CN112226828A - Method for preparing oriented nano-fibers by using folded substrate - Google Patents
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- CN112226828A CN112226828A CN202011056933.4A CN202011056933A CN112226828A CN 112226828 A CN112226828 A CN 112226828A CN 202011056933 A CN202011056933 A CN 202011056933A CN 112226828 A CN112226828 A CN 112226828A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
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Abstract
The invention discloses a method for preparing oriented nano fibers by using a folded substrate, which comprises the following steps: (1) folding and fixing the substrate: folding the substrate receiving the nanofibers into an accordion shape and fixing it on a rotating cylinder collection device; (2) preparing a spinning solution: adding a polymer into a solvent, stirring and dissolving to prepare a spinning solution; (3) electrostatic spinning: spinning according to the electrostatic spinning operation flow to obtain the oriented nanofiber. According to the invention, the substrate is simply folded and then fixed on the low-speed rotating and collecting device, and the oriented nanofiber can be prepared by operating according to the conventional electrostatic spinning process under the condition of only using a common electrostatic spinning device without modifying the device.
Description
Technical Field
The invention relates to preparation of oriented nano-fibers, belongs to the technical field of nano-materials, and particularly relates to a method for preparing oriented nano-fibers by using a folded substrate
Background
The electrostatic spinning technology has attracted extensive attention of researchers in recent years due to the fact that the electrostatic spinning technology is simple in equipment and device, high in universality, flexible and controllable, low in spinning cost and capable of continuously preparing ultra-long nano fibers of various materials and shapes. The common electrostatic spinning device mainly comprises a high-voltage electrostatic field generating device (a high-voltage power supply), a constant-speed micro-injection system (a micro-injection pump and an injector with a metal needle head) and a low-speed rotating collecting device (a grounding cylinder connected with a low-speed motor). The principle of electrostatic spinning is as follows: the metal needle of the injector is connected with the high-voltage end of the high-voltage power supply through a lead, and the collecting device is grounded, so that a high-voltage electrostatic field of dozens of kilovolts is formed between the metal needle and the collecting device; the polymer solution in the syringe flows out from the needle at a constant speed under the action of a micro-injection pump, and liquid drops are formed at the needle and carry positive charges; with the rise of voltage, the hemispherical liquid drop hung at the needle head becomes a cone (Taylor cone), after the voltage further rises to a certain critical value, the electric field force can overcome the surface tension of the liquid drop, and the charged liquid drop forms jet flow under the action of the electric field force and is ejected from the tip of the Taylor cone; the jet is further stretched under the action of the electric field force, the solvent in the jet is volatilized during the jetting and unstable 'whiplash' process, and finally the solidified nano-fibers are collected on a collecting device. In the prior art, in order to facilitate the transfer of collected nanofibers during electrospinning, a layer of substrate is usually coated on the surface of a collecting device, so that the nanofibers are deposited on the substrate, and the substrates are mainly films and dense meshes made of various metals or alloys, such as aluminum foils, copper meshes and the like. Because unstable whip exists in the electrostatic spinning process, the disordered nano fibers in the non-woven fabric form are usually prepared by using a common electrostatic spinning device. The disordered structure greatly limits the application of the composite material in the fields of biology, energy sources, composite reinforced materials and photoelectric information. Highly oriented and regularly arranged nanofibers are of great interest to researchers due to their particular mechanical, optical and electrical properties, and therefore, more and more researchers are beginning to focus on the research for producing oriented nanofibers.
