高性能碳纳米管/聚乙烯醇复合材料的制备及其物理和力学性能研究
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摘要
碳纳米管是碳原子组成的一维管状纳米材料,具有优异的力学性能和独特的传导性能。其拉伸强度可达63GPa,模量超过0.27TPa,是最强的纤维材料。采用碳纳米管作为聚合物材料的增强体,不仅可以显著提高聚合物的力学性能,同时能够赋予聚合物材料许多新的功能,实现多功能高强复合材料。然而由于碳纳米管的纳米尺度及团聚效应等因素使得制备理想结构的碳纳米管复合材料成为实现其优越性能的重要障碍。
目前广泛采用的碳纳米管复合材料制备方法还是基于将粉末状碳纳米管与聚合物介质相混合的方法。这些共混方法所制备的碳纳米管复合材料在力学性能上并没有充分体现碳纳米管的增强作用,其拉伸强度值往往只有几十兆帕。这主要是由于这些方法无法满足制备高强碳管复合材料的必要结构条件,即长碳纳米管以较高的纤维体积含量且排列规整地均匀分散在聚合物树脂中。因此,如何设计并采用一种新型的制备方法,在满足碳纳米管复合材料的结构条件的基础上实现高强高模碳纳米管复合材料并对复合材料的结构及性能进行系统研究成为本课题最主要的研究目的。
在本课题中,我们设计并首次实现了一种新型碳纳米管复合材料的制备方法,卷绕喷洒法。这种方法是将可纺丝碳纳米管阵列中抽取出的碳纳米管薄膜或丝束沿抽取方向卷绕在匀速转动的卷绕辊上,同时在卷绕辊表面喷洒一定浓度的聚合物喷洒液,使聚合物大分子随着喷洒液渗入每一层碳纳米管薄膜或丝束,并随着喷洒液的挥发与相邻碳纳米管相结合从而得到碳纳米管复合材料。若喷洒液中不含有任何聚合物大分子,相应方法也可制备成定向碳纳米管纸。通过卷绕喷洒工艺,我们采用不同结构参数的碳纳米管分别制备了高性能碳纳米管纸和碳纳米管复合材料,并对这些材料的结构及性能进行分析。根据对卷绕喷洒方法及工艺参数的研究和探讨,揭示了新型制备工艺对其结构和性能的影响规律；通过建立相关的理论模型和采用实验测试手段的方法,系统地研究了碳纳米管纸与复合材料的微观结构与其宏观性能间的关系。具体研究内容如下
首先,利用卷绕喷洒法采用三种不同碳纳米管标记为CNT-1, CNT-2和CNT-3分别制备成碳纳米管纸,通过透射电镜(TEM),拉曼光谱,光学显微镜和扫描电镜(SEM)对三种碳纳米管纸的形态和结构进行了表征并采用拉伸力学测试和四点接触法电阻测试对其拉伸性能和导电性能进行测试和对比分析。透射电镜图像显示CNT-1, CNT-2和CNT-3的管壁数目分别为3,6和50,经测量直径分别为8nm,8-10nm和45nm。拉曼光谱结果显示这三种碳纳米管D峰与G峰强度比值分别对应为0.54、0.63和0.35,表明CNT-3石墨化程度最高,缺陷最少。光学显微镜观察结果显示由等容量的去离子水和酒精混合配置的喷洒液在碳纳米管薄膜表面形成的接触角θ<90°,能够在短时间内渗入薄膜内部。SEM结果显示卷绕喷洒工艺不仅没有破坏碳纳米管薄膜高取向度的特征,且在一定程度减小了碳纳米管之间的空间距离,由此获得结构更加致密的高取向碳纳米管纸。CNT-1, CNT-2和CNT-3碳纳米管纸的平均强度依次为563MPa、423MPa、118MPa,平均模量依次为15.3GPa、10.1GPa、5.2GPa、与传统过滤法所制备的碳纳米管纸相比,定向碳纳米管纸具有优异的力学性能。随着碳纳米管直径的增大,碳纳米管纸的力学性能逐渐降低,符合有效截面利用率原理。四线法电阻测试结果显示碳纳米管纸的电导率随管壁数的增加分别547S/cm,356S/cm和288S/cm。高取向碳纳米管纸电导率的模型表明,其电导率的主要与单根碳纳米竹的平均电阻,碳纳米管的直径以及碳纳米管纸的孔隙率有关。
其次,在碳纳米管纸制备和研究的基础上,采用卷绕喷洒法以碳纳米管可纺丝阵列和水溶性聚乙烯醇溶液为原料制备了多壁(50壁)碳纳米管/聚乙烯醇复合材料。通过热失重分析(TGA), SEM,拉伸力学及电阻测试等方法研究了不同碳纳米管丝束抽取速度和喷洒溶液浓度对碳管复合材料结构和性能的影响。当喷洒聚合物溶液浓度为10g/L时,测试结果显示,随着碳纳米管丝束抽取速度从8mm/s增加到18mm/s,碳纳米管复合材料的平均强度从184MPa提高到289MPa,平均模量从14GPa提高到22GPa,电导率从115S/cm提高到157S/cm。拉伸断裂面的SEM结果显示,碳纳米管均匀分布在聚合物树脂中,其抽拔长度在5μm以内,远远小于其自身长度(700μm),说明卷绕喷洒工艺能够赋予碳纳米管与聚合物树脂之间很好的界面结合作用。当保持碳纳米管抽取速度为18mm/s时,随着碳纳米管喷洒溶液浓度从10g/L降低至2.5g/L,复合材料的平均强度从289MPa提高至937MPa,平均模量从22GPa提高到68GPa,电导率从157S/cm增加到589S/cm。TGA结果显示此时碳纳米管的含量高达57wt.%。拉伸断裂面的SEM图像中已观测不到连续相的聚合物树脂,均为抽拔出的碳纳米管,且能发现多壁碳纳米管特有的“剑鞘”断裂模式,说明外力通过聚合物介质有效地传递到了碳纳米管的外层竹壁上。当聚合物喷洒液的浓度进一步降低到1g/L时,复合材料的平均强度和模量相应降低至772MPa和58GPa,但导电性持续增加至747S/cm。
