Elastic composite release film with light release force and preparation method thereof
By adopting a three-layer composite membrane structure, combining ammonium bicarbonate dispersion and micro-nanoparticles, the problem of unstable release force of existing release membranes under different environmental conditions is solved, and higher material performance and adaptability are achieved.
Patent Information
- Application Number
- CN202411820136.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-11
- Publication Date
- 2025-05-23
AI Technical Summary
The release force of existing release films is unstable under different environmental conditions, making it difficult to meet the strict requirements of automated production lines. At the same time, the temperature resistance, chemical resistance and mechanical strength of the materials are insufficient, which cannot meet the needs of various application scenarios.
A three-layer composite membrane structure is adopted, including a substrate layer, a porous TPE layer and a micro-nanoparticle composite layer, and a porous structure is generated by dispersion of ammonium bicarbonate, combining solid and porous hollow silica particles to improve the elasticity and adhesion of the film.
The stability and adaptability of the release film are achieved, the stable release force is ensured under different environmental conditions, the temperature resistance, chemical resistance and mechanical strength of the material are improved, and the needs of a variety of application scenarios are met.
Abstract
Description
Technical Field
[0001] The invention relates to the field of polymer materials, and in particular to an elastic light release force composite release film and a preparation method thereof. Background Art
[0002] At present, Chinese enterprises have extensively deployed in the middle and back ends of the electronic industry chain. Due to rising costs in recent years or the need to serve local efficiency, some industrial chains and assembly links have tended to move abroad. However, in the long run, this has also promoted the structural upgrading and transformation of the domestic consumer electronics industry, focusing on higher value-added links in the industrial chain. The development of the industry has undoubtedly driven the demand for various raw materials in the upstream of the industrial chain. Various optical electronic films are a kind of high-performance material that is widely used. Not only does it have huge market potential, but the demand for domestic substitution is also increasingly strong. Release materials (especially release films) are often used as carriers in the fields of electronic tapes, die-cutting, protective films and semiconductor processes. Release films play an indispensable role in functional films as carriers to protect the adhesive layer, protecting the adhered object during the die-cutting process. In order to ensure a smooth peeling process without affecting the performance of the surface material, it is very important to choose a release film with appropriate release force. Although some progress has been made in the research of light release force composite release films, there are still some challenges and problems to be solved; for example, it is currently necessary to improve the stability of the release film to ensure that the release force of the release film is maintained within a very narrow range under different environmental conditions to meet the strict requirements of automated production lines; in addition to low peel force, it is also necessary to consider the material's comprehensive properties such as temperature resistance, chemical resistance, and mechanical strength to meet the needs of different application scenarios. Summary of the invention
[0003] Technical problem to be solved: The purpose of the present invention is to provide an elastic composite release film with light release force and a preparation method thereof, wherein the release film contains a hollow elastic structure to obtain a release film with light peeling force.
[0004] Technical solution: An elastic light release force composite release film, the release film comprises a substrate layer, a porous TPE layer and a micro-nano particle composite layer, the substrate layer, the porous TPE layer and the micro-nano particle composite layer are connected in sequence, the porous TPE layer has closed micron pores, and the micro-nano particle composite layer contains solid silica nanoparticles and porous hollow silica micron particles. Preferably, the substrate layer includes any one of TPU, PE, PET, OPP or PTFE. The preparation method of the above-mentioned elastic light release force composite release film comprises the following steps: S1. The same mass of TPE was dissolved in different masses of butyl acetate, mixed and stirred to obtain TPE-A solution and TPE-B solution; S2. The ammonium bicarbonate was ground and passed through a 100-150 mesh sieve, added to butyl acetate, and stirred to mix well to obtain an ammonium bicarbonate dispersion; S3. The TPE-A solution and the ammonium bicarbonate dispersion were mixed in equal volumes, and the ammonium bicarbonate was evenly dispersed in the solution system by ultrasound to obtain a mixed solution; S4. The surface of one side of the substrate layer is etched, and then the mixed solution is applied to one side of the etched surface of the substrate layer, and the substrate layer coated with the mixed solution is dried to obtain a porous TPE layer; S5. After