Ag glass and method of making the same

Abstract

The application relates to the technical field of anti-dazzle glass, in particular to AG glass and a preparation method thereof.The preparation method of the AG glass comprises the following steps: 1) coating: performing coating treatment on one surface of a glass substrate, the film layer is silicon nitride, and a glass substrate with a silicon nitride film layer is prepared; 2) etching: etching the glass substrate with the silicon nitride film layer by using an etching liquid, the etching liquid contains acid, and the acid is hydrofluoric acid.The preparation method provided in the application can obtain AG glass products with high roughness on the basis of not using traditional chemical frosting liquid, and compared with a traditional chemical frosting process, the preparation method has the advantages of simple process, small environmental pollution and the like.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of anti-glare glass, in particular to an AG glass and a preparation method thereof. BACKGROUND

[0002] AG (Anti-glare) glass, also known as anti-reflective glass or anti-glare glass. Generally, the smooth glass surface is processed to make the glass surface from a smooth surface to a rough surface, so that it changes from mirror reflection to diffuse reflection, so as to achieve the effect of anti-glare, thereby obtaining AG glass.

[0003] At present, AG glass is basically prepared by chemical frosting, that is, the glass surface needs to be frosted. Chemical frosting refers to soaking or flushing treatment of glass substrate with frosting liquid (mainly including ammonium fluoride, organic acid such as citric acid or inorganic acid such as sulfuric acid, and water, etc.) to make the glass surface frosted. As a conventional processing method of AG glass, chemical frosting can obtain AG products with different application scenarios and different functions, but due to the use of ammonium fluoride, organic acid and other substances, the substances themselves have a greater impact on the environment, and the treatment of wastewater and slag is difficult, which is contrary to the increasing demand of people for the environment, and the operation is harmful to the operator. The drawbacks of this frosting method are obvious.

[0004] AG glass can be applied to glass mouse pad, mobile phone back cover and other products. For glass mouse pad, the roughness of AG glass generally needs to be 0.4-0.6 μm, and the haze needs to be 28%-38%. The existing AG glass that can meet the use requirements of glass mouse pad is mainly prepared by the above-mentioned chemical frosting. Not only is it harmful to the operator and pollutes the environment, but also the operation process is relatively complex. Generally, a frosting liquid containing hydrogen fluoride and ammonium fluoride is used to frosted the glass substrate. The frosting solution not only has a certain volatility, but also has a high COD value and ammonia nitrogen value, which makes the treatment difficult and costly. SUMMARY

[0005] In view of the above defects of the traditional method, the purpose of the present application is to provide an AG glass and a preparation method thereof. The method of the present application can replace the traditional chemical frosting process to obtain a glass that meets the use requirements.

[0006] In a first aspect, the present application provides a preparation method of AG glass, which comprises:

[0007] 1) Film plating

[0008] One surface of the glass substrate is subjected to film plating treatment, and the film layer is silicon nitride (Si3N4), thereby obtaining a glass substrate with a silicon nitride film layer;

[0009] 2) etching

[0010] The glass substrate with the silicon nitride film layer is etched by an etching solution, the etching solution contains an acid, the acid is hydrofluoric acid, and the acid concentration in the etching solution is 0.2-5 mol / L.

[0011] Optionally, in step 1), the glass substrate is borosilicate glass, high-alumina glass or soda-lime glass.

[0012] Optionally, in step 1), the film coating process includes magnetron sputtering.

[0013] Further, the conditions of the magnetron sputtering include: base pressure ≤0.001 Pa, working pressure: 0.2-0.5 Pa, argon flow rate: 100-140 sccm, nitrogen flow rate: 100-140 sccm, target power: 9-11 kW, and target material: silicon target.

[0014] Further, the film coating process includes: under the action of an electric field E, electrons collide with argon atoms in the process of flying to the glass substrate, causing ionization to produce argon positive ions and new electrons, the new electrons fly to the substrate, and the argon positive ions accelerate to the silicon target under the action of the electric field and bombard the target surface with high energy, causing the target to sputter.

[0015] Optionally, in step 1), the film coating makes the thickness of the silicon nitride film layer on the glass substrate be 100-800 nm.

