CN110747581B - Integrated preparation device and method for large-area transparent flexible electrode - Google Patents
Integrated preparation device and method for large-area transparent flexible electrode Download PDFInfo
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
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- 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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- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0092—Electro-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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Abstract
The invention belongs to the technical field of electrode preparation, and particularly relates to an integrated preparation device and method of a large-area transparent flexible electrode. According to the invention, the size of the mesh of the substrate mask plate is controlled, so that nanofiber spinning can be stably received, and the stability and flatness of a nanofiber film are ensured; the invention utilizes the conveyor belt to convey in vacuum, ensures the continuity of each step, has simple and easy preparation method and low cost, and is suitable for large-scale production. The invention can be applied to the field of photoelectric devices such as large-area flexible displays, and has the advantages of simple preparation process, low cost and good application prospect.
Description
Technical Field
The invention belongs to the technical field of electrode preparation, and particularly relates to an integrated preparation device and method of a large-area transparent flexible electrode.
Background
With the progress of society, flexible transparent electrodes play a decisive role in touch screen display, skin wearable and implantable electronic equipment and the like. The improvement of the performance of the transparent electrode is particularly important as an essential component of the photoelectric device. ITO is a traditional material for preparing transparent electrodes due to its high electrical conductivity and high light transmittance. However, with the increasing demand for screen sizes in recent years, ITO has the disadvantages of being brittle, difficult to process, and lacking in flexibility. Therefore, other flexible transparent conductive films which can replace ITO in batch preparation are developed, and the flexible transparent conductive film with low cost becomes a focus of attention in recent years.
At present, in order to solve the problems, a mature electrostatic spinning technology is used for preparing the transparent flexible electrode. The electrostatic spinning technology is a method for preparing a nanofiber material by utilizing the breakdown effect of a high-voltage electrostatic field on a high-molecular solution, and finally forming nanofibers on a receiving device. However, the jet does not fall in a straight line on the receiving device during the whole spinning process. The needle and the receiving device of the jet do not move in the whole electrostatic spinning preparation process, the area of the obtained film is small, and the thickness is not uniform. The receiving device is generally a flat plate receiving device or a roller receiving device, the roller or the flat plate is generally a metal device, the shape is fixed, and the spinning film is not easy to take down after receiving. In the whole process of preparing the transparent electrode, all the stages are not continuous, certain processes are carried out in vacuum, and other processes can be carried out under normal environment, so that the starting and debugging of equipment are not continuous, and the factors can influence the properties of the film. Therefore, the development of a large-area flexible transparent conductive film technology with simple preparation process and excellent performance has very important significance.
Disclosure of Invention
In order to solve the problems, the invention provides an integrated preparation method of a large-area transparent flexible electrode.
The technical scheme of the invention is as follows:
an integrated preparation device of a large-area transparent flexible electrode comprises a high-voltage power supply 1, a liquid supply device 2, a mask plate 3 with adjustable mesh size, a heating device 4, a thermal evaporation device 5 and a film blowing device 6;
the high-voltage power supply 1, the heating device 4, the thermal evaporation device 5 and the film blowing device 6 are arranged in a row and fixed on the base; a conveying belt is arranged on the base, and the mask plate 3 with adjustable mesh size is arranged on the conveying belt;
the anode of the high-voltage power supply 1 is connected with the liquid supply device 2 through a lead, and the cathode of the high-voltage power supply is connected with the mask plate 3 with adjustable mesh size through a lead; the liquid supply device 2 controls the liquid supply speed by a flow pump and continuously supplies spinning liquid to the liquid supply device 2; when spinning begins, the mask plate 3 with the adjustable mesh size is arranged at the position 5-30cm below the liquid supply device 2 and used for receiving nanofiber spinning, and then the mask plate 3 with the adjustable mesh size is sequentially sent into the heating device 4, the thermal evaporation device 5 and the film blowing device 6 along with the movement of the conveying belt according to the sequence of the preparation process.
The mask plate 3 with the adjustable mesh size is of a net structure consisting of a plurality of copper wires, each copper wire is provided with a circuit switch, and the circuit switches where the copper wires are located are controlled to control the on-off of current on the copper wires, so that meshes with different sizes are formed.
The liquid supply device 2 comprises an infusion catheter, a needle head and an injector, and the injector is driven by a flow pump and provides spinning solution.
The mask plate 3 with adjustable mesh size has larger size, the length is 110-155mm, the width is 60-80mm, the plate thickness is 5-8mm, and the diameter of the copper wire is 0.5-1 mm.
