CN111575813B - Handheld electrostatic direct injection device and low-voltage electrostatic spinning method - Google Patents

Handheld electrostatic direct injection device and low-voltage electrostatic spinning method Download PDF

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CN111575813B
CN111575813B CN202010427773.3A CN202010427773A CN111575813B CN 111575813 B CN111575813 B CN 111575813B CN 202010427773 A CN202010427773 A CN 202010427773A CN 111575813 B CN111575813 B CN 111575813B
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voltage
conductive block
spinning
linear slit
liquid supply
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CN111575813A (en
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丁彬
龚小宝
岳云鹏
周文
斯阳
李晓然
印霞
俞建勇
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Donghua University
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0061Electro-spinning characterised by the electro-spinning apparatus
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0061Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0069Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0061Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0092Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Textile Engineering (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)

Abstract

The invention relates to a handheld electrostatic direct injection device and a low-voltage electrostatic spinning method. The handheld electrostatic direct injection device consists of a linear slit type spinning nozzle, a liquid supply device, a high-voltage inversion device and a power supply; the linear slit type spinneret comprises a conductive block and a solenoid, and a through linear slit is arranged in the conductive block; the conductive block is connected with the high-voltage inverter; the linear slit is communicated with the liquid supply device; the coil, the high-voltage inverter and the liquid supply device are all connected with a power supply. The low-voltage electrostatic spinning method comprises the following steps: the spinning solution dispersed with the magnetic nano-particles is sprayed out through a slit type spinneret to form conical liquid drops, and jet flow is formed by controlling the combined action of the conical liquid drops on electric field force and magnetic field force, so that the electrostatic spinning process is completed; the voltage of the low-voltage electrostatic spinning is 1-3 kV, and the magnetic field intensity is 0.05-0.1 mT. The invention solves the problems of high voltage, poor safety, less spinning jet and low yield of the existing portable electrostatic spinning equipment.

Description

Handheld electrostatic direct injection device and low-voltage electrostatic spinning method
Technical Field
The invention belongs to the technical field of portable electrostatic spinning devices, and relates to a handheld electrostatic direct injection device and a low-voltage electrostatic spinning method.
Background
The nanofiber shows many novel characteristics in the aspects of light, heat, magnetism, electricity and the like due to the small-size effect, the surface effect, the quantum size effect and the macroscopic quantum tunneling effect, and is highly concerned by researchers. At present, methods for preparing nanofibers include electrostatic spinning, drawing, template synthesis, phase separation, self-assembly, etc., wherein electrostatic spinning is based on the principle that a polymer solution or melt is charged and deformed in a high-voltage electrostatic field to form a suspended conical liquid drop at the end of a spray head; when the charge repulsion force of the surface of the liquid drop exceeds the surface tension force, polymer micro jet flows can be ejected at high speed on the surface of the liquid drop, and the jet flows are stretched at high speed by the electric field force within a short distance, volatilized and solidified by a solvent and finally deposited on a receiving polar plate to form polymer fibers. The electrostatic spinning method has been widely used for preparing nanofibers due to its characteristics in many aspects such as simple equipment, good process controllability, low cost, wide raw material sources, and the like. However, the current electrostatic spinning device has the defects of large volume, heavy weight, high price, portability and the like, so that the use of the electrostatic spinning device in outdoor places is limited. In order to solve the above problems, the prior art provides various solutions.
Patent CN201220605695.2 discloses a portable electrostatic spinning device, which changes the traditional spinning nozzle into a portable type, so as to achieve the purpose of portability and portability, but the device needs an external high voltage power supply and cannot meet the requirement of carrying about.
Patent CN201810216431.X discloses a hand-held melt electrostatic spinning preparation device and a use method, the device avoids the traditional screw extrusion mode by heating and melting materials through hot air, so as to achieve the purpose of portability, but the device needs an external high-voltage power supply and still cannot meet the requirement of carrying about.
The document "Portable Device for Point-of-Need Generation of Silver-nanoparticled Cellulose Acetate nanoparticles for Advanced Wood Dressing, Macromolecular Materials and Engineering,2018,303 (5)", 1700586, uses a micro injection pump, a micro high voltage power supply to prepare a Portable electrospinning Device, but the Device has high voltage, great safety hazard, large volume and weight, and is not easy to carry.
Patent CN201210229010.3 discloses a portable hand-held electrostatic spinning device, which utilizes a high voltage dc inverter to invert and boost a commercially available dry battery to tens of thousands of volts, and the positive level of the device is communicated with a stainless steel needle, thereby realizing the high voltage loading of the spinning solution in the injector. However, the device pushes the injector to advance for liquid supply through the pressure of fingers, so that the liquid supply speed is difficult to accurately regulate and control.