[0016] Optionally, in step 2), the etching solution further contains a monovalent alkali metal salt, and the molar ratio of the monovalent alkali metal salt to hydrofluoric acid is 1:(1-10).

[0017] Further, the monovalent alkali metal salt is sodium chloride and / or potassium chloride.

[0018] Optionally, in the etching solution, the concentration of hydrofluoric acid is 1-3 mol / L, and the molar ratio of the monovalent alkali metal salt to hydrofluoric acid is 1:(2-5).

[0019] Optionally, step 2) includes: soaking the glass substrate with the silicon nitride film layer in the etching solution, and making the silicon nitride react with the etching solution under bubbling conditions.

[0020] Further, the bubbling gas in the bubbling is air, and the bubbling flow rate is 150-250 L / min.

[0021] Further, in step 2), the temperature at which the silicon nitride reacts with the etching solution is 10-40°C, and the reaction time is 5-30 min.

[0022] Optionally, the preparation method further comprises: washing the etched glass.

[0023] In a second aspect, the present application provides an AG glass prepared by the preparation method of the first aspect of the present application.

[0024] Optionally, the AG glass has a roughness of 0.4 μm-0.6 μm, a haze of 28%-38%, an R sm 70 μm-150 μm, and a gloss of 25 GU-35 GU.

[0025] The preparation method of the AG glass provided by the present application can prepare an AG glass product with good AG performance without using a traditional chemical frosting solution. Compared with the traditional chemical frosting process, the preparation method has the advantages of simple process and small environmental pollution. Furthermore, the AG glass prepared by the preparation method of the present application has stable AG parameters, and is particularly suitable for (but not limited to) a mouse pad AG product. DETAILED DESCRIPTION

[0026] In order to facilitate the understanding of the present application, the present application will be described more fully below. The preferred embodiments of the present application are given below. However, the present application can be realized in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the disclosure of the present application more thorough and comprehensive.

[0027] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the present application belongs. The terminology used in the description of the present application herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the present application. As used herein, the term "and / or" includes any and all combinations of one or more of the associated listed items.

[0028] The present application provides a preparation method of an AG glass, which comprises:

[0029] 1) coating

[0030] coating a surface of a glass substrate to prepare a glass substrate with a silicon nitride film layer;

[0031] 2) etching

[0032] etching the glass substrate with a silicon nitride film layer using an etching solution, wherein the etching solution contains an acid, the acid is hydrofluoric acid, and the acid concentration in the etching solution is 0.2 mol / L-5 mol / L.

[0033] In the present application, the glass substrate can be cut into a target size (for example, 500mm x 600mm) before being coated.

[0034] In some embodiments, the glass substrate is borosilicate glass, aluminosilicate glass or soda-lime glass. Preferably, the glass substrate is soda-lime glass from the perspective of being suitable for a mouse pad.

[0035] In the present application, the thickness of the glass substrate can be 0.1mm-0.4mm.

[0036] In step 1), in order to prepare a film layer with uniform thickness, in some embodiments, the coating process comprises magnetron sputtering.

[0037] The coating process can comprise: under the action of an electric field E, electrons collide with argon atoms during flight to the glass substrate, causing ionization to produce argon positive ions and new electrons, the new electrons fly to the substrate, and the argon positive ions accelerate to the silicon target under the action of the electric field and bombard the target surface with high energy, causing the target to sputter.

[0038] In some embodiments, the coating conditions comprise: base pressure ≤0.001Pa, working pressure: 0.2Pa-0.5Pa, argon flow rate: 100sccm-140sccm, nitrogen flow rate: 100sccm-140sccm, target power: 9kW-11kW, and target material: silicon target.

[0039] In some embodiments, in step 1), the coating process makes the thickness of the silicon nitride film layer on the glass substrate 100nm-800nm, for example, 100nm, 150nm, 200nm, 250nm, 300nm, 350nm, 400nm, 450nm, 500nm, 550nm, 600nm, 650nm, 700nm, 750nm, 800nm.

[0040] Alternatively, the coating process makes the thickness of the silicon nitride film layer on the glass substrate 400nm-600nm.

