Preparation process of high-transparency conductive film

Abstract

The invention relates to the field of conductive film material processing, and particularly discloses a preparation process of a high-transparency conductive film, which comprises the following steps: S1, mixing aluminum oxide and zinc oxide to obtain mixed powder, grinding, and sintering to obtain an AZO target material; antimony trioxide and tin oxide are mixed to obtain a mixture, and the mixture is sintered into an ATO target material after being subjected to spheroidal graphite treatment; s2, mixing an AZO target material and an ATO target material to obtain a composite material, stirring to obtain a mixed material, sputtering the mixed material on a substrate through magnetron sputtering, controlling the preheating temperature of the substrate at 55-65 DEG C, and coating to obtain a finished product, the transparent conductive film has the advantages of high transparency, good conductivity and good flexibility.

Description

Technical Field

[0001] This application relates to the field of conductive film material processing, and more specifically, it relates to a process for preparing a highly transparent conductive film. Background Technology

[0002] Transparent conductive films are thin films that are both conductive and highly transparent in the visible light range. They mainly include metal film systems, oxide film systems, other compound film systems, polymer film systems, and composite film systems. Transparent conductive film materials have broad application prospects in many fields such as liquid crystal displays, touch screens, solar cells, and flexible displays.

[0003] Transparent conductive films combine high transmittance and low resistivity, meeting the requirements of display devices, solar cells and other devices for photoelectric synergy. Taking ITO thin films as an example, by adjusting the ratio of doping with tin oxide, the balance between transmittance and conductivity can be optimized. However, ITO thin films are brittle and cannot withstand bending or stretching, which limits their application in flexible electronic devices.

[0004] Therefore, how to prepare a thin film with high transparency, good conductivity, and good flexibility is a problem that needs to be solved. Summary of the Invention

[0005] In order to prepare a thin film with high transparency, good conductivity and good flexibility, this application provides a process for preparing a highly transparent conductive film.

[0006] This application provides a process for preparing a highly transparent conductive film, using the following technical solution: A process for preparing a highly transparent conductive film includes the following steps: S1. Alumina and zinc oxide are mixed to obtain a powder mixture, which is then ground and sintered into an AZO target material; antimony trioxide and tin oxide are mixed to obtain a mixture, which is then sintered into an ATO target material after ductile iron treatment. S2. After mixing AZO target material and ATO target material to obtain composite material, the mixture is stirred to obtain mixed material. The mixed material is then magnetron sputtered onto the substrate. The substrate preheating temperature is controlled at 55-65℃. After coating, the finished product is obtained.

[0007] By adopting the above technical solution, a target material is prepared by sintering alumina and zinc oxide together. Aluminum doping can replace the zinc sites, form free electrons, reduce resistivity, and improve conductivity. Furthermore, antimony trioxide and tin oxide can also exchange, reducing resistivity, thereby giving the sputtered film layer of the target material high conductivity.

[0008] Limiting the preheating temperature of the substrate suppresses excessive grain growth, reduces light scattering, and thus improves transparency. Furthermore, a substrate at 55-65°C can form a flexible transition layer during sputtering (AZO first, then ATO), further enhancing the flexibility of the film.

[0009] Preferably, the parameters of the magnetron sputtering are: the distance from the mixed material to the substrate is 90-110 mm, the magnetron sputtering working pressure is 0.4-0.6 Pa, and the hydrogen flow rate is 15-17 sccm.

[0010] By adopting the above technical solution and limiting the distance, sputtered particles undergo more collisions before reaching the substrate, resulting in a more uniform energy distribution. This helps to form a low-stress film, suppress crack formation, and improve the flexibility of the finished film.

[0011] Under low voltage conditions of 0.4-0.6 Pa, the mean free path of sputtered ions is longer, and the particles retain higher kinetic energy when they reach the substrate, which improves the density of the finished film, reduces crystallization defects, and lowers resistivity. Under low voltage conditions, the sputtered particles have higher energy, which can effectively suppress light scattering and improve the transparency of the film.

[0012] By limiting the hydrogen flow rate and utilizing the reducing properties of hydrogen, oxygen vacancy defects in AZO / ATO are reduced, increasing the concentration of free electrons, further reducing resistivity, and improving conductivity. Hydrogen doping can also improve the smoothness of the film surface, reduce light reflection loss, and ensure that the film has high transmittance.

