多孔氮化硅陶瓷的研究进展

综述了多孔氮化硅陶瓷材料的国内外研究现状和进展,介绍了多孔氮化硅陶瓷的主要制备方法,分析了微观组织对多孔氮化硅陶瓷力学性能的影响,并与其他多孔陶瓷进行了性能比较,最后展望了多孔氮化硅陶瓷的发展前景.     

低介电常数多孔氮化硅陶瓷材料的制备

采用有机泡沫前躯体浸渍工艺制备了低介电、低密度的氮化硅陶瓷。以氮化硅粉体为主要原料,制备粘度和流动性合适的水基料浆,并以软质聚氨酯泡沫塑料为载体,在真空状态下浸渍,然后在氧化气氛下排塑,在氮气气氛下烧结,得到了低介电常数的多孔氮化硅陶瓷材料。所制备的材料性能可达到：容积密度为0.12g/cm3、介电常数为1.15、介电...     

多孔氮化硅陶瓷透波材料研究进展

多孔氮化硅陶瓷透波材料具有优异的机械性能、耐热性能及介电性能,成为透波材料科学研究领域中的热点之一。本文介绍了多孔氮化硅陶瓷的主要制备技术,并对国内外多孔氮化硅陶瓷透波材料的应用研究进展进行了综述。     

Synthesis of Porous Silicon Nitride with Unidirectionally Aligned Channels Using Freeze-Drying Process

Porous silicon nitride with macroscopically aligned channels was synthesized using a freeze-drying process. Freezing of a water-based slurry of silicon nitride was done while unidirectionally controlling the growth direction of the ice. Pores were generated subsequently by sublimation of the columnar ice during freeze-drying. By sintering this green body, a porous silicon nitride with high porosity (over 50%) was obtained and its porosity was controllable by the slurry concentration. The porous Si₃N₄ had a unique microstructure, where macroscopically aligned open pores contained fibrous grains protruding from the internal walls of the Si₃N₄ matrix. It is hypothesized that vapor/solid phase reactions were important to the formation mechanism of the fibrous grains.     

多孔石英基体上CVD法沉积氮化硅涂层的工艺、结构与性能研究

以甲硅烷(20％甲硅烷+80％氢气)和氨气作为反应前驱体,选择孔隙率为20％左右的多孔石英陶瓷基体,采用CVD法在多孔石英基体表面制备了氮化硅涂层.研究了沉积反应温度、反应压力、反应气体配比以及沉积时间等工艺参数对附着力的影响,确定了CVD法制备氮化硅涂层的最佳工艺参数,通过对所得涂层及复合材料进行抗弯强度和介电性能的表征,探讨了氮化硅涂层对多孔石英基体力学性能和介电性能的影响.     

低热导率磷酸锆结合氮化硅多孔陶瓷的制备

采用无压烧结工艺制备ZrP2O7结合Si3N4多孔陶瓷,研究了孔隙率对材料抗弯强度和热导率的影响.结果表明:当孔隙率为20％q3％时,热导率为0.4～1.9 W/(m·K);当孔隙率为20％时,热导率下降至1.9 W/(m·K),但力学性能并没有明显降低.当Effective Medium Theory模型的比例系数为0.3、Maxwell-Eucken2模型的比例系数为0.7时,计算所得热导率与实验结果相符.     

酚醛树脂裂解法增强高气孔率多孔氮化硅陶瓷

以酚醛树脂为碳源,采用凝胶注模成型工艺,成功地制备出了具有较高气孔率、高强度、结构比较均匀的氮化硅多孔陶瓷。结果表明,制备出的坯体结构均匀、加工性能优良,烧成的多孔氮化硅陶瓷强度78M Pa,扎孔率可达63%。借助热重分析(TG)、红外分析仪(IR)、X射线衍射(X R D)、扫描电子显微镜(SE M)、A rchim edes法和三点弯曲法等方法对多孔氮化硅陶瓷的微观结构的形成和基本力学性能进行了研究。SE M照片显示气孔是由长柱状β-Si3N4晶搭接而成的,典型的纤维状多孔材料。SR D图谱显示有玻璃碳产生;酚醛树脂裂解所得的玻璃碳与Si3N4表面的SiO2以及Si3N4颗粒本身反应生成了SiC增强相。发育良好的柱晶结构、均匀的气孔分布、以及反应生成的SiC微晶是在材料在高气孔率下仍保持高强度的主要原因。     