[0041] In step 2), a rough surface can be formed by etching the glass substrate with the silicon nitride film layer using an etching solution. The inventors of the present application have found in research that when a glass substrate plated with a Si3N4 film layer is contacted with an HF solution, the following reaction occurs: Si3N4+4HF+9H2O==3H2SiO3+4NH4F, the generated H2SiO3 is a precipitate which adheres to the glass surface, hinders the contact between HF and Si3N4, and due to the disordered reaction, a uniform but disordered concave-convex shape is produced on the glass surface, the glass surface changes from a mirror surface to a rough surface, the mirror reflection changes to diffuse reflection, and thus an AG glass with anti-glare function can be obtained.

[0042] In some embodiments, the concentration of hydrofluoric acid in the etching solution is 1-5 mol / L, for example, 1 mol / L, 1.5 mol / L, 2 mol / L, 2.5 mol / L, 3 mol / L, 3.5 mol / L, 4 mol / L or 5 mol / L.

[0043] In some embodiments, the etching solution further comprises a monovalent alkali metal salt, and the molar ratio of the monovalent alkali metal salt to hydrofluoric acid is 1:(1-10).

[0044] Optionally, the monovalent alkali metal salt is sodium chloride and / or potassium chloride.

[0045] In the present application, the glass substrate plated with a Si3N4 film layer is contacted with HF and a monovalent alkali metal salt at the same time, not only the precipitate H2SiO3 adhering to the glass surface is generated, but also a fluorosilicate alkali metal salt is generated. Specifically, Si3N4 reacts with HF: Si3N4+12HF=3SiF4+4NH3, the generated SiF4 reacts with HF: SiF4+2HF=H2SiF6, H2SiF6 is generated, on the one hand, H2SiF6 undergoes a hydrolysis reaction: H2SiF6+3H2O=H2SiO3↓+6HF, to generate H2SiO3 precipitate, on the other hand, H2SiF6 reacts with the alkali metal salt to generate a precipitate of a fluorosilicate alkali metal salt (such as Na2SiF6, K2SiF6, for example, NaCl: H2SiF6+2NaCl=Na2SiF6↓+2HCl), and since the fluorosilicate alkali metal salt particles are fine, the roughness of the AG product can be reduced, and thus the roughness of the AG product can be further adjusted by the ratio of HF to the monovalent alkali metal salt in the etching solution. 6+ 2NaCl=Na2SiF6↓+2HCl), and since the fluorosilicate alkali metal salt particles are fine, the roughness of the AG product can be reduced, and thus the roughness of the AG product can be further adjusted by the ratio of HF to the monovalent alkali metal salt in the etching solution.

[0046] In some preferred embodiments, the concentration of hydrofluoric acid in the etching solution is 1-3 mol / L, and the molar ratio of the monovalent alkali metal salt to hydrofluoric acid is 1:(2-5), so that an AG glass with better comprehensive performance can be prepared.

[0047] In some embodiments, step 2) comprises: soaking the glass substrate with the silicon nitride film layer in the hydrofluoric acid solution, and reacting the silicon nitride with the etching solution under bubbling condition. By bubbling, the uniformity of the reaction can be further improved.

[0048] Optionally, in the bubbling, the bubbling gas used is air, and the bubbling flow rate is 150 L / min-250 L / min.

[0049] Optionally, the temperature for the reaction of the silicon nitride with the etching solution (i.e. the soaking temperature) is 10℃-40℃, such as 10℃, 15℃, 20℃, 25℃, 30℃, 35℃, 40℃.

[0050] Optionally, the reaction time of the silicon nitride with the etching solution (i.e. the soaking time) is 2 min-30 min, such as 10 min, 15 min, 20 min.

[0051] In some embodiments, the preparation method can further comprise: washing the etched glass (frosted glass) to remove the residual acid solution on the surface of the product.

[0052] The washing solution used in the washing can be a weak alkaline cleaning agent (such as a sodium hydroxide solution with a pH of 8-10) and pure water.

[0053] According to a specific embodiment, the preparation method of the AG glass of the present application comprises the following process flow:

[0054] S0: cutting

[0055] The glass substrate is cut, edged and cut into a target size;

[0056] S1: coating

[0057] The glass substrate is coated by a magnetron sputtering coating method (single-sided coating);

[0058] S2: etching

[0059] The coated glass substrate is soaked in the etching solution and bubbling is started to react the silicon nitride with the etching solution to form an AG effect;

[0060] S3: washing

[0061] The AG frosted glass obtained after etching is taken out of the etching tank and washed to remove the residual acid on the surface to obtain an AG glass with anti-glare function.

