CN113735463A - Method for producing chemically strengthened glass and method for managing stress characteristics of chemically strengthened glass - Google Patents
Method for producing chemically strengthened glass and method for managing stress characteristics of chemically strengthened glass Download PDFInfo
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- CN113735463A CN113735463A CN202110570623.2A CN202110570623A CN113735463A CN 113735463 A CN113735463 A CN 113735463A CN 202110570623 A CN202110570623 A CN 202110570623A CN 113735463 A CN113735463 A CN 113735463A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C21/00—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface
- C03C21/001—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions
- C03C21/002—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions to perform ion-exchange between alkali ions
Abstract
The present invention relates to a method for producing a chemically strengthened glass including the following (1) to (3). (1) A1 st glass and a 2 nd glass are immersed in the same molten salt composition and chemically strengthened simultaneously to obtain a 1 st chemically strengthened glass in which the 1 st glass is chemically strengthened and a 2 nd chemically strengthened glass in which the 2 nd glass is chemically strengthened, wherein the 2 nd glass is a glass in which at least one of a K-Na substitution rate and a Na-Li substitution rate in ion exchange is higher than that of the 1 st glass. (2) The stress characteristics of the 2 nd chemically strengthened glass were measured. (3) It was confirmed whether or not the stress characteristics of the 2 nd chemically strengthened glass are within the designed range.
Description
Technical Field
The present invention relates to a method for producing chemically strengthened glass and a method for managing stress characteristics of chemically strengthened glass.
Background
Chemically strengthened glass is used for cover glass of portable terminals and the like. Chemically strengthened glass is produced by bringing glass into contact with a molten salt such as sodium nitrate, thereby causing ion exchange between alkali metal ions contained in the glass and alkali metal ions having a larger ion radius contained in the molten salt, and forming a compressive stress layer in a surface portion of the glass. The strength of chemically strengthened glass is highly dependent on the stress characteristics expressed in terms of compressive stress values as a function of depth from the surface of the glass. Therefore, in the production of chemically strengthened glass, it is necessary to appropriately control the stress characteristics of chemically strengthened glass.
As a method for measuring the stress characteristics of a chemically strengthened glass without breaking, for example, patent document 1 discloses a method for measuring the surface stress of a strengthened glass (hereinafter, abbreviated as FSM). Patent document 2 discloses a method for measuring stress characteristics based on a change in the polarization phase of laser light (hereinafter also referred to simply as SLP).
Documents of the prior art
Patent document
Patent document 1: international publication No. 2017/115811
Patent document 2: international publication No. 2018/056121
Disclosure of Invention
FSM and SLP sometimes have low measurement accuracy of stress characteristics of chemically strengthened glass and are not easy to control quality. For example, FSM measures the stress characteristics based on the change in refractive index due to the change in glass composition caused by ion exchange, and therefore cannot be measured with high accuracy if the depth of the compressive stress layer is shallow or if the glass is not susceptible to a change in refractive index increase even after ion exchange. Further, since SLP measures stress characteristics based on a change in the polarization phase of laser light, it cannot measure the stress characteristics with high accuracy when the depth of the compressive stress layer is shallow. Further, in the production of chemically strengthened glass on an industrial scale, there is a problem that it is difficult to directly manage production conditions.
In view of the above circumstances, an object of the present invention is to provide a method for producing a chemically strengthened glass, which can suitably control the stress characteristics of the chemically strengthened glass.
The present inventors have found that the above problems can be solved by immersing a 1 st glass and a 2 nd glass, which is a glass having a faster K — Na substitution rate and/or Na — Li substitution rate in ion exchange than the 1 st glass, in the same molten salt composition and chemically strengthening the glass, and confirming the stress characteristics of the chemically strengthened glass in which the 2 nd glass is chemically strengthened, and have completed the present invention.
The present invention relates to a method for producing chemically strengthened glass, including the following (1) to (3).
(1) A1 st glass and a 2 nd glass are immersed in the same molten salt composition and chemically strengthened simultaneously to obtain a 1 st chemically strengthened glass in which the 1 st glass is chemically strengthened and a 2 nd chemically strengthened glass in which the 2 nd glass is chemically strengthened, wherein the 2 nd glass is a glass in which at least one of a K-Na substitution rate and a Na-Li substitution rate in ion exchange is higher than that of the 1 st glass.
(2) The stress characteristics of the 2 nd chemically strengthened glass were measured.
(3) It was confirmed whether or not the stress characteristics of the 2 nd chemically strengthened glass are within the designed range.
The present invention relates to a method for managing stress characteristics of chemically strengthened glass, which comprises the following (I) to (III).
(I) A1 st glass and a 2 nd glass are immersed in the same molten salt composition and chemically strengthened simultaneously to obtain a 1 st chemically strengthened glass in which the 1 st glass is chemically strengthened and a 2 nd chemically strengthened glass in which the 2 nd glass is chemically strengthened, wherein the 2 nd glass is a glass in which at least one of a K-Na substitution rate and a Na-Li substitution rate in ion exchange is higher than that of the 1 st glass.
(II) measuring the stress characteristics of the 2 nd chemically strengthened glass.
(III) confirming that the stress characteristics of the 2 nd chemically strengthened glass are within the designed range.
According to the method for producing a chemically strengthened glass of the present invention, the stress characteristics of a chemically strengthened glass, the stress characteristics of which are not easily measured, can be appropriately managed.
Drawings
Fig. 1 is a flowchart showing an embodiment of the present invention.
Fig. 2 is a flowchart showing an embodiment of the present invention.
Fig. 3 is a flowchart showing an embodiment of the present invention.
Fig. 4 is a flowchart showing an embodiment of the present invention.
Detailed Description
1. Method for producing chemically strengthened glass
The method for producing a chemically strengthened glass of the present invention (hereinafter, also simply referred to as the method of the present invention) includes the following steps (1) to (3).
(1) A1 st glass and a 2 nd glass are immersed in the same molten salt composition and chemically strengthened simultaneously to obtain a 1 st chemically strengthened glass in which the 1 st glass is chemically strengthened and a 2 nd chemically strengthened glass in which the 2 nd glass is chemically strengthened, wherein the 2 nd glass is a glass in which at least one of a K-Na substitution rate and a Na-Li substitution rate in ion exchange is higher than that of the 1 st glass.
(2) The stress characteristics of the 2 nd chemically strengthened glass were measured.
