A high-definition anti-glare nano AG film and its preparation method

Abstract

The present invention relates to the technical field of AG films, and specifically discloses a high-definition anti-glare nano-AG film sheet and a preparation method thereof. The high-definition anti-glare nano-AG film sheet includes a film substrate and a reaction synthesis microstructure layer and a first surface protection film layer that are sequentially laminated on the surface of the film substrate. The preparation method of the high-definition anti-glare nano-AG film sheet applies an ultraviolet light-curing surface material on the film substrate to form a film layer, and uses an imprint mold to press and imprint the film layer. Further through light curing, an imprint microstructure layer with a number of randomly distributed pits, protrusions or through holes on the surface is obtained. While ensuring the gloss and transmittance, the uneven surface structure of the imprint microstructure layer can be used to change the specular reflection of light into diffuse reflection, weaken the interference to the eyes, achieve the anti-glare effect, can well control the size uniformity and distribution uniformity of the particles, has good smoothness, improves the use feel, and can effectively avoid the formation of flash points.

Description

Technical Field

[0001] The present invention relates to the field of AG films, and particularly to a high-definition anti-glare nano AG film and a preparation method thereof. Background Art

[0002] In recent years, with the development of the flat panel display industry, it has strongly promoted the production and research and development of optical functional films; AG films are a general term for a class of functional films, and due to their good anti-fingerprint, oil stain, high light transmittance and other characteristics, they are widely used in the current market; during use, there are problems such as instability in gloss, haze, and roughness, and the spraying process is prone to uneven distribution and inconsistent size of coating particles, resulting in flash point phenomena and affecting the display effect; it brings great inconvenience to the use of the touch screen. Therefore, it is an urgent task to develop a hard coating with high-definition anti-glare function. Summary of the Invention

[0003] Object of the Invention: The object of the present invention is to provide a high-definition anti-glare nano AG film; another object of the present invention is to provide a preparation method of a high-definition anti-glare nano AG film.

[0004] Technical Solution: A high-definition anti-glare nano AG film sheet, which includes: a reinforced modified PE film sheet substrate, a nano zinc oxide transition layer, a nano Ag film layer, a reaction accumulation microstructure layer, and a modified surface protective film;

[0005] The preparation method of the reinforced modified PE film sheet substrate is as follows: Place the PE film sheet in a chlorine gas atmosphere, irradiate it with a mercury lamp UV at 40 °C for 8 h to obtain a chlorinated PE film sheet, take it out, place the chlorinated PE film sheet in a 60% ethanol aqueous solution with a volume 10 times that of the weight of the chlorinated PE film sheet, add aluminum trichloride with a weight 0.01 times that of the weight of the chlorinated PE film sheet, ultrasonically dissolve it, then add toluene with a weight 0.1 times that of the weight of the chlorinated PE film sheet, ultrasonically react at an external temperature of 80 °C for 4 h, and take it out and vacuum dry at 45 °C to obtain it;

[0006] The preparation method of the reaction accumulation microstructure layer is as follows: Under nitrogen protection, place the PET film sheet in dichloromethane with a volume 5 times that of the weight of the PET film sheet, add o-cresol with a mass 0.5 times that of the mass of the PET film sheet and triphenylphosphine with a mass 1.2 times that of the mass of the PET film sheet under ultrasonic treatment at 20 °C, stir to dissolve and clarify, cool the system to 0 ± 5 °C, maintain the same temperature and dropwise add diisopropyl azodicarboxylate with a mass 0.9 times that of the mass of the PET film sheet, after dropping, control the system temperature not to exceed 15 °C and react for 30 min, slowly add polyethylene glycol 6000 with a mass 2 times that of the mass of the PET film sheet, ultrasonically react for 2 h, take it out, wash it with ethanol, and dry it at 50 °C with air blast to obtain it;

[0007] The preparation method of the modified surface protective film layer is as follows: Place the PET film in neopentyl glycol with a volume 5 times that of the weight of the PET film. Add o-cresol with a mass 0.5 times that of the PET film and triphenylphosphine with a mass 1.2 times that of the PET film under ultrasonic conditions at 20°C. Stir until dissolved and clarified. Cool the system to 0 ± 5°C, and while maintaining the same temperature, dropwise add diisopropyl azodicarboxylate with a mass 0.9 times that of the PET film. React under ultrasonic conditions for 2 h, take out and wash with ethanol, and dry at 50°C with air blowing to obtain the product.

[0008] Preferably, for the reinforced and modified PE film substrate, the thickness range of the PE film substrate is 80 - 200 μm.

[0009] Preferably, the thickness of the nano-zinc oxide transition layer is 20 nm.

