A method for predicting and regulating the warpage value of chemically strengthened glass

Abstract

The application belongs to the technical field of chemically strengthened glass, and particularly relates to a prediction method and a regulation method of a warping value of chemically strengthened glass; the prediction method of the warping value of the chemically strengthened glass provided by the application is based on the mechanism that the average particle size of particles in a coating liquid precursor has a direct linear relationship with the warping value of the chemically strengthened glass, the warping value of the chemically strengthened glass is predicted by detecting the average particle size of the particles in the coating liquid in advance, and the warping prediction value of the chemically strengthened glass is calculated by establishing a warping value prediction formula, so that the technical problem that there is no prediction method of the warping value of the chemically strengthened glass in the prior art is solved.

Description

Technical Field

[0001] This application belongs to the field of chemically strengthened glass technology, and in particular relates to a method for predicting and controlling the warpage value of chemically strengthened glass. Background Technology

[0002] Chemically strengthened glass is obtained by ion exchange of float glass in a potassium nitrate molten salt bath. Chemically strengthened glass has high strength and good scratch and wear resistance, and is the basic material for tablet computers and smartphone touch screens. However, due to the different ion exchange rates between the tin-infiltrated side and the air side during the float glass ion exchange process, chemically strengthened glass warps, which affects its use.

[0003] Currently, Naoki Okahata et al. have used HF etching on the tin-infiltrated surface to achieve the same ionic state on both the upper and lower surfaces, which has provided guidance for reducing warpage. Satoshi Miyasaka et al. have used fluorinating agents to treat the glass surface, which can reduce warpage after ion strengthening. B. Navitt et al. have reduced warpage by reducing the degree of ion exchange during ion exchange through ion implantation. These methods require special electrical equipment, which increases the preparation cost of chemically strengthened glass. Coating the air surface of float glass with a coating solution to form a protective film, the particles in the protective film hinder ion exchange, which can reduce the difference in ion exchange rate between the tin-infiltrated surface and the air surface, thereby reducing the warpage value of chemically strengthened glass. This is a low-cost method for preparing chemically strengthened glass with low warpage value.

[0004] However, in the current methods for preparing low-warping chemically strengthened glass by coating the air surface of glass with a coating solution, the research on the effect of the coating solution on reducing the warping value of chemically strengthened glass is not in-depth enough. The relationship between the coating solution and the warping value of chemically strengthened glass is unclear. It is impossible to predict the warping value of chemically strengthened glass based on the coating solution, and it is also impossible to control the warping value of chemically strengthened glass. Summary of the Invention

[0005] In view of this, this application provides a method for predicting and controlling the warpage value of chemically strengthened glass, in order to solve the technical problem of the lack of a method for predicting the warpage value of chemically strengthened glass in the prior art.

[0006] The first aspect of this application provides a method for predicting the warpage value of chemically strengthened glass, including the following steps:

[0007] Step S1: Stir and mix the film-forming components, organic solvent, water and catalyst to obtain the coating solution;

[0008] Step S2: Measure the particles in the coating solution and obtain the average particle size;

[0009] Step S3: Based on the linear relationship between the average particle size and the warpage value of chemically strengthened glass, the warpage value of chemically strengthened glass is predicted.

[0010] Preferably, in step S1, the film-forming component includes at least one of tetraethyl orthosilicate and aluminum isopropoxide.

[0011] Preferably, in step S1, the stirring and mixing temperature is room temperature, and the time is 1 to 2 hours.

[0012] Preferably, in step S2, the method for measuring the particles in the coating solution includes alkaline titration or particle size distribution measurement.

[0013] Preferably, in the linear relationship between the average particle size of the particles and the warpage value of the chemically strengthened glass described in step S3, the fitting formula for the linear relationship is:

[0014] R = -0.0897 + 0.09960D, where R is the predicted warpage value and D is the average particle size.

[0015] Preferably, the organic solvent is selected from at least one of methanol, ethanol, n-propanol, n-butanol, and isopropanol.

[0016] Preferably, the catalyst is selected from at least one of hydrochloric acid, nitric acid, and acetic acid.

