By employing sintering additives of Li2CO3 and Y2O3,porous Si3N4 ceramics are prepared after experiencing the processes of sintering and post-vacuum heat treatment at 1680 and 1550°C,respectively.The experimental...By employing sintering additives of Li2CO3 and Y2O3,porous Si3N4 ceramics are prepared after experiencing the processes of sintering and post-vacuum heat treatment at 1680 and 1550°C,respectively.The experimental results demonstrate the completed phase transformation fromαtoβ-Si3N4 in Si3N4 ceramic samples with a amount of 1.60 wt%Li2CO3(0.65 wt%Li2O)and 0.33 wt%Y2O3 additives.The as-synthesized porous Si3N4 ceramics exhibit high flexural strength((126.7±2.7)MPa)and high open porosity of 50.4%at elevated temperature(1200°C).These results are attributed to the significant role of added Li2CO3 as sintering additive,where the volatilization of intergranular glassy phase occurs during sintering process.Therefore,porous Si3N4 ceramics with desired mechanical property prepared by altering the addition of sintering additives demonstrate their great potential as a promising candidate for high temperature applications.展开更多
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 wer...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.展开更多
The effect of rare earth oxides Y 2O 3 or CeO 2 on sintering properties of Si 3N 4 ceramics was studied and the mechanism of assisting action during sintering was analyzed. The results indicate that the best sint...The effect of rare earth oxides Y 2O 3 or CeO 2 on sintering properties of Si 3N 4 ceramics was studied and the mechanism of assisting action during sintering was analyzed. The results indicate that the best sintering properties appear in Si 3N 4 ceramics with 5% Y 2O 3 or 8% CeO 2. Secondary crystallites are formed at grain boundaries after heat treatment, which decreases the amount of glass phase and contributes to the improvement of high temperature mechanical properties of silicon nitride.展开更多
Grinding is a most important machining method for Si3N4 ceramics. Utilizing interracial chemistry reaction membrane between grinding fluid and Si3N4 ceramics can reduce friction factor, soften surface layer and meanwh...Grinding is a most important machining method for Si3N4 ceramics. Utilizing interracial chemistry reaction membrane between grinding fluid and Si3N4 ceramics can reduce friction factor, soften surface layer and meanwhile improve the grinding efficiency, which is a bran-new research direction. This article, based on high efficiency grinding of Si3N4 ceramics by the way of half plasticity removal, descanted on the assistant function of interface chemistry reaction to improve the removal rate of Si3N4 ceramics in the application of organic grinding fluids represented by alcohols grinding fluid. To target action mechanism research, it applies the methods of classification, comparison and induction, and advanced test equipments to explore the effects of long, short carbochain alcohol and their water solutions acting as grinding fluids. In addition, it also discusses the effective function of three groups of organic matters such as perhalogeno hydrocarbon, cationic surfactant and tetra ethoxysilane acting as grinding fluid components from different angles, reveals their mechanisms of action, and supplies theoretical basis for the development of machining ceramic grinding fluid of high efficiency, low cost.展开更多
Solid liquid state pressure bonding of Si 3N 4 ceramics with aluminum based alloys, which contain a small amount of intermetallic compounds Al 3Ti or Al 3Zr, was investigated. With this new method, the heat resistant ...Solid liquid state pressure bonding of Si 3N 4 ceramics with aluminum based alloys, which contain a small amount of intermetallic compounds Al 3Ti or Al 3Zr, was investigated. With this new method, the heat resistant properties of the bonding zone metal are improved, and the joints’ strengths at high temperature is increased. The joints’ shear strength at room temperature and at 600 ℃ reach 126～133 MPa and 32～34 MPa, respectively, with suitable bonding pressure. The reaction between aluminum and Si 3N 4 ceramics, which produces Al Si N O type compounds is the dominant interfacial reaction, while the reactions between the second active element Ti or Zr in the aluminum based alloys and Si 3N 4 ceramics also occur to some extend. [展开更多
