PA6/MWNTs复合纳米纤维纱连续静电纺丝的研究
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摘要
碳纳米管(CNTs)自1991年被发现以来,虽然只有短短20年,但由于其具有良好的电磁性能、力学性能和传热性能,在很多领域都得到了广泛应用。如:利用碳纳米管的高强度、优良的韧性和弹性模量,将其作为复合材料的增强体;利用其较好的宽频宽带吸收特性,用来制备吸波和屏蔽材料;利用其具有弹性高、密度低、强度高、隐身性优越、红外吸收性好、疏水性强等优点,与普通纤维混纺制成防弹衣等。
静电纺丝是制备纳米纤维最基本、最方便的方法之一,随着静电纺丝技术的发展,研究人员开始致力于将碳纳米管与静电纺丝技术相结合,试图制备出具有优良性能的纳米复合材料。当人们发现碳纳米管可在静电纺纤维中较好地沿着纤维轴向定向排列时,就更加热衷于利用静电纺丝技术制备聚合物/CNTs纳米复合纤维。目前,研究人员已经将PAN、PVA、PEO、PMMA、PA6、PBT、PLA和丝素等多种聚合物与单壁碳纳米管(SWNTs)或多壁碳纳米管(MWNTs)进行复合静电纺丝,但是所有产品基本都是纤维呈随机排列的非织造布,美国的Frangk Ko教授用静电纺丝的方法得到了PAN/SWNTs纱,少量以滚筒法和双电极法等制备的纤维束长度仅为数米或者数十厘米,没有实现类似于化学纤维纺丝的连续卷绕成筒。
为了实现高聚物/MWNTs复合纳米纤维纱的连续静电纺丝,本文将静电纺丝结合纤维在活性浴液中集束、一步法热拉伸定型、连续卷绕等技术,成功地实现了连续纺制PA6/MWNTs复合纳米纤维纱。并在此基础上,系统地探讨并优化了纺丝工艺参数,使连续纺制PA6/MWNTs复合纳米纤维纱技术具有更好的稳定性和可控性,真正实现了高聚物/MWNTs的连续静电纺丝。
本文在实现连续纺制PA6/MWNTs复合纳米纤维纱的基础上,还研究了纺丝工艺参数对纤维及纱线结构与性能的影响机理。同时,还探索了两种后加工技术(干热拉伸和湿热拉伸),改善了纱线的结构和性能。最后,本文还研究了PA6/MWNTs纳米纤维中MWNTs的分布及排列情况,以及纱线的导电性能。
研究表明在纺丝电压为18-20KV、纺丝高度为6cm、纺丝溶液中MWNTs质量百分数为0~3%、PA6质量百分数为25%、卷绕速度为1.80m/min ~12.6 m/min、0.5wt%的平平加O溶液作为收集浴液时,能实现PA6/MWNTs纳米纤维纱的稳定、连续静电纺丝。
纺丝电压、纺丝高度、MWNTs的含量、卷绕速度等都对PA6/MWNTs复合纳米纤维纱的结构与性能有很大的影响。随着纺丝电压的增大,PA6/MWNTs纳米纤维纱的直径、纤维结晶度、断裂强力增加;随着纺丝高度的增加,纤维的定向排列程度提高,结晶度增大,纤维直径先增大后减小,纱线直径逐渐减小,纱线的断裂强度和初始模量增加,断裂伸长率呈先增加后减小的变化;场强相同时,在高电压和高纺丝高度下,纤维的平行排列程度高,纱线的断裂强力、断裂伸长率、初始模量和断裂强度较大;纺丝溶液中MWNTs的质量百分数在0.4%-0.80%(纤维中MWNTs的质量百分数为1.57%-3.1%)时,随着MWNTs含量的增加,纱线的断裂强度和模量逐渐增加,伸长减小,当MWNTs质量百分数超过0.80%时,纱线的断裂强度随着MWNTs含量的增加反而减小;纺丝卷绕速度对纱线的力学性能的影响以9.00m/min为临界点,在1.80~9.00m/min之间,纱线的断裂强度和模量随速度的增加而增加,当速度超过9.00m/min时,纱线断裂强度反而有所下降。
在纱线的后加工过程中,干热拉伸的最大倍数可以达到1.6,湿热拉伸的最大倍数可以达到1.7。二者都能提高纱线的断裂强度和初始模量,拉伸倍数越高,纱线断裂强度和初始模量越大。干热拉伸后的纳米纤维纱断裂强度和初始模量分别可以达到初纺纱的2.47和2.35倍,湿热拉伸后的纳米纤维纱断裂强度和初始模量分别可以达到初纺纱的2.64和4.20倍。在改善PA6/MWNTs复合纳米纤维纱的力学性能方面,湿热拉伸的效果优于干热拉伸。MWNTs在PA6/MWNTs纳米纤维中呈现良好的排列,当MWNTs含量较高时会出现团聚现象,纱线的电导率随着MWNTs含量的增加而增加,所纺制的PA6/MWNTs纳米纤维纱比纯PA6纤维电导率提高了6个数量级。
通过本课题的研究在国内外首次实现了PA6/MWNTs纳米纤维纱的连续纺制,打破了静电纺纤维制品只能呈现无规则取向的局限,为连续静电纺制高聚物/MWNTs连续纳米纤维纱奠定了理论和实践基础。同时通过干热拉伸和湿热拉伸等二次加工技术,改善了纱线的力学性能,为提高静电纺复合纳米纤维纱力学性能提供了一条新的途径。通过研究MWNTs在静电纺高聚物/MWNTs纳米纤维中的排列及其对纱线电导率的影响,为制备导电纳米纤维也提供了一种全新的方法。