Patent CN201510214221.3 discloses a portable electrostatic spinning device, which controls the perfusion speed in the spinning process by pushing the syringe piston of the injector through a micro stepping motor; but the device has large volume and low integration level, can only realize the spinning of a single needle head, and has low efficiency.
Patent CN201810373378.4 discloses an air flow-assisted handheld portable electrospinning device and its application, the device makes directional deposition of handheld portable electrospinning fibers assisted by air flow, but the device pushes the injector to advance by the pressure of fingers to supply liquid, so that the liquid supply speed is difficult to be accurately controlled.
Therefore, a novel handheld electrostatic spinning device is urgently needed to be developed, which can solve the difficult problems of high voltage and low yield of the existing handheld spinning device and can solve the problems of low equipment integration level, large size, difficulty in carrying and low spinning efficiency.
Disclosure of Invention
The present invention is directed to solving the above problems of the prior art, and provides a handheld electrostatic direct injection device and a low voltage electrostatic spinning method. The invention provides a low-voltage electrostatic spinning method, which mainly reduces the voltage required by generating spinning jet flow by combining an electric field and a magnetic field.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a hand-held electrostatic direct injection device comprises a linear slit type spinning nozzle, a liquid supply device, a high-voltage inversion device and a power supply;
the linear slit spinneret comprises a conductive block (made of one of copper, iron and aluminum) and a solenoid; the conductive block is positioned in the solenoid, and a penetrating linear slit is arranged in the conductive block; the solenoid is an insulating cylindrical tube wound with coils, and the coils are arranged along the axial direction of the cylindrical tube; the linear slit extends along the axial direction of the cylindrical pipe;
the conductive block is connected with the high-voltage inverter; the linear slit is communicated with the liquid supply device; the coil, the high-voltage inverter and the liquid supply device are all connected with a power supply.
In the prior art, a handheld electrostatic spinning device is externally connected with a high-voltage power supply or is converted into high voltage through a high-voltage inverter, so that the purpose that the electrostatic spinning device can be carried and moved is achieved, however, the problems of poor safety and low spinning efficiency inevitably occur due to high spinning voltage;
the invention improves the spinning nozzle to ensure that the force required for generating the spinning jet is controlled by the electric field force FeRepulsive force F with electric chargecIs converted into an electric field force FeMagnetic field force FhRepulsive force F with electric chargecThe common acting force reduces the electric field force required by the formation of spinning jet flow, thereby reducing the spinning voltage, and concretely, the linear slit type spinneret provided by the invention comprises a conductive block and a solenoid; the conductive block is positioned in the solenoid, and a penetrating linear slit is arranged in the conductive block; the solenoid is a cylindrical pipe wound with coils, and the coils are arranged along the axial direction of the cylindrical pipe; the linear slit extends along the axial direction of the cylindrical pipe; the conductive block is connected with the high-voltage inverter; ", because the conductive block is connected with the high-voltage inverter, the spinning jet is subjected to an electric field force FeDirected from the conductive block toward the receiving substrate; the magnetic spinning solution spinning jet is subjected to magnetic field force F due to the fact that the solenoid is a cylindrical tube wound with coils, the coils are arranged along the axial direction of the cylindrical tube, the linear slit extends along the axial direction of the cylindrical tube, and the coils are connected with a power supplyhAnd magnetic field force FhIn the same direction as the electric field force FeThe direction of (a); the repulsion force F between the charges in the spinning jet is due to the mutual repulsion of the charges at the top and bottom of the conical shaped droplets extruded from the linear slitcIn the same direction as the electric field force FeThe direction of (a); because the conical liquid drop extruded from the linear slit has the tendency of shrinking under the action of the surface tension gamma, the spinning jet is subjected to the direction of the surface tension gamma and the electric field force FeIn opposite directions; the boundary condition for finally forming the stable jet is gamma-Fe+Fh+FcAnd is no longer γ ═ Fe+FcDesired F with γ remaining unchangedeThe required spinning voltage is reduced;
the spinning voltage is reduced, so that the safety is improved; the spinning voltage is reduced, so that the yield is higher under the same electricity consumption, namely the spinning efficiency is improved (the yield is higher compared with a single-needle type spray head due to the adoption of the linear slit).
As a preferred technical scheme:
according to the handheld electrostatic direct injection device, the linear slit type spinneret further comprises an insulating cylinder, and the linear slit is communicated with the liquid supply device through the insulating cylinder.
