CN103741229A - Preparation method for directionally-arranged electrospinning nanofibres and electrospinning device - Google Patents
Preparation method for directionally-arranged electrospinning nanofibres and electrospinning device Download PDFInfo
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Abstract
本发明公开了一种定向排列电纺纳米纤维的制备方法,包括以下步骤:将金属收集薄片进行折叠,然后清洗,放入干燥箱中备用;制备高聚物溶液作为电纺溶液;将制备的电纺溶液注入静电纺丝装置中;将制备的折叠的金属收集薄片作为收集板,开启静电纺丝装置,在电压为10-20KV的在外加电场作用下,并在收集距离10-30厘米的条件下,在金属收集薄片上收集定向排列的电纺纳米纤维,并通过调整金属收集薄片的方向得到所需形状的纳米纤维。本发明还提供一种静电纺丝装置。本发明采用折叠金属收集薄片法进行材料制备,即将收集装置--金属薄片进行如扇面一样的折叠,然后作为收集板收集纳米纤维,得到定向排列的电纺纳米纤维。
The invention discloses a method for preparing electrospun nanofibers in an oriented arrangement, which comprises the following steps: folding metal collection sheets, cleaning them, and putting them in a drying box for standby; preparing a high polymer solution as an electrospinning solution; The electrospinning solution is injected into the electrospinning device; the prepared folded metal collection sheet is used as a collecting plate, and the electrospinning device is turned on, under the action of an applied electric field at a voltage of 10-20KV, and at a collection distance of 10-30 cm Under the condition, the aligned electrospun nanofibers are collected on the metal collection sheet, and the desired shape nanofibers are obtained by adjusting the direction of the metal collection sheet. The invention also provides an electrostatic spinning device. The present invention adopts the method of folding metal collection flakes for material preparation, that is, the collection device—the metal flakes are folded like a fan, and then used as a collection plate to collect nanofibers to obtain oriented electrospun nanofibers.
Description
技术领域 technical field
本发明涉及一种纺丝加工的工艺及设备,特别是涉及一种制备超精细纤维的加工方法和装置,应用于纺织、生物医用材料、过滤及防护、催化、食品工程、化妆品等领域。 The invention relates to a spinning process and equipment, in particular to a processing method and device for preparing superfine fibers, which are applied in fields such as textiles, biomedical materials, filtration and protection, catalysis, food engineering, and cosmetics.
背景技术 Background technique
静电纺丝技术就是在高压电场下获得纳米纤维的一种技术。始于上世纪30年代,兴起于上世纪90年代。由于其制备工艺简单,成本低廉等特点越来越受到研究人员的重视。最初主要应用于纺织领域的生产和研究。随着研究的进展,静电纺丝技术又被引入到功能材料的制备中,如场效应二极管等材料等。近几年,其在无机材料制备方面的应用,由于无机电纺纳米纤维在在光、热、电、理学和化学等方面的特性及广泛的应用前景逐渐受到研究者的青睐,如MgO, NiO, ZnO以及碳纳米管电纺纤维都成为主要研究对象。此外,在生物医学方面的应用,尤其是作为细胞组织等的支架材料,也成为静电纺丝技术的研究热点之一。 Electrospinning technology is a technology to obtain nanofibers under high voltage electric field. It began in the 1930s and emerged in the 1990s. Because of its simple preparation process and low cost, it has attracted more and more attention from researchers. Initially it was mainly used in production and research in the textile field. With the progress of research, electrospinning technology has been introduced into the preparation of functional materials, such as field effect diodes and other materials. In recent years, its application in the preparation of inorganic materials has gradually been favored by researchers due to the characteristics and wide application prospects of inorganic electrospun nanofibers in terms of light, heat, electricity, physics and chemistry, such as MgO, NiO , ZnO and carbon nanotube electrospun fibers have become the main research objects. In addition, the application in biomedicine, especially as a scaffold material for cell tissue, has also become one of the research hotspots of electrospinning technology.