(3) It was confirmed whether or not the stress characteristics of the 2 nd chemically strengthened glass are within the designed range.
Fig. 1 is a flowchart showing the present embodiment. Hereinafter, the respective steps will be described with reference to embodiment 1 as the mode in which glass 2 is a glass having a higher K — Na substitution rate than glass 1 in ion exchange, and embodiment 2 as the mode in which glass 2 is a glass having a higher Na — Li substitution rate than glass 1.
[ embodiment 1]
< step (1): chemical strengthening Process
The step (1) is a step of obtaining a chemically strengthened glass by immersing a 1 st glass and a 2 nd glass in the same molten salt composition and chemically strengthening the same, wherein the 2 nd glass has a higher K-Na substitution rate and/or Na-Li substitution rate in ion exchange than the 1 st glass. Under the conditions of chemical strengthening in step (1) (hereinafter, also abbreviated as chemical strengthening conditions), glass obtained by chemically strengthening the 1 st glass is referred to as 1 st chemically strengthened glass, and glass obtained by chemically strengthening the 2 nd glass is referred to as 2 nd chemically strengthened glass.
The glass to be the base materials of the 1 st glass and the 2 nd glass may be ion-exchangeable glass, and may be either amorphous glass or crystallized glass. In a method for producing glass to be base materials of the 1 st glass and the 2 nd glass, for example, glass raw materials are appropriately mixed so as to obtain glass having a predetermined composition, and heated and melted in a glass melting furnace. Thereafter, the glass may be homogenized by bubbling, stirring, addition of a refining agent, or the like, formed into a glass plate having a predetermined thickness, and slowly cooled to obtain the glass plate. Alternatively, the sheet-like member may be formed into a plate shape by a method of forming the sheet into a block shape, slowly cooling the block, and then cutting the block.
Examples of the method of forming into a sheet include a float method, a pressure method, a melting method, and a downdraw method. Particularly, in the case of producing a large glass plate, the float process is preferable. Further, a continuous molding method other than the float method, such as a melting method and a downdraw method, is also preferable.
The glass ribbon obtained by molding is ground and polished as necessary to form a glass plate. In the case of cutting a glass plate into a predetermined shape and size, chamfering a glass plate, or the like, it is preferable that a compressive stress layer is formed on the end face by the chemical strengthening treatment if the cutting and chamfering of the glass plate are performed before the chemical strengthening treatment described later.
After the formed glass plate is subjected to chemical strengthening treatment, chemically strengthened glass is obtained by cleaning and drying. The chemical strengthening treatment is as follows: the glass is brought into contact with a metal salt (typically, lithium ion or sodium ion) by a method of immersing the glass in a molten solution (molten salt composition) containing a metal salt (for example, potassium nitrate) of metal ion (typically, sodium ion or potassium ion) having a large ionic radius, thereby replacing the metal ion (typically, sodium ion or potassium ion with respect to lithium ion) having a small ionic radius in the glass with the metal ion (typically, potassium ion with respect to sodium ion) having a large ionic radius in the metal salt.
From the viewpoint that the chemical strengthening treatment is fast and a large compressive stress can be formed by ion exchange, it is preferable to adopt a method of "Na — Li substitution" in which lithium ions in the glass are exchanged with sodium ions in the molten salt or a method of "K — Na substitution" in which sodium ions in the glass are exchanged with potassium ions in the molten salt.
The conditions for the chemical strengthening treatment are not particularly limited, and may be selected appropriately in consideration of the characteristics and composition of the glass, the type of the molten salt composition, and the chemical strengthening properties such as the surface Compressive Stress (CS) and the depth of the compressive stress layer (DOL) desired for the finally obtained chemically strengthened glass. In the present invention, the chemical strengthening treatment may be performed only once, or may be performed a plurality of times under different conditions of 2 or more (multi-step strengthening).
The conditions for the chemical strengthening treatment are not particularly limited, but the chemical strengthening treatment can be performed by immersing the glass sheet in a molten salt composition such as potassium nitrate heated to 360 to 600 ℃ for 0.1 to 500 hours. The heating temperature of the molten salt composition is preferably 375 to 500 ℃, and the time for immersing the glass plate in the molten salt composition is preferably 0.3 to 200 hours.
Examples of the molten salt used for the chemical strengthening treatment include nitrates, sulfates, carbonates, chlorides, and the like. Among them, examples of the nitrate include lithium nitrate, sodium nitrate, potassium nitrate, cesium nitrate, silver nitrate, and the like. Examples of the sulfate include lithium sulfate, sodium sulfate, potassium sulfate, cesium sulfate, and silver sulfate. Examples of the carbonate include lithium carbonate, sodium carbonate, and potassium carbonate. Examples of the chloride include lithium chloride, sodium chloride, potassium chloride, cesium chloride, and silver chloride. These molten salts may be used alone or in combination of two or more.
In the manufacturing method of the present invention, the 1 st glass is a glass to be a management target of stress characteristics, and the 2 nd glass is a monitoring sample. That is, in the manufacturing method of the present invention, the 2 nd glass is used as a monitoring sample, chemical strengthening is performed simultaneously with the 1 st glass, and the stress characteristics of the 1 st chemically strengthened glass are managed using the stress characteristics of the obtained 2 nd chemically strengthened glass as an index. The 2 nd glass is preferably a glass capable of measuring the stress characteristics with high accuracy even when chemically strengthened under the same conditions as those of the 1 st glass.
The 2 nd glass is a glass in which at least one of the K-Na substitution rate and the Na-Li substitution rate in ion exchange is higher than that of the 1 st glass. Here, the K — Na substitution rate refers to an ion exchange rate of sodium ions in the glass and potassium ions in the molten salt composition. Further, the Na — Li substitution rate means an ion exchange rate of lithium ions in the glass and sodium ions in the molten salt composition. The ion exchange rate (hereinafter, also referred to as a substitution rate) of the glass can be measured according to the chemical strengthening conditions and the ion depth after the chemical strengthening.
Specifically, the diffusion can be calculated by the following steps 1 to 3 based on the Fick's rule (the following equation).
In the above formula, D represents a diffusion coefficient (unit:. times.10)－12m2Per minute), C represents an ion concentration (unit: mol%), x represents the depth (. mu.m) from the glass surface.
