WO2016154901A1 - Composition de verre pour du verre d'aluminoborosilicate alcalin chimiquement renforcé à faible constante diélectrique - Google Patents

Composition de verre pour du verre d'aluminoborosilicate alcalin chimiquement renforcé à faible constante diélectrique Download PDF

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Publication number
WO2016154901A1
WO2016154901A1 PCT/CN2015/075528 CN2015075528W WO2016154901A1 WO 2016154901 A1 WO2016154901 A1 WO 2016154901A1 CN 2015075528 W CN2015075528 W CN 2015075528W WO 2016154901 A1 WO2016154901 A1 WO 2016154901A1
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WIPO (PCT)
Prior art keywords
glass
chemically strengthened
compressive stress
aluminoborosilicate
strengthened alkali
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PCT/CN2015/075528
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English (en)
Inventor
Jack Y. DING
Cherry Chen
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Kornerstone Materials Technology Company, Ltd.
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Priority to PCT/CN2015/075528 priority Critical patent/WO2016154901A1/fr
Priority to CN201580077196.7A priority patent/CN107531550A/zh
Priority to TW105110011A priority patent/TWI677481B/zh
Publication of WO2016154901A1 publication Critical patent/WO2016154901A1/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
    • 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
    • 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 glass composition for chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant, a method for manufacturing the chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constantand applications and uses for the chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant.
  • Chemically strengthened glass is typically significantly stronger than annealed glass due to the glass composition and the chemical strengthening process used to manufacture the glass. Such chemical strengthening processes can be used to strengthen glass of all sizes and shapes without creating optical distortion which enables the production of thin, small, and complex-shaped glass samples that are not capable of being tempered thermally. These properties have made chemically strengthened glass, and more specifically, chemically strengthened alkali-aluminosilicate glass, a popular and widely used choice for consumer mobile electronic devices such as smart phones, tablets and notepads.
  • the chemical strengthening processes typically include an ion exchange process.
  • the glass is placed in a molten salt containing ions having a larger ionic radius than the ions present in the glass, such that the smaller ions present in the glass are replaced by larger ions from the heated solution.
  • potassium ions in the molten salt replace smaller sodium ions present in the glass.
  • the replacement of the smaller sodiumions present in the glass by larger potassium ions from the heated solution results in the formation of a compressive stress layer on both surfaces of the glass and a central tension zone sandwiched between the compressive stress layers.
  • CT tensile stress
  • CS compressive stress
  • DOL depth of the compressive stesss layer
  • CT CS ⁇ DOL/ (t-2DOL)
  • cover glass it is desirable for cover glass to be as thin as possible.
  • CS/DOL ratio of compressive stress to depth of layer
  • the dielectric constant of glass can affect sensitivity, response time, electrical power consumption rate, as well as analog signal misjudgment rate of a touch device, resulting in a slow reaction.
  • the lower the dielectric constant the better the sensitivity, response time, power consumption rate, and accuracy.
  • the current dielectric constant of commercialized, chemically strengthened alumino-silicate glass is between 7.1-7.8 (measured at a frequency of 1 MHz) .
  • the proportion of glass forming materials is relatively low and the proportion of ionic compoundswith conductivity is relatively high compared to non-alkali alumino-silicate glass, such as thin-film transistor liquid-crystal display glass (TFT-LCD glass) .
  • TFT-LCD glass is non-alkali-aluminoborosilicate glass with a dielectric constant of about 5.2 to about 6.0.
  • the mechanical and physical properties that provide chemical strength should also be maintained while developing glass components with low dielectric constants.
  • a glass with high strength and low dielectric constant is desired.
  • the present invention provides an ion exchangeable glass composition for producing chemically strengthened alkali-aluminoborosilicate glass having a low dielectric constant and high strength.
  • the compositions have higher contents of boron oxide and good melting performance, which enables glass sheet forming in the overflow down-draw process.
  • the compositions have a high content of sodium oxide which makes the compositions suitable for the ion exchange process.
  • a silica-alumina-sodium oxide glass is provided that is easy to melt.
  • the dielectric constant of glass can be effectively improved.
  • the glass forming materials are mainly silica, boron oxide, phosphorous oxide, and beryllium oxide.
  • Beryllium oxide is toxic, and has been banned from consumer electronic products.
  • Phosphorous oxide is not suitable for the overflow down-draw process since it causes corrosion damage to precious metal equipment.
  • the boron oxide in TFT-LCG glass substrate can reach 6 to 11 weight percent. Currently, however, boron oxide is seldom used, or controlled to under 2 weight percent in chemically strengthened cover glass.
  • the present invention provides a chemically strengthened alkali-aluminoborosilicate glass composition with a low dielectric constant and an increased boron oxide content.
  • the dielectric constant is less thanabout 6.0, which is lower than the dielectric constant of currently commercialized alumino-silicate glass for touch displays.
