WO2020011167A1 - Verre d'aluminosilicate contenant du lithium pouvant subir un échange d'ions rapide - Google Patents

Verre d'aluminosilicate contenant du lithium pouvant subir un échange d'ions rapide Download PDF

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Publication number
WO2020011167A1
WO2020011167A1 PCT/CN2019/095289 CN2019095289W WO2020011167A1 WO 2020011167 A1 WO2020011167 A1 WO 2020011167A1 CN 2019095289 W CN2019095289 W CN 2019095289W WO 2020011167 A1 WO2020011167 A1 WO 2020011167A1
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WO
WIPO (PCT)
Prior art keywords
glass
lithium
containing aluminosilicate
ion exchange
aluminosilicate glass
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PCT/CN2019/095289
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English (en)
Chinese (zh)
Inventor
梁新辉
陈招娣
罗云侠
何石忠
林美灵
洪立昕
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科立视材料科技有限公司
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Publication of WO2020011167A1 publication Critical patent/WO2020011167A1/fr

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Classifications

    • 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
    • C03C3/097—Glass compositions containing silica with 40% to 90% silica, by weight containing phosphorus, niobium or tantalum
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B27/00—Tempering or quenching glass products
    • C03B27/02—Tempering or quenching glass products using liquid
    • C03B27/03—Tempering or quenching glass products using liquid the liquid being a molten metal or a molten salt
    • 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 belongs to the field of glass materials, and particularly relates to a lithium-containing aluminosilicate glass capable of quickly performing ion exchange.
  • aluminosilicate glass material is strengthened by ion exchange, it is widely used in protective cover products of electronic display products. Therefore, higher requirements are imposed on the mechanical properties of aluminosilicate glass, which makes aluminosilicate acid Salt glass must have a higher surface compressive stress (CS) and a deeper surface compressive stress layer depth (DOL).
  • CS surface compressive stress
  • DOL surface compressive stress layer depth
  • the strengthening of aluminosilicate glass generally uses ions with a smaller ionic radius on the glass surface (such as Na + fPLi + ) and ions in the molten salt (such as K + and Na + ) to replace each other, where Li + has With smaller ionic radii, exchange speed and exchange depth are better than Na + exchange. 5 See the prior art that many strengthenable aluminosilicate glasses are disclosed.
  • Patent CN102971267A provide an ion-exchanged glass, which does not contain lithium, and containing 0.1 to 10 mol% of 205 mol% and at least 5 eight 1203.
  • the presence of 2 0 5 enables the glass to perform ion exchange faster and to a greater depth than equivalent glass without P 2 0 5 .
  • this glass material compared with lithium-containing glass, it is difficult for this glass material to obtain a higher compression layer depth in a short time.
  • Patent CN105683106A provides an ion-exchangeable glass containing boron and phosphorus, and an ion-exchangeable glass containing Si0 2 , A1 2 0 3 , Na 2 0, MgO, B 2 0 3, and P 2 0 5 .
  • These ion-exchanged glasses have a compressive stress greater than 900 megapascals (MPa) at a depth of 45 or 50 microns (side), and some glass exhibit a compressive stress of at least 1 gigapascal (GPa).
  • MPa megapascals
  • GPa gigapascal
  • the ion exchange rate of these glasses is much faster than in the case of other alkaline aluminosilicate glasses, and the ion exchanged glass is resistant to damage by impact damage.
  • the glass contains a sufficient amount of B 2 0 3 and does not contain Li 2 0, so the improvement of the glass compressive stress layer is limited.
  • Patent CN103648996A provides an aluminosilicate glass article having a high compressive stress layer.
  • Said Glass articles include at least about 50 mol% SiO 2 and at least about 11 mol% Na 2
  • the glass contains a higher concentration of Na 2
  • Patent CN107531563A provides a strengthened glass, which is a strengthened glass having a thickness of 0.6 mm or less and a chemically strengthened compressive stress layer on the surface. But Li 2 in glass
  • the 0 concentration is less than 2wt%, so the depth of the compression stress layer is limited.
  • Patent US20170197869A1 provides a strengthened glass, but the glass contains a sufficiently high B 2 0 3 component, which will cause a reduction in surface compressive stress, and inhibit ion exchange in the glass, and it is difficult to quickly obtain a high ion exchange layer depth .
  • the present invention provides an aluminosilicate glass having a high compressive stress and a high compressive stress layer.