最后,采用性能优异的少壁(6壁)碳纳米管作为原料在改变喷洒聚合物溶液浓度的基础上对碳纳米管复合材料的力学和电学性能进行优化,并通过偏光拉曼光谱和SEM以及TGA测试对复合材料制备参数,微观结构以及宏观性能之间的关系进行了系统研究。当碳纳米管丝束抽取速度为18mm/s,喷洒液浓度为1g/L时,复合材料力学性能最好,其中平均拉伸强度可达1.7GPa,最高拉伸强度高达1.8GPa。拉伸模量受环境湿度影响,当湿度约为5%时,最大拉伸模量为96GPa,当湿度约超过50%时,拉伸模量为47GPa,此时最大断裂功可达112.3J/g。复合材料表面及其拉伸断裂面的SEM图像表明此时碳纳米管与聚合物形成最均匀的界面结构。喷洒液浓度高于1g/L时,有过量的聚合物包覆在碳管表面,喷洒液浓度低于1g/L时,复合材料表面存在没有聚合物填充的微孔。偏光拉曼测试的结果显示,当入射激光偏振方向与复合材料中碳管取向方向之间的夹角从0°增加至90°时,复合材料拉曼光谱的G’峰的均一化强度从1降低至0.493,说明了碳纳米管在复合材料中高度取向排列,复合材料具有各项异性的特征。而未经过真空热压的复合材料的G’峰的均一化强度仅降低至0.566,充分说明真空热压方法能够进一步优化碳纳米管在复合材料中的取向度。此外,四点接触法电阻测试结果显示此时碳管复合材料的电导率为693S/cm。随着喷洒溶液浓度降低至0.5g/L,复合材料的平均强度下降至1.5GPa,但其电导率仍然增加至781S/cm。
以上结果表明采用卷绕喷洒法制备高性能碳纳米管复合材料完全可行。与其他复合材料制备方法相比,这种方法能够同时满足复合材料中高体积含量的长碳纳米管以高度取向的排列方式与聚合物均匀有效地结合。在对碳纳米管丝束抽取速度及喷洒溶液浓度以及热压等方法优化的前提下,实现了高强度高模量的导电碳纳米管复合材料,为碳纳米管复合材料的制备方法提供了新的方向。此外,对复合材料结构,力学性能及电性能的研究为高性能碳纳米管复合材料的研究提供了必要的数据支持。
As a kind of one dimensional nano-sized material, carbon nanotube (CNT) possesses extraordinary mechanical properties and unique conductivity. The measured tensile strength of carbon nanotube is high up to63GPa and modulus is over0.27TPa. CNTs are the strongest fiber materials which make them ideal reinforcement for advanced composites. Reinforced with CNTs, polymer composites can obtain high performance with other new function, such as electrical or thermal conductive. However, realizing the outstanding properties of CNTs in polymer composites has many challenges, for CNTs are easy to aggregate together and hard to handle due to their small size. Fabricating CNT composites with desired structure is extremely difficult.
Common traditional methods for the fabrication of CNT-polymer composites are based on combining the carbon nanotube powder and polymer together in a way of solution or melt mixing. By these approaches, tensile properties of the composites are usually very low, less than100MPa. In order to fully utilize the mechanical properties of CNTs, it is desired to uniformly distribute among the polymer matrix the unidirectionally-aligned long tubes at a high fraction. Therefore, designing a new method for fabricating CNT composites with such desired structure and then investigating their properties is very important.
In this study, we demonstrate a one-step approach of "spray winding" to fabricate high-performance CNT composites. In this method, CNT sheets or ribbon, drawn out from CNT arrays are continuously collected (wound) onto a rotaing mandrel under the spray of a polymer solution. With the infiltration of solution into the CNT sheet and evaporation of solvent, polymer molecules have homogenous integration with CNTs, which is very critical in determining the