US20130209773A1 - Glass for chemical tempering, chemically tempered glass, and glass plate for display device - Google Patents

Glass for chemical tempering, chemically tempered glass, and glass plate for display device Download PDF

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Publication number
US20130209773A1
US20130209773A1 US13/841,268 US201313841268A US2013209773A1 US 20130209773 A1 US20130209773 A1 US 20130209773A1 US 201313841268 A US201313841268 A US 201313841268A US 2013209773 A1 US2013209773 A1 US 2013209773A1
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Prior art keywords
glass
chemical tempering
sio
glass plate
chemically tempered
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US13/841,268
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English (en)
Inventor
Jun Endo
Shusaku AKIBA
Kazutaka Ono
Tetsuya Nakashima
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AGC Inc
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Asahi Glass Co Ltd
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Application filed by Asahi Glass Co Ltd filed Critical Asahi Glass Co Ltd
Assigned to ASAHI GLASS COMPANY, LIMITED reassignment ASAHI GLASS COMPANY, LIMITED ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: AKIBA, SHUSAKU, ENDO, JUN, NAKASHIMA, TETSUYA, ONO, KAZUTAKA
Publication of US20130209773A1 publication Critical patent/US20130209773A1/en
Priority to US14/597,587 priority Critical patent/US10370286B2/en
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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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
    • C03C3/085—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal
    • 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
    • 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
    • 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
    • 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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
    • C03C3/085—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal
    • C03C3/087—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal containing calcium oxide, e.g. common sheet or container glass
    • 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
    • C03C4/00—Compositions for glass with special properties
    • 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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
    • C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
    • G02F1/1333—Constructional arrangements; Manufacturing methods
    • G02F1/133302—Rigid substrates, e.g. inorganic substrates
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/31—Surface property or characteristic of web, sheet or block
    • Y10T428/315—Surface modified glass [e.g., tempered, strengthened, etc.]

Definitions

  • the present invention relates to a display device for e.g. a mobile device such as a cell phone or a personal digital assistance (PDA), a large-sized flat screen television such as a large-sized liquid crystal television or a large-sized plasma television and a touch panel, a glass plate for a display device suitable for e.g. a cover glass for a display device, and chemically tempered glass or glass for chemical tempering suitable for such a glass plate for a display device.
  • a display device for e.g. a mobile device such as a cell phone or a personal digital assistance (PDA), a large-sized flat screen television such as a large-sized liquid crystal television or a large-sized plasma television and a touch panel, a glass plate for a display device suitable for e.g. a cover glass for a display device, and chemically tempered glass or glass for chemical tempering suitable for such a glass plate for a display device.
  • PDA personal digital assistance
  • cover glass protective glass
  • a cover glass to be used for protecting a display is also required to be made thin.
  • the thickness of the cover glass is made to be thin, the strength is lowered, and there has been a problem such that the cover glass itself is broken by e.g. a shock due to a falling or flying object in the case of an installed type or by dropping during the use in the case of a portable device, and the cover glass cannot perform the essential role to protect the display device.
  • the method to form a compressive stress layer on a glass surface may typically be an air quenching tempering method (physical tempering method) wherein a surface of a glass plate heated to near the softening point is quenched by air cooling or the like, or a chemical tempering method wherein alkali metal ions having a small ion radius (typically Li ions or Na ions) at a glass plate surface are exchanged with alkali ions having a larger ion radius (typically K ions) by ion exchange at a temperature lower than the glass transition point.
  • physical tempering method physical tempering method
  • chemical tempering method wherein alkali metal ions having a small ion radius (typically Li ions or Na ions) at a glass plate surface are exchanged with alkali ions having a larger ion radius (typically K ions) by ion exchange at a temperature lower than the glass transition point.
  • the thickness of the cover glass is required to be thin.
  • the air quenching tempering method is applied to a thin glass plate having a thickness of less than 2 mm, as required for a cover glass, the temperature difference between the surface and the inside tends not to arise, and it is thereby difficult to form a compressive stress layer, and the desired property of high strength cannot be obtained. Therefore, a cover glass tempered by the latter chemical tempering method is usually used.
