碳纳米管与聚酰亚胺界面优化、分子动力学模拟及其复合材料的结构性能表征
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摘要
碳纳米管的独特结构赋予了它特殊的力学、电学、热学性能,作为下一代多功能性复合材料的主体材料而备受关注。为了能够最大限度的利用碳纳米管的高强高韧的特性,成功解决碳纳米管分散、取向和界面问题因而成为重要的研究课题。同时,聚酰亚胺作为一种耐高温型树脂,在航空航天领域应用前景广阔,将这两者性能优异的材料组合制备复合材料,将会在多功能复合材料领域具有极大发展前景。但从目前已有的文献报道中可以看出,关于碳纳米管与聚酰亚胺复合材料的界面研究还相当有限,制备复合材料的方法也局限于将碳纳米管短纤分散于聚酰亚胺树脂中,获得纤维体积含量较低的复合材料。由于在复合材料中,增强体的形态、含量,以及增强体与基体间的界面对复合材料性能起到至关重要的影响,因此,本论文从改变碳纳米管结构和改善碳纳米管与聚酰亚胺界面的角度入手,旨在解决存在于传统碳纳米管复合材料中的分散、取向和界面问题。采用分子动力学模拟从微观角度深入探讨碳纳米管与聚酰亚胺树脂间的界面结合,以及利用等离子处理方法改善界面作用,提升复合材料的机械性能,并采用一种新型复合材料成型方法(喷覆卷绕法)制备单向碳纳米管增强聚酰亚胺复合材料,解决碳纳米管分散、取向和低纤维体积含量的问题,提高碳纳米管复合材料的力学、电学、热学性能。基于此,本文对于碳纳米管增强聚酰亚胺复合材料的研究从解决影响性能的本质入手,采用实验与分子动力学模拟两种手段,揭示改善复合材料界面与结构的方法,具有极为重要的指导意义。围绕该主题,课题开展的研究工作具体如下：
(1)为了改善碳纳米管与聚酰亚胺树脂的界面性能,采用常压射流等离子体处理碳纳米管集合体(碳纳米管纸)。碳纳米管经过分散、抽滤、烘干后得到厚度为70gm的碳纳米管纸,然后经由含氧等离子体处理后制备聚酰亚胺复合材料。处理前后的碳纳米管纸样品采用SEM、 XPS、静态接触角测试表征其表面形态及亲水性变化,结果表明,等离子体在不影响碳纳米管纸整体结构的同时有效“切断”碳纳米管头端,增加碳纳米管与树脂基体的纳米机械锁结。含氧等离子处理可增加碳纳米管纸表面亲水基团数量,静态接触角从123.2°到35.2°,由拒水性转变为亲水性。基于如上机械锁结和亲水性提高两方面的协同作用,复合材料在拉伸强力和模量方面体现出明显的提升,拉伸断裂界面也比未处理样品显示出更少的抽拔状态,体现出含氧等离子体处理可有效的改善碳纳米管与聚酰亚胺树脂的界面,使碳纳米管作为增强体更有效的承力。与此同时,复合材料的耐高温性质在等离子处理前后并未发生改变,在500℃前复合材料并未发生明显质量损失。
(2)为了研究碳纳米管结构对复合材料的性能影响,我们采用超取向碳纳米管阵列制备单向碳纳米管复合材料预浸料,并对预浸料进行拉伸预处理,已达到改善复合材料性能的目的。由于超取向碳纳米管阵列间很强的范德华力存在,可以抽出连续如长丝束般的碳纳米管片层,其间所有碳纳米管的取向一致,均沿长度方向有序排列,这一结构特性大大增强了电子和光子在碳纳米管中的传播。与以往传统碳纳米管短纤增强复合材料不同,这种连续结构不仅可以解决碳纳米管分散和取向问题,而且可以制备高纤维体积含量的复合材料,这对于提升碳纳米管各方面性能均有重要意义。预拉伸处理进一步改善了碳纳米管内部的取向和整体紧实度,将复合材料性能进一步提升。当碳纳米管的取向度和紧实度提高时,复合材料在杨氏模量、导电率、面内热传导系数方面,分别有262.0%,45.1%,69.0%的提高。导电率和面内热传导系数更达到了以往碳纳米管短纤复合材料无法达到的数值,分别为265.9S/cm和31.1W/mK。
(3)为了更为深入的探明碳纳米管与聚酰亚胺间的作用机理,尤其是分子级别的相互作用,并为复合材料设计提供理论依据,我们采用分子动力学模拟技术开展研究。分子动力学模拟技术是一种新兴的研究纳米级别相互作用的技术。本研究中,采用这种模拟技术模拟单根碳纳米管与聚酰亚胺间的抽拔,并根据体系能量变化分析碳纳米管与聚酰亚胺的作用机理,以及碳纳米管管壁数量对抽拔过程的影响,最终计算得到界面剪切强力数值。在模拟单根碳纳米管与单根聚酰亚胺长链的过程中,发现两者具有强烈的相互作用力,这种相互作用力直接对抽拔过程产生影响。此外,当施加不同大小的力试图抽拔碳纳米管时,我们发现临界拉力值的存在,即只有当拉力值大于临界拉力值时,抽拔过程才能够完成。影响这种临界拉力值的主要因素是碳纳米管管壁数量,单壁与双壁碳纳米管具有相同的临界拉力值,但三壁碳纳米管所需的临界拉力值要大于前两者。同时,类似的趋势也在抽拔位移中得到体现,这主要是由于碳纳米管管壁间的范德华力造成了碳纳米管与聚酰亚胺基体间的相互作用能差异,这种差异在单壁和双壁碳纳米管间较小,而对于三壁碳纳米管则较明显。最终经模拟计算所得的在不同拉力值作用下的界面剪切强力处于2～19MPa这个范围,符合碳纳米管增强复合材料在以往实验和模拟中数值的合理范围。
(4)碳纳米管体积含量对于碳纳米管复合材料的力学性能影响众所周知,即随着碳纳米管含量的增加,复合材料的拉伸强力和初始模量相应增加。但碳纳米管体积含量的增加是否会影响聚合物结构及链段取向及怎样影响,则是一个需要从微观作用机理进行研究的问题,但在以往的研究中未得到充分的研究。因此,我们采用分子动力学模拟这一手段,拟在分子级别对这一问题进行探讨和分析。首先我们建立不同碳纳米管体积含量和纯聚酰亚胺的模型,在单轴向拉伸状态下观察体系的模量变化,并在传统计算纤维体积含量的公式基础上进行修正,将碳纳米管与聚酰亚胺的界面作为孔隙讨论,精确纤维体积含量的计算。同时利用结晶态和非晶态聚酰亚胺两种模型模拟真实聚酰亚胺半晶态结构,利用“混合定律”计算随碳纳米管体积含量的变化和聚酰亚胺结晶度的变化。模拟最终得到的趋势能够很好验证实验中关于碳纳米管在聚合物基体中充当成核点的假设。