properties of CNT composites. The oriented CNT paper can also be achieved by spraying polymer-free solution. Through spray winding, CNTs with different number of walls were fabricated into high performance aligned CNT paper and composites. The mechanism and technological parameters of spray winding method was studied. In addition, structures and properties of produced CNT paper and composites were investigated. Specifically as following:
First, different CNTs, namely CNT-1, CNT-2and CNT-3were fabricated into CNT paper by spray winding. Through transmission electron microscope (TEM), Raman spectroscopy, optical microscope and scanning electron microscope (SEM), morphology and structure of the CNT paper were characterized. The tensile properties and electrical conductivity were investigated through tensile testing and four-point-probe resistance testing. TEM image of the individual CNTs showed the wall numbers of CNT-1, CNT-2and CNT-3are3,6and50respectively, and their diameters were measured to be8nm,8-10nm and45nm. Raman spectroscopy results showed the ratio ID/IG of the D and G band intensities of the CNTs are0.54,0.63and0.35correspondingly, which indicates CNT-3has the least defects. By optical microscopy, we observed that the sprayed solution made by mixing the same volume of DI water and ethanol can infiltrate into the CNT sheet instantly. The capillary force results from the evaporation of the solvent draws the neighboring CNTs together. SEM images demonstrated that the highly alignment of CNTs in the CNT sheet was not damaged after the spray winding technique. Moreover, the interspaces of CNTs were decreased, which resulted into a densely compact highly oriented CNT paper. The average tensile strengths of CNT-1, CNT-2and CNT-3paper were563MPa,423MPa and118MPa, with average modulus of15.3GPa,10.1GPa and5.2GPa respectively. Compared with the CNT paper made by traditional methods, the aligned CNT paper showed excellent mechanical properties. With increasing the CNT diameter, the mechanical properties of CNT paper is reduced, which is explained by the theory of effective cross-section area. According to the resistance results tested by four-point-probe method, the electrical conductivity of the three CNT paper were547S/cm,356S/cm and288S/cm. The electrical conductivity model indicated that the average resistance and diameter of the CNTs, porosity of CNT paper is the main factor to the resistance of CNT paper.