低介电高强度多孔氮化硅陶瓷的研制

以氮化硅为基体,通过加入一定量的特殊无机添加剂,控制好相关工艺参数成功地制备出低密高强低介电的多孔氮化硅材料。采用有机涂层对多孔氮化硅材料表面进行封孔处理,通过对封孔前后材料电性能的对比分析得出:涂层对封孔后表面致密的整体材料电性能影响微小。     

Thermal Shock Behavior of Isotropic and Anisotropic Porous Silicon Nitride

The thermal shock behavior of isotropic and anisotropic porous Si₃N₄ was evaluated using the water-quenching technique. The critical temperature difference for crack initiation was found to be strongly dependent on the ratio of fracture strength to elastic modulus. Because of a very high strain-to-failure, anisotropic porous Si₃N₄ showed no macroscopic cracks and was able to retain its strength even at a quenching-temperature difference of ∼1400°C.     

High-Strength Porous Silicon Carbide Ceramics by an Oxidation-Bonding Technique

Porous silicon carbide (SiC) ceramics were fabricated by an oxidation-bonding process in which the powder compacts are heated in air so that SiC particles are bonded to each other by oxidation-derived SiO₂ glass. Because of the crystallization of amorphous SiO₂ glass into cristobalite during sintering, the fracture strength of oxidation-bonded SiC ceramics can be retained to a relatively high level at elevated temperatures. It has been shown that the mechanical strength is strongly affected by particle size. When 0.6 μm SiC powders were used, a high strength of 185 MPa was achieved at a porosity of ∼31%. Moreover, oxidation-bonded SiC ceramics were observed to exhibit an excellent oxidation resistance.     

Fabrication and Microstructure of Silicon Nitride/Boron Nitride Nanocomposites

A chemical process for fabrication of Si₃N₄/BN nanocomposite was devised to improve the mechanical properties. Si₃N₄/BN nanocomposites containing 0 to 30 vol% hexagonal BN ( h -BN) were successfully fabricated by hot-pressing α-Si₃N₄ powders, on which turbostratic BN ( t -BN) with a disordered layer structure was partly coated. The t -BN coating on α-Si₃N₄ particles was prepared by reducing and heating α-Si₃N₄ particles covered with a mixture of boric acid and urea. TEM observations of this nanocomposite revealed that the nanosized hexagonal BN ( h -BN) particles were homogeneously dispersed within Si₃N₄ grains as well as at grain boundaries. As expected from the rules of composites, Young's modulus of both micro- and nanocomposites decreased with an increase in h -BN content, while the fracture strength of the nanocomposites prepared in this work was significantly improved, compared with the conventional microcomposites.     

Effect of β-Seed Addition on the Microstructural Evolution of Silicon Nitride Ceramics

When a small amount of β-Si₃N₄ seed particles is added during the preparation of Si₃N₄ ceramics, a bimodal microstructure is obtained by sintering at 1760°C. When the specimen is further heat-treated at 1900°C to enhance the bimodal characteristic, the growth of large β grains is limited. The addition of a controlled amount of β seeds of uniform and large size is suggested to obtain the intended bimodal microstructure of Si₃N₄ ceramics.     

氮化硅陶瓷在四大领域的研究及应用进展

氮化硅陶瓷不仅具有较高的力学性能还具有良好的透波性能、导热性能以及生物相容性能,是公认的综合性能最优的陶瓷材料。作为轴承球的致密氮化硅陶瓷广泛应用在机械领域;作为透波材料的多孔氮化硅陶瓷广泛应用在航空航天领域;随着对氮化硅陶瓷材料的深入研究,其在导热性和生物相容性方面的优异特性逐渐被科研工作者认识并得到开发和应用。本文详细阐述了氮化硅粉体的制备方法,并综述了氮化硅陶瓷作为结构陶瓷在机械领域和航空航天领域的研究进展,此外还介绍了其作为功能陶瓷在半导体领域、生物制药领域的研究和应用现状,最后对其未来发展进行了展望。     

Seamless Joining of Silicon Nitride Ceramics

High-strength joining of Si₃N₄ ceramics has been achieved by developing a process that effectively eliminates the seam, and may allow for fabrication of large or complex silicon nitride bodies. This approach to joining is based on the concept that when sintering aids are effective in bonding individual grains, they could be equally effective in joining bulk pieces of Si₃N₄. Optimization of the process led to Si₃N₄/Si₃N₄ joints with room-temperature bend strengths as high as 950 MPa, corresponding to more than 90% of the bulk strength of the Si₃N₄. At elevated temperatures of 1000° and 1200°C joint strengths of 666 and 330 MPa, respectively, were obtained, which are the highest values reported to date for these temperatures. These bend strengths are also more that 90% of the strength of bulk Si₃N₄ measured at these temperatures.     

