多孔BN/Si_3N_4复合陶瓷的制备与性能研究
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摘要
透波材料是一种集透波、防热、承载和抗蚀等多功能于一体的材料，它可以保护飞行器的天线系统，使其在恶劣环境下能够正常工作。随着飞行器的发展和飞行速度的不断提高，对透波材料介电性能、力学性能、寿命、工艺性和重量等方面要求越来越高。氮化硅（Si_3N_4）材料具有优异的力学性能、良好的热稳定性和耐腐蚀性能，是一种综合性能较高的飞行器天线罩用材料。但通过研究发现，Si_3N_4作为高速飞行器天线罩材料时，其介电性能不够理想，有待进一步提高。氮化硼（BN）具有比Si_3N_4更低的介电常数和介电损耗，而且在很宽的温度范围内具有优良的热、电性能稳定性，但其力学性能低于Si_3N_4、抗雨蚀性能差。本文将Si_3N_4和BN相结合，制备出具有Si_3N_4和BN各自优点的BN/Si_3N_4复合材料。
由于多孔陶瓷具有较低的介电常数和密度，因此在制备BN/Si_3N_4复合材料时，应尽可能提高材料的气孔率。本文通过采用叔丁醇（TBA）基凝胶注模成型工艺制备高气孔率、高强度、低介电常数和介电损耗的BN/Si_3N_4复合陶瓷。优化了TBA基凝胶注模成型工艺各阶段的工艺参数，使该工艺适用于制备高气孔率的BN/Si_3N_4复合陶瓷。通过研究，加入0.144g/l（相对于溶剂体积）分散剂的浆料的流变性能较好；催化剂（MBAM）和引发剂（APS）水溶液最佳含量分别为1.5wt%和30wt%（相对于单体），40℃下N2保护聚合及保湿干燥制度较为合理。
为了验证TBA基凝胶注模工艺在制备多孔BN/Si_3N_4复合陶瓷上的优越性，本文选取目前多孔陶瓷制备方法中应用最为广泛的干压成型工艺及造孔剂工艺与之进行对比实验，从微观结构到宏观性能进行了比较分析。研究发现，TBA基凝胶注模工艺的优势在于其能够制备出均匀可控，且具有高气孔率的结构。并可以通过调节固相含量得到不能性能的多孔BN/Si_3N_4复合陶瓷。当固相含量为7.5vol%时，气孔率为77.4%，介电常数为1.74；固相含量为30vol%时，气孔率为36.5%，抗弯强度为136±5.35MPa。
在浆料中初始固相含量固定为15%体积分数的基础上，分别研究了烧结助剂Y2O3-Al2O3和SiO2的含量以及烧结温度的影响。结果表明，多孔BN/Si_3N_4复合陶瓷的气孔率随着烧结助剂含量的提高而下降，孔径呈单峰分布，尺寸为微米级或亚微米级。抗弯强度随着烧结助剂含量的提高而增大，介电常数随之上升。当Y2O3-Al2O3含量为5wt%，SiO_2含量为7.5wt%时，多孔BN/Si_3N_4复合陶瓷的抗弯强度为65.84±3.08MPa，室温下的介电常数非常稳定，在2.39附近波动，介电损耗在3×10~(-3)以下，并具有优异的高温介电性能。通过对烧结温度的研究，结果发现，在1750℃烧结温度下，Si_3N_4发育良好，具有优异的综合性能。
研究了添加剂BN的加入量对多孔BN/Si_3N_4复合陶瓷的结构和性能的影响，对比了BN颗粒与BN晶须对样品的气孔率、显微结构、力学性能以及介电性能的影响。随着BN含量的提高，多孔BN/Si_3N_4陶瓷的气孔率呈现上升的趋势，而抗弯强度与介电常数则随之下降。由于BN晶须相对于BN颗粒具有长径比高的结构特征，借助其低介电常数与高长径比的特点，加入BN晶须的多孔BN/Si_3N_4复合陶瓷具有更加优良的介电性能和力学性能。
研究了多孔复合陶瓷透波机理。随着气孔率的增加，多孔复合陶瓷的介电常数减小，介电常数实际测试值与Lichtencker方程(ε)推倒公式计算值有较好吻合。物相的组成是影响复合陶瓷介电性能的重要因素，随着BN相含量的增加，复合陶瓷的介电常数减小；多孔复合陶瓷的晶界相、气孔结构以及杂质也是影响介电常数及介电损耗的主要因素，晶界相含量的减少会使介电损耗急剧下降，具有较大气孔尺寸的样品的介电损耗较小。
Aerospace wave-transparent materials have many function characteristicssuch as wave-transparency, heat insulation, carrying capacity, and erosionresistance, which allow them to protect the spacecrafts from the influence ofharsh environments. With the rapid development of aircrafts and the increase offlight speed, materials are required to possess a number of critical properties suchas good mechanical and dielectric properties, excellent thermal resistance andrain erosion resistance, have a light weight, and so on. Silicon nitride is one ofthe most promising ceramic materials for the applications of wave-transparentmaterials, due to its high mechanical strength, good thermal shock resistance andexcellent erosion resistance. However when silicon nitride is used as high-machmissile radome, the dielectric properties are poor relatively. Boron nitride hasbetter thermal stability, a lower dielectric constant than silicon nitride, and it hasmore stability of dielectric properties at high temperatures. The downside is thatthe mechanical properties and rain-erosion resistance of BN are poor. In order toimprove the dielectric properties of Si_3N_4ceramics, BN can be introduced intothe Si_3N_4matrix to fabricate BN/Si_3N_4wave-transparent composites withexcellent properties.
