZrO_2 nanocomposites

The Si3N4-based nanocomposites reinforced with micro ZrO2 and nano SiC particles were prepared by polarity dispersant and vacuum-sintering technology. The mechanical properties and microstructures were tested. The results show that appropriate amount of micro ZrO2 and nano SiC particles, not only enhance the microhardness, but also block the excessively growth of β-Si3N4 and β-Si3N4 grains, so they finally all grow up to uniformly pole-shaped grains. This process is similar to the strengthening and toughening mechanism of grain whiskers and makes a remarkable improvement on the toughness. Compared with Si3N4 ceramic, the toughness of Si3N4/SiC/ZrO2 nanocomposites are increased from 6.2 MPa·m1/2 to 11 MPa·m1/2.

Effect of hexagonal-BN on phase transformation of additive-free Si_3N_4 /SiC nanocomposites prepared from amorphous precursor

Si3N4/SiC nanocomposites are well known and attractive for advanced ceramic applications due to excellent mechanlcal and thermal properties, which make them suitable for use in turbine engines, heat exchangers, and other sophisticated applications. However, without the presence of additives, the fabrication of Si3N4/SiC composites is difficult. The additives form a liquid phase during sintering and facilitate the densification of the composite. However, the additives present a drawback at high temperatures since they decrease the mechanical properties of the composites. Recently, Si3N4/SiC composites were fabricated via the polymer precursor route without any additives, using electric field assisted sintering （EFAS）. In this study, fully densified Si3N4/SiC nanocomposites incorporating hexagonal-BN were successfully fabricated by hot pressing without any additives at 1700 ℃ for 2 h under vacuum at a pressure of 50 MPa （via the amorphous precursor route）. Moreover, the incorporation of additives and h-BN is found to decrease the content of SiC. The phase transformation, densification, microstructure, and mechanical properties were discussed and presented.

DIELECTRIC PROPERTIES OF NANO Si/C/N COMPOSITE POWDER AND NANO SiC POWDER AT HIGH FREQUENCIES AND MICROSTRUCTURE CHARACTERIZATION

The dielectric properties of nano Si/C/N composite powder and nano SiC powder at high frequencies have been studied. The nano Si/C/N composite powder and nano SiC powder were synthesized from hexamethyldisilazane ((Me 3Si) 2NH) (Me:CH 3) and SiH 4 C 2H 2 respectively by a laser induced gas phase reaction. The complex permittivities of the nano Si/C/N composite powder and nano SiC powder were measured between 8 2GHz and 12 4GHz. The real and imaginary parts of the complex permittivities of nano Si/C/N composite powder are much higher than those of nano SiC powder. The SiC microcrystalline in the nano Si/C/N composite powder dissolved a great deal of nitrogen. The local structure around Si atoms changed by introducing N into SiC. Carbon atoms around Si were substituted by N atoms. So charged defects and quasi free electrons moved in response to the electric field, diffusion or polarization current resulted from the field propagation. The high ε″and loss factor tgδ(ε″/ε′) of Si/C/N composite powder were due to the dielectric relaxation.

Effect of annealing on microstructure and properties of Si_3N_4-AlN composite ceramics

Aiming at developing novel microwave-transparent ceramics with low dielectric loss, high thermal conductivity and high strength, Si3Na-AIN （30%, mass fraction） composite ceramics with La203 as sintering additive were prepared by hot-pressing at 1 800 ℃ and subsequently annealed at 1 450 ℃ and 1 850 ℃ for 2 h and 4 h, respectively. The materials were characterized by XRD and SEM. The effect of annealing process on the phase composition, sintering performance, microstructure, bending strength, dielectric loss and thermal conductivity of the materials was investigated. The results showed that both annealing at 1 850 ℃ and 1 450 ℃ promoted the phase transformation of α-Si3N4 to β-Si3N4. After annealing at 1 850 ℃, grain growth to a certain extent occurred in the materials. Especially, the elongated β-Si3N4 grains showed a slight increase in diameter from 0.2 μm to 0.6 μm approximately and a decrease in aspect ratio. As a result, as the annealing time increased to 4 h, the bending strength declined from 456 MPa to 390 MPa, whereas the dielectric loss decreased to 2.15× 10^-3 and the thermal conductivity increased to 16.3 W/（m.K） gradually. When annealed at 1 450 ℃, increasing the annealing time to 4 h significantly promoted the crystallization of glassy phase to La2Si6N803 phase in the materials, which led to the increase in bending strength to 619 MPa and thermal conductivity to 15.9 W/（m·K）, respectively, and simultaneously the decrease in dielectric loss to 1.53× 10^-3.

