3A glass preparation method and 3A glass thereof

Abstract

The invention discloses a 3A glass preparation method and 3A glass thereof, and belongs to the technical field of optical glass preparation. The 3A glass preparation method comprises the specific steps of 1, AG treatment, 2, AR film coating, 3, AF treatment, 4, inspection and 5, double-sided shipment protection film covering. The step 1 comprises high-pressure deionized water cleaning, the step 2 comprises placing the glass substrate subjected to AG treatment on a carrier plate in a vacuum environment, and sequentially plating a base layer and alternately stacking low-refractive-index layers and high-refractive-index layers on the surface of the glass substrate subjected to AG treatment by adopting multi-target magnetron sputtering equipment and an adjustable magnet device to form a composite film layer, so that the edge optical effect is improved; and the binding force and the light transmittance between the film layers are improved.

Description

Technical Field

[0001] The invention belongs to the technical field of optical glass preparation, and specifically relates to a 3A glass preparation method and 3A glass. Background Art

[0002] 3A glass is AG, AR, and AF. AG glass, originally from Germany, is also known as low-reflection glass, anti-glare glass, and low-reflection glass. It features a specially processed surface that transforms the reflective surface of the original glass into a matte, non-reflective finish. This is achieved by subjecting one or both sides of a high-quality glass sheet to a special treatment that reduces its reflectivity compared to ordinary glass, reducing light reflectivity from 8% to below 1%. Typical testing criteria include transmittance, gloss, roughness, and haze, with some also testing for UV and infrared parameters. AR utilizes state-of-the-art magnetron sputtering technology to coat ordinary tempered glass with an anti-reflective coating. This effectively reduces inherent reflections and increases transmittance, making colors appear more vivid and realistic. AF anti-fingerprint coating forms a layer of nano-chemical material on the glass surface, minimizing surface tension and reducing the contact area between dust and the glass. This prevents fingerprints from leaving marks on the screen, keeping it clean while enhancing the glass's hardness and scratch resistance.

[0003] The existing 3A glass preparation process has the following technical bottlenecks: 1. During the AG treatment process, uneven coverage of the frosting liquid causes fluctuations in the etching rate, and acid etching residues cause surface microcracks, resulting in a yield rate of less than 70%; 2. During AR coating, the plasma distribution in the edge area is uneven, the film thickness gradient exceeds ±8%, and the edge transmittance drops by more than 15% compared with the center area; 3. The interfacial bonding between the AF film and the AR film is weak (<3B level), and the contact angle decays by >20° after 500 times of steel wool friction.

[0004] At the same time, the AF film layer is significantly affected by the AR effect, and is prone to insufficient bonding strength, low hardness, and friction resistance. Research on ultra-hard anti-glare and anti-reflective glass technology can effectively control light reflection issues on the glass surface and improve surface scratch resistance, thereby effectively extending the service life and user experience. Summary of the Invention

[0005] To solve the above-mentioned problems, the present invention discloses a 3A glass preparation method and its 3A glass, which improves the acid etching uniformity in the AG treatment stage, improves the optical effect of the glass substrate edge in the AR stage, and increases the bonding strength and transmittance performance of the AR film layer.