Modification of the collection device is one common method for obtaining oriented nanofibers, and some methods may modify both the collection device and the polymer solution. At present, the main methods for preparing the oriented nanofiber film mainly comprise the following steps: spin-on-collection methods such as making oriented nanofibers using physical drag from a cylinder rotating at high speed (typically above 2000rpm) rely on precise control of the spin rate, which is too low to orient the fibers well and too high to cause fiber breakage, which is not well-known; similar nanofibers prepared by using a thin disc rotating at a high speed have particularly good orientation degree due to the concentration of an electric field, but the collection area is limited to a very small area at the edge of the disc; and a wire drum which is made by uniformly arranging copper wires along the axis of the cylinder rotates at a low speed to prepare the oriented nano fibers, and the nano fibers prepared by the method are difficult to completely transfer on the wire drum. Frame collection methods the methods mainly obtain oriented nanofibers through the action of electrostatic fields generated between rectangular, annular and plate-shaped collecting electrodes placed in different ways on jet flows, and the collected fibers are generally limited in length. (III) the auxiliary electrode method changes the electric field environment by arranging the auxiliary electrode so as to change the stress of the jet flow to obtain the oriented nano fibers, but the large-size nano fiber film is difficult to prepare by independently depending on the auxiliary electrode, generally needs to be combined with a rotary collecting method, and the arrangement of some auxiliary electrodes is complex. The magnetic field auxiliary method (IV) is a magnetic electrostatic spinning Method (MES) which adds magnetic nano particles into a spinning solution, and then two magnets are parallelly placed on two sides of a collecting device to generate a magnetic field by utilizing the ordered arrangement behavior of the magnetic nano particles in the magnetic field. In summary, the above methods all rely to some extent on modifications to the collection device or the provision of auxiliary devices.
Disclosure of Invention
The invention provides a simple and feasible method for preparing oriented nano fibers, aiming at solving the problems in the current preparation of the oriented nano fibers.
The invention relates to a method for preparing oriented nano fibers by using a folded substrate, which comprises the following steps:
(1) folding and fixing the substrate: folding the substrate receiving the nanofibers into an accordion shape and fixing it on a rotating cylinder collection device;
(2) preparing a spinning solution: adding a polymer into a solvent, stirring and dissolving to prepare a spinning solution;
(3) electrostatic spinning: spinning according to the electrostatic spinning operation flow to obtain the oriented nanofiber.
In the above method, the folded substrate includes a plurality of peak portions, a plurality of valley portions, and a plurality of overlapping planes.
In the above method, the peak is in a ridge structure having a blade-like tip.
In the above method, when the folded substrate is fixed on the rotating cylinder collecting device, the ridge structures are arranged in parallel with the axis of rotation of the rotating cylinder, so that all the ridge structures are parallel to each other.
In the above method, the distance between every two adjacent blade-shaped tips is the same.
In the above method, the valley portion has a ridge structure.
In the method, the valley portion has a double-edge structure, and the double-edge structure can facilitate the fixation of the valley portion on the surface of the rotating cylinder.
In the above method, the width of the overlapped plane can be controlled manually when the substrate is folded, and generally, the widths of a plurality of overlapped planes are all 0.1-2cm, and the width of the overlapped plane refers to the distance between the crest edge and the trough edge.
In the above method, when the folded substrate is fixed on the rotating cylinder collecting device, the distance between two adjacent blade-shaped tips can be obviously controlled by the stretching degree of the folded substrate, and the distance between every two adjacent blade-shaped tips can be generally 0.1-2 cm.
As is well known to those skilled in the art, the substrate in step (1) is one of a thin film and a dense grid of various metals or alloy materials, such as aluminum foil, copper mesh, etc., for receiving the nanofibers; the polymer in step (2) may be any one of spinnable polymers, and the solvent is selected according to the polymer, for example, formic acid is selected as the solvent for Polyamide (PA), N-Dimethylformamide (DMF) is selected as the solvent for Polyacrylonitrile (PAN), water is selected as the solvent for polyvinyl alcohol (PVA), etc.; in the conventional electrostatic spinning operation flow in the step (3), a syringe is used as a storage device of a spinning solution, a metal needle is used as a spinning device, the spinning voltage can be generally adjusted within the range of 0-50KV, the distance from the needle to the blade-shaped tip of the substrate can be adjusted, and the liquid outlet speed of an injection pump can be accurately adjusted and controlled; in the conventional electrostatic spinning operation flow in the step (3), the linear speed of the blade-shaped tip of the substrate after the cylinder collecting device starts to rotate can be regulated and controlled by controlling the rotating speed of the motor; and (4) lapping the oriented nanofibers obtained in the step (3) between adjacent blade-shaped tips, wherein all the edge structures are arranged in parallel, and the edge structures are arranged in parallel with the rotating axis of the rotating cylinder, so that the orientation direction is consistent with the rotating direction of the rotating collecting device.
