碳纳米管/碳纤维多尺度增强体及其复合材料界面研究
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摘要
碳纳米管(CNTs)具有独特的一维管状结构和优异的力学性能,是纤维/晶须类复合材料增强相的终极形式。本文采用化学修饰方法将碳纳米管以化学键连接的形式引入到碳纤维表面,制备出碳纳米管/碳纤维多尺度增强体,并通过实验和分子模拟技术研究了其复合材料的界面性能。
首先研究了多壁碳纳米管的胺基功能化修饰工艺。采用不同的酸体系和处理条件对碳纳米管进行处理,研究了不同酸处理体系及处理条件下的处理效果。结果表明,采用浓硝酸与浓硫酸体积比为3:1的混酸作为酸氧化体系,在100℃水浴加热条件下处理8 h,可以在不损伤碳纳米管基本性能的基础上,在其表面产生大量羧基。羧基功能化的多壁碳纳米管在N,N-二甲基甲酰胺(DMF)溶液中,70℃恒温磁力搅拌作用下,与过量氯化亚砜反应72 h,可将多壁碳纳米管表面的羧基转化为反应活性更高的酰氯基团。并通过取代反应将1,6-己二胺接枝到碳纳米管端部。XPS及IR分析结果表明,碳元素中以C-NHx键形式结合的占碳元素全部结合方式中的6.60%,获得了较好的胺功能化处理效果。
其次,对碳纤维进行了酰氯功能化处理。研究了T300、T800和国产碳纤维(GCF)的酰氯化反应活性。XPS分析结果表明,三种碳纤维酰氯化反应活性大小次序为T300>T800>GCF。浓硝酸氧化后T300表面—COOH含量最高,为14.50%,酰氯化处理后表面Cl元素含量为3.88%;Cl元素与T300样品表面以酰氯共价键形式(O=C-C1)结合。处理后的碳纤维表面微晶尺寸变小,碳纤维棱角和边缘位置的不饱和的碳原子增多,表面活性增大。
再次,通过胺基与酰氯官能团间的取代反应,将碳纳米管接枝到碳纤维表面,制备出新型碳纳米管/碳纤维多尺度增强体,其中碳纳米管含量为1.2wt%。SEM结果表明,碳纳米管以两种方式接枝到碳纤维表面,一种为碳纳米管一端胺基官能团与碳纤维表面酰氯官能团发生亲核取代反应,与纤维轴向以一定角度枝接到碳纤维表面;另一种为碳纳米管两端的胺基官能团分别与两根碳纤维表面的酰氯官能团发生反应,将两根碳纤维连接起来。单纤维树脂微滴复合材料界面评价试验表明,由于在纤维表面引入了碳纳米管,复合材料界面剪切强度较T300提高了150%。探讨了碳纳米管/碳纤维多尺度增强体复合材料界面增效机制,主要为化学键增效机制、范德华力增效机制、浸润作用增效机制和机械啮合作用增效机制。
最后,利用分子模拟方法分别建立了碳纳米管/碳纤维多尺度增强体复合材料界面模型(model 1)和碳纤维复合材料模型(model 2),对其界面结构进行详细分析,从界面结合能的角度研究了碳纳米管/碳纤维多尺度增强体复合材料界面增效机制。模拟计算结果表明,model 1界面作用能较model 2提高了118.28%。其中主要贡献来自于界面间化学键能。非键作用能部分model 1较model 2提高了5.76%。即在不存在化学键合的情况下,影响碳纤维/环氧树脂复合材料界面结合强度的主要因素为范德华力,其次是界面相间的静电作用。结构分析表明,Model 1的接触层厚度大于model 2(分别为0.25 nm、0.10 nm); model 1中碳纤维表面第一、第二和第三层结构发生了不同程度的变化,而第四层结构基本没有发生变化;Model 2中界面作用只是导致碳纤维表面第一和第二层结构发生了变化。model 1中,环氧树脂浓度最大值出现在更靠近接触层附近处,且碳纤维表面沿Z方向0.9172 nm区域内的环氧树脂浓度高于model 2。界面处环氧树脂的浓度分布说明,model 1的界面作用能高于model 2。
Carbon nanotubes (CNTs) with tubular structures and excellent mechanical properties offer a kind of nanosized reinforcement for composite materials. Chemical method was employed to graft CNTs onto the carbon fiber surface to prepare a carbon nanotube/carbon fiber multi-scale reinforcement, and the interfacial properties of its composite were investigated by experiments and molecular simulation.