[0006] To achieve the above objectives, the specific technical solutions of this application are as follows: A 3A glass preparation method, comprising the following steps: 1. AG treatment → 2. AR coating → 3. AF treatment → 4. inspection → 5. double-sided protective film coating; The specific steps of the AG processing include: 1.1. Clean the glass substrate once; 1.2. Cover the back of the cleaned glass substrate with an acid-resistant protective film; 1.3. Acid washing to activate the surface of the glass substrate; 1.4. Secondary cleaning to remove acid residues; 1.5. Cover the front surface of the glass to be AG-etched with a layer of frosting liquid for frosting treatment; 1.6. Use high-pressure deionized water to remove excess frosting liquid residue during the third cleaning; 1.7. Make the front surface of the glass substrate fully react with the polishing liquid, roughen the front surface and form a matte non-reflective surface; 1.8. Use high-pressure deionized water to remove the residual polishing liquid during the fourth cleaning; 1.9. Wind shear to remove water residue; The specific steps of AR coating include: 2.1. Cleaning before cutting and AR; 2.2. Attach a PE electrostatic film to the front of the glass substrate and a high-temperature resistant protective film to the back; 2.3. Bond the back of the glass substrate to a carrier plate with an area larger than the glass substrate using high-temperature resistant double-sided tape, and then place the carrier plate on the coating substrate rack; 2.4. Remove the PE static film on the front to collect water vapor and remove water vapor from the glass surface; 2.5. Using a multi-target magnetron sputtering device and an adjustable magnet device in a vacuum environment, a base layer and alternately stacked low-refractive index layers and high-refractive index layers are sequentially deposited on the surface of the AG-treated glass substrate to form a composite film layer at a coating temperature of 80°C. 2.6. After annealing and cooling, remove the AR-coated glass substrate from the carrier; The specific steps of the AF processing include: 3.1. Clean the surface of the glass substrate using an ion source; 3.2. Use a multi-gun head to spray AF oil mainly composed of fluorosilane. The spraying time is 5 minutes and the spraying distance is 700-900mm. 3.3. Bake in a tunnel oven at 150°C for 30 minutes to solidify the film; The specific inspection steps include: removing the high-temperature resistant protective film on the back of the glass substrate and inspecting the film layer performance, wherein the film layer performance includes but is not limited to reflectivity, Mohs hardness, roughness, AF water drop angle, and AF friction resistance.

[0007] In the step 1.3, 5% citric acid is used for pickling activation, and the pickling activation treatment time is 3 minutes and the temperature is 25°C.

[0008] In step 1.5, the frosting liquid comprises 10-15 parts of 400 mesh barium sulfate, 15-20 parts of potassium fluoride, 30-40 parts of ammonium bifluoride, 3-5 parts of ferric chloride, 5-10 parts of hydrofluoric acid, and 20-30 parts of water. The frosting treatment time is 3 minutes and the temperature is 25°C.

[0009] In the step 1.7, the chemical polishing liquid is 20% HF acid, the chemical polishing treatment time is 20 minutes, and the temperature is 25°C.

[0010] In step 2.4, the treatment time of the water vapor collector is 3 minutes and the temperature is -135°C.

[0011] Furthermore, in step 2.5, the low refractive index layer is a SiO2 layer, the high refractive index layer is a Nb2O5 layer, the SiO2 layer and the Nb2O5 layer are alternately stacked at least twice, the first layer directly adjacent to the glass substrate is a SiO2AR coating base layer, and the top layer is a SiO2AF treatment base layer.

[0012] Preferably, the SiO2 layer and the Nb2O5 layer are stacked alternately three times, the first SiO2 layer has a thickness of 15-25nm as an AR coating base layer, the second Nb2O5 layer has a thickness of 5-15nm, the third SiO2 layer has a thickness of 35-55nm, the fourth Nb2O5 layer has a thickness of 35-50nm, the fifth SiO2 layer has a thickness of 15-25nm, the sixth Nb2O5 layer has a thickness of 30-50nm, and the top SiO2 layer has a thickness of 90-100nm as an AF treatment base layer. The total film thickness is (250m-320nm)±5nm.

[0013] Furthermore, the adjustable magnet device used in step 2.5 means that the distance between the magnet device and the target material can be adjusted to change the coating thickness, thereby meeting the requirement of inconsistent thickness of different layers.

[0014] A 3A glass is produced according to any one of the above methods for producing 3A glass.

