Preparation method of transparent conductive adhesive film
The preparation method involving multiple molding and vacuum treatment solves the problem of poor adhesion between the conductive layer and the substrate resin, improving the compactness and conductivity of the conductive film, making it suitable for flexible electronic devices.
Patent Information
- Application Number
- CN202310578541.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-05-22
- Publication Date
- 2026-01-13
- Estimated Expiration
- 2043-05-22
AI Technical Summary
In the existing transparent conductive film manufacturing process, the poor adhesion between the conductive layer and the base resin results in large spacing between conductive ions and low efficiency during conduction, which cannot meet the requirements of flexible electronic devices.
The process involves multiple molding steps, including vacuuming inside the mold, pressurizing and injecting mixed materials, further extruding the conductive film using a vacuum molding machine, and then processing with a centrifuge and film cutting machine to ensure a tight bond of the conductive materials.
It improves the compactness and conductivity of the conductive film, enhances the adhesion between the conductive layer and the base resin, and is suitable for flexible electronic devices.
Smart Images

Figure CN116494455B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of conductive adhesive film preparation technology, and more specifically, to a method for preparing a transparent conductive adhesive film. Background Technology
[0002] The preparation of transparent flexible conductive materials and their application in electronic devices has been a research hotspot in the field of flexible electronics in recent years, and they are key materials for developing flexible displays, photovoltaics, and photoelectric detection devices. Currently, the most widely used ceramic-based transparent conductive materials such as tin oxide (TO) are brittle and prone to cracking under stress, which cannot meet the requirements of flexible electronic devices. Metal nanowire networks, represented by silver nanowires (Ag NW), may well meet the needs of transparent flexible conductivity, thus requiring the use of transparent conductive films for conductive connections.
[0003] A search of existing published literature reveals that patent CN102863913B discloses a method for preparing conductive films. This method addresses the issue that existing conductive films rarely use epoxy resin matrices because achieving a sufficiently soft surface is difficult; most use PET matrices. The preparation methods typically involve hot pressing, where conductive fillers are injected into the matrix resin while the matrix softens. While the surface resistivity of the resulting conductive film meets requirements, the bulk resistivity is very low. This leads to poor film properties and weak adhesion between the conductive layer and the matrix resin. Under bending and stretching, the conductive network can be damaged, reflected in experimental data as an increase in resistivity during stretching and bending. This patent, however, uses a different method: 25%–35% hydrogenated bisphenol A type epoxy resin; 22%–25% epoxy resin reactive diluent; 0.5%–1.5% UV-resistant additive; 20%–30% hydrogenated alicyclic amine; 2.5%–4% modified amine curing accelerator; and 12%–27% conductive filler. The transparent conductive adhesive film has not only low surface resistivity but also low volume resistivity. When made into films of different thicknesses, the transparent conductive adhesive film of this invention has the advantages of good transparency, high conductivity, and high bonding strength. The preparation method of this invention is simple, the raw materials are readily available, and the preparation conditions are not harsh. However, this patent has the following defects.
[0004] Although the above-mentioned preparation method can achieve conductivity when preparing transparent conductive adhesive film, it does not involve multiple molding processes. As a result, the outer and inner conductive layers of the mixed material have poor adhesion, the spacing between conductive ions is large, and the conductivity is low. Therefore, there is a need to provide a method for preparing transparent conductive adhesive film. Summary of the Invention
[0005] To overcome the above-mentioned defects of the prior art, the present invention provides a method for preparing a transparent conductive adhesive film.
[0006] To achieve the above objectives, the present invention provides the following technical solution: a method for preparing a transparent conductive adhesive film, comprising the following specific steps:
[0007] S1. Preparation of conductive liquid: Add 30-50 parts of metal oxide powder and 20-30 parts of polyanion in π-conjugated conductive polymer to a stirrer. Weigh 5-10 parts of ferrous nitrosyl sulfate, add 50-60 parts of anhydrous ethanol according to the stoichiometric molar ratio, add 10-30 parts of silanol salt, and add 5-10 parts of citric acid. Adjust the pH to 2-3 with ammonia water. Reflux the sample at 80℃ to hydrolyze and condense it, and then slowly evaporate it at 120℃ to achieve the transformation from solution to sol to gel. Dry the gel at 50℃ to obtain a dry gel, and obtain an integral tablet at 130℃. Soak the tablet in sodium chloride solution for 50-60 minutes and let it stand for 30-40 minutes to mix and produce a conductive liquid.