[0010] Preferably, the thickness of the nano-Ag film layer is 50 nm.

[0011] Preferably, for the PET film of the reaction-deposited microstructure layer, the thickness range is 70 - 100 μm, the surface roughness Ra is 0.01 - 0.05 μm, and the surface roughness Rsm is 2 - 16 μm.

[0012] Preferably, for the PET layer of the surface protective film layer, the thickness range is 70 - 100 μm.

[0013] A preparation method of a high-definition anti-glare nano-AG film includes the following preparation steps:

[0014] S1. Use a VTC-600-1HD single-target magnetron sputtering instrument to deposit a layer of nano-zinc oxide on the reinforced and modified PE film substrate to obtain film material 1;

[0015] S2. Use a VTC-600-1HD single-target magnetron sputtering instrument to deposit a layer of silver film on the nano-zinc oxide coating side of the film material 1 obtained in step 1) to obtain film material 2;

[0016] S3. Coat an adhesive on one side of the silver film of the film material 2 obtained in step S2 and attach a reaction-deposited microstructure layer to obtain film material 3;

[0017] S4. Coat an adhesive on one side of the reaction-deposited microstructure layer of the film material 3 obtained in step S3 and attach a surface protective film layer to obtain the high-definition anti-glare low-flash-point AG film.

[0018] Preferably, the adhesives used in step S3 and step S4 are silicone resins, selected from any one of methyl MQ silicone resin and vinyl MQ silicone resin.

[0019] Beneficial effects:

[0020] 1. The substrate film is reinforced and modified by chlorination and alkylation reactions of the PE film substrate. The obtained substrate film is hard and has excellent electrical insulation properties.

[0021] 2. The polyethylene glycol 6000 is stacked on the surface of the PET material through Mitsunobu reaction to form a microstructured matte layer, which is more uniform and has better light transmittance compared to methods such as embossing.

[0022] 3. The PET material is modified through Mitsunobu reaction, and the obtained PET material has more excellent impact resistance. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 It is a schematic chemical reaction diagram of the reinforced and modified PE film substrate of the present invention;

[0024] Figure 2 It is a schematic chemical reaction diagram of the reaction stacking microstructured layer of the present invention;

[0025] Figure 3 It is a schematic chemical reaction diagram of the modified surface protective film layer of the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0026] To make the technical solutions of the present invention clearer, the following further describes the present invention in detail with reference to the accompanying drawings and specific embodiments. Example 1

[0027] Preparation of the reinforced and modified PE film substrate:

[0028] A PE film with a thickness of 80 μm is placed in a chlorine gas atmosphere and irradiated with a mercury lamp UV at 40 °C for 8 h to obtain a chlorinated PE film. Then it is taken out and placed in a 60% ethanol aqueous solution with a volume 10 times the weight of the chlorinated PE film. Aluminum trichloride with a weight 0.01 times the weight of the chlorinated PE film is added. After ultrasonic dissolution, toluene with a weight 0.1 times the weight of the chlorinated PE film is added, and the reaction is carried out by ultrasonic at an external temperature of 80 °C for 4 h. Then it is taken out and dried in vacuum at 45 °C to obtain the product.

[0029] Preparation of the reaction stacking microstructured layer:

[0030] Under nitrogen protection, a PET film with a thickness of 70 μm is placed in dichloromethane with a volume 5 times the weight of the PET film. At 20 °C under ultrasonic, o-cresol with a mass 0.5 times the mass of the PET film and triphenylphosphine with a mass 1.2 times the mass of the PET film are added, and stirred until dissolved and clarified. The system is cooled to 0 ± 5 °C, and diisopropyl azodicarboxylate with a mass 0.9 times the mass of the PET film is added dropwise while maintaining the same temperature. After the addition is completed, the system temperature is controlled not to exceed 15 °C and the reaction is carried out for 30 min. Then polyethylene glycol 6000 with a mass 2 times the mass of the PET film is slowly added, and the reaction is carried out by ultrasonic for 2 h. Then it is taken out, washed with ethanol, and dried at 50 °C by blowing air to obtain the product.

[0031] Preparation of modified surface protective film layer:

[0032] Place a PET film with a thickness of 70 μm into neopentyl glycol with a volume 5 times the weight of the PET film. Add o-cresol with a mass 0.5 times that of the PET film and triphenylphosphine with a mass 1.2 times that of the PET film under ultrasonic treatment at 20°C. Stir until dissolved and clarified. Cool the system to 0 ± 5°C, and while maintaining the same temperature, dropwise add diisopropyl azodicarboxylate with a mass 0.9 times that of the PET film. React under ultrasonic treatment for 2 h, take out and wash with ethanol, and dry at 50°C with air blowing to obtain the product.