综上所述,本文以碳纳米管增强聚酰亚胺复合材料为研究对象,从改善界面和改变碳纳米管结构的角度,探讨了提高复合材料宏观性能的有效途径；并采用分子动力学模拟的分析方法从微观角度深入分析了碳纳米管与聚酰亚胺在分子级别上的作用机理,为碳纳米管增强复合材料的设计提供了可参考的实验方法和理论依据,并为深入分析纳米增强聚合物基复合材料的性能及其影响机理提供了有效的研究思路。
Carbon nanotubes (CNTs) with unique structure and properties are in the vanguard of technological development of the time, and are predicted to be the best candidate as the multifunctional component of the next generation of composite materials.To fully utilize the unique mechanical and physical properties of carbon nanotubes, it is essential to assemble them into macroscopic structures. Polyimide, as the most well-known high temperature resistance polymer, is widely utilized in aerospace applications. Therefore, the combination of these two materials will be promising for multifunctional application. However, previous studies have confined to mix staple carbon nanotube with polymer solutions and fabricate composites with comparatively low volume fraction.In composite design, the morphology and content of reinforcement, and the interface between carbon nanotube and polymer are the main factors to determine the composite property. Thus, this dissertation aims to solve the CNTs dispersion, alignment and interface problems in carbon nanotube reinforced composite by demonstrating the interfacial property using molecular dynamics simulation and plasma treatment method, fabricating CNT composites with ideal structural features and excellent mechanical,thermal and electrical performances, and increasing the understanding of the structure-property relationship in these materials. The detailed studies are described below:
(1)Atmospheric plasma treatment is applied on carbon nanotube, in the form of bucky paper, to improve the interfacial interaction between carbon nanotube and polyimdie. The fabrication of bucky paper is consisted of dissolve, filtration and drying processes, following the plasma treatment and fabrication of composite. The SEM, XPS and static contact angle analysis are conducted to discover the morphology and hydrophilicty change before and after plasma treatment. It is shown that the plasma treatment can effectively "cut off' the heads of CNTs without altering the bulk properties of composite, which increase the nano-mechanical interlocking between CNTs and polymer. Besides, the number of oxygen-containing groups increases and contact angle transfers from hydrophobicity to hydrophilicity. Based on the two mechanisms, the mechanical property of composite is improved distinctly. The tensile fracture surface also shows that less pull-out happens after plasma treatment. And high temperature resistance is retained even after the plasma treatment.
