气泡静电纺产品成形机理及增韧应用研究
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摘要
纳米纤维是指直径小于100nm,长径比大于100的一维韧性固体材料。由于拥有高比表面积、高表面反应活性、高孔隙率、优良的热导与电导性能等诸多优点,纳米纤维在生物医用、催化过滤、传感器、复合材料等方面取得了广泛应用。相比于其他微米、纳米纤维的制备方法,静电纺丝是最直接、最有效的制备工艺,然而纤维细度较粗、副产品较多、产量较低等缺陷遏制了静电纺丝规模化、工业化的进程。为克服传统静电纺丝的发展瓶颈,气泡静电纺丝工艺应运而生。基于自然界蜘蛛纺丝的原理,气泡静电纺丝将气泡巧妙地引入纺丝过程,实现了优质高效地制备纳米纤维。
本文从纺丝的工艺参数着手,分别研究了纺丝电压、接收距离以及气体流量对纺丝过程中气泡、射流及产品的影响,着重讨论了电压的作用。借助标度律法、N-S方程对电场中的粘性气泡进行分析,得到电压与纤维直径存在：d=[α(V-V0)]-1/4的函数关系,即d∝V1/4。揭示出电压越高,气泡静电纺纤维直径越小。进行实验验证,发现该规律与实验数据能够很好的吻合。然后,讨论了接收距离的改变对纤维细度的影响。发现接收距离增大,纤维总体细度下降,在8cm时纤维的平均直径与最小直径同时优化,分别为100nm和36nm。在对气体流量的研究中得出：流量增大,纤维的直径先增大后减小,纺丝产量大有提高,但纤维形貌变差。当流量为0.4L/min时,平均直径和最小直径达到最小,分别为97nm和50nm。
溶液性能是最能影响气泡特性的参数集合。本文分别从溶液的粘度(浓度、分子量)、电导率、表面张力、溶剂等方面出发,讨论工艺过程与产品结构的变化,其中着重讨论了粘度的作用。运用标度律法分别讨论了粘度、浓度、直径三者之间的函数关系。通过PLA/DMF纺丝实验,得到溶液粘度与浓度存在关系：η∝c3,直径与浓度的关系为：d∝c2,于是推导出直径与粘度的关系满足：d∝η2/3。将粘度与纤维直径为坐标的函数点进行曲线拟合,得到函数关系：d∝η0.667,与理论推导结果完全吻合,由此可根据该关系对纤维产品进行调控。通过添加无机盐LiCl改善PLA/DMF的导电性能,发现随着电导率的增大,纤维形貌得到有效改善。但由于溶解度有限,溶解过饱和后电导率值恒定,再增大添加量反而导致产品形貌恶化。对表面张力的研究发现：添加非离子表面活性剂Span20的纺丝液粘度大幅降低,表面张力变化不大,导电率基本不变,纺丝产品只有微珠,无益于纺丝性能的改善。并通过将具有不同挥发性能的溶剂(二氯甲烷与N,N-二甲基甲酰胺)配比后配制纺丝液,可以制备表面多孔纳米纤维。
电场中气泡与射流的动力学特征是本文研究的核心内容。使用高速摄影仪拍摄出电场中气泡的变形过程,计算并证明了气泡泰勒锥的临界半锥角为33.02°。运用达朗贝尔原理研究了电场中射流的方向性运动,阐明气泡膜破碎边缘形成“脖颈”形态的力学成因。根据量纲分析法并运用Π定理,得到射流初始速度与气泡膜厚度的关系：(V是初始速度,FE为电场力,h气泡膜的厚度,ρ为溶液的密度,σ为表面张力),进一步根据能量法推导出：V=λ/h(λ为常数,λ=λFE1/2ρ-1/2)。说明气泡膜的厚度决定射流的速度,证明了气泡静电纺丝过程多重射流的产生部位位于气泡的上半部分。讨论了气泡静电纺的产品成形规律：(1)当气泡膜的雷诺数满足气泡破碎形成子气泡及层级射流,纺丝产品由一级或二级射流以及膜碎片形成。(2)气泡膜在电场中撕裂出宽度为a的矩形膜：当a→h,纺丝产品为球形微珠,微球直径满足d=6h；(3)当a/h=4π,纺丝产品为截面圆形的柱状纤维,纤维直径满足d=4h；(4)当a>>h,形成扁平的带状纤维。
本文将板壳振动理论引入产品成形分析。将撕裂出的矩形气泡膜视为矩形薄板,依据Rayleigh (?)去计算出薄板的固有频率为：(D为刚度)。于是,当h/a2< 借助流体力学软件Fluent进一步研究射流的动力学行为。通过模拟出纯电场的空间分布,有、无电场作用时射流的运动特性。并通过捕捉射流迹线图,以及纺丝实验验证,证实了气泡静电纺丝的射流也存在运动不稳定性。
最后,本文对气泡静电纺纳米纤维膜的应用进行了初步探索。利用热塑性塑料优越的力学性能和纳米纤维膜高比表面积、高孔隙率的特性,制备不同厚度的聚醚酰亚胺纳米纤维膜改善碳纤维复合材料的层间韧性。发现不同膜厚度增韧的双悬臂梁(DCB)试件的Ⅰ型层间断裂值(GIc)均有所提高,特别是膜厚为0.058±0.007mm时,层合板的增韧效果最好,比未增韧试件提高了114.55%；特别是当裂纹长度a=100mm时,GIC值提高了211.27%。而通过界面的SEM照片证实了纳米纤维膜在层间界面通过桥联约束效应及钉锚作用有效提高了复合材料的层间断裂韧性。
Nanofibers are defined as ductile materials with diameter less than100nm and length diameter ration more than100. Nowadays, nanofibers could be comprehensively applied to bio-technology, environment, energy, medical treatment, filtration, sensor and other industries. Electrospinning, as one simple and straightforward fabrication process, is widely adopted. Whereas, the drawbacks in fibers output and fineness to some extent impose restrictions on the future development of Electrospinning. To get rid of those problems, based on the mechanism of spider spinning, Bubble-electrospinning applies viscous bubbles into electrospinning process to prepare nanofibers with high quality and efficiency. It is a fantastic technique, which can impove the output and reduce the fibers fineness effectively.