[0008] S2. Mixing materials: Add 10-30 parts of polybutadiene rubber latex, 5-15 parts of methyl methacrylate monomer, 6-10 parts of styrene monomer, and 5-15 parts of acrylonitrile monomer to a mixer. After mixing, add half of the conductive liquid. Mix at a speed of 120-160 r / min for 5-10 minutes to form a mixed material.
[0009] S3. Mold cleaning: The molding mold needs to be flushed with 20-50 parts of anhydrous ethanol under pressure. During flushing, the inner walls of the upper and lower molds should be flushed simultaneously. After flushing, a wiping cloth should be placed against the inner walls of the upper and lower molds and rotated counterclockwise to ensure that the molding mold is free of impurities.
[0010] S4. Injection molding: Heat the inside of the molding mold to 80-120℃ and evacuate the inside of the mold for 5-10 minutes. Then increase the pressure to 1200-2000Pa to inject the mixed material into the molding mold. After molding, open the valve to release the pressure inside the molding mold. Then pull the upper mold upward and the lower mold downward to open the entire molding mold. Take out the transparent conductive film inside the molding mold when it cools down to 38-40℃.
[0011] S5. Secondary conductive coating: Place the removed transparent conductive film inside a centrifuge. Centrifuge at a speed of 150-180 r / min for 10-20 min. When there are no liquid impurities on the outside of the transparent conductive film, add the other half of the conductive liquid into the centrifuge. The conductive liquid needs to soak the transparent conductive film for 10-30 minutes. Then set the temperature to 50-80℃ and keep it warm for 5-10 minutes. After keeping it warm, remove the secondary transparent conductive film.
[0012] S6. Vacuum molding: Place the secondary transparent conductive film into the vacuum molding machine, set the negative pressure value to 500-700Pa, and press for 5-20 minutes to make the air bubbles on the outside of the secondary transparent conductive film disappear. Then the secondary transparent conductive film can be taken out.
[0013] S7. Film cutting and forming: Place the secondary transparent conductive film on a hydraulic film cutting machine and cut it to a length of 50-60cm and a width of 10-20cm. Each time the film is cut, the inspector needs to randomly select 5-10 transparent conductive films and check whether the dimensions of each mold are qualified. Pack the qualified transparent conductive films into boxes and store them to complete the preparation of the transparent conductive film.
[0014] Preferably, the metal oxide powder in S1 is selected from zirconium, titanium, aluminum, zinc, indium and tin, and ligands selected from neopentyl trifluoroacetylacetone, acetylacetone, trifluoroacetylacetone and hexafluoroacetylacetone. The polyanion in the π-conjugated conductive polymer in S1 is poly(3,4-ethylenedioxythiophene) or polypyrrole. The dry gel in S1 is heat-treated at high temperature for a certain time to obtain ultrafine powder at 100°C. The powder is pressed into sheets (d=2-4mm) under a hydrostatic pressure of 200Pa.
[0015] Preferably, in step S2, the speed of the mixer is controlled at 40-60 r / min, the mixing time is 10-30 minutes, the temperature is heated to 80℃ and then kept at that temperature for 10-20 minutes, and the color of the mixed material in step S2 changes from yellow to transparent, and the color change waiting time is 10-20 minutes.
[0016] Preferably, the flushing pressure in step S3 is 100-300 Pa, the flushing time is not less than 5-10 minutes, and the flushing water temperature is maintained at 40-50℃.
[0017] Preferably, in step S4, 5-10 cooling fans are installed to cool the mold, and they are distributed sequentially on the outside of the mold. The distance between two adjacent cooling fans is set to 50-100cm.
[0018] Preferably, in step S6, 2-5 observers need to surround the secondary transparent conductive film 3-5 times, and they need to keep the same direction when surrounding it.
[0019] Preferably, the number of inspectors in S7 is set to 2-4, and after each inspection, personal information needs to be signed on the inspection form. Two copies of the inspection form need to be prepared.