Elevated-Temperature Mechanical Properties of Silicon Nitride/Boron Nitride Fibrous Monolithic Ceramics

A unique, all-ceramic material capable of nonbrittle fracture via crack deflection and delamination has been mechanically characterized from 25° through 1400°C. This material, fibrous monoliths, was comprised of unidirectionally aligned 250 μm diameter silicon nitride cells surrounded by 10 to 20 μm thick boron nitride cell boundaries. The average flexure strengths of fibrous monoliths were 510 and 290 MPa for specimens tested at room temperature and 1300°C, respectively. Crack deflection in the BN cell boundaries was observed at all temperatures. Characteristic flexural responses were observed at temperatures between 25° and 1400°C. Changes in the flexural response at different temperatures were attributed to changes in the physical properties of either the silicon nitride cells or boron nitride cell boundary.     

三维网络结构多孔氮化硅陶瓷增强体的制备

以Si3N4和Si粉为主要原料,Al2O3、Y2O3等为助剂,制备Si3N4料浆,用有机前驱体浸渍和二次烧成工艺来制备具有网络结构的多孔氮化硅陶瓷增强体.结果表明:二次烧成能显著提高材料性能,烧成温度在1600～1700℃为宜.用XRD、SEM、XEDS等对二次烧成材料的显微结构和晶相进行分析,研究二次烧成制度改善材料性能的原因,以利于更好的优化工艺.     

Bonding of Dense Silicon Nitride with Carbon Interlayers

Diffusion bonding of dense Si₃N4 containing 10% Ce₂O₃, 7% A1₂O₃, and 2% Y₂O₃ was attempted through hot pressing at temperatures of 1000° to 1400°C. Physically vapor-deposited (PVD) carbon and paraffin-wax candle soot were tried as interlayers. The interfaces were analyzed through optical and scanning electron microscopy, and through X-ray photoelectron spectroscopy. The bonding temperature could be reduced from 1400° (without interlayers) to 1100°C with PVD carbon or candle soot. From C Is and Si 2p spectra, the formation of SiC at the interface through the reaction of C with the silicon oxynitride layer has been identified.     

Thermal Shock Behavior of Porous Silicon Carbide Ceramics

Using the water-quenching technique, the thermal shock behavior of porous silicon carbide (SiC) ceramics was evaluated as a function of quenching temperature, quenching cycles, and specimen thickness. It is shown that the residual strength of the quenched specimens decreases gradually with increases in the quenching temperature and specimen thickness. Moreover, it was found that the fracture strength of the quenched specimens was not affected by the increase of quenching cycles. This suggests a potential advantage of porous SiC ceramics for cyclic thermal-shock applications.     

Porous 2H-Silicon Carbide Ceramics Fabricated by Carbothermal Reaction between Silicon Nitride and Carbon

Porous SiC ceramics were synthesized by sintering pressed and pressed/CIPed powder compacts of α-Si₃N₄, carbon (Si₃N₄:C = 1:3 mol as ratio), and sintering aids, at 1600°C for few hours to achieve a reaction, and subsequently sintering at a temperature range of 1750°–1900°C, in an argon atmosphere. High porosities from 45%–65% were achieved by low shrinkage with large weight loss. Formation of pure 2H-SiC phase via a reaction between Si₃N₄ and carbon can be demonstrated by X-ray diffractometry. The resultant porous SiC samples were characterized by SiC grain microstructures, pore-size distribution, and flexural strength. This method has the advantage of fabricating high-porous SiC ceramics with fine microstructure and good properties at a relatively low temperature.     

基于熔融沉积技术的多孔氮化硅陶瓷制备与烧结研究

通过增材制造制备复杂结构的多孔氮化硅陶瓷备受关注。然而,由于陶瓷脆而硬的特性不能直接用于挤压成型。因此,开发一种兼备高温流动稳定性、高均匀性双重功能的多孔氮化硅陶瓷喂料的方法,成功解决陶瓷不能直接应用于熔融沉积成型的困难。即加入石蜡、塑料等有机成分来使陶瓷粉末易于加热为熔融状态,并具有较好的流动性。此外,通过引入表面活性剂、有机粘结剂对陶瓷粉料进行表面改性,提升融合水平。该方法成功地解决了陶瓷不能直接应用于熔融沉积成型的困难,也适用于大范围陶瓷体系基于熔融沉积技术制备,最后对制备的夹层结构陶瓷力热电性能进行测试。