Carbon nanotube (CNTs), which possesses excellent electromagnetic and mechanical properties as well as famous thermo conductive property, has attracted tremendous attention from its discovery in 1991. It has been used as a kind of reinforcement for its outstanding strength, excellent toughness and modulus of elasticity. It also can be used to prepare absorbing and shielding materials for its famous broadband absorbing character. Besides that, some researchers blended it with common fibers to produce bullet-proof vests for its high flexibility, low density, famous thermo conductive property, outstanding mechanical property, well infrared absorption and hydrophobic properties.
Electrospinning is one of the most basic and convenient method to produce nanofibers, with the development of this technology, researchers began to focus on CNTs combined with electrospinning technology, try to prepare nanocomposite with excellent performance, especially when they found that CNTs can array along with the axis of the nanofiber. Presently, researchers have prepared PAN, PVA, PEO, PMMA, PA6, PBT and PLA with MWNTs or SWNTs nanofibers by electrospinning, however, most of the products by electrospinning are porous nonwovens with randomly oriented nanofiber. Prof. Frangk Ko obtained PAN/SWNTs nanofiber filaments by electrospinning, some researchers used rotate drum or double electrodes as the negative electrode obtained nanofiber filaments, whereas the length is only about several meters or even centimeters, it cannot successively rotated up like synthetic fiber spinning.
In order to obtain Polymer/MWNTs nanofiber filament, we combine electrospinning method with bundling in the bath, heat setting by one-step stretch and successive rotation etc. technology, finally we successful gained consecutive PA6/MWNTs nanofiber filament. After that, we systematically discussed and optimized the parameters of the spinning process and make this method more stable and controllable.
In this paper, we studied the impact mechanism of the parameters of the spinning process on the structure and properties of nanofiber filament and discovered two kinds of post-processing technology(wet post-draw and dry post-draw) to optimize the structure and properties of the filament. In the end, we discussed the microstructure and the arrangement of MWNTs in the nanofibers both with the conductivities of the filaments.
The results show that when the spinning voltage was 18-20KV, the spinning distance was 6cm, the contents of MWNTs and PA6 were 0-3% and 25% respectively, the rotating speed was 1.80m/min ~12.6 m/min and use 0.5wt% peregal O aqueous solution as collection bath, the spinning process would be stable and successive.