[0020] The technical effects and advantages of this invention are as follows:
[0021] This invention involves injecting the mixed materials into a molding die, molding and pressing it, then opening a valve to release the internal pressure of the molding die, and then pulling the upper mold of the molding die upwards. Once there are no liquid impurities on the outside of the transparent conductive film, the other half of the conductive liquid is added to a centrifuge. The second transparent conductive film is then placed in a vacuum molding machine for pressing, which fully compresses and mixes the various conductive materials. The double pressing reduces the gaps between the conductive materials, improves the tightness, and therefore results in better conductivity.
[0022] This invention enables the addition of polyanions from metal oxide powder and π-conjugated conductive polymers into a mixer. Ferrous nitrosyl sulfate is weighed, and anhydrous ethanol is added according to the stoichiometric molar ratio. Citric acid is then added, and the pH is adjusted to 2-3 with ammonia. This process ensures that conductive ions are fully dispersed on each membrane, forming multi-point conductive connections. It also prevents the aggregation of conductive ions, resulting in uniform dispersion and better conductivity.
[0023] This invention employs a process of vacuuming the inside of the mold and then applying additional pressure to inject the mixed material into the molding mold. The secondary transparent conductive film is then placed in a vacuum molding machine under negative pressure, which eliminates air bubbles on the outside of the secondary transparent conductive film. Vacuuming is guaranteed during each molding process to ensure that external air cannot enter the interior of the film and to avoid the formation of micro-bubbles, thus effectively improving the tightness.
[0024] In summary, through the interaction of the above-mentioned multiple processes, the mixed materials are first injected into the molding mold, and after molding, the various conductive materials are fully squeezed and mixed. Then, ferrous sulfate is weighed, and anhydrous ethanol is added according to the stoichiometric molar ratio. Citric acid is then added, and the pH is adjusted to 2-3 with ammonia. This ensures that the conductive ions are fully dispersed on each membrane. Finally, after evacuating the mold, the secondary transparent conductive film is placed in a vacuum molding machine under negative pressure. All of these processes effectively improve the tightness and conductivity of the membrane, resulting in better conductivity. Attached Figure Description
[0025] Figure 1 This is a schematic diagram of the preparation method of a transparent conductive adhesive film according to the present invention. Detailed Implementation
[0026] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. Example
[0027] A method for preparing a transparent conductive adhesive film includes the following specific steps:
[0028] S1. Preparation of conductive liquid: 30 parts of metal oxide powder and 20 parts of polypyrrole are added to a mixer. 5 parts of ferrous nitrosyl sulfate are weighed and 50 parts of anhydrous ethanol are added according to the stoichiometric molar ratio. 10 parts of silanol salt and 5 parts of citric acid are added. The pH is adjusted to 2 with ammonia. The sample is refluxed at 80℃ to hydrolyze and condense. Then, it is slowly evaporated at 120℃ to achieve the transformation from solution to sol to gel. The sample is dried at 50℃ to obtain a dry gel. The dry gel is heat-treated at high temperature for a certain time to obtain an ultrafine powder at 100℃. The powder is pressed into a sheet (d=2mm) under a hydrostatic pressure of 200Pa. The sheet is then pressed into a whole tablet at 130℃. The tablet is immersed in sodium chloride solution for 50 minutes and allowed to stand for 30 minutes to mix and produce a conductive liquid.
[0029] S2. Mixing materials: Add 10 parts of polybutadiene rubber latex, 5 parts of methyl methacrylate monomer, 6 parts of styrene monomer, and 5 parts of acrylonitrile monomer to a mixer. Control the mixer speed at 40 r / min and the mixing time at 10 minutes. Heat to 80℃ and keep warm for 10 minutes. After mixing, add half of the conductive liquid and mix at 120 r / min for 5 minutes. The color of the mixed material changes from yellow to transparent, and the color change waiting time is 10 minutes to form the mixed material.
[0030] S3. Mold cleaning: The molding mold needs to be flushed with 20 parts of anhydrous ethanol under pressure. The flushing pressure is 100Pa and the flushing time is not less than 5 minutes. The flushing water temperature should be kept at 40℃. During flushing, the inner walls of the upper mold and the lower mold should be flushed simultaneously. After flushing, a wiping cloth should be placed on the inner walls of the upper mold and the lower mold and rotated counterclockwise to ensure that the molding mold is free of impurities.
