均匀分散的碳纳米管增强铝基复合材料的制备与性能
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摘要
碳纳米管（CNTs）具有优异的力学、物理性能以及低的密度而被认为是金属基复合材料（MMCs）理想的增强相，然而CNTs易于团聚的特性阻碍了高性能CNTs增强MMCs的制备和发展。针对这一问题，本文提出首先采用化学气相沉积法（CVD）原位合成CNTs均匀分散在铝粉表面的CNTs/Al复合粉末，进而将复合粉末机械球磨后粉末冶金成型（原位合成-短时球磨-粉末冶金法）制备复合材料的新思路；对整个制备过程的各个影响参数进行了系统的研究，并对复合材料的组织、性能、界面结合和强化机制进行了探讨。
首先采用浸渍法制备了催化剂前躯体，经直接还原后在铝粉基体上沉积了Ni、Co、Cu三种纳米催化剂颗粒，然后采用CVD法合成了CNTs/Al复合粉末；系统研究了铝基体上CVD法原位合成CNTs的多种影响因素（包括催化剂种类与含量、合成温度、反应气氛和时间）。结果表明：采用Ni、Co、Cu三种催化剂均可以在铝基体上合成多壁CNTs，但Cu催化合成CNTs的石墨晶化程度较低；以0.5wt.%的Ni或Co作为催化剂，在600℃的合成温度下，分别选择CH4或C2H2作为碳源，可以在铝粉表面合成均匀分散的，高纯度、管径均匀、石墨化程度良好的CNTs，所得CNTs/Al粉末适合进一步制备复合材料。
对原位合成的CNTs/Al粉末直接粉末冶金成型（原位合成-粉末冶金法）制备了CNTs/Al复合材料，发现当CNTs含量为1.5wt.%时，复合材料的压缩性能最佳，其压缩屈服强度和弹性模量分别为纯铝的2.2倍和3倍；然而继续提高CNTs含量后，复合材料的压缩性能大幅下降，即采用该方法能够实现CNTs在铝粉基体上的均匀负载量在2.5wt.%以下，CNTs含量在此及以上的复合材料力学性能会恶化。此外，CNTs的加入降低了铝基体的耐蚀性，并且随CNTs含量增多，复合材料的耐蚀性变差。
针对“原位合成-粉末冶金”制备方法存在的问题，进一步采用“原位合成-短时球磨-粉末冶金”工艺制备了CNTs/Al复合材料，即对原位合成的粉末通过短时球磨形成CNTs均匀分散嵌入铝基体内部的复合结构，以此来进一步提高CNTs在铝基体内的最大均匀分散量，着重研究了球磨参数（包括过程控制剂、球磨转速和时间）对CNTs的结构、分散和复合材料性能的影响。结果表明：对于2.5wt.%-CNTs/Al复合材料，在优化后的球磨转速500rpm，不添加过程控制剂的条件下，随球磨时间的增加（≤120min），所制备的复合材料组织更加致密，硬度和抗拉强度均不断提高，确定了90min为最佳的球磨时间，所得复合材料硬度和抗拉强度分别为纯铝的2.4倍和2.7倍，为经过相同球磨时间铝的1.6倍和1.5倍，且延伸率在15%以上，表现出强韧兼备的特点；随着CNTs含量的增加（≤4.5wt.%），复合材料的硬度和抗拉强度不断上升，均在CNTs含量为4.5wt.%时达到最高，此时硬度和抗拉强度为HV131.2和420MPa，分别为纯铝的3.3倍和3.4倍；CNTs的加入可以有效的降低铝基体的热膨胀系数（CTE），随CNTs含量的增多，复合材料的CTE不断下降。
对于采用“原位合成-短时球磨-粉末冶金”制备的CNTs/Al复合材料，研究了球磨过程和烧结温度两个关键因素对CNTs结构演变和CNT-Al界面的影响，并在此基础上探讨了CNTs/Al复合材料的强化机制。结果表明：短时球磨过程对CNTs的结构损伤较小，嵌入铝基体内部的CNTs保持了良好的结构；复合材料的抗拉强度和延伸率均在630℃的烧结温度下达到极大值，而继续提高烧结温度后，复合材料的拉伸性能变差；630℃烧结条件下得到CNTs/Al复合材料中CNT-Al的界面反应存在三种形式，即无明显界面反应、生成CNT@Al4C3结构、完全转变成为Al4C3相，此时少量出现的纳米级Al4C3提高了界面结合强度，利于复合材料性能的提高。复合材料强度的显著提升源于载荷在基体和增强相间的有效传递，CNTs作为载荷的主要承担者起直接强化作用，以及CNTs加入铝基体中引起的位错强化、细晶强化作用，还有以上几种强化机制的协同强化作用。
Due to the low density and excellent mechanical and physical properties, carbonnanotubes (CNTs) have been regarded as the ideal reinforcement for metal matrixcomposites (MMCs). However, the difficulty in achieving uniform dispersion ofCNTs in matrix hampers the development of CNT-reinforced MMCs. To solve thisissue, a novel approach is developed in this dissertation to fabricate CNT/Alcomposites, which consists of in-situ synthesis of CNTs, short-time ball-milling, andpowder metallurgy. The influence of fabrication conditions on the properties ofCNT/Al composites were investigated systematically. Furthermore, the structure,properties, interfacial bonding and strengthening mechanism of CNT-reinforce Alcomposites were discussed.