[0033] The specific preparation process is as follows:

[0034] 1) Use a VTC-600-1HD single-target magnetron sputtering instrument to deposit a nano-zinc oxide layer with a thickness of 20 nm on the reinforced and modified PE film substrate to obtain film material 1;

[0035] 2) Use a VTC-600-1HD single-target magnetron sputtering instrument to deposit a silver film with a thickness of 50 nm on the nano-zinc oxide coating side of the film material 1 obtained in step 1) to obtain film material 2;

[0036] 3) Coating a layer of methyl MQ silicone resin adhesive on one side of the silver film of the film material 2 obtained in step 2), and attaching a reaction-accumulated microstructure layer to obtain film material 3;

[0037] 4) Coating a layer of methyl MQ silicone resin adhesive on one side of the reaction-accumulated microstructure layer of the film material 3 obtained in step 3), and attaching a surface protective film layer to obtain the high-definition anti-glare low-flash-point AG film. Example 2

[0038] Preparation of reinforced and modified PE film substrate:

[0039] Place a PE film with a thickness of 120 μm under a chlorine gas atmosphere, irradiate it with a mercury lamp UV at 40°C for 8 h to obtain a chlorinated PE film. Take it out, place the chlorinated PE film into a 60% ethanol aqueous solution with a volume 10 times the weight of the chlorinated PE film, add aluminum trichloride with a weight 0.01 times that of the chlorinated PE film. After ultrasonic dissolution, add toluene with a weight 0.1 times that of the chlorinated PE film, and react under ultrasonic treatment at an external temperature of 80°C for 4 h. Take it out and dry in vacuum at 45°C to obtain the product;

[0040] Preparation of reaction-accumulated microstructure layer:

[0041] Under nitrogen protection, a PET film with a thickness of 80 μm was placed in dichloromethane with a volume 5 times the weight of the PET film. At 20 °C under ultrasonic treatment, o-cresol with a mass 0.5 times that of the PET film and triphenylphosphine with a mass 1.2 times that of the PET film were added. After stirring until dissolved and clarified, the system was cooled to 0 ± 5 °C. While maintaining the same temperature, diisopropyl azodicarboxylate with a mass 0.9 times that of the PET film was added dropwise. After the addition was complete, the system temperature was controlled not to exceed 15 °C and reacted for 30 min. Polyethylene glycol 6000 with a mass 2 times that of the PET film was slowly added, and the reaction was carried out under ultrasonic treatment for 2 h. Then it was taken out, washed with ethanol, and dried at 50 °C under blowing to obtain the product;

[0042] Preparation of the modified surface protective film layer:

[0043] A PET film with a thickness of 80 μm was placed in neopentyl glycol with a volume 5 times the weight of the PET film. At 20 °C under ultrasonic treatment, o-cresol with a mass 0.5 times that of the PET film and triphenylphosphine with a mass 1.2 times that of the PET film were added. After stirring until dissolved and clarified, the system was cooled to 0 ± 5 °C. While maintaining the same temperature, diisopropyl azodicarboxylate with a mass 0.9 times that of the PET film was added dropwise, and the reaction was carried out under ultrasonic treatment for 2 h. Then it was taken out, washed with ethanol, and dried at 50 °C under blowing to obtain the product.

[0044] The specific preparation process is as follows:

[0045] 1) A 20-nm-thick nano-zinc oxide layer was deposited on the reinforced and modified PE film substrate using a VTC-600-1HD single-target magnetron sputtering instrument to obtain film material 1;

[0046] 2) A 50-nm-thick silver film was deposited on the nano-zinc oxide coating side of the film material 1 obtained in step 1) using a VTC-600-1HD single-target magnetron sputtering instrument to obtain film material 2;

[0047] 3) A layer of vinyl MQ silicone resin adhesive was coated on one side of the silver film of the film material 2 obtained in step 2), and a reaction-accumulated microstructure layer was attached to obtain film material 3;

[0048] 4) A layer of vinyl MQ silicone resin adhesive was coated on one side of the reaction-accumulated microstructure layer of the film material 3 obtained in step 3), and a surface protective film layer was attached to obtain the high-definition anti-glare low-flash-point AG film. Example 3

[0049] Preparation of the reinforced and modified PE film substrate:

[0050] A PE film with a thickness of 200 μm was placed in a chlorine gas atmosphere and irradiated with UV light from a mercury lamp at 40 °C for 8 h to obtain a chlorinated PE film. The film was taken out and placed in a 60% ethanol aqueous solution with a volume 10 times the weight of the chlorinated PE film. Aluminum trichloride with a weight 0.01 times the weight of the chlorinated PE film was added. After ultrasonic dissolution, toluene with a weight 0.1 times the weight of the chlorinated PE film was added, and the reaction was carried out under ultrasonic waves at an external temperature of 80 °C for 4 h. Then it was taken out and dried in vacuum at 45 °C to obtain the product.