[ Step 1] A chemically strengthened glass which has been strengthened at a temperature T (in:. degree.C.) and for a time T (in minutes) is prepared.
[ Step 2] the ion diffusion curve in the depth direction was measured for the chemically strengthened glass prepared in Step 1.
Specifically, the composition ratio is evaluated for the cross-section of the chemically strengthened glass by, for example, EPMA, SIMS, or the like. The ion depth curve in the depth direction of the K ion is measured in the case of K-Na substitution, or the ion depth curve in the depth direction of the Na ion is measured in the case of Na-Li substitution.
[ Step3 ] the measured ion depth curve was fitted to the following equation. In the following formula, c (x) is an ion concentration at a depth x (μm) from the glass surface.
D in the formula is a diffusion coefficient (multiplied by 10) of temperature T (unit:. degree. C.)－12m2Per minute), the rate of substitution was determined.
The stress characteristics of the 1 st chemically strengthened glass can be managed by using the stress characteristics of the 2 nd chemically strengthened glass as an index, since the 2 nd glass has a higher K-Na substitution rate or Na-Li substitution rate in ion exchange than the 1 st glass.
Embodiment 1 of the production method of the present invention is a mode in which ion exchange (K — Na substitution) of sodium ions in the glass and potassium ions in the molten salt composition is performed in the chemical strengthening in step (1). In the first embodiment, the glass No. 2 preferably has a higher K-Na substitution rate than the glass No. 1. In embodiment 1, the K-Na substitution rate of the 2 nd glass is preferably 1.1 times or more, more preferably 1.5 times or more, further preferably 2.0 times or more, and particularly preferably 4.0 times or more the K-Na substitution rate of the 1 st glass.
By setting the K-Na substitution rate of the 2 nd glass to 1.1 times or more the K-Na substitution rate of the 1 st glass, the stress characteristics of the 2 nd chemically strengthened glass can be used as a target index, and the stress characteristics of the 1 st chemically strengthened glass can be further appropriately controlled. The K-Na substitution rate of the 2 nd glass is generally 10000 times or less as high as that of the 1 st glass.
The K — Na substitution rate can be easily evaluated by a ratio of the depth of compressive stress layer DOL by strengthening the first glass and the second glass under the same strengthening conditions. Note that DOL is substantially proportional to the square root of the diffusion rate, and thus the square of the DOL ratio corresponds to the rate of substitution. Similarly, in the FSM, the number of interference fringes is substantially proportional to DOL, and thus can be easily evaluated by the DOL ratio.
In embodiment 1 of the production method of the present invention, when the diffusion depth of potassium ions is preferably 10 μm or less as the 1 st chemically strengthened glass, for example, it is difficult to measure the stress characteristics with high accuracy, and thus management of the stress characteristics of the 1 st chemically strengthened glass using the stress characteristics of the 2 nd chemically strengthened glass as an index is useful. From the viewpoint of reducing the tensile stress in balance with the compressive stress and suppressing the progress of the flaw due to the tensile stress, the diffusion layer depth of potassium ions in the 1 st chemically strengthened glass is more preferably 8 μm or less, still more preferably 6 μm or less, particularly preferably 4 μm or less, and still more preferably 2 μm or less. And typically preferably 1 μm or more.
The depth of the potassium ion diffusion layer in the chemically strengthened glass can be measured by EPMA or SIMS. Here, the ion diffusion depth is a depth at which a value larger than a value obtained by adding 5% of a difference between the maximum value and the minimum value to the minimum value is obtained when the difference between the maximum value and the minimum value is 100% in an ion distribution from the glass surface toward the glass center. When the corresponding value is 2 or more, the diffusion layer depth is set to be the depth from the glass surface close to the center of the sheet thickness.
In embodiment 1 of the production method of the present invention, the 2 nd glass is preferably a glass in which the refractive index is increased by replacing sodium ions in the 2 nd glass with potassium ions. As described above, it is difficult to accurately measure the stress characteristics of FSM in glass in which the refractive index does not change even when ion exchange is performed. In one embodiment of the production method of the present invention, by making the 2 nd glass a glass whose refractive index is increased by ion exchange, even if the 1 st glass is a glass whose refractive index is not changed by ion exchange, the stress characteristics of the 2 nd chemically strengthened glass can be appropriately controlled by using the stress characteristics of the 1 st chemically strengthened glass as an index.
In embodiment 1 of the production method of the present invention, it is preferable that the composition of the 2 nd glass contains Na in an oxide basis in an amount larger than that of the 1 st glass2O is preferably 1 mol% or more, more preferably 2 mol% or more, and further preferably 4 mol% or more. By containing Na in a larger amount than the composition of the No. 1 glass2O is preferably 1 mol% or more, so that the ion exchange rate can be increased, thereby using the stress characteristics of the 2 nd chemically strengthened glass as an indexThe stress characteristics of the 1 st chemically strengthened glass can be appropriately controlled.
From the viewpoint of improving the measurement accuracy of the stress characteristics, the thickness of the 2 nd glass is preferably 0.2 to 2.5mm, more preferably 0.3 to 2.0mm, and still more preferably 0.4 to 1.0 mm. In addition, the thickness of the 1 st glass is preferably 0.3 to 2.5mm, more preferably 0.4 to 2.0mm, and still more preferably 0.5 to 1.0mm, from the viewpoint of improving the measurement accuracy of the stress characteristics.
In one embodiment of the production method of the present invention, it is preferable to use 2 or more kinds of glasses having different compositions as the 2 nd glass. By using 2 or more kinds of glasses having different compositions as the 2 nd glass, the accuracy of management of the stress characteristics of the 1 st chemically strengthened glass can be improved. Also, by using 2 or more kinds of glasses having different compositions as the 2 nd glass, 2 or more kinds of conditions of chemical strengthening can be managed.
In one embodiment of the production method of the present invention, the 1 st chemically strengthened glass preferably has a visible light transmittance of 80% or more, more preferably 84% or more, and still more preferably 86% or more, in terms of a thickness of 0.7 mm. The 1 st chemically strengthened glass typically has a visible light transmittance of 88% or more in terms of a thickness of 0.7 mm. The 2 nd chemically strengthened glass preferably has a visible light transmittance of 80% or more, more preferably 84% or more, and still more preferably 86% or more, in terms of a thickness of 0.7 mm. The 2 nd chemically strengthened glass typically has a visible light transmittance of 88% or more in terms of a thickness of 0.7 mm.