[0013] Preferably, the specific steps of the stirring treatment in S2 are as follows: Toluene solution is added to the composite material, and then a silane coupling agent is added, the silane coupling agent accounting for 1-2% of the mass of the composite material. The mixture is stirred evenly and reacted at 68-74℃ for 2-3 hours, and then the toluene solvent is removed.

[0014] By adopting the above technical solution, toluene, as a solvent, can effectively dissolve residual grease or organic matter on the target surface, reduce film defects caused by impurities during sputtering, improve film smoothness, reduce light reflection loss, and improve transmittance. Furthermore, the target surface treated with toluene is more likely to expose active sites such as hydroxyl groups, providing connection points for subsequent bonding of silane coupling agents.

[0015] With the addition of silane coupling agent and a limited temperature, the silane coupling agent can react with the hydroxyl groups on the surface of AZO and ATO targets, improving the compatibility and adhesion between the target and the substrate. The uniform coupling layer formed on the target surface can reduce sputtered particle scattering, improve carrier mobility, and enhance conductivity.

[0016] Preferably, the silane coupling agent is composed of an aminosilane coupling agent and a hydroxysilane coupling agent in a mass ratio of 1:0.5-1.

[0017] By adopting the above technical solution, the amino group in the aminosilane coupling agent can easily connect with the hydroxyl group on the target surface. In addition, the amino group can also interact with organic matter in the subsequent sputtering process, reduce the interface defect density, and improve the adhesion of the film layer, so that the sputtered film layer can be stably attached to the substrate surface. At the same time, the reducing property of the amino group can inhibit the oxidation of zinc ions in the AZO target material, reduce oxygen vacancy defects, and improve conductivity.

[0018] The combination of aminosilane coupling agents and hydroxysilane coupling agents allows the amino and hydroxyl groups to be linked by hydrogen bonds, resulting in a tighter bond between the silane coupling agents and an increase in the density of the finished film. This, in turn, improves both conductivity and conductivity uniformity. The hydroxyl groups in the hydroxysilane coupling agent can connect with the hydroxyl groups on the target surface, complementing the aminosilane coupling agent and optimizing the deposition uniformity of sputtered particles. Furthermore, the polar effect of the hydroxyl groups in the silane coupling agent reduces light scattering loss, thus ensuring the transparency of the film.

[0019] Preferably, in S1, zinc oxide accounts for 1.5-2% of the mass of aluminum oxide, antimony trioxide accounts for 1.60-2.35% of the mass of tin oxide, and in S2, the mass ratio of AZO target material to ATO target material is 1:0.8-1.5.

[0020] By adopting the above technical solution and limiting the ratio between raw materials, the sputtered film layer can have high conductivity, high transparency, and good flexibility.

[0021] Preferably, 0.25-0.38% by weight of epoxy-based polyethylene glycol dopamine is added to the powder mixture of S1, and then it is ground.

[0022] By adopting the above technical solution, the epoxy groups in epoxy-based polyethylene glycol dopamine facilitate ring-opening reactions with the hydroxyl groups on the surfaces of alumina and zinc oxide, thereby improving the bonding strength between particles inside the target material and reducing the generation of grain boundary cracks during sintering. The catechol groups of dopamine further stabilize the dispersion of zinc and chloride ions through metal chelation, inhibiting abnormal grain growth during high-temperature sintering. In addition, the polyethylene glycol segments improve the density of the target material, enabling the sputtering of the target material onto the substrate surface to further enhance the flexibility of the finished film.

[0023] Preferably, the specific steps of the spheroidizing process in S1 are as follows: First, add 0.2-0.4% by weight of polyethylene glycol microparticles to the mixture, spheroidize the microparticles during the addition process, and then perform post-treatment after spheroidizing.

