Anti-reflection glass and preparation method therefor

Abstract

Disclosed are a type of anti-reflection glass and a preparation method therefor. The method comprises the following steps: S1, preparing an H-layer coating solution, and then accurately measuring a refractive index and solid content thereof; S2, preparing an L-layer coating solution, and then accurately measuring a refractive index and solid content thereof; S3, using optical film system design software to calculate a required refractive index and thickness of each layer in an MHL film system; S4, on the basis of a calculated required refractive index for an M-layer coating solution, mixing the H-layer coating solution and the L-layer coating solution, to obtain a refractive index required for the M-layer coating solution, preparing the M-layer coating solution, and then accurately measuring the refractive index and solid content of the M-layer coating solution; S5, accurately adjusting the required solid contents for the M-layer coating solution, H-layer coating solution and L-layer coating solution for the second time; S6, sequentially performing coating, surface drying and pre-curing of the M-layer coating solution, the H-layer coating solution and the L-layer coating solution; S7, placing pre-cured optical glass into a high-temperature oven for curing, to obtain anti-reflection glass.

Description

Antireflection glass and preparation method thereof TECHNICAL FIELD

[0001] The present application belongs to the technical field of functional glass, and particularly relates to an antireflection glass and a preparation method thereof. BACKGROUND

[0002] With a substantial reduction in price, display screens, especially liquid crystal display screens, are everywhere in life, such as mobile phones, tablets, notebook computers, televisions and other special display screens.

[0003] The surface of a liquid crystal display screen is mainly made of cellulose triacetate and glass. When the eyes look at the screen, ambient stray light will enter the eyes together with the light on the screen image. In order to reduce the influence of ambient stray light on the display effect, there are four methods to reduce the glare of the screen, which are micron anti-glare (AG), antireflection film (AR) with multi-layer optical structure, moth-eye micro-nano structure and nano microspheres that can reduce glare.

[0004] Among them, AG processing has a particle diameter of micron level, and haze will easily cause a flash point, so in the field of high-definition display screens, the antireflection film (AR) with multi-layer optical structure has a significant advantage for high-resolution image display.

[0005] The conventional implementation of the antireflection film (AR) is mainly vacuum evaporation coating (PVD), magnetron sputtering and liquid roller coating or coating methods. Among them, the adhesion and wear resistance of PVD coating on glass are relatively poor, and magnetron sputtering is commonly used in the display screen field to make super-hard AR coating, and the reflectivity can be <1.0%.

[0006] The existing photovoltaic glass coating uses double-layer coating, which has the advantages of high efficiency of 11 square per minute and low cost. The double-layer antireflection coating liquid and process of 1.30-1.35 and 1.44-1.48 are commonly used in the field of display screens, and the reflectivity can be lower than 1.2, but the wear resistance is far inferior to that of super-hard AR coating.

[0007] Magnetron sputtering is used to make super-hard AR coating on display screens. Because the production equipment is expensive, the production capacity is low (only 30 pieces of 12-inch glass cover plate per hour for medium-sized equipment), and the yield is low, the cost of display screen cover glass AR is very high, and only a few manufacturers can use it.

[0008] However, coating the anti-reflective coating (AR) on the glass by the dip coating process also brings significant problems, the biggest problem is that if the glass that has been chemically tempered is used for dip coating process, due to the difference in the solvent volatilization speed between the periphery and the middle of the glass during the dip coating process, the thickness difference is generated, that is, the periphery is relatively thick, and the middle is relatively thin, and there is a significant color difference between the periphery and the middle of the glass, and the part with the color difference is the invalid edge. If the substrate is plastic, the invalid edge can be removed by mechanical processing, if the glass that has been chemically tempered is used, the problem brought by removing the invalid edge by mechanical processing or laser processing is mainly low processing efficiency and high cost, and more importantly, the impact resistance of the tempered glass is reduced.

[0009] Therefore, if a coating that can resist chemical tempering can be developed, the coating process is first performed on the untempered glass, the invalid edge is removed by mechanical processing, and then the glass is chemically tempered after edge grinding and polishing, the low-cost and high-efficiency AR processing can be realized, and the impact resistance of the glass can be ensured.