[0015] Compared with the prior art, the present invention has the following advantages: 1. In the AG stage, this application uses a four-stage gradient cleaning system combined with surface activation treatment to increase the frosting liquid infiltration uniformity to more than 95%. The third and fourth cleanings are cleaned with high-pressure deionized water to improve the cleanliness of the glass substrate, enhance the AG treatment effect and subsequent AR effect; 2. The existing AR coating has poor edge optical effects because the edge of the glass substrate is more susceptible to the influence of gas in the vacuum than the center of the glass substrate. Therefore, the glass substrate to be coated is attached to the center of a larger carrier, thus solving the problems of poor edge optical effects and narrow window during coating. 3. By using the first layer of SiO2 as the base layer for AR coating, and the top layer of coating is also SiO2 as the base layer for subsequent AF treatment, the bonding strength and hardness are increased; 4. A gradient refractive interface is constructed by alternately stacking SiO2 layers with a lower refractive index than the glass substrate and Nb2O5 layers with a higher refractive index than the glass substrate to improve the transmission performance. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 It is a schematic flow chart of a method for preparing 3A glass; Figure 2 This is a structural diagram of 3A glass; Figure 3 3A glass reflectivity curve in the visible light range of the embodiment; It should be noted that in Figure 3 In the figure, X is the wavelength in nm; Y refers to the reflectivity in %, the incident angle of 0 degrees refers to vertical incidence, and IDEAL refers to the brand of the detector.

[0017] List of Figure Symbols: 1. Glass substrate; 2. SiO2AR coating base layer; 3. Second Nb2O5 layer; 4. Third SiO2 layer; 5. Fourth Nb2O5 layer; 6. Fifth SiO2 layer; 7. Sixth Nb2O5 layer; 8. SiO2AF treatment base layer; 9. AF layer. DETAILED DESCRIPTION

[0018] The present invention will be further described below with reference to the accompanying drawings and specific embodiments. It should be understood that the following specific embodiments are only used to illustrate the present invention and are not used to limit the scope of the present invention.

[0019] It should be noted that, in order to make the objectives, technical solutions, and advantages of the present invention more clear, the technical solutions of the present invention will be clearly and completely described below in conjunction with specific embodiments of the present invention and corresponding drawings. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0020] like Figure 1 As shown, a 3A glass preparation method includes the following specific steps: 1. AG treatment → 2. AR coating → 3. AF treatment → 4. Inspection → 5. Double-sided shipping protective film coating.

[0021] The specific steps of the AG processing include: 1.1. Clean the glass substrate once; 1.2. Cover the back of the cleaned glass substrate with an acid-resistant protective film; 1.3. Acid washing to activate the surface of the glass substrate; 1.4. Secondary cleaning to remove acid residues; 1.5. Cover the front surface of the glass to be AG-etched with a layer of frosting liquid for frosting treatment; 1.6. Use high-pressure deionized water to remove excess frosting liquid residue during the third cleaning; 1.7. Make the front surface of the glass substrate fully react with the polishing liquid, roughen the front surface and form a matte non-reflective surface; 1.8. Use high-pressure deionized water to remove the residual polishing liquid during the fourth cleaning; 1.9. Wind shearing removes water residue, improves the cleanliness of the glass substrate, and improves the AG treatment effect and subsequent AR effect; The specific steps of AR coating include: 2.1. Cleaning before cutting and AR; 2.2. Attach a PE electrostatic film to the front of the glass substrate and a high-temperature resistant protective film to the back; 2.3. The back of the glass substrate is bonded to a carrier plate larger than the glass substrate using high-temperature resistant double-sided tape, and then the carrier plate is mounted on a coating substrate rack. The glass substrate to be coated is placed in the middle of the larger carrier plate, thereby solving the problems of poor edge optical effect and narrow window during coating. 2.4. Remove the PE static film on the front to collect water vapor and remove water vapor from the glass surface; 2.5. Using a multi-target magnetron sputtering device and an adjustable magnet device in a vacuum environment, a base layer and alternately stacked low-refractive index layers and high-refractive index layers are sequentially deposited on the surface of the AG-treated glass substrate to form a composite film layer at a coating temperature of 80°C. 2.6. After annealing and cooling, remove the AR-coated glass substrate from the carrier; The specific steps of the AF processing include: 3.1. Clean the surface of the glass substrate using an ion source; 3.2. Spray fluorosilane-based AF oil through a multi-gun head, with a spraying time of 5 minutes and a spraying distance of 700-900mm. Usually, a six-axis robotic arm equipped with an ultrasonic atomizing spray gun is used, with the atomized particle size controlled at 5-8μm and the fluorosilane film thickness at 80-100nm. 3.3. Bake in a tunnel oven at 150°C for 30 minutes to solidify the film; The specific inspection steps include: removing the high-temperature resistant protective film on the back of the glass substrate and inspecting the film layer performance, wherein the film layer performance includes but is not limited to reflectivity, Mohs hardness, roughness, AF water drop angle, and AF friction resistance.