The Ni, Co, and Cu catalyst precursors on Al powder were prepared byimpregnation route, and then CNTs were synthesized by in-situ chemical vapordeposition. Thus, CNT/Al composite powders were obtained. It was found that themuti-walled CNTs can be synthesized on Al matrix by using Ni, Co, and Cu catalysts.But the CNTs synthesized using Cu catalyst show a relatively low crystallization.Using0.5wt.%Co and Ni catalysts, the homogeneously dispersed CNTs on the Alpowder surface with relatively high purity, uniform diameters, and crystallization canbe obtained at600℃and underCH4and C2H2as carbon sources, respectively. Theobtained CNT/Al composite powders are suited to further preparation of composite.
CNT/Al composites were prepared by direct powder metallurgy of the in-situsynthesized composite powders. It was found that the maximum content of CNTsuniformly dispersed in Al matrix is2.5wt.%, and the mechanical properties of thecomposites decrease rapidly when the content of CNTs is more than2.5wt.%. Theoptimized CNT content is1.5wt.%, at which the composites show best compressiveproperty, and the compressive yield strength and compressive elastic modulus is2.2and3.0times as large as that of pure Al, respectively. Moreover, the corrosionresistance of Al matrix decreases with the increase of CNTs content.
In order to further improve the maximally uniform dispersion content in Alpowder matrix, ball-milling was introduced into the fabrication process of CNT/Alcomposites. The execution of ball milling for a short time can further improve the dispersion of CNTs fabricated by in-situ CVD. Meanwhile, CNTs are implanteddeeply into the matrix. The effects of ball milling parameters on the structure anddispersion of CNTs and the properties of CNT/Al composites were investigated. Itwas found that under the optimized milling conditions (ball-milling speed of500rpm,no process control agent added), with the increasing of milling time (≤120min), thedensity, hardness and tensile strength of2.5wt.%-CNT/Al composites increase. Thecomposites through90min of ball milling show well-balanced strength and ductility,whose hardness and tensile strength are2.4and2.7times as large as that of pure Al,and1.6and1.5times as large as that of the pure Al through the same milling process,respectively. Moreover, the elongation is larger than15%. With the increase of CNTcontent, the hardness and tensile strength of CNT/Al composites increase. The4.5wt.%-CNT/Al composites show largest hardness (HV131.2) and tensile strength (420MPa), which is2.3and2.4times more than that of pure Al, respectively. Furthermore,the coefficient of thermal expansion of CNT/Al composites is reduced significantlycompared with Al matrix, which decreases with the increase of the CNT content.
The effects of ball milling process and sintering temperature on the evolution ofCNT structure and the interface between CNTs and Al were studied. Thestrengthening mechanisms of CNT/Al composites were discussed. The results showedthat the short-time ball milling causes relatively small damage to CNT structure, andthe CNTs implanted into Al matrix possess well structure. The tensile strength andelongation of CNT/Al composite both reach maximum as630℃sinteringtemperature. The tensile properties of composites decrease when the sinteringtemperature is above Al melting point. There are three different forms of interfacialreaction between CNTs and Al matrix in the composites obtained at630℃sinteringtemperature: no distinct interface reaction, forming CNT@Al4C3structure, andcompletely forming Al4C3phase. The nano-sized Al4C3phase with small content canincrease the interface bonding between CNTs and Al, and is beneficial for theimprovement of the composite properties. The remarkable improvement of themechanical properties of CNT/Al composites results from the cooperative action ofseveral reinforcement mechanisms, including effective load transmission, dislocationstrengthening and grain refining strengthening.
