化学共沉积法制备纳米金刚石/铜基复合材料的研究
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摘要
纳米金刚石(ND)不仅具有金刚石高硬度、高导热、高耐磨等性能,同时兼有纳米粒子的特性,因此受到广泛的关注。纳米金刚石作为增强相制备的金属基复合材料在很多需要高强度、高导电的工业领域具有广泛的应用前景。但是传统制备工艺很难克服纳米颗粒极易团聚和与金属基体浸润性不良的问题。本课题首次采用化学共沉积-粉末冶金法,并通过纳米金刚石表面改性,探索了制备纳米金刚石弥散强化铜基(ND/Cu)复合材料的新方法。
通过化学共沉积工艺制备了ND/Cu复合粉体,并采用粉末冶金工艺制备了ND/Cu复合材料。研究了不同制备工艺参数(包括:煅烧温度、还原温度、初压压力、烧结温度、烧结时间、复压压力)对复合粉末、复合材料微观组织与性能的影响,确定了最佳的制备工艺参数。
采用石墨化、酸处理、化学镀等方法对纳米金刚石进行表面改性。改性后的纳米金刚石的分散性均有不同程度的提高。其中经表面石墨化和HF酸两步处理的纳米金刚石表现出良好的分散性,显著降低ND的团聚。经两步处理后的纳米金刚石所制备的复合材料,晶粒细小,纳米金刚石均匀分布于铜基体中,界面结合良好,起到了弥散强化的作用。因此,具有较高的硬度和电导率。
采用高分辨透射电镜(HRTEM)分析了ND/Cu复合材料的微观组织和界面特征。结果表明:纳米金刚石颗粒弥散分布于铜晶粒中,界面结合紧密,并存在位错、孪晶等亚结构。研究了不同ND含量对复合材料性能的影响,发现随着ND含量的增加,复合材料的密度、电导率随之下降,硬度逐渐升高,抗拉强度在含量为3wt.%时为最高值。随着ND含量的增加,ND/Cu复合材料的抗软化温度升高,当ND含量大于3wt.%时,抗软化温度大于600℃。3wt.%ND/Cu复合材料具有很好的综合性能。探讨了化学共沉积法制备的ND/Cu复合材料的强化机制主要为细晶强化和弥散强化。
Due to the properties of high hardness, high thermal conductivity, high wearing resistant, and the characters of nanoparticle, nanodiamond (ND) has attracted wide research attentions. ND reinforced metal matrix composites have a promising application in the fields which need the materials with high strength, high electric conductivity, and good high temperature performance. However, when ND was taken into consideration, a few problems, such as the aggregations of ND particles and the poor wettability between diamond and copper, could not be overcome by traditional preparation methods. In this paper, a novel method called“chemical co-deposition”was introduced to prepare ND/Cu composite powders. ND particles were functionalized by three modification methods for uniform dispersion, and ND/Cu composites were fabricated by powder metallurgy.
ND/Cu composite powders were prepared by chemical co-deposition route, and ND/Cu composites were fabricated by powder metallurgy. The influence of different processing parameters (including: calcination temperature, reduction temperature, pressing, sintering temperature, sintering time and repressing) on the microstructure and performance of composite powders and ND/Cu composite bulks were investigated, and then processing parameters were optimized.
The ND particles were modified by graphitization, acid treatment and electroless plating, respectively. The dispersibility of ND was great improved after modification. The ND particles, treated by graphitization and HF acid, could homogeneously disperse in composite powders and composite bulks. Fine grains and good interfacial combination of the composites were obtained. Thus, the surface treated ND/Cu composites show higher hardness and conductivity properties than untreated ones due to dispersion strengthen effect.