The present invention forms a plurality of parallel blade-like structures by folding the substrate in an accordion shape, where the electric field is concentrated to create a stronger electric field where charged objects are preferentially attracted. During spinning, the folded substrate is fixed on a rotary collecting device, and charged jet flow ejected from a stainless steel needle head is evaporated by a solvent to form charged nano fibers which are mainly acted by two electrostatic forces in the process of falling onto the substrate. The first electrostatic force is originated from the high voltage electrostatic field applied by the high voltage power supply, under the action of the electrostatic force, the charged nano-fiber is attracted to the knife-edge-shaped tip which is closest to the stainless steel needle on the substrate, because the aluminum foil is in a rotating state, the next knife-edge-shaped tip is rotated to the position which is closest to the stainless steel needle, and the charged nano-fiber is immediately attracted to the knife-edge-shaped tip, so that the charged nano-fiber moves from one knife-edge-shaped tip to the other knife-edge-shaped tip to span the gap between the adjacent knife-edge-shaped tips and is lapped between the adjacent knife-edge-shaped tips; the second type of electrostatic force is due to the electrostatic field generated by the nanofibres having reached the substrate, since the charged nanofibres having reached the substrate are charged with the same kind of charge as the nanofibres having reached the substrate, the charged nanofibres are subjected to electrostatic repulsion, which causes the nanofibres to be stretched along the shortest distance in the gap between the blade-like tips, thereby further aligning the nanofibres.
In the prior art, in order to facilitate the transfer of collected nanofibers during electrospinning, a substrate is usually coated on the surface of a collecting device, so that the nanofibers are deposited on the substrate. According to the invention, the substrate is simply folded and then fixed on the low-speed rotating and collecting device, and the oriented nanofibers can be collected by operating according to the conventional electrostatic spinning process under the condition of only using a common electrostatic spinning device without modifying the device.
The technical scheme of the invention has the advantages that the raw materials are easy to obtain, the implementation is simple and convenient, the used material is a substrate for receiving the nano fibers by electrostatic spinning, and the substrate is simply folded and then fixed on a rotary collecting device, so that the preparation of the experimental device is completed; the experimental conditions are easy to meet, the requirement on the rotating speed can be met by using a common motor without using a high-speed motor, and potential safety hazards caused by high-speed rotation are avoided; the product is convenient to transfer, and after spinning is finished, the folded substrate can be directly taken down, and can be further transferred to other substrates according to the use requirements; the applicability is wide, and the method is theoretically suitable for all spinnable substances because the method does not relate to the chemical property of the polymer; a large amount of oriented nano fibers can be obtained on a large scale; the degree of orientation of the obtained oriented nanofibers is superior to that of the general method.
Drawings
Fig. 1 is a schematic view of a folded and fixed substrate, in which: 1. overlap plane, 2, knife-edge-like tip, 3, rotation axis of rotating cylinder collector, 4, rotating cylinder collector, 5, folding substrate.
FIG. 2 is a scanning electron micrograph of the oriented nanofibers prepared in example 1
Fig. 3 is a scanning electron micrograph of the aligned nanofibers prepared in comparative example 1.
Fig. 4 is a scanning electron micrograph of the oriented nanofibers prepared in example 2.
Fig. 5 is a scanning electron micrograph of the oriented nanofibers prepared in example 3.
Fig. 6 is a scanning electron micrograph of the oriented nanofibers prepared in example 4.
Fig. 7 is a scanning electron micrograph of the oriented nanofibers prepared in example 5.
FIG. 8 is a scanning electron micrograph of nanofibers prepared according to example 6.
