WO2020045093A1 - Procédé d'acquisition de répartition de contrainte de verre trempé et procédé de fabrication de verre trempé - Google Patents

Procédé d'acquisition de répartition de contrainte de verre trempé et procédé de fabrication de verre trempé Download PDF

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Publication number
WO2020045093A1
WO2020045093A1 PCT/JP2019/031953 JP2019031953W WO2020045093A1 WO 2020045093 A1 WO2020045093 A1 WO 2020045093A1 JP 2019031953 W JP2019031953 W JP 2019031953W WO 2020045093 A1 WO2020045093 A1 WO 2020045093A1
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Prior art keywords
stress distribution
tempered glass
glass
stress
tempered
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PCT/JP2019/031953
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English (en)
Japanese (ja)
Inventor
聡司 大神
Original Assignee
Ａｇｃ株式会社
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Filing date
Publication date
Application filed by Ａｇｃ株式会社 filed Critical Ａｇｃ株式会社
Priority to KR1020217003694A priority Critical patent/KR102667994B1/ko
Priority to CN201980051963.5A priority patent/CN112534228B/zh
Priority to JP2020539330A priority patent/JPWO2020045093A1/ja
Publication of WO2020045093A1 publication Critical patent/WO2020045093A1/fr
Priority to JP2023069475A priority patent/JP2023089250A/ja

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
    • G01L1/00—Measuring force or stress, in general
    • G01L1/24—Measuring force or stress, in general by measuring variations of optical properties of material when it is stressed, e.g. by photoelastic stress analysis using infrared, visible light, ultraviolet
    • G01L1/241—Measuring force or stress, in general by measuring variations of optical properties of material when it is stressed, e.g. by photoelastic stress analysis using infrared, visible light, ultraviolet by photoelastic stress analysis
    • 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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
    • G01L1/00—Measuring force or stress, in general
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
    • G01L1/00—Measuring force or stress, in general
    • G01L1/24—Measuring force or stress, in general by measuring variations of optical properties of material when it is stressed, e.g. by photoelastic stress analysis using infrared, visible light, ultraviolet

