Anti-reflection surface treatment process of tempered film

Abstract

The invention relates to the technical field of surface treatment of optical glass, in particular to an anti-reflection surface treatment process of a tempered film, which sequentially comprises the following steps: mechanical cleaning, chemical activation, surface hydroxylation, bottom layer film coating, middle layer film coating, outer surface layer film coating and UV curing of a hydrophobic layer. Three layers of thin films with specific optical properties are coated on the surface of an object, the uniformity of the film layers is very good, and the film layers are particularly suitable for base materials with regular shapes (such as planes and spherical lenses); the film thickness can be accurately controlled through the lifting speed and the liquid medicine concentration; a very compact film layer with excellent optical performance can be formed; a plurality of base materials can be treated at a time (in batch production), and the anti-reflection effect of the surface of the tempered film is remarkably improved. The optical element is especially suitable for applications sensitive to cost or having specific shape requirements, the light transmission performance and visual experience of the optical element are remarkably improved, and the practicability is high.

Description

Technical Field

[0001] The present invention relates to the technical field of surface treatment of optical glass, and in particular to an anti-reflection surface treatment process of a tempered film. Background Art

[0002] Optical glass is widely used in camera lenses, telescopes, glasses, display screens, and other fields. It is also widely used in consumer electronics (lenses, screens), medical equipment (endoscopes), automobiles (lidar, HUD), security monitoring, and other fields. However, surface reflection can lead to light efficiency loss (5% to 10%) and reduced image quality.

[0003] With technological advancements and rising consumer demand for high-quality optical products, reducing light reflection and increasing light transmittance have become increasingly important. Anti-reflective coatings can significantly enhance the performance of optical glass, reducing reflected light and improving image quality and visual experience.

[0004] Demand for tempered protective films for mobile phone screens has also surged. However, traditional vacuum coating (PVD / CVD) equipment is typically used for anti-reflective surface treatment. However, this equipment is expensive, energy-intensive, and difficult to process for curved surfaces, making it difficult to use in the lower-profit-margin tempered film manufacturing sector. These significant drawbacks hinder actual production and processing. Summary of the Invention

[0005] The technical problem to be solved by the present invention is to provide an anti-reflective surface treatment process for tempered film, which does not require the use of expensive vacuum coating equipment, improves the uniformity of the coating through ultrasonic-assisted impregnation and rheological control, and achieves a refractive index gradient of 1.2 to 1.7 by adjusting the sol composition to achieve improved anti-reflective effect.

[0006] In order to solve the above technical problems, the present invention adopts the following technical solution: an anti-reflective surface treatment process of a tempered film comprises the following steps: A. Mechanical cleaning: Use a roller brush dipped in isopropyl alcohol to wipe the tempered film substrate to remove surface particles; B. Chemical activation: First, soak the tempered film substrate in a 6-8% NaOH solution for 12-15 minutes, then rinse with deionized water, and then soak in a 0.15-0.25 mol / L HCl solution for 6-8 minutes, and finally ultrasonically clean with deionized water for 11-13 minutes; C. Surface hydroxylation: Place the clean tempered film obtained in step B in an oxygen plasma treatment chamber for 6 to 8 minutes until active —OH groups are generated on the surface of the clean tempered film; D. Bottom coating; E. Middle layer coating; F. Surface coating; G. UV curing the hydrophobic layer: Use ultraviolet light to cure the tempered film obtained in step F. The wavelength of the ultraviolet light is 370-380nm, the intensity is 53-60mW / cm², and the illumination time is 6-8 minutes to form a highly cross-linked hydrophobic network layer structure.

[0007] Preferably, the bottom coating step D comprises the following steps: D1. Preparation of bottom impregnation sol: Mix a sol with a molar ratio of SiO2:TiO2 = 7:3.5 to 7:4, add 1.5% to 2.5% by mass of a coupling agent, model KH-550, and continue stirring for 25 to 30 hours and age for 13 to 15 hours to obtain a bottom impregnation sol; D2. First Dip and Pull: Place the tempered film substrate obtained in step C into the bottom impregnation sol solution for the first dip and pull until the impregnation sol solution completely covers the tempered film substrate. After staying for 70 to 80 seconds, pull it out of the impregnation sol solution; D3. Dry and solidify the tempered film to form a dense film on the surface of the tempered film.