[0010] SUMMARY

[0011] To solve the above problems, the present application provides a kind of anti-reflective glass and its preparation method.

[0012] The present application adopts the following technical solutions:

[0013] A kind of anti-reflective glass preparation method, specifically comprising the following steps:

[0014] S1, the nano titanium dioxide sol, silane coupling agent, water, acid catalyst and alcohol solvent are mixed uniformly, after 4-48 hours of maturation reaction at 25-80 DEG C, the H layer plating solution with solid content of 3.0-8.0% is configured, and the refractive index and solid content of the H layer plating solution are accurately determined;

[0015] S2, the silica sol, silane coupling agent, water, acid catalyst and alcohol solvent are mixed uniformly, after 4-48 hours of maturation reaction at 25-80 DEG C, the L layer plating solution with solid content of 3.0-8.0% is configured, and the refractive index and solid content of the L layer plating solution are accurately determined;

[0016] S3, optical film system design is carried out, and the refractive index and thickness required by each layer of the MHL film system are calculated by optical film system design software;

[0017] S4, the refractive index required by the M layer plating solution is obtained by compounding the refractive index required by the M layer plating solution from the H layer plating solution and the L layer plating solution, the M layer plating solution with solid content of 3.0-8.0% is configured, and the refractive index and solid content of the M layer plating solution are accurately determined;

[0018] S5, according to the thickness of dip coating needs, fixed range of pulling speed, respectively twice accurate adjustment of M layer plating solution, H layer plating solution and L layer plating solution required solid content;

[0019] S6, coating the required thickness of M layer plating solution on optical glass, then surface dry, then pre-curing, and then cooling to room temperature, then coating the required thickness of H layer plating solution, then surface dry, then pre-curing, and then cooling to room temperature, finally coating the required thickness of L layer plating solution, then surface dry, then pre-curing.

[0020] S7, the pre-cured optical glass is put into a high temperature oven for curing to obtain an antireflection glass.

[0021] Preferably, step S7 is followed by step S8, and the specific process of step S8 is that the coated antireflection glass is CNC processed to remove the invalid edge or edge grinding treatment according to the drawing, and then enters a potassium nitrate chemical tempering furnace for tempering treatment.

[0022] Preferably, the silane coupling agent in steps S1 and S2 is one or a combination of more than one of Y-R1-Si(OR2)3 or Si(OR2)3 or Si(OR2)4, wherein Y is an organic functional group, OR2 is a siloxy group, and R1 is methyl, ethyl, propyl, isopropyl or butyl.

[0023] Preferably, the initial solid content of the H layer plating solution, the L layer plating solution and the M layer plating solution in steps S1, S2 and S4 is 3-8%, and the viscosity of the H layer plating solution, the L layer plating solution and the M layer plating solution is 1.0-4.0cp.

[0024] Preferably, the specific process of step S6 is: coating the required thickness of M layer plating solution on optical glass, then surface drying at 50-80℃ for 3-15 minutes, then pre-curing at 100-200℃ for 3-15 minutes, and then cooling to room temperature, then coating the required thickness of H layer plating solution, then surface drying at 50-80℃ for 3-10 minutes, then pre-curing at 100-200℃ for 3-15 minutes, and then cooling to room temperature, finally coating the required thickness of L layer plating solution, then surface drying at 50-80℃ for 3-15 minutes, and then pre-curing at 100-200℃ for 3-15 minutes.

[0025] Preferably, the film thickness of the M layer antireflection coating, the H layer antireflection coating and the L layer antireflection coating in the antireflection glass after step S7 is 60-200nm.

[0026] Preferably, in the antireflection glass after curing in step S7, the refractive index of the M layer antireflection coating is 1.60-1.80, and the film thickness is 60-120 nm; the refractive index of the H layer antireflection coating is 1.80-2.10, and the film thickness is 60-120 nm; and the refractive index of the L layer antireflection coating is 1.30-1.50, and the film thickness is 60-200 nm.