  • Soda lime glass is inexpensive and has a feature that the surface compressive stress S of a compressive stress layer formed at the surface of the glass by the chemical tempering can be made to be at least 550 MPa, but there has been a problem that it has been difficult to make the thickness t of the compressive stress layer to be at least 30 ⁇ m.
  • Such SiO 2 —Al 2 O 3 —Na 2 O type glass has a feature that it is possible not only to make the above S to be at least 550 MPa but also to make the above t to be at least 30 ⁇ m.
  • Patent Document 1 JP-A-2007-11210
  • Patent Document 2 US Patent Application Publication No. 2009/0298669
  • a mobile device is dropped from the user's hand, pocket or bag and its cover glass gets flaws (indentations), or the dropped mobile device may be stepped on or the user may sit on the mobile device put in the pocket, and a heavy load may thereby be applied to the cover glass in many cases.
  • a flat screen television such as a liquid crystal television or a plasma television, particularly a large-sized flat screen television having a size of at least 20 inches, is likely to have flaws since its cover glass has a large size, and as the screen is large, the probability of breakage from the flaws as the breakage origin is high. Further, when a flat screen television is used as hung on the wall, it may fall down, and in such a case, a large load may be applied to the cover glass.
  • a touch panel is likely to have flaws such as scratches at the time of its use.
  • the present invention provides glass for chemical tempering, which comprises, as represented by mole percentage based on oxides, from 62 to 68% of SiO 2 , from 6 to 12% of Al 2 O 3 , from 7 to 13% of MgO, from 9 to 17% of Na 2 O, and from 0 to 7% of K 2 O, wherein the difference (R 2 O ⁇ Al 2 O 3 ) obtained by subtracting the content of Al 2 O 3 from the total content of R 2 O i.e. Na 2 O and K 2 O, is less than 10%, and when ZrO 2 is contained, its content is at most 0.8%.
  • the difference (R 2 O ⁇ Al 2 O 3 ) obtained by subtracting the content of Al 2 O 3 from the total content of R 2 O i.e. Na 2 O and K 2 O is less than 10%, and when ZrO 2 is contained, its content is at most 0.8%.
  • from 62 to 68% means at least 62% and at most 68%.
  • the present invention further provides the above glass for chemical tempering, which contains from 64 to 67% of SiO 2 , and from 6 to 7.5% of Al 2 O 3 , wherein the total content of SiO 2 and Al 2 O 3 is from 69 to 73%.
  • the present invention further provides glass for chemical tempering, which comprises, as represented by mole percentage based on oxides, from 62 to 66% of SiO 2 , from 6 to 12% of Al 2 O 3 , from 7 to 13% of MgO, from 9 to 17% of Na 2 O, and from 0 to 7% of K 2 O, wherein (R 2 O ⁇ Al 2 O 3 ) is less than 10%, and when ZrO 2 is contained, its content is at most 0.8% (hereinafter this glass for chemical tempering will sometimes be referred to as glass A).
  • the present invention further provides glass for chemical tempering, which comprises, as represented by mole percentage based on oxides, from 64 to 68% of SiO 2 , from 6 to 11% of Al 2 O 3 , from 7 to 12% of MgO, from 12 to 17% of Na 2 O, and from 0 to 6% of K 2 O, wherein (R 2 O ⁇ Al 2 O 3 ) is less than 10%, and when ZrO 2 is contained, its content is at most 0.8% (hereinafter this glass for chemical tempering will sometimes be referred to as glass B).
  • glass for chemical tempering comprises, as represented by mole percentage based on oxides, from 64 to 68% of SiO 2 , from 6 to 11% of Al 2 O 3 , from 7 to 12% of MgO, from 12 to 17% of Na 2 O, and from 0 to 6% of K 2 O, wherein (R 2 O ⁇ Al 2 O 3 ) is less than 10%, and when ZrO 2 is contained, its content is at most 0.8% (hereinafter this glass for
  • the present invention further provides the above glass for chemical tempering, which contains from 65 to 68% of SiO 2 , from 7 to 10% of Al 2 O 3 , and from 0 to 2.5% of K 2 O, wherein the total content of SiO 2 and Al 2 O 3 is from 73.5 to 76%.
