高频微波衰减陶瓷的制备与频谱特性研究
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摘要
微波衰减材料广‘泛应用于微波电真空器件、消极电子对抗和微波测量系统中。AlN具有适中的介电常数、高的热导率、好的化学和热稳定性以及高的电阻率；导电颗粒Mo、W具有与AlN匹配的热膨胀系数和较高的热导率,可以作为良好的微波衰减剂,因此,AlN/导电颗粒复合陶瓷以其优异的综合性能和对环境的友好性成为替代传统微波衰减材料的最佳选择。然而在AlN/Mo复合微波衰减陶瓷体系中,一方面,复合陶瓷的渗流阂值对原材料和加工工艺极其敏感；另一方面,AlN/Mo复合陶瓷的电阻率特别敏感于Mo的添加量变化,因而形成的电阻突变范围很窄,很难有效地控制电阻率以获得较好的介电性能。因此,这些不利因素成为亟待解决的问题。
本文研究的目的就是在探究改变原材料及制备工艺对AlN/Mo复合陶瓷的渗流阈值的影响及由此带来的介电性能的影响的同时,在此基础上通过添加半导体颗粒SiC形成AlN/Mo/SiC复合体系,尝试做到有效而精确控制复合体系电阻率,使其电阻率发生突变的范围得以展宽,最终使复合陶瓷具有高热导率和良好的微波衰减性能。
在AlN/Mo复合陶瓷的烧结过程中,混料方式和烧结温度等对AlN/Mo复合陶瓷在无压烧结方式下的烧结致密化起着关键性的作用。另外,导电颗粒Mo的加入有利于AlN/Mo复合陶瓷的致密烧结。在烧结温度为1750℃下,不同Mo含量的样品的致密度均超过了98%,当Mo含量达到32%以上,试样的致密度接近理论致密度。
对于改变原料粒径和工艺制备的AlN/Mo复合微波衰减陶瓷,其渗流阈值为37.45%左右,相比于在之前工作中得到23%有了明显的提高。在此基础上测得,AlN/Mo复合陶瓷在渗流闽值附近的介电常数已经变大。但热导率随着Mo的添加量的增加出现下降。
SiC的添加对AlN/Mo/SiC的烧结致密度会产生显著的影响,因而选择合适的烧结方式和工艺,调整SiC的添加含量到一个合适的范围,是制备高致密度的AlN/Mo/SiC复合陶瓷的关键。
相对于AlN/Mo体系而言,SiC添加后的体系在一定范围内没有再出现电阻率的非线性突变现象,而是随着SiC添加量的增加,电阻率在一定范围内缓慢下降,说明SiC的添加有效地阻断了Mo颗粒形成的渗流通道,从而达到了展宽体系渗流阂值的目的。
SiC含量对AlN/Mo/SiC复合陶瓷的介电性能和热导率均有显著影响。其介电常数和损耗随着SiC添加量的增加而增大。复合陶瓷的热导率则呈下降趋势,这和致密度、各相的相对含量,各相的热导率及分布状态有着密切的关系。
Microwave attenuation materials are widely used in vacuum microwave electronic devices, negative electronic countermeasure and microwave measuring system. AlN exhibits good thermal properties, electrical insulation and good chemical properties. Mo and W are suitable as attenuation substance in AlN composite ceramics for their appropriate thermal expansion coefficient and high thermal conductivity. It is such excellent properties and its healthy attribute that makes this kind of material could be taken as the alternative microwave attenuation materials. However, in this system, for one thing, the percolation threshold is very sensitive to the raw materials and preparation process so that it results in the change of dielectric properties of AIN/Mo composite ceramics. For another thing, the electrical resistivity of composite ceramics is too sensitive to the change of Mo content, so it is so difficult to control the electrical resistivity to obtain good dielectric properties. Therefore, the problems mentioned above need prompt solutions.
In this work, the purpose of the study is to investigate the influence of the raw materials and preparation process on the percolation threshold of AIN/Mo composite ceramics and on this basis, study the process that how it change the dielectric properties. Furthermore, by adding proper amount of SiC, AIN/Mo/SiC composite ceramics were produced with high relative density. The purpose of adding SiC was to widen the range of the percolation threshold so that the composite ceramics could have proper dielectric properties that we expected, and at last, achieve the objective that obtain the material with excellent microwave attenuation properties.
During the process of sintering, the method of mixing and the sintering temperature both have influence on the relative density of AIN/Mo composite ceramics produced by pressureless sintering process. In addition, adding Mo particles is helpful to the process of sintering. When the sintering temperature reaches 1750℃, the relative density of AIN/Mo composite ceramics with different Mo content exceed 98%. Especially, when the volume fraction of Mo content reaches 32% and above, the relative density of this kind of ceramics approaches its theoretical value.
For AIN/Mo composite ceramics which is produced by changing the radius of the raw materials and preparation process, its percolation threshold has reached 37.45%. Comparing with value of 23% obtained in some formal works, it has increased greatly. On this basis, the measurement of dielectric constant shows that the dielectric constant of AlN/Mo composite ceramics has increased at the point closed to the percolation threshold. However, the thermal conductivity of AIN/Mo composite ceramics decreases because of the increase of Mo content.
The addition of SiC has great influence on the relative density of AIN/Mo/SiC composite ceramics. Therefore, both choosing proper method of sintering and preparation process and adjusting the SiC content are key points to prepare AIN/Mo/SiC composite ceramics with high relative density.
Comparing to AIN/Mo composite ceramics, when adding some SiC particles, the electric resistivity of AIN/Mo/SiC composite ceramics decreases gently instead of showing no-linear abrupt change. This result states that the addition of SiC has break down the channel which was made by the joint of Mo particles and achieving the goal of widening the range of the percolation threshold.
