AlN和BN/AlN复相陶瓷的放电等离子烧结及其组织与性能研究
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摘要
本文采用放电等离子烧结(SPS)方法制备了AlN陶瓷及BN/AlN复相陶瓷。系统研究了烧结助剂及烧结工艺对AlN陶瓷及BN/AlN复相陶瓷的显微组织结构、热学及介电性能的影响规律,探讨了AlN陶瓷及BN/AlN复相陶瓷的SPS致密化机制,揭示了复合烧结助剂的作用机理。利用后续热处理工艺,对AlN陶瓷及BN/AlN复相陶瓷的显微组织进行调整,改善其热学及介电性能,探讨了热处理工艺的可行性。
研究发现,采用SPS方法制备AlN陶瓷时,烧结助剂添加量在2~3wt.%左右,在短时间内可以实现液相烧结机制。只加入单一稀土氧化物烧结助剂,AlN陶瓷的晶格参数c轴尺寸数值与热导率变化不一致,烧结助剂对AlN陶瓷晶格纯化效果不明显。晶间相的分布和数量对AlN陶瓷的热学和介电性能有重要影响。以Sm_2O_3为烧结助剂的AlN陶瓷的显微组织均匀,热导率较高。添加不同稀土氧化物的AlN陶瓷热导率与介电性能差别不明显。
以稀土氧化物和CaF_2为复合烧结助剂不仅可以通过与Al_2O_3反应驱除AlN晶格内部的氧杂质,还可以通过生成可挥发相降低晶间相含量,有效地改善AlN陶瓷的热导率与介电性能。添加复合烧结助剂制备的AlN陶瓷的c轴尺寸变化趋势与热导率变化趋势基本相同,AlN晶格纯化效果显著。当稀土氧化物和CaF_2的比例为2:1时,AlN陶瓷的显微组织结构均匀,晶间相分布合理,AlN晶粒发育完善,具有较好的热学与介电性能,有效地实现了复合烧结助剂的双重作用。HREM分析表明,在SPS快速烧结过程中,复合烧结助剂形成的液相在降温过程中在AlN晶粒之间形成少量非晶物质,对材料的性能有一定的影响。
引入合适的烧结助剂,采用SPS技术可成功制备致密的BN/AlN复相陶瓷。复合烧结助剂在制备BN/AlN复相陶瓷过程中同样可起到双重效果,对促进材料的致密化和改善材料性能起到了重要的作用。h-BN没有出现定向排列倾向,片状的BN分布在AlN晶粒周围,阻碍了AlN晶粒的生长,对复相陶瓷的性能有影响。随复合烧结助剂添加量的增加,复相陶瓷中AlN晶粒尺寸增加,热导率先上升后下降,介电常数与致密度变化趋势相同,而介电损耗则呈现先下降后上升趋势。BN加入量越多,其交叉堆积现象明显,复相陶瓷显微组织均匀性与致密度均有所下降,介电常数降低而介电损耗增加。
AlN陶瓷经过热处理后,随着主晶粒的进一步的发育长大,使晶间相的分布向更有利于热导率的方向发展,同时某些晶间相挥发,使晶间相含量降低,材料的组成更加纯净。加入复合烧结助剂的AlN陶瓷,尤其是加入CaF_2多的试样,纯化AlN晶格效果更明显,热导率显著提高。热处理之后的AlN陶瓷介电常数和介电损耗均有所下降。HREM分析表明,即使经过热处理,AlN晶粒之间少量的非晶物质也不能完全排除。
BN/AlN复相陶瓷经过热处理后,AlN、BN主晶相晶粒尺寸均有所增加,晶间相含量降低,热导率提高。可挥发性晶间相的挥发,使复相陶瓷的致密度下降,介电常数下降。热处理使材料内部缺陷减少,杂质元素含量降低,复相陶瓷的介电损耗有所改善。
AlN ceramics and BN/AlN composites were prepared by Spark Plasma Sintering (SPS) method. The effects of sintering additives and sintering technology on microstructure and thermal and dielectric properties of AlN ceramics and BN/AlN composites were systematically investigated. The densification mechanism during SPS process and the mechanism of multiple component sintering additives were revealed. Mcirostructures were controlled and thermal and dielectric properties of AlN ceramics and BN/AlN composites were improved by heat treatment, and the feasibility of heat treatment technology was investigated.