Secondly, based on the research of CNT paper by spray winding, multi-walled (50walls) CNTs (MWNTs) and water soluble poly (vinyl alcohol)(PVA) were fabricated into MWNT/PVA composites by spraying the PVA solution. Influence of different drawing speed and polymer solution concentration to the structure and properties of CNT composites were investigated through thermal gravimetric analysis (TGA), SEM, tensile and resistance testing. Under the10g/L-PVA solution spraying, with increasing the CNT ribbon drawing speed of8mm/s to18mm/s, the average tensile strength of MWNT/PVA composites was improved from184MPa to289MPa, with average modulus improved from14GPa to22GPa, electrical conductivity improved from115S/cm to157S/cm. SEM image of the fractured surface showed that MWNTs were uniformly distributed into the polymer matrix, with a pull out length of less than5μm, which indicated a good interface between nanotubes and PVA polymer. When the drawing speed of ribbon was kept at18mm/s, with decreasing of the PVA concentration from10g/L to2.5g/L, the average tensile strength of MWNT/PVA composites was improved from289MPa to937MPa, with modulus improvement from22GPa to68GPa and electrical conductivity from157S/cm to589S/cm. The mass fraction of the composites with highest strength was tested to be53%based on the TGA results. The SEM image of the fracture surfaced demonstrated a CNT rich cross section. The typical "sword in sheath" breaking of MWNT can be found, which suggested an effective load transfer from the matrix to the nanotubes. With decreasing the polymer concentration to1g/L, the mechanical properties of composites was decreased with an average strength and modulus of772MPa and58GPa. However, the electrical conductivity was still improved to747S/cm.
At last, in order to improved the mechanical and conductivity properties of the composites, few-walled (6walls) CNTs (FWNTs) were used with different concentration of sprayed PVA solution. By polarized Raman spectroscopy, SEM, TGA and other testing method, the relationship between processing, structure and properties of the composites were systematically studied. When the drawing speed of the CNT ribbon is18mm/s and sprayed solution concentration is1g/L, FWNT composites achieved the best mechanical properties with an average tensile strength of1.7GPa and the highest tensile strength of1.8GPa. The tensile modulus is found to be affected by the embient humidity. When the humidity is about5%, the highest modulus of composites reached to96GPa. When humidity is over50%, the composites film has a modulus of47GPa and a toughness of over100J/g. SEM images of the surface and cross-section of the composites demonstrated that the1g/L solution produced an optimized structure with relatively high CNT fraction and no void. There was excessive matrix around the nanotubes when the concentration of the sprayed PVA solution was2g/L and there were micrometer-sized voids within the composites when the concentration is0.5g/L. Polarized Raman spectroscopy analysis of the composites with optimal structure showed that the normalized G'-band Raman intensity decreased from1to0.493when the angle between the composites film and the polarization axis of the incident laser beam was changed from0°to90°. This indicated an anisotropic characteristic of the composites with highly aligned CNTs. Composites before hot-pressing has a decreased normalized intensity of0.566, which stated that the degree of alignment can be further improved by the vacuum aid hot-pressing process. Additionally, the electrical conductivity of the composites with the best mechanical properties was calculated to be693S/cm after4-point-probe resistance testing. With decreasing the polymer concentration to0.5g/L during fabrication, the average tensile strength of the compsites decreased to1.5GPa. However, the conductivity of the composites increased to781S/cm.
