碳纳米管增强铝基复合材料的制备及组织性能研究
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摘要
本文以多壁碳纳米管为增强体,利用粉末冶金方法制备了体积分数为0~4.2%的碳纳米管增强2024铝基复合材料。对制备过程中所涉及的碳纳米管的纯化、碳纳米管与合金粉末的均匀混合、碳纳米管在铝基体中的热稳定性、复合材料的致密化进行了系统地研究与分析,运用扫描电镜、透射电镜、X射线衍射、X射线光电子能谱和高分辩电镜以及万能电子拉伸机、热分析仪、维氏硬度等分析测试手段,评价了复合材料的制备工艺,观察分析复合材料的显微组织结构,测试了复合材料的室温力学性能,并对微观组织结构影响材料宏观力学性能的机制进行了初步探讨。
对碳纳米管不同时间下硝酸回流的研究表明,随着回流时间的增加,碳纳米管的长径比减少;碳纳米管中sp2与sp3杂化态碳的原子比下降,表面缺陷减少,且表面引入的含氧官能团的含量增加。硝酸回流后的碳纳米管的分散效果要比未回流的好,且回流时间越长,分散效果越好。当碳纳米管的含量小于2.1vol.%时,通过超声加机械搅拌能将碳纳米管均匀的分散在合金粉末的表面,而当碳纳米管的含量达到4.2vol.%时,碳纳米管在合金粉末表面形成团聚。结合合金粉末和碳纳米管的表面结构,分析了碳纳米管的纯化与分散以及碳纳米管与合金粉末均匀混合的机理。
对碳纳米管在合金粉末中热稳定性进行研究,结果表明当温度超过合金粉末的熔点时,碳纳米管在铝中是不稳定的,部分碳纳米管容易与铝发生反应生成具有针状的纳米Al4C3相;碳纳米管与铝反应的活化能为194.01 kJ/mol,比石墨与铝的高;反应生成的Al4C3相与铝基体之间界面为直接结合,界面结合紧密,且Al4C3相和铝基体发现有(200) Al //(00012)Al C的位向关系。利用高HRTEM和XPS分析,讨论碳纳米管与铝反应的机理。
挤压后的复合材料中铝晶粒的尺寸显著小于基体材料中铝晶粒的,碳纳米管能够有效地抑制铝晶粒的粗化,细化铝晶粒尺寸。此外,碳纳米管在复合材料中是稳定的,主要分布在复合材料中铝晶粒的内部和晶界处,部分碳纳米管周围存在位错缠结现象。碳纳米管和铝基体之间的界面为直接原子结合,界面光滑、平直,不存在中间相,两者为完全共格界面。碳纳米管与铝基体之间发现有的位向关系。
碳纳米管的含量显著影响复合材料的力学性能,随着碳纳米管含量的增加,复合材料的硬度、抗拉强度、弹性模量和屈服强度先升高然后下降,当碳纳米管的含量为2.1vol.%时,复合材料的硬度、抗拉强度、弹性模量和屈服强度达到最大值,分别为136.2kg/mm2、521.7MPa、92.2GPa和497.7MPa。与相同条件下制备的2024Al基体材料相比,分别提高了33.0%、34.6%、20.8%和39.7%。当碳纳米管含量较少时,复合材料的断裂主要是碳纳米管的拔出或拔断,且拔出长度很短,同时伴有碳纳米管的桥联发生,随着碳纳米管含量的增加,拔出或拔断的数量也增加。而当碳纳米含量较多时,复合材料的断裂主要以碳纳米管的脱粘和拔出为主,拔出长度很长。结合复合材料的微观组织结构和力学性能,讨论碳纳米管增强铝基复合材料的强化基理。(200) Al //(101?1)CNTs
2024Al matrix composites reinforced with 0~4.2vol.% carbon nanotubes (CNTs) were fabricated by powder metallurgy technique. The purification of CNTs, uniformly dispersion of CNTs among alloy powders, the thermal stability of CNTs and Al and the densification of the composites were systemically investigated and analyzed. By using SEM, TEM, XRD, XPS, HRTEM, DSC, tensile test and hardness test techniques, the microstructure, the mechanical properties and the processing parameters of the composites were examined and optimized. In addition, the effects of the microstructure on the overall mechanical properties were related.