  • the present invention further provides the above glass for chemical tempering, wherein the content of SiO 2 is at most 66%.
  • the present invention further provides the above glass for chemical tempering, which is to be used for obtaining glass, of which a compressive stress layer formed on the glass surface by chemical tempering has a thickness t of at least 30 ⁇ m and a surface compressive stress S of at least 550 MPa.
  • the present invention further provides the above glass for chemical tempering, wherein F1/F0 can be made to be at least 0.9, where F0 is a flexural strength of a chemically tempered glass plate which is obtained by chemically tempering a glass plate made of the glass for chemical tempering and having a thickness of 1 mm and a size of 5 mm ⁇ 40 mm and which has t of at least 30 ⁇ m and S of at least 550 MPa, and F1 is a flexural strength of such a chemically tempered glass plate having a Vickers indenter impressed thereinto with a force of 9.8N.
  • F0 is a flexural strength of a chemically tempered glass plate which is obtained by chemically tempering a glass plate made of the glass for chemical tempering and having a thickness of 1 mm and a size of 5 mm ⁇ 40 mm and which has t of at least 30 ⁇ m and S of at least 550 MPa
  • F1 is a flexural strength of such a chemically tempered glass
  • the present invention further provides the above glass for chemical tempering, wherein F2/F0 can be made to be at least 0.7, where F0 is a flexural strength of a chemically tempered glass plate which is obtained by chemically tempering a glass plate made of the glass for chemical tempering and having a thickness of 1 mm and a size of 5 mm ⁇ 40 mm and which has t of at least 30 ⁇ m and S of at least 550 MPa, and F2 is a flexural strength of such a chemically tempered glass plate having a Vickers indenter impressed thereinto with a force of 19.6N.
  • F0 is a flexural strength of a chemically tempered glass plate which is obtained by chemically tempering a glass plate made of the glass for chemical tempering and having a thickness of 1 mm and a size of 5 mm ⁇ 40 mm and which has t of at least 30 ⁇ m and S of at least 550 MPa
  • F2 is a flexural strength of such a chemically tempered glass
  • the present invention further provides chemically tempered glass, which is obtained by chemically tempering the above glass for chemical tempering.
  • the present invention further provides a chemically tempered glass plate which is a glass plate made of the above chemically tempered glass and having a thickness of from 0.4 to 1.2 mm, wherein F1/F0 is at least 0.9, where F0 is its flexural strength and F1 is a flexural strength of the glass plate having a Vickers indenter impressed thereinto with a force of 9.8N.
  • the present invention further provides a chemically tempered glass plate which is a glass plate made of the above chemically tempered glass and having a thickness of from 0.4 to 1.2 mm, wherein F2/F0 is at least 0.7, where F0 is its flexural strength and F2 is a flexural strength of the glass plate having a Vickers indenter impressed thereinto with a force of 19.6N.
  • the present invention further provides a glass plate for a display device, which is made of the above chemically tempered glass or the above chemically tempered glass plate.
  • the present invention further provides a display device, which has a cover glass comprising the above glass plate for a display device.
  • the present invention further provides the above display device, which is a mobile device, a touch panel or a flat screen television with a size of at least 20 inches.
  • the present inventors have found that SiO 2 and Al 2 O 3 in glass prevent lowering of the strength which takes place when an indentation is imparted to the glass even if the glass is chemically tempered, while ZrO 2 promotes lowering of the strength and that if it is attempted to reduce ZrO 2 in order to prevent lowering of the strength, the glass transition point Tg tends to decrease thus leading to such a problem that stress relaxation is likely to occur.
  • the strength of glass is less likely to be lowered even if indentations are imparted to chemically tempered glass during its use, whereby it is possible to obtain chemically tempered glass which is less likely to be broken even if a load such as a shock or static load is imparted to the glass, and glass for chemical tempering, which is suitable for such chemically tempered glass.