In conclusion, spray winding approach is absolutely feasible for the fabrication of high performance CNT-polymer composites. Compared with other methods, this approach can obtain the desired CNT composites structure with high fractional long and aligned CNT uniformly distributed into the polymer matrix. Though optimizing the process, such as ribbon drawing speed, solution concentration and vacuum aid hot-pressing, high strength and modulus conductive CNT composites is successfully achieved. The influence of the process to the structure and properties of the composites was systematically studied.
目前广泛采用的碳纳米管复合材料制备方法还是基于将粉末状碳纳米管与聚合物介质相混合的方法。这些共混方法所制备的碳纳米管复合材料在力学性能上并没有充分体现碳纳米管的增强作用,其拉伸强度值往往只有几十兆帕。这主要是由于这些方法无法满足制备高强碳管复合材料的必要结构条件,即长碳纳米管以较高的纤维体积含量且排列规整地均匀分散在聚合物树脂中。因此,如何设计并采用一种新型的制备方法,在满足碳纳米管复合材料的结构条件的基础上实现高强高模碳纳米管复合材料并对复合材料的结构及性能进行系统研究成为本课题最主要的研究目的。
在本课题中,我们设计并首次实现了一种新型碳纳米管复合材料的制备方法,卷绕喷洒法。这种方法是将可纺丝碳纳米管阵列中抽取出的碳纳米管薄膜或丝束沿抽取方向卷绕在匀速转动的卷绕辊上,同时在卷绕辊表面喷洒一定浓度的聚合物喷洒液,使聚合物大分子随着喷洒液渗入每一层碳纳米管薄膜或丝束,并随着喷洒液的挥发与相邻碳纳米管相结合从而得到碳纳米管复合材料。若喷洒液中不含有任何聚合物大分子,相应方法也可制备成定向碳纳米管纸。通过卷绕喷洒工艺,我们采用不同结构参数的碳纳米管分别制备了高性能碳纳米管纸和碳纳米管复合材料,并对这些材料的结构及性能进行分析。根据对卷绕喷洒方法及工艺参数的研究和探讨,揭示了新型制备工艺对其结构和性能的影响规律；通过建立相关的理论模型和采用实验测试手段的方法,系统地研究了碳纳米管纸与复合材料的微观结构与其宏观性能间的关系。具体研究内容如下
首先,利用卷绕喷洒法采用三种不同碳纳米管标记为CNT-1, CNT-2和CNT-3分别制备成碳纳米管纸,通过透射电镜(TEM),拉曼光谱,光学显微镜和扫描电镜(SEM)对三种碳纳米管纸的形态和结构进行了表征并采用拉伸力学测试和四点接触法电阻测试对其拉伸性能和导电性能进行测试和对比分析。透射电镜图像显示CNT-1, CNT-2和CNT-3的管壁数目分别为3,6和50,经测量直径分别为8nm,8-10nm和45nm。拉曼光谱结果显示这三种碳纳米管D峰与G峰强度比值分别对应为0.54、0.63和0.35,表明CNT-3石墨化程度最高,缺陷最少。光学显微镜观察结果显示由等容量的去离子水和酒精混合配置的喷洒液在碳纳米管薄膜表面形成的接触角θ<90°,能够在短时间内渗入薄膜内部。SEM结果显示卷绕喷洒工艺不仅没有破坏碳纳米管薄膜高取向度的特征,且在一定程度减小了碳纳米管之间的空间距离,由此获得结构更加致密的高取向碳纳米管纸。CNT-1, CNT-2和CNT-3碳纳米管纸的平均强度依次为563MPa、423MPa、118MPa,平均模量依次为15.3GPa、10.1GPa、5.2GPa、与传统过滤法所制备的碳纳米管纸相比,定向碳纳米管纸具有优异的力学性能。随着碳纳米管直径的增大,碳纳米管纸的力学性能逐渐降低,符合有效截面利用率原理。四线法电阻测试结果显示碳纳米管纸的电导率随管壁数的增加分别547S/cm,356S/cm和288S/cm。高取向碳纳米管纸电导率的模型表明,其电导率的主要与单根碳纳米竹的平均电阻,碳纳米管的直径以及碳纳米管纸的孔隙率有关。