  • An object of the present invention is to provide a lithium-containing aluminosilicate glass capable of quickly performing ion exchange in view of the shortcomings of the prior art.
  • the lithium-containing aluminosilicate glass that can be quickly ion-exchanged has a composition in terms of mole percentage and contains 60 to 66% SiO 2 , 12 to 18% A1 2 0 3 , 4 to 6%.
  • the MgO concentration is not less than 3 mol%.
  • the concentration of B 2 0 3 is not higher than 0.1 mol%.
  • 0 concentration is not higher than 0.1 mol%.
  • the lithium-containing aluminosilicate glass that can be quickly ion-exchanged has a strain point temperature greater than 550 ° C; and a Vickers hardness greater than 600MPa.
  • the lithium-containing aluminosilicate glass capable of performing ion exchange quickly has a compressive stress layer depth of at least 5 (Vm.
  • the lithium-containing aluminosilicate glass that can be quickly ion-exchanged has a compressive stress region with a compressive stress of at least
  • the lithium-containing aluminosilicate glass provided by the present invention does not contain boron and potassium components (contents of which are not higher than 0.1 mol%) that rapidly reduce the compressive stress of the glass ion exchange surface area, and by introducing an appropriate amount of Divalent cationic oxides and monovalent cationic alkali metal oxides with low levels are controlled to obtain glasses with a high Vickers hardness value.
  • the low temperature characteristics of lithium-containing aluminosilicate glass can be improved, which can reduce the stress relaxation during glass ion exchange. Therefore, a high surface compressive stress is obtained; in addition, an appropriate amount of a divalent cationic oxide can improve the ability of the glass to resist external damage and high crack resistance.
  • the SiO 2 in the glass of the present invention is mainly a glass forming body, and one of the necessary components constitutes a glass mesh-like main structure.
  • the glass contains 310 2 with a concentration of 58 ⁇ 68 mol%, and a sufficient amount of SiO j Wuyu glass has better chemical stability, mechanical properties and molding properties.
  • Si0 2 will increase the melting temperature too high, especially under the condition of high concentration of alumina in the glass, the concentration of Si0 2 should be controlled below 68 mol%, preferably below 66 mol%, more preferably below 64 Mol%; too low SiO 2 concentration in the glass will lead to deterioration of the aging resistance and surface mechanical properties of the glass, increasing the chance of scratching the ultra-thin glass during cold processing and cleaning. Therefore, the SiO 2 concentration should be controlled higher than about 58 mol%, preferably higher than about 60 mol%, and more preferably higher than about 62 mol%.
  • A1 2 0 3 glass is one of the essential components are an integral, high alkali concentration in the glass composition, the majority of the alumina tend to be glass network tetrahedral intermediate aluminoxane constituting the glass network Main structure, which improves glass stability and mechanical properties.
  • A1 2 0 3 Alumino-tetrahedron formed in glass in glass The volume is larger than the volume of the silicon tetrahedron, and the volume of the glass expands, which reduces the density of the glass.
  • A1 2 0 3 belongs to extremely refractory oxide, which can rapidly increase the viscosity of the glass, which makes it more difficult to clarify and homogenize the glass.
  • the number of bubbles and defects of molybdenum and rhodium in the glass will increase sharply.
  • the concentration causes the glass liquidus temperature to increase rapidly, making it difficult to form. Therefore, the concentration of A1 2 0 3 in the glass is about 12 mol% to 18 mol%, preferably about 12 mol% to 17 mol%.
  • Li 2 0 in the glass of the present invention is one of the ion-exchange components.
  • the present invention proves through a large number of experiments that lithium-containing glass can be exchanged by Li + and Na + in the glass at a suitable temperature at a suitable temperature. Get high compressive stress layer depth.
  • Li 2 0 glass viscosity characteristics make rapid decline, in particular to reduce significantly the high temperature viscosity, facilitate melting and refining glass, offers the possibility to A1 2 0 3 concentration of the high concentration of glass, the present invention is not low concentration of Li 2 0 At a concentration of about 4 mol%, if the concentration is lower than 4 mol%, the exchange amount of Li + and Na + in the glass is insufficient, and it is difficult to obtain a high compressive stress layer depth; but for high concentration Li 2 0 concentration glass, its liquidus temperature varies with the glass The viscosity decreases, so that the glass becomes easily devitrified.
  • the 0 concentration is less than about 8 mol%, preferably about 4 to 6 mol%.