  • the dielectric constant of the glass can be lowered by increasing the content of silica and boron oxide in the glass and decreasing the proportion of ionic compounds for conductivity, such as sodium oxide, potassium oxide, magnesia and calcium oxide.
  • the proportions of the different glass components affect the properties of the glass.
  • the appropriate proportion of aluminum oxide and sodium oxide are added.
  • appropriate amounts of magnesium oxide can be added. Compared to increasing the proportion of metallic oxides such as calcium oxide, potassium oxide, and zinc oxide, increasing magnesium oxide is a good choice since it can lower the specific weight of the glass and increase the strength of the glass.
  • the ion exchangeable glass compositionfor producing chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant includes:
  • the ion exchangeable glass compositionfor producing chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant includes from about 60.0 to about 70.0 mol%of silicon dioxide (SiO 2 ) .
  • Silicon dioxide is the largest single component of the alkali-aluminoborosilicate glass and together with boron trioxide forms the matrix of the glass. Silicon dioxide also serves as a structural coordinator of the glass and contributes formability, rigidity and chemical durability to the glass.
  • silicon dioxide raises the melting temperature of the glass composition such that the molten glass becomes very difficult to handle, which may result in difficulty forming the glass.
  • silicon dioxide detrimentally tends to cause the liquidus temperature of the glass to substantially increase, especially in glass compositions having a high concentration of sodium oxide or magnesium oxide, and also tends to cause devitrification of the glass.
  • the ion exchangeable glass compositionfor producing chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant includes from about 6.0to about 10.0mol%of aluminum oxide (Al 2 O 3 ) .
  • Al 2 O 3 aluminum oxide
  • the aluminum oxide enhances the strength of the alkali-aluminoborosilicate glass and facilitates the ion-exchange between sodium ions in the glass and potassium ions in the molten salt.
  • the dielectric constant increases due to the enlargement of the glass network ring structure.
  • the amount of aluminum oxide in the glass represents a compromise among glass properties such as dielectric constant, ion-exchange depth and glass strength.
  • the ion exchangeable glass compositionfor producing chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant includes from about 5.0 to about 10.0mol%of sodium oxide (Na 2 O) .
  • Alkali metal oxides serve as aids in achieving low liquidus temperatures and low melting temperatures.
  • Na 2 O is used to enable successful ion exchange.
  • sodium oxide is included in the composition in the concentrations described herein.
  • the ion exchangeable glass compositionfor producing chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant includes from about 0 to about 5.0mol%of potassium oxide (K 2 O) .
  • the ion exchangeable glass compositionfor producing chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant includes from about 15.0 to about 25.0mol%of boron trioxide (B 2 O 3 ) .
  • Boron trioxide serves as a flux as well as a glass coordinator.
  • the glass melting temperature and dielectric constant both tend to decrease with an increasing concentration of boron trioxide.
  • the direction of ion-exchange between sodium and potassium ions is negatively affected by an increasing concentration of boron trioxide.
  • the ion exchangeable glass compositionfor producing chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant includes from about 0 to about 3.0mol%of magnesium oxide (MgO) .
  • the ion exchangeable glass compositionfor producing chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant includes from about 1.0 to about 2.0 mol%of magnesium oxide.
  • Magnesium oxide is also believed to increase the strength of the glass and to decrease the specific weight of the glass as compared to other alkaline oxides such ascalcium oxide (CaO) , strontium oxide (SrO) and barium oxide (BaO) .
  • the glass has a liquidus temperature (the temperature at which a crystal is first observed) of at least about 750°C. According to several exemplary embodiments of the ion exchangeable glass compositionfor producing chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant described above, the glass has a liquidus temperature of at least about 800°C.
  • the glass has a liquidus temperature of at least about 850°C. According to several exemplary embodiments of the ion exchangeable glass compositionfor producing chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant described above, the glass has a liquidus temperature of at least about 900°C. According to several exemplary embodiments of the ion exchangeable glass compositionfor producing chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant described above, the glass has a liquidus temperature of from about 750°Cto about 900°C.
  • the present invention provides a method for manufacturing a chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant.
  • the method includes:
  • the manufacture of the chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant may be carried out using conventional overflow down-draw methods which are well known to those of ordinary skill in the art and which customarily include a directly or indirectly heated precious metal system consisting of a homogenization device, a device to lower the bubble content by means of fining (refiner) , a device for cooling and thermal homogenization, a distribution device and other devices.
  • the floating method includes floating molten glass on a bed of molten metal, typically tin, resulting in glass that is very flat and has a uniform thickness.