the solid silica nanoparticles and the porous hollow silica microparticles are mixed evenly, they are added to the TPE-B solution and stirred to mix evenly to obtain a micro-nanoparticle composite solution; S6. Coat the micro-nanoparticle composite solution onto the surface of the porous TPE layer and dry it at room temperature to obtain a release film. Preferably, the concentration of the TPE-A solution is 12-24 wt %, and the concentration of the TPE-B solution is 1-3 wt %. Preferably, the concentration of the ammonium bicarbonate dispersion in step S2 is 0.5-1 wt %. Preferably, in step S4, the drying temperature is 40-60° C. and the drying time is 10-30 min. Preferably, in step S5, the volume ratio of the solid silica nanoparticles to the porous hollow silica microparticles is 2-4:1, and the volume concentration of the solid silica nanoparticles in the TPE-B solution is 5-8 vt%. Preferably, the method for preparing the porous hollow silica micron particles in step S5 comprises the following steps: S11. Add micron-sized polystyrene spheres to an ammonia / ethanol / water solution and disperse them evenly by ultrasonic to obtain a 5-10wt% polystyrene sphere suspension; S12. Add tetraethyl orthosilicate dropwise to the polystyrene ball suspension, stir and react at a speed of 100-200 r / min for 10-30 h to obtain core-shell silica microspheres; S13. The core-shell silica microspheres were added to a 0.001-0.01 mol / L sodium hydroxide solution and subjected to ultrasonic reaction for 10-20 h to obtain porous core-shell silica microspheres; S14. Add the porous core-shell structured silica microspheres into tetrahydrofuran, stir at 50-60°C for 20-40h to dissolve the core layer, and obtain porous hollow silica microparticles. Preferably, the volume ratio of tetraethyl orthosilicate, ammonia water, ethanol and water is 1-2:15-20:22-30:40-50. Beneficial effects: The elastic light release force composite release film of the present invention has the following advantages: 1. The release film of the present invention is a three-layer composite film, including a substrate layer, a porous TPE layer and a micro-nano particle composite layer. The porous TPE layer generates a closed porous structure by adding ammonium bicarbonate. Under pressure, the porous TPE layer makes the film have a certain elasticity, which is conducive to the peeling of the release film; 2. The present invention uses micro-nano structured silicon dioxide to form a micro-nano structure on the surface of the release film. At the same time, the micron silicon dioxide is porous silicon dioxide, which is conducive to the molecular weight of the TPE solution penetrating the particles, improving the adhesion of the micro-nano silicon dioxide on the surface of the release film and improving the residual adhesion rate; 3. The pore size of the TPE in the present invention will affect the release effect of the release film. Too large pores are not conducive to the rebound of the film, and too small pores have no elasticity. The use of 100-150 mesh ammonium bicarbonate can achieve a suitable pore size after decomposition, which is conducive to the peeling of the film; 4. In the present invention, the hardness of the substrate layer is greater than that of the TPE layer, and the composite of soft and hard film layers is beneficial to improving the release effect of the release film. DETAILED DESCRIPTION The present invention will be further described below in conjunction with embodiments, which are explanations of the present invention and are not limited to the following embodiments: Example 1 A method for preparing an elastic light release force composite release film, the preparation method comprising the following steps: S1. The same mass of TPE was dissolved in different masses of butyl acetate, mixed and stirred to obtain a 12wt% TPE-A solution and a 1wt% TPE-B solution; S2. The ammonium bicarbonate was ground and passed through a 100 mesh sieve, and then added to butyl acetate, and stirred to mix well to obtain a 0.5wt% ammonium bicarbonate dispersion; S3. The TPE-A solution and the ammonium bicarbonate dispersion were mixed in equal volumes, and the ammonium bicarbonate was evenly dispersed in the solution system by ultrasound to obtain a mixed solution; S4. Etching one side of the TPU substrate layer, and then coating the mixed solution on one side of the etched surface of the TPU substrate layer, and drying the TPU substrate layer coated with the mixed solution at a temperature of 40 ° C for 30 min to obtain a porous TPE layer; S5. After the solid silica nanoparticles and the porous hollow silica microparticles are mixed evenly, the volume ratio of the solid silica nanoparticles to the porous hollow silica microparticles is 4:1, and the solid silica nanoparticles are added to the TPE-B solution, and the volume concentration of the solid silica nanoparticles in the TPE-B solution is 5vt%, and the mixture is stirred and mixed evenly to obtain a micro-nano particle composite solution; S6. coating the micro-nano particle composite solution onto the surface of the porous TPE layer to obtain a micro-nano particle composite layer, and finally drying at room temperature to obtain a release film; The method for preparing the porous hollow silica micron particles in step S5 comprises the following steps: S11. Add micron-sized polystyrene spheres to an ammonia / ethanol / water solution and disperse them evenly by ultrasonic to obtain a 5 wt % polystyrene sphere suspension; S12. Tetraethyl orthosilicate was added dropwise