In some cases, depending on design properties (for example, colored AG glass), the visible light transmittance is preferably 80% or less. In this case, as the 1 st chemically strengthened glass, for example, since it is difficult to measure the stress characteristics by a non-destructive test such as SLP when the visible light transmittance in terms of the sheet thickness of 0.7mm is preferably 60% or less, it is useful to manage the stress characteristics of the 1 st chemically strengthened glass using the stress characteristics of the 2 nd chemically strengthened glass as an index. From the above viewpoint, the visible light transmittance is more preferably 40% or less, and still more preferably 20% or less. And typically 0.01% or more.
In one embodiment of the production method of the present invention, when the number of interference fringes observed as the 1 st chemically strengthened glass by a surface stress meter based on the principle of observation of the optical waveguide effect is preferably 2 or less, it is difficult to measure the stress characteristics by a non-destructive test such as FSM, and therefore management of the stress characteristics of the 1 st chemically strengthened glass using the stress characteristics of the 2 nd chemically strengthened glass as an index is useful. From the above viewpoint, the 1 st chemically strengthened glass more preferably has 1 or less of the interference fringes.
In one embodiment of the production method of the present invention, when the refractive index of the 1 st chemically strengthened glass is preferably out of the range of 1.40 to 1.62, for example, it is difficult to measure the stress characteristics by a non-destructive test such as FSM, and therefore, management of the stress characteristics of the 1 st chemically strengthened glass using the stress characteristics of the 2 nd chemically strengthened glass as an index is useful. From the above viewpoint, the refractive index of the 1 st chemically strengthened glass is more preferably out of the range of 1.4 to 1.7.
< step (2): process for measuring stress characteristics
The step (2) is a step of measuring the stress characteristics of the 2 nd chemically strengthened glass obtained in the step (1). Examples of the stress characteristics include surface Compressive Stress (CS), depth of layer of compressive stress (DOL), tensile stress at the center of the sheet thickness (CT), sheet thickness, bending strength, crack initiation load (クラック · イニシエーション · ロード), depth of diffusion layer of potassium ions, depth of diffusion layer of sodium ions, and the like. From the viewpoint of improving the accuracy of the management of the stress characteristics of the 1 st chemically strengthened glass, among these, at least one selected from the group consisting of CS, DOL and CT is preferable, CS and DOL are more preferable, CS, DOL and CT are further preferable, and a curve showing the diffusion layer depth of potassium ions and the diffusion layer depth of sodium ions is particularly preferable.
The method for measuring the stress characteristics may be appropriately selected from conventionally known methods, and is not particularly limited, and for example, the stress characteristics are measured by a birefringence meter using a sample obtained by thinning a cross section of a glass plate. The birefringence meter is a device for measuring the retardation due to stress using a polarizing microscope, a liquid crystal display compensator, or the like, and includes, for example, a birefringence imaging system Abrio-IM manufactured by CRi corporation.
The value of the compressive stress in the vicinity of the surface of the glass sheet may be measured, for example, by using an optical waveguide surface stress meter (FSM-6000 manufactured by TOYOBO Co., Ltd.). According to the optical waveguide surface stress meter, the stress value can be measured without performing processing such as thinning of a glass sample.
The internal stress value of the glass can be measured, for example, by a scattered light photoelastic stress meter (e.g., SLP-2000 available from TOYOBO Co., Ltd.). The scattered light photoelastic stress meter can measure the stress value without performing processing such as slicing of a glass sample, regardless of the refractive index distribution inside the glass.
< step (3): stress characteristic evaluation Process
The step (3) is a step of confirming whether or not the stress characteristics of the 2 nd chemically strengthened glass measured in the step (2) are within the designed range, and the stress characteristics of the 1 st chemically strengthened glass are managed by setting the stress characteristics of the 2 nd chemically strengthened glass within the management range. In the step (3), if the stress characteristic of the 2 nd chemically strengthened glass is within the designed range, it can be judged that the stress characteristic of the 1 st chemically strengthened glass is within the designed range.
The "designed range" of the stress characteristics of the 1 st chemically strengthened glass is set from the viewpoint of quality design. For example, the stress characteristics of the 1 st chemically strengthened glass are difficult to measure in FSM and SLP, but stress measurement is possible in a failure test (Abrio, etc.). By measuring the stress characteristics in advance by a fracture test, the allowable range of the stress characteristics of the 1 st chemically strengthened glass satisfying the required characteristics can be determined. In order to set the stress characteristics of the 1 st chemically strengthened glass within the designed range, the 1 st glass is chemically strengthened under conditions within the designed range. The conditions for chemical strengthening include, for example, temperature, time, and salt concentration contained in the molten salt composition.
Whether or not the chemical strengthening condition of the 1 st glass is the "condition within the designed range" can be determined by whether or not the stress characteristic of the 2 nd chemically strengthened glass is included in the range of the stress characteristic when the 2 nd glass is chemically strengthened under the condition within the designed range. The range of the stress characteristics when the 2 nd glass is chemically strengthened under the condition that the stress characteristics of the 2 nd chemically strengthened glass are included in the designed range is referred to as "the stress characteristics of the 2 nd chemically strengthened glass are within the designed range". The stress characteristics and the conditions of chemical strengthening of the No. 2 chemically strengthened glass are known.
One example of the step (3) is a method of confirming whether or not the stress characteristic of the 2 nd chemically strengthened glass measured in the step (2) is within a designed range with respect to the value of the stress characteristic (for example, CS, DOL) of the 2 nd chemically strengthened glass. If the value of the stress characteristic of the 2 nd chemically strengthened glass is within the designed range, it can be judged that the stress characteristic of the 1 st chemically strengthened glass is within the designed range. Further, if the value of the stress characteristic of the 2 nd chemically strengthened glass is within the designed range, it can be judged that the condition for chemically strengthening the 1 st glass is within the designed range.
Specifically, the range of the stress characteristic of the 2 nd chemically strengthened glass, which is used for determining that the condition for chemically strengthening the 1 st glass is within the designed range, is controlled such that CS is within a range of preferably ± 100MPa, more preferably ± 50MPa, and still more preferably ± 30MPa, as the design value. For example, DOL is controlled in a range of preferably. + -.10 μm, more preferably. + -.5 μm, and still more preferably. + -.3 μm from the design value.
