硅氮氧陶瓷纤维增强氮化硼陶瓷基透波复合材料的制备与性能研究
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摘要
本文瞄准高超音速飞行器对天线罩(天线窗)提出的长时、耐温、透波、承载的工作要求,尤其是长时间耐高温的特别要求,在综述国内外透波材料研究进展的基础上,分析现有耐高温透波材料的优缺点,以硅氮氧纤维和环硼氮烷分别作为增强体和陶瓷先驱体,采用先驱体浸渍-裂解(PIP)工艺制备了(单向)硅氮氧纤维增强氮化硼(SiNO_f/BN)陶瓷基透波复合材料,对其力、电、热性能进行了测试和评价。
研究了裂解速率、裂解温度等因素对氮化硼陶瓷先驱体环硼氮烷的陶瓷产率以及裂解产物性质的影响。结果表明,陶瓷产率随裂解速率升高而降低;裂解温度越高,其产物密度和结晶度越高,稳定性越好,在升温速率10℃/min、1000℃裂解温度条件下,环硼氮烷聚合物的陶瓷产率约为88.95wt%。
研究和分析了热处理工艺对硅氮氧纤维力学性能的影响规律,采用SEM、TEM、XRD表征了纤维热处理前后外观形貌、内部结构的变化。结果表明,纤维力学性能对热处理温度和次数比较敏感。在空气气氛中,纤维强度随温度升高而降低,在1100℃处理后强度只有原纤维的40%左右;随着热处理次数的增加,纤维的强度有所损失,在第一次处理后,下降幅度约20%,但在第二次处理以后,下降幅度约5%的水平。热处理升温速率、保温时间对纤维力学性能影响不大。
采用PIP工艺制备了SiNO_f/BN复合材料,并对影响其力学性能的关键工艺因素进行研究和分析。先驱体环硼氮烷对硅氮氧纤维浸润性较好,单向纤维预制件内部孔隙较大,使得SiNO_f/BN复合材料致密化效率高,经过2次PIP循环以后,即可达到较高密度,此后增长幅度趋于平缓。随着循环次数增加,SiNO_f/BN复合材料孔隙率逐渐降低,密度逐渐提高,弯曲强度和弯曲模量随之提高。在800℃~1000℃裂解温度范围内,SiNO_f/BN复合材料的弯曲强度和弯曲模量与裂解温度正相关,分别由800℃的128.9MPa和23.5GPa上升到1000℃的148.2MPa和26.2GPa;但在不同裂解温度下,SiNO_f/BN复合材料的致密化行为保持一致。延长裂解保温时间,SiNO_f/BN复合材料密度提高,相应地其弯曲强度和弯曲模量均有所提高,但提高幅度不大,裂解保温时间不是影响SiNO_f/BN复合材料力学性能的关键因素。在1600℃热处理后,SiNO_f/BN复合材料中的硅氮氧纤维因结晶和部分分解,失去增强功能,导致复合材料的力学性能严重下降。
考察了SiNO_f/BN复合材料的介电性能和热物理性能。在800℃~1000℃裂解温度范围内,其相对介电常数与裂解温度正相关,由3.45上升到3.83;而其介电损耗角正切则与裂解温度负相关,由7.0x10~(-3)下降到4.6x10~(-3)。不同裂解温度制备的SiNO_f/BN复合材料介电性能相差不大。在室温100℃和室温~200℃范围内,其比热分别为0.91kJ/kg·℃和0.97kJ/kg·℃,导热系数分别为1.2W/m·K和1.3W/m·K。在室温~800℃范围内,热膨胀系数为2.20~2.75x10~(-6)/K,其平均变化在10%范围以内。
将SiNO_f/BN和SiO_(2f)/BN复合材料各项性能进行了对比研究,二者在介电性能和热稳定性方面相差不大,但是在耐高温性能方面,前者相对后者能够保持更强的高温力学性能。
As the key component of hypersonic aircraft, the radome must possess multifunction such as long life, thermal protection, electromagnetic tranparence and load bearing, especially the former two requirements. In this dissertation, aiming at requirements of radome, based on the review of wave-transparent materials, the disadvantages of existing material systems were analyzed, the SiNO fiber reinforced boron nitride ceramic matrix (SiNO_f/BN) wave-transparent composites were prepared by precursor infiltration and pyrolysis (PIP) process with Borazine as the precursor. The mechanical, dielectric and thermophysical properties of the composites were measured and evaluated. The following research was designed and conceived.