[0031] S4. Injection molding: Heat the inside of the molding mold to 80°C and evacuate the inside of the mold for 5 minutes. Then, increase the pressure to 1200Pa to inject the mixed material into the molding mold. After molding, open the valve to release the pressure inside the molding mold. Then, pull the upper mold upward and the lower mold downward to open the entire molding mold. Remove the transparent conductive film inside the molding mold when it cools down to 38°C. Five cooling fans need to be installed for cooling. They are distributed in sequence on the outside of the molding mold, with a spacing of 50cm between adjacent cooling fans.
[0032] S5. Secondary conductive coating: Place the removed transparent conductive film inside a centrifuge. Centrifuge at a speed of 150 r / min for 10 min. When there are no liquid impurities on the outside of the transparent conductive film, add the other half of the conductive liquid into the centrifuge. The conductive liquid needs to soak the transparent conductive film for 10 minutes. Then set the temperature to 50℃ and keep it warm for 5 minutes. After keeping it warm, remove the secondary transparent conductive film.
[0033] S6. Vacuum molding: The secondary transparent conductive film is placed in a vacuum molding machine. The negative pressure value is set to 500Pa for 5 minutes to make the air bubbles on the outside of the secondary transparent conductive film disappear. Two observers need to surround the secondary transparent conductive film 3 times while keeping the same direction. Then the secondary transparent conductive film can be removed.
[0034] S7. Film cutting and forming: Place the secondary transparent conductive film on a hydraulic film cutting machine and cut it to a length of 50cm and a width of 10cm. Each time the film is cut, 5 transparent conductive films need to be randomly selected by 2 inspectors. After each inspection, personal information needs to be signed on the inspection form. Two copies of the inspection form need to be prepared. Check whether the dimensions of each mold are qualified. Pack the qualified transparent conductive films into boxes and store them to complete the preparation of the transparent conductive film. Example
[0035] A method for preparing a transparent conductive adhesive film includes the following specific steps:
[0036] S1. Preparation of conductive liquid: 40 parts of metal oxide powder and 25 parts of polypyrrole are added to a mixer. 8 parts of ferrous nitrosyl sulfate are weighed and 55 parts of anhydrous ethanol are added according to the stoichiometric molar ratio. 20 parts of silanol salt and 8 parts of citric acid are added. The pH is adjusted to 2 with ammonia. The sample is refluxed at 80℃ to hydrolyze and condense. Then, it is slowly evaporated at 120℃ to achieve the transformation from solution to sol to gel. The sample is dried at 50℃ to obtain a dry gel. The dry gel is heat-treated at high temperature for a certain time to obtain an ultrafine powder at 100℃. The powder is pressed into a sheet (d=3mm) under a hydrostatic pressure of 200Pa. The sheet is then placed in a sodium chloride solution for 55 minutes and allowed to stand for 35 minutes to mix and produce a conductive liquid.
[0037] S2. Mixing materials: Add 20 parts of polybutadiene rubber latex, 10 parts of methyl methacrylate monomer, 8 parts of styrene monomer, and 10 parts of acrylonitrile monomer to a mixer. Control the mixer speed at 50 r / min and the mixing time at 20 minutes. Heat to 80℃ and keep warm for 15 minutes. After mixing, add half of the conductive liquid and mix at 140 r / min for 8 minutes. The color of the mixed material changes from yellow to transparent, and the color change waiting time is 15 minutes to form the mixed material.
[0038] S3. Mold cleaning: The molding mold needs to be flushed with 30 parts of anhydrous ethanol under pressure. The flushing pressure is 200Pa and the flushing time is not less than 8 minutes. The flushing water temperature must be kept at 45℃. During flushing, the inner walls of the upper mold and the lower mold should be flushed simultaneously. After flushing, a wiping cloth should be placed against the inner walls of the upper mold and the lower mold and rotated counterclockwise to ensure that the molding mold is free of impurities.