An integrated preparation method of a large-area transparent flexible electrode uses the integrated preparation device of the large-area transparent flexible electrode, a layer of nanofiber film prepared from organic polymer solution is coated on a mask plate 3 with adjustable mesh size as a substrate, and the nanofiber film is loaded with nano Ag, so that the large-area transparent flexible electrode is obtained, and the whole preparation process is in a vacuum environment; the method comprises the following steps:
(1) preparing a large-area nanofiber film:
and (2) starting the high-voltage power supply 1, switching on a liquid supply device 2 connected with the high-voltage power supply 1, controlling the liquid supply rate by a flow pump, extending the spinning solution downwards from a needle head of the liquid supply device 2 along with gravity to form nanofiber spinning, and receiving the nanofiber spinning by a mask plate 3 with adjustable mesh size below the liquid supply device 2 to obtain the nanofiber film.
(2) And (3) driving the nanofiber film obtained in the step (1) to enter a heating device 4 by the mask plate 3 with adjustable mesh size through the movement of the conveyor belt, and heating for 10-15min at the temperature of 80-120 ℃.
(3) Through the movement of the conveying belt, the mask plate 3 with adjustable mesh size drives the nanofiber film obtained in the step (2) to enter a thermal evaporation device 5, and the pressure of the whole device is controlled at 10 during working-5And (4) below Pa, loading nano Ag on the nano fiber film to obtain the large-area transparent flexible electrode.
(4) And (3) driving the large-area transparent flexible electrode obtained in the step (3) to be placed in a film blowing device 6 by the mask plate 3 with adjustable mesh size through the movement of the conveying belt, and blowing the film for 10-15min to finish the whole preparation process.
The thickness of the nanofiber film is 200-500 nm.
The nanofiber spinning film can detect the uniformity of the spinning film by measuring the resistance value of the copper wire on the mask plate 3 with adjustable mesh size.
The organic polymer solution is used as spinning solution, preferably PVA1788, PVA1750 or PVP solution, with the concentration of 10% -15%.
The invention has the beneficial effects that:
1. according to the invention, the size of the mesh of the substrate mask plate is controlled, so that the nanofiber spinning can be stably received, and the stability and flatness of the nanofiber film are ensured.
2. The invention utilizes the conveyor belt to convey in vacuum, ensures the continuity of each step, has simple and easy preparation method and low cost, and is suitable for large-scale production.
3. The invention can change the size of the mask plate and can obtain the transparent flexible electrode with the required area.
4. The mask plate with adjustable mesh size used in the invention is convenient for taking down the nanofiber spinning film and can be repeatedly used
5. The invention can be applied to the field of photoelectric devices such as large-area flexible displays, and has the advantages of simple preparation process, low cost and good application prospect.
Drawings
FIG. 1 is a schematic view of the apparatus of the present invention.
In the figure: the device comprises a high-voltage power supply 1, a liquid supply device 2, a mask plate with adjustable mesh size 3, a heating device 4, a thermal evaporation device 5, a film blowing device 6, control buttons 7, 8, 9, 10 and 11, copper wires 12, 13, 14, 15, 16, 17, 18, 19 and 20.
FIG. 2 is a schematic plan view of a mask control method with adjustable mesh size according to the present invention.
Fig. 3 and 4 are electron micrographs of nanofiber films prepared according to the present invention at different positions.
Detailed Description
The following further describes a specific embodiment of the present invention with reference to the drawings and technical solutions.
An integrated preparation device of a large-area transparent flexible electrode is shown in figure 1 and comprises a high-voltage power supply 1, a liquid supply device 2, a mesh size-adjustable mask plate 3, a heating device 4, a thermal evaporation device 5 and a film blowing device 6, wherein five control buttons 7, 8, 9, 10 and 11 are used for controlling connection or disconnection of copper wires corresponding to the mesh size-adjustable mask plate 3 and the power supply.
The integrated preparation device is used for preparing the large-area transparent flexible electrode, and comprises the following specific steps:
example 1:
(1) the preparation method comprises the steps of preparing a large-area nanofiber transparent film, connecting the anode of a high-voltage power supply 1 to a liquid supply device 2 through a lead, controlling the liquid supply rate of the liquid supply device 2 through a flow pump, and continuously supplying 10% PVA spinning solution to the liquid supply device. And a mask plate 3 with adjustable mesh size is arranged at a position 5cm below the liquid supply device and used for receiving the nanofibers, and the mask plate is connected with the negative electrode of the high-voltage power supply through a wire.