Fabrication and characterization of SiO_(2(f))/Si)_3N_4 composites

A silicon dioxide fiber-reinforced silicon nitride matrix （SiOJSi3N4） composite used for radomes was prepared by chemical vapor infiltration （CVI） process using the SiCl4-NH3-H2 system. The effects of the process conditions, including infiltration temperature, infiltration time, and gas flux were investigated. The energy dispersion spectra （EDS） result showed that the main elements of this composite contained Si, N, and O. The X-ray diffraction （XRD） results indicated that phases of the composite before and after treatment at 1350℃ were all amorphous. A little fiber pull-out was observed on the cross section of the composite by scan electron microscope （SEM）. As a result, the composite exhibited good thermal stability, but an appropriate interface was necessary between the fiber and the matrix.

Processing and performance of 2D fused-silica fiber reinforced porous Si_3N_4 matrix composites

Two-dimension （2D） fused-silica fiber reinforced porous silicon nitride matrix composites were fabricated using slurry impregnation and cyclic infiltration with colloidal silica sol. The microstructure and fracture surface were characterized by SEM, the mechanical behavior was investigated by three-point bending test, and the dielectric constant was also measured by impedance analysis. The microstructure showed that the fiber and the matrix had a physical bonding, forming a clearance interface. The mechanical behavior suggested that the porous matrix acted as crack deflection, and the fracture surface had a lot of fiber pull-out. However, the interlaminar shear strength was not so good. The dielectric constant of the composites at room temperature was about 2.8-3.1. The relatively low dielectric constant and non-catastrophic failure indicated the potential application in the radome materials field. 2008 University of Science and Technology Beijing. All rights reserved.

晶硅切割废粉为原料的反应烧结Si_3N_4结合SiC复相陶瓷的工艺研究

以晶硅切割废料Si粉和SiC为原料,Y2O3-Al2O3-Fe2O3为复合烧结助剂,反应烧结法制备低压铸造升液管用Si3N4/SiC复相陶瓷材料。设计L9(34)正交实验,研究了原料中Si、助剂Al2O3、Y2O3和Fe2O3的含量对陶瓷材料力学性能的影响和优化。采用X射线衍射(XRD)和扫描电镜(SEM)对复合材料的相组成、断口形貌进行分析。结果表明,反应烧结后试样生成Si3N4结合SiC晶粒为主相的烧结体,并含有少量SiALON及未反应的Si。Si含量对力学性能的影响最为显著,通过对正交试验的验证,20wt%Si、3.2wt%Al2O3、0.8wt%Fe2O3和2 wt%Y2O3时烧结体抗弯强度最高。

放电等离子快速烧结SiC晶须增强Si_3N_4BN层状复合材料

采用放电等离子烧结技术(SPS)快速烧结了SiC晶须增强的Si3N4/BN层状复合材料.利用SPS技术,在烧结温度为1650℃、保温15min的条件下,材料的密度可达3.18g/cm3,抗弯强度高达600MPa,断裂功达到3500J/m2.研究表明:特殊的层状结构、SiC晶须的拔出与折断是材料断裂功提高的主要原因.X射线衍射及扫描电子显微镜研究表明:α-Si3N4已经在短短的烧结过程中全部转变成长柱状的β-Si3N4,并且长柱状的β-Si3N4和SiC晶须具有明显的织构.

反应烧结制备Si3N4/SiC复相陶瓷及其力学性能研究

以两种不同配比Y2O3/Al2O3(A,2:3;B,3:1,总量15 wt%)为烧结助剂,通过添加不同质量分数的SiC粉体,反应烧结制备了高强度的氮化硅/碳化硅复相陶瓷。并对材料的相组成、相对密度、显微结构和力学性能进行了分析。结果表明:在1700℃保温2 h情况下,烧结助剂A与B对应的样品中α-Si3N4相全部转化为β-Si3N4;添加5wt%SiC,烧结助剂A对应样品的相对密度达到最大值94.8%,且抗弯强度为521.8 MPa,相对于不添加SiC样品的抗弯强度(338.7 MPa)提高了约54.1%。SiC能有效改善氮化硅基陶瓷力学性能,且Si3N4/SiC复相陶瓷断裂以沿晶断裂方式为主。

Si_3N_4-Fe对Al_2O_3-SiC-C质铁沟浇注料性能的影响

利用Si3N4 的优良性质及金属塑性相Fe的作用 ,将其添加到高炉出铁沟用Al2 O3-SiC -C浇注料中 ,以改善材料的力学性能和抗氧化性能。对高温处理后试样强度、显气孔率测试以及对氧化层的SEM分析 ,结果表明 ,添加适量的Si3N4 -Fe ,材料的显气孔率降低 ,强度提高 ,抗氧化性增强。