  • a display device for e.g. a mobile device, a touch panel, a flat screen television, etc., wherein such chemically tempered glass is used as a glass plate for the display device, such as a cover glass.
  • FIG. 1 is a graph showing the relation between R obtained by calculation from the glass composition and the decrease ratio r of the surface compressive stress due to an increase of the Na concentration in the molten potassium salt.
  • the chemically tempered glass, the chemically tempered glass plate and the glass plate for a display device of the present invention are each obtained by chemically tempering the glass for chemical tempering of the present invention (hereinafter referred to as the glass of the present invention), and hereinafter they will generally be referred to as the tempered glass of the present invention.
  • the above S of the tempered glass of the present invention is preferably at least 550 MPa, more preferably more than 700 MPa. Further, S is typically at most 1,200 MPa.
  • the above t of the tempered glass of the present invention is preferably at least 30 ⁇ m, more preferably exceeds 40 ⁇ m. Further, t is typically at most 70 ⁇ m.
  • the method of chemical tempering treatment to obtain the tempered glass of the present invention is not particularly limited so long as Na 2 O in the glass surface layer can be ion exchanged with K 2 O in the molten salt, and it may, for example, be a method of immersing the glass in a heated potassium nitrate (KNO 3 ) molten salt.
  • KNO 3 molten salt may be one which contains e.g. NaNO 3 in an amount of at most about 5%, in addition to KNO 3 .
  • Chemical tempering treatment conditions to form a chemically tempered layer (compressive stress layer) having a desired surface compressive stress on the glass may vary depending upon e.g. the thickness in the case of a glass plate. However, it is typical to immerse a glass substrate in a KNO 3 molten salt at from 350 to 550° C. for from 2 to 20 hours. From the economical viewpoint, the immersion is carried out preferably under conditions of from 350 to 500° C. and from 2 to 16 hours, and more preferably, the immersion time is from 2 to 10 hours.
  • a glass plate obtained by chemically tempering a glass plate made of the glass of the present invention and having a thickness of from 0.4 to 1.2 mm is preferably one wherein F1/F0 is at least 0.9, where F0 is its flexural strength and F1 is a flexural strength of the glass plate having a Vickers indenter impressed thereinto with a force of 9.8N. If F1/F0 is not at least 0.9, the glass tends to be readily broken when an indentation is formed on the surface of the glass plate with a force of 9.8N. More preferably, F1/F0 is at least 0.95.
  • a glass plate obtained by chemically tempering a glass plate made of the glass of the present invention and having a thickness of from 0.4 to 1.2 mm is preferably one wherein F2/F0 is at least 0.7, where F0 is its flexural strength and F2 is a flexural strength of the glass plate having a Vickers indenter impressed thereinto with a force of 19.6N. If F2/F0 is not at least 0.7, the glass tends to be readily broken when an indentation is formed on the surface of the glass plate with a force of 19.6N.
  • F2/F0 is more preferably at least 0.8, particularly preferably at least 0.9.
  • t is from 40 to 60 ⁇ m
  • S is from 650 to 820 MPa.
  • the glass plate for a display device of the present invention is usually obtained by chemically tempering a glass plate obtained by processing a glass plate made of the glass of the present invention by e.g. cutting, hole making, polishing, etc.
  • the thickness of the glass plate for a display device of the present invention is typically from 0.3 to 2 mm, usually from 0.4 to 1.2 mm.
  • the glass plate for a display device of the present invention is typically a cover glass.
  • a method for producing a glass plate made of the above glass of the present invention is not particularly limited, and for example, various raw materials are mixed in proper amounts, heated and melted at from about 1,400 to 1,700° C. and then homogenized by deforming, stirring or the like and formed into a plate by a well-known float process, downdraw method or press method, which is annealed and then cut into a desired size to obtain the glass plate.
  • the glass transition point Tg of the glass of the present invention is preferably at least 400° C. If it is lower than 400° C., the surface compressive stress is likely to be relaxed during the ion exchange, and no adequate stress may be obtained. It is typically at least 570° C., preferably at least 600° C.