首先采用浸渍法制备了催化剂前躯体，经直接还原后在铝粉基体上沉积了Ni、Co、Cu三种纳米催化剂颗粒，然后采用CVD法合成了CNTs/Al复合粉末；系统研究了铝基体上CVD法原位合成CNTs的多种影响因素（包括催化剂种类与含量、合成温度、反应气氛和时间）。结果表明：采用Ni、Co、Cu三种催化剂均可以在铝基体上合成多壁CNTs，但Cu催化合成CNTs的石墨晶化程度较低；以0.5wt.%的Ni或Co作为催化剂，在600℃的合成温度下，分别选择CH4或C2H2作为碳源，可以在铝粉表面合成均匀分散的，高纯度、管径均匀、石墨化程度良好的CNTs，所得CNTs/Al粉末适合进一步制备复合材料。
对原位合成的CNTs/Al粉末直接粉末冶金成型（原位合成-粉末冶金法）制备了CNTs/Al复合材料，发现当CNTs含量为1.5wt.%时，复合材料的压缩性能最佳，其压缩屈服强度和弹性模量分别为纯铝的2.2倍和3倍；然而继续提高CNTs含量后，复合材料的压缩性能大幅下降，即采用该方法能够实现CNTs在铝粉基体上的均匀负载量在2.5wt.%以下，CNTs含量在此及以上的复合材料力学性能会恶化。此外，CNTs的加入降低了铝基体的耐蚀性，并且随CNTs含量增多，复合材料的耐蚀性变差。
针对“原位合成-粉末冶金”制备方法存在的问题，进一步采用“原位合成-短时球磨-粉末冶金”工艺制备了CNTs/Al复合材料，即对原位合成的粉末通过短时球磨形成CNTs均匀分散嵌入铝基体内部的复合结构，以此来进一步提高CNTs在铝基体内的最大均匀分散量，着重研究了球磨参数（包括过程控制剂、球磨转速和时间）对CNTs的结构、分散和复合材料性能的影响。结果表明：对于2.5wt.%-CNTs/Al复合材料，在优化后的球磨转速500rpm，不添加过程控制剂的条件下，随球磨时间的增加（≤120min），所制备的复合材料组织更加致密，硬度和抗拉强度均不断提高，确定了90min为最佳的球磨时间，所得复合材料硬度和抗拉强度分别为纯铝的2.4倍和2.7倍，为经过相同球磨时间铝的1.6倍和1.5倍，且延伸率在15%以上，表现出强韧兼备的特点；随着CNTs含量的增加（≤4.5wt.%），复合材料的硬度和抗拉强度不断上升，均在CNTs含量为4.5wt.%时达到最高，此时硬度和抗拉强度为HV131.2和420MPa，分别为纯铝的3.3倍和3.4倍；CNTs的加入可以有效的降低铝基体的热膨胀系数（CTE），随CNTs含量的增多，复合材料的CTE不断下降。
对于采用“原位合成-短时球磨-粉末冶金”制备的CNTs/Al复合材料，研究了球磨过程和烧结温度两个关键因素对CNTs结构演变和CNT-Al界面的影响，并在此基础上探讨了CNTs/Al复合材料的强化机制。结果表明：短时球磨过程对CNTs的结构损伤较小，嵌入铝基体内部的CNTs保持了良好的结构；复合材料的抗拉强度和延伸率均在630℃的烧结温度下达到极大值，而继续提高烧结温度后，复合材料的拉伸性能变差；630℃烧结条件下得到CNTs/Al复合材料中CNT-Al的界面反应存在三种形式，即无明显界面反应、生成CNT@Al4C3结构、完全转变成为Al4C3相，此时少量出现的纳米级Al4C3提高了界面结合强度，利于复合材料性能的提高。复合材料强度的显著提升源于载荷在基体和增强相间的有效传递，CNTs作为载荷的主要承担者起直接强化作用，以及CNTs加入铝基体中引起的位错强化、细晶强化作用，还有以上几种强化机制的协同强化作用。
Due to the low density and excellent mechanical and physical properties, carbonnanotubes (CNTs) have been regarded as the ideal reinforcement for metal matrixcomposites (MMCs). However, the difficulty in achieving uniform dispersion ofCNTs in matrix hampers the development of CNT-reinforced MMCs. To solve thisissue, a novel approach is developed in this dissertation to fabricate CNT/Alcomposites, which consists of in-situ synthesis of CNTs, short-time ball-milling, andpowder metallurgy. The influence of fabrication conditions on the properties ofCNT/Al composites were investigated systematically. Furthermore, the structure,properties, interfacial bonding and strengthening mechanism of CNT-reinforce Alcomposites were discussed.