The investigation of the effect of refluence time on CNTs in nitric acid showed that the aspect ratio, the ratio of hybridizable C atom of sp2 and sp3 and surfacial defects of CNTs reduce, meanwhile, the functional groups containing oxygen element increase when refluence time increases. The dispersion of CNTs after refluence is better than that of CNTs before refluence, and dispersing ability increases with refluence time increasing. CNTs can homogenously distributed on the surface of alloy powders when the content of CNTs is less than 2.1vol.% with mechanical stirring assisting ultrasonic shaker. However, CNTs form conglobations when content is 4.2vol.%. The mechanisms of the purification and dispersion of CNTs, the dispersion of CNTs among alloy powders were discussed based on surfacial structure of CNTs and alloy powders.
The study of thermal stability of CNTs in Al matrix indicated that CNTs and Al react and form nano-Al4C3 phases with needle shape when the temperature is above the melting of alloy aluminum. The activation energy of the reacton between CNTs and Al is 194.01 kJ/mol, which is higher than that of graphite and Al. Moreover, the interface of Al4C3 phases and Al matrix keep directly atom bonding, and bond tightly. It also were found that an orientation relationship of (200) Al //(00012)Al C exists between Al4C3 phases and Al matrix. The reaction mechanisms of CNTs and Al matrix were taken over by HRTEM and XPs analysis.
The grain size of composites is finer than that of the matrix materials after hot extrusion, so CNTs can restrain the growth of Al grains in compoises, and fine the Al grains. Moreover, CNTs were very stabile in the present fabrication method, and mainly distributes on the grains boundary and inner-grains of the composite matrix. The interfaces of CNTs and Al matrix are very clean and straight. CNTs and Al matrix keep directly atom bonding, and exist (200) Al //(101? 1)CNTs orientation relationship.
CNTs content affected significantly the mechanical properties of the composites. The hardness, tensile strength, Young’s modulus and yield strength of the composites firstly increase and then reduce with CNTs content increasing. The hardness, tensile strength, Young’s modulus and yield strength reache the maximum value, 136.2 kg/mm2、521.7 MPa、92.2 GPa and 497.7 MPa respectively, when CNTs content is 2.1vol.%. They are increased 33.0%、34.6%、20.8% and 39.7% in relation to the matrix during the same fabrication. The fracture manners involves the bridging, the pull-out and pulling to rupture, and the length of CNTs pulled out is very short, when small amount of CNTs were added to Al matrix, however, the pull out and debonding took placed in the composite with larger amount of CNTs, and the length of CNTs pulled out is very longer in relation to that of 2.1vol.% CNT composite. The strengthening mechanisms of CNTs reinforced metal matrix composites were discussed according to the microstructure and mechanical properties of the composites
对碳纳米管不同时间下硝酸回流的研究表明,随着回流时间的增加,碳纳米管的长径比减少;碳纳米管中sp2与sp3杂化态碳的原子比下降,表面缺陷减少,且表面引入的含氧官能团的含量增加。硝酸回流后的碳纳米管的分散效果要比未回流的好,且回流时间越长,分散效果越好。当碳纳米管的含量小于2.1vol.%时,通过超声加机械搅拌能将碳纳米管均匀的分散在合金粉末的表面,而当碳纳米管的含量达到4.2vol.%时,碳纳米管在合金粉末表面形成团聚。结合合金粉末和碳纳米管的表面结构,分析了碳纳米管的纯化与分散以及碳纳米管与合金粉末均匀混合的机理。
对碳纳米管在合金粉末中热稳定性进行研究,结果表明当温度超过合金粉末的熔点时,碳纳米管在铝中是不稳定的,部分碳纳米管容易与铝发生反应生成具有针状的纳米Al4C3相;碳纳米管与铝反应的活化能为194.01 kJ/mol,比石墨与铝的高;反应生成的Al4C3相与铝基体之间界面为直接结合,界面结合紧密,且Al4C3相和铝基体发现有(200) Al //(00012)Al C的位向关系。利用高HRTEM和XPS分析,讨论碳纳米管与铝反应的机理。
挤压后的复合材料中铝晶粒的尺寸显著小于基体材料中铝晶粒的,碳纳米管能够有效地抑制铝晶粒的粗化,细化铝晶粒尺寸。此外,碳纳米管在复合材料中是稳定的,主要分布在复合材料中铝晶粒的内部和晶界处,部分碳纳米管周围存在位错缠结现象。碳纳米管和铝基体之间的界面为直接原子结合,界面光滑、平直,不存在中间相,两者为完全共格界面。碳纳米管与铝基体之间发现有的位向关系。
碳纳米管的含量显著影响复合材料的力学性能,随着碳纳米管含量的增加,复合材料的硬度、抗拉强度、弹性模量和屈服强度先升高然后下降,当碳纳米管的含量为2.1vol.%时,复合材料的硬度、抗拉强度、弹性模量和屈服强度达到最大值,分别为136.2kg/mm2、521.7MPa、92.2GPa和497.7MPa。与相同条件下制备的2024Al基体材料相比,分别提高了33.0%、34.6%、20.8%和39.7%。当碳纳米管含量较少时,复合材料的断裂主要是碳纳米管的拔出或拔断,且拔出长度很短,同时伴有碳纳米管的桥联发生,随着碳纳米管含量的增加,拔出或拔断的数量也增加。而当碳纳米含量较多时,复合材料的断裂主要以碳纳米管的脱粘和拔出为主,拔出长度很长。结合复合材料的微观组织结构和力学性能,讨论碳纳米管增强铝基复合材料的强化基理。(200) Al //(101?1)CNTs