  • Na 2 0 in the glass is one of the essential components, which provides a large amount of free oxygen source, which destroys the glass silicon oxygen network structure, greatly reduces the viscosity of the glass, and helps the glass to melt and clarify.
  • the higher concentration of Na 2 0 provides the possibility for chemical strengthening of glass. Therefore, the Na 2 0 concentration in the present invention is not less than about 7 mol%
  • the Na 2 0 concentration in the glass is preferably less than about 11 mol%.
  • the high compressive stress layer in the present invention is mainly formed by Li + and Na exchange.
  • the glass of the present invention ⁇ 2 0 concentration Below 0.1 mol%, it is mainly introduced by the impurity concentration of the raw material.
  • Concentration ratio control is less than or equal to 1.2, too high R 2 0 / A1 2 0 3 concentration ratio reduces glass strain point temperature and surface Vickers hardness, it is difficult to reach strain point temperature 550 ° C or higher and Vickers hardness before strengthening is 6 or higher
  • the component B 2 0 3 is a network-forming body oxide, which can significantly reduce the strain point temperature of the glass, and there is an oxide volatilization phenomenon during high-temperature melting, which is not conducive to the stability of the glass component.
  • B 2 0 3 is not conducive to high compressive stress and high stress layer depth of the glass. Therefore, in the present invention, the concentration of 2 3 is less than 0.1 mol%, and the concentration of B 2 0 3 is preferably 0. Mol%.
  • P 2 0 5 is a glass forming body component, which is interconnected by a [PO 4 ] tetrahedron to form a network, but the network structure formed by P 2 0 5 is layered, and the layers are connected to each other by Van der Waals force. Therefore, P 2 0 5 in glass has the effects of low viscosity, poor chemical stability and large thermal expansion coefficient.
  • P 2 0 5 concentration to promote glass strengthening process from the ion exchange, the rapid stress layer plays an important role to obtain higher compression. Therefore, in the present invention, the concentration of P 2 0 5 is limited to 1 mol% to 4 mol%, and the concentration of P 2 0 5 is preferably 1.5 mol% to 3.5 mol%.
  • the glass of the present invention contains a divalent cationic oxide, which is an outer body component of the glass network, which destroys the integrity of the glass structure and reduces the melting temperature of the glass. It is a good flux to facilitate clarification, but at the same time improves the glass's
  • the linear thermal expansion coefficient value reduces the temperature of the strain point of the glass, while improving the glass elastic modulus and mechanical properties.
  • Divalent cation oxides have advantages in increasing the compressive stress on the glass surface. Experiments in the present invention show that ZnO and SrO in glass have the same effect on improving the compressive stress on the glass surface as MgO. It is especially important that ZnO strengthens the glass strengthening performance. The depth of the stress layer has an improvement effect.
  • the MgO concentration in the glass of the present invention is about 0.1 mol% to 8 mol%, and the MgO concentration is preferably 3 mol% to 8 mol%.
  • the ZnO concentration in the glass is about 0 mol% to 3 mol%, but an excessively high ZnO concentration in the glass will cause a significant increase in the crystallization tendency of the glass. Therefore, the ZnO concentration is preferably about 0.5 mol% to 2 mol%.
  • the SrO concentration in the glass of the present invention is about 0 mol% to 3 mol%, and the SrO concentration is preferably about 0 mol% to 2 mol%.
  • the content of the divalent cation oxide RO is controlled between 2.5 mol% to 11 mol%. If the concentration is higher than 11 mol%, the high divalent cation oxide concentration in the glass will significantly increase the efficiency of hindering ion exchange. And the increase of the liquidus temperature of the glass is not conducive to the production process; if the concentration is lower than 2.4 mol%, the glass will stick. The degree is too high, preferably 4 to 7 mol%.
  • compressive stress and a compressive stress layer are generated on the surface of the glass by ion exchange between small ions in the glass and large ions in the molten salt, and the compressive stress layer is formed by lithium ion exchange with sodium ion and sodium Ions are exchanged with potassium ions.