  • the temperature T2 at which the viscosity of the glass of the present invention becomes 10 2 dPa ⁇ s is preferably at most 1,650° C. If T2 exceeds 1,650° C., melting of the glass tends to be difficult.
  • the temperature T4 at which the viscosity of the glass of the present invention becomes 10 4 dPa ⁇ s is preferably at most 1,250° C. If T4 exceeds 1,250° C., molding of the glass tends to be difficult.
  • the specific gravity d of the glass of the present invention is preferably at most 2.60, more preferably at most 2.55.
  • the glass of the present invention is preferably glass A.
  • the glass of the present invention is preferably glass B.
  • composition of the glass of the present invention will be described by using contents represented by mole percentage unless otherwise specified.
  • SiO 2 is a component to constitute a glass matrix and is essential. If the SiO 2 content is less than 62%, lowering of the strength tends to occur when an indentation is formed, cracking tends to occur when scratch is formed, the weather resistance tends to be low, the specific gravity tends to increase, or the glass tends to be unstable when the liquid phase temperature is raised. SiO 2 is preferably at least 63%, and in glass B, it is at least 64%, preferably at least 65%. If SiO 2 exceeds 68%, T2 or T4 tends to increase, whereby melting or molding of the glass tends to be difficult. SiO 2 is preferably at most 66%, more preferably at most 65.5%, and in glass A, it is at most 66%.
  • SiO 2 is typically from 63 to 65%, and the SiO 2 content as represented by mole percentage is typically less than 64%.
  • Al 2 O 3 is a component to improve the ion exchange performance and the weather resistance, and is essential. If it is less than 6%, lowering of the strength tends to occur when an indentation is formed, or it tends to be difficult to obtain the desired surface compressive stress S or compressive stress layer thickness t by ion exchange.
  • Al 2 O 3 is preferably at least 6.5%, more preferably at least 7%, particularly preferably at least 7.5%. If Al 2 O 3 exceeds 12%, T2 or T4 tends to increase, whereby melting or molding of the glass tends to be difficult, or the liquid phase temperature tends to be high to cause devitrification. It is preferably at most 11.5%, and in glass B, it is preferably at most 10%.
  • the total content of SiO 2 and Al 2 O 3 is preferably at least 71%. If the total content is less than 71%, lowering of the strength tends to occur when an indentation is formed, and it is typically more than 72%. In glass B, the total content is typically from 73.5 to 76%.
  • MgO is a component which may decrease the ion exchange rate, but it is a component to prevent cracking or to improve the melting property, and thus is essential. If MgO is less than 7%, T2 or T4 tends to increase, whereby melting or molding of the glass tends to be difficult, and it is preferably at least 7.5%, more preferably at least 8%. If MgO exceeds 13%, the liquid phase temperature tends to increase to cause devitrification, or lowering of the strength tends to occur when an indentation is formed, and it is preferably at most 12.5%, more preferably at most 12%. In glass B, it is at most 12%. In a case where it is desired to more certainly prevent lowering of the strength when an indentation is formed on the glass surface, MgO is typically from 8 to 11%.
  • Na 2 O is a component to form a surface compressive stress layer by ion exchange and to improve the melting property of the glass, and is essential. If the Na 2 O content is less than 9%, it tends to be difficult to form a desired surface compressive stress layer by ion exchange, and it is preferably at least 9.5%, more preferably at least 10%, particularly preferably at least 10.5%. In glass B, it is at least 12%. If Na 2 O exceeds 17%, the weather resistance tends to decrease, or cracking is likely to be formed from an indentation. It is preferably at most 16%.
  • the total content of Na 2 O and MgO is preferably from 21 to 25%. If the total content is less than 21%, T2 or T4 tends to increase, whereby melting or molding of the glass tends to be difficult. If the total content exceeds 25%, cracking tends to be formed from an indentation, or lowering of the strength tends to occur when an indentation is formed.