Firstly, amino functional technics of CNTs were studied. Different acid systems and treatment conditions were used in the modification of CNTs and their functional efficiencies were evaluated. Results shows that sufficient carboxyl could be generated on the surfaces of CNTs without any damage to their properties in the system of nitric and sulphuric acid with a volume ratio of 3:1 in water bath (100℃) for 8 h. The carboxyl could be transformed into carbonyl chloride groups when multi-walled carbon nanotubes (MWCNTs) were put into the solution of DMF and excessive of thionyl chloride at 70℃with magnetic stirring for 72 h. Then hexamethylene diamine were grafted onto the end caps of CNTs. XPS and IR results indicate that there is 6.60% of C-NHx in the surface of CNTs, which suggests that preferable amino functional effect was obtained.
Secondly, acylation functionalization treatment was carried out on carbon fiber surfaces. Surface reactivity of three kinds of carbon fiber, T300, T800 and home-made carbon fiber, were examined by acid treatment followed by acylation reaction with SOCl2. XPS was employed to analyze the surface chemical properties of specimens of acid treatment and acylation reaction. Results indicates that the content of–COOH group, 14.50%, after acid treatment on T300 surface is the maximal, as well as the content of Cl element which is up to 3.88% after acylation reaction, and Cl elements link to the fiber surface by acyl chlorine covalent bond. The crystallite size on treated carbon fiber surfaces decreased and unsaturated carbon atoms of carbon fiber edges and borders increased, leading to more reactive carbon fiber surfaces.
In succession, to prepare a carbon nanotube/carbon fiber multi-scale reinforcement (MSR), MWCNTs functionalized at the end caps with hexamethylene diamine (HMD) are grafted onto the surfaces of carbon fibers treated with acylchloride. It was found that the grafting increases the weight of carbon fiber by 1.2%. SEM shows that MWCNTs were grafted onto carbon fiber surface by two means, one was sticking to the carbon fiber surface at different angles, and the other was that the amino groups at MWCNTs end caps reacted with the acyl chlorides of two carbon fibers respectively and joined them up.
Single fiber polymer matrix droplet composite interfacial evaluation test indicate that the interfacial shearing strength (IFSS) was improved by 150% that that of the as received T300 composite. The mechanisms of the improved IFSS were discussed. It was found that the improved IFSS primarily relies in interfacial chemical bonding, vanderwaals effect, better soakage and mechanical joggling. Finally, interfacial structure models of carbon nanotube/carbon fiber multi-scale reinforcement (Model 1) and carbon fiber composites (Model 2) were established and analyzed respectively by molecular simulation, from which the mechanism of the improved IFSS was examined in view of the interfacial bonding energy. Simulation results indicate that the interfacial bonding energy of model 1 was improved by 118.28% than that of model 2, which was mainly contributed by chemical bond energy. The non-bond interaction of model 1was increased by 5.76% than that of the model 2. It is to say that the primary factor which affects the interfacial bonding strength of carbon fiber/epoxy composite is vanderwaals when there are no chemical bonds exist, and the other is the interfacial static interaction. Structure analyses show that the contact layer thickness of bigger that that of the model 2 (2.5 ?、1.0 ? respectively). The structure of first three layers of the carbon fiber changed in different degree, while the fourth layer remains unchanged. In model 2, only the first and the second layer structures changed at the interfacial interaction. In model 1, the maximum concentration of epoxy presented closer at contact layer and the concentration was higher in the 9.172 ? areas along Z direction than that in model 2. It can be concluded from the concentration distribution of epoxy that the interfacial bonding energy is higher that model 2.
