Ti-Si-Fe合金添加量对Si_(3)N_(4)结合SiC材料结构与性能的影响

为促进Si_(3)N_(4)结合SiC耐火材料的致密化,降低Si粉氮化温度,以SiC颗粒和细粉、Si粉为主要原料,利用从高钛型高炉渣提取的Ti-Si-Fe合金部分取代Si粉,在埋碳气氛下于1350℃反应烧结5 h,制备了Si_(3)N_(4)结合SiC耐火材料。研究了Ti-Si-Fe合金添加量(加入质量分数分别为0、1.8%、3.6%、5.4%、7.2%)对Si粉的氮化行为、材料力学性能和显微结构的影响,并探讨了氮化反应烧结机制。结果表明:1)随着Ti-Si-Fe合金添加量的增加,材料的常温力学性能和高温抗折强度明显改善,荷重软化温度均超过1700℃,Ti-Si-Fe合金添加量超过3.6%(w)后材料性能的增幅变缓;2)Ti-Si-Fe合金促进了Si粉在较低温度下的完全氮化和材料的反应烧结,Ti-Si-Fe合金中各物相及Si粉氮化反应的体积增加能够充填气孔,氮化产物改善骨料与基质、基质内部的结合状态,从而提高材料的致密化程度,改善力学性能;3)引入Ti-Si-Fe合金后,反应体系中形成了富含Ti、Si、N、Fe成分的液相,氮化物的形成除传统的VS、VLS机制外,溶解-沉淀机制在短柱状β-Si_(3)N_(4)、粒状TiN的形成中起到主导作用,交错连结的α-Si_(3)N_(4)晶须、短柱状β-Si_(3)N_(4)、粒状TiN对材料的力学性能起到增强作用。

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

SiC/SiBCN-Si_(3)N_(4)复合材料力学性能研究

为了深入了解SiC/SiBCN-Si_(3)N_(4)材料微观形貌与高温力学行为,建立科学可靠的定量表征方法,本文使用多种表征手段对SiC/SiBCN-Si_(3)N_(4)材料进行定量观测,首先进行材料孔隙率及密度的测试,随后进行材料高温原位力学性能测试并对材料损伤机理进行了分析,最后基于试验数据构建了一种可解释的深度学习模型,实现了材料高温非线性本构关系预测。样件力学性能分析结果表明:平均应力预测误差为0.27%~0.59%、平均应变预测误差为1.96%~3.41%;同时通过量化分析明确了影响力学性能的因素依次为温度、偏轴角度、孔隙率及密度。本文实现了不同环境温度、偏轴角度与外载荷作用下SiC/SiBCN-Si_(3)N_(4)宏观力学性能的预测,可为陶瓷基复合材料高温本构模型的建立提供新思路。

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.

Step-scheme porous g-C3N4/Zn0.2Cd0.8S-DETA composites for efficient and stable photocatalytic H2 production

In recent years,environmental pollution and energy crisis have become increasingly serious issues owing to the burning of fossil fuels.Among the many technologies,decomposition of water to produce hydrogen has attracted much attention because of its sustainability and non-polluting characteristic.However,highly efficient decomposition of water that is driven by visible light is still a challenge.Herein,we report the large-scale preparation of step-scheme porous graphite carbon nitride/Zn0.2Cd0.8S-diethylenetriamine(Pg-C3N4/Zn0.2Cd0.8S-DETA)composite by a facile solvothermal method.It was found by UV-vis spectroscopy that 15%Pg-C3N4/Zn0.2Cd0.8S-DETA exhibited suitable visible absorption edge and band gap for water decomposition.The hydrogen production rate of 15%Pg-C3N4/Zn0.2Cd0.8S-DETA composite was 6.69 mmol g^-1 h^-1,which was 16.73,1.61,and 1.44 times greater than those of Pg-C3N4,CdS-DETA,and Zn0.2Cd0.8S-DETA,respectively.In addition,15%Pg-C3N4/Zn0.2Cd0.8S-DETA composite displayed excellent photocatalytic stability,which was maintained for seven cycles of photocatalytic water splitting test.We believe that 15%Pg-C3N4/Zn0.2Cd0.8S-DETA composite can be a valuable guide for the development of solar hydrogen production applications in the near future.