Si_3N_4/SiC纳米复合陶瓷的微观结构

利用ＪＥＭ２０００ＥＸⅡ高分辨电镜和ＨＦ２０００冷场发射枪透射电镜对Ｓｉ３Ｎ４ＳｉＣ纳米复合陶瓷材料的微观组织、结构和成分进行了研究。结果表明，ＳｉＣ颗粒弥散分布在基体相β－Ｓｉ３Ｎ４晶内和晶界。晶内ＳｉＣ颗粒与基体相的界面结构有三种类型：１）直接结合的界面；２）完全非晶态的界面；３）混合型的界面。晶间ＳｉＣ颗粒与基体相的界面大部分是直接结合的。

采用SiC/Si_3N_4陶瓷先驱体连接反应烧结SiC

采用SiC/Si3N4陶瓷先驱体聚硅氮烷连接反应烧结碳化硅陶瓷,研究了连接温度、连接压力、浸渍/裂解增强处理对连接强度的影响。结果表明:在1100℃~1400℃温度范围内,连接强度先升高后降低;连接过程中施加适当的轴向压力可提高连接层致密度;浸渍/裂解增强处理可大幅度提高接头强度。当连接温度为1300℃,连接压力为15kPa,经3次增强处理的连接件抗弯强度达最大值169.1MPa。这种连接件的断口表面粘有大量SiC母材。由XRD研究表明,随着温度的逐步升高,聚硅氮烷的裂解产物发生了由非晶态向晶态的转变。微观结构及成分分析显示:连接层为厚度2μm^3μm的SiCN无定形陶瓷,其结构较为均匀致密;连接层与基体间界面接合良好。

烧结工艺对Si_3N_4-SiC材料性能的影响

本文采用氮化硅作为碳化硅材料的结合相的方法制备氮化硅结合碳化硅耐火材料 ,通过对氮化硅结合碳化硅的烧结工艺过程的探讨 ,推导了理论密度、气孔率与生坯密度的关系及影响材料氮化率的关系式 。

燃烧合成理论基础和合成SiC/Si_3N_4复相原料进展

综述了燃烧合成法的热力学和动力学理论基础,并介绍了计算机模拟燃烧合成过程的研究进展。随着高性能SiC/Si3N4纳米陶瓷的发展,采用燃烧合成方法廉价制备SiC/Si3N4原料粉体将成为研究热点,机械活化法、化学激励法、气相法、低温合成法、复合法和计算机模拟等技术将加速高性能SiC/Si3N4原料粉体商业化开发进程。

B_4C加入量对Si_3N_4结合SiC材料抗氧化性的影响

为提高Si_3N_4结合SiC材料的高温抗氧化性,在黑碳化硅(粒度1.43~0.5和≤0.5 mm的颗粒料及粒度≤0.064 mm细粉)、硅粉(粒度≤0.043 mm)的基础配料中引入不同含量的B4C,以木质素磺酸钙为结合剂,经混练、成型、烘干后,在N2气氛下1 450℃保温10 h热处理,制备了Si_3N_4结合SiC材料。研究了900℃水蒸气气氛下,B_4C加入量(质量分数分别为0.4%、0.8%、1.2%、1.6%)对Si_3N_4结合Si C材料抗氧化性的影响。结果表明:Si_3N_4结合SiC材料中加入B_4C后,材料的体积密度增大,显气孔率减小,质量变化率改变,体积变化率减小,材料的抗氧化性得到显著提高,最合适的B_4C加入量(w)为0.4%。

稻壳灰制备Si_3N_4/SiC复合粉体的研究

本文主要研究不同的SiO2∶C比例对所制备Si3N4/SiC复合粉体组成的影响。采用生物质能电厂所产生的工业废弃物稻壳灰和炭黑为原料,以稻壳灰中的SiO2为标准与炭黑配成不同比例的粉料,在氮气气氛下经1550℃保温3 h热处理。采用X射线衍射(XRD)和扫描电子显微镜(SEM)分析烧后试样的物相组成和显微结构。结果表明:当SiO2∶C为5∶6时得到的产物为Si3N4/SiC复合粉体;当SiO2∶C为5∶2和5∶3时,得到产物的组成为SiC、O'-Sialon和β-Si3N4。

Si_3N_(4(p))/SiC_((w))协同复合MoSi_2材料的强韧化及机理研究

采用X射线衍射(XRD)、扫描电子显微镜(SEM)、维氏硬度计、电子万能材料试验机研究MoSi2-Si3N4(p)/SiC(w)复合材料的结构、形貌、硬度、断裂韧性,并对SiC晶须和Si3N4颗粒复合强韧化MoSi2的机理进行了探讨。结果表明,SiC晶须和Si3N4颗粒对MoSi2具有协同强韧化作用,MoSi2-20%Si3N4(p)-20%SiC(w)(体积分数,下同)复合材料的抗弯强度达427MPa,室温断裂韧性达到10.4MPa·m1/2,均高于单一强韧化剂的强韧化效果。MoSi2-20%Si3N4(p)-20%SiC(w)复合材料的强化机理为细晶强化和弥散强化;韧化机制为细晶韧化、裂纹偏转与分支和微桥接韧化。