[0017] A second aspect of this application provides a method for controlling the warpage value of chemically strengthened glass, the method comprising the steps of:

[0018] Step D1: Based on the linear relationship between the average particle size and the warpage value of chemically strengthened glass, prepare a coating solution containing particles with different average particle sizes;

[0019] Step D2: Coating solution containing particles of different average particle sizes is applied to the air surface of the glass to chemically strengthen it and obtain chemically strengthened glass.

[0020] Preferably, in step D1, the process of preparing a coating solution containing particles with different average particle sizes includes: mixing 28.7 volume parts of film-forming components, 47.8 volume parts of alcohol, 23 volume parts of water and 0.5 volume parts of hydrochloric acid by volume to obtain a coating solution, adjusting the volume ratio of ethanol and isopropanol in the alcohol to prepare a coating solution containing particles with different average particle sizes.

[0021] Preferably, the volume ratio of ethanol to isopropanol is 1:0 to 0.08.

[0022] Preferably, in step D2, the temperature for chemical strengthening is 410°C and the time is 4 hours.

[0023] It should be noted that the control method provided in this application adjusts the volume ratio of ethanol and isopropanol to prepare a coating solution containing particles with different average particle sizes, which is then coated onto the air surface of the glass for chemical strengthening, thereby controlling the warpage value of the chemically strengthened glass.

[0024] In summary, this application provides a method for predicting and controlling the warpage value of chemically strengthened glass. The method for predicting the warpage value of chemically strengthened glass provided by this application includes first preparing a coating solution such as tetraethyl orthosilicate / aluminum isopropoxide, then measuring the average particle size of the particles in the tetraethyl orthosilicate / aluminum isopropoxide coating solution, and then predicting the warpage value of chemically strengthened glass based on the linear relationship between the average particle size and the warpage value of chemically strengthened glass. The prediction method provided by this application is based on the discovery that the particle size in the temporary film coated on the glass air surface has a direct linear relationship with the warpage value of chemically strengthened glass, thereby predicting the warpage value of chemically strengthened glass based on the average particle size. The prediction method has a high prediction accuracy and solves the technical problem of the lack of a prediction method for the warpage value of chemically strengthened glass in the prior art. Attached Figure Description

[0025] To more clearly illustrate the technical solutions in the specific embodiments of this application or the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this application. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0026] Figure 1 This is a schematic diagram of linear regression fitting based on the average particle size of particles in the coating solution and the corresponding warpage value of chemically strengthened glass in Example 2 of this application.

[0027] Figure 2 This is a schematic diagram showing the relationship between the volume ratio of ethanol and isopropanol and the average particle size of the particles in the coating solution in Example 3 of this application.

[0028] Figure 3 This is a schematic diagram showing the relationship between the average particle size of the particles in the coating solution and the warpage value of the chemically strengthened glass in Example 3 of this application. Detailed Implementation

[0029] This application provides a method for predicting and controlling the warpage value of chemically strengthened glass, which solves the technical problem of the lack of a method for predicting the warpage value of chemically strengthened glass in the prior art.

[0030] The technical solutions of this application will now be clearly and completely described with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of this application. Based on the embodiments of this application, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this application.

[0031] Example 1

[0032] In view of the current lack of methods for predicting the warpage value of chemically strengthened glass, Example 1 of this application provides a method for predicting the warpage value of chemically strengthened glass. The prediction method includes first stirring and mixing film-forming components such as tetraethyl orthosilicate and aluminum isopropoxide, organic solvent, water and catalyst to obtain a coating solution, then measuring the particles in the coating solution to obtain the average particle size, and then predicting the warpage value of chemically strengthened glass based on the linear relationship between the average particle size and the warpage value of chemically strengthened glass. The prediction method provided in this application is based on the discovery that the particle size in the temporary film coated on the glass air surface has a direct linear relationship with the warpage value of chemically strengthened glass, thereby predicting the warpage value of chemically strengthened glass based on the average particle size. The prediction method has a high prediction accuracy and overcomes the current lack of methods for predicting the warpage value of chemically strengthened glass.