to the polystyrene ball suspension, the volume ratio of tetraethyl orthosilicate, ammonia, ethanol and water was 2:20:30:50, and the reaction was stirred at a speed of 200 r / min for 10 h to obtain core-shell silica microspheres; S13. The core-shell silica microspheres were added to a 0.001 mol / L sodium hydroxide solution and subjected to ultrasonic reaction for 10 h to obtain porous core-shell silica microspheres; S14. Add the porous core-shell structured silica microspheres into tetrahydrofuran, stir at 50°C for 40 hours to dissolve the core layer, and obtain porous hollow silica microparticles. Example 2 A method for preparing an elastic light release force composite release film, the preparation method comprising the following steps: S1. The same mass of TPE was dissolved in different masses of butyl acetate, mixed and stirred to obtain a 24wt% TPE-A solution and a 3wt% TPE-B solution; S2. The ammonium bicarbonate was ground and passed through a 150 mesh sieve, and then added to butyl acetate, and stirred to mix well to obtain a 1wt% ammonium bicarbonate dispersion; S3. The TPE-A solution and the ammonium bicarbonate dispersion were mixed in equal volumes, and the ammonium bicarbonate was evenly dispersed in the solution system by ultrasound to obtain a mixed solution; S4. Etching one side of the PET substrate layer, and then applying the mixed solution to one side of the etched surface of the PET substrate layer, and drying the PET substrate layer coated with the mixed solution at a temperature of 60° C. for 10 min to obtain a porous TPE layer; S5. After the solid silica nanoparticles and the porous hollow silica microparticles are mixed evenly, the volume ratio of the solid silica nanoparticles to the porous hollow silica microparticles is 2:1, and the solid silica nanoparticles are added to the TPE-B solution, and the volume concentration of the solid silica nanoparticles in the TPE-B solution is 8vt%, and the mixture is stirred and mixed evenly to obtain a micro-nano particle composite solution; S6. coating the micro-nano particle composite solution onto the surface of the porous TPE layer to obtain a micro-nano particle composite layer, and finally drying at room temperature to obtain a release film; The method for preparing the porous hollow silica micron particles in step S5 comprises the following steps: S11. Add micron-sized polystyrene spheres to an ammonia / ethanol / water solution and disperse them evenly by ultrasonication to obtain a 10 wt % polystyrene sphere suspension; S12. TEOS was added dropwise to the polystyrene ball suspension, wherein the volume ratio of TEOS, aqueous ammonia, ethanol and water was 1:15:22:40, and the reaction was stirred at a speed of 100 r / min for 30 h to obtain core-shell silica microspheres; S13. The core-shell silica microspheres were added to a 0.01 mol / L sodium hydroxide solution and subjected to ultrasonic reaction for 20 h to obtain porous core-shell silica microspheres; S14. Add the porous core-shell structured silica microspheres into tetrahydrofuran, stir at 60°C for 20 hours to dissolve the core layer, and obtain porous hollow silica microparticles. Example 3 A method for preparing an elastic light release force composite release film, the preparation method comprising the following steps: S1. The same mass of TPE was dissolved in different masses of butyl acetate, mixed and stirred to obtain a TPE-A solution having a concentration of 15wt% and a TPE-B solution having a concentration of 1.5wt%; S2. The ammonium bicarbonate was ground and passed through a 100 mesh sieve, and then added to butyl acetate, and stirred to mix well to obtain a concentration of 0.6wt% ammonium bicarbonate dispersion; S3. The TPE-A solution and the ammonium bicarbonate dispersion were mixed in equal volumes, and the ammonium bicarbonate was evenly dispersed in the solution system by ultrasound to obtain a mixed solution; S4. Etching one side of the TPU substrate layer, and then coating the mixed solution on one side of the etched surface of the TPU substrate layer, and drying the TPU substrate layer coated with the mixed solution at a temperature of 40 ° C for 30 min to obtain a porous TPE layer; S5. After the solid silica nanoparticles and the porous hollow silica microparticles are mixed evenly, the volume ratio of the solid silica nanoparticles to the porous hollow silica microparticles is 2.5:1, and the solid silica nanoparticles are added to the TPE-B solution, and the volume concentration of the solid silica nanoparticles in the TPE-B solution is 6vt%, and the mixture is stirred and mixed evenly to obtain a micro-nano particle composite solution; S6. coating the micro-nano particle composite solution onto the surface of the porous TPE layer to obtain a micro-nano particle composite layer, and finally drying at room temperature to obtain a release film; The method for preparing the porous hollow silica micron particles in step S5 comprises the following steps: S11. The micron-sized polystyrene spheres were added to an ammonia / ethanol / water solution and ultrasonically dispersed to obtain a 6.5 wt% polystyrene sphere suspension; S12. TEOS was added dropwise to the polystyrene ball suspension, wherein the volume ratio of TEOS, aqueous ammonia, ethanol and water was 1:15:22:40, and the reaction was stirred at a speed of 100 r / min for 30 h to obtain core-shell silica microspheres; S13. The core-shell silica microspheres were added to a 0.005 mol / L sodium hydroxide solution and subjected to ultrasonic reaction for 20 h