In this research, in the beginning we discuss the effects of operating parameters(such as voltage, collecting distance, flow rate) and the solution property(such as viscosity, conductivity, surface tension, solvent volatility) on the bubble deformation process, the movement of jets and the morphology of as-spun nanofibers. The effects of voltage and solution viscosity are focused to be analyzed. The scaling laws about fiber diameter and voltage:d∝V4, and fiber diameter and viscosity:d∝η2/3, are respectively deduced. And both of their accuracies are confirmed by the experiment results.
The dynamics characteristics of bubble and charged jets in the electric field are the core content of this thesis. The bubble rupture process is filmed by high speed camera. Accordingly, The half angle of taylor cone measured is33.02°, which is coincided with the theoretical value that is caculated theoretically. We analyze the directional motion of jets using d'Alembert principle, and discussed the reason why the rim of bubble forms neck-like configuration. Then, using dimension analysis, we obtain the relation between the initial velocity of a debris with the film thickness, which reads where FE is the electronic force, ρ is the liquid density and h is the film thickness. The constants λ and β can be determined by experiments. As a result, the initial velocity can be obtained by an energy approach. It can be predicted that smaller thickness results in a larger ejection velocity, this is the reasons why multiple jets from upper half of the bubble, because the upper half has smaller h than that of the bottom half. Through the analysis and discussions in detail, a law on the bubble-electrospun production formation is concluded:In case the ruptured film retracts to be daughter bubbles. The daughter bubbles may continues to be broken to form sub-daughter bubbles, and the process repeats until some a hierarchical ruptured bubble is pulled upwards to form a charged jet, nanofibers are obtained; when the thickness and the width of the jet satisfies h/a=4π,fibers are bubble-electrospun with diameter of4h; and when a→h, the thickness scales with the width, micro-spheres can be found.
Furthermore, oscillation theory is introduced to elaborate the nanofibers shaping mechanism. A short strip sticked to a large piece of a ruptured film is formed, which is regarded as a thin rectangular plate. The plate's natural frequency fn can be caculated by Rayleigh's method approximately: In case far from the natural frequency, no pulsation occurs, and continuous strip-like fibers can be obtained; when h/a2≌fn/k, the plate pulsates (that is, they oscillate in size) at its natural frequency Consequently backbone-like fibers are formed. In case fe≌fn, the frequency of external excitation fe is close to fn, the plate resonates at the same time absorbs energy from external surroundings to maximum extent. The plate can't afford that, and then plate texture is damaged, micro-spheres are likely to be formed.