[0062] In the method provided in the present application, the non-AG surface of the glass can not be protected by coating, compared with the non-AG surface of the glass substrate in the traditional frosting process which must be protected by coating, and the process is obviously simplified and the cost is obviously reduced.

[0063] The present application also provides the AG glass prepared by the preparation method of the first aspect of the present application. The AG glass prepared by the method of the present application is an AG frosting glass, and the AG glass prepared by the method is particularly suitable for application to a mouse pad product.

[0064] In some preferred embodiments, the roughness of the AG glass is 0.4 μm-0.6 μm, the haze is 28%-38%, the R sm The gloss is 70 μm-150 μm-150 μm, and the gloss is 25 GU-35 GU.

[0065] The following are specific embodiments of the present application.

[0066] The embodiments are used to illustrate the AG glass and the preparation method thereof of the present application.

[0067] In the following examples and comparative examples, the glass substrate is soda-lime glass (500 mm x 600 mm).

[0068] Example 1

[0069] The glass substrate is sent into a flat plate cleaning machine for cleaning, and then Si3N4 is plated on one surface of the glass substrate by magnetron sputtering. Specifically, the glass substrate is attached to a carrier plate, and Si3N4 film is plated on the glass substrate by magnetron sputtering in a plasma region provided with a silicon target, wherein the background pressure is ≤0.001 Pa, the working pressure is 0.4 Pa, the argon flow rate is 120 sccm, the nitrogen flow rate is 120 sccm, and the target power is 10 kW.

[0070] The plated glass substrate with a Si3N4 thickness of 500 nm is prepared by the above method.

[0071] Then, the plated glass substrate is immersed in an etching solution (the etching solution is an aqueous solution of hydrofluoric acid and sodium chloride, the concentration of hydrofluoric acid is 3 mol / L, and the molar ratio of sodium chloride to hydrofluoric acid is 1:2), air is introduced for bubbling (gas flow rate is 200 L / min), and bubbling is carried out at 30°C for 15 min to obtain the etched plated glass.

[0072] Finally, the etched glass is sequentially cleaned with a weak alkaline cleaning agent and pure water, and then dried to obtain the AG glass, which is denoted as G1.

[0073] Example 2

[0074] The glass substrate is sent into a flat plate cleaning machine for cleaning, and then Si3N4 is plated on one surface of the glass substrate by magnetron sputtering. Specifically, the glass substrate is pasted onto a carrier plate, and then Si3N4 film is plated on the glass substrate by magnetron sputtering in a plasma region provided with a silicon target. In this process, the base pressure is less than or equal to 0.001 Pa, the working pressure is 0.4 Pa, the argon flow rate is 120 sccm, the nitrogen flow rate is 120 sccm, and the target power is 10 kW.

[0075] In this way, a glass substrate with a Si3N4 film with a thickness of 500 nm is prepared.

[0076] Then, the glass substrate with the film is immersed in an etching solution (the etching solution is an aqueous solution of hydrofluoric acid and sodium chloride, the concentration of the hydrofluoric acid is 1 mol / L, and the molar ratio of the sodium chloride to the hydrofluoric acid is 1:5), and air is bubbled (the gas flow rate is 200 L / min) at 30°C for 15 min to obtain the etched glass substrate with the film.

[0077] Finally, the etched glass substrate is sequentially cleaned with a weak alkaline cleaning agent and pure water, and then dried to obtain an AG glass, which is denoted as G2.

[0078] Example 3

[0079] The glass substrate is sent into a flat plate cleaning machine for cleaning, and then Si3N4 is plated on one surface of the glass substrate by magnetron sputtering. Specifically, the glass substrate is pasted onto a carrier plate, and then Si3N4 film is plated on the glass substrate by magnetron sputtering in a plasma region provided with a silicon target. In this process, the base pressure is less than or equal to 0.001 Pa, the working pressure is 0.4 Pa, the argon flow rate is 120 sccm, the nitrogen flow rate is 120 sccm, and the target power is 10 kW.

[0080] In this way, a glass substrate with a Si3N4 film with a thickness of 500 nm is prepared.