to obtain porous core-shell silica microspheres; S14. Add the porous core-shell structured silica microspheres into tetrahydrofuran, stir at 50°C for 35 hours to dissolve the core layer, and obtain porous hollow silica microparticles. Example 4 A method for preparing an elastic light release force composite release film, the preparation method comprising the following steps: S1. The same mass of TPE was dissolved in different masses of butyl acetate, mixed and stirred to obtain a 20wt% TPE-A solution and a 2.5wt% TPE-B solution; S2. The ammonium bicarbonate was ground and passed through a 150 mesh sieve, added to butyl acetate, and stirred to mix well to obtain a concentration of 0.9wt% ammonium bicarbonate dispersion; S3. The TPE-A solution and the ammonium bicarbonate dispersion were mixed in equal volumes, and the ammonium bicarbonate was evenly dispersed in the solution system by ultrasound to obtain a mixed solution; S4. Etching one side of the surface of the TPU substrate layer, and then coating the mixed solution on one side of the etched surface of the TPU substrate layer, and drying the TPU substrate layer coated with the mixed solution at a temperature of 60 ° C for 10 min to obtain a porous TPE layer; S5. After the solid silica nanoparticles and the porous hollow silica microparticles are mixed evenly, the volume ratio of the solid silica nanoparticles to the porous hollow silica microparticles is 3.5:1, and the solid silica nanoparticles are added to the TPE-B solution, and the volume concentration of the solid silica nanoparticles in the TPE-B solution is 7vt%, and the mixture is stirred and mixed evenly to obtain a micro-nanoparticle composite solution; S6. coating the micro-nano particle composite solution onto the surface of the porous TPE layer to obtain a micro-nano particle composite layer, and finally drying at room temperature to obtain a release film; The method for preparing the porous hollow silica micron particles in step S5 comprises the following steps: S11. The micron-sized polystyrene spheres were added to an ammonia / ethanol / water solution and ultrasonically dispersed to obtain a 8.5 wt% polystyrene sphere suspension; S12. Tetraethyl orthosilicate was added dropwise to the polystyrene ball suspension, the volume ratio of tetraethyl orthosilicate, ammonia, ethanol and water was 2:20:30:50, and the reaction was stirred at a speed of 200 r / min for 10 h to obtain core-shell silica microspheres; S13. The core-shell silica microspheres were added to a 0.008 mol / L sodium hydroxide solution and subjected to ultrasonic reaction for 10 h to obtain porous core-shell silica microspheres; S14. Add the porous core-shell structured silica microspheres into tetrahydrofuran, stir at 60°C for 25 hours to dissolve the core layer, and obtain porous hollow silica microparticles. Example 5 A method for preparing an elastic light release force composite release film, the preparation method comprising the following steps: S1. The same mass of TPE was dissolved in different masses of butyl acetate, mixed and stirred to obtain a TPE-A solution having a concentration of 18wt% and a TPE-B solution having a concentration of 2wt%; S2. The ammonium bicarbonate was ground and passed through a 150 mesh sieve, and then added to butyl acetate, and stirred to mix well to obtain a concentration of 0.75wt% ammonium bicarbonate dispersion; S3. The TPE-A solution and the ammonium bicarbonate dispersion were mixed in equal volumes, and the ammonium bicarbonate was evenly dispersed in the solution system by ultrasound to obtain a mixed solution; S4. Etching one side of the TPU substrate layer, and then coating the mixed solution on one side of the etched surface of the TPU substrate layer, and drying the TPU substrate layer coated with the mixed solution at a temperature of 50 ° C for 20 min to obtain a porous TPE layer; S5. After the solid silica nanoparticles and the porous hollow silica microparticles are mixed evenly, the volume ratio of the solid silica nanoparticles to the porous hollow silica microparticles is 3:1, and the solid silica nanoparticles are added to the TPE-B solution, and the volume concentration of the solid silica nanoparticles in the TPE-B solution is 6.5vt%, and the mixture is stirred and mixed evenly to obtain a micro-nano particle composite solution; S6. coating the micro-nano particle composite solution onto the surface of the porous TPE layer to obtain a micro-nano particle composite layer, and finally drying at room temperature to obtain a release film; The method for preparing the porous hollow silica micron particles in step S5 comprises the following steps: S11. The micron-sized polystyrene spheres were added to an ammonia / ethanol / water solution and ultrasonically dispersed to obtain a 7 wt % polystyrene sphere suspension; S12. TEOS was added dropwise to the polystyrene ball suspension, the volume ratio of TEOS, ammonia, ethanol and water was 1.5:18:25:45, and the reaction was stirred at a speed of 150 r / min for 20 h to obtain core-shell silica microspheres; S13. The core-shell silica microspheres were added to a 0.006 mol / L sodium hydroxide solution and subjected to ultrasonic reaction for 15 h to obtain porous core-shell silica microspheres; S14. Add the porous core-shell structured silica microspheres into tetrahydrofuran, stir at 55°C for 30 hours to dissolve the core layer, and obtain porous hollow silica microparticles. Comparative Example 1 A method for preparing an elastic light release force composite release film, the