There are strong affections on the structure and properties of PA6/MWNTs nanofiber filaments by the concentrations of MWNTs, the spinning voltage, spinning distance and rotating speed. The diameters, degree of crystalline and breaking stress of the PA6/MWNTs nanofiber filaments improved according with the increase of the spinning voltage, the alignment property of the filaments and the degree of crystalline improved, the diameters of the fibers increased firstly and then decreased while the diameters of the filaments decreased, the breaking stress and initial module enhanced while the breaking strain increased firstly and the decreased according with the increase of the spinning distance. The alignment and mechanical properties of the nanofiber filament are much better in the higher spinning voltage and spinning distance when the strength of the electrical field is homology. The results also show that when the concentrations of MWNTs varied between 0.4wt%-0.8 wt%(1.57wt%-3.1wt% in the nanofiber), the increase of MWNTs content enhances the initial modules and breaking stress but reduces the breaking strain, while the breaking stress decreases when the MWNTs concentration exceeds 0.8 wt %. The initial modules and breaking stress increased as the the spinning speed raised at the range of 1.8-9.0m/min, but declined when the speed exceeded 9.0m/min.
The mechanical properties of the as-spun filaments can be improved by either dry or wet post-drawing, the maximum dry and wet post-drawn ratios are 1.6 and 1.7 respectively. The mechanical property of the filament improved much more with the increase of the post-drawn ratios and the enhancement effect on the filaments by wet post-drawing is better than that dry post-drawing. The breaking stress and initial modules of the nanofiber filaments can reach 2.47 and 2.35 times respectively compared to the as-spun yarns after dry post-drawing, while 2.64 and 4.20 times increased after wet post-drawing.
MWNTs can array properly in the PA6/MWNTs nanofibers but united together when the contents of it overtop its limit. The conductivity of the filaments improved according with the contents of MWNTs increased. In this study, we successfully improved the conductivity of PA6/MWNTs nanofiber filaments by 6 orders compared to the pure PA6 nanofiber filaments.
The study of this paper firstly make consecutive PA6/MWNTs nanofiber filaments come true at home and abroad which break the restriction that electrospinning composite materials can only present as nonwovens with randomly oriented nanofibers, it established the theoretical and practical basis for preparing MWNTs/polymer nanofiber filaments by electrospinning. In the same time, we improved the mechanical property of the filament by dry or wet post-drawn and other post processing methods which provide a new way to enhance the mechanical property of nanocomposite fibers by electrospinning. Apart from that, We discussed the microstructure and the arrangement of MWNTs in the nanofibers both with the conductivities of the filaments, it also offered a unique technical to produce conductive nanofiber.