The experimental results shows that only 2~3wt.% sintering additive is enough to realize the liquid phase sintering mechanism in the short SPS term. When introducing single sintering additive, the change of the c-axis size is different from that of thermal conductivity of AlN ceramics, and the purifying effect of the sintering additive isn’t obvious. The distribution and content of the secondary phases play important roles on the thermal and dielectric properties of AlN ceramics. The AlN ceramics with uniform microstructures with Sm_2O_3 as sintering additive have higher thermal concuctivity than that of other samples. There is no obvious difference about the thermal conductivity and dielectric property between AlN ceramics with different sintering additives.
The multiple component sintering additive not only removes oxygen impurity by reacting with Al_2O_3 but also reduces the content of grain boundaries by forming the evaporable secondary phases, thermal conductivity and dielectric property of AlN ceramics are greatly improved. The change of the c-axis size is basically same as that of thermal conductivity of AlN ceramics with multiple component sintering additives, and the purifying effect of the sintering additive is obvious. The sintering additive composition of 2:1(Y_2O_3(Sm_2O_3):CaF_2) is beneficial to improve thermal and dielectric properties of AlN ceramics, which has uniform microstructure, suitable distribution of secondary phase and perfect AlN grain. That is to say, the sintering additive composition of 2:1 is favourable to realize the double effect of multiple component sintering additive. The HREM results show that a little amphous phase existes between AlN grains formes during the liquid cooling process, which has impact on the property on the AlN ceramics.
Dense BN/AlN composites can be successfully fabricated by SPS method with suitable sintering additives. The multiple component sintering additive can also play double effects during preparing BN/AlN composites, and plays important role on promoting densification process and improving property. H-BN don’t have the tendency of directional arrangement, and the flaky BN grain locates at the around of AlN grains, which inhabites the growth of AlN grain and has impact on the property of materials. The AlN grain size increases and thermal conductivity firstly increases and then reduces with increasing multiple component sintering additive content. The change tendency of dielectric constant is same as that of relative density, but the dielectric loss firstly deduces and then increases. The BN cross stacking tendency is obvious, the uniformity of microstructures decreases, the relative density and dielectric constant reduces and dielectric loss increases with increasing BN content.
The heat treatment is introduced to lower the content and to modify the distribution of grain boundary, which is beneficial to purify the lattice and accelerate the AlN growth. The AlN ceramics with multiple component sintering additives, especially the speciman introducing more CaF_2, the effect of purify AlN lattice is obvious and thermal conductivity is greatly improved. After the heat treatment, both the dielectric constant and dielectric loss deduces. The HREM result showes that the amphous phase cann’t be removed through the heat treatment.
Both the size of AlN and BN in the BN/AlN composites increases after heat treatment. In addition, the content of secondary phase deduces and thermal conductivity improves. Because of the evaporating secondary phase, both the relative density and dielectric constant deduces. The dielectric loss is improved because of the decreasing defect and impurity element.
研究发现,采用SPS方法制备AlN陶瓷时,烧结助剂添加量在2~3wt.%左右,在短时间内可以实现液相烧结机制。只加入单一稀土氧化物烧结助剂,AlN陶瓷的晶格参数c轴尺寸数值与热导率变化不一致,烧结助剂对AlN陶瓷晶格纯化效果不明显。晶间相的分布和数量对AlN陶瓷的热学和介电性能有重要影响。以Sm_2O_3为烧结助剂的AlN陶瓷的显微组织均匀,热导率较高。添加不同稀土氧化物的AlN陶瓷热导率与介电性能差别不明显。
以稀土氧化物和CaF_2为复合烧结助剂不仅可以通过与Al_2O_3反应驱除AlN晶格内部的氧杂质,还可以通过生成可挥发相降低晶间相含量,有效地改善AlN陶瓷的热导率与介电性能。添加复合烧结助剂制备的AlN陶瓷的c轴尺寸变化趋势与热导率变化趋势基本相同,AlN晶格纯化效果显著。当稀土氧化物和CaF_2的比例为2:1时,AlN陶瓷的显微组织结构均匀,晶间相分布合理,AlN晶粒发育完善,具有较好的热学与介电性能,有效地实现了复合烧结助剂的双重作用。HREM分析表明,在SPS快速烧结过程中,复合烧结助剂形成的液相在降温过程中在AlN晶粒之间形成少量非晶物质,对材料的性能有一定的影响。
引入合适的烧结助剂,采用SPS技术可成功制备致密的BN/AlN复相陶瓷。复合烧结助剂在制备BN/AlN复相陶瓷过程中同样可起到双重效果,对促进材料的致密化和改善材料性能起到了重要的作用。h-BN没有出现定向排列倾向,片状的BN分布在AlN晶粒周围,阻碍了AlN晶粒的生长,对复相陶瓷的性能有影响。随复合烧结助剂添加量的增加,复相陶瓷中AlN晶粒尺寸增加,热导率先上升后下降,介电常数与致密度变化趋势相同,而介电损耗则呈现先下降后上升趋势。BN加入量越多,其交叉堆积现象明显,复相陶瓷显微组织均匀性与致密度均有所下降,介电常数降低而介电损耗增加。
AlN陶瓷经过热处理后,随着主晶粒的进一步的发育长大,使晶间相的分布向更有利于热导率的方向发展,同时某些晶间相挥发,使晶间相含量降低,材料的组成更加纯净。加入复合烧结助剂的AlN陶瓷,尤其是加入CaF_2多的试样,纯化AlN晶格效果更明显,热导率显著提高。热处理之后的AlN陶瓷介电常数和介电损耗均有所下降。HREM分析表明,即使经过热处理,AlN晶粒之间少量的非晶物质也不能完全排除。