首先研究了多壁碳纳米管的胺基功能化修饰工艺。采用不同的酸体系和处理条件对碳纳米管进行处理,研究了不同酸处理体系及处理条件下的处理效果。结果表明,采用浓硝酸与浓硫酸体积比为3:1的混酸作为酸氧化体系,在100℃水浴加热条件下处理8 h,可以在不损伤碳纳米管基本性能的基础上,在其表面产生大量羧基。羧基功能化的多壁碳纳米管在N,N-二甲基甲酰胺(DMF)溶液中,70℃恒温磁力搅拌作用下,与过量氯化亚砜反应72 h,可将多壁碳纳米管表面的羧基转化为反应活性更高的酰氯基团。并通过取代反应将1,6-己二胺接枝到碳纳米管端部。XPS及IR分析结果表明,碳元素中以C-NHx键形式结合的占碳元素全部结合方式中的6.60%,获得了较好的胺功能化处理效果。
其次,对碳纤维进行了酰氯功能化处理。研究了T300、T800和国产碳纤维(GCF)的酰氯化反应活性。XPS分析结果表明,三种碳纤维酰氯化反应活性大小次序为T300>T800>GCF。浓硝酸氧化后T300表面—COOH含量最高,为14.50%,酰氯化处理后表面Cl元素含量为3.88%;Cl元素与T300样品表面以酰氯共价键形式(O=C-C1)结合。处理后的碳纤维表面微晶尺寸变小,碳纤维棱角和边缘位置的不饱和的碳原子增多,表面活性增大。
再次,通过胺基与酰氯官能团间的取代反应,将碳纳米管接枝到碳纤维表面,制备出新型碳纳米管/碳纤维多尺度增强体,其中碳纳米管含量为1.2wt%。SEM结果表明,碳纳米管以两种方式接枝到碳纤维表面,一种为碳纳米管一端胺基官能团与碳纤维表面酰氯官能团发生亲核取代反应,与纤维轴向以一定角度枝接到碳纤维表面;另一种为碳纳米管两端的胺基官能团分别与两根碳纤维表面的酰氯官能团发生反应,将两根碳纤维连接起来。单纤维树脂微滴复合材料界面评价试验表明,由于在纤维表面引入了碳纳米管,复合材料界面剪切强度较T300提高了150%。探讨了碳纳米管/碳纤维多尺度增强体复合材料界面增效机制,主要为化学键增效机制、范德华力增效机制、浸润作用增效机制和机械啮合作用增效机制。
最后,利用分子模拟方法分别建立了碳纳米管/碳纤维多尺度增强体复合材料界面模型(model 1)和碳纤维复合材料模型(model 2),对其界面结构进行详细分析,从界面结合能的角度研究了碳纳米管/碳纤维多尺度增强体复合材料界面增效机制。模拟计算结果表明,model 1界面作用能较model 2提高了118.28%。其中主要贡献来自于界面间化学键能。非键作用能部分model 1较model 2提高了5.76%。即在不存在化学键合的情况下,影响碳纤维/环氧树脂复合材料界面结合强度的主要因素为范德华力,其次是界面相间的静电作用。结构分析表明,Model 1的接触层厚度大于model 2(分别为0.25 nm、0.10 nm); model 1中碳纤维表面第一、第二和第三层结构发生了不同程度的变化,而第四层结构基本没有发生变化;Model 2中界面作用只是导致碳纤维表面第一和第二层结构发生了变化。model 1中,环氧树脂浓度最大值出现在更靠近接触层附近处,且碳纤维表面沿Z方向0.9172 nm区域内的环氧树脂浓度高于model 2。界面处环氧树脂的浓度分布说明,model 1的界面作用能高于model 2。
Carbon nanotubes (CNTs) with tubular structures and excellent mechanical properties offer a kind of nanosized reinforcement for composite materials. Chemical method was employed to graft CNTs onto the carbon fiber surface to prepare a carbon nanotube/carbon fiber multi-scale reinforcement, and the interfacial properties of its composite were investigated by experiments and molecular simulation.