[0024] By adopting the above technical solution, polyethylene glycol microparticles can be uniformly mixed with antimony trioxide and tin oxide. The polar segments in the polyethylene glycol microparticles are adsorbed onto the surface of tin oxide and antimony trioxide powders through hydrogen bonds, weakening the van der Waals forces between particles and reducing hard agglomeration caused by mechanical forces during the sputtering process. Furthermore, polyethylene glycol undergoes pyrolysis during high-temperature sintering, releasing moisture and carbon dioxide to form micro- and nano-scale pores, relieving sintering shrinkage stress, preventing target material cracking, and ensuring the toughness and strength of the target material. The carbon after polyethylene glycol decomposition can also migrate in the grain boundaries, inhibiting abnormal grain enlargement and optimizing the conductivity and conductivity uniformity of the target material. After the target material is sputtered into a film, the finished film layer has good conductivity and flexibility.

[0025] Preferably, the post-processing steps are as follows: after spheroidizing, 0.12-0.24% by mass of hydroxyapatite nanowires are added to the ball milling material. During the addition process, the ball milling material is continuously stirred at a speed of 500-1000 r / min to ensure uniform mixing.

[0026] By adopting the above technical solution, the combination of hydroxyapatite nanowires and polyethylene glycol can promote the uniform distribution of hydroxyapatite nanowires in antimony trioxide and tin oxide. The high specific surface area and high flexibility of hydroxyapatite nanowires further improve the density of sputtered film, and ensure grain boundary penetration to avoid agglomeration, thereby refining grain size and reducing resistivity, so that the finished film has high conductivity and good flexibility.

[0027] Preferably, the substrate is a PET film.

[0028] By adopting the above technical solution, the PET film has high transparency and good flexibility. As a substrate, after sputtering, the finished film layer has high transparency while also having good flexibility and conductivity.

[0029] Preferably, the PET film is made from a PET base film through oxygen plasma treatment.

[0030] By adopting the above technical solution, oxygen plasma treatment can improve the surface roughness of PET base film, enhance the adhesion effect and stability between sputtered particles and base film, and form chemical bonds with oxygen-containing polar groups adsorbing sputtered particles, thereby strengthening the interfacial bonding strength and improving the flexibility, strength and conductivity uniformity of the film layer.

[0031] In summary, this application has the following beneficial effects: 1. Target materials are prepared by sintering a mixture of alumina and zinc oxide. Aluminum doping can replace zinc sites, forming free electrons, reducing resistivity, and improving conductivity. Furthermore, antimony trioxide and tin oxide can exchange, further reducing resistivity, thus resulting in a film with high conductivity after sputtering. Limiting the substrate preheating temperature suppresses excessive grain growth, reduces light scattering, and improves transparency. A substrate temperature of 55-65℃ allows for the formation of a flexible transition layer during sputtering (AZO followed by ATO), further enhancing the film's flexibility. 2. Toluene, as a solvent, can effectively dissolve residual grease or organic matter on the target surface, reduce film defects caused by impurities during sputtering, improve film flatness, reduce light reflection loss, and increase transmittance. Furthermore, the target surface treated with toluene is more likely to expose active sites such as hydroxyl groups, providing connection points for subsequent bonding of silane coupling agents. With the addition of silane coupling agents and a limited temperature, the silane coupling agents can react with the hydroxyl groups on the surface of AZO and ATO targets, improving the compatibility and adhesion between the target and the substrate. The uniform coupling layer formed on the target surface can reduce sputtering particle scattering, increase carrier mobility, and improve conductivity.

[0032] 3. The combination of hydroxyapatite nanowires and polyethylene glycol can promote the uniform distribution of hydroxyapatite nanowires in antimony trioxide and tin oxide. The high specific surface area and high flexibility of hydroxyapatite nanowires further improve the density of sputtered films, and ensure grain boundary penetration to avoid agglomeration, thereby refining grain size and reducing resistivity, so that the finished film has high conductivity and good flexibility. Detailed Implementation

[0033] The present application will be further described in detail below with reference to the embodiments.

[0034] All of the following ingredients are commercially available. Example

[0035] Of the following raw materials, epoxy-based polyethylene glycol dopamine was purchased from Shanghai Tuoyang Biotechnology Co., Ltd.; all other raw materials are commercially available.