在生物医学材料和无机功能纳米纤维的应用中,对纤维的结构和形貌都有严格的要求,尤其是纤维排列方向。定向排列的电纺纳米纤维更切合其在生物医学和功能器件中的应用要求。 In the application of biomedical materials and inorganic functional nanofibers, there are strict requirements on the structure and morphology of the fibers, especially the orientation of the fibers. Oriented electrospun nanofibers are more suitable for their application requirements in biomedicine and functional devices.
在纺织领域,为了获得定向排列的纤维束,较早展开了对定向排列电纺纳米纤维的研究。采用高速旋转的收集装置、利用铝制锥形盘、三角形旋转框架、铜线框制成的旋转鼓、平行电极等都可以获得不同程度定向排列的电纺纳米纤维。 In the field of textiles, in order to obtain aligned fiber bundles, research on aligned electrospun nanofibers has been carried out earlier. Electrospun nanofibers with different degrees of alignment can be obtained by using a high-speed rotating collection device, using an aluminum conical disk, a triangular rotating frame, a rotating drum made of a copper wire frame, and parallel electrodes.
发明内容 Contents of the invention
为了解决现有技术问题,本发明的目的在于克服已有技术存在的不足,提供一种定向排列电纺纳米纤维的制备方法和静电纺丝装置,采用折叠金属收集薄片法进行材料制备,即将收集装置--金属薄片进行如扇面一样的折叠,然后作为收集板收集纳米纤维,得到定向排列的电纺纳米纤维。 In order to solve the problems of the prior art, the object of the present invention is to overcome the deficiencies in the prior art, and provide a preparation method and an electrospinning device for aligning electrospun nanofibers. The material is prepared by folding a metal collection sheet method, which is about to collect The device--the metal sheet is folded like a fan, and then used as a collecting plate to collect nanofibers to obtain aligned electrospun nanofibers.
为达到上述发明创造目的,本发明采用下述技术方案: In order to achieve the above invention creation purpose, the present invention adopts the following technical solutions:
一种定向排列电纺纳米纤维的制备方法,其特征在于,包括以下步骤: A preparation method for aligned electrospun nanofibers, characterized in that it comprises the following steps:
a. 将金属收集薄片进行折叠,然后清洗,放入干燥箱中备用;折叠制备的金属收集薄片的断面优选为成锯齿状;采用的金属收集薄片优选为铝箔或铜箔; a. Fold the metal collection sheet, then clean it, and put it in a dry box for subsequent use; the section of the metal collection sheet prepared by folding is preferably jagged; the metal collection sheet used is preferably aluminum foil or copper foil;
b. 制备高聚物溶液作为电纺溶液; b. Prepare polymer solution as electrospinning solution;
c. 将在上述步骤b中制备的电纺溶液注入静电纺丝装置中; c. Inject the electrospinning solution prepared in the above step b into the electrospinning device;
d. 将在上述步骤a中制备的折叠的金属收集薄片作为收集板,开启静电纺丝装置,在电压为10-20KV的在外加电场作用下,并在收集距离10-30厘米的条件下,在金属收集薄片上收集定向排列的电纺纳米纤维,并通过调整金属收集薄片的方向得到所需形状的纳米纤维;调整金属收集薄片的方向优选采用改变金属收集薄片的放置角度来实现。 d. Use the folded metal collection sheet prepared in the above step a as a collection plate, turn on the electrospinning device, under the action of an applied electric field with a voltage of 10-20KV, and under the condition of a collection distance of 10-30 cm, The aligned electrospun nanofibers are collected on the metal collection sheet, and the nanofibers of the desired shape are obtained by adjusting the direction of the metal collection sheet; adjusting the direction of the metal collection sheet is preferably achieved by changing the placement angle of the metal collection sheet.
作为上述本发明技术方案进一步优选的技术方案,在上述折叠的金属收集薄片上收集到的定向排列电纺纳米纤维为直线型、十字型的、米字型或者放射状。 As a further preferred technical solution of the above-mentioned technical solution of the present invention, the aligned electrospun nanofibers collected on the above-mentioned folded metal collection sheet are linear, cross-shaped, square-shaped or radial.
作为上述本发明技术方案进一步优选的技术方案,在上述步骤b中,所制备的高聚物溶液为单一高分子聚合物溶液、不同高聚物的混合溶液或高聚物与无机物的混合溶液。 As a further preferred technical solution of the above technical solution of the present invention, in the above step b, the prepared high polymer solution is a single high molecular polymer solution, a mixed solution of different high polymers or a mixed solution of high polymers and inorganic substances .