[0008] Preferably, the middle layer coating step E comprises the following steps: E1. Prepare the middle layer impregnation sol: Take a ZrO2 sol with a molar concentration of 0.35-0.4, dope it with 11%-15% by mass of SiO2 nanoparticles (to prevent cracking), and then add 0.6%-0.8% by mass of oxalic acid (dispersant). Use the cavitation effect of ultrasound to physically disperse the sol for 35-40 minutes; E2. Second dip and pull: Place the tempered film substrate obtained in step D into the bottom impregnation sol solution for a second dip and pull until the impregnation sol solution completely covers the tempered film substrate. After staying for 70 to 80 seconds, pull it out of the impregnation sol solution. E3. Dry and solidify the tempered film to form a dense film on the surface of the tempered film.

[0009] Preferably, the dipping movement speed and the pulling movement speed are both uniformly 16 to 23 mm / min, and the residence time is 45 to 55 seconds (to ensure sufficient wetting).

[0010] Preferably, the drying and curing step is: first, the tempered film obtained in the previous step is placed in a holding box with a temperature of 26-30°C and a humidity of 55-60% and allowed to stand for 35-40 minutes for pre-gelation, then the tempered film is placed in a constant temperature oven at 82-86°C and allowed to stand for 35-40 minutes for preliminary polycondensation, and finally the temperature of the constant temperature oven is adjusted to 120°C and maintained for 30 minutes (to form a dense film).

[0011] Preferably, the outer layer coating step F comprises the following steps: F1. Preparation of a sol solution for impregnation of the outer layer: dilute a fluorosilicone resin with ethanol to a weight percentage of 6-8%, add a photoinitiator at a weight percentage of 2.3-2.6%, and stir in the dark to obtain a sol solution for impregnation of the outer layer; F2, the third dipping and pulling: put the tempered film obtained in step E into the outer layer dipping sol solution, Dipping speed: 23-28 mm / min, Residence time: 35-40 seconds (to prevent the bottom layer from re-dissolving), Pulling speed: 8-9mm / min (reduce the risk of sagging), F3, Strengthening treatment (improving durability): Heat treatment and cross-linking: The tempered film obtained in step F is placed in an oven at 155-160°C for curing for 1.2-1.5 hours (to enhance interlayer bonding strength).

[0012] Preferably, the fluorosilicone resin is an anti-fingerprint liquid product of model KY-130 produced by Shin-Etsu Chemical Co., Ltd.

[0013] Preferably, the photoinitiator is an ultraviolet photoinitiator of model Irgacure 184 produced by BASF, Germany.

[0014] Preferably, in step B, the temperature of the NaOH solution is 63° C. to 68° C., and the tempered film substrate is immersed in the NaOH solution for 12 to 15 minutes.

[0015] The beneficial effects of the present invention are as follows: The present invention provides an anti-reflective surface treatment process for tempered film. This process coats the surface of an object with three thin films having specific optical properties. The film uniformity is excellent and is particularly suitable for substrates with regular shapes (such as flat and spherical lenses). The film thickness can be precisely controlled by the pull-up speed and the concentration of the chemical solution. A very dense film layer with excellent optical properties can be formed. Multiple substrates can be treated in a single pass (mass production), significantly enhancing the anti-reflective effect of the tempered film surface. This process is particularly suitable for cost-sensitive applications or those requiring specific shapes, significantly improving the light transmission performance and visual experience of optical components, and is highly practical. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 This is a flow diagram of the anti-reflective surface treatment process of the present invention. DETAILED DESCRIPTION

[0017] In order to facilitate understanding by those skilled in the art, the present invention will be further described below with reference to the embodiments. The contents mentioned in the embodiments are not intended to limit the present invention.

[0018] like Figure 1 As shown, embodiment 1 of an anti-reflective surface treatment process for a tempered film includes the following steps: A. Mechanical cleaning: Use a roller brush dipped in isopropyl alcohol to wipe the tempered film substrate to remove surface particles; B. Chemical activation: First, soak the tempered film substrate in a 7.8% NaOH solution for 13.5 minutes, then rinse with deionized water, then soak in a 0.18 mol / L HCl solution for 6.7 minutes, and finally ultrasonically clean with deionized water for 12 minutes; C. Surface hydroxylation: Place the clean tempered film obtained in step B in an oxygen plasma treatment chamber for 6.5 minutes until active —OH groups are generated on the surface of the clean tempered film; D. Bottom coating: The bottom coating step D specifically includes the following steps: D1. Preparation of bottom impregnation sol: Mix sol with a molar ratio of SiO2:TiO2 = 7:3.8, add 2% by mass of coupling agent KH-550, continue stirring for 28 hours, and age for 14 hours to obtain bottom impregnation sol; D2. First Dip-Pulling: Place the tempered film substrate obtained in step C into the bottom impregnation sol solution for the first dip-pulling until the impregnation sol solution completely covers the tempered film substrate. After staying for 76 seconds, pull it out of the impregnation sol solution. D3. Dry and solidify the tempered film to form a dense film on the surface of the tempered film; E. Middle layer coating; the middle layer coating step E specifically includes the following steps: E1. Prepare the middle-layer impregnation sol: Take a ZrO2 sol with a molar concentration of 0.38, dope it with 13% by mass of SiO2 nanoparticles, and then add 0.7% by mass of oxalic acid (dispersant). Use the cavitation effect of ultrasound to physically disperse the sol for 38 minutes. The addition of SiO2 nanoparticles effectively prevents the middle-layer coating from cracking during the curing process. The addition of oxalic acid causes the particles in the impregnation sol to form soluble complexes, thereby preventing particle aggregation, precipitation or flocculation, allowing the solid particles to be stably and evenly suspended in the liquid medium, significantly improving the impregnation efficiency.