SiC content has great influence on the dielectric properties and the thermal conductivity of AIN/Mo/SiC composite ceramics. The dielectric constant and dielectric loss increase with the increase of SiC content. Its thermal conductivity decreases with the increase of SiC content, which is closely related to these factors:the relative density, the relative content of each phase, the thermal conductivity of each phase and the distribution model of each phase.
本文研究的目的就是在探究改变原材料及制备工艺对AlN/Mo复合陶瓷的渗流阈值的影响及由此带来的介电性能的影响的同时,在此基础上通过添加半导体颗粒SiC形成AlN/Mo/SiC复合体系,尝试做到有效而精确控制复合体系电阻率,使其电阻率发生突变的范围得以展宽,最终使复合陶瓷具有高热导率和良好的微波衰减性能。
在AlN/Mo复合陶瓷的烧结过程中,混料方式和烧结温度等对AlN/Mo复合陶瓷在无压烧结方式下的烧结致密化起着关键性的作用。另外,导电颗粒Mo的加入有利于AlN/Mo复合陶瓷的致密烧结。在烧结温度为1750℃下,不同Mo含量的样品的致密度均超过了98%,当Mo含量达到32%以上,试样的致密度接近理论致密度。
对于改变原料粒径和工艺制备的AlN/Mo复合微波衰减陶瓷,其渗流阈值为37.45%左右,相比于在之前工作中得到23%有了明显的提高。在此基础上测得,AlN/Mo复合陶瓷在渗流闽值附近的介电常数已经变大。但热导率随着Mo的添加量的增加出现下降。
SiC的添加对AlN/Mo/SiC的烧结致密度会产生显著的影响,因而选择合适的烧结方式和工艺,调整SiC的添加含量到一个合适的范围,是制备高致密度的AlN/Mo/SiC复合陶瓷的关键。
相对于AlN/Mo体系而言,SiC添加后的体系在一定范围内没有再出现电阻率的非线性突变现象,而是随着SiC添加量的增加,电阻率在一定范围内缓慢下降,说明SiC的添加有效地阻断了Mo颗粒形成的渗流通道,从而达到了展宽体系渗流阂值的目的。
SiC含量对AlN/Mo/SiC复合陶瓷的介电性能和热导率均有显著影响。其介电常数和损耗随着SiC添加量的增加而增大。复合陶瓷的热导率则呈下降趋势,这和致密度、各相的相对含量,各相的热导率及分布状态有着密切的关系。
Microwave attenuation materials are widely used in vacuum microwave electronic devices, negative electronic countermeasure and microwave measuring system. AlN exhibits good thermal properties, electrical insulation and good chemical properties. Mo and W are suitable as attenuation substance in AlN composite ceramics for their appropriate thermal expansion coefficient and high thermal conductivity. It is such excellent properties and its healthy attribute that makes this kind of material could be taken as the alternative microwave attenuation materials. However, in this system, for one thing, the percolation threshold is very sensitive to the raw materials and preparation process so that it results in the change of dielectric properties of AIN/Mo composite ceramics. For another thing, the electrical resistivity of composite ceramics is too sensitive to the change of Mo content, so it is so difficult to control the electrical resistivity to obtain good dielectric properties. Therefore, the problems mentioned above need prompt solutions.
In this work, the purpose of the study is to investigate the influence of the raw materials and preparation process on the percolation threshold of AIN/Mo composite ceramics and on this basis, study the process that how it change the dielectric properties. Furthermore, by adding proper amount of SiC, AIN/Mo/SiC composite ceramics were produced with high relative density. The purpose of adding SiC was to widen the range of the percolation threshold so that the composite ceramics could have proper dielectric properties that we expected, and at last, achieve the objective that obtain the material with excellent microwave attenuation properties.
During the process of sintering, the method of mixing and the sintering temperature both have influence on the relative density of AIN/Mo composite ceramics produced by pressureless sintering process. In addition, adding Mo particles is helpful to the process of sintering. When the sintering temperature reaches 1750℃, the relative density of AIN/Mo composite ceramics with different Mo content exceed 98%. Especially, when the volume fraction of Mo content reaches 32% and above, the relative density of this kind of ceramics approaches its theoretical value.
For AIN/Mo composite ceramics which is produced by changing the radius of the raw materials and preparation process, its percolation threshold has reached 37.45%. Comparing with value of 23% obtained in some formal works, it has increased greatly. On this basis, the measurement of dielectric constant shows that the dielectric constant of AlN/Mo composite ceramics has increased at the point closed to the percolation threshold. However, the thermal conductivity of AIN/Mo composite ceramics decreases because of the increase of Mo content.
The addition of SiC has great influence on the relative density of AIN/Mo/SiC composite ceramics. Therefore, both choosing proper method of sintering and preparation process and adjusting the SiC content are key points to prepare AIN/Mo/SiC composite ceramics with high relative density.
Comparing to AIN/Mo composite ceramics, when adding some SiC particles, the electric resistivity of AIN/Mo/SiC composite ceramics decreases gently instead of showing no-linear abrupt change. This result states that the addition of SiC has break down the channel which was made by the joint of Mo particles and achieving the goal of widening the range of the percolation threshold.
SiC content has great influence on the dielectric properties and the thermal conductivity of AIN/Mo/SiC composite ceramics. The dielectric constant and dielectric loss increase with the increase of SiC content. Its thermal conductivity decreases with the increase of SiC content, which is closely related to these factors:the relative density, the relative content of each phase, the thermal conductivity of each phase and the distribution model of each phase.
引文
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