Detailed Description
Example 1
The invention discloses an embodiment for preparing oriented nano fibers by using a folded substrate, which comprises the following specific steps:
(1) folding and fixing the aluminum foil: folding the aluminum foil substrate into an accordion shape with the width of an overlapping plane of 1 cm; fixing the rotary drum collecting device with glue, and ensuring the distance between two adjacent blade-shaped tips to be 1 cm;
(2) preparing a spinning solution: weighing 10g of polyamide 66(PA66) and adding the polyamide 66 into 90g of formic acid, and magnetically stirring the mixture at room temperature for 12 hours to obtain a uniformly dispersed 10 wt% PA 66-formic acid spinning solution;
(3) electrostatic spinning: in the electrostatic spinning process, a 10ml needle cylinder and a stainless steel needle head with the inner diameter of 0.72mm are used as a storage device of spinning solution; the linear velocity of the blade-shaped tip of the aluminum foil is about 1 m/s; the spinning voltage is 20KV, and the distance from the needle head to the blade-shaped tip of the aluminum foil is 6 cm; the liquid outlet speed controlled by a micro-injection pump is 0.5 ml/h; the spinning time is 10 min.
Comparative example 1
By adopting a conventional preparation mode, the aluminum foil substrate is not folded and is directly fixedly coated on the rotating cylinder collecting device, and the preparation process comprises the following steps:
(1) fixing an aluminum foil: fixing the aluminum foil on a rotary cylinder collecting device by using glue;
(2) preparing a spinning solution: weighing 10g of polyamide 66(PA66) and adding the polyamide 66 into 90g of formic acid, and magnetically stirring the mixture at room temperature for 12 hours to obtain a uniformly dispersed 10 wt% PA 66-formic acid spinning solution;
(3) electrostatic spinning: in the electrostatic spinning process, a 10ml needle cylinder and a stainless steel needle head with the inner diameter of 0.72mm are used as a storage device of spinning solution; the linear speed of the rotating cylinder collecting device at the aluminum foil position is about 1 m/s; the spinning voltage is 20KV, and the distance from the needle head to the aluminum foil is 6 cm; the liquid outlet speed controlled by a micro-injection pump is 0.5 ml/h; the spinning time is 10 min.
Example 2
The invention discloses an embodiment for preparing oriented nano fibers by using a folded substrate, which comprises the following specific steps:
(1) folding and fixing the copper mesh: folding the copper mesh substrate into an accordion shape with the width of an overlapped plane of 1 cm; fixing the rotary drum collecting device with glue, and ensuring the distance between two adjacent blade-shaped tips to be 1 cm;
(2) preparing a spinning solution: weighing 10g of polyamide 66(PA66) and adding the polyamide 66 into 90g of formic acid, and magnetically stirring the mixture at room temperature for 12 hours to obtain a uniformly dispersed 10 wt% PA 66-formic acid spinning solution;
(3) electrostatic spinning: in the electrostatic spinning process, a 10ml needle cylinder and a stainless steel needle head with the inner diameter of 0.72mm are used as a storage device of spinning solution; the linear velocity of the blade-shaped tip of the aluminum foil is about 1 m/s; the spinning voltage is 20KV, and the distance from the needle head to the blade-shaped tip of the copper mesh is 6 cm; the liquid outlet speed controlled by a micro-injection pump is 0.5 ml/h; the spinning time is 30 min.
Example 3
The invention discloses an embodiment for preparing oriented nano fibers by using a folded substrate, which comprises the following specific steps:
(1) folding and fixing the aluminum foil: folding the aluminum foil substrate into an accordion shape with the width of an overlapping plane of 1 cm; fixing the rotary drum collecting device on a rotary drum collecting device by using an adhesive tape, and ensuring that the distance between two adjacent blade-shaped tips is 1 cm;
(2) preparing a spinning solution: weighing 10g of polyamide 66(PA66) and adding the polyamide 66 into 90g of formic acid, and magnetically stirring the mixture at room temperature for 12 hours to obtain a uniformly dispersed 10 wt% PA 66-formic acid spinning solution;
(3) electrostatic spinning: in the electrostatic spinning process, a 10ml needle cylinder and a stainless steel needle head with the inner diameter of 0.72mm are used as a storage device of spinning solution; the linear speed of the blade-shaped tip of the copper mesh is about 1 m/s; the spinning voltage is 20KV, and the distance from the needle head to the blade-shaped tip of the aluminum foil is 6 cm; the liquid outlet speed controlled by a micro-injection pump is 0.5 ml/h; the spinning time was 1 h.