[0081] Then, the glass substrate with the film is immersed in an etching solution (the etching solution is an aqueous solution of hydrofluoric acid and sodium chloride, the concentration of the hydrofluoric acid is 1 mol / L, and the molar ratio of the sodium chloride to the hydrofluoric acid is 1:3), and air is bubbled (the gas flow rate is 200 L / min) at 30°C for 15 min to obtain the etched glass substrate with the film.

[0082] Finally, the etched glass substrate is sequentially cleaned with a weak alkaline cleaning agent and pure water, and then dried to obtain an AG glass, which is denoted as G3.

[0083] Example 4

[0084] The glass substrate is sent into a flat plate cleaning machine for cleaning, and then Si3N4 is plated on one surface of the glass substrate by magnetron sputtering. Specifically, the glass substrate is pasted onto a carrier plate, and then Si3N4 film is plated on the glass substrate by magnetron sputtering in a plasma region provided with a silicon target, wherein the base pressure is less than or equal to 0.001 Pa, the working pressure is 0.4 Pa, the argon flow rate is 120 sccm, the nitrogen flow rate is 120 sccm, and the target power is 10 kW.

[0085] In the above manner, a glass substrate with a Si3N4 film with a thickness of 500 nm is prepared.

[0086] Then, the glass substrate with the film is immersed in an etching solution (the etching solution is an aqueous solution of hydrofluoric acid and sodium chloride, the concentration of the hydrofluoric acid is 3 mol / L, and the molar ratio of the sodium chloride to the hydrofluoric acid is 1:1), and air is bubbled (the gas flow rate is 200 L / min) at 30°C for 15 min to obtain the etched glass substrate with the film.

[0087] Finally, the etched glass substrate is sequentially cleaned with a weak alkaline cleaning agent and pure water, and then dried to obtain an AG glass, which is denoted as G4.

[0088] Example 5

[0089] The glass substrate is sent into a flat plate cleaning machine for cleaning, and then Si3N4 is plated on one surface of the glass substrate by magnetron sputtering. Specifically, the glass substrate is pasted onto a carrier plate, and then Si3N4 film is plated on the glass substrate by magnetron sputtering in a plasma region provided with a silicon target, wherein the base pressure is less than or equal to 0.001 Pa, the working pressure is 0.4 Pa, the argon flow rate is 120 sccm, the nitrogen flow rate is 120 sccm, and the target power is 10 kW.

[0090] In the above manner, a glass substrate with a Si3N4 film with a thickness of 500 nm is prepared.

[0091] Then, the glass substrate with the film is immersed in an etching solution (the etching solution is an aqueous solution of hydrofluoric acid and sodium chloride, the concentration of the hydrofluoric acid is 3 mol / L, and the molar ratio of the sodium chloride to the hydrofluoric acid is 1:1), and air is bubbled (the gas flow rate is 200 L / min) at 30°C for 15 min to obtain the etched glass substrate with the film.

[0092] Finally, the etched glass substrate is sequentially cleaned with a weak alkaline cleaning agent and pure water, and then dried to obtain an AG glass, which is denoted as G4.

[0093] Comparative Example 1

[0094] The glass substrate is sent into a flat plate cleaning machine for cleaning, and Si3N4 is plated on one surface of the glass substrate by magnetron sputtering. Specifically, the glass substrate is pasted onto a carrier plate, and Si3N4 film is plated on the glass substrate by magnetron sputtering through a plasma region provided with a silicon target, wherein the base pressure is ≤0.001 Pa, the working pressure is 0.4 Pa, the argon flow rate is 120 sccm, the nitrogen flow rate is 120 sccm, and the target power is 10 kW.

[0095] In the above manner, a plated glass substrate with a Si3N4 thickness of 500 nm is prepared.

[0096] Next, the plated glass substrate is immersed in an etching solution (the etching solution is an aqueous solution of hydrofluoric acid with a concentration of 10 mol / L), air is introduced for bubbling (gas flow rate: 200 L / min), and the bubbling is performed at 30°C for 15 min to obtain an etched plated glass.

[0097] Finally, the etched glass is sequentially cleaned with a weak alkaline cleaning agent and pure water, and dried to obtain an AG glass, which is denoted as D-G1.