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 smal...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.展开更多
Bonding of Si 3N 4 ceramic was performed with Y 2O 3 Al 2O 3 SiO 2(YAS) X glass solders,which were mixed with TiO 2 (YT) and Si 3N 4 (YN), respectively. The effects of bonding conditions and interfacial r...Bonding of Si 3N 4 ceramic was performed with Y 2O 3 Al 2O 3 SiO 2(YAS) X glass solders,which were mixed with TiO 2 (YT) and Si 3N 4 (YN), respectively. The effects of bonding conditions and interfacial reaction on the joint strength were studied. The joint strength in different bonding conditions was measured by four point bending tests. The interfacial microstructures were observed and analyzed by SEM, EPMA and XRD. It is shown that with the increase of bonding temperature and holding time, the joint strength increases reaching a peak, and then decreases. When TiO 2 is put into YAS solder,the bonding interface with Si 3N 4/(Y Sialon glass+TiN)/TiN/Y Sialon glass is formed. When YAS solder is mixed with Si 3N 4 powder, the interfacial residual thermal stress may be decreased, and then the joint strength is enhanced. According to microanalyses, the bonding strength is related to interfacial reaction.展开更多
Inorganic coating was fabricated on the surface of the porous Si3N4 ceramic by polymer derived（PD） and spraying technology, via using vinyl-polysilazane（PSN-1） as a preceramic polymer and Si3N4 and lithium alumino...Inorganic coating was fabricated on the surface of the porous Si3N4 ceramic by polymer derived（PD） and spraying technology, via using vinyl-polysilazane（PSN-1） as a preceramic polymer and Si3N4 and lithium aluminosilicate（LAS） powders as fillers. The phase and microstructure of the coatings were analyzed by X-ray diffraction（XRD） analysis and scanning electron microscopy（SEM）, respectively. The effect of the coatings on mechanical property and humidity resistance of the porous Si3N4 ceramic was investigated. The experimental results showed that we successfully fabricated the uniform and dense coating which preferably combined with the substrate upon the addition of fillers. The bending strength of the porous Si3N4 ceramic sprayed the coating increased by more than 18%, and the surface hardness increased by 1.7 times. The apparent porosity of the materials reduced by an average of 97.7%, and water absorption was below 0.5%. Therefore, the prepared coating with preferable density had an obviously moisture-proof and enhanced effect on the porous Si3N4 ceramic.展开更多
基金Project(202045007)supported by the Start-up Funds for Outstanding Talents in Central South University,China。
文摘By employing sintering additives of Li2CO3 and Y2O3,porous Si3N4 ceramics are prepared after experiencing the processes of sintering and post-vacuum heat treatment at 1680 and 1550°C,respectively.The experimental results demonstrate the completed phase transformation fromαtoβ-Si3N4 in Si3N4 ceramic samples with a amount of 1.60 wt%Li2CO3(0.65 wt%Li2O)and 0.33 wt%Y2O3 additives.The as-synthesized porous Si3N4 ceramics exhibit high flexural strength((126.7±2.7)MPa)and high open porosity of 50.4%at elevated temperature(1200°C).These results are attributed to the significant role of added Li2CO3 as sintering additive,where the volatilization of intergranular glassy phase occurs during sintering process.Therefore,porous Si3N4 ceramics with desired mechanical property prepared by altering the addition of sintering additives demonstrate their great potential as a promising candidate for high temperature applications.
基金Project(50872052) supported by the National Natural Science Foundation of ChinaProject(2009AA05Z313) supported by the National High Technology Research and Development Program of ChinaProject supported by the Commission of Science,Technology and Industry for National Defence,China
文摘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.