The discipline of the pyrolytic product characteristics with heating ratio and pyrolysising temperature was investigated. The ceramic yield was decreased when the heating ratio elevated. With the increasing of pyrolysis temperature, the density, crystallinity and stability of pyrolytic product inceased. In N2 atmosphere, with 10℃/min, at 1000℃, the ceramic yield was about 88.95wt%.
The effects of the calefactive velocity, treating time, temperature and times on the mechanical properties of SiNO fiber were studied via XRD, SEM, TEM to examine its surface performances and structures. It showed that the strength of SiNO fiber was sensitive to the treating temperature and times. The strength decreased while the heating temperature increased. After heated at 1100℃in air, the residual strength ratio of the fiber is only 40%. With the increase of treating time, the strength of SiNO fiber also decreased with more than 20% after the first time and smoothly at 5% level after the following times. But the calefactive velocity and treating time had low influence to the strength of SiNO fiber.
SiNO_f/BN composites were prepared from Borazine by PIP process and the key factors that effect the mechanical properties of it were investigated and analyzed. Because the precursor Borazine had good wet-ability to SiNO fibers and the preformed unit of unidirectional fibers had comparatively holes, the density of the composites increased fast with the PIP cycle doing. With the increase of PIP cycles, the porosity of the composites decreased, the density increased, hence the mechanical properties enhanced. With the increase of pyrolysis temperature from 800℃to 1000℃, the flexural strength and elastic modulus of the composites increased from 128.9MPa and 23.5GPa to 148.2MPa and 26.2GPa respectively. But at different pyrolysis temperature, the densification behavior was consistent. The mechanical properties of the composites varied little with different pyrolysis time. After heat treated at 1600℃, the SiNO fibers in the composites were crystallized and partial decomposed led to lost the enhancing function, hence the mechanical properties of the composites decreased seriously.
The dielectric and thermo physical properties of SiNO_f/BN composites were tested and studied. When the pyrolysis temperature increased from 800℃to 1000℃, the dielectric constant increased from 3.45 to 3.83, while the loss tangent decreased from 7.0x10~(-3) to 4.6x10~(-3). Composites pyrolyzed at different temperature all had good dielectric properties that could meet the operating requirements. The specific heat capacity and thermal conductivity (from R.T. to 100℃and R.T. to 200℃) was 0.91kJ/kg·℃~0.97kJ/kg·℃and 1.2W/m·K~1.3W/m·K respectively. From R.T. to 800℃, the average CTE was 2.20~2.75x10~(-6)/K and varied less than 10%.
Various performances of SiNO_f/BN were studied contrast to that of SiO_(2f)/BN. They were differed tiny in dielectric and thermo physical properties. But the former could maintain most of the mechanical properties at high temperature better than that of the latter.
研究了裂解速率、裂解温度等因素对氮化硼陶瓷先驱体环硼氮烷的陶瓷产率以及裂解产物性质的影响。结果表明,陶瓷产率随裂解速率升高而降低;裂解温度越高,其产物密度和结晶度越高,稳定性越好,在升温速率10℃/min、1000℃裂解温度条件下,环硼氮烷聚合物的陶瓷产率约为88.95wt%。
研究和分析了热处理工艺对硅氮氧纤维力学性能的影响规律,采用SEM、TEM、XRD表征了纤维热处理前后外观形貌、内部结构的变化。结果表明,纤维力学性能对热处理温度和次数比较敏感。在空气气氛中,纤维强度随温度升高而降低,在1100℃处理后强度只有原纤维的40%左右;随着热处理次数的增加,纤维的强度有所损失,在第一次处理后,下降幅度约20%,但在第二次处理以后,下降幅度约5%的水平。热处理升温速率、保温时间对纤维力学性能影响不大。
采用PIP工艺制备了SiNO_f/BN复合材料,并对影响其力学性能的关键工艺因素进行研究和分析。先驱体环硼氮烷对硅氮氧纤维浸润性较好,单向纤维预制件内部孔隙较大,使得SiNO_f/BN复合材料致密化效率高,经过2次PIP循环以后,即可达到较高密度,此后增长幅度趋于平缓。随着循环次数增加,SiNO_f/BN复合材料孔隙率逐渐降低,密度逐渐提高,弯曲强度和弯曲模量随之提高。在800℃~1000℃裂解温度范围内,SiNO_f/BN复合材料的弯曲强度和弯曲模量与裂解温度正相关,分别由800℃的128.9MPa和23.5GPa上升到1000℃的148.2MPa和26.2GPa;但在不同裂解温度下,SiNO_f/BN复合材料的致密化行为保持一致。延长裂解保温时间,SiNO_f/BN复合材料密度提高,相应地其弯曲强度和弯曲模量均有所提高,但提高幅度不大,裂解保温时间不是影响SiNO_f/BN复合材料力学性能的关键因素。在1600℃热处理后,SiNO_f/BN复合材料中的硅氮氧纤维因结晶和部分分解,失去增强功能,导致复合材料的力学性能严重下降。
考察了SiNO_f/BN复合材料的介电性能和热物理性能。在800℃~1000℃裂解温度范围内,其相对介电常数与裂解温度正相关,由3.45上升到3.83;而其介电损耗角正切则与裂解温度负相关,由7.0x10~(-3)下降到4.6x10~(-3)。不同裂解温度制备的SiNO_f/BN复合材料介电性能相差不大。在室温100℃和室温~200℃范围内,其比热分别为0.91kJ/kg·℃和0.97kJ/kg·℃,导热系数分别为1.2W/m·K和1.3W/m·K。在室温~800℃范围内,热膨胀系数为2.20~2.75x10~(-6)/K,其平均变化在10%范围以内。