静电纺丝是制备纳米纤维最基本、最方便的方法之一,随着静电纺丝技术的发展,研究人员开始致力于将碳纳米管与静电纺丝技术相结合,试图制备出具有优良性能的纳米复合材料。当人们发现碳纳米管可在静电纺纤维中较好地沿着纤维轴向定向排列时,就更加热衷于利用静电纺丝技术制备聚合物/CNTs纳米复合纤维。目前,研究人员已经将PAN、PVA、PEO、PMMA、PA6、PBT、PLA和丝素等多种聚合物与单壁碳纳米管(SWNTs)或多壁碳纳米管(MWNTs)进行复合静电纺丝,但是所有产品基本都是纤维呈随机排列的非织造布,美国的Frangk Ko教授用静电纺丝的方法得到了PAN/SWNTs纱,少量以滚筒法和双电极法等制备的纤维束长度仅为数米或者数十厘米,没有实现类似于化学纤维纺丝的连续卷绕成筒。
为了实现高聚物/MWNTs复合纳米纤维纱的连续静电纺丝,本文将静电纺丝结合纤维在活性浴液中集束、一步法热拉伸定型、连续卷绕等技术,成功地实现了连续纺制PA6/MWNTs复合纳米纤维纱。并在此基础上,系统地探讨并优化了纺丝工艺参数,使连续纺制PA6/MWNTs复合纳米纤维纱技术具有更好的稳定性和可控性,真正实现了高聚物/MWNTs的连续静电纺丝。
本文在实现连续纺制PA6/MWNTs复合纳米纤维纱的基础上,还研究了纺丝工艺参数对纤维及纱线结构与性能的影响机理。同时,还探索了两种后加工技术(干热拉伸和湿热拉伸),改善了纱线的结构和性能。最后,本文还研究了PA6/MWNTs纳米纤维中MWNTs的分布及排列情况,以及纱线的导电性能。
研究表明在纺丝电压为18-20KV、纺丝高度为6cm、纺丝溶液中MWNTs质量百分数为0~3%、PA6质量百分数为25%、卷绕速度为1.80m/min ~12.6 m/min、0.5wt%的平平加O溶液作为收集浴液时,能实现PA6/MWNTs纳米纤维纱的稳定、连续静电纺丝。
纺丝电压、纺丝高度、MWNTs的含量、卷绕速度等都对PA6/MWNTs复合纳米纤维纱的结构与性能有很大的影响。随着纺丝电压的增大,PA6/MWNTs纳米纤维纱的直径、纤维结晶度、断裂强力增加;随着纺丝高度的增加,纤维的定向排列程度提高,结晶度增大,纤维直径先增大后减小,纱线直径逐渐减小,纱线的断裂强度和初始模量增加,断裂伸长率呈先增加后减小的变化;场强相同时,在高电压和高纺丝高度下,纤维的平行排列程度高,纱线的断裂强力、断裂伸长率、初始模量和断裂强度较大;纺丝溶液中MWNTs的质量百分数在0.4%-0.80%(纤维中MWNTs的质量百分数为1.57%-3.1%)时,随着MWNTs含量的增加,纱线的断裂强度和模量逐渐增加,伸长减小,当MWNTs质量百分数超过0.80%时,纱线的断裂强度随着MWNTs含量的增加反而减小;纺丝卷绕速度对纱线的力学性能的影响以9.00m/min为临界点,在1.80~9.00m/min之间,纱线的断裂强度和模量随速度的增加而增加,当速度超过9.00m/min时,纱线断裂强度反而有所下降。
在纱线的后加工过程中,干热拉伸的最大倍数可以达到1.6,湿热拉伸的最大倍数可以达到1.7。二者都能提高纱线的断裂强度和初始模量,拉伸倍数越高,纱线断裂强度和初始模量越大。干热拉伸后的纳米纤维纱断裂强度和初始模量分别可以达到初纺纱的2.47和2.35倍,湿热拉伸后的纳米纤维纱断裂强度和初始模量分别可以达到初纺纱的2.64和4.20倍。在改善PA6/MWNTs复合纳米纤维纱的力学性能方面,湿热拉伸的效果优于干热拉伸。MWNTs在PA6/MWNTs纳米纤维中呈现良好的排列,当MWNTs含量较高时会出现团聚现象,纱线的电导率随着MWNTs含量的增加而增加,所纺制的PA6/MWNTs纳米纤维纱比纯PA6纤维电导率提高了6个数量级。
通过本课题的研究在国内外首次实现了PA6/MWNTs纳米纤维纱的连续纺制,打破了静电纺纤维制品只能呈现无规则取向的局限,为连续静电纺制高聚物/MWNTs连续纳米纤维纱奠定了理论和实践基础。同时通过干热拉伸和湿热拉伸等二次加工技术,改善了纱线的力学性能,为提高静电纺复合纳米纤维纱力学性能提供了一条新的途径。通过研究MWNTs在静电纺高聚物/MWNTs纳米纤维中的排列及其对纱线电导率的影响,为制备导电纳米纤维也提供了一种全新的方法。
Carbon nanotube (CNTs), which possesses excellent electromagnetic and mechanical properties as well as famous thermo conductive property, has attracted tremendous attention from its discovery in 1991. It has been used as a kind of reinforcement for its outstanding strength, excellent toughness and modulus of elasticity. It also can be used to prepare absorbing and shielding materials for its famous broadband absorbing character. Besides that, some researchers blended it with common fibers to produce bullet-proof vests for its high flexibility, low density, famous thermo conductive property, outstanding mechanical property, well infrared absorption and hydrophobic properties.