[0036] Example 1: A preparation process for a highly transparent conductive film: S1. Alumina and zinc oxide are mixed, with zinc oxide accounting for 1.85% of the mass of alumina, to obtain a mixed powder. The powder is then ground to an average particle size of 3 μm, and then heated to 1300℃ at a heating rate of 5℃ / min. It is sintered at 15 MPa for 8 hours to obtain AZO target material. Antimony trioxide and tin oxide powders are mixed to obtain a mixture, with antimony trioxide accounting for 2% of the mass of tin oxide. The mixture is spheroidized to an average particle size of 5 μm, and then heated to 1350℃ at a heating rate of 5℃ / min. It is sintered at 15 MPa for 8 hours to obtain ATO target material. S2. Mix 1 kg of AZO target material and 1 kg of ATO target material to obtain a composite material. Then add 10 kg of toluene solution and mix thoroughly. Add 0.03 kg of silane coupling agent, which consists of aminosilane coupling agent and hydroxysilane coupling agent in a mass ratio of 1:0.8. Mix thoroughly and react at 70°C for 2.5 h. Then remove the toluene solvent to obtain a mixed material. Sputter the mixed material onto a substrate using magnetron sputtering. The distance between the mixed material and the substrate is 100 mm. The magnetron sputtering working pressure is 0.5 Pa, the hydrogen flow rate is 16 sccm, and the substrate preheating temperature is controlled at 60°C. The substrate is a PET film, which is prepared by oxygen plasma treatment of PET base film for 2 min. After magnetron sputtering, the finished product is obtained.

[0037] Example 2: The difference between this example and Example 1 is that: S1. Alumina and zinc oxide are mixed, with zinc oxide accounting for 1.6% of the mass of alumina, to obtain a mixed powder. The powder is then ground to an average particle size of 3 μm, and then heated to 1300℃ at a heating rate of 5℃ / min. It is sintered at 15 MPa for 8 h to obtain AZO target material. Antimony trioxide and tin oxide powders are mixed to obtain a mixture, with antimony trioxide accounting for 1.52% of the mass of tin oxide. The mixture is spheroidized to an average particle size of 5 μm, and then heated to 1350℃ at a heating rate of 5℃ / min. It is sintered at 15 MPa for 8 h to obtain ATO target material. S2. Mix 1 kg of AZO target material and 0.8 kg of ATO target material to obtain a composite material. Then add 10 kg of toluene solution and mix thoroughly. Add 0.018 kg of silane coupling agent, which consists of aminosilane coupling agent and hydroxysilane coupling agent in a mass ratio of 1:0.5. Mix thoroughly and react at 68℃ for 3 hours. Then remove the toluene solvent to obtain a mixed material. Sputter the mixed material onto a substrate using magnetron sputtering. The distance between the mixed material and the substrate is 90 mm. The magnetron sputtering working pressure is 0.4 Pa, the hydrogen flow rate is 15 sccm, and the substrate preheating temperature is controlled at 55℃. The substrate is a PET film, which is prepared by oxygen plasma treatment of PET base film for 2 minutes. After magnetron sputtering, the finished product is obtained.

[0038] Example 3: The difference between this example and Example 1 is that: S1. Alumina and zinc oxide are mixed, with zinc oxide accounting for 2% of the mass of alumina, to obtain a mixed powder. The powder is then ground to an average particle size of 3 μm, and then heated to 1300℃ at a heating rate of 5℃ / min. The powder is sintered at 15 MPa for 8 hours to obtain AZO target material. Antimony trioxide and tin oxide powders are mixed to obtain a mixture, with antimony trioxide accounting for 2.35% of the mass of tin oxide. The mixture is spheroidized to an average particle size of 5 μm, and then heated to 1350℃ at a heating rate of 5℃ / min. The mixture is sintered at 15 MPa for 8 hours to obtain ATO target material. S2. Mix 1 kg of AZO target material and 1.5 kg of ATO target material to obtain a composite material. Then add 10 kg of toluene solution and mix thoroughly. Add 0.05 kg of silane coupling agent, which consists of aminosilane coupling agent and hydroxysilane coupling agent in a mass ratio of 1:1. Mix thoroughly and react at 74℃ for 2 hours. Then remove the toluene solvent to obtain a mixed material. Sputter the mixed material onto a substrate using magnetron sputtering. The distance between the mixed material and the substrate is 110 mm. The magnetron sputtering working pressure is 0.6 Pa, the hydrogen flow rate is 17 sccm, and the substrate preheating temperature is controlled at 65℃. The substrate is a PET film, which is prepared by oxygen plasma treatment of PET base film for 2 minutes. After magnetron sputtering, the finished product is obtained.

