WO2012093525A1 - Procédé pour la fabrication de matériau en verre renforcé - Google Patents

Procédé pour la fabrication de matériau en verre renforcé Download PDF

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Publication number
WO2012093525A1
WO2012093525A1 PCT/JP2011/077127 JP2011077127W WO2012093525A1 WO 2012093525 A1 WO2012093525 A1 WO 2012093525A1 JP 2011077127 W JP2011077127 W JP 2011077127W WO 2012093525 A1 WO2012093525 A1 WO 2012093525A1
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WO
WIPO (PCT)
Prior art keywords
compressive stress
stress layer
glass material
tempered glass
layer
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Application number
PCT/JP2011/077127
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English (en)
Japanese (ja)
Inventor
昌志 田部
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日本電気硝子株式会社
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Publication date
Application filed by 日本電気硝子株式会社 filed Critical 日本電気硝子株式会社
Priority to JP2011551338A priority Critical patent/JPWO2012093525A1/ja
Publication of WO2012093525A1 publication Critical patent/WO2012093525A1/fr

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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
    • C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
    • 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

Definitions

  • the present invention relates to a method for producing a tempered glass material.
  • the present invention relates to a method for producing a tempered glass material having a compressive stress layer on the surface.
  • Patent Document 1 listed below describes a method for flattening by wet etching after chemically strengthening a glass substrate as a method for producing a chemically strengthened strengthened glass substrate.
  • wet etching is performed for a relatively long time using a relatively high concentration of hydrofluoric acid. Is called. Specifically, it is described that wet etching is performed for 10 minutes using 0.5% by mass of hydrofluoric acid and wet etching is performed for 0.5 minutes using 15% by mass of hydrofluoric acid.
  • Patent Document 1 the method for producing a tempered glass substrate described in Patent Document 1 has a problem that it is difficult to produce a tempered glass substrate having sufficiently high strength.
  • the present invention has been made in view of such points, and an object thereof is to provide a method capable of producing a tempered glass material having high strength.
  • the method for producing a tempered glass material according to the present invention relates to a method for producing a tempered glass material in which a compressive stress layer is formed on the surface layer.
  • the manufacturing method of the tempered glass material which concerns on this invention is equipped with the preparation process and the chemical etching process.
  • a preparation process is a process of preparing the glass material in which the compressive-stress layer was formed in the surface layer.
  • the chemical etching step is a step of chemically etching the surface layer of the compressive stress layer.
  • the preparing step may be a compressive stress layer forming step of forming a compressive stress layer on the surface layer of the glass material.
  • the compressive stress layer forming step may be a step of forming the compressive stress layer by exchanging ions in the surface layer of the glass material with ions having a larger ion radius than the ions.
  • the surface layer of the compressive stress layer is preferably chemically etched so that the compressive stress reduction rate of the compressive stress layer is 5% or less.
  • the preparation step and the chemical etching step so that the compressive stress of the compressive stress layer after chemical etching is in the range of 300 MPa to 1200 MPa.
  • the compressive stress layer forming step it is preferable to perform the compressive stress layer forming step so that the compressive stress of the compressive stress layer before chemical etching is in the range of 320 MPa to 1250 MPa.
  • the surface layer of the compressive stress layer is chemically etched using hydrofluoric acid having an HF concentration of 0.01% by mass to 0.1% by mass as an etchant for 1 second to 22 minutes.
  • chemical etching may be performed by immersing the glass material in an etching solution.
  • the chemical etching step it is preferable to perform chemical etching so that the thickness reduction due to etching is 0.1 ⁇ m to 3 ⁇ m.
  • a method capable of producing a tempered glass material having high strength can be provided.
  • FIG. 1 is a schematic cross-sectional view of a glass plate according to an embodiment of the present invention.
  • FIG. 2 is a schematic cross-sectional view of a glass plate after a compressive stress layer forming step is performed in an embodiment of the present invention.
  • FIG. 3 is a schematic cross-sectional view of a tempered glass sheet manufactured in one embodiment of the present invention.
  • FIG. 4 is a photomicrograph of the end face of the evaluation sample before etching.
  • FIG. 5 is a photomicrograph of the end face of the evaluation sample 8.
  • the tempered glass material may not be a tempered glass plate. That is, the tempered glass material may not be plate-shaped.
  • the tempered glass material may have, for example, a rectangular parallelepiped shape or a spherical shape.
  • the glass plate 10 (refer FIG. 1) used as the base material of the tempered glass plate 1 is prepared.
  • the glass plate 10 is typically a stress-substantially homogeneous glass plate that does not have a compressive stress layer.
  • the glass plate 10 has a shape corresponding to the shape of the tempered glass plate 1 to be manufactured. For this reason, for example, when manufacturing a rectangular parallelepiped tempered glass material, a rectangular parallelepiped glass material may be prepared.
  • the glass plate 10 can form a compressive stress layer 11a described later.
  • a compressive stress layer 11a when the compressive stress layer 11a is formed by an ion exchange method, a glass plate containing an alkali metal ion such as sodium ion can be used as the glass plate 10, for example.
  • an alkali-free glass plate may be used as the glass plate 10.
  • a compressive stress layer forming step is performed. Thereby, the preparation process which prepares the glass plate 10 in which the compressive-stress layer was formed in the surface layer 10a is performed.
  • a compressive stress layer is formed on the surface layer 10 a of the glass plate 10.