  • the ion-exchangeable glass composition is melted for up to about 8 hours at about 450°C.
  • the ion-exchangeable glass composition is melted for up to about 16 hours at about 450°C.
  • the ion-exchangeable glass composition is melted for up to about 24 hours at about 450°C.
  • the ion exchangeable glass composition is annealed at a rate of about 0.5°C/hour until it reaches room temperature (or about 21°C) .
  • the ion exchangeable glass composition for producing chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant described above is chemically strengthened according to conventional ion exchange conditions.
  • the ion exchange process occurs in a molten salt bath.
  • the molten salt is potassium nitrate (KNO 3 ) .
  • the ion exchange treatment takes place at a temperature range of from about 390°C to about 450°C. According to several exemplary embodiments of the method for manufacturing a chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant described above, the ion exchange treatment takes place at about 450°C. According to several exemplary embodiments of the method for manufacturing a chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant described above, the ion exchange treatment takes place at temperatures of at least about 450°C. According to several exemplary embodiments of the method for manufacturing a chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant described above, the ion exchange treatment takes place at temperatures of up to about 450°C.
  • the ion exchange treatment is conducted for up to about 4 hours. According to several exemplary embodiments of the method for manufacturing a chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant described above, the ion exchange treatment is conducted for up to about 8 hours. According to several exemplary embodiments of the method for manufacturing a chemically strengthened alkali- aluminoborosilicate glass with a low dielectric constant described above, the ion exchange treatment is conducted for up to about 16 hours. According to several exemplary embodiments of the method for manufacturing a chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant described above, the ion exchange treatment is conducted for about 24 hours.
  • the glass has a surface compressive stress layer having a compressive stress of at least about 100MPa. According to several exemplary embodiments of the chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant described above, the glass has a surface compressive stress layer having a compressive stress of at least about 150MPa. According to several exemplary embodiments of the chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant described above, the glass has a surface compressive stress layer having a compressive stress of at least about 200MPa.
  • the glass has a surface compressive stress layer having a compressive stress of at least about 250 MPa. According to several exemplary embodiments of the chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant described above, the glass has a surface compressive stress layer having a compressive stress of from about 100 MPa to about 250 MPa. According to several exemplary embodiments of the chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant described above, the glass has a surface compressive stress layer having a compressive stress of from about140MPa to about 260 MPa.
  • the glass has a surface compressive stress layer having a compressive stress of from about 150 MPa to about 250 MPa. According to several exemplary embodiments of the chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant described above, the glass has a surface compressive stress layer having a compressive stress of from about 160 MPa to about 240MPa.
  • the glass has a surface compressive stress layer having a depth of at least about 16.0 ⁇ m. According to several exemplary embodiments of the chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant described above, the glass has a surface compressive stress layer having a depth of at least about 17.0 ⁇ m. According to several exemplary embodiments of the chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant described above, the glass has a surface compressive stress layer having a depth of at least about 20.0 ⁇ m.
  • the glass has a surface compressive stress layer having a depth of at least about 27.0 ⁇ m. According to several exemplary embodiments of the chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant described above, the glass has a surface compressive stress layer having a depth of from about 15.0 ⁇ m to about 35.0 ⁇ m. According to several exemplary embodiments of the chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant described above, the glass has a surface compressive stress layer having a depth of from about 17.0 ⁇ m to about 28.0 ⁇ m.
  • the glass has a surface compressive stress layer having a depth of from about 20.0 ⁇ m to 30.0 ⁇ m.
  • the glass has a dielectric constant (1 MHz, 5V at 25°C) of from about 5.0 to about 6.5. According to several exemplary embodiments of the chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant described above, the glass has a dielectric constant (1 MHz, 5V at 25°C) of from about 5.3 to about 6.0. According to several exemplary embodiments of the chemically strengthened alkali-aluminoborosilicate glass with a low dielectric constant described above, the glass has a dielectric constant (1 MHz, 5V at 25°C) of less than about 6.0.
  • the glass has a density of up to about 2.29 g/cm 3 and a linear coefficient of expansion ⁇ 25-300 10 -7 /°C of from about 53.0 to about 70.0.
  • the glass has a density of less than about 2.3 g/cm 3 .