将SiNO_f/BN和SiO_(2f)/BN复合材料各项性能进行了对比研究,二者在介电性能和热稳定性方面相差不大,但是在耐高温性能方面,前者相对后者能够保持更强的高温力学性能。
As the key component of hypersonic aircraft, the radome must possess multifunction such as long life, thermal protection, electromagnetic tranparence and load bearing, especially the former two requirements. In this dissertation, aiming at requirements of radome, based on the review of wave-transparent materials, the disadvantages of existing material systems were analyzed, the SiNO fiber reinforced boron nitride ceramic matrix (SiNO_f/BN) wave-transparent composites were prepared by precursor infiltration and pyrolysis (PIP) process with Borazine as the precursor. The mechanical, dielectric and thermophysical properties of the composites were measured and evaluated. The following research was designed and conceived.
The discipline of the pyrolytic product characteristics with heating ratio and pyrolysising temperature was investigated. The ceramic yield was decreased when the heating ratio elevated. With the increasing of pyrolysis temperature, the density, crystallinity and stability of pyrolytic product inceased. In N2 atmosphere, with 10℃/min, at 1000℃, the ceramic yield was about 88.95wt%.
The effects of the calefactive velocity, treating time, temperature and times on the mechanical properties of SiNO fiber were studied via XRD, SEM, TEM to examine its surface performances and structures. It showed that the strength of SiNO fiber was sensitive to the treating temperature and times. The strength decreased while the heating temperature increased. After heated at 1100℃in air, the residual strength ratio of the fiber is only 40%. With the increase of treating time, the strength of SiNO fiber also decreased with more than 20% after the first time and smoothly at 5% level after the following times. But the calefactive velocity and treating time had low influence to the strength of SiNO fiber.
SiNO_f/BN composites were prepared from Borazine by PIP process and the key factors that effect the mechanical properties of it were investigated and analyzed. Because the precursor Borazine had good wet-ability to SiNO fibers and the preformed unit of unidirectional fibers had comparatively holes, the density of the composites increased fast with the PIP cycle doing. With the increase of PIP cycles, the porosity of the composites decreased, the density increased, hence the mechanical properties enhanced. With the increase of pyrolysis temperature from 800℃to 1000℃, the flexural strength and elastic modulus of the composites increased from 128.9MPa and 23.5GPa to 148.2MPa and 26.2GPa respectively. But at different pyrolysis temperature, the densification behavior was consistent. The mechanical properties of the composites varied little with different pyrolysis time. After heat treated at 1600℃, the SiNO fibers in the composites were crystallized and partial decomposed led to lost the enhancing function, hence the mechanical properties of the composites decreased seriously.
The dielectric and thermo physical properties of SiNO_f/BN composites were tested and studied. When the pyrolysis temperature increased from 800℃to 1000℃, the dielectric constant increased from 3.45 to 3.83, while the loss tangent decreased from 7.0x10~(-3) to 4.6x10~(-3). Composites pyrolyzed at different temperature all had good dielectric properties that could meet the operating requirements. The specific heat capacity and thermal conductivity (from R.T. to 100℃and R.T. to 200℃) was 0.91kJ/kg·℃~0.97kJ/kg·℃and 1.2W/m·K~1.3W/m·K respectively. From R.T. to 800℃, the average CTE was 2.20~2.75x10~(-6)/K and varied less than 10%.
Various performances of SiNO_f/BN were studied contrast to that of SiO_(2f)/BN. They were differed tiny in dielectric and thermo physical properties. But the former could maintain most of the mechanical properties at high temperature better than that of the latter.
引文
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