< step (4): process for determining conditions for chemical strengthening
The production method of the present invention may further include step (4) after steps (1) to (3). The step (4) is a step of determining the chemical strengthening conditions of the step (1) based on the stress characteristics of the 2 nd chemically strengthened glass, and the chemical strengthening conditions are calculated and managed based on the stress characteristics of the 2 nd chemically strengthened glass. Fig. 2 shows a flowchart for explaining an embodiment including steps (1) to (4).
In one mode of step (4), for example, based on the measurement result of the stress characteristic of the 2 nd chemically strengthened glass in step (2), the chemical strengthening condition in step (1) is identified and compared with a preset "designed range of the chemical strengthening condition for the 1 st glass", and it is determined whether or not the chemical strengthening condition in step (1) is within the designed range.
< step (1'): process for obtaining relationship between stress characteristics and conditions for chemical strengthening
In the case where the relationship between the stress characteristics of the 2 nd glass and the chemical strengthening conditions is not known, the production method of the present invention may include the step (1') before the step (1). The step (1') is a step of determining the relationship between the chemical strengthening condition and the stress characteristic of the composition of the 2 nd glass. Specifically, the procedure is as follows. The step (1 ') is a step of chemically strengthening a 3 rd glass having the same composition as the 2 nd glass to obtain a 3 rd chemically strengthened glass, measuring the stress characteristics of the 3 rd chemically strengthened glass, and obtaining the correlation between the stress characteristics of the 3 rd chemically strengthened glass and the conditions of the chemical strengthening in the step (1'). Preferably, the design range of step (3) is determined by using the correlation between the stress characteristics of the 3 rd chemically strengthened glass and the conditions of the chemical strengthening in step (1').
Fig. 3 shows a flowchart for explaining an embodiment including step (1') before step (1) and step (4) after steps (1) to (3).
Examples of the method for determining the stress characteristics and the conditions for chemical strengthening include the methods described in Maya Hatano et al, Key Engineering Materials,1662-9795, Vol.702, and p.32-36.
The 2 nd glass and the 3 rd glass are glasses having the same composition. From the viewpoint of improving the prediction accuracy of the relationship between the stress characteristics in the step (1') and the conditions for chemical strengthening, it is preferable that the thicknesses of the 2 nd glass and the 3 rd glass are the same.
As an embodiment of the step (1 '), for example, the following step (1 ' a) or (1 ' b) can be given. (1' a) the 3 rd glass is chemically strengthened under a plurality of different conditions (e.g., temperature, time, salt concentration), and the correlation with the temperature, time, and salt concentration is determined for each stress characteristic (e.g., CS, DOL). Using the correlation obtained from the experimental points, the stress characteristic assumed under the reinforcement condition is (CS)sim、DOLsim). (1' b) stress characteristics (for example, CS and DOL) of a chemically strengthened glass obtained by chemically strengthening a 3 rd glass under a plurality of different conditions (for example, temperature, time, and salt concentration) were calculated by a strengthening simulation (finite element method, etc.), and a simulated value of the obtained stress characteristics was defined as (CS, DOL)sim、DOLsim)。
The step (4) in the embodiment including the step (1') and the steps (1) to (4) includes, for example, the following steps (4-1) to (4-3). A flowchart of this method is shown in fig. 4.
(4-1) candidate conditions are determined for the conditions (for example, temperature, time, and salt concentration) for chemical strengthening in the step (1) based on the correlation determined in the step (1'). The number of candidate conditions may be 2 or more. The candidate condition can be obtained, for example, by using a simulated value of the stress characteristic (for example, CS) obtained in step (1simAnd DOLsim) Measurement of stress characteristics (for example, CS) of chemically strengthened glass 2expAnd DOLexp) A method in which a condition that becomes an approximate value is used as a candidate condition; and a method of investigating the relationship between the chemical strengthening condition and the stress characteristic by a finite element method or the like, and estimating the chemical strengthening condition from the stress characteristic.
(4-2) the stress characteristic of the 2 nd chemically strengthened glass is measured (for example, CS) for each candidate condition obtained in the step (4-1)expAnd DOLexp) And analog values (e.g. CS)simAnd DOLsim) The error (for example, CS error and DOL error) of the stress characteristic value represented by the following formula (i) is obtained.
Stress characteristic value error (measured value of stress characteristic-simulated value of stress characteristic)/measured value of stress characteristic … formula (i)
When the stress characteristics are CS and DOL, for example, the CS error and DOL error are expressed by the following expressions (ii) and (iii), respectively.
Error of CS ═ CSexp－CSsim)/CSexp… formula (ii)
DOL error ═ DOLexp－DOLsim)/DOLexp… formula (iii)
(4-3) for each candidate condition, the sum of squares of errors of each stress characteristic value is obtained, and the condition that the sum of squares of errors is the minimum is determined as the condition for chemical strengthening in the step (1). When the stress characteristic values are CS and DOL, for example, the sum of squares of the errors is expressed by the following formula (iv).
Sum of squares of errors CS error plus square of DOL error … equation (iv)
In the case of using 2 or more types of glasses having different compositions from each other as the 2 nd glass, in the step (4-3), the condition of chemical strengthening in which the square sum of the errors is obtained for the 2 nd chemically strengthened glass having each composition one by one and the sum thereof is minimized is determined as the condition of chemical strengthening in the step (1).
Specifically, for example, when 2 or more kinds of glasses (2 nd glass a and 2 nd glass b) having different compositions from each other are used as the 2 nd glass, the step (4) includes the following steps (4 '-1) to (4' -3).
(4 '-1) based on the correlation obtained in the step (1'), candidates of the conditions (for example, temperature, time, and salt concentration) for chemical strengthening in (1) are obtained.
(4 '-2) the error of the stress characteristic value was determined for each of the 2 nd chemically strengthened glasses a and b under the condition of the candidate selected in (4' -1).
(4' -3) for each of the 2 nd chemically strengthened glasses a and b, the sum of squares of errors in the stress characteristic values was determined, and the sum of squares of errors in the 2 nd chemically strengthened glass a and the sum of squares of errors in the 2 nd chemically strengthened glass b, that is, the sum of squares of errors represented by the following formula (v), was determined. The chemical strengthening condition in which the sum of squares of the errors is minimized is determined as the chemical strengthening condition in step (1).