Definitions

  • the present invention relates to a method for obtaining a stress distribution of a tempered glass and a method for manufacturing a tempered glass.
  • glass may be used for the display unit and the housing body.
  • a so-called tempered glass having a surface layer (ion exchange layer) formed by ion exchange on the glass surface is used.
  • aluminosilicate glass containing lithium has been widely used.
  • chemically strengthened glass in which both ion exchange of lithium ion in glass and sodium ion in molten salt and ion exchange of sodium ion in glass and potassium ion in molten salt are performed. It has been known.
  • the stress distribution of the tempered glass containing lithium and having undergone two types of ion exchange shows a characteristic of bending at a predetermined glass depth (DOL_TP).
  • the refractive index distribution shows characteristics as shown in FIG.
  • the stress distribution on the glass surface layer side than DOL_TP is measured, and the stress distribution on the glass deep layer side from DOL_TP is determined in advance by the stress distribution of the tempered glass manufactured under the same tempering conditions. It was measured and calculated based on the results of the previous measurement. This eliminates the need to measure the stress distribution on the glass deeper side than DOL_TP in the tempered glass manufacturing process, thereby shortening the measurement time.
  • the present invention has been made in view of the above points, and has as its object to improve the accuracy of calculating the stress distribution on the glass deeper side than DOL_TP in tempered glass.
  • the method for obtaining the stress distribution of the present tempered glass is as a preliminary preparation, measuring the stress distribution for a plurality of tempered glasses including tempered glass having different tempering conditions, and measuring the stress distribution on the glass surface layer side more than the glass depth at the bending position.
  • the relationship between the first stress distribution and the second stress distribution is determined based on the measurement result of the first stress distribution and the measurement result of the second stress distribution on the glass deeper side than the glass depth.
  • Deriving the parameters shown, and using the parameters to determine the stress distribution of the tempered glass to be measured, comprising the step of obtaining the stress distribution, the step of obtaining the stressed glass for the tempered glass to be measured
  • the method includes a step of measuring a first stress distribution and a step of calculating the second stress distribution based on the parameter.
  • the accuracy of calculating the stress distribution on the deeper side of the glass than DOL_TP can be improved.
  • FIG. 1 is a diagram illustrating a stress distribution in the depth direction of the tempered glass.
  • CS2 is a stress value at the outermost surface
  • CS_TP is a stress value at a position where the stress distribution is bent
  • CT is a stress value at the deepest portion of the glass (that is, the center portion in the plate thickness direction).
  • DOL_TP is the glass depth where the stress distribution is bent
  • DOL_zero is the glass depth where the stress value becomes zero
  • DOL_tail is the glass depth where the stress value becomes the same value as CT.
  • the stress distribution on the glass surface side from DOL_TP is referred to as a first stress distribution
  • the stress distribution on the glass depth side from DOL_TP is referred to as a second stress distribution.
  • the first stress distribution can be measured by photoelasticity techniques, for example, by propagating light along the glass surface using the optical waveguide effect.
  • two types of light components P-polarized light and S-polarized light
  • the two types of bright line arrays are imaged by an image sensor such as a CCD (Charge Coupled Device), and the positions of at least two or more bright lines in each of the two types of bright line arrays are used to form tempered glass corresponding to two types of light components.
  • the refractive index distribution from the surface to the depth direction is calculated.
  • the first stress distribution from the surface of the tempered glass to the depth direction can be calculated based on the difference between the refractive index distributions of the two types of light components and the photoelastic constant of the glass.
  • the first stress distribution can be measured, for example, using a glass surface stress meter FSM-6000LE manufactured by Orihara Seisakusho.
  • the first stress distribution may be measured by any method other than the above, for example, by the well-known inverse @ WKB method (for example, see US Pat. No. 9,140,543).
  • the measurement using the optical waveguide effect can measure only a portion where the refractive index decreases from the glass surface toward the glass deep layer. Therefore, this method can be used only for the measurement of the first stress distribution.
  • the second stress distribution can be measured, for example, using the principle of photoelastic stress measurement using the polarization phase difference of laser light and scattered light.
  • the polarization phase difference of the laser light is changed by one or more wavelengths with respect to the wavelength of the laser light, and the scattered light emitted when the laser light having the changed polarization
  • a plurality of images are taken at time intervals to obtain a plurality of images.
  • a periodic luminance change of the scattered light is measured using the plurality of acquired images, a phase change of the luminance change is calculated, and a second stress distribution can be calculated based on the phase change.
  • the second stress distribution can be measured using, for example, a scattered light photoelastic stress meter SLP-1000 manufactured by Orihara Seisakusho.
  • the second stress distribution may be measured by any method other than the above.
  • the second stress distribution is obtained by using, for example, a scattered light photoelastic stress meter SLP-2000 or SCALP-04 or SCALP-05 manufactured by Orihara Seisakusho, or a birefringence imaging device abrio manufactured by CRi, USA. It may be measured.
  • the reflected light and scattered light on the glass surface overlap with the scattered light from inside the glass and interfere with the measurement, and the measurement accuracy near the glass surface is low. Therefore, this method can be used only for measuring the second stress distribution.
  • the manufacturing process of the tempered glass may include a step of measuring the first stress distribution and the second stress distribution, and making a shipping judgment based on the first stress distribution and the second stress distribution.
  • the measurement time becomes longer and the productivity is reduced.
  • the first stress distribution and the second stress distribution are each measured in advance by an appropriate measurement method, and a database is created.
  • a parameter indicating the relationship between the stress distribution and the second stress distribution is derived.
  • the first stress distribution is measured, and the second stress distribution is calculated based on parameters derived in advance. This will be described in detail below with reference to FIG.
  • FIG. 2 is an example of a flowchart showing a method for obtaining a stress distribution of a tempered glass.
  • Step S10 in FIG. 2 is a preparatory process performed independently of the tempered glass manufacturing process.