本发明还提供一种实施定向排列电纺纳米纤维的制备方法的静电纺丝装置,包括高压电源、毛细管喷射装置和收集器,收集器接地,将电纺溶液注入毛细管喷射装置中,通过控制高压电源,在毛细管喷射装置和收集器之间的纳米纤维生成和收集空间内施加电场作用,使毛细管喷射装置的喷嘴处的电纺溶液液滴由球状被拉长为锥状, 形成泰勒锥,当电场强度增加至设定的临界值时,从泰勒锥中喷射形成溶液射流,溶液射流在电场作用下被进一步迅速拉细形成铺展的电纺丝,收集器由金属薄片折叠形成金属收集薄片载体,通过方向控制装置变换金属薄片的位置和方向,来调节收集器相对于溶液射流的位置和角度,使收集距离保持在10-30厘米之间,在电压为10-20KV的在外加电场作用下,在邻近收集器的空间区域形成有规则的静电纺丝电场分布,引导从泰勒锥喷出的直径为纳米级的铺展的电纺丝,以设定的方向有规则地定向排列散落在收集器的上凸起处和凹槽处,从而在收集器得到所需形状的纳米纤维。 The present invention also provides an electrospinning device for implementing the preparation method of aligned electrospun nanofibers, including a high-voltage power supply, a capillary injection device and a collector, the collector is grounded, and the electrospinning solution is injected into the capillary injection device. Power supply, apply an electric field in the nanofiber generation and collection space between the capillary jet device and the collector, so that the electrospinning solution droplet at the nozzle of the capillary jet device is elongated from a spherical shape to a cone shape, forming a Taylor cone, when When the electric field strength increases to the set critical value, the solution jet is sprayed from the Taylor cone, and the solution jet is further rapidly thinned under the action of the electric field to form a spread electrospinning. The collector is folded from a metal sheet to form a metal collection sheet carrier. Change the position and direction of the metal sheet through the direction control device to adjust the position and angle of the collector relative to the solution jet, so that the collection distance is kept between 10-30 cm. Under the action of an external electric field with a voltage of 10-20KV, A regular electrospinning electric field distribution is formed in the space area adjacent to the collector to guide the spread electrospinning filaments with a diameter of nanometers ejected from the Taylor cone, and to be regularly oriented in a set direction and scattered on the collector. On the protrusions and grooves, so that the nanofibers of the desired shape are obtained in the collector.
上述本发明静电纺丝装置中,构成收集器的金属薄片的断面优选为成锯齿状,在锯齿状的收集装置的凸起处和凹槽处制备定向排列电纺纳米纤维。 In the above-mentioned electrospinning device of the present invention, the section of the metal sheet constituting the collector is preferably zigzag, and aligned electrospun nanofibers are prepared at the protrusions and grooves of the zigzag collector.
上述本发明静电纺丝装置中,构成收集器的金属薄片优选采用铝箔或铜箔。 In the above-mentioned electrospinning device of the present invention, aluminum foil or copper foil is preferably used as the metal sheet constituting the collector.
本发明与现有技术相比较,具有如下显而易见的突出实质性特点和显著优点: Compared with the prior art, the present invention has the following obvious outstanding substantive features and significant advantages:
1. 本发明无需加装或改装静电纺丝装置,只需将收集装置--金属收集薄片稍作改动,改变静电纺丝电场分布,引导从毛细管喷射装置针头喷出的电纺丝定向排列,制备定向排列电纺纳米纤维; 1. The present invention does not need to install or refit the electrospinning device, only needs to slightly modify the collection device--the metal collection sheet, change the distribution of the electrospinning electric field, and guide the directional arrangement of the electrospinning sprayed from the needle of the capillary injection device, Preparation of aligned electrospun nanofibers;
2. 本发明可以根据实际需要,通过调整收集器放置位置和空间倾斜角度来制备复杂形状的纳米纤维,可以实现直线型、十字型的、米字型或者放射状电纺纳米纤维的定制,并且可以根据实际需要,通过调整收集装置的放置位置来制备复杂形状的纳米纤维。 2. The present invention can prepare nanofibers of complex shapes by adjusting the position of the collector and the inclination angle of the space according to actual needs, and can realize the customization of linear, cross-shaped, rice-shaped or radial electrospun nanofibers, and can According to actual needs, nanofibers with complex shapes can be prepared by adjusting the placement position of the collecting device.