[0033] As a preferred embodiment, this application provides a specific fitting formula for the linear relationship between the average particle size and the warpage value of chemically strengthened glass. The fitting formula is R = -0.0897 + 0.09960D, where R is the predicted warpage value and D is the average particle size of the silicon particles. It should be noted that after detecting the average particle size based on the fitting formula provided in this application, the warpage value of the chemically strengthened glass can be obtained by substituting it into the formula.

[0034] Preferably, in order to avoid uneven stirring affecting the distribution of particles in the coating solution and reducing the accuracy of particle size detection during the process of obtaining the positive coating solution, this application selects room temperature for stirring and mixing for 1.5 hours.

[0035] Preferably, in order to improve the accuracy of particle measurement and avoid the influence of the operator on the particle size measurement results, this application selects a particle size analyzer to measure the average particle size of the particles in the coating solution; alternatively, the average particle size of the particles in the coating solution can be directly measured by alkaline titration, which reduces the cost of purchasing a particle size analyzer.

[0036] Preferably, the method for predicting the warpage value of chemically strengthened glass provided in this application is applicable to tetraethyl orthosilicate coating solutions prepared with any one of the organic solvents selected from methanol, ethanol, n-propanol, n-butanol, and isopropanol, and is also applicable to coating solutions prepared with any two organic solvents, such as ethanol and isopropanol.

[0037] In summary, this application utilizes the mechanism that there is a direct linear relationship between the average particle size of the particles in the coating solution for air-coating float glass and the warpage value of chemically strengthened glass. That is, by using the average particle size of the particles in the coating solution to adjust the ion exchange channels and ion exchange rate during chemical strengthening, the warpage value of chemically strengthened glass can be predicted. At the same time, by utilizing the linear relationship between the average particle size and the warpage value of chemically strengthened glass, the warpage value of chemically strengthened glass can be controlled by configuring coating solutions with different particle sizes.

[0038] Example 2

[0039] Example 2 of this application is an example of verifying the accuracy of the prediction method for the warpage value of chemically strengthened glass; it includes the steps of establishing a prediction formula for the warpage value of chemically strengthened glass, the steps of using the prediction formula for the warpage value of chemically strengthened glass to make predictions, and the steps of verifying the accuracy of the prediction method for the warpage value of chemically strengthened glass.

[0040] The steps for establishing the prediction formula for the warpage value of chemically strengthened glass include: firstly, performing linear regression fitting based on the average particle size of silicon particles in multiple actual coating solutions and the corresponding warpage value of chemically strengthened glass to obtain a fitting curve formula. This fitting curve formula is the warpage value prediction formula R = -0.0897 + 0.09960D, where R is the predicted warpage value and D is the average particle size of silicon particles. The average particle size of silicon particles in multiple coating solutions and the corresponding warpage value of chemically strengthened glass are shown in Table 1, and the linear regression fitting diagram is shown in... Figure 1 As shown.

[0041]

[0042]

[0043] Table 1

[0044] The steps for predicting the warpage value of chemically strengthened glass using the formula are as follows: As shown in Table 2, 28.7 ml of tetraethyl orthosilicate, 47.8 ml of alcohol, 23 ml of water, and 0.5 ml of hydrochloric acid are first stirred and mixed in a volume ratio. After 1.5 h of stirring and mixing, the tetraethyl orthosilicate coating solution is obtained. Then, the average particle size of silicon particles in the tetraethyl orthosilicate coating solution is measured to obtain the average particle size of silicon particles. The average particle size of silicon particles is then substituted into the warpage value prediction formula R = -0.0897 + 0.09960D, where R is the predicted warpage value and D is the average particle size of silicon particles. The average particle size of silicon particles in the tetraethyl orthosilicate coating solution and the predicted warpage value of chemically strengthened glass are shown in Table 2.

[0045] organic solvents Average particle size of silicon microparticles (nm) Predicted warpage value (mm) for chemically strengthened glass methanol 1.2 0.02982 ethanol 1.7 0.07962 n-Propanol 2.9 0.19914 n-Butanol 3.2 0.22902

[0046] Table 2

[0047] The steps to verify the accuracy of the prediction method for warpage values ​​of chemically strengthened glass include: as shown in Table 3.