Electrospinning is one of the most basic and convenient method to produce nanofibers, with the development of this technology, researchers began to focus on CNTs combined with electrospinning technology, try to prepare nanocomposite with excellent performance, especially when they found that CNTs can array along with the axis of the nanofiber. Presently, researchers have prepared PAN, PVA, PEO, PMMA, PA6, PBT and PLA with MWNTs or SWNTs nanofibers by electrospinning, however, most of the products by electrospinning are porous nonwovens with randomly oriented nanofiber. Prof. Frangk Ko obtained PAN/SWNTs nanofiber filaments by electrospinning, some researchers used rotate drum or double electrodes as the negative electrode obtained nanofiber filaments, whereas the length is only about several meters or even centimeters, it cannot successively rotated up like synthetic fiber spinning.
In order to obtain Polymer/MWNTs nanofiber filament, we combine electrospinning method with bundling in the bath, heat setting by one-step stretch and successive rotation etc. technology, finally we successful gained consecutive PA6/MWNTs nanofiber filament. After that, we systematically discussed and optimized the parameters of the spinning process and make this method more stable and controllable.
In this paper, we studied the impact mechanism of the parameters of the spinning process on the structure and properties of nanofiber filament and discovered two kinds of post-processing technology(wet post-draw and dry post-draw) to optimize the structure and properties of the filament. In the end, we discussed the microstructure and the arrangement of MWNTs in the nanofibers both with the conductivities of the filaments.
The results show that when the spinning voltage was 18-20KV, the spinning distance was 6cm, the contents of MWNTs and PA6 were 0-3% and 25% respectively, the rotating speed was 1.80m/min ~12.6 m/min and use 0.5wt% peregal O aqueous solution as collection bath, the spinning process would be stable and successive.
There are strong affections on the structure and properties of PA6/MWNTs nanofiber filaments by the concentrations of MWNTs, the spinning voltage, spinning distance and rotating speed. The diameters, degree of crystalline and breaking stress of the PA6/MWNTs nanofiber filaments improved according with the increase of the spinning voltage, the alignment property of the filaments and the degree of crystalline improved, the diameters of the fibers increased firstly and then decreased while the diameters of the filaments decreased, the breaking stress and initial module enhanced while the breaking strain increased firstly and the decreased according with the increase of the spinning distance. The alignment and mechanical properties of the nanofiber filament are much better in the higher spinning voltage and spinning distance when the strength of the electrical field is homology. The results also show that when the concentrations of MWNTs varied between 0.4wt%-0.8 wt%(1.57wt%-3.1wt% in the nanofiber), the increase of MWNTs content enhances the initial modules and breaking stress but reduces the breaking strain, while the breaking stress decreases when the MWNTs concentration exceeds 0.8 wt %. The initial modules and breaking stress increased as the the spinning speed raised at the range of 1.8-9.0m/min, but declined when the speed exceeded 9.0m/min.
The mechanical properties of the as-spun filaments can be improved by either dry or wet post-drawing, the maximum dry and wet post-drawn ratios are 1.6 and 1.7 respectively. The mechanical property of the filament improved much more with the increase of the post-drawn ratios and the enhancement effect on the filaments by wet post-drawing is better than that dry post-drawing. The breaking stress and initial modules of the nanofiber filaments can reach 2.47 and 2.35 times respectively compared to the as-spun yarns after dry post-drawing, while 2.64 and 4.20 times increased after wet post-drawing.
MWNTs can array properly in the PA6/MWNTs nanofibers but united together when the contents of it overtop its limit. The conductivity of the filaments improved according with the contents of MWNTs increased. In this study, we successfully improved the conductivity of PA6/MWNTs nanofiber filaments by 6 orders compared to the pure PA6 nanofiber filaments.
The study of this paper firstly make consecutive PA6/MWNTs nanofiber filaments come true at home and abroad which break the restriction that electrospinning composite materials can only present as nonwovens with randomly oriented nanofibers, it established the theoretical and practical basis for preparing MWNTs/polymer nanofiber filaments by electrospinning. In the same time, we improved the mechanical property of the filament by dry or wet post-drawn and other post processing methods which provide a new way to enhance the mechanical property of nanocomposite fibers by electrospinning. Apart from that, We discussed the microstructure and the arrangement of MWNTs in the nanofibers both with the conductivities of the filaments, it also offered a unique technical to produce conductive nanofiber.
引文
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