[0039] S4. Injection molding: Heat the inside of the molding mold to 100℃ and evacuate the inside of the mold for 8 minutes. Then increase the pressure to 1800Pa to inject the mixed material into the molding mold. After molding, open the valve to release the pressure inside the molding mold. Then pull the upper mold upward and the lower mold downward to open the entire molding mold. Remove the transparent conductive film inside the molding mold when it cools down to 38-40℃. Cooling requires the installation of 8 cooling fans, which are distributed in sequence on the outside of the molding mold. The distance between two adjacent cooling fans is set to 50-100cm.
[0040] S5. Secondary conductive coating: Place the removed transparent conductive film inside a centrifuge. Centrifuge at a speed of 170 r / min for 15 min. When there are no liquid impurities on the outside of the transparent conductive film, add the other half of the conductive liquid into the centrifuge. The conductive liquid needs to soak the transparent conductive film for 20 minutes. Then set the temperature to 70℃ and keep it warm for 8 minutes. After keeping it warm, remove the secondary transparent conductive film.
[0041] S6. Vacuum molding: Place the secondary transparent conductive film into the vacuum molding machine and set the negative pressure to 600Pa for 10 minutes to make the air bubbles on the outside of the secondary transparent conductive film disappear. Two observers need to surround the secondary transparent conductive film 3-5 times while keeping the same direction when circling. Then the secondary transparent conductive film can be removed.
[0042] S7. Film cutting and forming: Place the secondary transparent conductive film on a hydraulic film cutting machine and cut it to a length of 55cm and a width of 15cm. Each time the film is cut, 8 transparent conductive films need to be randomly selected by 3 inspectors. After each inspection, personal information needs to be signed on the inspection form. Two copies of the inspection form need to be prepared. Check whether the dimensions of each mold are qualified. Pack the qualified transparent conductive films into boxes and store them to complete the preparation of the transparent conductive film. Example
[0043] A method for preparing a transparent conductive adhesive film includes the following specific steps:
[0044] S1. Preparation of conductive liquid: 50 parts of metal oxide powder and 30 parts of polypyrrole are added to a mixer. 10 parts of ferrous nitrosyl sulfate are weighed and 60 parts of anhydrous ethanol are added according to the stoichiometric molar ratio. 30 parts of silanol salt and 10 parts of citric acid are added. The pH is adjusted to 3 with ammonia. The sample is refluxed at 80℃ to hydrolyze and condense. Then, it is slowly evaporated at 120℃ to achieve the transformation from solution to sol to gel. The sample is dried at 50℃ to obtain a dry gel. The dry gel is heat-treated at high temperature for a certain time to obtain an ultrafine powder at 100℃. The powder is pressed into a sheet (d=4mm) under a hydrostatic pressure of 200Pa. The sheet is then placed in a sodium chloride solution for 60 minutes and allowed to stand for 40 minutes to mix and produce a conductive liquid.
[0045] S2. Mixing materials: Add 30 parts of polybutadiene rubber latex, 15 parts of methyl methacrylate monomer, 10 parts of styrene monomer, and 15 parts of acrylonitrile monomer to a mixer. Control the mixer speed at 60 r / min and the mixing time at 30 minutes. Heat to 80℃ and keep warm for 20 minutes. After mixing, add half of the conductive liquid and mix at 160 r / min for 10 minutes. The color of the mixed material changes from yellow to transparent, and the color change waiting time is 20 minutes to form the mixed material.
[0046] S3. Mold cleaning: The molding mold needs to be flushed with 50 parts of anhydrous ethanol under pressure. The flushing pressure is 300Pa and the flushing time is not less than 10 minutes. The flushing water temperature must be kept at 50℃. During flushing, the inner walls of the upper mold and the lower mold should be flushed simultaneously. After flushing, a wiping cloth should be placed against the inner walls of the upper mold and the lower mold and rotated counterclockwise to ensure that the molding mold is free of impurities.
[0047] S4. Injection molding: Heat the inside of the molding mold to 120℃ and evacuate the inside of the mold for 10 minutes. Then increase the pressure to 2000Pa to inject the mixed material into the molding mold. After molding, open the valve to release the pressure inside the molding mold. Then pull the upper mold upward and the lower mold downward to open the entire molding mold. Remove the transparent conductive film inside the molding mold when it cools down to 40℃. Cooling requires the installation of 10 cooling fans, which are distributed in sequence on the outside of the molding mold. The distance between two adjacent cooling fans is set to 100cm.