According to the handheld electrostatic direct injection device, the conductive block is of a circular truncated cone-shaped structure and is coaxial with the cylindrical pipe; the linear slit is of a cuboid structure; the insulating cylinder is a circular truncated cone cylinder and is coaxial with the conductive block, the small end of the insulating cylinder is connected with the large end of the conductive block, and the large end of the insulating cylinder is connected with the liquid supply device.
According to the handheld electrostatic direct injection device, the diameter of the large end of the conductive block is 3-4 cm, the diameter of the small end of the conductive block is 2-3 cm, and the height of the conductive block is 0.5-1 cm; the length of the linear slit is equal to the height of the conductive block, the width of the cross section of the linear slit is 0.3-1.0 mm, and the length of the cross section is 2-4 mm smaller than the diameter of the small end of the conductive block, so that the spinning solution can form conical liquid drops as much as possible after exiting the slit, and the yield is improved; the wall thickness of the cylindrical pipe is 1-2 mm, the outer diameter is 5-6 cm, and the height is 6-7 cm; the wall thickness of the insulating cylinder is 1-3 mm, the outer diameter of the large end is 5-6 cm, the outer diameter of the small end is 3-4 cm, and the height is 3-5 cm.
In the above handheld electrostatic direct injection device, the value range of the number N of turns of the coil is [10,40]The resistance of the coil is 1-2 omega, the voltage of the power supply is 3V, and the high-voltage inverter is used for converting the voltage from 3V to 1-3 kV. The boundary condition for forming a stable jet is γ ═ Fe+Fh+FcFrom which the electrostatic spinning critical voltage V can be approximated0
Figure BDA0002499330350000031
Where R is the width of the slit, γ is the surface tension, l is the distance between the spinneret and the receiving substrate, and u is the magnetic permeability (constant, 4 π × 10)-7) I is the coil current (determined by the supply voltage and the coil resistance), N is the number of coil turns, and Q is the magnetic charge (constant);
from the above formula, it can be seen that under the condition that the surface tension gamma of the spinning solution, the receiving distance l (i.e. the distance between the spinneret and the receiving substrate) and the width R of the slit are not changed, the critical voltage V of the spinning can be obviously reduced by increasing the number of turns N of the coil of the solenoid and the coil current I0In order to achieve a reduction in the critical voltage V of the spinning0The invention controls the value range of the number N of the coil turns to be [10,40]]And meanwhile, the power supply voltage is controlled to be 3V (the reason that 3V voltage is used is that dry batteries can be used for supplying power, and the size is small so that the carrying is convenient), smooth spinning can be finally realized under the smaller electrostatic spinning voltage of 1-3 kV, the electrostatic spinning voltage is far lower than that of the prior art (generally over 10 kV), and the problem that the safety is poor due to the fact that the voltage of the portable electrostatic spinning equipment in the prior art is higher is finally effectively solved.
The handheld electrostatic direct injection device comprises a liquid supply device, a liquid supply device and a control device, wherein the liquid supply device comprises a micro stepping motor, a driving electric plate and a liquid supply tank; the driving electric plate is simultaneously connected with a power supply and a micro stepping motor, and the micro stepping motor is connected with a propelling rod of the liquid supply tank (the rotating speed of the micro stepping motor determines the moving speed of the propelling rod).
The invention also provides a low-voltage electrostatic spinning method, wherein the spinning solution dispersed with magnetic nanoparticles is sprayed out through a slit spinneret to form a conical liquid drop, the conical liquid drop is controlled to be acted by electric field force and magnetic field force in the same direction between the slit spinneret and a receiving base material to form jet flow, the jet flow is further stretched and refined, and the jet flow is deposited on the receiving base material to form a fiber film;
the voltage required by the generation of spinning jet flow is effectively reduced by combining an electric field and a magnetic field, the voltage of low-voltage electrostatic spinning is 1-3 kV, and the strength of the magnetic field is 0.05-0.1 mT.
As a preferred technical scheme:
in the low-voltage electrostatic spinning method, the magnetic nanoparticles are magnetic silica nanoparticles or ferroferric oxide nanoparticles.
The low-voltage electrostatic spinning method comprises the following other process parameters: the solution perfusion speed during spinning is 0.1-50 mL/h, and if the perfusion speed is too low, the spinning yield is low, the perfusion speed is too high, the liquid output is large, and continuous spinning is difficult; the distance between slot type spinning jet and the receiving substrate is 5~15cm, and the distance is too close, and the efflux can't stretch the solidification completely, and the distance is too far away, leads to the electric field to reduce, can't form the efflux.