[0022] In the step 1.3, 5% citric acid is used for pickling activation, and the pickling activation treatment time is 3 minutes and the temperature is 25°C.

[0023] In step 1.5, the frosting liquid comprises 10-15 parts of 400 mesh barium sulfate, 15-20 parts of potassium fluoride, 30-40 parts of ammonium bifluoride, 3-5 parts of ferric chloride, 5-10 parts of hydrofluoric acid, and 20-30 parts of water. The frosting treatment time is 3 minutes and the temperature is 25°C.

[0024] In the step 1.7, the chemical polishing liquid is 20% HF acid, the chemical polishing treatment time is 20 minutes, the temperature is 25°C, and nano-scale pits Ra = 0.12-0.15 μm are formed by F⁻ ion reaction.

[0025] In step 2.4, the treatment time of the water vapor collector is 3 minutes and the temperature is -135°C.

[0026] Furthermore, in step 2.5, the low refractive index layer is a SiO2 layer, the high refractive index layer is a Nb2O5 layer, and the SiO2 layer and the Nb2O5 layer are alternately stacked at least twice. The first layer directly adjacent to the glass substrate serves as a SiO2AR coating base layer, and the top layer is a SiO2AF treatment base layer to improve bonding strength and prevent the coating from falling off and affecting its optical properties and hardness.

[0027] Preferably, the SiO2 layer and the Nb2O5 layer are stacked alternately three times, the thickness of the first SiO2 layer is 15-25nm, the thickness of the second Nb2O5 layer is 5-15nm, the thickness of the third SiO2 layer is 35-55nm, the thickness of the fourth Nb2O5 layer is 35-50nm, the thickness of the fifth SiO2 layer is 15-25nm, the thickness of the sixth Nb2O5 layer is 30-50nm, the thickness of the top SiO2 layer is 90-100nm, and the total film thickness is (250m-320nm)±5nm.

[0028] A 3A glass was manufactured by the above-mentioned manufacturing method of the 3A glass, with a reflectivity of ≤0.65@450-650nm, a Mohs hardness of 5, an adhesion of 5B, a 60° gloss of 115±8, a haze of 4±2, and a roughness Ra of 0.06±0.03μm.

[0029] When the 3A glass produced by the production method of the 3A glass of the present application was rubbed under the conditions of 0000# steel wool 1 kgf (2cm*2cm) / speed 60 turns / min, stroke 50 mm, 3000 turns, after rubbing for about 2000 times, the water drop angle was 115°±5°, and there were no friction marks on the surface of the 3A glass.

[0030] In addition, it is worth noting that the adjustable magnet device used in step 2.5 means that the distance between the magnet device and the target material can be adjusted, thereby changing the magnetic field strength and then changing the coating thickness. The same device meets the requirements of inconsistent coating thicknesses of different layers, thereby improving work efficiency.

[0031] In summary, the 3A glass prepared by the simple preparation method of the present application solves the existing problems of poor edge optical effect, narrow window, and shedding and hardness caused by insufficient film bonding strength.

[0032] It should be noted that the above is only an embodiment of the present invention and is not intended to limit the scope of protection of the present invention. For those skilled in the art, any modification, equivalent replacement, improvement, expansion, etc. made within the spirit and principle of the present invention are included in the scope of protection of the present invention.

Claims

1. A method for preparing 3A glass, characterized in that: The specific steps include:

1. AG treatment → 2. AR coating → 3. AF treatment → 4. Inspection → 5. Double-sided shipping protective film; The specific steps of the AG processing include: 1.

1. Clean the glass substrate once; 1.

2. Cover the back of the cleaned glass substrate with an acid-resistant protective film; 1.

3. Acid washing to activate the surface of the glass substrate; 1.

4. Secondary cleaning to remove acid residues; 1.

5. Cover the front surface of the glass to be AG-etched with a layer of frosting liquid for frosting treatment; 1.

6. Use high-pressure deionized water to remove excess frosting liquid residue during the third cleaning; 1.

7. Make the front surface of the glass substrate fully react with the polishing liquid, roughen the front surface and form a matte non-reflective surface; 1.