With the aid of Fluent software, the space distribution of electric field is demonstrated vividly. And the jet motion is simulated under the circumstance whether the electric field exsits or not. The velocity contours show the bending instability happens when the jet flies to the collector. And this phenomenon can be verified from the optical photos of spinning process.
At last, the application of bubble-electrospun nanofibers is explored. PEI nanofibers mebranes are used to improve the interfacial toughness of the carbon fiber reinforced composites. When the thickness of membrane is0.058±0.007mm, the value of GIC of DCB sample increases by114.55%in contrast to the untoughened, which is attributed to the nail-anchorage action.
本文从纺丝的工艺参数着手,分别研究了纺丝电压、接收距离以及气体流量对纺丝过程中气泡、射流及产品的影响,着重讨论了电压的作用。借助标度律法、N-S方程对电场中的粘性气泡进行分析,得到电压与纤维直径存在：d=[α(V-V0)]-1/4的函数关系,即d∝V1/4。揭示出电压越高,气泡静电纺纤维直径越小。进行实验验证,发现该规律与实验数据能够很好的吻合。然后,讨论了接收距离的改变对纤维细度的影响。发现接收距离增大,纤维总体细度下降,在8cm时纤维的平均直径与最小直径同时优化,分别为100nm和36nm。在对气体流量的研究中得出：流量增大,纤维的直径先增大后减小,纺丝产量大有提高,但纤维形貌变差。当流量为0.4L/min时,平均直径和最小直径达到最小,分别为97nm和50nm。
溶液性能是最能影响气泡特性的参数集合。本文分别从溶液的粘度(浓度、分子量)、电导率、表面张力、溶剂等方面出发,讨论工艺过程与产品结构的变化,其中着重讨论了粘度的作用。运用标度律法分别讨论了粘度、浓度、直径三者之间的函数关系。通过PLA/DMF纺丝实验,得到溶液粘度与浓度存在关系：η∝c3,直径与浓度的关系为：d∝c2,于是推导出直径与粘度的关系满足：d∝η2/3。将粘度与纤维直径为坐标的函数点进行曲线拟合,得到函数关系：d∝η0.667,与理论推导结果完全吻合,由此可根据该关系对纤维产品进行调控。通过添加无机盐LiCl改善PLA/DMF的导电性能,发现随着电导率的增大,纤维形貌得到有效改善。但由于溶解度有限,溶解过饱和后电导率值恒定,再增大添加量反而导致产品形貌恶化。对表面张力的研究发现：添加非离子表面活性剂Span20的纺丝液粘度大幅降低,表面张力变化不大,导电率基本不变,纺丝产品只有微珠,无益于纺丝性能的改善。并通过将具有不同挥发性能的溶剂(二氯甲烷与N,N-二甲基甲酰胺)配比后配制纺丝液,可以制备表面多孔纳米纤维。
电场中气泡与射流的动力学特征是本文研究的核心内容。使用高速摄影仪拍摄出电场中气泡的变形过程,计算并证明了气泡泰勒锥的临界半锥角为33.02°。运用达朗贝尔原理研究了电场中射流的方向性运动,阐明气泡膜破碎边缘形成“脖颈”形态的力学成因。根据量纲分析法并运用Π定理,得到射流初始速度与气泡膜厚度的关系：(V是初始速度,FE为电场力,h气泡膜的厚度,ρ为溶液的密度,σ为表面张力),进一步根据能量法推导出：V=λ/h(λ为常数,λ=λFE1/2ρ-1/2)。说明气泡膜的厚度决定射流的速度,证明了气泡静电纺丝过程多重射流的产生部位位于气泡的上半部分。讨论了气泡静电纺的产品成形规律：(1)当气泡膜的雷诺数满足气泡破碎形成子气泡及层级射流,纺丝产品由一级或二级射流以及膜碎片形成。(2)气泡膜在电场中撕裂出宽度为a的矩形膜：当a→h,纺丝产品为球形微珠,微球直径满足d=6h；(3)当a/h=4π,纺丝产品为截面圆形的柱状纤维,纤维直径满足d=4h；(4)当a>>h,形成扁平的带状纤维。
本文将板壳振动理论引入产品成形分析。将撕裂出的矩形气泡膜视为矩形薄板,依据Rayleigh (?)去计算出薄板的固有频率为：(D为刚度)。于是,当h/a2<
最后,本文对气泡静电纺纳米纤维膜的应用进行了初步探索。利用热塑性塑料优越的力学性能和纳米纤维膜高比表面积、高孔隙率的特性,制备不同厚度的聚醚酰亚胺纳米纤维膜改善碳纤维复合材料的层间韧性。发现不同膜厚度增韧的双悬臂梁(DCB)试件的Ⅰ型层间断裂值(GIc)均有所提高,特别是膜厚为0.058±0.007mm时,层合板的增韧效果最好,比未增韧试件提高了114.55%；特别是当裂纹长度a=100mm时,GIC值提高了211.27%。而通过界面的SEM照片证实了纳米纤维膜在层间界面通过桥联约束效应及钉锚作用有效提高了复合材料的层间断裂韧性。
Nanofibers are defined as ductile materials with diameter less than100nm and length diameter ration more than100. Nowadays, nanofibers could be comprehensively applied to bio-technology, environment, energy, medical treatment, filtration, sensor and other industries. Electrospinning, as one simple and straightforward fabrication process, is widely adopted. Whereas, the drawbacks in fibers output and fineness to some extent impose restrictions on the future development of Electrospinning. To get rid of those problems, based on the mechanism of spider spinning, Bubble-electrospinning applies viscous bubbles into electrospinning process to prepare nanofibers with high quality and efficiency. It is a fantastic technique, which can impove the output and reduce the fibers fineness effectively.