Has the advantages that:
(1) according to the handheld electrostatic direct injection device, the spinning voltage is 1-3 kV, and the problems of high voltage and poor safety of the conventional portable electrostatic spinning equipment are solved;
(2) the handheld electrostatic direct injection device overcomes the defects of less spinning jet flow and low yield of portable electrostatic spinning equipment;
(3) the handheld electrostatic direct injection device is high in integration level, small in size, convenient to carry and wide in application range;
(4) the low-voltage electrostatic spinning method reduces the voltage required by generating the spinning jet flow by combining the electric field and the magnetic field, and has ingenious conception and obvious effect.
Drawings
FIG. 1 is a schematic view of a handheld electrostatic direct injection device of the present invention;
FIG. 2 is a schematic view of a line slit spinneret according to the present invention;
the spinning device comprises a 1-linear slit type spinneret, a 2-liquid supply device, a 3-power supply, a 4-high-voltage inverter, a 5-slit type nozzle, a 6-hollow cylindrical solenoid, a 7-insulating cylinder, 8-conductive blocks, a 9-linear slit, 10-spinning liquid, 11-coils, 12-micro stepping motors, 13-driving electric plates, 14-liquid supply tanks, 15-pushing rods of the liquid supply tanks and 16-spinning jet.
Detailed Description
The invention will be further illustrated with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
As shown in fig. 1, the handheld electrostatic direct injection device is composed of a linear slit type spinneret 1, a liquid supply device 2, a high-voltage inverter device 4 and a power supply 3;
as shown in fig. 2, the linear slit spinneret 1 is composed of a conductive block 8, a solenoid 6 and an insulating cylinder 7, the insulating cylinder 7 and the conductive block 8 together form a slit nozzle 5, and a spinning solution 10 is extruded from the slit nozzle 5 to become a spinning jet 16; the conductive block 8 is positioned inside the solenoid 6, and a through linear slit 9 is arranged inside the conductive block 8; the solenoid 6 is an insulating cylindrical tube wound with a coil 11, the coil 11 is arranged along the axial direction of the cylindrical tube, the value range of the number N of turns of the coil 11 is [10,40], and the resistance of the coil 11 is 1-2 omega; the linear slit 9 extends along the axial direction of the cylindrical pipe;
the conductive block 8 is connected with the high-voltage inverter 4; the linear slit 9 is communicated with the liquid supply device 2 through the insulating cylinder 7; the coil 11, the high-voltage inverter 4 and the liquid supply device 2 are all connected with the power supply 3, the voltage of the power supply 3 is 3V, and the high-voltage inverter 4 is used for converting the voltage from 3V to 1-3 kV;
the conductive block 8 is in a circular truncated cone-shaped structure and is coaxial with the cylindrical tube; the linear slit 9 is of a cuboid structure; the insulating cylinder 7 is a circular truncated cone cylinder and is coaxial with the conductive block 8, the small end of the insulating cylinder 7 is connected with the large end of the conductive block 8, and the large end of the insulating cylinder 7 is connected with the liquid supply device 2;
the diameter of the large end of the conductive block 8 is 3-4 cm, the diameter of the small end is 2-3 cm, and the height is 0.5-1 cm; the height of the linear slit 9 is equal to that of the conductive block 8, the width of the cross section of the linear slit is 0.3-1.0 mm, and the length of the cross section is 2-4 mm smaller than the diameter of the small end of the conductive block; the wall thickness of the cylindrical pipe is 1-2 mm, the outer diameter is 5-6 cm, and the height is 6-7 cm; the wall thickness of the insulating cylinder 7 is 1-3 mm, the outer diameter of the large end is 5-6 cm, the outer diameter of the small end is 3-4 cm, and the height is 3-5 cm;
as shown in fig. 1, the liquid supply device 2 is composed of a micro stepping motor 12, a driving electric plate 13 and a liquid supply tank 14; the driving electric plate 13 is connected with the power supply 3 and the micro stepping motor 12 at the same time, and the micro stepping motor 12 is connected with the propelling rod 15 of the liquid supply groove.
