硼掺杂碳纳米管的制备及其在镁基复合材料中的应用
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摘要
碳纳米管(CNTs)凭借其超强的力学性能成为复合材料的理想增强体。镁及其合金作为基体的主要特点是密度低、比强度和比刚度高。对于CNTs增强镁基复合材料,CNTs与镁之间的界面的物理和化学特性对其性能起着核心作用。界面结构的优化和稳定决定了CNTs和镁性能能否充分发挥进而获得综合性能优异的复合材料。因此,研究CNTs和镁的界面性质和结合状态,对发展高性能镁基复合材料具有重要意义。
本论文为改善CNTs与镁基体之间的界面结合性,分别采用高温气相法和固态气相法制备了硼掺杂CNTs(BCNTs),然后采用超声和化学的方法对BCNTs和CNTs进行分散,在此基础上本实验通过粉末冶金结合热挤压的方法分别制备了BCNTs/Mg和CNTs/Mg复合材料。
分别通过高温气化B_2O_3和B、固态气相法制备了硼掺杂CNTs,探讨了硼掺杂对CNTs形貌与结构的影响,并研究了CNTs的酸化处理对其硼原子掺杂比例的影响。采用XPS测试了硼原子的掺杂比例,采用TEM和Raman分析了BCNTs的形貌和结构。结果表明:采用高温气化B_2O_3或B的方法和固态气相法能有效实现对CNTs进行硼掺杂,但CNTs的酸化处理会降低硼原子的掺杂比例。
采用3-磺丙基十六烷基二甲基铵分别对BCNTs和CNTs进行分散,然后通过粉末冶金结合热挤压法分别制备了BCNTs/Mg和CNTs/Mg复合材料,研究了BCNTs和CNTs含量以及硼掺杂对复合材料的显微组织、硬度、拉伸和压缩性能、摩擦磨损性能的影响,探讨了BCNTs和CNTs与镁基体的界面结合性。结果表明:表面活性剂能提高BCNTs和CNTs在基体中的分散性;随着CNTs含量的增大,CNTs/Mg显微硬度增大,抗拉强度、抗压强度呈峰值,延伸率则呈下降趋势,当CNTs含量为1.0wt.%时,复合材料的抗拉强度达最大值243.4MPa,抗压强度为434.8MPa。硼掺杂能改善CNTs与Mg基体的界面结合,有效提高材料的强度。当BCNTs含量为1.0wt.%时,BCNTs/Mg的抗拉强度和抗压强度分别为258.3MPa和473.2MPa,较CNTs/Mg分别提高了6.1%和8.8%,当BCNTs添加量达到1.5wt.%时,拉伸强度提高达18.7%。断口形貌观察表明CNTs在断口处呈拔出状态,而BCNTs被基体包覆,断口处呈拔断状态,说明硼掺杂改善了复合材料的界面结合性。
Carbon nanotubes (CNTs) have been considered to be a perfect reinforcement for composites due to its superior mechanical properties. Magnesium and its alloys are used as martix due to their low density, high specific strength and stiffness. The physico-chemical characteristic of the interface between CNTs and Mg matrix play a critical role in developing the CNTs reinforced Mg matrix composites with high performance. Therefore,interfacial reactions, the effects of interfaces on properties and the effective ways to control interfacial reactions are significant to Mg matrix composites with high performance.
In this paper, in order to improve the interfacial bonding between CNTs and Mg matrix, boron-doped CNTs (BCNTs) were firstly prepared by calcining the mixture of B_2O_3 or B and CNTs, solid-state gas-phase boronisation. Then the CNTs and BCNTs were dispersed in Mg powder by ultrasonic and chemical method. Finally, the composites were prepared by powder metallurgy combined with hot extrusion technique.
BCNTs were prepared by calcining the mixture of B_2O_3 or B and CNTs, solid-state gas-phase boronisation respectively. The impact of acidification on B-doped ratio of the CNTs was also investigated. XPS was used to validate B-doped ratio, TEM and Raman were used to analyze morphology and structure of BCNTs. The results showed that BCNTs can be successfully prepared by above methods. However, B-doped ratio was reduced by acidification of the CNTs.
3-(N, N-Dimethylpalmitylammonio) propanesulfonate was used to enhance the dispersion of CNTs and BCNTs, the distribution of CNTs and BCNTs were observed by SEM, and the result indicated a better dispersion of CNTs and BCNTs in Mg powder. After obtaining composite powders, CNTs and BCNTs reinforced Mg composites were prepared by powder metallurgy combined with hot extrusion. The effects of reinforcement content and B-doping on microstructure, hardness, tensile properties, compressive properties, friction and wear properties were investigated. In addition, the interface between BCNTs and Mg were observed. The results showed that with the increase of CNTs and BCNTs content, the microhardness of the composites was increased, tensile strength and compressive strength increased firstly and then decreased, elongation decreased. The microhardness was up to 66HV when the content of CNTs in the CNTs/Mg composites is 1.5wt.%. Tensile strength and compressive strength were up to 243.4MPa and 434.8MPa when using 1.0wt.% CNTs in the composites. B-doping can improve interface between CNTs and Mg and increase strength of composites effectively. Tensile and compressive strength were 258.3MPa (+6.1%) and 473.2MPa (+8.8%) respectively for the 1.0wt.% BCNTs/Mg composites. Compressive strength of the 1.5wt.%BCNTs/Mg composites is 18.7% higher than that of the 1.5wt.%CNTs/Mg composites. The fracture observation showed that CNTs were pulled out, but BCNTs were pulled off in the fractured surface, indicating that B-doping can enhance the interfacial bonding between Mg and CNTs.