  • the glass is chemically strengthened by ion exchange treatment at a temperature of from about 390°C to about 450°C for about 2 to about 8 hours and the glass has: (1) a surface compressive stress layer having a compressive stress of at least about 150MPa and the depth of the surface compressive stress layer is at least about 17.0 ⁇ m, and (2) a dielectric constant of less than 6.0.
  • the glass is chemically strengthened by ion exchange treatment at a temperature of about 450°C for about 8 hours and the glass has: (1) a surface compressive stress layer having a compressive stress of from about 150MPa to about 250MPa and the depth of the surface compressive stress layer is from about 17.0 ⁇ m to about 28.0 ⁇ m, and (2) a dielectric constant of from about 5.3 to about 6.0.
  • the glass may be used as a protective glass in applications such as solar panels, refrigerator doors, and other household products.
  • the glass may be used as a protective glass for televisions, as safety glass for automated teller machines, and additional electronic products.
  • the glass may be used as cover glass for consumer mobile electronic devices such as smart phones, tablets and note pads.
  • the glass may also be used in applications such as automobile windshields and as the substrate form architectural smart windows.
  • the glass may be used as a touch screen or touch panel due to its high strength.
  • Batch materials as shown in Table 2 were weighed and mixed before being added to a 2 liter plastic container.
  • the batch materials used were of chemical reagent grade quality.
  • the particle size of the sand was between 0.045 and 0.25 mm.
  • a tumbler was used for mixing the raw materials to make a homogenous batch as well as to break up soft agglomerates.
  • the mixed batch was transferred from the plastic container to an 800 ml.
  • the platinum-rhodium crucible was placed in an alumina backer and loaded in a high temperature furnace equipped with MoSi heating elements operating at a temperature of 900°C. The temperature of the furnace was gradually increased to 1620°C and the platinum-rhodium crucible with its backer was held at this temperature for 4 hours.
  • the glass sample was then formed by pouring the molten batch materials from the platinum-rhodium crucible onto a stainless steel plate to form a glass patty. While the glass patty was still hot, it was transferred to an annealerand held at a temperature of 500°C for 2 hours and was then cooled at a rate of 0.5°C/min to 430°C. After that, the sample was cooled naturally to room temperature (21°C) .
  • the glass sample was then chemically strengthened by placing it in a molten salt bath tank, in which the constituent sodium ions in the glass were exchanged with externally supplied potassium ions at a temperature of 450°C which was less than the strain point of the glass for 8 hours.
  • the glass sample was strengthened by ion exchange to produce a compressive stress layer at the treated surface.
  • the measurement of the compressive stress at the surface of the glass and the depth of the compressive stress layer were determined by using a polarization microscope (Berek compensator) on sections of the glass.
  • the compressive stress of the surface of the glass was calculated from the measured dual refraction assuming a stress-optical constant of 0.30 (nm*cm/N) (Scholze, H., Nature, Structure and Properties, Springer-Verlag, 1988, p. 260) .
  • compositions shown in Table 1 above are shown below in Table 3 in the column designated as “Ex. 1” .
  • Additional compositions shown in Table 3 and designated as “Ex. 2” to “Ex. 10” were prepared in a similar manner as described above for the composition designated as Ex. 1.
  • ⁇ d density (g/ml) , which is measured with the Archimedes method (ASTM C693 ) ;
  • ⁇ n D refractive index, which is measured by refractometry
  • ⁇ coefficient of thermal expansion (CTE) which is the amount of linear dimensional change from 50 to 300°C, as measured by dilatometry;
  • ⁇ T melting the melting temperature at the viscosity of 10 2 poise, as measured by high temperature cylindrical viscometry
  • ⁇ T working glass working temperature at the viscosity of 10 4 poise as measured by high temperature cylindrical viscometry
  • ⁇ T liquidus liquidus temperature where the first crystal is observed in a boat within a gradient temperature furnace (ASTM C829-81) , generally test is 24 hours for crystallization;
  • ⁇ T soften glass softening temperature at the viscosity of 10 7.6 poise as measured by the fiber elongation method
  • ⁇ T annealing glass annealing temperature at the viscosity of 10 13 poise as measured by the fiber elongation method
  • ⁇ T strain glass strain temperature at the viscosity of 10 14.5 poise and measured by the fiber elongation method
  • ⁇ k dielectric constant measured at 25°C, 1 MHz, and 5 V as measured by SJ/T 11043-1996 wherein the frequency was 1MHz;
  • ⁇ Loss tan Loss tangent measured at 1 MHz and 5 V as measured by SJ/T 11043-1996 wherein the frequency was 1 MHz;
  • ⁇ Poisson’s Ratio ratio of transverse contraction strain to longitudinal extension strain in the direction of stretching force as measured by the ASTM E1876 resonance method
  • ⁇ CS compressive stress (in-plane stress which tends to compact the atoms in the surface) after chemical strengthening at 450°C for 8 hours;
  • ⁇ DOL depth of layer which represents the depth of compression below the surface to the nearest zero stress plane after chemical strengthening at 450°C for 8 hours;
  • any spatial references such as, for example, “upper, ” “lower, ” “above, ” “below, ” “between, ” “bottom, ” “vertical, ” “horizontal, ” “angular, ” “upwards, ” “downwards, ” “side-to-side, ” “left-to-right, ” “left, ” “right, ” “right-to-left, ” “top-to-bottom, ” “bottom-to-top, ” “top, ” “bottom, ” “bottom-up, ” “top-down, “ etc. , are for the purpose of illustration only and do not limit the specific orientation or location of the structure described above.