[0039] Example 4: The difference between this example and Example 1 is that: S1. Alumina and zinc oxide are mixed, with zinc oxide accounting for 1.85% of the mass of alumina, to obtain a mixed powder. 0.32% (by mass) of epoxy-based polyethylene glycol dopamine is added to the mixed powder, which is then ground to an average particle size of 3 μm. The mixture is then heated to 1300℃ at a heating rate of 5℃ / min and sintered at 15 MPa for 8 hours to obtain an AZO target. Antimony trioxide and tin oxide powders are mixed, with antimony trioxide accounting for 2.25% (by mass of tin oxide), and mixed uniformly to obtain a mixture. Polyethylene glycol microparticles (0.3% by weight) were added to the mixture, and spheroidization was performed during the addition process to obtain spheroidized material. Hydroxyapatite nanowires (0.2% by weight) with an average length of 50 nm were added to the ball milling material. During the addition process, the ball milling material was continuously stirred at a speed of 800 r / min to ensure uniform mixing. The spheroidized material was spheroidized to an average particle size of 5 μm, and then heated to 1350℃ at a heating rate of 5℃ / min. The material was sintered at a pressure of 15 MPa for 8 h to obtain the ATO target material.

[0040] Example 5: The difference between this example and Example 1 is that: S1. Alumina and zinc oxide are mixed, with zinc oxide accounting for 1.85% of the mass of alumina, to obtain a mixed powder. 0.25% (by mass) of epoxy-based polyethylene glycol dopamine is added to the mixed powder, which is then ground to an average particle size of 3 μm. The mixture is then heated to 1300℃ at a rate of 5℃ / min and sintered at 15 MPa for 8 hours to obtain an AZO target. Antimony trioxide and tin oxide powders are mixed, with antimony trioxide accounting for 2.25% (by mass of tin oxide), and mixed uniformly to obtain a mixture. Polyethylene glycol microparticles (0.2% by weight) were added to the mixture, and spheroidization was performed during the addition process to obtain spheroidized material. Hydroxyapatite nanowires (0.2% by weight) with an average length of 50 nm were added to the ball milling material. During the addition process, the ball milling material was continuously stirred at a speed of 800 r / min to ensure uniform mixing. The material was spheroidized to an average particle size of 5 μm, and then heated to 1350 °C at a heating rate of 5 °C / min. The material was sintered at a pressure of 15 MPa for 8 h to obtain the ATO target material.

[0041] Example 6: The difference between this example and Example 1 is that: S1. Alumina and zinc oxide are mixed, with zinc oxide accounting for 1.85% of the mass of alumina, to obtain a mixed powder. 0.38% of the mass of epoxy-based polyethylene glycol dopamine is added to the mixed powder, which is then ground to an average particle size of 3 μm. The mixture is then heated to 1300℃ at a heating rate of 5℃ / min and sintered at 15 MPa for 8 hours to obtain an AZO target. Antimony trioxide and tin oxide powders are mixed, with antimony trioxide accounting for 2.25% of the mass of tin oxide. The mixture is homogeneous to obtain a mixed material. First, add... 0.4% by weight of polyethylene glycol microparticles were added to the mixture, and spheroidization was carried out during the addition process to obtain spheroidized material. 0.24% by weight of hydroxyapatite nanowires with an average length of 50 nm were added to the ball milling material. During the addition process, the ball milling material was continuously stirred at a speed of 1000 r / min to mix evenly. The spheroidized material was spheroidized to an average particle size of 5 μm, and then heated to 1350℃ at a heating rate of 5℃ / min. The material was sintered at a pressure of 15 MPa for 8 h to obtain ATO target material.

[0042] Example 7: The difference between this example and Example 1 is that: No silane coupling agent was added to S1.

[0043] Example 8: The difference between this example and Example 4 is that: S1 does not contain epoxy-based polyvinyl alcohol dopamine.