  • the ion exchange process of the glass is described as follows: the annealed glass block is prepared into a glass sheet with a thickness of about 0.7 mm, and the glass sheet is cleaned with ultrasonic waves for standby; the glass sheet is pre-heated at 250 ° C to 300 ° C, and the glass product is soaked In 380 ° C ⁇ 430 ° C molten salt, the molten salt contains more than 20% sodium nitrate molten salt of sodium nitrate, soaking time is about 20 ⁇ 120 minutes, and the glass flakes are taken out and soaked in 380 ⁇ 410 ° C In the molten salt, the molten salt contains less than 20% sodium nitrate potassium salt molten salt, and the immersion time is 10 to 90 minutes; the glass is taken out of the surface to be tested for molten salt treatment.
  • a compressive stress and a compressive stress layer are formed on the surface of the glass sheet. As shown in FIG. 1, a compressive stress and a compressive stress layer are formed on the surface of the glass sheet. As shown in FIG. 1, a compressive stress and a compressive stress layer are formed on the surface of the glass sheet. As shown in FIG. 1, a compressive stress and a compressive stress layer are formed on the surface of the glass sheet. As shown in FIG. 1, a compressive stress and a compressive stress layer are formed on the surface of the glass sheet.
  • the glass of the present invention phosphorus (P 2 0 5 concentration limits in mole% 1 ⁇ 4 mole%), a high ion exchange can be implemented quickly by the introduction of lithium (Li 2 0 concentration of not less than about 4 mol%) and The depth of the layer, thereby improving the scratch resistance of the glass, so that the glass has a high compressive stress and compressive stress layer;
  • the glass of the present invention is optimized by optimizing the monovalent cationic oxide (R 2 0 / A1 2 0 3 concentration ratio is less than or equal to 1.2
  • divalent cation oxide (RO content is controlled to 2.5 mol% ⁇ 11 mol%), so that the glass has a high Vickers hardness value.
  • FIG. 1 is a surface compressive stress distribution diagram of glass after ion exchange; after ion exchange of glass of thickness t, a sodium-potassium exchange layer is formed on the glass surface, that is, a surface compressive stress layer CS1, an ion-exchange layer DOL1, and lithium-sodium exchange
  • the layer is a surface compressive stress layer CS2, an ion exchange layer DOL2, and forms a central tensile stress (Central Tensile Stress, CT for short) in the glass.
  • a sodium-potassium exchange layer is formed on the glass surface, that is, a surface compressive stress layer CS1, an ion-exchange layer DOL1, and lithium-sodium exchange
  • the layer is a surface compressive stress layer CS2, an ion exchange layer DOL2, and forms a central tensile stress (Central Tensile Stress, CT for short) in the glass.
  • CT Central Tensile Stress
  • Table 2 is a formula No. 2 in Table 1 according to the purity and moisture content of each raw material to prepare a batch; the raw material composition shown in Table 1 is weighed and mixed to obtain uniform ingredients; and Transfer the batch from a plastic bottle to about 800 ml of molybdenum crucible, place the molybdenum crucible in a silicon molybdenum rod high temperature furnace, gradually raise the temperature to 1650 ° C, and maintain the temperature for 3 to 8 hours. The glass bubbles are discharged and stirred by stirring. Glass homogenization is eliminated.
  • the molten liquid is poured into a heat-resistant stainless steel mold for molding, then the glass block is taken out and moved into a box annealing furnace for a heat treatment at 600 ° C for about 2 hours, and then reduced to a rate of less than 1 ° C / min. 550 ° C, and then naturally cooled to room temperature.
  • chemical-grade compound raw materials should be selected.
  • Liquidus temperature that is, the maximum temperature of devitrification of glass in a temperature difference furnace is used to indicate that the duration of the devitrification process is usually 24 hours;
  • Softening point temperature The viscosity of the glass is a softening point temperature of 10 % poise, measured according to ASTM C-338 fiber elongation detection method;
  • D annealing point temperature the temperature of the glass viscosity of 10 13 poise, measured according to ASTM C-336 fiber elongation detection method
  • E. Strain point temperature The temperature at which the glass viscosity is 10 ⁇ poise, measured according to ASTM C-336 fiber elongation detection method;
  • F. CS1, DOL1 are CS1, DOL1 of the glass after optical ion exchange using FSM-6000LE surface stress meter to test the glass using optical waveguide technology;
  • G. CS2, DOL2 are glass ion exchange using the SLP-1000 surface stress meter using scattered light elasticity technology to test CS2, DOL2 values;
  • H. Vickers hardness TMVP-1S Vickers hardness tester is used to test the un-reinforced and strengthened glass surface Vickers. Hardness value, the test conditions are: an applied force of 200 g and an application time of 15 s.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Ceramic Engineering (AREA)
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  • Thermal Sciences (AREA)
  • Glass Compositions (AREA)