[0027] Preferably, the curing temperature in step S7 is 200-600℃, and the curing time is 10-180 minutes.

[0028] An antireflection glass prepared by the preparation method of the antireflection glass.

[0029] From the above scheme, a more optimal scheme can be obtained, that is, after the L layer, the M layer antireflection coating, the H layer antireflection coating and the L layer antireflection coating are coated with four layers of coating solution, the optical film system design software simulation can achieve better optical effect than the MHL three layers. The optical effect can be better than the design effect of four layers or three layers of coating film by using six layers or eight layers of even layers or five layers, seven layers of odd layers or even more layers of coating film design. The difference lies in that the more the number of coating layers, the better the optical effect, but the lower the yield and the higher the cost. In the industrialization link, it is necessary to reasonably design the above-mentioned three layers, four layers, five layers or other multi-layer coating structure according to the optical effect and cost structure.

[0030] After the above technical scheme is adopted, the antireflection glass prepared by the present application has the following advantages compared with the background art: in the antireflection glass prepared by the present application, the film thickness of the M layer antireflection coating, the H layer antireflection coating and the L layer antireflection coating is 60-200 nm, which is lower than 60 nm and is not good for precise control of the film thickness, and is higher than 200 nm, which is not conducive to the generation of optical interference effect; before the optical glass is coated with a coating, the reflectivity is 4%, and after the optical glass is coated with the M layer coating solution, the H layer coating solution and the L layer coating solution of the present application and is cured, the reflectivity of the prepared antireflection glass is reduced to 0.8%, and the antireflection effect of the light can be realized; the present application adopts sol-gel coating, which has the characteristics of good wear resistance, good chemical resistance, good light aging resistance and good weather resistance, and has the advantages of high production efficiency, large size and special-shaped parts compared with traditional magnetron sputtering and PVD coating. In addition, the most significant feature is that the coating can be resistant to chemical tempering of potassium nitrate at 420 degrees or above for 180 minutes without being damaged. BRIEF DESCRIPTION OF DRAWINGS

[0031] Fig. 1 is a structural schematic view of the antireflection glass prepared by the present application;

[0032] Figure 2 is a reflectivity curve comparison diagram of the anti-reflection glass prepared by the present application and ordinary glass;

[0033] Figure 3 is a transmittance curve comparison diagram of the anti-reflection glass prepared by the present application and ordinary glass. DETAILED DESCRIPTION

[0034] In order to make the purpose, technical scheme and advantages of the present application more clear, the present application is further described in detail below in combination with the drawings and examples. It should be understood that the specific examples described herein are only used to explain the present application and do not limit the present application.

[0035] Referring to Figures 1 to 3.

[0036] A preparation method of anti-reflection glass, specifically comprising the following steps:

[0037] S1, uniformly mix nano-titanium dioxide sol, silane coupling agent, water, acid catalyst and alcohol solvent, after 4-48 hours of maturation reaction at 25-80℃, prepare H-layer coating solution with solid content of 3.0-8.0%, and then accurately determine the refractive index and solid content of the H-layer coating solution;

[0038] S2, uniformly mix silica sol, silane coupling agent, water, acid catalyst and alcohol solvent, after 4-48 hours of maturation reaction at 25-80℃, prepare L-layer coating solution with solid content of 3.0-8.0%, and then accurately determine the refractive index and solid content of the L-layer coating solution;

[0039] S3, design optical film system, and calculate the refractive index and thickness required for each layer of the MHL film system by using optical film system design software;

[0040] S4, according to the refractive index required for the M-layer coating solution, obtain the refractive index required for the M-layer coating solution by compounding the H-layer coating solution and the L-layer coating solution, prepare M-layer coating solution with solid content of 3.0-8.0%, and then accurately determine the refractive index and solid content of the M-layer coating solution;

[0041] S5, according to the thickness required for dip coating, fix the pulling speed, and accurately adjust the solid content required for the M-layer coating solution, the H-layer coating solution and the L-layer coating solution respectively for the second time;

[0042] S6, coat the M-layer coating solution with the required thickness on the optical glass, then surface dry, then pre-cure, and then cool to room temperature; then coat the H-layer coating solution with the required thickness, then surface dry, then pre-cure, and then cool to room temperature; finally coat the L-layer coating solution with the required thickness, then surface dry, then pre-cure;

[0043] S7, put the pre-cured optical glass into a high-temperature oven for curing to obtain anti-reflection glass.