In situ fabrication of CdMoO4/g-C3N4 composites with improved charge separation and photocatalytic activity under visible light irradiation

To further improve the charge separation and photocatalytic activities of g-C3N4 and CdMoO4 under visible light irradiation,CdMoO4/g-C3N4 composites were rationally synthesized by a facile precipitation-calcination procedure.The crystal phases,morphologies,chemical compositions,textural structures,and optical properties of the as-prepared composites were characterized by the corresponding analytical techniques.The photocatalytic activities toward degradation of rhodamine B solution were evaluated under visible light irradiation.The results revealed that integrating CdMoO4 with g-C3N4 could remarkably improve the charge separation and photocatalytic activity,compared with those of pristine g-C3N4 and CdMoO4.This would be because the CdMoO4/g-C3N4 composites could facilitate the transfer and separation of the photoexcited electron-hole pairs,which was confirmed by electrochemical impedance spectroscopy,transient photocurrent responses,and photoluminescence measurements.Moreover,active species trapping experiments demonstrated that holes(h+)and superoxide radicals(?O2?)were the main active species during the photocatalytic reaction.A possible photocatalytic mechanism was proposed on the basis of the energy band structures determined by Mott-Schottky tests.This work would provide further insights into the rational fabrication of composites for organic contaminant removal.

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 ℃ .

In-situ polymerization for PPy/g-C_3N_4 composites with enhanced visible light photocatalytic performance

Polypyrrole‐modified graphitic carbon nitride composites(PPy/g‐C3N4)are fabricated using an in‐situ polymerization method to improve the visible light photocatalytic activity of g‐C3N4.The PPy/g‐C3N4 is applied to the photocatalytic degradation of methylene blue(MB)under visible light irradiation.Various characterization techniques are employed to investigate the relationship between the structural properties and photoactivities of the as‐prepared composites.Results show that the specific surface area of the PPy/g‐C3N4 composites increases upon assembly of the amorphous PPy nanoparticles on the g‐C3N4 surface.Owing to the strong conductivity,the PPy can be used as a transition channel for electrons to move onto the g‐C3N4 surface,thus inhibiting the recombination of photogenerated carriers of g‐C3N4 and improving the photocatalytic performance.The elevated light adsorption of PPy/g‐C3N4 composites is attributed to the strong absorption coefficient of PPy.The composite containing 0.75 wt%PPy exhibits a photocatalytic efficiency that is 3 times higher than that of g‐C3N4 in 2 h.Moreover,the degradation kinetics follow a pseudo‐first‐order model.A detailed photocatalytic mechanism is proposed with·OH and·O2-radicals as the main reactive species.The present work provides new insights into the mechanistic understanding of PPy in PPy/g‐C3N4 composites for environmental applications.

Mechanical Properties and Microstructure of Si_(3)N_(4)-TiC Nanocomposites

Si3N4/TiC nanocomposite ceramics have been fabricated by hot pressing technique with Al2O3 and Y2O3 as additives. The results showed that well dispersed composite powder was carried out by adding dispersant and adjusting pH values of suspensions. Remarkable increase in flexural strength at room temperatures was obtained by adding nanoparticles in Si3N4 matrix with 10% （wt pct） of nano-Si3N4 and 15% of nano-TiC. The flexural strength, fracture toughness and hardness were 1025 MPa, 7.5 MPa.m^1/2 and 15.6 GPa, respectively. The microstructures of materials were analyzed by scanning electron microscopy （SEM） and transmission electron microscopy （TEM）, which indicated that TiC nanoparticles distribute in the matrix and at the grain boundaries. According to the fracture form, low contents of nano particles could refine matrix grains and lead to the crack deflection as well as crack pinning. The multiplex microstructure was formed by mixing nano-Si3N4 particles. The crack trajectories exhibited crack deflection, rod-like grain bridging and pull-out.

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.

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.

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.

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。

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。

Investigation on The Properties of Fe-Si_3N_4 Bonded SiC Composite

The mechanical properties of pressureless sintering Fe-Si_ 3N_ 4 bonded SiC and Si_ 3N_ 4 bonded SiC with same manufacture process have been compared in this paper. The oxidizing mechanism of Fe-Si_ 3N_ 4 bonded SiC ceramic matrix composite has been investigated especially through TG-DSC (thermo gravimetric analysis-differential scanning calorimeter) experiment. During oxidation procedure the main reaction is the oxidation of SiC and Si_ 3N_ 4, SiO_ 2 which form protecting film to prevent further oxidizing. And residual iron in the samples become Fe_ 2O_ 3 and Fe_ 3O_ 4,_ the oxidation kinetics at 1100～1300℃ of Fe-Si_ 3N_ 4 bonded SiC has been studied especially. The weight gain per unit area at initial stage changes according to beeline rule, in the middle according to conic, and in the last oxidation period follows parabola rule.

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。