[0051] Preparation of the reaction-deposited microstructural layer:

[0052] Under nitrogen protection, a PET film with a thickness of 100 μm was placed in dichloromethane with a volume 5 times the weight of the PET film. At 20 °C under ultrasonic conditions, o-cresol with a mass 0.5 times the mass of the PET film and triphenylphosphine with a mass 1.2 times the mass of the PET film were added, and the mixture was stirred until dissolved and clarified. The system was cooled to 0 ± 5 °C, and diisopropyl azodicarboxylate with a mass 0.9 times the mass of the PET film was added dropwise while maintaining the same temperature. After the addition was completed, the system temperature was controlled not to exceed 15 °C and the reaction was carried out for 30 min. Then polyethylene glycol 6000 with a mass 2 times the mass of the PET film was slowly added, and the reaction was carried out under ultrasonic waves for 2 h. After taking it out, it was washed with ethanol and dried in a blast at 50 °C to obtain the product.

[0053] Preparation of the modified surface protective film layer:

[0054] A PET film with a thickness of 100 μm was placed in neopentyl glycol with a volume 5 times the weight of the PET film. At 20 °C under ultrasonic conditions, o-cresol with a mass 0.5 times the mass of the PET film and triphenylphosphine with a mass 1.2 times the mass of the PET film were added, and the mixture was stirred until dissolved and clarified. The system was cooled to 0 ± 5 °C, and diisopropyl azodicarboxylate with a mass 0.9 times the mass of the PET film was added dropwise while maintaining the same temperature. The reaction was carried out under ultrasonic waves for 2 h. After taking it out, it was washed with ethanol and dried in a blast at 50 °C to obtain the product.

[0055] The specific preparation process is as follows:

[0056] 1) Use a VTC-600-1HD single-target magnetron sputtering instrument to deposit a 20-nm-thick nano-zinc oxide layer on the reinforced and modified PE film substrate to obtain film material 1;

[0057] 2) Use a VTC-600-1HD single-target magnetron sputtering instrument to deposit a 50-nm-thick silver film on the nano-zinc oxide coating side of the film material 1 obtained in step 1) to obtain film material 2;

[0058] 3) Coating a layer of methyl MQ silicone resin adhesive on the silver film side of the film material 2 obtained in step 2) and attaching the reaction-deposited microstructural layer to obtain film material 3;

[0059] 4) On one side of the reaction-deposited microstructure layer of the film material 3 obtained in step 3), a layer of methyl MQ silicone resin adhesive is coated, and a surface protective film layer is attached to obtain the high-definition anti-glare low-flash-point AG film sheet. Comparative Example 1

[0060] Same as Example 1, except that the PE film substrate is not reinforced and modified. Comparative Example 2

[0061] Same as Example 1, except that a conventional embossed PET film is used to replace the reaction-deposited microstructure layer. Comparative Example 3

[0062] Same as Example 1, except that the PET protective film is not modified;

[0063] The AG films obtained in Examples 1 to 3 and Comparative Examples 1 to 3 were tested, and the test results are shown in Table 1;

[0064] Table 1 Test results of AG film sheets in Examples and Comparative Examples:

[0065]

[0066] It can be seen from the results in Table 1 that from the data of Examples 1 to 3 and Comparative Example 1, reinforcing and modifying the PE film substrate can improve the haze and total light transmittance of the film; from the data of Examples 1 to 3 and Comparative Example 2, using the reaction-deposited microstructure layer can improve the 60° gloss, haze and total light transmittance of the film; from the data of Examples 1 to 3 and Comparative Example 3, modifying the PET protective film can effectively improve the corrosion resistance of the film. A high-definition anti-glare nano-AG film prepared by the present invention has better product performance through the mutual cooperation of each component. By reinforcing and modifying the PE film substrate, modifying the surface protective film layer and preparing the reaction-deposited microstructure layer, the film has higher total light transmittance, better clarity, better anti-glare effect, and good acid corrosion resistance.

[0067] The above-described embodiments only represent several implementation manners of the present invention, and the description is relatively specific and detailed, but it should not be construed as a limitation on the scope of the patent of the present invention. It should be noted that for those of ordinary skill in the art, without departing from the concept of the present invention, several deformations and improvements can still be made, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention should be subject to the appended claims.