preparation method comprising the following steps: S1. Dissolve two portions of TPE in butyl acetate, mix and stir to obtain a TPE solution having a concentration of 15 wt %; S2. The ammonium bicarbonate was ground and passed through a 150 mesh sieve, and then added to butyl acetate, and stirred to mix well to obtain a concentration of 0.75wt% ammonium bicarbonate dispersion; S3. The TPE solution and the ammonium bicarbonate dispersion were mixed in equal volumes, and the ammonium bicarbonate was evenly dispersed in the solution system by ultrasound to obtain a mixed solution; S4. Etching one side of the TPU substrate layer, and then coating the mixed solution on one side of the etched surface of the TPU substrate layer, and drying the TPU substrate layer coated with the mixed solution at a temperature of 50 ° C for 20 min to obtain a porous TPE layer; S5. After the solid silica nanoparticles and the porous hollow silica microparticles are mixed evenly, the volume ratio of the solid silica nanoparticles to the porous hollow silica microparticles is 3:1, and the solid silica nanoparticles are added to the TPE solution, and the volume concentration of the solid silica nanoparticles in the TPE solution is 6.5vt%, and the mixture is stirred and mixed evenly to obtain a micro-nanoparticle composite solution; S6. coating the micro-nano particle composite solution onto the surface of the porous TPE layer to obtain a micro-nano particle composite layer, and finally drying at room temperature to obtain a release film; The method for preparing the porous hollow silica micron particles in step S5 comprises the following steps: S11. The micron-sized polystyrene spheres were added to an ammonia / ethanol / water solution and ultrasonically dispersed to obtain a 7 wt % polystyrene sphere suspension; S12. TEOS was added dropwise to the polystyrene ball suspension, the volume ratio of TEOS, ammonia, ethanol and water was 1.5:18:25:45, and the reaction was stirred at a speed of 150 r / min for 20 h to obtain core-shell silica microspheres; S13. The core-shell silica microspheres were added to a 0.006 mol / L sodium hydroxide solution and subjected to ultrasonic reaction for 15 h to obtain porous core-shell silica microspheres; S14. Add the porous core-shell structured silica microspheres into tetrahydrofuran, stir at 55°C for 30 hours to dissolve the core layer, and obtain porous hollow silica microparticles. Comparative Example 2 A method for preparing an elastic light release force composite release film, the preparation method comprising the following steps: S1. The same mass of TPE was dissolved in different masses of butyl acetate, mixed and stirred to obtain a TPE-A solution having a concentration of 18wt% and a TPE-B solution having a concentration of 2wt%; S2. Etching one side of the TPU substrate layer, then coating the TPE-A solution on one side of the etched surface of the TPU substrate layer, and drying the TPU substrate layer coated with the TPE-A solution at a temperature of 50° C. for 20 min to obtain a porous TPE layer; S3. After the solid silica nanoparticles and the porous hollow silica microparticles are mixed evenly, the volume ratio of the solid silica nanoparticles to the porous hollow silica microparticles is 3:1, and the solid silica nanoparticles are added to the TPE-B solution, and the volume concentration of the solid silica nanoparticles in the TPE-B solution is 6.5vt%, and the mixture is stirred and mixed evenly to obtain a micro-nano particle composite solution; S4. coating the micro-nano particle composite solution onto the surface of the porous TPE layer to obtain a micro-nano particle composite layer, and finally drying at room temperature to obtain a release film; The method for preparing the porous hollow silica micron particles in step S5 comprises the following steps: S11. The micron-sized polystyrene spheres were added to an ammonia / ethanol / water solution and ultrasonically dispersed to obtain a 7 wt % polystyrene sphere suspension; S12. TEOS was added dropwise to the polystyrene ball suspension, the volume ratio of TEOS, ammonia, ethanol and water was 1.5:18:25:45, and the reaction was stirred at a speed of 150 r / min for 20 h to obtain core-shell silica microspheres; S13. The core-shell silica microspheres were added to a 0.006 mol / L sodium hydroxide solution and subjected to ultrasonic reaction for 15 h to obtain porous core-shell silica microspheres; S14. Add the porous core-shell structured silica microspheres into tetrahydrofuran, stir at 55°C for 30 hours to dissolve the core layer, and obtain porous hollow silica microparticles. Comparative Example 3 A method for preparing an elastic light release force composite release film, the preparation method comprising the following steps: S1. The same mass of TPE was dissolved in different masses of butyl acetate, mixed and stirred to obtain a TPE-A solution having a concentration of 18wt% and a TPE-B solution having a concentration of 2wt%; S2. The ammonium bicarbonate was ground and passed through a 300 mesh sieve, and then added to butyl acetate, and stirred to mix well to obtain a concentration of 0.75wt% ammonium bicarbonate dispersion; S3. The TPE-A solution and the ammonium bicarbonate dispersion were mixed in equal volumes, and the ammonium bicarbonate was evenly dispersed in the solution system by ultrasound to obtain a mixed solution; S4. Etching one side of the TPU substrate layer, and then coating the mixed solution on one side of the etched surface of the TPU substrate layer, and