(2) And (2) heating the nanofiber film obtained in the step (1) for 15min at the temperature of 100 ℃ by a heating device 4.
(3) Putting the nanofiber film obtained in the step (2) into a thermal evaporation device 5, wherein the pressure of the whole device is controlled at 10 during operation-5The content of the compound is less than Pa,and loading nano Ag on the obtained nano fiber film to obtain the large-area transparent flexible electrode.
(4) And (4) blowing the large-area transparent electrode obtained in the step (3) for 15min by using a film blowing device 6 to obtain a flexible large-area transparent electrode film.
Example 2:
(1) and preparing a large-area nanofiber transparent film, wherein the anode of the high-voltage power supply 1 is connected to a liquid supply device 2 through a lead, and the liquid supply device 2 controls the liquid supply speed through a flow pump and continuously provides 12% PVA spinning solution to the liquid supply device. A mask plate 3 with adjustable mesh size is arranged 15cm below the liquid supply device and used for receiving the nano fibers, and the mask plate is connected with the negative electrode of the high-voltage power supply through a lead.
(2) And (2) heating the nanofiber film obtained in the step (1) for 12min at 120 ℃ by a heating device 4.
(3) Putting the nanofiber film obtained in the step (2) into a thermal evaporation device 5, wherein the pressure of the whole device is controlled at 10 during operation-5And (4) below Pa, loading nano Ag on the obtained nano fiber film to obtain the large-area transparent flexible electrode.
(4) And (4) blowing the large-area transparent electrode obtained in the step (3) for 12min by using a film blowing device 6 to obtain a flexible large-area transparent electrode film.
Example 3:
(1) preparing a large-area nano-fiber transparent film, which comprises the following components: the positive pole of the high-voltage power supply 1 is connected to the liquid supply device 2 through a lead, the liquid supply rate of the liquid supply device 2 is controlled by a flow pump, and PVA spinning solution with the concentration of 15% is continuously supplied to the liquid supply device. And a mask plate 3 with adjustable mesh size is arranged at a position 30cm below the liquid supply device and used for receiving the nano fibers, and the mask plate is connected with the negative electrode of the high-voltage power supply through a lead.
(2) And (2) heating the nanofiber film obtained in the step (1) for 10min at the temperature of 80 ℃ by a heating device 4.
(3) Putting the nanofiber film obtained in the step (2) into a thermal evaporation device 5, wherein the pressure of the whole device is controlled at 10 during operation-5Pa or less, loading the nanofiber film with the nano AAnd g, obtaining the large-area transparent flexible electrode.
(4) And (4) blowing the large-area transparent electrode obtained in the step (3) for 10min by using a film blowing device 6 to obtain a flexible large-area transparent electrode film.
Example 4
The control method of the mask plate 3 with the adjustable mesh size in the step 1 comprises the following steps: as shown in fig. 2, the power supply connected with the fixed opening copper wires 13, 15, 17 and 19 starts the preparation process, and the resistance of the copper wires is detected in real time and displayed through an ohmmeter. When the resistance value of a certain area is detected to be larger, the thickness of the nanofiber film in the area is indicated to be insufficient, the mesh size can be reduced by turning on the power supply connected with the copper wires 12, 14, 16, 18 and 20 at the corresponding positions through the control buttons 7, 8, 9, 10 and 11, the thickness of the nanofiber film in the area is increased, and the uniformity of the prepared nanofiber film is ensured.
Comparative analysis of results
FIG. 3 is a scanning electron microscope image of a nanofiber film surface structure obtained by receiving a 12% PVA solution through a mask with adjustable meshes and heating the PVA solution at 120 ℃ for 12min, and as can be seen from FIG. 3, the prepared film is uniform and complete in appearance.
FIG. 4 is a scanning electron microscope image of a specific intersection of nanofiber films prepared by receiving a 12% PVA solution through a mask with adjustable meshes and heating at 120 ℃ for 12min, and it can be seen from FIG. 4 that the film at the specific intersection is dense in shape and can be used for preparing a flexible electrode.
According to the technical scheme, the large-area flexible electrode integrated preparation method can obtain the flexible electrode with good conductivity and light transmittance, can accelerate the preparation speed, ensures that the electrodes are generated in vacuum in the preparation process, is free from pollution, and can be widely applied to the fields of display touch screens and the like.