8. Use high-pressure deionized water to remove the residual polishing liquid during the fourth cleaning; 1.

9. Wind shear to remove water residue; The specific steps of AR coating include: 2.

1. Cleaning before cutting and AR; 2.

2. Attach a PE electrostatic film to the front of the glass substrate and a high-temperature resistant protective film to the back; 2.

3. Bond the back of the glass substrate to a carrier plate with an area larger than the glass substrate using high-temperature resistant double-sided tape, and then place the carrier plate on the coating substrate rack; 2.

4. Remove the PE static film on the front to collect water vapor and remove water vapor from the glass surface; 2.

5. Using a multi-target magnetron sputtering device and an adjustable magnet device in a vacuum environment, a base layer and alternately stacked low refractive index layers and high refractive index layers are sequentially plated on the surface of the AG-treated glass substrate to form a composite film layer; 2.

6. After annealing and cooling, remove the AR coated glass substrate from the carrier; The specific steps of the AF processing include: 3.

1. Clean the surface of the glass substrate using an ion source; 3.

2. Use a multi-gun head to spray AF oil mainly composed of fluorosilane. The spraying time is 5 minutes and the spraying distance is 700-900mm. 3.

3. Bake in a tunnel oven at 150°C for 30 minutes to solidify the film; The specific inspection steps include: removing the high-temperature resistant protective film on the back of the glass substrate and inspecting the film layer performance, wherein the film layer performance includes but is not limited to reflectivity, Mohs hardness, roughness, AF water drop angle, and AF friction resistance.

2. The method for preparing 3A glass according to claim 1, wherein: In the step 1.3, 5% citric acid is used for pickling activation, and the pickling activation treatment time is 3 minutes and the temperature is 25°C.

3. The method for preparing 3A glass according to claim 1, wherein: In step 1.5, the frosting liquid comprises 10-15 parts of 400 mesh barium sulfate, 15-20 parts of potassium fluoride, 30-40 parts of ammonium bifluoride, 3-5 parts of ferric chloride, 5-10 parts of hydrofluoric acid, and 20-30 parts of water. The frosting treatment time is 3 minutes and the temperature is 25°C.

4. The method for preparing 3A glass according to claim 1, wherein: In the step 1.7, the chemical polishing liquid is 20% HF acid, the chemical polishing treatment time is 20 minutes, and the temperature is 25°C.

5. The method for preparing 3A glass according to claim 1, wherein: In step 2.4, the treatment time of the water vapor collector is 3 minutes and the temperature is -135°C.

6. The method for preparing 3A glass according to claim 1, wherein: In step 2.5, the low refractive index layer is a SiO2 layer, the high refractive index layer is a Nb2O5 layer, the SiO2 layer and the Nb2O5 layer are alternately stacked at least twice, the first layer directly adjacent to the glass substrate is a SiO2AR coating base layer, and the top layer is a SiO2AF treatment base layer.

7. The method for preparing 3A glass according to claim 6, wherein: The SiO2 layer and the Nb2O5 layer are stacked alternately three times, the thickness of the first SiO2 layer is 15-25nm, the thickness of the second Nb2O5 layer is 5-15nm, the thickness of the third SiO2 layer is 35-55nm, the thickness of the fourth Nb2O5 layer is 35-50nm, the thickness of the fifth SiO2 layer is 15-25nm, the thickness of the sixth Nb2O5 layer is 30-50nm, the thickness of the top SiO2 layer is 90-100nm, and the total film thickness is (250m-320nm)±5nm.

8. The method for preparing 3A glass according to claim 1, wherein: The adjustable magnet device used in step 2.5 means that the distance between the magnet device and the target material can be adjusted to change the coating thickness to meet the requirement of inconsistent thickness of different layers.

9. 3A glass, prepared according to the 3A glass preparation method according to any one of claims 1 to 8.

Images