[0044] The step S7 is followed by a step S8, and the specific process of the step S8 is that the coated anti-reflection glass is subjected to CNC machining to remove the invalid edges or edge grinding treatment according to the drawing, and then is subjected to a tempering treatment in a potassium nitrate chemical tempering furnace.

[0045] The silane coupling agent in the steps S1 and S2 is one or a combination of multiple of Y-R1-Si(OR2)3 or Si(OR2)3 or Si(OR2)4, wherein Y is an organic functional group, OR2 is a siloxy group, and R1 is a methyl group, an ethyl group, a propyl group, an isopropyl group or a butyl group.

[0046] The initial solid content of the H-layer coating solution, the L-layer coating solution and the M-layer coating solution in the steps S1, S2 and S4 is 3-8%, and the viscosity of the H-layer coating solution, the L-layer coating solution and the M-layer coating solution is 1.0-4.0 cp.

[0047] The specific process of the step S6 is that the M-layer coating solution with a required thickness is coated on the optical glass, followed by a surface drying at 50-80℃ for 3-15 minutes, and then a pre-curing at 100-200℃ for 3-15 minutes, and then cooling to room temperature; then the H-layer coating solution with a required thickness is coated, followed by a surface drying at 50-80℃ for 3-10 minutes, and then a pre-curing at 100-200℃ for 3-15 minutes, and then cooling to room temperature; and finally the L-layer coating solution with a required thickness is coated, followed by a surface drying at 50-80℃ for 3-15 minutes, and then a pre-curing at 100-200℃ for 3-15 minutes.

[0048] The film thickness of the M-layer anti-reflection coating, the H-layer anti-reflection coating and the L-layer anti-reflection coating in the anti-reflection glass after the step S7 is curing is 60-200 nm.

[0049] The refractive index of the M-layer anti-reflection coating is 1.60-1.80, the film thickness is 60-120 nm; the refractive index of the H-layer anti-reflection coating is 1.80-2.10, the film thickness is 60-120 nm; and the refractive index of the L-layer anti-reflection coating is 1.30-1.50, the film thickness is 60-200 nm.

[0050] The curing temperature in the step S7 is 200-600℃, and the curing time is 10-180 minutes.

[0051] The reflectivity curve comparison between the anti-reflection glass prepared by the method and the ordinary glass is shown in Fig. 2, and the transmittance curve comparison between the anti-reflection glass prepared by the method and the ordinary glass is shown in Fig. 3.

[0052] An anti-reflection glass is prepared by the method.

[0053] The M layer, H layer and L layer of the antireflection glass each has at least one layer, that is, the number of layers of the antireflection coating of the antireflection glass can be three, four, five, six, etc., for example, when the number of layers is four, from the inside to the outside, the layers can be optical glass, L layer antireflection coating, M layer antireflection coating, H layer antireflection coating and L layer antireflection coating, and the refractive index and film thickness of each layer can be obtained according to the optical film system design software, and the thickness and refractive index of the film system design and the optical effect can be flexibly adjusted in step S6, and examples are not listed one by one due to the limited length.

[0054] The above description is only the preferred embodiment of the present application, but the protection scope of the present application is not limited to this. Any changes or replacements within the technical range disclosed by the present application can be easily thought by those skilled in the art, and should be covered in the protection scope of the present application. Therefore, the protection scope of the present application should be subject to the protection scope of the claims.