BN/AlN复相陶瓷经过热处理后,AlN、BN主晶相晶粒尺寸均有所增加,晶间相含量降低,热导率提高。可挥发性晶间相的挥发,使复相陶瓷的致密度下降,介电常数下降。热处理使材料内部缺陷减少,杂质元素含量降低,复相陶瓷的介电损耗有所改善。
AlN ceramics and BN/AlN composites were prepared by Spark Plasma Sintering (SPS) method. The effects of sintering additives and sintering technology on microstructure and thermal and dielectric properties of AlN ceramics and BN/AlN composites were systematically investigated. The densification mechanism during SPS process and the mechanism of multiple component sintering additives were revealed. Mcirostructures were controlled and thermal and dielectric properties of AlN ceramics and BN/AlN composites were improved by heat treatment, and the feasibility of heat treatment technology was investigated.
The experimental results shows that only 2~3wt.% sintering additive is enough to realize the liquid phase sintering mechanism in the short SPS term. When introducing single sintering additive, the change of the c-axis size is different from that of thermal conductivity of AlN ceramics, and the purifying effect of the sintering additive isn’t obvious. The distribution and content of the secondary phases play important roles on the thermal and dielectric properties of AlN ceramics. The AlN ceramics with uniform microstructures with Sm_2O_3 as sintering additive have higher thermal concuctivity than that of other samples. There is no obvious difference about the thermal conductivity and dielectric property between AlN ceramics with different sintering additives.
The multiple component sintering additive not only removes oxygen impurity by reacting with Al_2O_3 but also reduces the content of grain boundaries by forming the evaporable secondary phases, thermal conductivity and dielectric property of AlN ceramics are greatly improved. The change of the c-axis size is basically same as that of thermal conductivity of AlN ceramics with multiple component sintering additives, and the purifying effect of the sintering additive is obvious. The sintering additive composition of 2:1(Y_2O_3(Sm_2O_3):CaF_2) is beneficial to improve thermal and dielectric properties of AlN ceramics, which has uniform microstructure, suitable distribution of secondary phase and perfect AlN grain. That is to say, the sintering additive composition of 2:1 is favourable to realize the double effect of multiple component sintering additive. The HREM results show that a little amphous phase existes between AlN grains formes during the liquid cooling process, which has impact on the property on the AlN ceramics.
Dense BN/AlN composites can be successfully fabricated by SPS method with suitable sintering additives. The multiple component sintering additive can also play double effects during preparing BN/AlN composites, and plays important role on promoting densification process and improving property. H-BN don’t have the tendency of directional arrangement, and the flaky BN grain locates at the around of AlN grains, which inhabites the growth of AlN grain and has impact on the property of materials. The AlN grain size increases and thermal conductivity firstly increases and then reduces with increasing multiple component sintering additive content. The change tendency of dielectric constant is same as that of relative density, but the dielectric loss firstly deduces and then increases. The BN cross stacking tendency is obvious, the uniformity of microstructures decreases, the relative density and dielectric constant reduces and dielectric loss increases with increasing BN content.
The heat treatment is introduced to lower the content and to modify the distribution of grain boundary, which is beneficial to purify the lattice and accelerate the AlN growth. The AlN ceramics with multiple component sintering additives, especially the speciman introducing more CaF_2, the effect of purify AlN lattice is obvious and thermal conductivity is greatly improved. After the heat treatment, both the dielectric constant and dielectric loss deduces. The HREM result showes that the amphous phase cann’t be removed through the heat treatment.
Both the size of AlN and BN in the BN/AlN composites increases after heat treatment. In addition, the content of secondary phase deduces and thermal conductivity improves. Because of the evaporating secondary phase, both the relative density and dielectric constant deduces. The dielectric loss is improved because of the decreasing defect and impurity element.
引文
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