A low-voltage electrostatic spinning method is disclosed, wherein the spinning voltage is 1-3 kV, the handheld electrostatic direct injection device is adopted, a power supply is started, a liquid supply device, a high-voltage inverter and a coil of a solenoid are in working states, the liquid supply device sends spinning liquid (polyurethane, polystyrene, polyacrylonitrile or polyvinylidene fluoride, N-dimethylformamide or N, N-dimethylacetamide, the content of the polymer in the spinning liquid is 4-13 wt%, and the content of the magnetic nanoparticles is 0.005-0.02 wt%) with magnetic nanoparticles dispersed in the spinning liquid to the top end of a slit spinning nozzle to form conical liquid drops; the high-pressure device makes the spinning solution charged with positive electricity and forms an electric field between the spinning nozzle and the receiving substrate; the solenoid forms a magnetic field at the slit, the magnetic field strength is 0.05-0.1 mT (magnetic field strength B is uMI, u is permeability (constant, 4 pi x 10)-7) I is the coil current (determined by the supply voltage and the coil resistance), N is the number of coil turns); the magnetic charged conical liquid drops form jet flow under the combined action of electric field force and magnetic field force; the jet stream further stretches and thins and finally deposits on the receiving substrate to form a fiber film. Wherein the solution perfusion speed during spinning is 0.1-50 mL/h; the distance between the slit spinneret and the receiving base material is 5-15 cm.

Claims (6)

1. A hand-held electrostatic direct injection device is characterized in that: consists of a linear slit type spinning nozzle, a liquid supply device, a high-voltage inversion device and a power supply;
the linear slit spinneret comprises a conductive block and a solenoid; the conductive block is positioned in the solenoid, and a penetrating linear slit is arranged in the conductive block; the solenoid is an insulating cylindrical tube wound with coils, and the coils are arranged along the axial direction of the cylindrical tube; the linear slit extends along the axial direction of the cylindrical pipe, and conical liquid drops formed on the linear slit are positioned in the solenoid;
the conductive block is in a circular truncated cone-shaped structure and is coaxial with the cylindrical tube; the linear slit is of a cuboid structure; the insulating cylinder is a circular truncated cone cylinder and is coaxial with the conductive block, the small end of the insulating cylinder is connected with the large end of the conductive block, and the large end of the insulating cylinder is connected with the liquid supply device;
the diameter of the large end of the conductive block is 3-4 cm, the diameter of the small end of the conductive block is 2-3 cm, and the height of the conductive block is 0.5-1 cm; the length of the linear slit is equal to the height of the conductive block, the width of the cross section of the linear slit is 0.3-1.0 mm, and the length of the cross section is 2-4 mm smaller than the diameter of the small end of the conductive block; the wall thickness of the cylindrical pipe is 1-2 mm, the outer diameter is 5-6 cm, and the height is 6-7 cm; the wall thickness of the insulating cylinder is 1-3 mm, the outer diameter of the large end is 5-6 cm, the outer diameter of the small end is 3-4 cm, and the height is 3-5 cm;
the value range of the number N of turns of the coil is [10,40], the resistance of the coil is 1-2 omega, the voltage of a power supply is 3V, and the high-voltage inverter is used for converting the voltage from 3V to 1-3 kV;
the conductive block is connected with the high-voltage inverter; the linear slit is communicated with the liquid supply device; the coil, the high-voltage inverter and the liquid supply device are all connected with a power supply.
2. The handheld electrostatic direct injection device of claim 1, wherein the line slot spinneret further comprises an insulating cylinder, and the line slot communicates with the liquid supply device through the insulating cylinder.
3. The handheld electrostatic direct injection device of claim 1, wherein the liquid supply device is composed of a micro stepping motor, a driving electric plate and a liquid supply tank; the driving electric plate is simultaneously connected with a power supply and a micro stepping motor, and the micro stepping motor is connected with a propelling rod of the liquid supply tank.
4. A low voltage electrospinning method using a handheld electrostatic direct injection device according to any of claims 1 to 3, characterized by: the spinning solution dispersed with the magnetic nano-particles is sprayed out through a slit type spinneret to form a conical liquid drop, a jet flow is formed by controlling the conical liquid drop to be acted by an electric field force and a magnetic field force in the same direction between the slit type spinneret and a receiving base material, the jet flow is further stretched and refined, and the jet flow is deposited on the receiving base material to form a fiber film;
the voltage of the low-voltage electrostatic spinning is 1-3 kV, and the strength of the magnetic field is 0.05-0.1 mT.
5. The low-voltage electrospinning method of claim 4, wherein the magnetic nanoparticles are magnetic silica nanoparticles or ferroferric oxide nanoparticles.
6. The low-voltage electrospinning method according to claim 4, wherein the other process parameters of the low-voltage electrospinning are as follows: the solution filling speed during spinning is 0.1-50 mL/h; the distance between the slit spinneret and the receiving base material is 5-15 cm.
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