其次,在碳纳米管纸制备和研究的基础上,采用卷绕喷洒法以碳纳米管可纺丝阵列和水溶性聚乙烯醇溶液为原料制备了多壁(50壁)碳纳米管/聚乙烯醇复合材料。通过热失重分析(TGA), SEM,拉伸力学及电阻测试等方法研究了不同碳纳米管丝束抽取速度和喷洒溶液浓度对碳管复合材料结构和性能的影响。当喷洒聚合物溶液浓度为10g/L时,测试结果显示,随着碳纳米管丝束抽取速度从8mm/s增加到18mm/s,碳纳米管复合材料的平均强度从184MPa提高到289MPa,平均模量从14GPa提高到22GPa,电导率从115S/cm提高到157S/cm。拉伸断裂面的SEM结果显示,碳纳米管均匀分布在聚合物树脂中,其抽拔长度在5μm以内,远远小于其自身长度(700μm),说明卷绕喷洒工艺能够赋予碳纳米管与聚合物树脂之间很好的界面结合作用。当保持碳纳米管抽取速度为18mm/s时,随着碳纳米管喷洒溶液浓度从10g/L降低至2.5g/L,复合材料的平均强度从289MPa提高至937MPa,平均模量从22GPa提高到68GPa,电导率从157S/cm增加到589S/cm。TGA结果显示此时碳纳米管的含量高达57wt.%。拉伸断裂面的SEM图像中已观测不到连续相的聚合物树脂,均为抽拔出的碳纳米管,且能发现多壁碳纳米管特有的“剑鞘”断裂模式,说明外力通过聚合物介质有效地传递到了碳纳米管的外层竹壁上。当聚合物喷洒液的浓度进一步降低到1g/L时,复合材料的平均强度和模量相应降低至772MPa和58GPa,但导电性持续增加至747S/cm。
最后,采用性能优异的少壁(6壁)碳纳米管作为原料在改变喷洒聚合物溶液浓度的基础上对碳纳米管复合材料的力学和电学性能进行优化,并通过偏光拉曼光谱和SEM以及TGA测试对复合材料制备参数,微观结构以及宏观性能之间的关系进行了系统研究。当碳纳米管丝束抽取速度为18mm/s,喷洒液浓度为1g/L时,复合材料力学性能最好,其中平均拉伸强度可达1.7GPa,最高拉伸强度高达1.8GPa。拉伸模量受环境湿度影响,当湿度约为5%时,最大拉伸模量为96GPa,当湿度约超过50%时,拉伸模量为47GPa,此时最大断裂功可达112.3J/g。复合材料表面及其拉伸断裂面的SEM图像表明此时碳纳米管与聚合物形成最均匀的界面结构。喷洒液浓度高于1g/L时,有过量的聚合物包覆在碳管表面,喷洒液浓度低于1g/L时,复合材料表面存在没有聚合物填充的微孔。偏光拉曼测试的结果显示,当入射激光偏振方向与复合材料中碳管取向方向之间的夹角从0°增加至90°时,复合材料拉曼光谱的G’峰的均一化强度从1降低至0.493,说明了碳纳米管在复合材料中高度取向排列,复合材料具有各项异性的特征。而未经过真空热压的复合材料的G’峰的均一化强度仅降低至0.566,充分说明真空热压方法能够进一步优化碳纳米管在复合材料中的取向度。此外,四点接触法电阻测试结果显示此时碳管复合材料的电导率为693S/cm。随着喷洒溶液浓度降低至0.5g/L,复合材料的平均强度下降至1.5GPa,但其电导率仍然增加至781S/cm。
以上结果表明采用卷绕喷洒法制备高性能碳纳米管复合材料完全可行。与其他复合材料制备方法相比,这种方法能够同时满足复合材料中高体积含量的长碳纳米管以高度取向的排列方式与聚合物均匀有效地结合。在对碳纳米管丝束抽取速度及喷洒溶液浓度以及热压等方法优化的前提下,实现了高强度高模量的导电碳纳米管复合材料,为碳纳米管复合材料的制备方法提供了新的方向。此外,对复合材料结构,力学性能及电性能的研究为高性能碳纳米管复合材料的研究提供了必要的数据支持。
As a kind of one dimensional nano-sized material, carbon nanotube (CNT) possesses extraordinary mechanical properties and unique conductivity. The measured tensile strength of carbon nanotube is high up to63GPa and modulus is over0.27TPa. CNTs are the strongest fiber materials which make them ideal reinforcement for advanced composites. Reinforced with CNTs, polymer composites can obtain high performance with other new function, such as electrical or thermal conductive. However, realizing the outstanding properties of CNTs in polymer composites has many challenges, for CNTs are easy to aggregate together and hard to handle due to their small size. Fabricating CNT composites with desired structure is extremely difficult.