  • K 2 O is not essential but is a component to increase the ion exchange rate, and thus, it may be contained up to 7%. If K 2 O exceeds 7%, lowering of the strength tends to occur when an indentation is formed, or cracking tends to be formed from an indentation, and it is preferably at most 6.5%, more preferably at most 6%. In glass B, it is at most 6%, preferably at most 2.5%. When K 2 O is contained, its content is preferably at least 0.5%.
  • the total content of R 2 O i.e. Na 2 O and K 2 O is preferably at most 22%. If R 2 O exceeds 22%, the weather resistance tends to be low, or cracking tends to be formed from an indentation. It is preferably at most 21%, more preferably at most 20%, and in glass B, it is preferably at most 18%. Further, R 2 O is preferably at least 14%, typically at least 15%.
  • the total content of Na 2 O, K 2 O and MgO is preferably from 24 to 28%. If the total content is less than 24%, T2 or T4 tends to increase, whereby melting or molding of the glass tends to be difficult, and if it exceeds 28%, cracking tends to be formed from an indentation, or lowering of the strength tends to occur when an indentation is formed. It is typically at most 27%.
  • Na 2 O is from 11 to 16% or from 12 to 16%
  • K 2 O is from 0 to 5%
  • R 2 O is from 15 to 17%
  • Na 2 O is typically from 13.5 to 16%.
  • the difference (R 2 O ⁇ Al 2 O 3 ) obtained by subtracting Al 2 O 3 from R 2 O is preferably less than 10%. If said difference is at least 10%, Tg tends to be low, or stress relaxation tends to occur during the chemical tempering.
  • ZrO 2 is not essential, but may be contained within a range of up to 0.8% in order to lower the viscosity at a high temperature or to increase the surface compressive stress. If ZrO 2 exceeds 0.8%, lowering of the strength tends to occur, or chipping is likely to occur. It is preferably at most 0.7%, more preferably at most 0.6%, particularly preferably at most 0.55%, and in glass B, it is preferably at most 0.5%.
  • the glass of the present invention is preferably one wherein R calculated by the following formula by using the contents of the respective components of SiO 2 , Al 2 O 3 , MgO, CaO, ZrO 2 , Na 2 O and K 2 O is at least 0.66:
  • R 0.029 ⁇ SiO 2 +0.021 ⁇ Al 2 O 3 +0.016 ⁇ MgO ⁇ 0.004 ⁇ CaO+0.016 ⁇ ZrO 2 +0.029 ⁇ Na 2 O+0 ⁇ K 2 O ⁇ 2.002
  • the ion exchange treatment for chemical tempering is carried out by immersing glass containing sodium (Na) in a molten potassium salt, and as the potassium salt, potassium nitrate or a mixed salt of potassium nitrate and sodium nitrate is used.
  • the present inventors have considered that there may be a relation between the composition of Na-containing glass and such a phenomenon that by repeating ion exchange treatment of immersing the Na-containing glass in a molten potassium salt many times to obtain chemically tempered glass, the Na concentration in the molten potassium salt increases and at the same time, the surface compressive stress of the chemically tempered glass becomes small, and have conducted the following experiment.
  • glass plates were subjected to ion exchange of immersing for 10 hours in a molten potassium salt having a KNO 3 content of 100% and having a temperature of 400° C. to obtain chemically tempered glass plates, whereupon their surface compressive stresses CS1 (unit: MPa) were measured.
  • glass A27 is glass used for a cover glass for a mobile device.
  • these 29 types of glass plates were subjected to ion exchange of immersing for 10 hours in a molten potassium salt having a KNO 3 content of 95% and a NaNO 3 content of 5% and having a temperature of 400° C. to obtain chemically tempered glass plates, whereupon their surface compressive stresses CS2 (unit: MPa) were measured.
  • r of conventional cover glass A27 is 0.65.
  • the correlation coefficient is 0.97.
  • R is at least 0.66
  • the above r can be made to be at least 0.66 and as a result, it is possible to ease controls of the Na concentration in the molten salt as compared with conventional one, or it is possible to reduce the frequency of replacement of the molten salt.
  • R is preferably at least 0.68.