附图说明 Description of drawings
图1是本发明实施例一静电纺丝装置结构示意图。 Fig. 1 is a schematic structural diagram of an electrospinning device according to Embodiment 1 of the present invention.
具体实施方式 Detailed ways
本发明的优选实施例详述如下: Preferred embodiments of the present invention are described in detail as follows:
实施例一:Embodiment one:
在本实施例中,参见图1,一种静电纺丝装置,包括高压电源1、毛细管喷射装置2和收集器6,收集器6接地,将电纺溶液注入毛细管喷射装置2中,通过控制高压电源1,在毛细管喷射装置2和收集器6之间的纳米纤维生成和收集空间内施加电场作用,使毛细管喷射装置2的喷嘴处的电纺溶液液滴由球状被拉长为锥状, 形成泰勒锥3,当电场强度增加至设定的临界值时,从泰勒锥3中喷射形成溶液射流4,溶液射流4在电场作用下被进一步迅速拉细形成铺展的电纺丝5,收集器6由金属薄片折叠形成金属收集薄片载体,通过方向控制装置变换金属薄片的位置和方向,来调节收集器6相对于溶液射流4的位置和角度,使收集距离保持在10-30厘米之间,在电压为10-20KV的在外加电场作用下,在邻近收集器6的空间区域形成有规则的静电纺丝电场分布,引导从泰勒锥3喷出的直径为纳米级的铺展的电纺丝5,以设定的方向有规则地定向排列散落在收集器6的上凸起处和凹槽处,从而在收集器6得到所需形状的纳米纤维。 In this embodiment, referring to FIG. 1, an electrospinning device includes a high-voltage power supply 1, a capillary jet device 2, and a collector 6. The collector 6 is grounded, and the electrospinning solution is injected into the capillary jet device 2. By controlling the high-voltage The power source 1 applies an electric field in the nanofiber generation and collection space between the capillary jet device 2 and the collector 6, so that the electrospinning solution droplet at the nozzle of the capillary jet device 2 is elongated from a spherical shape to a cone shape, forming Taylor cone 3, when the electric field strength increases to a set critical value, the solution jet 4 is ejected from the Taylor cone 3, and the solution jet 4 is further rapidly thinned under the action of the electric field to form a spread electrospinning 5, and the collector 6 The metal collecting sheet carrier is formed by folding the metal sheet, and the position and direction of the metal sheet are changed by the direction control device to adjust the position and angle of the collector 6 relative to the solution jet 4, so that the collecting distance is kept between 10-30 cm. Under the action of an applied electric field with a voltage of 10-20KV, a regular electrospinning electric field distribution is formed in the space area adjacent to the collector 6, guiding the spread electrospinning 5 with a diameter of nanometers ejected from the Taylor cone 3, The nanofibers are regularly arranged in a set direction and scattered on the upper protrusions and grooves of the collector 6 , so that the nanofibers of the desired shape are obtained in the collector 6 .
使用本实施例静电纺丝装置进行定向排列电纺纳米纤维的制备方法,包括以下步骤: Use the electrospinning device of this embodiment to carry out the preparation method of aligned electrospun nanofibers, comprising the following steps:
a. 将铝箔折叠成锯齿状,分别依次放入丙酮、乙醇和蒸馏水中超声脱脂20分钟,用蒸馏水再次漂洗后放于真空干燥箱备用; a. Fold the aluminum foil into a zigzag shape, put it in acetone, ethanol and distilled water for ultrasonic degreasing for 20 minutes, rinse again with distilled water and put it in a vacuum drying oven for later use;
b.将高聚物或其混合物的溶液配置静电纺丝溶液; b. The solution of the polymer or its mixture is configured as an electrospinning solution;
c. 将在上述步骤b中配好的静电纺丝液注入到静电纺丝装置中,并将处理好的铝箔安装在图1所示的电极处,调节接收距离为15cm,电压为18KV,进行静电纺丝,铝箔上会接收到一层纳米纤维; c. Inject the electrospinning solution prepared in the above step b into the electrospinning device, and install the processed aluminum foil on the electrode shown in Figure 1, adjust the receiving distance to 15cm, and the voltage to 18KV, and carry out Electrospinning, a layer of nanofibers is received on the aluminum foil;
d.接收铺展的电纺丝5时,可以根据需要调整铝箔的方向,得到十字型的纳米纤维。 d. When receiving the spread electrospun yarn 5, the direction of the aluminum foil can be adjusted as required to obtain cross-shaped nanofibers.