Example 4
The invention discloses an embodiment for preparing oriented nano fibers by using a folded substrate, which comprises the following specific steps:
(1) folding and fixing the aluminum foil: folding the aluminum foil substrate into an accordion shape with the width of an overlapping plane of 1 cm; fixing the rotary drum collecting device on a rotary drum collecting device by using an adhesive tape, and ensuring that the distance between two adjacent blade-shaped tips is 0.5 cm;
(2) preparing a spinning solution: 12.5g of polyamide 66(PA66) was weighed into 87.5g of formic acid and stirred magnetically at room temperature for 12h to obtain a homogeneously dispersed 12.5 wt% PA 66-formic acid spinning solution;
(3) electrostatic spinning: in the electrostatic spinning process, a 10ml needle cylinder and a stainless steel needle head with the inner diameter of 0.72mm are used as a storage device of spinning solution; the linear velocity of the blade-shaped tip of the aluminum foil is about 1 m/s; spinning voltage is 25KV, and the distance from the needle head to the blade-shaped tip of the aluminum foil is 10 cm; the liquid outlet speed controlled by a micro-injection pump is 0.5 ml/h; the spinning time is 20 min.
Example 5
The invention discloses an embodiment for preparing oriented nano fibers by using a folded substrate, which comprises the following specific steps:
(1) folding and fixing the aluminum foil: folding the aluminum foil substrate into an accordion shape with the width of an overlapping plane of 1 cm; fixing the rotary drum collecting device on a rotary drum collecting device by using an adhesive tape, and ensuring that the distance between two adjacent blade-shaped tips is 0.5 cm;
(2) preparing a spinning solution: weighing 15g of polyamide 66(PA66) and adding the polyamide 66 into 85g of formic acid, and magnetically stirring the mixture at room temperature for 12 hours to obtain a uniformly dispersed 15 wt% PA 66-formic acid spinning solution;
(3) electrostatic spinning: in the electrostatic spinning process, a 10ml needle cylinder and a stainless steel needle head with the inner diameter of 0.72mm are used as a storage device of spinning solution; the linear velocity of the blade-shaped tip of the aluminum foil is about 1 m/s; spinning voltage is 25KV, and the distance from the needle head to the blade-shaped tip of the aluminum foil is 10 cm; the liquid outlet speed controlled by a micro-injection pump is 0.5 ml/h; the spinning time is 10 min.
Example 6
The invention uses a folded substrate to prepare an embodiment of an oriented nano, and the specific steps of the embodiment are as follows:
(1) folding and fixing the aluminum foil: folding the aluminum foil substrate into an accordion shape with the width of an overlapping plane of 1 cm; fixing the rotary drum collecting device on a rotary drum collecting device by using an adhesive tape, and ensuring that the distance between two adjacent blade-shaped tips is 0.3 cm;
(2) preparing a spinning solution: weighing 9g of Polyacrylonitrile (PAN), adding the Polyacrylonitrile (PAN) into 91g N, N-Dimethylformamide (DMF), and magnetically stirring at room temperature for 12 hours to obtain a uniformly dispersed 9 wt% PAN-DMF spinning solution;
(3) electrostatic spinning: in the electrostatic spinning process, a 10ml needle cylinder and a stainless steel needle head with the inner diameter of 0.72mm are used as a storage device of spinning solution; the linear velocity of the blade-shaped tip of the aluminum foil is about 1 m/s; the spinning voltage is 10KV, and the distance from the needle head to the blade-shaped tip of the aluminum foil is 6 cm; the liquid outlet speed controlled by a micro-injection pump is 0.4 ml/h; the spinning time is 10 min.