Claims (8)
1. An integrated preparation device of a large-area transparent flexible electrode comprises a high-voltage power supply (1), a liquid supply device (2), a heating device (4) and a thermal evaporation device (5), and is characterized by further comprising a mask plate (3) with adjustable mesh size and a film blowing device (6);
the high-voltage power supply (1), the heating device (4), the thermal evaporation device (5) and the film blowing device (6) are arranged in a row and fixed on the base; a conveying belt is arranged on the base, and a mask plate (3) with adjustable mesh size is arranged on the conveying belt;
the anode of the high-voltage power supply (1) is connected with the liquid supply device (2) through a wire, and the cathode of the high-voltage power supply is connected with the mask plate (3) with adjustable mesh size through a wire; the liquid supply device (2) controls the liquid supply speed by a flow pump and continuously supplies spinning liquid to the liquid supply device (2); when spinning begins, the mask plate (3) with the adjustable mesh size is arranged at a position 5-30cm below the liquid supply device (2) and used for receiving nanofiber spinning, and then the mask plate (3) with the adjustable mesh size is sequentially conveyed into the heating device (4), the thermal evaporation device (5) and the film blowing device (6) along with the movement of the conveying belt according to the sequence of the preparation process.
2. The integrated preparation device of the large-area transparent flexible electrode according to claim 1, characterized in that the mask plate (3) with adjustable mesh size is a mesh structure consisting of a plurality of copper wires, each copper wire is provided with a circuit switch, and the on-off of the current on the copper wire is controlled by controlling the circuit switch of each copper wire, so that meshes with different sizes are formed.
3. The integrated preparation device of the large-area transparent flexible electrode as claimed in claim 1 or 2, wherein the mask plate (3) with adjustable mesh size has a length of 110-155mm, a width of 60-80mm, a plate thickness of 5-8mm and a copper wire diameter of 0.5-1 mm.
4. The integrated preparation device of the large-area transparent flexible electrode according to claim 1 or 2, wherein the liquid supply device (2) comprises an infusion catheter, a needle and a syringe, and the syringe is driven by a flow pump to provide a spinning solution.
5. The integrated preparation device of the large-area transparent flexible electrode according to claim 3, wherein the liquid supply device (2) comprises an infusion catheter, a needle and a syringe, and the syringe is driven by a flow pump to provide a spinning solution.
6. An integrated preparation method of a large-area transparent flexible electrode, which is prepared by adopting the device of claims 1-5, and is characterized in that a layer of nanofiber film prepared from organic polymer solution is coated on a mask plate (3) with adjustable mesh size as a substrate, and nano Ag is loaded on the nanofiber film, so that the large-area transparent flexible electrode is obtained, and the whole preparation process is in a vacuum environment; the method comprises the following steps:
(1) preparing a large-area nanofiber film:
starting a high-voltage power supply (1), conducting a liquid supply device (2) connected with the high-voltage power supply (1), controlling the liquid supply speed by a flow pump, extending a spinning solution downwards from a needle head of the liquid supply device (2) along with gravity to form nanofiber spinning, and receiving the nanofiber spinning by a mask plate (3) with adjustable mesh size below the liquid supply device (2) to obtain a nanofiber film;
(2) by moving the conveyor belt, the mask plate (3) with adjustable mesh size drives the nanofiber film obtained in the step (1) to enter a heating device (4) and is heated for 10-15min at the temperature of 80-120 ℃;
(3) the mask plate (3) with adjustable mesh size drives the nanofiber film obtained in the step (2) to enter a thermal evaporation device (5) through the movement of the conveying belt, and the pressure of the whole device is controlled at 10 during working-5Below Pa, loading nano Ag on the nano fiber film to obtain a large-area transparent flexible electrode;
(4) and (3) driving the large-area transparent flexible electrode obtained in the step (3) to be placed in a film blowing device (6) by the aid of the movement of the conveying belt and the mask plate (3) with adjustable mesh size, and blowing the film for 10-15min to finish the whole preparation process.
7. The integrated preparation method of the large-area transparent flexible electrode according to claim 6, wherein the organic polymer solution is used as a spinning solution, and PVA1788, PVA1750 or PVP solution is adopted, and the concentration is 10% -15%.
8. The integrated preparation method of the large-area transparent flexible electrode as claimed in claim 6 or 7, wherein the thickness of the nanofiber membrane is 200-500 nm.
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