The microstructure and interfacial characterization of ND/Cu composites were analyzed by TEM and HRTEM. The results demonstrated that ND particles homogeneously dispersed in copper matrix, and the interface between copper and ND was clean and tight. The grains of copper matrix were fine, and dislocations and twins in the matrix could be found. The influence of ND content on composites performances was studied. With the increase of ND content, the hardness, tensile strength and resistive softening properties of the composites could be improved, but the density and conductivity were decreased. 3wt.% ND/Cu composite has the best combined performances. The main strengthen mechanism of ND/Cu composites prepared by chemical co-deposition method are fine grain strengthening and dispersion strengthening.
通过化学共沉积工艺制备了ND/Cu复合粉体,并采用粉末冶金工艺制备了ND/Cu复合材料。研究了不同制备工艺参数(包括:煅烧温度、还原温度、初压压力、烧结温度、烧结时间、复压压力)对复合粉末、复合材料微观组织与性能的影响,确定了最佳的制备工艺参数。
采用石墨化、酸处理、化学镀等方法对纳米金刚石进行表面改性。改性后的纳米金刚石的分散性均有不同程度的提高。其中经表面石墨化和HF酸两步处理的纳米金刚石表现出良好的分散性,显著降低ND的团聚。经两步处理后的纳米金刚石所制备的复合材料,晶粒细小,纳米金刚石均匀分布于铜基体中,界面结合良好,起到了弥散强化的作用。因此,具有较高的硬度和电导率。
采用高分辨透射电镜(HRTEM)分析了ND/Cu复合材料的微观组织和界面特征。结果表明:纳米金刚石颗粒弥散分布于铜晶粒中,界面结合紧密,并存在位错、孪晶等亚结构。研究了不同ND含量对复合材料性能的影响,发现随着ND含量的增加,复合材料的密度、电导率随之下降,硬度逐渐升高,抗拉强度在含量为3wt.%时为最高值。随着ND含量的增加,ND/Cu复合材料的抗软化温度升高,当ND含量大于3wt.%时,抗软化温度大于600℃。3wt.%ND/Cu复合材料具有很好的综合性能。探讨了化学共沉积法制备的ND/Cu复合材料的强化机制主要为细晶强化和弥散强化。
Due to the properties of high hardness, high thermal conductivity, high wearing resistant, and the characters of nanoparticle, nanodiamond (ND) has attracted wide research attentions. ND reinforced metal matrix composites have a promising application in the fields which need the materials with high strength, high electric conductivity, and good high temperature performance. However, when ND was taken into consideration, a few problems, such as the aggregations of ND particles and the poor wettability between diamond and copper, could not be overcome by traditional preparation methods. In this paper, a novel method called“chemical co-deposition”was introduced to prepare ND/Cu composite powders. ND particles were functionalized by three modification methods for uniform dispersion, and ND/Cu composites were fabricated by powder metallurgy.
ND/Cu composite powders were prepared by chemical co-deposition route, and ND/Cu composites were fabricated by powder metallurgy. The influence of different processing parameters (including: calcination temperature, reduction temperature, pressing, sintering temperature, sintering time and repressing) on the microstructure and performance of composite powders and ND/Cu composite bulks were investigated, and then processing parameters were optimized.
The ND particles were modified by graphitization, acid treatment and electroless plating, respectively. The dispersibility of ND was great improved after modification. The ND particles, treated by graphitization and HF acid, could homogeneously disperse in composite powders and composite bulks. Fine grains and good interfacial combination of the composites were obtained. Thus, the surface treated ND/Cu composites show higher hardness and conductivity properties than untreated ones due to dispersion strengthen effect.
The microstructure and interfacial characterization of ND/Cu composites were analyzed by TEM and HRTEM. The results demonstrated that ND particles homogeneously dispersed in copper matrix, and the interface between copper and ND was clean and tight. The grains of copper matrix were fine, and dislocations and twins in the matrix could be found. The influence of ND content on composites performances was studied. With the increase of ND content, the hardness, tensile strength and resistive softening properties of the composites could be improved, but the density and conductivity were decreased. 3wt.% ND/Cu composite has the best combined performances. The main strengthen mechanism of ND/Cu composites prepared by chemical co-deposition method are fine grain strengthening and dispersion strengthening.
引文
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