[0019] E2. Second dip and pull: Place the tempered film substrate obtained in step D into the bottom impregnation sol solution for a second dip and pull until the impregnation sol solution completely covers the tempered film substrate. After staying for 75 seconds, pull it out of the impregnation sol solution; E3. Dry and solidify the tempered film to form a dense film on the surface of the tempered film; F. Surface coating: The surface coating step F specifically includes the following steps: F1. Preparation of outer layer impregnation sol: Fluorosilicone resin was diluted with ethanol to 7% by weight, and 2.5% by weight of a photoinitiator was added. The mixture was stirred in the dark to obtain an outer layer impregnation sol.

[0020] F2. Third dipping and pulling: Place the tempered film obtained in step E into the outer layer dipping sol solution at a dipping speed of 25 mm / min and a residence time of 38 seconds, which effectively prevents the bottom layer from re-dissolving. The pulling speed is 8.5 mm / min, which greatly reduces the risk of sagging and has high reliability. F3. Heat treatment and cross-linking: The tempered film obtained in step F is placed in a 158°C oven for curing for 1.3 hours. After this strengthening treatment, the interlayer bonding strength between the bottom coating layer, the middle coating layer, and the outer coating layer is greatly enhanced, and the durability is greatly improved; G. UV curing the hydrophobic layer: The tempered film obtained in step F is cured by ultraviolet light. The wavelength of the ultraviolet light is 375nm, the intensity is 57mW / cm², and the illumination time is 7 minutes to form a highly cross-linked hydrophobic network layer structure.

[0021] In the first embodiment, the dipping movement speed and the pulling movement speed are both uniformly set at 19 mm / min, and the residence time is 50 seconds, ensuring that the tempered film is fully wetted.

[0022] In the first embodiment of the present invention, the drying and curing steps are as follows: first, the tempered film obtained in the previous step is placed in a holding box with a temperature of 28°C and a humidity of 58% and allowed to stand for 37 minutes for pre-gelation; then, the tempered film is placed in a constant temperature oven at 83°C and allowed to stand for 37 minutes for preliminary polycondensation; finally, the temperature of the constant temperature oven is adjusted to 120°C and maintained for 30 minutes to form a dense film, thereby further improving reliability.

[0023] In the first embodiment, the fluorosilicone resin is an anti-fingerprint liquid product of model KY-130 produced by Shin-Etsu Chemical Co., Ltd.

[0024] In the first embodiment, the photoinitiator is an ultraviolet photoinitiator of model number Irgacure 184 produced by BASF of Germany.

[0025] In the first embodiment, in step B, the temperature of the NaOH solution is 65° C., and the tempered film substrate is immersed in the NaOH solution for 13 minutes.

[0026] The present invention's anti-reflective surface treatment process for tempered glass films coats the surface of an object with three thin layers of thin films with specific optical properties. The resulting films are highly uniform and are particularly suitable for substrates with regular shapes (such as flat and spherical lenses). The film thickness can be precisely controlled by the pull-up speed and the concentration of the chemical solution, resulting in a highly dense film layer with excellent optical properties. Multiple substrates can be treated in a single pass, enabling mass production and significantly improving the anti-reflective effect of the tempered glass surface. This process is particularly suitable for cost-sensitive applications or those requiring specific shapes, significantly enhancing the light transmission and visual experience of optical components, and is highly practical.