[0098] Comparative Example 2

[0099] The glass substrate is sent into a flat plate cleaning machine for cleaning, and Si3N4 is plated on one surface of the glass substrate by magnetron sputtering. Specifically, the glass substrate is pasted onto a carrier plate, and Si3N4 film is plated on the glass substrate by magnetron sputtering through a plasma region provided with a silicon target, wherein the base pressure is ≤0.001 Pa, the working pressure is 0.4 Pa, the argon flow rate is 120 sccm, the nitrogen flow rate is 120 sccm, and the target power is 10 kW.

[0100] In the above manner, a plated glass substrate with a Si3N4 thickness of 500 nm is prepared.

[0101] Next, the plated glass substrate is immersed in an etching solution (the etching solution is an aqueous solution of hydrofluoric acid with a concentration of 10 mol / L), air is introduced for bubbling (gas flow rate: 200 L / min), and the bubbling is performed at 30°C for 15 min to obtain an etched plated glass.

[0102] Finally, the etched glass is sequentially cleaned with a weak alkaline cleaning agent and pure water, and dried to obtain an AG glass, which is denoted as D-G1.

[0103] Comparative Example 3

[0104] The glass substrate is sent into a flat plate cleaning machine for cleaning, and SiO2 is plated on one surface of the glass substrate by magnetron sputtering. Specifically, the glass substrate is pasted onto a carrier plate, and the SiO2 film layer is plated on the glass substrate by magnetron sputtering through a plasma region provided with a silicon target. In this process, the base pressure is less than or equal to 0.001 Pa, the working pressure is 0.4 Pa, the argon flow rate is 120 sccm, the nitrogen flow rate is 120 sccm, and the target power is 10 kW.

[0105] In this way, the glass substrate with a SiO2 film layer with a thickness of 500 nm is prepared.

[0106] Next, the glass substrate with the film layer is immersed in the etching solution (the same as in Example 1), and air is introduced for bubbling (gas flow rate: 200 L / min) at 30°C for 15 min to obtain the etched glass substrate with the film layer.

[0107] Finally, the etched glass substrate is sequentially cleaned with a weak alkaline cleaning agent and pure water, and dried to obtain the AG glass, which is denoted as D-G3.

[0108] Example 6

[0109] The glass substrate is sent into a flat plate cleaning machine for cleaning, and SiO2 is plated on one surface of the glass substrate by magnetron sputtering. Specifically, the glass substrate is pasted onto a carrier plate, and the SiO2 film layer is plated on the glass substrate by magnetron sputtering through a plasma region provided with a silicon target. In this process, the base pressure is less than or equal to 0.001 Pa, the working pressure is 0.4 Pa, the argon flow rate is 120 sccm, the nitrogen flow rate is 120 sccm, and the target power is 10 kW.

[0110] In this way, the glass substrate with a SiO2 film layer with a thickness of 500 nm is prepared.

[0111] Next, the glass substrate with the film layer is immersed in the etching solution (the same as in Example 1), and air is introduced for bubbling (gas flow rate: 200 L / min) at 30°C for 15 min to obtain the etched glass substrate with the film layer.

[0112] Finally, the etched glass substrate is sequentially cleaned with a weak alkaline cleaning agent and pure water, and dried to obtain the AG glass, which is denoted as D-G3.

[0113] Example 7

[0114] The glass substrate is sent into a flat plate cleaning machine for cleaning, and then Si3N4 is plated on one surface of the glass substrate by magnetron sputtering. Specifically, the glass substrate is pasted onto a carrier plate, and then Si3N4 film is plated on the glass substrate by magnetron sputtering in a plasma region provided with a silicon target, wherein the base pressure is less than or equal to 0.001 Pa, the working pressure is 0.4 Pa, the argon flow rate is 120 sccm, the nitrogen flow rate is 120 sccm, and the target power is 10 kW.

[0115] In the above manner, a glass substrate with a Si3N4 film with a thickness of 500 nm is prepared.

[0116] Then, the glass substrate with the film is immersed in an etching solution (the etching solution is an aqueous solution of hydrofluoric acid and potassium chloride, the concentration of the hydrofluoric acid is 2 mol / L, and the molar ratio of the potassium chloride to the hydrofluoric acid is 1:4), air is bubbled (the gas flow rate is 180 L / min), and the glass substrate is bubbled at 30°C for 15 min to obtain an etched glass substrate with the film.