文摘The effect of rare earth oxides Y 2O 3 or CeO 2 on sintering properties of Si 3N 4 ceramics was studied and the mechanism of assisting action during sintering was analyzed. The results indicate that the best sintering properties appear in Si 3N 4 ceramics with 5% Y 2O 3 or 8% CeO 2. Secondary crystallites are formed at grain boundaries after heat treatment, which decreases the amount of glass phase and contributes to the improvement of high temperature mechanical properties of silicon nitride.
文摘Grinding is a most important machining method for Si3N4 ceramics. Utilizing interracial chemistry reaction membrane between grinding fluid and Si3N4 ceramics can reduce friction factor, soften surface layer and meanwhile improve the grinding efficiency, which is a bran-new research direction. This article, based on high efficiency grinding of Si3N4 ceramics by the way of half plasticity removal, descanted on the assistant function of interface chemistry reaction to improve the removal rate of Si3N4 ceramics in the application of organic grinding fluids represented by alcohols grinding fluid. To target action mechanism research, it applies the methods of classification, comparison and induction, and advanced test equipments to explore the effects of long, short carbochain alcohol and their water solutions acting as grinding fluids. In addition, it also discusses the effective function of three groups of organic matters such as perhalogeno hydrocarbon, cationic surfactant and tetra ethoxysilane acting as grinding fluid components from different angles, reveals their mechanisms of action, and supplies theoretical basis for the development of machining ceramic grinding fluid of high efficiency, low cost.
文摘Solid liquid state pressure bonding of Si 3N 4 ceramics with aluminum based alloys, which contain a small amount of intermetallic compounds Al 3Ti or Al 3Zr, was investigated. With this new method, the heat resistant properties of the bonding zone metal are improved, and the joints’ strengths at high temperature is increased. The joints’ shear strength at room temperature and at 600 ℃ reach 126～133 MPa and 32～34 MPa, respectively, with suitable bonding pressure. The reaction between aluminum and Si 3N 4 ceramics, which produces Al Si N O type compounds is the dominant interfacial reaction, while the reactions between the second active element Ti or Zr in the aluminum based alloys and Si 3N 4 ceramics also occur to some extend. [
文摘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.
文摘Bonding of Si 3N 4 ceramic was performed with Y 2O 3 Al 2O 3 SiO 2(YAS) X glass solders,which were mixed with TiO 2 (YT) and Si 3N 4 (YN), respectively. The effects of bonding conditions and interfacial reaction on the joint strength were studied. The joint strength in different bonding conditions was measured by four point bending tests. The interfacial microstructures were observed and analyzed by SEM, EPMA and XRD. It is shown that with the increase of bonding temperature and holding time, the joint strength increases reaching a peak, and then decreases. When TiO 2 is put into YAS solder,the bonding interface with Si 3N 4/(Y Sialon glass+TiN)/TiN/Y Sialon glass is formed. When YAS solder is mixed with Si 3N 4 powder, the interfacial residual thermal stress may be decreased, and then the joint strength is enhanced. According to microanalyses, the bonding strength is related to interfacial reaction.
文摘Inorganic coating was fabricated on the surface of the porous Si3N4 ceramic by polymer derived（PD） and spraying technology, via using vinyl-polysilazane（PSN-1） as a preceramic polymer and Si3N4 and lithium aluminosilicate（LAS） powders as fillers. The phase and microstructure of the coatings were analyzed by X-ray diffraction（XRD） analysis and scanning electron microscopy（SEM）, respectively. The effect of the coatings on mechanical property and humidity resistance of the porous Si3N4 ceramic was investigated. The experimental results showed that we successfully fabricated the uniform and dense coating which preferably combined with the substrate upon the addition of fillers. The bending strength of the porous Si3N4 ceramic sprayed the coating increased by more than 18%, and the surface hardness increased by 1.7 times. The apparent porosity of the materials reduced by an average of 97.7%, and water absorption was below 0.5%. Therefore, the prepared coating with preferable density had an obviously moisture-proof and enhanced effect on the porous Si3N4 ceramic.