Abstract

L'invention concerne un verre d'aluminosilicate contenant du lithium pouvant subir un échange d'ions rapide. Les compositions du verre comprennent, en pourcentages molaires, 58 à 68 % de SiO2, 12 à 18 % d'Al2O 3, 4 à 8 % de Li 2O, 7 à 11 % de Na2O, 0,1 à 8 % de MgO, 0 à 3 % de ZnO, 0 à 2 % de SrO, 1 à 4 % de P2O 5 et 0 à 5 % de SnO 2, où R 2O/Al 2O 3 ≤ 1,2, 2,5 ≤ RO ≤ 11, RO étant la somme des oxydes cationiques divalents dans le verre d'aluminosilicate contenant du lithium, et R 2O étant la somme des oxydes cationiques monovalents dans le verre d'aluminosilicate contenant du lithium. En introduisant des constituants de lithium et de phosphore dans la composition de verre, et en régulant raisonnablement la teneur en sodium dans le verre, une profondeur de couche d'échange d'ions élevée peut être rapidement réalisée, ce qui permet d'améliorer la capacité de résistance aux rayures du verre.
PCT/CN2019/095289 2018-07-13 2019-07-09 Verre d'aluminosilicate contenant du lithium pouvant subir un échange d'ions rapide WO2020011167A1 (fr)

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CN201810766723.0A CN108585481A (zh) 2018-07-13 2018-07-13 一种可快速进行离子交换的含锂铝硅酸盐玻璃
CN201810766723.0 2018-07-13

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CN109279787A (zh) * 2018-11-22 2019-01-29 科立视材料科技有限公司 一种可快速离子交换的高铝玻璃
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CN110563337A (zh) * 2019-09-09 2019-12-13 深圳精匠云创科技有限公司 一种锂铝硅酸盐纳米晶玻璃陶瓷的强化方法
CN113480157A (zh) * 2021-08-17 2021-10-08 京东方杰恩特喜科技有限公司 钢化玻璃及其制备方法
CN114380496B (zh) * 2021-12-31 2023-10-24 河北光兴半导体技术有限公司 玻璃组合物、碱性锂铝硅酸盐玻璃及其应用
CN114394745B (zh) * 2022-01-07 2024-02-20 彩虹集团（邵阳）特种玻璃有限公司 铝硅酸盐玻璃及其制备方法和盖板玻璃
CN117800594A (zh) * 2023-06-28 2024-04-02 湖南旗滨新材料有限公司 锂铝硅酸盐玻璃组合物、锂铝硅酸盐强化玻璃及制备方法

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