[0048] S5. Secondary conductive coating: Place the removed transparent conductive film inside a centrifuge. Centrifuge at a speed of 180 r / min for 20 min. When there are no liquid impurities on the outside of the transparent conductive film, add the other half of the conductive liquid into the centrifuge. The conductive liquid needs to soak the transparent conductive film for 30 minutes. Then set the temperature to 80℃ and keep it warm for 10 minutes. After keeping it warm, remove the secondary transparent conductive film.
[0049] S6. Vacuum molding: The secondary transparent conductive film is placed in a vacuum molding machine and the negative pressure is set to 700Pa for 20 minutes to make the air bubbles on the outside of the secondary transparent conductive film disappear. Five observers need to surround the secondary transparent conductive film five times while keeping the same direction when circling. Then the secondary transparent conductive film can be removed.
[0050] S7. Film cutting and forming: Place the secondary transparent conductive film on a hydraulic film cutting machine and cut it to a length of 60cm and a width of 20cm. Each time the film is cut, 10 transparent conductive films need to be randomly selected by 4 inspectors. After each inspection, personal information needs to be signed on the inspection form. Two copies of the inspection form need to be prepared. Check whether the dimensions of each mold are qualified. Pack the qualified transparent conductive films into boxes and store them to complete the preparation of the transparent conductive film.
[0051] Transmission rate % Resistivity (Ω·m) Temperature resistance ℃ Example 1 92 25 380 Example 2 91 20 360 Example 3 92.8 18 395
[0052] By comparing the above three sets of embodiments, it can be seen that Embodiment 3 has the highest transmittance, thus having a better transparency effect. It also has the lowest resistivity, resulting in a better conductivity effect and a higher conductivity resistance temperature. Therefore, by fully extruding and mixing various conductive materials and performing double film pressing, the gaps between conductive materials are reduced, and the tightness is improved, thus resulting in better conductivity.
[0053] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.
Claims
1. A method for preparing a transparent conductive adhesive film, characterized by: The specific steps include: S1, preparation of conductive liquid, metal oxide powder 30-50 parts, polyanion in π conjugated system conductive polymer 20-30 parts, into the blender, and weigh nitrosyl iron sulfate 5-10 parts, according to the stoichiometric molar ratio of anhydrous ethanol 50-60 parts, and add silanol 10-30 parts, add citric acid 5-10 parts, adjust pH to 2-3 with ammonia water, sample is refluxed at 80℃ to hydrolyze and condense, then slowly evaporated at 120℃ to realize the conversion of solution-sol-gel, dried at 50℃ to get dry gel, get whole tablet at 130℃, put the tablet in sodium chloride solution for 50-60 minutes, stand for 30-40 minutes, mix to produce conductive liquid; S2, mixing materials, adding polybutadiene rubber latex 10-30 parts, methyl methacrylate monomer 5-15 parts, styrene monomer 6-10 parts, acrylonitrile monomer 5-15 parts into the mixer, mixing, then adding half of the conductive liquid at a speed of 120-160 r / min, mixing time is 5-10 minutes, forming mixed materials; S3, mold cleaning, the forming mold needs to be washed with anhydrous ethanol 20-50 parts, and the upper mold inner wall and the lower mold inner wall of the forming mold need to be washed synchronously during washing, then wipe the upper mold inner wall and the lower mold inner wall with a cloth and rotate counterclockwise to ensure that the forming mold is free of impurities; S4, injection molding, heat the inside of the forming mold to 80-120℃, and vacuum the inside of the mold for 5-10 minutes, then pressurize to 1200-2000 Pa to make the mixed materials enter the forming mold, open the valve to release the pressure in the mold, pull the upper mold of the forming mold upward, the lower mold of the forming mold acts as a downward pull, the whole forming mold is opened, and the transparent conductive film in the forming mold is taken out when the temperature of the transparent conductive film is reduced to 38-40℃; S5, secondary conductive film coating, place the taken transparent conductive film in the centrifuge, the centrifuge rotates at a speed of 150-180 r / min, and the centrifugation time is 10-20 min, then add the other half of the conductive liquid into the centrifuge, and the conductive liquid needs to soak the transparent conductive film for 10-30 minutes, then set the temperature to 50-80℃ for 5-10 minutes, and take out the secondary transparent conductive film after the temperature is kept constant; S6, vacuum molding, put the secondary transparent conductive film into the vacuum molding machine, set the negative pressure value to 500-700 Pa, and keep the negative pressure for 5-20 minutes to make the bubbles outside the secondary transparent conductive film disappear, then take out the secondary transparent conductive film; S7, film cutting, place the secondary transparent conductive film on the hydraulic film cutting machine, cut the film to a length of 50-60 cm and a width of 10-20 cm, and randomly select 5-10 pieces of transparent conductive film for each cutting to check the size of each mold, pack and store the qualified transparent conductive film, and the preparation of the transparent conductive film is completed.