drying the TPU substrate layer coated with the mixed solution at a temperature of 50 ° C for 20 min to obtain a porous TPE layer; S5. After the solid silica nanoparticles and the porous hollow silica microparticles are mixed evenly, the volume ratio of the solid silica nanoparticles to the porous hollow silica microparticles is 3:1, and the solid silica nanoparticles are added to the TPE-B solution, and the volume concentration of the solid silica nanoparticles in the TPE-B solution is 6.5vt%, and the mixture is stirred and mixed evenly to obtain a micro-nano particle composite solution; S6. coating the micro-nano particle composite solution onto the surface of the porous TPE layer to obtain a micro-nano particle composite layer, and finally drying at room temperature to obtain a release film; The method for preparing the porous hollow silica micron particles in step S5 comprises the following steps: S11. The micron-sized polystyrene spheres were added to an ammonia / ethanol / water solution and ultrasonically dispersed to obtain a 7 wt % polystyrene sphere suspension; S12. TEOS was added dropwise to the polystyrene ball suspension, the volume ratio of TEOS, ammonia, ethanol and water was 1.5:18:25:45, and the reaction was stirred at a speed of 150 r / min for 20 h to obtain core-shell silica microspheres; S13. The core-shell silica microspheres were added to a 0.006 mol / L sodium hydroxide solution and subjected to ultrasonic reaction for 15 h to obtain porous core-shell silica microspheres; S14. Add the porous core-shell structured silica microspheres into tetrahydrofuran, stir at 55°C for 30 hours to dissolve the core layer, and obtain porous hollow silica microparticles. Comparative Example 4 A method for preparing an elastic light release force composite release film, the preparation method comprising the following steps: S1. The same mass of TPE was dissolved in different masses of butyl acetate, mixed and stirred to obtain a TPE-A solution having a concentration of 18wt% and a TPE-B solution having a concentration of 2wt%; S2. After grinding the ammonium bicarbonate through a 20-mesh sieve, it was added to butyl acetate and stirred to mix well to obtain a concentration of 0.75wt% ammonium bicarbonate dispersion; S3. The TPE-A solution and the ammonium bicarbonate dispersion were mixed in equal volumes, and the ammonium bicarbonate was evenly dispersed in the solution system by ultrasound to obtain a mixed solution; S4. Etching one side of the TPU substrate layer, and then coating the mixed solution on one side of the etched surface of the TPU substrate layer, and drying the TPU substrate layer coated with the mixed solution at a temperature of 50 ° C for 20 min to obtain a porous TPE layer; S5. After the solid silica nanoparticles and the porous hollow silica microparticles are mixed evenly, the volume ratio of the solid silica nanoparticles to the porous hollow silica microparticles is 3:1, and the solid silica nanoparticles are added to the TPE-B solution, and the volume concentration of the solid silica nanoparticles in the TPE-B solution is 6.5vt%, and the mixture is stirred and mixed evenly to obtain a micro-nano particle composite solution; S6. coating the micro-nano particle composite solution onto the surface of the porous TPE layer to obtain a micro-nano particle composite layer, and finally drying at room temperature to obtain a release film; The method for preparing the porous hollow silica micron particles in step S5 comprises the following steps: S11. The micron-sized polystyrene spheres were added to an ammonia / ethanol / water solution and ultrasonically dispersed to obtain a 7 wt % polystyrene sphere suspension; S12. TEOS was added dropwise to the polystyrene ball suspension, the volume ratio of TEOS, ammonia, ethanol and water was 1.5:18:25:45, and the reaction was stirred at a speed of 150 r / min for 20 h to obtain core-shell silica microspheres; S13. The core-shell silica microspheres were added to a 0.006 mol / L sodium hydroxide solution and subjected to ultrasonic reaction for 15 h to obtain porous core-shell silica microspheres; S14. Add the porous core-shell structured silica microspheres into tetrahydrofuran, stir at 55°C for 30 hours to dissolve the core layer, and obtain porous hollow silica microparticles. Comparative Example 5 A method for preparing an elastic light release force composite release film, the preparation method comprising the following steps: S1. The same mass of TPU was dissolved in different masses of tetrahydrofuran, mixed and stirred to obtain a TPU-A solution having a concentration of 8wt% and a TPU-B solution having a concentration of 2wt%; S2. The ammonium bicarbonate was ground and passed through a 150 mesh sieve, added to tetrahydrofuran, and stirred to mix well to obtain a 0.75wt% ammonium bicarbonate dispersion; S3. The TPU-A solution and the ammonium bicarbonate dispersion were mixed in equal volumes, and the ammonium bicarbonate was evenly dispersed in the solution system by ultrasound to obtain a mixed solution; S4. Etching one side of the TPU substrate layer, and then coating the mixed solution on one side of the etched surface of the TPU substrate layer, and drying the TPU substrate layer coated with the mixed solution at a temperature of 50 ° C for 20 min to obtain a porous TPU layer; S5. After the solid silica nanoparticles and the porous hollow silica microparticles are mixed evenly, the volume ratio of the solid silica nanoparticles to the porous hollow silica microparticles is 3:1, and the solid