[0044] Example 9: The difference between this example and Example 4 is that: No polyethylene glycol microparticles were added to S1.

[0045] Example 10: The difference between this example and Example 4 is that: No hydroxyapatite nanowires were added to S1.

[0046] Comparative Example Comparative Example 1: The difference between this comparative example and Example 1 is that: The preheating temperature is 120℃.

[0047] Performance testing 1. Transparency Detection Finished films were prepared using the methods of Examples 1-6 and Comparative Example 1, respectively. The transmittance was tested and the data were recorded in accordance with GB / T2410.

[0048] 2. Conductivity testing Finished films were prepared using the methods described in Examples 1-7 and 9, respectively. Resistivity was tested and data were recorded in accordance with GB / T26598.

[0049] 3. Flexibility test Finished films were prepared using the methods of Examples 1-10 and Comparative Example 1, respectively. A bending tester was used to bend the films 20,000 times at a bending radius of 3 mm, and the increase in resistivity was detected. The greater the increase in resistivity, the worse the flexibility. The data were recorded.

[0050] Table 1 Performance Test Table (In the table, " / " indicates that the corresponding embodiment or comparative example did not test this item, so there is no data) project transmittance / % resistivity / Ω·cm resistivity increase / % Example 1 91.4 <![CDATA[3.3×10 -4 ]]> 4.8 Example 2 91.1 <![CDATA[3.6×10 -4 ]]> 5.0 Example 3 91.6 <![CDATA[3.1×10 -4 ]]> 4.7 Example 4 92.8 <![CDATA[2.2×10 -4 ]]> 3.7 Example 5 92.6 <![CDATA[2.4×10 -4 ]]> 3.9 Example 6 92.9 <![CDATA[2.1×10 -4 ]]> 3.5 Example 7 / <![CDATA[4.2×10 -4 ]]> 5.4 Example 8 / / 4.2 Example 9 / <![CDATA[2.7×10 -4 ]]> 4.3 Example 10 / / 4.5 Comparative Example 1 89.8 / 5.6 As can be seen from Examples 1-3 and Table 1, the conductive film prepared in this application has high transmittance, low resistivity, and a small increase in resistivity after bending, indicating that the conductive film has the advantages of high transparency, high conductivity, and high flexibility.

[0051] As can be seen from Examples 1 and 4-6 and Table 1, adding epoxy-based polyethylene glycol dopamine to treat AZO targets and adding polyethylene glycol microparticles and hydroxyapatite nanowires to treat ATO targets can improve the transparency, conductivity and flexibility of conductive films.

[0052] Combining Examples 1 and 7 with Table 1, it can be seen that no silane coupling agent was added in Example 7S1. Compared with Example 1, the resistivity of Example 7 is greater than that of Example 1, and the increase in resistivity is greater than that of Example 1. This indicates that the addition of silane coupling agent can react with the hydroxyl groups on the surface of AZO and ATO targets, improving the compatibility and adhesion between the target and the substrate. The uniform coupling layer formed on the target surface can reduce sputtered particle scattering, improve carrier mobility, and improve conductivity; it can also reduce light scattering loss, ensure transparency, and maintain flexibility.

[0053] Combining Examples 4 and 8-10 with Table 1, it can be seen that no epoxy-based polyvinyl alcohol dopamine was added in Example 8S1. Compared with Example 4, the resistivity increase in Example 8 was greater than that in Example 4. This indicates that epoxy-based polyethylene glycol dopamine inhibits abnormal grain growth during high-temperature sintering and improves the flexibility of the target material. After the target material is sputtered onto the substrate surface, it can further improve the flexibility of the finished film.

[0054] In Example 9S1, no polyethylene glycol microparticles were added. Compared to Example 4, the resistivity of Example 9 was greater than that of Example 4, and the increase in resistivity was greater than that of Example 4. This indicates that the polyethylene glycol microparticles pyrolyze during high-temperature sintering, releasing moisture and carbon dioxide to form micro- and nano-scale pores. This relieves sintering shrinkage stress, prevents the target material from cracking, and thus improves the toughness and strength of the finished film. The carbon after the decomposition of polyethylene glycol can also migrate in the grain boundaries, inhibiting abnormal grain enlargement and optimizing the conductivity and conductivity uniformity of the target material.