(2) In order to reveal the structure-related property, we adopt a new fabrication method named spray-winding to make carbon nanotube reinforced polyimide composite. Due to the strong Van der Waals between CNTs, the CNT can be pulled out in the form of continuous ribbons, in which CNTs keep oriented and aligned along the longitudinal direction. The unique structure helps the electron and phonon transmission, thus improving the electrical and thermal properties. Compared with the traditional carbon nanotube reinforced composite, this continuous structure not only solves the dispersion and alignment problems, but improve volume fraction to a high level.We further use pre-stretch treatment to improve the alignment and compactness of CNT prepregs, thus obtaining better mechanical, electrical and thermal properties.
(3) To discover the interaction mechanism between carbon nanotube and polyimide, especially in the molecular scale, we need a special tool—molecular dynamics simulation to achieve this goal. Compared with experimental techniques, this computational method is more effective and time-saving. Single chain simulation is firstly to employ to find that the interaction energy between carbon nanotube and polyimide is very high, and this phenomon is also verified in pull-out simulation where co-movement occurs. Limiting pulling force is found in pull-out simualtions, above which the pull-out process can not be achieved. For SWNT and DWNT, the limiting pulling forces are the same value, but for TWNT, it is higher than the SWNT and DWNT. This is due to the inter-tube interactions during pull-out. The interfacial shear strength is calculated to be around5～30MPa which are in the reasonable value among previous experimental and simulation values.
(4) The volume fraction of carbon nanotube is an important factor influencing the properties of composite. How the volume faction affects the polymer chain structure configuration is meaningful in composite design, but no previous study has been done. Therefore, we use molecular dynamics simulation to build composite and polyimide structures separately and invesitigate the polymer configuration change with the increasing of volume fraction. We modify the traditional volume fraction formula and regard the interface as the voids in calculation. Meanwhile, we make "fully crystallized" and "fully amorphous" polyimide structure in simulation and calculate the crystallinity using the rule of mixture. The simulation results are in the agreement with assumption that carbon nanotubes act as the nucleation site in composite.
To sum up, this paper discusses the effective methods to improve the propertyies of carbon nanotube based composite by improving the interface and changing carbon nanotube structure. The molecular dynamics simulation is applied to investigate the micro-scale mechanism of carbon nanotube and polyimide interactions, thus providing valid methods and evidence for composite design and opening up a new vision for nano-reinforced composite studies.