2. The method for preparing a transparent conductive adhesive film according to claim 1, characterized in that: The metal oxide powder in S1 is selected from the group consisting of zirconium, titanium, aluminum, zinc, indium and tin, and a ligand selected from the group consisting of pivaloyltrifluoroacetylacetone, acetylacetone, trifluoroacetylacetone and hexafluoroacetylacetone. 3.The method of claim 1, wherein the transparent conductive adhesive film is prepared by the steps of: coating a transparent conductive layer on a substrate; coating a transparent adhesive layer on the transparent conductive layer; and coating a protective layer on the transparent adhesive layer. The polyanion in the π-conjugated conductive polymer in S1 is poly(3,4-ethylenedioxythiophene) or polypyrrole.
4. The method for preparing a transparent conductive adhesive film according to claim 1, characterized in that: The xerogel in S1 is heat treated at high temperature for a certain period of time to obtain ultrafine powder at 100°C, and the powder is pressed into a sheet (d=2-4mm) under a hydrostatic pressure of 200Pa.
5. The method for preparing a transparent conductive adhesive film according to claim 1, characterized in that: The rotation speed of the mixer in S2 is controlled at 40-60r / min, and the mixing time is 10-30 minutes, and the temperature is heated to 80°C and then kept for 10-20 minutes.
6. The method for preparing a transparent conductive adhesive film according to claim 1, characterized in that: The color of the mixed material in S2 changes from yellow to transparent, and the waiting time for color change is 10-20 minutes. 7.The method of claim 1, wherein the transparent conductive adhesive film is prepared by the steps of: coating a transparent conductive layer on a substrate; coating a transparent adhesive layer on the transparent conductive layer; and coating a protective layer on the transparent adhesive layer. The flushing pressure in S3 is 100-300Pa, the flushing time is not less than 5-10 minutes, and the flushing water temperature needs to be kept at 40-50°C. 8.The method of claim 1, wherein the transparent conductive adhesive film is prepared by the steps of: coating a transparent conductive layer on a substrate; coating a transparent adhesive layer on the transparent conductive layer; and coating a protective layer on the transparent adhesive layer. In S4, 5-10 heat dissipation fans are installed to cool down, which are distributed in the external position of the forming mold, and the distance between the adjacent two heat dissipation fans is 50-100cm. 9.The method of claim 1, wherein the transparent conductive adhesive film is prepared by the steps of: coating a transparent conductive layer on a substrate; coating a transparent adhesive layer on the transparent conductive layer; and coating a protective layer on the transparent adhesive layer. In S6, 2-5 observers are needed to surround the secondary transparent conductive film for 3-5 circles, and the same direction is maintained during the surrounding. 10.The method of claim 1, wherein the transparent conductive adhesive film is prepared by the steps of: coating a transparent conductive layer on a substrate; coating a transparent adhesive layer on the transparent conductive layer; and coating a protective layer on the transparent adhesive layer. The number of inspectors in S7 is set to 2-4, and after each inspection, the personal information needs to be signed on the inspection table, and two copies of the inspection table need to be prepared.
Citation Information
Patent Citations
Novel transparent conductive film and preparation method thereof
CN102863913B
Preparation method of nickel-based silver conductive slurry
CN102723142A
Formula and preparation method of epoxy resin based anisotropic conductive adhesive film
CN104673111A