[0048] organic solvents Average particle size of silicon microparticles (nm) Warpage value of chemically strengthened glass (mm) methanol 1.2 0.0300 ethanol 1.7 0.0801 n-Propanol 2.9 0.2003 n-Butanol 3.2 0.2303

[0049] Table 3

[0050] Comparing the data in Tables 2 and 3, it can be seen that the predicted warpage value of chemically strengthened glass provided in this application differs from the actual warpage value by approximately 0.62%. This indicates that the prediction method provided in this application has high accuracy and can be used as a method for predicting the warpage value of chemically strengthened glass in the process of preparing low-warpage chemically strengthened glass by coating the glass air surface with a coating solution.

[0051] Example 3

[0052] This embodiment provides an example of controlling the warpage value of chemically strengthened glass by controlling the average particle size of silicon microparticles in the coating solution; it includes: firstly, mixing 28.7 ml of tetraethyl orthosilicate, 47.8 ml of alcohol, 23 ml of water, and 0.5 ml of hydrochloric acid in a volume ratio, stirring for 1.5 hours to obtain a tetraethyl orthosilicate coating solution; then, coating the tetraethyl orthosilicate coating solution onto the air surface of float glass using a roller coating method, and then placing it in a potassium nitrate molten salt bath for chemical strengthening to obtain chemically strengthened glass. The chemical strengthening temperature is 410°C, and the time is 4 hours; then, the warpage value of the chemically strengthened glass is measured; wherein, the 47.8 ml of alcohol is composed of ethanol and isopropanol in volume ratios of 1:0, 1:0:02, 1:0.04, 1:0.06, and 1:0.08, and the average particle size of silicon microparticles in the tetraethyl orthosilicate coating solution and the warpage value of the chemically strengthened glass are as follows. Figure 2-3 As shown.

[0053] from Figure 3 It can be seen that the tetraethyl orthosilicate coating solutions prepared by the two organic solvents provided in Example 3 of this application are also applicable to the coating solutions for air-surface coating of float glass. The particle size of silicon particles has a direct linear relationship with the warpage value of chemically strengthened glass, which demonstrates the universality of the prediction and control methods provided in the embodiments of this application.

[0054] At the same time, from Figure 2 As can be seen, the tetraethyl orthosilicate coating solution prepared by the two organic solvents provided in Example 3 of this application can control the average particle size of silicon microparticles in the tetraethyl orthosilicate coating solution by controlling the volume ratio of ethanol and isopropanol, thereby controlling the warpage value of chemically strengthened glass.

[0055] The above embodiments are only used to illustrate the technical solutions of this application, and are not intended to limit them. Although this application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of this application.

Claims

1. A method of predicting the warpage value of a chemically strengthened glass, characterized by, The method comprises the steps of: S1, mixing the film-forming component, the organic solvent, water and the catalyst to obtain a coating solution; S2, measuring the microparticles in the coating solution to obtain the average particle size of the microparticles; S3, predicting the chemical strengthening glass warpage value according to the linear relationship between the average particle size of the microparticles and the chemical strengthening glass warpage value; In S1, the film-forming component comprises at least one of tetraethyl orthosilicate and aluminum isopropyl alcohol; In S3, the linear relationship between the average particle size of the microparticles and the chemical strengthening glass warpage value is R=-0.0897+0.09960D, wherein R is the predicted warpage value and D is the average particle size of the microparticles.

2. The method of claim 1, wherein the chemical strengthening glass has a thickness of 0.5 mm or less. In S1, the temperature of the mixing is room temperature and the mixing time is 1-2 hours.

3. The method of claim 1, wherein the chemical strengthening glass has a thickness of 0.5 mm or less. In S2, the measurement method of the microparticles in the coating solution comprises an alkali titration method or a particle size instrument measurement method.

4. The method of claim 1, wherein the chemical strengthening glass has a thickness of 0.5 mm or less. The organic solvent is selected from at least one of methanol, ethanol, n-propanol, n-butanol and isopropyl alcohol.

5. The method of claim 1, wherein the chemical strengthening glass has a thickness of 0.5 mm or less. The catalyst is selected from at least one of hydrochloric acid, nitric acid and acetic acid.

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