Common traditional methods for the fabrication of CNT-polymer composites are based on combining the carbon nanotube powder and polymer together in a way of solution or melt mixing. By these approaches, tensile properties of the composites are usually very low, less than100MPa. In order to fully utilize the mechanical properties of CNTs, it is desired to uniformly distribute among the polymer matrix the unidirectionally-aligned long tubes at a high fraction. Therefore, designing a new method for fabricating CNT composites with such desired structure and then investigating their properties is very important.
In this study, we demonstrate a one-step approach of "spray winding" to fabricate high-performance CNT composites. In this method, CNT sheets or ribbon, drawn out from CNT arrays are continuously collected (wound) onto a rotaing mandrel under the spray of a polymer solution. With the infiltration of solution into the CNT sheet and evaporation of solvent, polymer molecules have homogenous integration with CNTs, which is very critical in determining the properties of CNT composites. The oriented CNT paper can also be achieved by spraying polymer-free solution. Through spray winding, CNTs with different number of walls were fabricated into high performance aligned CNT paper and composites. The mechanism and technological parameters of spray winding method was studied. In addition, structures and properties of produced CNT paper and composites were investigated. Specifically as following:
First, different CNTs, namely CNT-1, CNT-2and CNT-3were fabricated into CNT paper by spray winding. Through transmission electron microscope (TEM), Raman spectroscopy, optical microscope and scanning electron microscope (SEM), morphology and structure of the CNT paper were characterized. The tensile properties and electrical conductivity were investigated through tensile testing and four-point-probe resistance testing. TEM image of the individual CNTs showed the wall numbers of CNT-1, CNT-2and CNT-3are3,6and50respectively, and their diameters were measured to be8nm,8-10nm and45nm. Raman spectroscopy results showed the ratio ID/IG of the D and G band intensities of the CNTs are0.54,0.63and0.35correspondingly, which indicates CNT-3has the least defects. By optical microscopy, we observed that the sprayed solution made by mixing the same volume of DI water and ethanol can infiltrate into the CNT sheet instantly. The capillary force results from the evaporation of the solvent draws the neighboring CNTs together. SEM images demonstrated that the highly alignment of CNTs in the CNT sheet was not damaged after the spray winding technique. Moreover, the interspaces of CNTs were decreased, which resulted into a densely compact highly oriented CNT paper. The average tensile strengths of CNT-1, CNT-2and CNT-3paper were563MPa,423MPa and118MPa, with average modulus of15.3GPa,10.1GPa and5.2GPa respectively. Compared with the CNT paper made by traditional methods, the aligned CNT paper showed excellent mechanical properties. With increasing the CNT diameter, the mechanical properties of CNT paper is reduced, which is explained by the theory of effective cross-section area. According to the resistance results tested by four-point-probe method, the electrical conductivity of the three CNT paper were547S/cm,356S/cm and288S/cm. The electrical conductivity model indicated that the average resistance and diameter of the CNTs, porosity of CNT paper is the main factor to the resistance of CNT paper.