silica nanoparticles are added to the TPU-B solution. The volume concentration of the solid silica nanoparticles in the TPU-B solution is 6.5vt%, and the mixture is stirred and mixed evenly to obtain a micro-nano particle composite solution; S6. coating the micro-nano particle composite solution onto the surface of the porous TPU layer to obtain a micro-nano particle composite layer, and finally drying at room temperature to obtain a release film; The method for preparing the porous hollow silica micron particles in step S5 comprises the following steps: S11. The micron-sized polystyrene spheres were added to an ammonia / ethanol / water solution and ultrasonically dispersed to obtain a 7 wt % polystyrene sphere suspension; S12. TEOS was added dropwise to the polystyrene ball suspension, the volume ratio of TEOS, ammonia, ethanol and water was 1.5:18:25:45, and the reaction was stirred at a speed of 150 r / min for 20 h to obtain core-shell silica microspheres; S13. The core-shell silica microspheres were added to a 0.006 mol / L sodium hydroxide solution and subjected to ultrasonic reaction for 15 h to obtain porous core-shell silica microspheres; S14. Add the porous core-shell structured silica microspheres into tetrahydrofuran, stir at 55°C for 30 hours to dissolve the core layer, and obtain porous hollow silica microparticles. Comparative Example 6 A method for preparing an elastic light release force composite release film, the preparation method comprising the following steps: S1. The same mass of TPE was dissolved in different masses of butyl acetate, mixed and stirred to obtain a TPE-A solution having a concentration of 18wt% and a TPE-B solution having a concentration of 2wt%; S2. The ammonium bicarbonate was ground and passed through a 150 mesh sieve, and then added to butyl acetate, and stirred to mix well to obtain a concentration of 0.75wt% ammonium bicarbonate dispersion; S3. The TPE-A solution and the ammonium bicarbonate dispersion were mixed in equal volumes, and the ammonium bicarbonate was evenly dispersed in the solution system by ultrasound to obtain a mixed solution; S4. Etching one side of the TPU substrate layer, and then coating the mixed solution on one side of the etched surface of the TPU substrate layer, and drying the TPU substrate layer coated with the mixed solution at a temperature of 50 ° C for 20 min to obtain a porous TPE layer; S5. The solid silica nanoparticles are added to the TPE-B solution, the volume concentration of the solid silica nanoparticles in the TPE-B solution is 6.5vt%, and the mixture is stirred to obtain a nanoparticle composite solution; S6. Coating the nanoparticle composite solution onto the surface of the porous TPE layer, and finally drying at room temperature to obtain a release film. Comparative Example 7 A method for preparing an elastic light release force composite release film, the preparation method comprising the following steps: S1. The same mass of TPE was dissolved in different masses of butyl acetate, mixed and stirred to obtain a TPE-A solution having a concentration of 18wt% and a TPE-B solution having a concentration of 2wt%; S2. The ammonium bicarbonate was ground and passed through a 150 mesh sieve, and then added to butyl acetate, and stirred to mix well to obtain a concentration of 0.75wt% ammonium bicarbonate dispersion; S3. The TPE-A solution and the ammonium bicarbonate dispersion were mixed in equal volumes, and the ammonium bicarbonate was evenly dispersed in the solution system by ultrasound to obtain a mixed solution; S4. Etching one side of the TPU substrate layer, and then coating the mixed solution on one side of the etched surface of the TPU substrate layer, and drying the TPU substrate layer coated with the mixed solution at a temperature of 50 ° C for 20 min to obtain a porous TPE layer; S5. After the solid silica nanoparticles and the solid silica microparticles are evenly mixed, the volume ratio of the solid silica nanoparticles to the solid silica microparticles is 3:1, and the solid silica nanoparticles are added to the TPE-B solution, and the volume concentration of the solid silica nanoparticles in the TPE-B solution is 6.5vt%, and the mixture is stirred and mixed to obtain a micro-nanoparticle composite solution; S6. coating the micro-nano particle composite solution onto the surface of the porous TPE layer to obtain a micro-nano particle composite layer, and finally drying at room temperature to obtain a release film. Performance Test: The release films of the above-mentioned embodiments and comparative examples were subjected to a 180° peeling test for peeling force and residual adhesion rate, using the optical functional film release film method in GB / T25256-2010, and the peeling rate was 300 mm / min. <![CDATA[Peeling force / cN·(25 mm) -1 > Residual adhesion rate / % Example 1 1.3 95.6 Example 2 1.5 94.7 Example 3 1.4 96.2 Example 4 1.3 95.7 Example 5 1.3 96.4 Comparative Example 1 3.6 90.1 Comparative Example 2 8.9 95.2 Comparative Example 3 4.2 89.6 Comparative Example 4 5.8 94.8 Comparative Example 5 4.9 88.7 Comparative Example 6 2.7 92.3 Comparative Example 7 1.4 91.4 Obviously, the above embodiments are merely examples for the purpose of clear explanation, and are not intended to limit the implementation methods. For those skilled in the art, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to list all the implementation methods here. The obvious changes or modifications derived therefrom are still within the scope of protection of the present invention.