图1为带有带有锯齿形收集板的静电纺丝装置示意图。本实施例利用折叠成锯齿状的收集器6改变静电纺丝过程中的电场分布,利用锯齿形的收集器6对静电纺丝过程中电场分布的改变来引导电纺丝沿特定方向进行排列,制备定向排列的纳米纤维。本实施例方法工艺简单,将作为收集器6的铝箔进行折叠,使之呈锯齿状即可实现电场分布的定制。 Figure 1 is a schematic diagram of an electrospinning setup with a zigzag collector plate. In this embodiment, the zigzag collector 6 is used to change the electric field distribution during the electrospinning process, and the zigzag collector 6 is used to change the electric field distribution during the electrospinning process to guide the electrospinning to arrange in a specific direction. Preparation of aligned nanofibers. The process of the method in this embodiment is simple, and the electric field distribution can be customized by folding the aluminum foil used as the collector 6 to make it zigzag.
实施例二:Embodiment two:
本实施例与实施例一基本相同,特别之处在于: This embodiment is basically the same as Embodiment 1, especially in that:
在本实施例中,根据需要调整铝箔的方向,得到米字型的纳米纤维,通过调整收集装置的放置位置来制备比实施例一更加复杂形状的纳米纤维。 In this example, the direction of the aluminum foil was adjusted as needed to obtain rice-shaped nanofibers, and nanofibers with more complex shapes than in Example 1 were prepared by adjusting the placement position of the collecting device.
实施例三:Embodiment three:
本实施例与前述实施例基本相同,特别之处在于: This embodiment is basically the same as the previous embodiment, and the special features are:
在本实施例中,根据需要调整铝箔的方向,得到放射状的纳米纤维,通过调整收集装置的放置位置来制备比实施例一和实施例二更加复杂形状的纳米纤维。 In this example, the direction of the aluminum foil was adjusted as needed to obtain radial nanofibers, and nanofibers with more complex shapes than those in Examples 1 and 2 were prepared by adjusting the placement position of the collecting device.
上面结合附图对本发明实施例进行了说明,但本发明不限于上述实施例,还可以根据本发明的发明创造的目的做出多种变化,凡依据本发明技术方案的精神实质和原理下做的改变、修饰、替代、组合、简化,均应为等效的置换方式,只要符合本发明的发明目的,只要不背离本发明定向排列电纺纳米纤维的制备方法和静电纺丝装置的技术原理和发明构思,都属于本发明的保护范围。 The embodiments of the present invention have been described above in conjunction with the accompanying drawings, but the present invention is not limited to the above-mentioned embodiments, and various changes can also be made according to the purpose of the invention of the present invention. The changes, modifications, substitutions, combinations, and simplifications should be equivalent replacement methods, as long as they meet the purpose of the present invention, as long as they do not deviate from the technical principle of the preparation method of oriented array electrospun nanofibers and the electrospinning device of the present invention and inventive concepts all belong to the protection scope of the present invention. the
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN112870997A (en) * | 2020-12-11 | 2021-06-01 | 天津工业大学 | Preparation method of coaxial electrostatic solution jet spinning oriented nano hollow fiber membrane |
| CN114870095A (en) * | 2022-05-06 | 2022-08-09 | 南通大学 | Method for constructing tissue engineering graft with surface having anisotropic nano topological structure |
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| CN114870095A (en) * | 2022-05-06 | 2022-08-09 | 南通大学 | Method for constructing tissue engineering graft with surface having anisotropic nano topological structure |
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