[0055] In Example 10S1, no hydroxyapatite nanowires were added. Compared to Example 4, the resistivity increase in Example 10 was greater than that in Example 4. This indicates that the high specific surface area and high flexibility of the hydroxyapatite nanowires further improve the density of the sputtered film, ensure grain boundary permeability to avoid agglomeration, thereby refining the grain size and reducing the resistivity. This results in a finished film with high conductivity and good flexibility.

[0056] Combining Example 1 and Comparative Example 1 with Table 1, it can be seen that, compared with Example 1, the transmittance of Comparative Example 1 is lower than that of Example 1, and the increase in resistivity is greater than that of Example 1. This indicates that the preheating temperature is higher, which can easily affect the transparency. Furthermore, a substrate at 55-65°C can form a flexible transition layer during the sputtering process (AZO first, then ATO), which further improves the flexibility of the film.

[0057] This specific embodiment is merely an explanation of this application and is not intended to limit it. After reading this specification, those skilled in the art can make modifications to this embodiment without contributing any inventive step, but such modifications are protected by patent law as long as they fall within the scope of the claims of this application.

Claims

1. A process for preparing a highly transparent conductive film, characterized in that, Includes the following steps: S1. Alumina and zinc oxide are mixed to obtain a powder mixture, which is then ground and sintered into an AZO target material; antimony trioxide and tin oxide are mixed to obtain a mixture, which is then sintered into an ATO target material after ductile iron treatment. S2. After mixing AZO target material and ATO target material to obtain composite material, the mixture is stirred to obtain mixed material. The mixed material is then magnetron sputtered onto the substrate. The substrate preheating temperature is controlled at 55-65℃. After coating, the finished product is obtained.

2. The preparation process of a highly transparent conductive film according to claim 1, characterized in that: The parameters for magnetron sputtering are as follows: the distance from the mixed material to the substrate is 90-110 mm, the magnetron sputtering working pressure is 0.4-0.6 Pa, and the hydrogen flow rate is 15-17 sccm.

3. The preparation process of a highly transparent conductive film according to claim 1, characterized in that: The specific steps of the stirring process in S2 are as follows: Toluene solution is added to the composite material, and then silane coupling agent is added. The silane coupling agent accounts for 1-2% of the mass of the composite material. The mixture is stirred evenly and reacted at 68-74℃ for 2-3 hours. Then the toluene solvent is removed.

4. The preparation process of a highly transparent conductive film according to claim 3, characterized in that: The silane coupling agent is composed of an aminosilane coupling agent and a hydroxysilane coupling agent in a mass ratio of 1:0.5-1.

5. The preparation process of a highly transparent conductive film according to claim 1, characterized in that: In S1, zinc oxide accounts for 1.5-2% of the mass of aluminum oxide, and antimony trioxide accounts for 1.60-2.35% of the mass of tin oxide. In S2, the mass ratio of AZO target material to ATO target material is 1:0.8-1.

5.

6. The preparation process of a highly transparent conductive film according to claim 1, characterized in that: The powder mixture of S1 contains 0.25-0.38% by weight of epoxy-based polyethylene glycol dopamine, and then it is ground.

7. The preparation process of a highly transparent conductive film according to claim 1, characterized in that: The specific steps of the spheroidizing process in S1 are as follows: First, add 0.2-0.4% of polyethylene glycol microparticles by mass of the mixture, and spheroidize them during the addition process. After spheroidizing, post-treatment is performed.

8. The preparation process of a highly transparent conductive film according to claim 7, characterized in that: The specific post-processing steps are as follows: After spheroidizing, spheroidized material is obtained. Hydroxyapatite nanowires with a mass of 0.12-0.24% are added to the spheroidized material. During the addition process, the spheroidized material is continuously stirred at a speed of 500-1000 r / min to ensure uniform mixing.

9. The preparation process of a highly transparent conductive film according to claim 1, characterized in that: The substrate is a PET film.

10. The preparation process of a highly transparent conductive film according to claim 9, characterized in that: The PET film is made by treating a PET base film with oxygen plasma.