2024Al matrix composites reinforced with 0~4.2vol.% carbon nanotubes (CNTs) were fabricated by powder metallurgy technique. The purification of CNTs, uniformly dispersion of CNTs among alloy powders, the thermal stability of CNTs and Al and the densification of the composites were systemically investigated and analyzed. By using SEM, TEM, XRD, XPS, HRTEM, DSC, tensile test and hardness test techniques, the microstructure, the mechanical properties and the processing parameters of the composites were examined and optimized. In addition, the effects of the microstructure on the overall mechanical properties were related.
The investigation of the effect of refluence time on CNTs in nitric acid showed that the aspect ratio, the ratio of hybridizable C atom of sp2 and sp3 and surfacial defects of CNTs reduce, meanwhile, the functional groups containing oxygen element increase when refluence time increases. The dispersion of CNTs after refluence is better than that of CNTs before refluence, and dispersing ability increases with refluence time increasing. CNTs can homogenously distributed on the surface of alloy powders when the content of CNTs is less than 2.1vol.% with mechanical stirring assisting ultrasonic shaker. However, CNTs form conglobations when content is 4.2vol.%. The mechanisms of the purification and dispersion of CNTs, the dispersion of CNTs among alloy powders were discussed based on surfacial structure of CNTs and alloy powders.
The study of thermal stability of CNTs in Al matrix indicated that CNTs and Al react and form nano-Al4C3 phases with needle shape when the temperature is above the melting of alloy aluminum. The activation energy of the reacton between CNTs and Al is 194.01 kJ/mol, which is higher than that of graphite and Al. Moreover, the interface of Al4C3 phases and Al matrix keep directly atom bonding, and bond tightly. It also were found that an orientation relationship of (200) Al //(00012)Al C exists between Al4C3 phases and Al matrix. The reaction mechanisms of CNTs and Al matrix were taken over by HRTEM and XPs analysis.
The grain size of composites is finer than that of the matrix materials after hot extrusion, so CNTs can restrain the growth of Al grains in compoises, and fine the Al grains. Moreover, CNTs were very stabile in the present fabrication method, and mainly distributes on the grains boundary and inner-grains of the composite matrix. The interfaces of CNTs and Al matrix are very clean and straight. CNTs and Al matrix keep directly atom bonding, and exist (200) Al //(101? 1)CNTs orientation relationship.
CNTs content affected significantly the mechanical properties of the composites. The hardness, tensile strength, Young’s modulus and yield strength of the composites firstly increase and then reduce with CNTs content increasing. The hardness, tensile strength, Young’s modulus and yield strength reache the maximum value, 136.2 kg/mm2、521.7 MPa、92.2 GPa and 497.7 MPa respectively, when CNTs content is 2.1vol.%. They are increased 33.0%、34.6%、20.8% and 39.7% in relation to the matrix during the same fabrication. The fracture manners involves the bridging, the pull-out and pulling to rupture, and the length of CNTs pulled out is very short, when small amount of CNTs were added to Al matrix, however, the pull out and debonding took placed in the composite with larger amount of CNTs, and the length of CNTs pulled out is very longer in relation to that of 2.1vol.% CNT composite. The strengthening mechanisms of CNTs reinforced metal matrix composites were discussed according to the microstructure and mechanical properties of the composites
引文
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