Claims

1. A high-definition anti-glare nano AG film, characterized in that: The high-definition anti-glare nano-AG film comprises: a reinforced modified PE film substrate, a nano zinc oxide transition layer, a nano Ag film layer, a reaction accumulation microstructure layer, and a modified surface protection film layer; The preparation method of the reinforced modified PE film substrate is as follows: placing the PE film in a chlorine atmosphere, irradiating the film with a mercury lamp UV at 40°C for 8 hours to obtain a chlorinated PE film, taking out the chlorinated PE film, placing the chlorinated PE film in a 60% ethanol aqueous solution with a volume 10 times the weight of the chlorinated PE film, adding aluminum chloride with a weight 0.01 times the weight of the chlorinated PE film, ultrasonically dissolving, adding toluene with a weight 0.1 times the weight of the chlorinated PE film, ultrasonically reacting at an external temperature of 80°C for 4 hours, taking out and vacuum drying at 45°C to obtain the film; The preparation method of the reaction accumulation microstructure layer is as follows: under nitrogen protection, the PET film is placed in dichloromethane with a volume 5 times the weight of the PET film, and o-cresol with a mass 0.5 times the mass of the PET film and triphenylphosphine with a mass 1.2 times the mass of the PET film are added under ultrasound at 20°C, and the mixture is stirred to dissolve and clarify, and the system is cooled to 0±5°C, and diisopropyl azodicarboxylate with a mass 0.9 times the mass of the PET film is added dropwise at the same temperature, and the system temperature is controlled not to exceed 15°C for reaction for 30 minutes after the addition is completed, and polyethylene glycol 6000 with a mass 2 times the mass of the PET film is slowly added, and the reaction is carried out under ultrasound for 2 hours, and the mixture is taken out and washed with ethanol, and dried at 50°C with air blowing. The preparation method of the modified surface protective film layer is as follows: a PET film is placed in neopentyl glycol with a volume 5 times the weight of the PET film, o-cresol with a mass 0.5 times the mass of the PET film and triphenylphosphine with a mass 1.2 times the mass of the PET film are added under ultrasound at 20°C, the solution is stirred to clarify, the system is cooled to 0±5°C, and diisopropyl azodicarboxylate with a mass 0.9 times the mass of the PET film is added dropwise at the same temperature, ultrasonically reacted for 2 hours, taken out and washed with ethanol, and dried at 50°C by blowing air.

2. The high-definition anti-glare nano AG film according to claim 1, characterized in that: The reinforced modified PE film substrate has a thickness ranging from 80 to 200 μm.

3. The high-definition anti-glare nano AG film according to claim 1, characterized in that: The thickness of the nano zinc oxide transition layer is 20 nm.

4. The high-definition anti-glare nano AG film according to claim 1, characterized in that: The thickness of the nano-Ag film layer is 50nm.

5. The high-definition anti-glare nano AG film according to claim 1, characterized in that: The thickness of the reaction-stacked microstructure layer PET film is in the range of 70 to 100 μm, the surface roughness Ra of the reaction-stacked microstructure layer is in the range of 0.01 to 0.05 μm, and the surface roughness Rsm is in the range of 2 to 16 μm.

6. The high-definition anti-glare nano AG film according to claim 1, characterized in that: The surface protection film layer PET layer has a thickness ranging from 70 to 100 μm.

7. A method for preparing a high-definition anti-glare nano-AG film according to any one of claims 1 to 6, characterized in that: The method comprises the following preparation steps: S1. Using a VTC-600-1HD single-target magnetron sputtering apparatus, a layer of nano zinc oxide was plated on the reinforced modified PE film substrate to obtain film material 1; S2, using a VTC-600-1HD single-target magnetron sputtering apparatus to coat a layer of silver film on the nano zinc oxide coating side of the film material 1 obtained in step S1, to obtain film material 2; S3, coating a layer of adhesive on one side of the silver film of the film material 2 obtained in step S2, and attaching the reaction-deposited microstructure layer thereon to obtain a film material 3; S4, coating a layer of adhesive on one side of the reaction-deposited microstructure layer of the film material 3 obtained in step S3, and then attaching a surface protection film layer thereto, so as to obtain the high-definition anti-glare low-flash point AG film.

8. The method for preparing the high-definition anti-glare nano AG film according to claim 7, characterized in that: The adhesive applied in step S3 and step S4 is an organic silicone resin selected from any one of methyl MQ silicone resin and vinyl MQ silicone resin, and the adhesive coating thickness is 20 μm.

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