  • the method for forming the compressive stress layer is not particularly limited.
  • the compressive stress layer may be formed by an air cooling strengthening method in which the surface layer is rapidly cooled by blowing cold air to the surface layer, or the compressive stress layer may be formed by an ion exchange method.
  • the ion exchange method is a method of forming a compressive stress layer by exchanging ions in the surface layer 10a of the glass plate 10 with ions having an ion radius larger than that of the ions.
  • FIG. 2 shows a schematic cross-sectional view of the glass plate 11 on which the compressive stress layer 11a is formed.
  • the ion exchange conditions such as the type of ion exchange solution, temperature, and immersion time are the type of glass plate 10 to be used, the thickness of the compressive stress layer 11a to be formed, and the magnitude of the compressive stress of the compressive stress layer 11a to be formed. It can be set as appropriate according to the situation.
  • the temperature of the ion exchange solution can be, for example, about 400 ° C. to 500 ° C.
  • the immersion time of the glass plate 10 in the ion exchange solution can be, for example, about 1 hour to 10 hours.
  • the thickness of the compressive stress layer 11a can be, for example, 20 ⁇ m to 70 ⁇ m, and preferably 30 ⁇ m to 50 ⁇ m.
  • the compressive stress of the compressive stress layer 11a is preferably 320 MPa to 1250 MPa.
  • the compressive stress of the compressive stress layer 11a is more preferably 430 MPa to 1160 MPa.
  • the compressive stress of the compressive stress layer 11a is more preferably 570 MPa to 850 MPa.
  • the compressive stress of the compressive stress layer 11a is more preferably 700 MPa to 850 MPa. This is because if the compressive stress of the compressive stress layer 11a is too low, the strength of the tempered glass plate 1 may be too low. On the other hand, if the compressive stress of the compressive stress layer 11a is too high, the internal stress of the tempered glass plate 1 becomes too high and may lead to self-destruction.
  • the “thickness of the compressive stress layer” means the depth of the region where the optical waveguide effect is generated by the compressive stress of the surface layer of the tempered glass plate.
  • “thickness of compressive stress layer” and “compressive stress value” are values measured by using FSM-6000 manufactured by Orihara Seisakusho and setting photoelastic constants according to the glass material at appropriate times. .
  • the compressive stress layer 1a is formed by chemically etching only the surface layer of the compressive stress layer 11a.
  • strength can be manufactured so that it may be supported also in the experiment example mentioned later.
  • the reason why the strength is improved by chemically etching the surface layer of the compressive stress layer 11a is not clear, it is considered that the surface scratches, cracks, etc. disappear, or the surface is flattened.
  • the compression stress layer 11a has a compressive stress reduction rate, that is, a value obtained by subtracting the compressive stress of the compressive stress layer 1a from the compressive stress of the compressive stress layer 11a.
  • the ratio [((compressive stress of compressive stress layer 11a) ⁇ (compressive stress of compressive stress layer 1a)) / (compressive stress of compressive stress layer 11a)] to stress is 5% or less, more preferably 2% or less. It is preferable to chemically etch the surface layer of the compressive stress layer 11a within the range.
  • the compressive stress layer forming step and the etching step so that the compressive stress of the compressive stress layer 1a is in the range of 300 MPa to 1200 MPa. More preferably, the compressive stress layer forming step and the etching step are performed so that the compressive stress of the compressive stress layer 1a is in the range of 400 MPa to 1100 MPa. More preferably, the compressive stress layer forming step and the etching step are performed so that the compressive stress of the compressive stress layer 1a is in the range of 540 MPa to 820 MPa.
  • the compressive stress layer forming step and the etching step are performed so that the compressive stress of the compressive stress layer 1a is in the range of 720 MPa to 820 MPa. This is because if the compressive stress of the compressive stress layer 1a is too low, the strength of the tempered glass plate 1 may be too low. On the other hand, if the compressive stress of the compressive stress layer 1a is too high, the internal stress of the tempered glass plate 1 becomes too high and may lead to self-destruction.
  • chemical etching is preferably performed for 1 second to 22 minutes using hydrofluoric acid having an HF concentration of 0.01% by mass to 0.1% by mass as an etchant. More preferably, chemical etching is performed for 30 seconds to 22 minutes using hydrofluoric acid having an HF concentration of 0.03% to 0.1% by mass as an etchant.
  • the etching solution is not limited to hydrofluoric acid.
  • hydrochloric acid, sulfuric acid, nitric acid, ammonium fluoride, alkali metal hydroxide, aqueous ammonia, buffered hydrofluoric acid, and the like are preferably used.
  • the chemical etching may be performed, for example, by applying an etching solution to the surface of the compressive stress layer 11a, but is preferably performed by immersing the glass plate 11 in the etching solution. In the chemical etching step, it is preferable to stir the etching solution.
  • the chemical etching step it is preferable to perform chemical etching so that the amount of decrease in the thickness of the compressive stress layer 11a due to etching falls within the range of 0.1 ⁇ m to 3 ⁇ m, and the amount of decrease in the thickness of the compressive stress layer 11a due to etching. More preferably, the chemical etching is performed so that the thickness is in the range of 0.5 ⁇ m to 3 ⁇ m.
  • a glass base material made of Nippon Electric Glass Co., Ltd. made of chemically strengthened glass (material name: CX-01) having a thickness of 1 mm is cut into a size of 40 mm ⁇ 80 mm, and the end surface is mirror-polished to obtain a size of 40 mm ⁇ 80 mm ⁇ 1 mm.
  • a glass plate was created.
  • An end face of the sample before etching is shown in FIG.
  • a photomicrograph of the end face of the evaluation sample 8 is shown in FIG. From the photographs shown in FIGS. 4 and 5, it can be seen that if the etching time is too long, the end face is damaged by the etching.