[0117] Finally, the etched glass substrate with the film is sequentially cleaned with a weak alkaline cleaning agent and pure water, and then dried to obtain an AG glass, which is denoted as G7.

[0118] Example 8

[0119] The glass substrate is sent into a flat plate cleaning machine for cleaning, and then Si3N4 is plated on one surface of the glass substrate by magnetron sputtering. Specifically, the glass substrate is pasted onto a carrier plate, and then Si3N4 film is plated on the glass substrate by magnetron sputtering in a plasma region provided with a silicon target, wherein the base pressure is less than or equal to 0.001 Pa, the working pressure is 0.4 Pa, the argon flow rate is 120 sccm, the nitrogen flow rate is 120 sccm, and the target power is 10 kW.

[0120] In the above manner, a glass substrate with a Si3N4 film with a thickness of 500 nm is prepared.

[0121] Then, the glass substrate with the film is immersed in an etching solution (the etching solution is an aqueous solution of hydrofluoric acid and potassium chloride, the concentration of the hydrofluoric acid is 2 mol / L, and the molar ratio of the potassium chloride to the hydrofluoric acid is 1:4), air is bubbled (the gas flow rate is 180 L / min), and the glass substrate is bubbled at 30°C for 15 min to obtain an etched glass substrate with the film.

[0122] Finally, the etched glass substrate with the film is sequentially cleaned with a weak alkaline cleaning agent and pure water, and then dried to obtain an AG glass, which is denoted as G7.

[0123] Comparative Example 4

[0124] The glass substrate is sent into a flat plate cleaning machine for cleaning, and then Si3N4 is plated on one surface of the glass substrate by magnetron sputtering. The specific operation is as follows: the glass substrate is pasted on a carrier plate, and then the Si3N4 film layer is plated on the glass substrate by magnetron sputtering through a plasma area provided with a silicon target, wherein the base pressure is ≤0.001 Pa, the working pressure is 0.4 Pa, the argon flow rate is 120 sccm, the nitrogen flow rate is 120 sccm, and the target power is 10 kW.

[0125] In the above manner, the plated glass substrate with a Si3N4 thickness of 500 nm is prepared.

[0126] Then, the plated glass substrate is immersed in an etching solution (the etching solution is an aqueous solution of hydrofluoric acid and calcium chloride, the concentration of hydrofluoric acid is 10 mol / L, and the molar ratio of calcium chloride to hydrofluoric acid is 1:4), and air is introduced for bubbling (the gas flow rate is 200 L / min), and the bubbling is performed at 30°C for 15 min to obtain the etched plated glass.

[0127] Finally, the etched glass is sequentially cleaned with a weak alkaline cleaning agent and pure water, and then dried to obtain the AG glass, which is denoted as D-G4.

[0128] Comparative Example 5

[0129] The side of the glass substrate which does not need to be etched is protected by silk-screen coating with an etching-resistant ink;

[0130] The side of the glass substrate which needs to be etched is cleaned, and then placed in a frosting device in a wet state, the frosting device is provided with a frosting solution, and the temperature is controlled at 20°C for immersion for 180 s, and the glass substrate is oscillated during the immersion; (the frosting solution is composed of the following components in percentage by mass: 16% ammonium bifluoride, 12% ammonium fluoride, 18% concentrated hydrochloric acid, 10% concentrated sulfuric acid, 3% potassium sulfate, 3% tricalcium phosphate, and water in balance).

[0131] Then, the frosted glass substrate is subjected to chemical polishing treatment, that is, the frosted glass substrate is immersed in an etching solution (the etching solution is an aqueous solution of hydrofluoric acid, and the concentration of hydrofluoric acid is 3 mol / L), and air is introduced for bubbling (the gas flow rate is 200 L / min), and the bubbling is performed at 30°C for 15 min to obtain the chemically polished plated glass.

[0132] Finally, the chemically polished frosted glass substrate is sequentially cleaned with a weak alkaline cleaning agent and pure water, and then dried to obtain the AG glass, which is denoted as D-G5.