In this research, in the beginning we discuss the effects of operating parameters(such as voltage, collecting distance, flow rate) and the solution property(such as viscosity, conductivity, surface tension, solvent volatility) on the bubble deformation process, the movement of jets and the morphology of as-spun nanofibers. The effects of voltage and solution viscosity are focused to be analyzed. The scaling laws about fiber diameter and voltage:d∝V4, and fiber diameter and viscosity:d∝η2/3, are respectively deduced. And both of their accuracies are confirmed by the experiment results.
The dynamics characteristics of bubble and charged jets in the electric field are the core content of this thesis. The bubble rupture process is filmed by high speed camera. Accordingly, The half angle of taylor cone measured is33.02°, which is coincided with the theoretical value that is caculated theoretically. We analyze the directional motion of jets using d'Alembert principle, and discussed the reason why the rim of bubble forms neck-like configuration. Then, using dimension analysis, we obtain the relation between the initial velocity of a debris with the film thickness, which reads where FE is the electronic force, ρ is the liquid density and h is the film thickness. The constants λ and β can be determined by experiments. As a result, the initial velocity can be obtained by an energy approach. It can be predicted that smaller thickness results in a larger ejection velocity, this is the reasons why multiple jets from upper half of the bubble, because the upper half has smaller h than that of the bottom half. Through the analysis and discussions in detail, a law on the bubble-electrospun production formation is concluded:In case the ruptured film retracts to be daughter bubbles. The daughter bubbles may continues to be broken to form sub-daughter bubbles, and the process repeats until some a hierarchical ruptured bubble is pulled upwards to form a charged jet, nanofibers are obtained; when the thickness and the width of the jet satisfies h/a=4π,fibers are bubble-electrospun with diameter of4h; and when a→h, the thickness scales with the width, micro-spheres can be found.
Furthermore, oscillation theory is introduced to elaborate the nanofibers shaping mechanism. A short strip sticked to a large piece of a ruptured film is formed, which is regarded as a thin rectangular plate. The plate's natural frequency fn can be caculated by Rayleigh's method approximately: In case far from the natural frequency, no pulsation occurs, and continuous strip-like fibers can be obtained; when h/a2≌fn/k, the plate pulsates (that is, they oscillate in size) at its natural frequency Consequently backbone-like fibers are formed. In case fe≌fn, the frequency of external excitation fe is close to fn, the plate resonates at the same time absorbs energy from external surroundings to maximum extent. The plate can't afford that, and then plate texture is damaged, micro-spheres are likely to be formed.
With the aid of Fluent software, the space distribution of electric field is demonstrated vividly. And the jet motion is simulated under the circumstance whether the electric field exsits or not. The velocity contours show the bending instability happens when the jet flies to the collector. And this phenomenon can be verified from the optical photos of spinning process.
At last, the application of bubble-electrospun nanofibers is explored. PEI nanofibers mebranes are used to improve the interfacial toughness of the carbon fiber reinforced composites. When the thickness of membrane is0.058±0.007mm, the value of GIC of DCB sample increases by114.55%in contrast to the untoughened, which is attributed to the nail-anchorage action.
引文
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