The oriented nanofibers prepared in examples 1 to 6 and comparative example 1 were observed by scanning electron microscopy. The nanofibers prepared in example 1 (fig. 2) are well aligned and have particularly significant orientation; whereas the nanofibers prepared in comparative example 1 (fig. 3) were completely disordered and disordered; example 2 although the kind of the substrate was changed and the spinning time was extended based on example 1, the produced nanofibers (fig. 3) had a significant orientation of most fibers except that the very individual fiber orientation was somewhat random; example 3 the spinning time was greatly extended to 1h based on example 1, the thickness of the collected nanofiber membrane was significantly increased, but the degree of orientation of the prepared nanofibers (fig. 4) was not significantly deteriorated, and the degree of orientation of the majority of fibers was still good; in example 4, the mass concentration of the spinning solution was increased to 12.5% as compared to example 1, and the produced nanofibers (fig. 5) were changed from cylindrical to ribbon shapes, and although the morphology of the nanofibers was changed, the degree of orientation of the nanofibers was not affected, and the produced nanofibers were highly oriented and had excellent orientation; the spinning solution in example 5 is further increased to 15%, and the prepared nanofiber (fig. 6) still has obvious orientation; in example 6, the type of the spinning material was changed, but the produced nanofibers (fig. 7) still had a relatively significant orientation. With the synthesis of examples 1-3, the method of the present invention can prepare highly oriented nanofibers within 0-1h of spinning time; by combining the embodiments 1 and 2, the method of the invention has no special requirements on the specific material and appearance of the used metal or alloy substrate; by combining the embodiments 1, 4 and 5, the method of the present invention can prepare highly oriented nanofibers in a relatively wide concentration range, and although the concentration of the spinning solution may change the morphology of the prepared nanofibers, the method does not affect the orientation degree; combining examples 1 and 5, the process of the present invention is broadly applicable to the preparation of oriented nanofibers using a variety of spinnable polymers.
It should be noted that the technical contents described above are only explained and illustrated to enable those skilled in the art to know the technical spirit of the present invention, and therefore, the technical contents are not to limit the scope of the present invention. The scope of the invention is defined by the appended claims. It should be understood by those skilled in the art that any modification, equivalent replacement, and improvement made based on the spirit of the present invention should be considered to be within the spirit and scope of the present invention.
Claims (10)
1. A method of making oriented nanofibers using a folded substrate, comprising the steps of:
(1) folding and fixing the substrate: folding the substrate receiving the nanofibers into an accordion shape and fixing it on a rotating cylinder collection device;
(2) preparing a spinning solution: adding a polymer into a solvent, stirring and dissolving to prepare a spinning solution;
(3) electrostatic spinning: spinning according to the electrostatic spinning operation flow to obtain the oriented nanofiber.
2. The method of claim 1, wherein the folded substrate comprises peaks and valleys and a plurality of overlapping planes.
3. The method of claim 2 wherein said peaks are in the form of ridge structures having knife-edge like tips.
4. The method of claim 3, wherein the ridge structure is positioned parallel to the axis of rotation of the rotating cylinder when the rotating cylinder is attached to the collection device.
5. A method according to claim 3, wherein the spacing between each two adjacent blade-like tips is the same.
6. The method of claim 1, wherein the valleys are in a rib configuration.
7. The method of claim 1, wherein the valleys are in a double-edged configuration.
8. The method of claim 2, wherein the plurality of overlapping planes each have a width of 0.1 cm to 2cm when the substrate is folded.
9. A method according to claim 3 or 5, wherein the folded substrate is held on the rotating cylindrical collector means such that the spacing between each two adjacent knife-edge like tips is between 0.1 and 2 cm.
10. An oriented nanofiber prepared by the process of any one of claims 1 to 9.
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