The sum of squares of errors (sum of squares of errors of the 2 nd chemically strengthened glass a) + (sum of squares of errors of the 2 nd chemically strengthened glass b) … formula (v)
[ 2 nd embodiment ]
Embodiment 2 of the production method of the present invention is a case where ion exchange between lithium ions in glass and sodium ions in a molten salt composition is performed during chemical strengthening. Embodiment 2 is the same as embodiment 1 except for the points described below. In embodiment 2, the Na-Li substitution rate of glass No. 2 is preferably higher than that of glass No. 1.
In embodiment 2 of the production method of the present invention, the Na — Li substitution rate of the 2 nd glass is preferably 1.1 times or more, more preferably 1.5 times or more, further 2.0 times or more, and particularly preferably 4.0 times or more the Na — Li substitution rate of the 1 st glass. By setting the Na-Li substitution rate of the 2 nd glass to 1.1 times or more the Na-Li substitution rate of the 1 st glass, the stress characteristics of the 1 st chemically strengthened glass can be easily appropriately controlled using the stress characteristics of the 2 nd chemically strengthened glass as an index. From the viewpoint of properly managing the stress characteristics of the 1 st chemically strengthened glass, the Na — Li substitution rate of the 2 nd glass is preferably 10000 times or less the Na — Li substitution rate of the 1 st glass.
The first glass and the second glass can be strengthened under the same strengthening conditions, and the ratio of the depth of compressive stress layer DOL can be easily evaluated. Note that DOL is approximately proportional to the square root of the diffusion rate, and thus the square of the DOL ratio corresponds to the magnification of the substitution rate.
In embodiment 2 of the manufacturing method of the present invention, as the 1 st chemically strengthened glass, for example, if the diffusion depth of sodium ions is preferably 50 μm or less, it is difficult to measure the stress characteristics with SLP accurately, and thus management of the stress characteristics of the 1 st chemically strengthened glass using the stress characteristics of the 2 nd chemically strengthened glass as an index is useful. From the above viewpoint, the diffusion depth of sodium ions in the 1 st chemically strengthened glass is more preferably 45 μm or less, still more preferably 40 μm or less, and particularly preferably 35 μm or less. And typically, it is preferably 30 μm or more.
The diffusion layer depth of sodium ions in the chemically strengthened glass can be measured by SIMS.
2. Method for managing stress characteristics of chemically strengthened glass
The method for controlling the stress characteristics of the chemically strengthened glass of the present invention (hereinafter, also abbreviated as the method for controlling the present invention) includes the following steps (I) to (III).
(I) A1 st glass and a 2 nd glass are immersed in the same molten salt composition and chemically strengthened simultaneously to obtain a 1 st chemically strengthened glass in which the 1 st glass is chemically strengthened and a 2 nd chemically strengthened glass in which the 2 nd glass is chemically strengthened, wherein the 2 nd glass is a glass in which at least one of a K-Na substitution rate and a Na-Li substitution rate in ion exchange is higher than that of the 1 st glass.
(II) measuring the stress characteristics of the 2 nd chemically strengthened glass.
(III) confirming that the stress characteristics of the 2 nd chemically strengthened glass are within the designed range.
The steps (I) to (III) are the same as the steps (1) to (3) described in the description of the method for producing chemically strengthened glass. According to the management method of the present invention, even if the 1 st glass is a glass whose stress characteristics are not easily measured by a non-destructive test, the stress characteristics of the 1 st chemically strengthened glass can be estimated by using the stress characteristics of the 2 nd chemically strengthened glass as an index, and the stress characteristics of the chemically strengthened glass can be appropriately managed.
Examples
The following examples of the present invention are specifically described, but the present invention is not limited to these examples. Examples 1 and 2 are examples.
[ measurement method ]
(CS and DOL)
CS was measured using an optical waveguide surface stress meter (FSM-6000, manufactured by Inkurt Co., Ltd.), and DOL was measured using a birefringence stress meter (Abrio, manufactured by Inkurt Co., Ltd.).
(speed of replacement)
The replacement rate is determined at steps 1-3.
[ example 1]
< step (1 ') > A step of obtaining a 3 rd chemically strengthened glass by chemically strengthening a 3 rd glass having the same composition as the 2 nd glass, and determining the relationship between the stress characteristics of the 3 rd chemically strengthened glass and the conditions for chemical strengthening in step (1')/A
(production of glass for chemical strengthening)
Glass raw materials are mixed so as to become glass compositions 2A and 2B described later in < step (1) > and are subjected to dissolution and polishing to produce a glass sheet for chemical strengthening. As the glass raw material, a general glass raw material such as an oxide, a hydroxide, a carbonate, etc. was appropriately selected, and the glass was weighed so as to be 900 g. The mixed glass raw materials are put into a platinum crucible and melted and defoamed at 1700 ℃. The glass was flowed onto a carbon plate to obtain a glass block. The obtained peeled glass was processed and mirror-polished to obtain a glass plate of chemical strengthening glass having a thickness t of 0.7 mm.
(3 rd production of chemically strengthened glass and evaluation of relationship between stress Properties and chemical strengthening conditions)
The obtained glass for chemical strengthening was used as a 3 rd chemically strengthened glass, and the relationship between the stress characteristics and the chemical strengthening conditions was evaluated. The concentration of salt (KNO in the molten salt composition) in the glass for chemical strengthening obtained above was determined from a simulation3Content) of a chemically strengthened glass obtained by chemically strengthening the glass in a range of 95 to 100 mass% on a 0.5 mass% scale, a temperature in a range of 380 to 450 ℃ on a 5 ℃ scale, and a time in a range of 15 to 180 minutes on a 5 minute scalesimAnd DOLsim). In each condition, chemically strengthened glass obtained by chemically strengthening glass for chemical strengthening having the same composition as that of the glass composition 2A is collectively referred to as 3A, and chemically strengthened glass obtained by chemically strengthening glass for chemical strengthening having the same composition as that of the glass composition 2B is collectively referred to as 3B.
< step (1) > Process for obtaining the 1 st chemically strengthened glass and the 2 nd chemically strengthened glass
(production of glass for chemical strengthening)
Thereafter, a glass plate for chemical strengthening having a thickness t of 0.7mm was obtained by mirror polishing in the same manner as in the step (1') so that the glass composition 1, 2A or 2B was represented by a molar percentage based on oxides.