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  • Chemical & Material Sciences (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)

Abstract

L'invention concerne un procédé de fabrication d'un matériau en verre renforcé présentant un degré élevé de résistance. Une étape de gravure chimique est réalisée en vue de la gravure chimique d'une couche de contrainte de compression de surface d'un matériau en verre, la couche de contrainte de compression étant formée en tant que la couche de surface.
PCT/JP2011/077127 2011-01-07 2011-11-25 Procédé pour la fabrication de matériau en verre renforcé WO2012093525A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2011551338A JPWO2012093525A1 (ja) 2011-01-07 2011-11-25 強化ガラス材の製造方法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2011001667 2011-01-07
JP2011-001667 2011-01-07

Publications (1)

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WO2012093525A1 true WO2012093525A1 (fr) 2012-07-12

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TW (1) TW201231418A (fr)
WO (1) WO2012093525A1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014013996A1 (fr) * 2012-07-17 2014-01-23 旭硝子株式会社 Procédé de fabrication pour lamelle couvre-objet renforcée, et lamelle couvre-objet renforcée
WO2014045809A1 (fr) * 2012-09-20 2014-03-27 旭硝子株式会社 Procédé de fabrication de verre chimiquement renforcé
WO2013071021A3 (fr) * 2011-11-10 2014-10-02 Corning Incorporated Renforcement du verre à l'acide
CN114105493A (zh) * 2021-11-08 2022-03-01 江西水晶光电有限公司 一种提升摄像头保护盖板强度的工艺

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000207730A (ja) * 1999-01-12 2000-07-28 Ishizuka Glass Co Ltd 磁気記録媒体用ガラス基板
JP2000311336A (ja) * 1999-04-28 2000-11-07 Nippon Sheet Glass Co Ltd 磁気ディスク用基板の作製方法、その方法により得られた磁気ディスク用基板及び磁気記録媒体
JP2002174810A (ja) * 2000-12-08 2002-06-21 Hoya Corp ディスプレイ用ガラス基板及びその製造方法並びにこれを用いたディスプレイ
JP2010168270A (ja) * 2008-12-26 2010-08-05 Hoya Corp ガラス基材及びその製造方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000207730A (ja) * 1999-01-12 2000-07-28 Ishizuka Glass Co Ltd 磁気記録媒体用ガラス基板
JP2000311336A (ja) * 1999-04-28 2000-11-07 Nippon Sheet Glass Co Ltd 磁気ディスク用基板の作製方法、その方法により得られた磁気ディスク用基板及び磁気記録媒体
JP2002174810A (ja) * 2000-12-08 2002-06-21 Hoya Corp ディスプレイ用ガラス基板及びその製造方法並びにこれを用いたディスプレイ
JP2010168270A (ja) * 2008-12-26 2010-08-05 Hoya Corp ガラス基材及びその製造方法

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013071021A3 (fr) * 2011-11-10 2014-10-02 Corning Incorporated Renforcement du verre à l'acide
JP2014534945A (ja) * 2011-11-10 2014-12-25 コーニング インコーポレイテッド ガラスの酸強化
US8978414B2 (en) 2011-11-10 2015-03-17 Corning Incorporated Acid strengthening of glass
US9505653B2 (en) 2011-11-10 2016-11-29 Corning Incorporated Acid strengthening of glass
WO2014013996A1 (fr) * 2012-07-17 2014-01-23 旭硝子株式会社 Procédé de fabrication pour lamelle couvre-objet renforcée, et lamelle couvre-objet renforcée
WO2014045809A1 (fr) * 2012-09-20 2014-03-27 旭硝子株式会社 Procédé de fabrication de verre chimiquement renforcé
CN114105493A (zh) * 2021-11-08 2022-03-01 江西水晶光电有限公司 一种提升摄像头保护盖板强度的工艺

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TW201231418A (en) 2012-08-01
JPWO2012093525A1 (ja) 2014-06-09

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