本论文为改善CNTs与镁基体之间的界面结合性,分别采用高温气相法和固态气相法制备了硼掺杂CNTs(BCNTs),然后采用超声和化学的方法对BCNTs和CNTs进行分散,在此基础上本实验通过粉末冶金结合热挤压的方法分别制备了BCNTs/Mg和CNTs/Mg复合材料。
分别通过高温气化B_2O_3和B、固态气相法制备了硼掺杂CNTs,探讨了硼掺杂对CNTs形貌与结构的影响,并研究了CNTs的酸化处理对其硼原子掺杂比例的影响。采用XPS测试了硼原子的掺杂比例,采用TEM和Raman分析了BCNTs的形貌和结构。结果表明:采用高温气化B_2O_3或B的方法和固态气相法能有效实现对CNTs进行硼掺杂,但CNTs的酸化处理会降低硼原子的掺杂比例。
采用3-磺丙基十六烷基二甲基铵分别对BCNTs和CNTs进行分散,然后通过粉末冶金结合热挤压法分别制备了BCNTs/Mg和CNTs/Mg复合材料,研究了BCNTs和CNTs含量以及硼掺杂对复合材料的显微组织、硬度、拉伸和压缩性能、摩擦磨损性能的影响,探讨了BCNTs和CNTs与镁基体的界面结合性。结果表明:表面活性剂能提高BCNTs和CNTs在基体中的分散性;随着CNTs含量的增大,CNTs/Mg显微硬度增大,抗拉强度、抗压强度呈峰值,延伸率则呈下降趋势,当CNTs含量为1.0wt.%时,复合材料的抗拉强度达最大值243.4MPa,抗压强度为434.8MPa。硼掺杂能改善CNTs与Mg基体的界面结合,有效提高材料的强度。当BCNTs含量为1.0wt.%时,BCNTs/Mg的抗拉强度和抗压强度分别为258.3MPa和473.2MPa,较CNTs/Mg分别提高了6.1%和8.8%,当BCNTs添加量达到1.5wt.%时,拉伸强度提高达18.7%。断口形貌观察表明CNTs在断口处呈拔出状态,而BCNTs被基体包覆,断口处呈拔断状态,说明硼掺杂改善了复合材料的界面结合性。
Carbon nanotubes (CNTs) have been considered to be a perfect reinforcement for composites due to its superior mechanical properties. Magnesium and its alloys are used as martix due to their low density, high specific strength and stiffness. The physico-chemical characteristic of the interface between CNTs and Mg matrix play a critical role in developing the CNTs reinforced Mg matrix composites with high performance. Therefore,interfacial reactions, the effects of interfaces on properties and the effective ways to control interfacial reactions are significant to Mg matrix composites with high performance.
In this paper, in order to improve the interfacial bonding between CNTs and Mg matrix, boron-doped CNTs (BCNTs) were firstly prepared by calcining the mixture of B_2O_3 or B and CNTs, solid-state gas-phase boronisation. Then the CNTs and BCNTs were dispersed in Mg powder by ultrasonic and chemical method. Finally, the composites were prepared by powder metallurgy combined with hot extrusion technique.
BCNTs were prepared by calcining the mixture of B_2O_3 or B and CNTs, solid-state gas-phase boronisation respectively. The impact of acidification on B-doped ratio of the CNTs was also investigated. XPS was used to validate B-doped ratio, TEM and Raman were used to analyze morphology and structure of BCNTs. The results showed that BCNTs can be successfully prepared by above methods. However, B-doped ratio was reduced by acidification of the CNTs.
3-(N, N-Dimethylpalmitylammonio) propanesulfonate was used to enhance the dispersion of CNTs and BCNTs, the distribution of CNTs and BCNTs were observed by SEM, and the result indicated a better dispersion of CNTs and BCNTs in Mg powder. After obtaining composite powders, CNTs and BCNTs reinforced Mg composites were prepared by powder metallurgy combined with hot extrusion. The effects of reinforcement content and B-doping on microstructure, hardness, tensile properties, compressive properties, friction and wear properties were investigated. In addition, the interface between BCNTs and Mg were observed. The results showed that with the increase of CNTs and BCNTs content, the microhardness of the composites was increased, tensile strength and compressive strength increased firstly and then decreased, elongation decreased. The microhardness was up to 66HV when the content of CNTs in the CNTs/Mg composites is 1.5wt.%. Tensile strength and compressive strength were up to 243.4MPa and 434.8MPa when using 1.0wt.% CNTs in the composites. B-doping can improve interface between CNTs and Mg and increase strength of composites effectively. Tensile and compressive strength were 258.3MPa (+6.1%) and 473.2MPa (+8.8%) respectively for the 1.0wt.% BCNTs/Mg composites. Compressive strength of the 1.5wt.%BCNTs/Mg composites is 18.7% higher than that of the 1.5wt.%CNTs/Mg composites. The fracture observation showed that CNTs were pulled out, but BCNTs were pulled off in the fractured surface, indicating that B-doping can enhance the interfacial bonding between Mg and CNTs.
引文
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