Porous composite ceramics have low dielectric constant and low density.They can not only satisfy the need to transmit signals with high speed, but alsoare able to overcome the brittleness of ceramic by designing and testingmulti-system materials. In this work porous BN/Si_3N_4composite ceramics with highporosity, high strength and excellent dielectric properties have been synthesized bygel-casting process.
Parameters in the preparation process were thoroughly investigated andoptimized; the TBA-based gel-casting process has been improved to become a maturepreparation technique in preparing porous BN/Si_3N_4composite ceramics. The resultsshowed that the slurry with1.44g/l dispersant added had the best stability. Thecatalyst (MBAM) and initiator (APS) aqueous solution of the best content was1.5wt% and30wt%(to monomer), respectively. The green body was moisturizing dried at40°C in N2environment.
Secondly, porous BN/Si_3N_4composite ceramics was fabricated by dry-pressingmethod, pore-forming agent method and TBA-based gel-casting process. It was foundthat the advantages of TBA-based gel-casting in fabricating porous BN/Si_3N_4composite ceramics could be ascribed to its feasibility in obtaining a homogeneousand controllable structure. And also, through TBA-based gel-casting we could gethigh porosity. When the porosity was36.5%, the flexural strength was136±5.35MPaand when the porosity was77.4%, the dielectric constant was1.74.
At a fixed solid loading of15vol%of initial slurry, the effect of the content ofsintering additives Y2O3-Al2O3and SiO2and sintering temperature on the propertieswas analyzed. The results showed that the porosity increased with the higher amountsof sintering additives. A uniform pore size distribution was observed, and the medianpore size was micron or submicron. The flexural strength and dielectric constant ofporous BN/Si_3N_4ceramics increased when the content of sintering additives increased.When the content of Y2O3-Al2O3was5wt%, the content of SiO2was7.5wt%, andthe flexural strength was65.84±3.08MPa. At room temperature, porous BN/Si_3N_4composite ceramics had excellent and stable dielectric properties at7~18GHzfrequency. The dielectric constant was2.39, and the dielectric loss stayed between1.5~3.5×10~(-3). The porous BN/Si_3N_4composite ceramics had excellent dielectricproperties at high temperatures.
Furthermore, the effect of BN contents on the microstructure and properties ofporous BN/Si_3N_4composite ceramics was analyzed. The porosity, microstructure,mechanical properties, and dielectric properties of BN particles and BN whiskerswere compared in porous BN/Si_3N_4composite ceramics. When the content of BNincreased the porosity of BN/Si_3N_4composite ceramics increased while the dielectricconstant and flexural strength decreased. The porous Si_3N_4composite ceramics withBN whiskers had better dielectric and mechanical properties.