Claims

1. A method for producing an antireflection glass, characterized by, Specifically comprising the following steps: S1, mixing nano titanium dioxide sol, silane coupling agent, water, acid catalyst and alcohol solvent uniformly, after aging reaction at 25-80℃ for 4-48 hours, configuring H layer coating solution with solid content of 3.0-8.0%, and then accurately measuring the refractive index and solid content of the H layer coating solution; S2, mixing silica sol, silane coupling agent, water, acid catalyst and alcohol solvent uniformly, after aging reaction at 25-80℃ for 4-48 hours, configuring L layer coating solution with solid content of 3.0-8.0%, and then accurately measuring the refractive index and solid content of the L layer coating solution; S3, optical film system design, calculating the refractive index and thickness required for each layer of MHL film system by optical film system design software; S4, according to the refractive index required for M layer coating solution, the required refractive index of M layer coating solution is obtained by compounding H layer coating solution and L layer coating solution, and M layer coating solution with solid content of 3.0-8.0% is configured, and then the refractive index and solid content of the M layer coating solution are accurately measured; S5, according to the thickness required for dip coating respectively, fixing the range of pulling speed, and adjusting the solid content required for M layer coating solution, H layer coating solution and L layer coating solution respectively twice; S6, coating the required thickness of M layer coating solution on the optical glass, then surface drying, then pre-curing, and then cooling to room temperature; then coating the required thickness of H layer coating solution, then surface drying, then pre-curing, and then cooling to room temperature; finally, coating the required thickness of L layer coating solution, then surface drying, and then pre-curing; S7, placing the pre-cured optical glass into a high temperature oven for curing to obtain antireflection glass.

2. A method of making a glass with reduced reflection and increased transmission according to claim 1, characterized in that: After step S7, step S8 is further included, and the specific process of step S8 is that the antireflection glass with coating is CNC processed to remove invalid edges or ground edge treatment according to the drawing, and then enters the potassium nitrate chemical tempering furnace for tempering treatment.

3. The method of claim 1, wherein the glass is a low-iron glass.

3. The method of claim 1, wherein the glass is a low-iron glass. The silane coupling agent in steps S1 and S2 is one or a combination of Y-R1-Si(OR2)3 or Si(OR2)3 or Si(OR2)4, wherein Y is an organic functional group, OR2 is siloxy, and R1 is methyl, ethyl, propyl, isopropyl or butyl.

4. The method of claim 1, wherein the glass is a low-iron glass. The initial solid content of the H layer coating solution, the L layer coating solution and the M layer coating solution in steps S1, S2 and S4 is 3-8%, and the viscosity of the H layer coating solution, the L layer coating solution and the M layer coating solution is 1.0-4.0cp.

5. The method of claim 1, wherein the glass is a low-iron glass. The specific process of step S6 is: coating the required thickness of M layer coating solution on the optical glass, then surface drying at 50-80℃ for 3-15 minutes, then pre-curing at 100-200℃ for 3-15 minutes, and then cooling to room temperature; then coating the required thickness of H layer coating solution, then surface drying at 50-80℃ for 3-10 minutes, then pre-curing at 100-200℃ for 3-15 minutes, and then cooling to room temperature; finally, coating the required thickness of L layer coating solution, surface drying at 50-80℃ for 3-15 minutes, and then pre-curing at 100-200℃ for 3-15 minutes.

6. The method of claim 1 wherein the glass is a low-iron glass. The film thickness of the M layer, the H layer and the L layer in the anti-reflection glass after curing in step S7 is 60-200 nm.

7. The method of claim 1, wherein the glass is a low-iron glass. The refractive index of the M layer is 1.60-1.80, the film thickness is 60-120 nm; the refractive index of the H layer is 1.80-2.10, the film thickness is 60-120 nm; the refractive index of the L layer is 1.30-1.50, the film thickness is 60-200 nm.

8. The method for preparing anti-reflection glass according to claim 1, wherein: The curing temperature in the curing in step S7 is 200-600 ℃, and the curing time is 10-180 minutes.

9. An antireflective glass, characterized by: The anti-reflection glass is prepared by the method of any one of claims 1-8.

10. A transparent, antireflective glass according to claim 9, wherein: The M layer, the H layer and the L layer are combined into four, six, eight even layers or five, seven odd layers or even more layers in the anti-reflection glass, which can achieve better optical effect than the MHL three-layer optical design.

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