  • step S10 first, a stress distribution is measured for a plurality of tempered glasses including tempered glasses having different tempering conditions. Specifically, for example, the first stress distribution is measured using FSM-6000LE, and the second stress distribution is measured using SLP-1000. Then, a parameter indicating the relationship between the first stress distribution and the second stress distribution is derived based on the measurement result of the first stress distribution and the measurement result of the second stress distribution.
  • the first stress distribution can be represented, for example, by ⁇ 1 (x, Bn).
  • x indicates the position of the tempered glass in the depth direction
  • Bn indicates fitting parameters.
  • Bn may be plural.
  • the first stress distribution can be, for example, linearly approximated.
  • the first stress distribution is represented by ⁇ 1 (x, x), where CS2 is the stress value on the outermost surface and a is the gradient of the stress on the tempered glass surface.
  • Bn) CS2 + ax (fitting).
  • the first stress distribution may be expressed by any fitting function as long as the first stress distribution is a first-order function or more and two or more parameters are used.
  • the second stress distribution can be represented, for example, as ⁇ 2 (x, Cm, CT).
  • x indicates a position in the depth direction of the tempered glass
  • Cm indicates a parameter derived in step S10.
  • the parameter Cm may be plural (C1, C2,).
  • the parameter Cm can be derived, for example, for each sheet thickness of tempered glass. Alternatively, the thickness of the tempered glass may be included in the parameter.
  • a correlation diagram between CS2 and Cm and a correlation diagram between a and Cm can be obtained based on the measurement result of the first stress distribution and the measurement result of the second stress distribution.
  • the relationship between CS2 and a and Cm can be derived.
  • Cm can be represented by a linear function of CS2 and a.
  • Cm may be represented by a quadratic or higher function of CS2 and a. That is, Cm can be a function of first order or higher of Bn.
  • step S20 the stress distribution of the tempered glass to be measured is determined.
  • Step S20 can be included in a tempered glass manufacturing process.
  • Step S20 includes a step S201 of measuring a first stress distribution for the tempered glass to be measured and a step S202 of calculating a second stress distribution based on the parameter Cm derived in step S10.
  • step S201 the first stress distribution of the tempered glass to be measured is measured using, for example, FSM-6000LE.
  • CS2 and a can be obtained by FSM-6000LE.
  • step S202 the second stress distribution is calculated (the second stress distribution is not measured).
  • the second stress distribution is represented by ⁇ 2 (x, Cm, CT)
  • Cm is a first-order function of CS2 and a, but since CS2 and a are known in step S201, Cm is also known.
  • the second stress distribution can be calculated by obtaining CT in step S202.
  • the first stress distribution and the second stress distribution are determined based on the stress distribution measurement results for a plurality of tempered glasses including tempered glasses having different tempering conditions. Derive a parameter indicating the relationship. Then, a second stress distribution is calculated based on the derived parameters.
  • step S10 shown in FIG. 2 will be described.
  • a 0.7 mm-thick lithium-containing aluminosilicate glass was chemically strengthened under the four tempering conditions (conditions 1 to 4) shown in Table 1 to produce a tempered glass.
  • the first stress distribution was measured by FSM-6000LE (manufactured by Orihara Seisakusho, hereinafter referred to as FSM), and the second stress distribution was measured by SLP-1000 (manufactured by Orihara Seisakusho, hereinafter SLP). 1) to obtain the characteristic values of the stress distribution shown in FIG. Table 2 shows the obtained characteristic values.
  • the second stress distribution measured by the SLP is obtained by fitting the equation (1) to the measurement result. Therefore, for comparison, the measurement results (second stress distribution) by SLP of the four tempered glasses chemically strengthened under the conditions 1 to 4 were fitted by the equation (1) to obtain the average parameters CS0 and c ( Comparative Example in Table 3).
  • the measurement results (second stress distribution) of the four tempered glasses chemically strengthened under the conditions 1 to 4 by SLP were fitted by the equation (2) to obtain the parameters C 1 to C 6 .
  • the slope a of the stress may be obtained by dividing the CS value measured by the FSM and the DOL.
  • the fitting may be determined by a least square method or the like so that an error is minimized.
  • step S20 in FIG. 2 will be described.
  • Eight types of samples in which the concentration of the reinforcing salt was changed were prepared, and the first stress distribution was measured by FSM.
  • CT was obtained from the result of the first stress distribution measured by the FSM and the second stress distribution derived from the parameters of the comparative example in Table 3 (Comparative Example in Table 4).
  • CT was obtained from the result of the first stress distribution measured by the FSM and the second stress distribution derived from the parameters of the example of Table 3 (Example of Table 4).
  • CT was actually measured by SLP, and the results are shown in Table 4 together with the CTs obtained in Comparative Examples and Examples.
  • Table 4 shows the correlation coefficient between the actually measured value and the comparative example, and the correlation coefficient between the actually measured value and the example.
  • the FSM measurement values for the tempered glass having different tempering conditions are included in the fitting function ⁇ 2 as a part of the parameters, so that the second stress distribution can be accurately calculated even if the tempered glass to be measured changes. Become.
  • step S10 the concentration of the strengthening salt is changed as an example of the change of the strengthening conditions of the strengthened glass, but the thickness of the glass, the strengthening temperature and the strengthening time may be changed, and there is no limitation on the changing conditions.
  • the concentration of the strengthening salt may be added to the molten salt which increases or decreases when a new tempered glass is strengthened many times.
  • a mixed salt of KNO 3 , NaNO 3 , and LiNO 3 was used in the second chemical strengthening.
  • a mixture of three kinds of KNO 3 , NaNO 3 , and LiNO 3 may be used.
  • Cm can be a function of the first order or more of the thickness, and for example, the second stress distribution may be fitted by Expression (3).
  • the plate thickness may be measured simultaneously with the stress measurement in step S20.
  • Cm can be a function of the first order or more of the strengthening time t CS and the strengthening time T CS .
  • the second stress distribution is expressed by Equation (4). May be fitted.
  • the second stress distribution may be fitted by equation (5).
  • the plate thickness may be measured simultaneously with the stress measurement in step S20.
  • the second stress distribution may be fitted by equation (6).
  • the plate thickness may be measured simultaneously with the stress measurement in step S10 and / or S20.
  • the second stress distribution may be fitted with equation (7).
  • the refractive index or the refractive index distribution of the tempered glass may be measured at the time of the first stress measurement, and the characteristic value may be used as a function of Cm.
  • the characteristic value for example, the surface layer refractive index, the deepest part refractive index, the minimum value of the refractive index, and the maximum value / minimum value of the change rate of the refractive index change of the tempered glass can be used.
  • Cm can be a function of the first order or higher of the surface layer refractive index or the deepest part refractive index of the tempered glass.