Glass composition 1: containing SiO2、Al2O3And Li2O and containing Na2Composition of O4.8%
Glass composition 2A: containing SiO2 64％、Al2O3 8％、Na2O 13％、K2O4% and MgO 11%.
Glass composition 2B: with SiO2 64％、Al2O3 11％、Na2O 16％、K2O1% and MgO 8%.
A glass plate for chemical strengthening having a thickness of 0.7mm and comprising glass composition 1, 2A or 2B was treated with a solution containing 96.5 mass% of KNO3And 3.5 mass% of NaNO3The molten salt composition of (3) is chemically strengthened at 390 ℃ for 4 hours. The stress characteristics and the substitution rate ratio of the obtained chemically strengthened glass were evaluated, and the results are shown in table 1. The substitution rate ratio is obtained by squaring the DOL ratio.
TABLE 1
| Glass composition | 1 | 2A | 2B |
| CS(MPa) | 976 | 605 | 860 |
| DOL(μm) | 4.1 | 26.2 | 20.1 |
| DOL ratio | 1.0 | 6.4 | 4.9 |
| Ratio of displacement rates | 1.0 | 40.8 | 24.0 |
(production of chemically strengthened glass 1, 2A, 2B)
The glass plates for chemical strengthening were subjected to ion exchange treatment under the conditions shown in table 2A to obtain 1 st chemically strengthened glass (chemically strengthened glass 1) and 2 nd chemically strengthened glass (chemically strengthened glass 2A and 2B). The salt concentration in Table 2A means KNO in the molten salt composition3The balance of NaNO3。
< step (2) > step of measuring stress characteristics of the 2 nd chemically strengthened glass
The chemically strengthened glasses 2A and 2B produced in step (1) were evaluated for CS and DOL. The results are respectively taken as CSexpAnd DOLexpShown in table 2A.
< step (3) > step of confirming whether or not the stress characteristics of the No. 2 chemically strengthened glass are within the designed range
Table 2B shows the design ranges of the stress characteristics of the 2 nd chemically strengthened glass obtained in advance. The results in Table 2A were confirmed to be within the ranges in Table 2B.
< step (4) > step of determining conditions for chemical strengthening
Stress Characteristics (CS) of the chemically strengthened glasses 3A and 3B obtained in the step (1')simAnd DOLsim) The stress characteristic value (CS) of the chemically strengthened glass 2A, 2B measured in the step (2) is compared with the stress characteristic value (CS) of the chemically strengthened glass 2A, 2B measured in the step (2)expAnd DOLexp) The closest condition is set as candidate conditions 1-1 to 1-5. Will be provided withThe results are shown in Table 3.
The stress characteristic values (CS) of the chemically strengthened glasses 3A and 3B are used as the basis of the candidate conditions 1-1 to 1-5 thus obtainedsimAnd DOLsim) And stress characteristic value (CS) of chemically strengthened glasses 2A and 2BexpAnd DOLexp) The Sum of squares of errors (Δ 3A, Δ 3B) is obtained by the above equations (ii) to (iv), and the Sum of squares of errors (Sum) is obtained by the above equation (v).
TABLE 2A
TABLE 2B
[ TABLE 3 ]
As shown in tables 2A and 2B, the results shown in table 2A are within the ranges shown in table 2B. In table 3, the sum of squares of errors Δ 3A and Δ 3B and the sum of squares of errors are the minimum value surrounded by a thick frame. The candidate condition 1-1 for minimizing the sum of squares as shown in Table 3 is the same as the chemical strengthening conditions of the chemically strengthened glasses 2A and 2B shown in Table 2A. It can be seen that by using 2 types of 2 nd glasses, the chemical strengthening conditions for strengthening the 1 st glass can be identified.
[ example 2]
< step (1 ') > A step of obtaining a 3 rd chemically strengthened glass by chemically strengthening a 3 rd glass having the same composition as the 2 nd glass, and determining the relationship between the stress characteristics of the 3 rd chemically strengthened glass and the conditions for the chemical strengthening in step (1')/A
As in example 1, the stress Characteristics (CS) of the chemically strengthened glass 3A and the chemically strengthened glass 3B were determined by simulation as the 3 rd chemically strengthened glasssimAnd DOLsim)。
< step (1) > Process for obtaining the 1 st chemically strengthened glass and the 2 nd chemically strengthened glass
Chemical strengthening was performed on the glass for chemical strengthening in the same manner as in example 1 except that the conditions for chemical strengthening in example 1 were changed to the conditions shown in table 4A, to produce chemically strengthened glass 1 (chemically strengthened glass 1) and chemically strengthened glasses 2A and 2B. The salt concentration in Table 4A means KNO in the molten salt composition3The balance of NaNO3。
< step (2) > step of measuring stress characteristics of the 2 nd chemically strengthened glass
The chemically strengthened glasses 2A and 2B produced in step (1) were evaluated for CS and DOL in the same manner as in example 1. The results are respectively taken as CSexpAnd DOLexpShown in table 4A.
< step (3) > step of confirming whether or not the stress characteristics of the No. 2 chemically strengthened glass are within the designed range
Table 4B shows the design ranges of the stress characteristics of the 2 nd chemically strengthened glass obtained in advance. The results in Table 4A were confirmed to be within the ranges in Table 4B.
< step (4) > step of determining conditions for chemical strengthening
Stress Characteristics (CS) of the chemically strengthened glasses 3A and 3B obtained in the step (1')simAnd DOLsim) The stress characteristic value (CS) of the chemically strengthened glass 2A or 2B measured in the step (2) is compared with the stress characteristic value (CS) of the chemically strengthened glassexpAnd DOLexp) The closest condition is the candidate conditions 2-1 to 2-5. The results are shown in Table 5.
The stress characteristic value (CS) obtained in the step (1') is used for each of the candidate conditions 2-1 to 2-5simAnd DOLsim) And the stress characteristic value (CS) obtained in the step (2)expAnd DOLexp) The Sum of squares of the errors (Δ 3A, Δ 3B) is obtained, and the Sum of squares of the errors (Sum) is obtained. The results are shown in Table 5.