(1)为了改善碳纳米管与聚酰亚胺树脂的界面性能,采用常压射流等离子体处理碳纳米管集合体(碳纳米管纸)。碳纳米管经过分散、抽滤、烘干后得到厚度为70gm的碳纳米管纸,然后经由含氧等离子体处理后制备聚酰亚胺复合材料。处理前后的碳纳米管纸样品采用SEM、 XPS、静态接触角测试表征其表面形态及亲水性变化,结果表明,等离子体在不影响碳纳米管纸整体结构的同时有效“切断”碳纳米管头端,增加碳纳米管与树脂基体的纳米机械锁结。含氧等离子处理可增加碳纳米管纸表面亲水基团数量,静态接触角从123.2°到35.2°,由拒水性转变为亲水性。基于如上机械锁结和亲水性提高两方面的协同作用,复合材料在拉伸强力和模量方面体现出明显的提升,拉伸断裂界面也比未处理样品显示出更少的抽拔状态,体现出含氧等离子体处理可有效的改善碳纳米管与聚酰亚胺树脂的界面,使碳纳米管作为增强体更有效的承力。与此同时,复合材料的耐高温性质在等离子处理前后并未发生改变,在500℃前复合材料并未发生明显质量损失。
(2)为了研究碳纳米管结构对复合材料的性能影响,我们采用超取向碳纳米管阵列制备单向碳纳米管复合材料预浸料,并对预浸料进行拉伸预处理,已达到改善复合材料性能的目的。由于超取向碳纳米管阵列间很强的范德华力存在,可以抽出连续如长丝束般的碳纳米管片层,其间所有碳纳米管的取向一致,均沿长度方向有序排列,这一结构特性大大增强了电子和光子在碳纳米管中的传播。与以往传统碳纳米管短纤增强复合材料不同,这种连续结构不仅可以解决碳纳米管分散和取向问题,而且可以制备高纤维体积含量的复合材料,这对于提升碳纳米管各方面性能均有重要意义。预拉伸处理进一步改善了碳纳米管内部的取向和整体紧实度,将复合材料性能进一步提升。当碳纳米管的取向度和紧实度提高时,复合材料在杨氏模量、导电率、面内热传导系数方面,分别有262.0%,45.1%,69.0%的提高。导电率和面内热传导系数更达到了以往碳纳米管短纤复合材料无法达到的数值,分别为265.9S/cm和31.1W/mK。
(3)为了更为深入的探明碳纳米管与聚酰亚胺间的作用机理,尤其是分子级别的相互作用,并为复合材料设计提供理论依据,我们采用分子动力学模拟技术开展研究。分子动力学模拟技术是一种新兴的研究纳米级别相互作用的技术。本研究中,采用这种模拟技术模拟单根碳纳米管与聚酰亚胺间的抽拔,并根据体系能量变化分析碳纳米管与聚酰亚胺的作用机理,以及碳纳米管管壁数量对抽拔过程的影响,最终计算得到界面剪切强力数值。在模拟单根碳纳米管与单根聚酰亚胺长链的过程中,发现两者具有强烈的相互作用力,这种相互作用力直接对抽拔过程产生影响。此外,当施加不同大小的力试图抽拔碳纳米管时,我们发现临界拉力值的存在,即只有当拉力值大于临界拉力值时,抽拔过程才能够完成。影响这种临界拉力值的主要因素是碳纳米管管壁数量,单壁与双壁碳纳米管具有相同的临界拉力值,但三壁碳纳米管所需的临界拉力值要大于前两者。同时,类似的趋势也在抽拔位移中得到体现,这主要是由于碳纳米管管壁间的范德华力造成了碳纳米管与聚酰亚胺基体间的相互作用能差异,这种差异在单壁和双壁碳纳米管间较小,而对于三壁碳纳米管则较明显。最终经模拟计算所得的在不同拉力值作用下的界面剪切强力处于2～19MPa这个范围,符合碳纳米管增强复合材料在以往实验和模拟中数值的合理范围。
(4)碳纳米管体积含量对于碳纳米管复合材料的力学性能影响众所周知,即随着碳纳米管含量的增加,复合材料的拉伸强力和初始模量相应增加。但碳纳米管体积含量的增加是否会影响聚合物结构及链段取向及怎样影响,则是一个需要从微观作用机理进行研究的问题,但在以往的研究中未得到充分的研究。因此,我们采用分子动力学模拟这一手段,拟在分子级别对这一问题进行探讨和分析。首先我们建立不同碳纳米管体积含量和纯聚酰亚胺的模型,在单轴向拉伸状态下观察体系的模量变化,并在传统计算纤维体积含量的公式基础上进行修正,将碳纳米管与聚酰亚胺的界面作为孔隙讨论,精确纤维体积含量的计算。同时利用结晶态和非晶态聚酰亚胺两种模型模拟真实聚酰亚胺半晶态结构,利用“混合定律”计算随碳纳米管体积含量的变化和聚酰亚胺结晶度的变化。模拟最终得到的趋势能够很好验证实验中关于碳纳米管在聚合物基体中充当成核点的假设。
综上所述,本文以碳纳米管增强聚酰亚胺复合材料为研究对象,从改善界面和改变碳纳米管结构的角度,探讨了提高复合材料宏观性能的有效途径；并采用分子动力学模拟的分析方法从微观角度深入分析了碳纳米管与聚酰亚胺在分子级别上的作用机理,为碳纳米管增强复合材料的设计提供了可参考的实验方法和理论依据,并为深入分析纳米增强聚合物基复合材料的性能及其影响机理提供了有效的研究思路。
Carbon nanotubes (CNTs) with unique structure and properties are in the vanguard of technological development of the time, and are predicted to be the best candidate as the multifunctional component of the next generation of composite materials.To fully utilize the unique mechanical and physical properties of carbon nanotubes, it is essential to assemble them into macroscopic structures. Polyimide, as the most well-known high temperature resistance polymer, is widely utilized in aerospace applications. Therefore, the combination of these two materials will be promising for multifunctional application. However, previous studies have confined to mix staple carbon nanotube with polymer solutions and fabricate composites with comparatively low volume fraction.In composite design, the morphology and content of reinforcement, and the interface between carbon nanotube and polymer are the main factors to determine the composite property. Thus, this dissertation aims to solve the CNTs dispersion, alignment and interface problems in carbon nanotube reinforced composite by demonstrating the interfacial property using molecular dynamics simulation and plasma treatment method, fabricating CNT composites with ideal structural features and excellent mechanical,thermal and electrical performances, and increasing the understanding of the structure-property relationship in these materials. The detailed studies are described below:
(1)Atmospheric plasma treatment is applied on carbon nanotube, in the form of bucky paper, to improve the interfacial interaction between carbon nanotube and polyimdie. The fabrication of bucky paper is consisted of dissolve, filtration and drying processes, following the plasma treatment and fabrication of composite. The SEM, XPS and static contact angle analysis are conducted to discover the morphology and hydrophilicty change before and after plasma treatment. It is shown that the plasma treatment can effectively "cut off' the heads of CNTs without altering the bulk properties of composite, which increase the nano-mechanical interlocking between CNTs and polymer. Besides, the number of oxygen-containing groups increases and contact angle transfers from hydrophobicity to hydrophilicity. Based on the two mechanisms, the mechanical property of composite is improved distinctly. The tensile fracture surface also shows that less pull-out happens after plasma treatment. And high temperature resistance is retained even after the plasma treatment.
(2) In order to reveal the structure-related property, we adopt a new fabrication method named spray-winding to make carbon nanotube reinforced polyimide composite. Due to the strong Van der Waals between CNTs, the CNT can be pulled out in the form of continuous ribbons, in which CNTs keep oriented and aligned along the longitudinal direction. The unique structure helps the electron and phonon transmission, thus improving the electrical and thermal properties. Compared with the traditional carbon nanotube reinforced composite, this continuous structure not only solves the dispersion and alignment problems, but improve volume fraction to a high level.We further use pre-stretch treatment to improve the alignment and compactness of CNT prepregs, thus obtaining better mechanical, electrical and thermal properties.
(3) To discover the interaction mechanism between carbon nanotube and polyimide, especially in the molecular scale, we need a special tool—molecular dynamics simulation to achieve this goal. Compared with experimental techniques, this computational method is more effective and time-saving. Single chain simulation is firstly to employ to find that the interaction energy between carbon nanotube and polyimide is very high, and this phenomon is also verified in pull-out simulation where co-movement occurs. Limiting pulling force is found in pull-out simualtions, above which the pull-out process can not be achieved. For SWNT and DWNT, the limiting pulling forces are the same value, but for TWNT, it is higher than the SWNT and DWNT. This is due to the inter-tube interactions during pull-out. The interfacial shear strength is calculated to be around5～30MPa which are in the reasonable value among previous experimental and simulation values.
(4) The volume fraction of carbon nanotube is an important factor influencing the properties of composite. How the volume faction affects the polymer chain structure configuration is meaningful in composite design, but no previous study has been done. Therefore, we use molecular dynamics simulation to build composite and polyimide structures separately and invesitigate the polymer configuration change with the increasing of volume fraction. We modify the traditional volume fraction formula and regard the interface as the voids in calculation. Meanwhile, we make "fully crystallized" and "fully amorphous" polyimide structure in simulation and calculate the crystallinity using the rule of mixture. The simulation results are in the agreement with assumption that carbon nanotubes act as the nucleation site in composite.
To sum up, this paper discusses the effective methods to improve the propertyies of carbon nanotube based composite by improving the interface and changing carbon nanotube structure. The molecular dynamics simulation is applied to investigate the micro-scale mechanism of carbon nanotube and polyimide interactions, thus providing valid methods and evidence for composite design and opening up a new vision for nano-reinforced composite studies.
引文
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