  • the glass of the present invention essentially comprises the above-described components, but may contain other components within a range not to impair the object of the present invention.
  • the total content of such components is preferably at most 5%, typically at most 3%.
  • the total content of SiO 2 , Al 2 O 3 , MgO, Na 2 O and K 2 O is particularly preferably at least 98%. Now, such other components will be exemplified.
  • CaO, SrO and BaO may be contained in order to improve the melting property at a high temperature or to prevent devitrification, but they may lower the ion exchange rate or resistance against cracking.
  • the content of each component is preferably at most 1%, more preferably at most 0.5%. Further, in such a case, the total content of these three components is preferably at most 1%, more preferably at most 0.5%.
  • ZnO may be contained in a certain case, in order to improve the melting property of glass at a high temperature, but its content in such a case is preferably at most 1%. In a case of production by a float process, ZnO is preferably at most 0.5%. If ZnO exceeds 0.5%, it is likely to be reduced during the float forming to form a product defect. Typically no ZnO is contained.
  • B 2 O 3 may be contained within a range of e.g. less than 1% in some cases, in order to improve the melting property of glass at a high temperature. If B 2 O 3 is at least 1%, homogeneous glass tends to be hardly obtainable, and the glass forming may be difficult, or the chipping resistance may deteriorate. Typically no B 2 O 3 is contained.
  • TiO 2 is likely to deteriorate the visible light transmittance and to color glass to be brown when it is coexistent with Fe ions in the glass, and therefore, its content is preferably at most 1% if contained, and typically, it is not contained.
  • Li 2 O is a component to lower the strain point and to bring about a stress relaxation thereby to make it difficult to stably obtain a surface compressive stress layer and therefore it is preferably not contained, and even if contained, its content is preferably less than 1%, more preferably at most 0.05%, particularly preferably less than 0.01%.
  • SO 3 As a clarifying agent at the time of melting glass, SO 3 , a chloride, a fluoride or the like may suitably be contained.
  • components which may be included as impurities in raw materials such as Fe 2 O 3 , NiO, Cr 2 O 3 , etc. having an absorption in a visible light range as far as possible, and the content of each of them is preferably at most 0.15%, more preferably at most 0.1%, particularly preferably at most 0.05%, as represented by mass percentage.
  • R 2 O ⁇ Al 2 O 3 is less than 10%, and also in the case of the following glass C, the object of the present invention can be accomplished, and yet, the above-mentioned r can be made large.
  • the description relating to the glass of the present invention is applicable as it is, except for R 2 O ⁇ Al 2 O 3 being less than 10%, and in glass C, it is preferred that R 2 O ⁇ Al 2 O 3 is made to be less than 10%.
  • Glass C Glass for chemical tempering, which comprises, as represented by mole percentage based on oxides, from 63 to 66% of SiO 2 , from 7 to 10% of Al 2 O 3 , from 8 to 12% of MgO, from 12 to 17% of Na 2 O, and from 0 to 3% of K 2 O, wherein when ZrO 2 is contained, its content is at most 0.5%, and wherein R calculated by the following formula by using the contents of the respective components of SiO 2 , Al 2 O 3 , MgO, CaO, ZrO 2 , Na 2 O and K 2 O is at least 0.66:
  • R 0.029 ⁇ SiO 2 +0.021 ⁇ Al 2 O 3 +0.016 ⁇ MgO ⁇ 0.004 ⁇ CaO+0.016 ⁇ ZrO 2 +0.029 ⁇ Na 2 O+0 ⁇ K 2 O ⁇ 2.002
  • Ex. 1 to 9 are Working Examples of the present invention and Ex. 10 to 20 are Comparative Examples.
  • glass in Ex. 11 is similar to Example 19 in the above-mentioned Patent Document 2, and glasses in Ex. 20, 13 and 21 are, respectively, the same as Example 1, Example 14 and Comparative Example 54 in the same Document.
  • the glass compositions in Tables 4 to 6 are compositions as represented by mole percentage, while in Tables 7 to 9, compositions as represented by mass percentage of glasses in Ex. 1 to 21 are shown.