TABLE 4A
TABLE 4B
TABLE 5
As shown in tables 4A and 4B, the results shown in table 4A were within the range shown in table 4B. In table 5, the sum of the square sums Δ 3A and Δ 3B of the errors and the sum of the square sums of the errors are surrounded by a thick frame to be the minimum value. As shown in table 5, the candidate condition 2-1 in which the sum of squares of errors Δ 3A, Δ 3B and the sum of squares of errors are minimum values is the same condition as the chemical strengthening condition of the chemically strengthened glass 2A, 2B shown in table 4A. It can be seen that by using any of the 2 nd glasses, the chemical strengthening conditions for strengthening the 1 st glass can be identified.
From the above results, it is understood that according to the production method of the present invention, the stress characteristics of the chemically strengthened glass can be appropriately controlled, and the chemically strengthened glass 1 in which the 1 st glass is chemically strengthened can be produced.
In addition, by examining the range of stress characteristics (for example, CS and DOL) that can be specified as the candidate conditions, for example, 2-1 in advance, and checking whether or not the stress characteristics of the 2 nd chemically strengthened glass are within the "designed range" in the step (3) or the step (III), the stress characteristics of the chemically strengthened glass can be evaluated or managed efficiently.
The present invention is described in detail with reference to specific embodiments, but it is apparent to those skilled in the art that various modifications and variations can be applied without departing from the scope and spirit of the present invention.
The present application was made based on Japanese patent application No. 2020 and 092689, filed on 27/5/2020, the contents of which are incorporated by reference.
Claims (20)
1. A method for producing a chemically strengthened glass, comprising the following (1) to (3):
(1) chemically strengthening a 1 st glass and a 2 nd glass by immersing them in the same molten salt composition to obtain a 1 st chemically strengthened glass in which the 1 st glass is chemically strengthened and a 2 nd chemically strengthened glass in which the 2 nd glass is chemically strengthened, the 2 nd glass being a glass in which at least one of a K-Na substitution rate and a Na-Li substitution rate in ion exchange is higher than that of the 1 st glass,
(2) measuring the stress characteristics of the 2 nd chemically strengthened glass,
(3) it was confirmed whether or not the stress characteristics of the 2 nd chemically strengthened glass are within the designed range.
2. The method for producing chemically strengthened glass according to claim 1, further comprising the following (4),
(4) determining the conditions of the chemical strengthening of the (1) according to the stress characteristics of the 2 nd chemically strengthened glass.
3. The method for producing a chemically strengthened glass according to claim 1 or 2, wherein, prior to the step (1), the method comprises the steps of (1'),
(1') A3 rd glass having the same composition as the 2 nd glass is chemically strengthened to obtain a 3 rd chemically strengthened glass, and the stress characteristics of the 3 rd chemically strengthened glass are measured to determine the relationship between the chemical strengthening conditions and the stress characteristics of the composition of the 2 nd glass.
4. The method for producing a chemically strengthened glass according to any one of claims 1 to 3, wherein the stress characteristic of the step (2) is at least one selected from a surface compressive stress CS, a compressive stress depth of layer DOL and a tensile stress CT at a sheet thickness center.
5. The method for producing a chemically strengthened glass according to any one of claims 2 to 4, wherein the conditions for the chemical strengthening in the step (1) include a dipping time of the 1 st glass and the 2 nd glass in the molten salt composition and a temperature of the molten salt composition.
6. The method for producing a chemically strengthened glass according to any one of claims 1 to 5, wherein the thickness of the 2 nd glass is 0.3 to 2.5 mm.
7. The method for producing a chemically strengthened glass according to any one of claims 3 to 6, wherein a plate thickness of the 2 nd glass is the same as a plate thickness of the 3 rd glass.
8. The method for producing a chemically strengthened glass according to any one of claims 1 to 7, wherein 2 or more types of glasses having different compositions are used as the 2 nd glass.
9. The method for producing a chemically strengthened glass according to any one of claims 1 to 8, wherein the rate of K-Na substitution in the 2 nd glass is higher than that in the 1 st glass.
10. The method for producing chemically strengthened glass according to claim 9, wherein the diffusion depth of potassium ions in the 1 st chemically strengthened glass is 10 μm or less.
11. The method for producing a chemically strengthened glass according to claim 9 or 10, wherein the K-Na substitution rate of the 2 nd glass is 1.1 times or more the K-Na substitution rate of the 1 st glass.
12. The method for producing a chemically strengthened glass according to any one of claims 9 to 11, wherein the 2 nd glass is a glass in which a refractive index is increased by replacing sodium ions in the 2 nd glass with potassium ions.
13. The method for producing a chemically strengthened glass according to any one of claims 9 to 12, wherein the composition of the 2 nd glass is compared with the composition of the 1 st glass in terms of oxide basisContains Na in a large amount2O1 mol% or more.
14. The method for producing a chemically strengthened glass according to any one of claims 1 to 8, wherein the Na-Li substitution rate of the 2 nd glass is higher than that of the 1 st glass.
15. The method for producing chemically strengthened glass according to claim 14, wherein the diffusion depth of sodium ions in the 1 st chemically strengthened glass is 50 μm or less.
16. The method for producing a chemically strengthened glass according to claim 14 or 15, wherein the Na — Li substitution rate of the 2 nd glass is 1.1 times or more the Na-Li substitution rate of the 1 st glass.
17. The method for producing a chemically strengthened glass according to any one of claims 1 to 16, wherein the 1 st chemically strengthened glass has a visible light transmittance of 80% or less in terms of a sheet thickness of 0.7 mm.
18. The method for producing a chemically strengthened glass according to any one of claims 1 to 16, wherein 1 or less of interference fringes are observed with a surface stress meter based on the principle of observation of the optical waveguide effect with respect to the 1 st chemically strengthened glass.
19. The method for producing a chemically strengthened glass according to any one of claims 1 to 16, wherein the refractive index of the 1 st chemically strengthened glass is out of the range of 1.40 to 1.62.
20. A method for managing stress characteristics of chemically strengthened glass, comprising the following (I) to (III):
(I) chemically strengthening a 1 st glass and a 2 nd glass by immersing them in the same molten salt composition to obtain a 1 st chemically strengthened glass in which the 1 st glass is chemically strengthened and a 2 nd chemically strengthened glass in which the 2 nd glass is chemically strengthened, the 2 nd glass being a glass in which at least one of a K-Na substitution rate and a Na-Li substitution rate in ion exchange is higher than that of the 1 st glass,
(II) measuring the stress characteristics of the 2 nd chemically strengthened glass,
(III) confirming that the stress characteristics of the 2 nd chemically strengthened glass are within the designed range.
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