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  • 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)
  • Glass Compositions (AREA)

Abstract

La présente invention concerne une composition de verre pour produire du verre d'aluminoborosilicate alcalin chimiquement renforcé à faible constante diélectrique et un procédé de fabrication du verre d'aluminoborosilicate alcalin chimiquement renforcé à faible constante diélectrique. Le verre d'aluminoborosilicate alcalin chimiquement renforcé peut être utilisé comme verre protecteur à résistance élevée pour écrans tactiles, verre protecteur pour cellules solaires et verre de sécurité feuilleté. La faible constante diélectrique du verre améliore la sensibilité, le temps de réponse, la consommation d'énergie et la précision.
PCT/CN2015/075528 2015-03-31 2015-03-31 Composition de verre pour du verre d'aluminoborosilicate alcalin chimiquement renforcé à faible constante diélectrique WO2016154901A1 (fr)

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PCT/CN2015/075528 WO2016154901A1 (fr) 2015-03-31 2015-03-31 Composition de verre pour du verre d'aluminoborosilicate alcalin chimiquement renforcé à faible constante diélectrique
CN201580077196.7A CN107531550A (zh) 2015-03-31 2015-03-31 具有低介电常数的化学强化碱铝硼硅酸玻璃的玻璃组成物
TW105110011A TWI677481B (zh) 2015-03-31 2016-03-30 具低介電常數化學強化鹼鋁硼矽酸玻璃的玻璃組成物

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CN104024173A (zh) * 2011-12-27 2014-09-03 旭硝子株式会社 静电电容式触摸传感器用表面玻璃

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WO2018187391A1 (fr) * 2017-04-04 2018-10-11 Corning Incorporated Structure multicouche et son procédé de fabrication
CN110691761A (zh) * 2017-04-04 2020-01-14 康宁股份有限公司 多层结构及其制造方法
CN110691761B (zh) * 2017-04-04 2022-03-29 康宁股份有限公司 多层结构及其制造方法
US11591257B2 (en) 2017-04-04 2023-02-28 Corning Incorporated Multi-layer structure and method of making same

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