Secondly, based on the research of CNT paper by spray winding, multi-walled (50walls) CNTs (MWNTs) and water soluble poly (vinyl alcohol)(PVA) were fabricated into MWNT/PVA composites by spraying the PVA solution. Influence of different drawing speed and polymer solution concentration to the structure and properties of CNT composites were investigated through thermal gravimetric analysis (TGA), SEM, tensile and resistance testing. Under the10g/L-PVA solution spraying, with increasing the CNT ribbon drawing speed of8mm/s to18mm/s, the average tensile strength of MWNT/PVA composites was improved from184MPa to289MPa, with average modulus improved from14GPa to22GPa, electrical conductivity improved from115S/cm to157S/cm. SEM image of the fractured surface showed that MWNTs were uniformly distributed into the polymer matrix, with a pull out length of less than5μm, which indicated a good interface between nanotubes and PVA polymer. When the drawing speed of ribbon was kept at18mm/s, with decreasing of the PVA concentration from10g/L to2.5g/L, the average tensile strength of MWNT/PVA composites was improved from289MPa to937MPa, with modulus improvement from22GPa to68GPa and electrical conductivity from157S/cm to589S/cm. The mass fraction of the composites with highest strength was tested to be53%based on the TGA results. The SEM image of the fracture surfaced demonstrated a CNT rich cross section. The typical "sword in sheath" breaking of MWNT can be found, which suggested an effective load transfer from the matrix to the nanotubes. With decreasing the polymer concentration to1g/L, the mechanical properties of composites was decreased with an average strength and modulus of772MPa and58GPa. However, the electrical conductivity was still improved to747S/cm.
At last, in order to improved the mechanical and conductivity properties of the composites, few-walled (6walls) CNTs (FWNTs) were used with different concentration of sprayed PVA solution. By polarized Raman spectroscopy, SEM, TGA and other testing method, the relationship between processing, structure and properties of the composites were systematically studied. When the drawing speed of the CNT ribbon is18mm/s and sprayed solution concentration is1g/L, FWNT composites achieved the best mechanical properties with an average tensile strength of1.7GPa and the highest tensile strength of1.8GPa. The tensile modulus is found to be affected by the embient humidity. When the humidity is about5%, the highest modulus of composites reached to96GPa. When humidity is over50%, the composites film has a modulus of47GPa and a toughness of over100J/g. SEM images of the surface and cross-section of the composites demonstrated that the1g/L solution produced an optimized structure with relatively high CNT fraction and no void. There was excessive matrix around the nanotubes when the concentration of the sprayed PVA solution was2g/L and there were micrometer-sized voids within the composites when the concentration is0.5g/L. Polarized Raman spectroscopy analysis of the composites with optimal structure showed that the normalized G'-band Raman intensity decreased from1to0.493when the angle between the composites film and the polarization axis of the incident laser beam was changed from0°to90°. This indicated an anisotropic characteristic of the composites with highly aligned CNTs. Composites before hot-pressing has a decreased normalized intensity of0.566, which stated that the degree of alignment can be further improved by the vacuum aid hot-pressing process. Additionally, the electrical conductivity of the composites with the best mechanical properties was calculated to be693S/cm after4-point-probe resistance testing. With decreasing the polymer concentration to0.5g/L during fabrication, the average tensile strength of the compsites decreased to1.5GPa. However, the conductivity of the composites increased to781S/cm.
In conclusion, spray winding approach is absolutely feasible for the fabrication of high performance CNT-polymer composites. Compared with other methods, this approach can obtain the desired CNT composites structure with high fractional long and aligned CNT uniformly distributed into the polymer matrix. Though optimizing the process, such as ribbon drawing speed, solution concentration and vacuum aid hot-pressing, high strength and modulus conductive CNT composites is successfully achieved. The influence of the process to the structure and properties of the composites was systematically studied.
引文
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