Lastly, the wave-transparent mechanism was investigated. The dielectricconstant of porous BN/Si_3N_4composite ceramics was decreased while theporosity increased. The relationship between the dielectric constant and porositywas consistent with Lichtencker's logarithmic equation (ε). Phase composition was another important factor on dielectric properties. The increase of BN with alow dielectric constant could decrease the dielectric constant of the composites.The dielectric constant of BN/Si_3N_4composites could be calculated by themultiphase Lichtencker's logarithmic equation (ε). Furthermore, we discussed theinfluence of the grain boundary phase, the pore structure and impurity ondielectric properties especially dielectric loss. The content of the grain boundaryphase decrease was beneficial for the dielectric loss. The samples with biggerpore size had small dielectric loss.
由于多孔陶瓷具有较低的介电常数和密度，因此在制备BN/Si_3N_4复合材料时，应尽可能提高材料的气孔率。本文通过采用叔丁醇（TBA）基凝胶注模成型工艺制备高气孔率、高强度、低介电常数和介电损耗的BN/Si_3N_4复合陶瓷。优化了TBA基凝胶注模成型工艺各阶段的工艺参数，使该工艺适用于制备高气孔率的BN/Si_3N_4复合陶瓷。通过研究，加入0.144g/l（相对于溶剂体积）分散剂的浆料的流变性能较好；催化剂（MBAM）和引发剂（APS）水溶液最佳含量分别为1.5wt%和30wt%（相对于单体），40℃下N2保护聚合及保湿干燥制度较为合理。
为了验证TBA基凝胶注模工艺在制备多孔BN/Si_3N_4复合陶瓷上的优越性，本文选取目前多孔陶瓷制备方法中应用最为广泛的干压成型工艺及造孔剂工艺与之进行对比实验，从微观结构到宏观性能进行了比较分析。研究发现，TBA基凝胶注模工艺的优势在于其能够制备出均匀可控，且具有高气孔率的结构。并可以通过调节固相含量得到不能性能的多孔BN/Si_3N_4复合陶瓷。当固相含量为7.5vol%时，气孔率为77.4%，介电常数为1.74；固相含量为30vol%时，气孔率为36.5%，抗弯强度为136±5.35MPa。
在浆料中初始固相含量固定为15%体积分数的基础上，分别研究了烧结助剂Y2O3-Al2O3和SiO2的含量以及烧结温度的影响。结果表明，多孔BN/Si_3N_4复合陶瓷的气孔率随着烧结助剂含量的提高而下降，孔径呈单峰分布，尺寸为微米级或亚微米级。抗弯强度随着烧结助剂含量的提高而增大，介电常数随之上升。当Y2O3-Al2O3含量为5wt%，SiO_2含量为7.5wt%时，多孔BN/Si_3N_4复合陶瓷的抗弯强度为65.84±3.08MPa，室温下的介电常数非常稳定，在2.39附近波动，介电损耗在3×10~(-3)以下，并具有优异的高温介电性能。通过对烧结温度的研究，结果发现，在1750℃烧结温度下，Si_3N_4发育良好，具有优异的综合性能。
研究了添加剂BN的加入量对多孔BN/Si_3N_4复合陶瓷的结构和性能的影响，对比了BN颗粒与BN晶须对样品的气孔率、显微结构、力学性能以及介电性能的影响。随着BN含量的提高，多孔BN/Si_3N_4陶瓷的气孔率呈现上升的趋势，而抗弯强度与介电常数则随之下降。由于BN晶须相对于BN颗粒具有长径比高的结构特征，借助其低介电常数与高长径比的特点，加入BN晶须的多孔BN/Si_3N_4复合陶瓷具有更加优良的介电性能和力学性能。
研究了多孔复合陶瓷透波机理。随着气孔率的增加，多孔复合陶瓷的介电常数减小，介电常数实际测试值与Lichtencker方程(ε)推倒公式计算值有较好吻合。物相的组成是影响复合陶瓷介电性能的重要因素，随着BN相含量的增加，复合陶瓷的介电常数减小；多孔复合陶瓷的晶界相、气孔结构以及杂质也是影响介电常数及介电损耗的主要因素，晶界相含量的减少会使介电损耗急剧下降，具有较大气孔尺寸的样品的介电损耗较小。
Aerospace wave-transparent materials have many function characteristicssuch as wave-transparency, heat insulation, carrying capacity, and erosionresistance, which allow them to protect the spacecrafts from the influence ofharsh environments. With the rapid development of aircrafts and the increase offlight speed, materials are required to possess a number of critical properties suchas good mechanical and dielectric properties, excellent thermal resistance andrain erosion resistance, have a light weight, and so on. Silicon nitride is one ofthe most promising ceramic materials for the applications of wave-transparentmaterials, due to its high mechanical strength, good thermal shock resistance andexcellent erosion resistance. However when silicon nitride is used as high-machmissile radome, the dielectric properties are poor relatively. Boron nitride hasbetter thermal stability, a lower dielectric constant than silicon nitride, and it hasmore stability of dielectric properties at high temperatures. The downside is thatthe mechanical properties and rain-erosion resistance of BN are poor. In order toimprove the dielectric properties of Si_3N_4ceramics, BN can be introduced intothe Si_3N_4matrix to fabricate BN/Si_3N_4wave-transparent composites withexcellent properties.