Firstly, amino functional technics of CNTs were studied. Different acid systems and treatment conditions were used in the modification of CNTs and their functional efficiencies were evaluated. Results shows that sufficient carboxyl could be generated on the surfaces of CNTs without any damage to their properties in the system of nitric and sulphuric acid with a volume ratio of 3:1 in water bath (100℃) for 8 h. The carboxyl could be transformed into carbonyl chloride groups when multi-walled carbon nanotubes (MWCNTs) were put into the solution of DMF and excessive of thionyl chloride at 70℃with magnetic stirring for 72 h. Then hexamethylene diamine were grafted onto the end caps of CNTs. XPS and IR results indicate that there is 6.60% of C-NHx in the surface of CNTs, which suggests that preferable amino functional effect was obtained.
Secondly, acylation functionalization treatment was carried out on carbon fiber surfaces. Surface reactivity of three kinds of carbon fiber, T300, T800 and home-made carbon fiber, were examined by acid treatment followed by acylation reaction with SOCl2. XPS was employed to analyze the surface chemical properties of specimens of acid treatment and acylation reaction. Results indicates that the content of–COOH group, 14.50%, after acid treatment on T300 surface is the maximal, as well as the content of Cl element which is up to 3.88% after acylation reaction, and Cl elements link to the fiber surface by acyl chlorine covalent bond. The crystallite size on treated carbon fiber surfaces decreased and unsaturated carbon atoms of carbon fiber edges and borders increased, leading to more reactive carbon fiber surfaces.
In succession, to prepare a carbon nanotube/carbon fiber multi-scale reinforcement (MSR), MWCNTs functionalized at the end caps with hexamethylene diamine (HMD) are grafted onto the surfaces of carbon fibers treated with acylchloride. It was found that the grafting increases the weight of carbon fiber by 1.2%. SEM shows that MWCNTs were grafted onto carbon fiber surface by two means, one was sticking to the carbon fiber surface at different angles, and the other was that the amino groups at MWCNTs end caps reacted with the acyl chlorides of two carbon fibers respectively and joined them up.
Single fiber polymer matrix droplet composite interfacial evaluation test indicate that the interfacial shearing strength (IFSS) was improved by 150% that that of the as received T300 composite. The mechanisms of the improved IFSS were discussed. It was found that the improved IFSS primarily relies in interfacial chemical bonding, vanderwaals effect, better soakage and mechanical joggling. Finally, interfacial structure models of carbon nanotube/carbon fiber multi-scale reinforcement (Model 1) and carbon fiber composites (Model 2) were established and analyzed respectively by molecular simulation, from which the mechanism of the improved IFSS was examined in view of the interfacial bonding energy. Simulation results indicate that the interfacial bonding energy of model 1 was improved by 118.28% than that of model 2, which was mainly contributed by chemical bond energy. The non-bond interaction of model 1was increased by 5.76% than that of the model 2. It is to say that the primary factor which affects the interfacial bonding strength of carbon fiber/epoxy composite is vanderwaals when there are no chemical bonds exist, and the other is the interfacial static interaction. Structure analyses show that the contact layer thickness of bigger that that of the model 2 (2.5 ?、1.0 ? respectively). The structure of first three layers of the carbon fiber changed in different degree, while the fourth layer remains unchanged. In model 2, only the first and the second layer structures changed at the interfacial interaction. In model 1, the maximum concentration of epoxy presented closer at contact layer and the concentration was higher in the 9.172 ? areas along Z direction than that in model 2. It can be concluded from the concentration distribution of epoxy that the interfacial bonding energy is higher that model 2.
引文
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