The Ni, Co, and Cu catalyst precursors on Al powder were prepared byimpregnation route, and then CNTs were synthesized by in-situ chemical vapordeposition. Thus, CNT/Al composite powders were obtained. It was found that themuti-walled CNTs can be synthesized on Al matrix by using Ni, Co, and Cu catalysts.But the CNTs synthesized using Cu catalyst show a relatively low crystallization.Using0.5wt.%Co and Ni catalysts, the homogeneously dispersed CNTs on the Alpowder surface with relatively high purity, uniform diameters, and crystallization canbe obtained at600℃and underCH4and C2H2as carbon sources, respectively. Theobtained CNT/Al composite powders are suited to further preparation of composite.
CNT/Al composites were prepared by direct powder metallurgy of the in-situsynthesized composite powders. It was found that the maximum content of CNTsuniformly dispersed in Al matrix is2.5wt.%, and the mechanical properties of thecomposites decrease rapidly when the content of CNTs is more than2.5wt.%. Theoptimized CNT content is1.5wt.%, at which the composites show best compressiveproperty, and the compressive yield strength and compressive elastic modulus is2.2and3.0times as large as that of pure Al, respectively. Moreover, the corrosionresistance of Al matrix decreases with the increase of CNTs content.
In order to further improve the maximally uniform dispersion content in Alpowder matrix, ball-milling was introduced into the fabrication process of CNT/Alcomposites. The execution of ball milling for a short time can further improve the dispersion of CNTs fabricated by in-situ CVD. Meanwhile, CNTs are implanteddeeply into the matrix. The effects of ball milling parameters on the structure anddispersion of CNTs and the properties of CNT/Al composites were investigated. Itwas found that under the optimized milling conditions (ball-milling speed of500rpm,no process control agent added), with the increasing of milling time (≤120min), thedensity, hardness and tensile strength of2.5wt.%-CNT/Al composites increase. Thecomposites through90min of ball milling show well-balanced strength and ductility,whose hardness and tensile strength are2.4and2.7times as large as that of pure Al,and1.6and1.5times as large as that of the pure Al through the same milling process,respectively. Moreover, the elongation is larger than15%. With the increase of CNTcontent, the hardness and tensile strength of CNT/Al composites increase. The4.5wt.%-CNT/Al composites show largest hardness (HV131.2) and tensile strength (420MPa), which is2.3and2.4times more than that of pure Al, respectively. Furthermore,the coefficient of thermal expansion of CNT/Al composites is reduced significantlycompared with Al matrix, which decreases with the increase of the CNT content.
The effects of ball milling process and sintering temperature on the evolution ofCNT structure and the interface between CNTs and Al were studied. Thestrengthening mechanisms of CNT/Al composites were discussed. The results showedthat the short-time ball milling causes relatively small damage to CNT structure, andthe CNTs implanted into Al matrix possess well structure. The tensile strength andelongation of CNT/Al composite both reach maximum as630℃sinteringtemperature. The tensile properties of composites decrease when the sinteringtemperature is above Al melting point. There are three different forms of interfacialreaction between CNTs and Al matrix in the composites obtained at630℃sinteringtemperature: no distinct interface reaction, forming CNT@Al4C3structure, andcompletely forming Al4C3phase. The nano-sized Al4C3phase with small content canincrease the interface bonding between CNTs and Al, and is beneficial for theimprovement of the composite properties. The remarkable improvement of themechanical properties of CNT/Al composites results from the cooperative action ofseveral reinforcement mechanisms, including effective load transmission, dislocationstrengthening and grain refining strengthening.
引文
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