[0027] A second embodiment of an anti-reflective surface treatment process for a tempered film differs from the first embodiment described above in that: In step B, the mass percentage concentration of the NaOH solution is 8%, the soaking time of the tempered film substrate in the NaOH solution is 12 minutes, the molar concentration of the HCl solution is 0.15 mol / L, the soaking time of the tempered film substrate in the HCl solution is 8 minutes, and the ultrasonic cleaning time with deionized water is 13 minutes.

[0028] In step D, the molar ratio of SiO2 to TiO2 in the mixed sol is 7:3.5, the mass percentage of the coupling agent model KH-550 is 2.5%, and the aging time after continuous stirring for 30 hours is 13 hours.

[0029] In step E, a middle-layer impregnation sol solution is prepared: a ZrO2 sol with a molar concentration of 0.4 is doped with 11% SiO2 nanoparticles, which can also achieve the purpose of crack prevention. Oxalic acid with a mass percentage concentration of 0.8% is then added. Due to its dispersant effect, the particles in the impregnation sol solution form soluble complexes, thereby preventing the particles from aggregating, settling or flocculating. The solid particles can be stably and evenly suspended in the liquid medium, significantly improving the impregnation efficiency. The sol is physically dispersed using the cavitation effect of ultrasound for 35 minutes.

[0030] In step F, the weight percentage of the fluorosilicone resin in the ethanol diluent is 6%, the weight percentage of the photoinitiator is 2.6%, the third dipping speed is 28 mm / min, the residence time is 40 seconds to prevent the bottom layer from re-dissolving, and the pulling speed is 8 mm / min, which effectively reduces the risk of sagging.

[0031] Example 3 of an anti-reflective surface treatment process for a tempered film differs from the above-mentioned Example 1 in that: in step B, the mass percentage concentration of the NaOH solution is 6%, the tempered film substrate is immersed in the NaOH solution for 15 minutes, the molar concentration of the HCl solution is 0.25 mol / L, the tempered film substrate is immersed in the HCl solution for 6 minutes, and the time for ultrasonic cleaning with deionized water is 11 minutes.

[0032] In step D, the molar ratio of SiO2 to TiO2 in the mixed sol is 7:4, the mass percentage of the coupling agent model KH-550 is 1.5%, and the stirring time is continued for 25 hours and then the aging time is 15 hours.

[0033] In step E, a sol solution for the middle impregnation layer is prepared: a ZrO2 sol with a molar concentration of 0.35 is doped with 15% SiO2 nanoparticles to prevent cracking. Oxalic acid is then added at a concentration of 0.6% by weight to form soluble complexes with the particles within the impregnation sol. This prevents particle aggregation, precipitation, or flocculation, allowing the solid particles to be stably and evenly suspended in the liquid medium, significantly improving impregnation efficiency. The sol is then physically dispersed using ultrasonic cavitation for 40 minutes.

[0034] In step F, the weight percentage of fluorosilicone resin in the ethanol diluent is 8%, the weight percentage of the photoinitiator is 2.3%, the third dipping speed is 23 mm / min, the residence time is 35 seconds to prevent the bottom layer from re-dissolving, and the pulling speed is 9 mm / min to reduce the risk of sagging.

[0035] In the description of the present invention, it should be noted that, for directional words, such as the terms "center", "horizontal (X)", "longitudinal (Y)", "vertical (Z)", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise" and the like, indicating directions and positional relationships, are based on the directions or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific direction, be constructed and operated in a specific direction, and cannot be understood as limiting the specific scope of protection of the present invention.

[0036] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features. Therefore, the terms "first" and "second" may explicitly or implicitly refer to one or more of these features. Throughout the description of the present invention, "several" means two or more, unless otherwise specifically defined.

[0037] In the present invention, unless otherwise specified or limited, the terms "assemble," "connect," and "connect" should be understood in a broad sense. For example, they may refer to fixed connection, detachable connection, or integral connection; mechanical connection; direct connection, connection through an intermediate medium, or internal communication between two components. Those skilled in the art will understand the specific meanings of the above terms in the present invention based on specific circumstances.

[0038] The above-described embodiments merely represent several implementations of the present invention. While the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that a person skilled in the art would be able to make various modifications and improvements without departing from the spirit of the present invention, all of which fall within the scope of protection of the present invention. Therefore, the scope of protection of the present invention shall be determined by the appended claims.