  • the specific gravity d the average linear expansion coefficient ⁇ (unit: ⁇ 7 /° C.), the glass transition point Tg (unit: ° C.), the temperature T2 (unit: ° C.) at which the viscosity becomes to be 10 2 dPa ⁇ s, and the temperature T4 (unit: ° C.) at which the viscosity becomes to be 10 4 dPa ⁇ s, are shown in Tables. Measurements thereof were carried out as follows.
  • Tg By means of a differential dilatometer and using quartz glass as a reference sample, the expansion rate of glass at the time of raising the temperature from room temperature at a rate of 5° C./min, was measured to the yield point, whereby in the thermal expansion curve thereby obtained, a temperature corresponding to a folding point was taken as the glass transition point.
  • T2, T4 Measured by a rotational viscometer.
  • both surfaces of each glass plate having a thickness of 1 mm and a size of 5 mm ⁇ 40 mm obtained as described above in Ex. 1 to 8 and 10 to 14, was mirror-polished with cerium oxide and then subjected to the following chemical tempering treatment. That is, such a glass plate was immersed in a molten potassium salt at 450° C. for 270 minutes in Ex. 1, 2 or 7, for 120 minutes in Ex. 3, for 300 minutes in Ex. 4, 180 minutes in Ex. 5, for 320 minutes in Ex. 6, for 210 minutes in Ex. 8, for 195 minutes in Ex. 10, for 330 minutes in Ex. 11, for 300 minutes in Ex. 12, for 450 minutes in Ex. 13, or for 1380 minutes in Ex. 14, for tempering treatment to obtain a chemically tempered glass plate.
  • a molten potassium salt at 450° C. for 270 minutes in Ex. 1, 2 or 7, for 120 minutes in Ex. 3, for 300 minutes in Ex. 4, 180 minutes in Ex. 5, for 320 minutes in Ex. 6, for 210 minutes in Ex. 8, for 195
  • the KNO 3 content was from 95 to 100%, and the NaNO 3 content was from 0 to 5%.
  • the specific KNO 3 content was 99% in Ex. 1, 2 or 11, 100% in Ex. 3, 10 or 13, 95% in Ex. 4, 5 or 14, 99.3% in Ex. 6, 97% in Ex. 7 or 8, or 99.5% in Ex. 12.
  • the flexural strength was measured, and an average value F0 (unit: MPa) of flexural strength was obtained.
  • F0 unit: MPa
  • the accuracy of flexural strength measurement was ⁇ 30 MPa
  • the measurement of the flexural strength was carried out by a three point flexural test under conditions of a span of 30 mm and a crosshead speed of 0.5 mm/min.
  • F1 is lower than F0, while with those obtained by chemically tempering glasses in Ex. 1 to 8, F1 has the same or substantially the same value as F0. Further, with those obtained by chemically tempering glasses in Ex. 1 to 8, the difference between F0 and F2 is smaller as compared with those obtained by chemically tempering glasses in Ex. 11 to 14. With those obtained by chemically tempering glasses in Ex. 4 and 8, F2 is also the same or substantially the same as F0, which shows that the advantageous effects of the present invention are particularly high. Further, with one obtained by chemically tempering glass in Ex. 10, F1 has substantially the same value as F0, but Tg is low.
  • the present invention is useful for e.g. a cover glass for a display device. Further, it is useful also for e.g. a solar cell substrate or a window glass for aircrafts.

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CN103097315B (zh) 2015-10-14
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US10370286B2 (en) 2019-08-06
WO2012043482A1 (ja) 2012-04-05
JP5672405B2 (ja) 2015-02-18
US20150126354A1 (en) 2015-05-07
TWI534114B (zh) 2016-05-21
CN104609724A (zh) 2015-05-13
JPWO2012043482A1 (ja) 2014-02-06
CN103097315A (zh) 2013-05-08
JP5796581B2 (ja) 2015-10-21
CN105110636A (zh) 2015-12-02
JP2015024955A (ja) 2015-02-05
KR101790483B1 (ko) 2017-10-25

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