[0133] Performance test

[0134] The performances of the AG glasses (G1-G8 and D-G1-D-G5) prepared in the above examples and comparative examples are tested, wherein the product roughness and R smRoughness: tested by roughness tester; Haze: tested by transmittance haze tester; Gloss: tested by gloss meter.

[0135] The test results are shown in Table 1.

[0136] Table 1

[0137]

[0138]

[0139] Note: In Comparative Example 2, nitric acid did not react with silicon nitride.

[0140] In combination with the data in Table 1, it can be seen from the comparison of Examples 1-8 and Comparative Examples 1-4 that the AG glass prepared by the method of the present application has appropriate roughness and haze, and is suitable for use as a mouse pad.

[0141] In addition, it can be seen from the comparison of Examples 1-3 and Examples 4-5, and the comparison of Examples 6-7 and Example 8 that the introduction of an appropriate proportion of monovalent alkali metal in the etching solution is beneficial to improving the AG parameters of the AG product.

[0142] It can be seen from the comparison of Examples 1-8 and Comparative Example 5 that, compared with the traditional chemical sandblasting method, the preparation method of Examples 1-8 is simple.

[0143] The technical features of the above-described embodiments can be combined in any manner. In order to make the description concise, not all possible combinations of the technical features in the above-described embodiments are described, however, as long as the combinations of the technical features do not contradict each other, they should be considered as within the scope of the present application.

[0144] The above-described embodiments only express several implementation manners of the present application, and the description is relatively specific and detailed, but it should not be understood as a limitation on the scope of the present application. It should be pointed out that, for those skilled in the art, without departing from the concept of the present application, a number of modifications and improvements can be made, which are all within the protection scope of the present application. Therefore, the protection scope of the present application should be subject to the appended claims.

Claims

1. A method for preparing AG glass, characterized in that, The preparation method includes: 1) Coating A glass substrate is prepared by coating one surface of a glass substrate with silicon nitride. 2) Etching The glass substrate with silicon nitride film is etched using an etching solution containing an acid and a monovalent alkali metal salt. The acid is hydrofluoric acid, and the concentration of the acid in the etching solution is 1 mol / L-5 mol / L. The molar ratio of the monovalent alkali metal salt to hydrofluoric acid is 1:(1-10). The AG glass has a roughness of 0.4μm-0.6μm, a haze of 28%-38%, and R... sm The thickness ranges from 70μm to 150μm, and the gloss level is 25GU to 35GU.

2. The preparation method according to claim 1, characterized in that, In step 1), the glass substrate is borosilicate glass, high-alumina glass, or soda-lime glass.

3. The preparation method according to claim 1, characterized in that, In step 1), the coating process includes magnetron sputtering, and the conditions for magnetron sputtering include: background pressure ≤ 0.001 Pa, working pressure: 0.2 Pa - 0.5 Pa, argon flow rate: 100 sccm - 140 sccm, nitrogen flow rate: 100 sccm - 140 sccm, target power: 9 kW - 11 kW, and target material: silicon target.

4. The preparation method according to claim 1, characterized in that, In step 1), the thickness of the silicon nitride film on the glass substrate is 100nm-800nm ​​through the coating process.

5. The preparation method according to claim 1, characterized in that, In step 2), the monovalent alkali metal salt is sodium chloride and / or potassium chloride.

6. The preparation method according to claim 5, characterized in that, The concentration of hydrofluoric acid in the etching solution is 1 mol / L-3 mol / L, and the molar ratio of the monovalent alkali metal salt to hydrofluoric acid is 1:(2-5).

7. The preparation method according to any one of claims 1-6, characterized in that, Step 2) includes: The glass substrate with the silicon nitride film is immersed in the etching solution, and under bubbling conditions, the silicon nitride reacts with the etching solution.

8. The preparation method according to claim 7, characterized in that, The bubbling gas in the bubble is air, and the bubbling flow rate is 150L / min-250L / min.

9. The preparation method according to claim 7, characterized in that, In step 2), the temperature at which the silicon nitride reacts with the etching solution is 10℃-40℃ and the reaction time is 5min-30min.

10. The preparation method according to claim 1, characterized in that, The preparation method also includes washing the etched glass.

11. AG glass prepared by the preparation method according to any one of claims 1-10.

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