Porous composite ceramics have low dielectric constant and low density.They can not only satisfy the need to transmit signals with high speed, but alsoare able to overcome the brittleness of ceramic by designing and testingmulti-system materials. In this work porous BN/Si_3N_4composite ceramics with highporosity, high strength and excellent dielectric properties have been synthesized bygel-casting process.
Parameters in the preparation process were thoroughly investigated andoptimized; the TBA-based gel-casting process has been improved to become a maturepreparation technique in preparing porous BN/Si_3N_4composite ceramics. The resultsshowed that the slurry with1.44g/l dispersant added had the best stability. Thecatalyst (MBAM) and initiator (APS) aqueous solution of the best content was1.5wt% and30wt%(to monomer), respectively. The green body was moisturizing dried at40°C in N2environment.
Secondly, porous BN/Si_3N_4composite ceramics was fabricated by dry-pressingmethod, pore-forming agent method and TBA-based gel-casting process. It was foundthat the advantages of TBA-based gel-casting in fabricating porous BN/Si_3N_4composite ceramics could be ascribed to its feasibility in obtaining a homogeneousand controllable structure. And also, through TBA-based gel-casting we could gethigh porosity. When the porosity was36.5%, the flexural strength was136±5.35MPaand when the porosity was77.4%, the dielectric constant was1.74.
At a fixed solid loading of15vol%of initial slurry, the effect of the content ofsintering additives Y2O3-Al2O3and SiO2and sintering temperature on the propertieswas analyzed. The results showed that the porosity increased with the higher amountsof sintering additives. A uniform pore size distribution was observed, and the medianpore size was micron or submicron. The flexural strength and dielectric constant ofporous BN/Si_3N_4ceramics increased when the content of sintering additives increased.When the content of Y2O3-Al2O3was5wt%, the content of SiO2was7.5wt%, andthe flexural strength was65.84±3.08MPa. At room temperature, porous BN/Si_3N_4composite ceramics had excellent and stable dielectric properties at7~18GHzfrequency. The dielectric constant was2.39, and the dielectric loss stayed between1.5~3.5×10~(-3). The porous BN/Si_3N_4composite ceramics had excellent dielectricproperties at high temperatures.
Furthermore, the effect of BN contents on the microstructure and properties ofporous BN/Si_3N_4composite ceramics was analyzed. The porosity, microstructure,mechanical properties, and dielectric properties of BN particles and BN whiskerswere compared in porous BN/Si_3N_4composite ceramics. When the content of BNincreased the porosity of BN/Si_3N_4composite ceramics increased while the dielectricconstant and flexural strength decreased. The porous Si_3N_4composite ceramics withBN whiskers had better dielectric and mechanical properties.
Lastly, the wave-transparent mechanism was investigated. The dielectricconstant of porous BN/Si_3N_4composite ceramics was decreased while theporosity increased. The relationship between the dielectric constant and porositywas consistent with Lichtencker's logarithmic equation (ε). Phase composition was another important factor on dielectric properties. The increase of BN with alow dielectric constant could decrease the dielectric constant of the composites.The dielectric constant of BN/Si_3N_4composites could be calculated by themultiphase Lichtencker's logarithmic equation (ε). Furthermore, we discussed theinfluence of the grain boundary phase, the pore structure and impurity ondielectric properties especially dielectric loss. The content of the grain boundaryphase decrease was beneficial for the dielectric loss. The samples with biggerpore size had small dielectric loss.
引文
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