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Surface Treatment Of Glass (AREA)
  • Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)

Abstract

L'invention concerne un procédé d'acquisition de la répartition de contrainte de verre trempé comprenant une étape dans laquelle, à titre de préparation avancée, des répartitions de contrainte pour une pluralité de feuilles de verre trempé comprenant des feuilles de verre trempé ayant différentes conditions de trempe sont mesurées et les résultats de la mesure de premières répartitions de contrainte davantage vers les surfaces supérieures des feuilles de verre que les profondeurs de verre aux positions où les répartitions de contrainte se plient et les résultats de la mesure de secondes répartitions de contrainte davantage vers les surfaces inférieures des feuilles de verre que les profondeurs de verre sont utilisés pour dériver un paramètre indiquant la relation entre les premières répartitions de contrainte et les secondes répartitions de contrainte et une étape dans laquelle le paramètre est utilisé pour déterminer la répartition de contrainte du verre trempé à mesurer. L'étape dans laquelle la répartition de contrainte est déterminée comprend une étape de mesure de la première répartition de contrainte du verre trempé à mesurer et une étape de calcul de la seconde répartition de contrainte sur la base du paramètre.
PCT/JP2019/031953 2018-08-29 2019-08-14 Procédé d'acquisition de répartition de contrainte de verre trempé et procédé de fabrication de verre trempé WO2020045093A1 (fr)

Priority Applications (4)

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KR1020217003694A KR102667994B1 (ko) 2018-08-29 2019-08-14 강화 유리의 응력 분포의 취득 방법, 강화 유리의 제조 방법
CN201980051963.5A CN112534228B (zh) 2018-08-29 2019-08-14 强化玻璃的应力分布的取得方法及强化玻璃的制造方法
JP2020539330A JPWO2020045093A1 (ja) 2018-08-29 2019-08-14 強化ガラスの応力分布の取得方法、強化ガラスの製造方法
JP2023069475A JP2023089250A (ja) 2018-08-29 2023-04-20 強化ガラスの応力分布の取得方法、強化ガラスの製造方法

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JP2018160215 2018-08-29

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20220380250A1 (en) * 2021-05-25 2022-12-01 AGC Inc. Inference method, quality control method, chemically strengthened glass, inference program, storage medium, inference device, and method of manufacturing chemically strengthened glass

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Publication number Priority date Publication date Assignee Title
JP2011527661A (ja) * 2008-07-11 2011-11-04 コーニング インコーポレイテッド 民生用途のための圧縮面を有するガラス
US20130233020A1 (en) * 2012-03-12 2013-09-12 Douglas Clippinger Allan Methods for producing ion-exchangeable glasses
JP2016142600A (ja) * 2015-01-30 2016-08-08 有限会社折原製作所 表面応力測定方法、表面応力測定装置
US20170082577A1 (en) * 2015-09-17 2017-03-23 Corning Incorporated Methods of characterizing ion-exchanged chemically strengthened glasses containing lithium

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Publication number Priority date Publication date Assignee Title
TWI771909B (zh) * 2015-12-08 2022-07-21 美商康寧公司 S型應力輪廓及製造方法
CN109906365B (zh) * 2016-09-26 2021-09-14 折原制作所有限公司 强化玻璃的应力测量装置、强化玻璃的应力测量方法、强化玻璃的制造方法、强化玻璃

Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
JP2011527661A (ja) * 2008-07-11 2011-11-04 コーニング インコーポレイテッド 民生用途のための圧縮面を有するガラス
US20130233020A1 (en) * 2012-03-12 2013-09-12 Douglas Clippinger Allan Methods for producing ion-exchangeable glasses
JP2016142600A (ja) * 2015-01-30 2016-08-08 有限会社折原製作所 表面応力測定方法、表面応力測定装置
US20170082577A1 (en) * 2015-09-17 2017-03-23 Corning Incorporated Methods of characterizing ion-exchanged chemically strengthened glasses containing lithium

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20220380250A1 (en) * 2021-05-25 2022-12-01 AGC Inc. Inference method, quality control method, chemically strengthened glass, inference program, storage medium, inference device, and method of manufacturing chemically strengthened glass

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JPWO2020045093A1 (ja) 2021-08-10
KR20210045989A (ko) 2021-04-27
CN112534228A (zh) 2021-03-19
JP2023089250A (ja) 2023-06-27
CN112534228B (zh) 2022-08-16
KR102667994B1 (ko) 2024-05-23

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