Claims

1. The anti-reflective surface treatment process of the tempered film is characterized by The steps include: A. Mechanical cleaning: Use a roller brush dipped in isopropyl alcohol to wipe the tempered film substrate to remove surface particles; B. Chemical activation: First, soak the tempered film substrate in a 6-8% NaOH solution for 12-15 minutes, then rinse with deionized water, and then soak in a 0.15-0.25 mol / L HCl solution for 6-8 minutes, and finally ultrasonically clean with deionized water for 11-13 minutes; C. Surface hydroxylation: Place the clean tempered film obtained in step B in an oxygen plasma treatment chamber for 6 to 8 minutes until active —OH groups are generated on the surface of the clean tempered film; D. Bottom coating; E. Middle layer coating; F. Surface coating; G. UV curing the hydrophobic layer: Use ultraviolet light to cure the tempered film obtained in step F. The wavelength of the ultraviolet light is 370-380nm, the intensity is 53-60mW / cm², and the illumination time is 6-8 minutes to form a highly cross-linked hydrophobic network layer structure.

2. The anti-reflective surface treatment process for a tempered film according to claim 1, characterized in that: The bottom coating step D comprises the following steps: D1. Preparation of bottom impregnation sol: Mix a sol with a molar ratio of SiO2:TiO2 = 7:3.5 to 7:4, add 1.5% to 2.5% by mass of a coupling agent, model KH-550, and continue stirring for 25 to 30 hours and age for 13 to 15 hours to obtain a bottom impregnation sol; D2. First Dip and Pull: Place the tempered film substrate obtained in step C into the bottom impregnation sol solution for the first dip and pull until the impregnation sol solution completely covers the tempered film substrate. After staying for 70 to 80 seconds, pull it out of the impregnation sol solution; D3. Dry and solidify the tempered film to form a dense film on the surface of the tempered film.

3. The anti-reflective surface treatment process for a tempered film according to claim 1, characterized in that: The middle layer coating step E comprises the following steps: E1. Prepare the middle layer impregnation sol: Take a ZrO2 sol with a molar concentration of 0.35-0.4, dope it with 11%-15% SiO2 nanoparticles, and then add 0.6%-0.8% oxalic acid by weight. Use the cavitation effect of ultrasound to physically disperse the sol for 35-40 minutes; E2. Second dip and pull: Place the tempered film substrate obtained in step D into the bottom impregnation sol solution for a second dip and pull until the impregnation sol solution completely covers the tempered film substrate. After staying for 70 to 80 seconds, pull it out of the impregnation sol solution. E3. Dry and solidify the tempered film to form a dense film on the surface of the tempered film.

4. The anti-reflective surface treatment process for a tempered film according to claim 2 or 3, characterized in that: The dipping movement speed and the pulling movement speed are both uniformly 16 to 23 mm / min, and the residence time is 45 to 55 seconds.

5. The anti-reflective surface treatment process for a tempered film according to claim 2 or 3, characterized in that: The drying and curing steps are as follows: first, the tempered film obtained in the previous step is placed in a holding box with a temperature of 26-30°C and a humidity of 55-60% and is allowed to stand for 35-40 minutes for pre-gelation; then, the tempered film is placed in a constant temperature oven at 82-86°C and is allowed to stand for 35-40 minutes for preliminary polycondensation; finally, the temperature of the constant temperature oven is adjusted to 120°C and maintained for 30 minutes.

6. The anti-reflective surface treatment process for a tempered glass film according to claim 1, characterized in that: The outer surface coating step F comprises the following steps: F1. Preparation of a sol solution for impregnation of the outer layer: dilute a fluorosilicone resin with ethanol to a weight percentage of 6-8%, add a photoinitiator at a weight percentage of 2.3-2.6%, and stir in the dark to obtain a sol solution for impregnation of the outer layer; F2, the third dipping and pulling: put the tempered film obtained in step E into the outer layer dipping sol solution, Dipping speed: 23-28 mm / min, Dwell time: 35 to 40 seconds, Pulling speed: 8-9 mm / min, F3. Heat treatment and cross-linking: The tempered film obtained in step F is placed in an oven at 155-160°C for curing for 1.2-1.5 hours.

7. The anti-reflective surface treatment process for a tempered film according to claim 6, characterized in that: The fluorosilicone resin is an anti-fingerprint liquid product of model KY-130 produced by Shin-Etsu Chemical Co., Ltd.

8. The anti-reflective surface treatment process for a tempered film according to claim 6, characterized in that: The photoinitiator is an ultraviolet photoinitiator of model Irgacure 184 produced by BASF of Germany.

9. The anti-reflective surface treatment process for a tempered film according to claim 1, characterized in that: In the step B, the temperature of the NaOH solution is 63° C. to 68° C., and the tempered film substrate is immersed in the NaOH solution for 12 to 15 minutes.

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