Claims
1. An elastic light release force composite release film, characterized in that: The release film comprises a substrate layer, a porous TPE layer and a micro-nano particle composite layer, wherein the substrate layer, the porous TPE layer and the micro-nano particle composite layer are connected in sequence, the porous TPE layer has closed micron pores, and the micro-nano particle composite layer contains solid silicon dioxide nanoparticles and porous hollow silicon dioxide micron particles.
2. The elastic light release force composite release film according to claim 1, characterized in that: The substrate layer includes any one of TPU, PE, PET, OPP or PTFE.
3. The method for preparing the elastic light release force composite release film according to claim 1, characterized in that: The preparation method comprises the following steps: S1. The same mass of TPE was dissolved in different masses of butyl acetate, mixed and stirred to obtain TPE-A solution and TPE-B solution; S2. The ammonium bicarbonate was ground and passed through a 100-150 mesh sieve, added to butyl acetate, and stirred to mix well to obtain an ammonium bicarbonate dispersion; S3. The TPE-A solution and the ammonium bicarbonate dispersion were mixed in equal volumes, and the ammonium bicarbonate was evenly dispersed in the solution system by ultrasound to obtain a mixed solution; S4. The surface of one side of the substrate layer is etched, and then the mixed solution is applied to one side of the etched surface of the substrate layer, and the substrate layer coated with the mixed solution is dried to obtain a porous TPE layer; S5. After the solid silica nanoparticles and the porous hollow silica microparticles are mixed evenly, they are added to the TPE-B solution and stirred to mix evenly to obtain a micro-nanoparticle composite solution; S6. Coat the micro-nanoparticle composite solution onto the surface of the porous TPE layer and dry it at room temperature to obtain a release film.
4. The method for preparing the elastic light release force composite release film according to claim 1, characterized in that: The concentration of the TPE-A solution is 12-24 wt %, and the concentration of the TPE-B solution is 1-3 wt %.
5. The method for preparing the elastic light release force composite release film according to claim 1, characterized in that: The concentration of the ammonium bicarbonate dispersion in step S2 is 0.5-1 wt %.
6. The method for preparing the elastic light release force composite release film according to claim 1, characterized in that: In step S4, the drying temperature is 40-60° C. and the drying time is 10-30 min.
7. The method for preparing the elastic light release force composite release film according to claim 1, characterized in that: In the step S5, the volume ratio of the solid silica nanoparticles to the porous hollow silica microparticles is 2-4:1, and the volume concentration of the solid silica nanoparticles in the TPE-B solution is 5-8 vt%.
8. The method for preparing the elastic light release force composite release film according to claim 2, characterized in that: The method for preparing the porous hollow silica micron particles in step S5 comprises the following steps: S11. Add micron-sized polystyrene spheres to an ammonia / ethanol / water solution and disperse them evenly by ultrasonic to obtain a 5-10wt% polystyrene sphere suspension; S12. Add tetraethyl orthosilicate dropwise to the polystyrene ball suspension, stir and react at a speed of 100-200 r / min for 10-30 h to obtain core-shell silica microspheres; S13. The core-shell silica microspheres were added to a 0.001-0.01 mol / L sodium hydroxide solution and subjected to ultrasonic reaction for 10-20 h to obtain porous core-shell silica microspheres; S14. Add the porous core-shell structured silica microspheres into tetrahydrofuran, stir at 50-60°C for 20-40h to dissolve the core layer, and obtain porous hollow silica microparticles.
9. The method for preparing the elastic light release force composite release film according to claim 8, characterized in that: The volume ratio of the tetraethyl orthosilicate, ammonia water, ethanol and water is 1-2:15-20:22-30:40-50.