WO2023082936A1 - Verre cristallin et verre cristallin renforcé et leurs procédés de préparation - Google Patents

Verre cristallin et verre cristallin renforcé et leurs procédés de préparation Download PDF

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WO2023082936A1
WO2023082936A1 PCT/CN2022/125285 CN2022125285W WO2023082936A1 WO 2023082936 A1 WO2023082936 A1 WO 2023082936A1 CN 2022125285 W CN2022125285 W CN 2022125285W WO 2023082936 A1 WO2023082936 A1 WO 2023082936A1
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crystallized glass
strengthened
compressive stress
mgo
minutes
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PCT/CN2022/125285
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English (en)
Chinese (zh)
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森田荣光
山下丰
邓镇泉
文晓媛
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深圳旭安光学有限公司
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Publication of WO2023082936A1 publication Critical patent/WO2023082936A1/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
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • 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

Definitions

  • the invention relates to the technical field of glass products, in particular to a glass-ceramic, a strengthened glass-ceramic and a preparation method thereof.
  • Crystallized glass came into being.
  • Patent Document 1 Japanese Patent Laid-Open No. 2021-042116
  • Patent Document 2 Japanese Patent Laid-Open No. 2014-114200 disclose crystallized glass and its preparation method.
  • Crystallized glass is also called glass ceramics, and is a material in which crystals are precipitated inside the glass by heat-treating the glass.
  • Crystallized glass is a material having a crystalline phase and a glass phase, and is distinguished from an amorphous solid.
  • the crystal phase of crystallized glass is discriminated using the peak angle appearing in the X-ray diffraction pattern of X-ray diffraction analysis.
  • the main indicators to measure the performance of chemically strengthened glass are glass surface compressive stress (CS, Compressive Stress) and compressive stress layer depth (DOL, Depth of Compressive Stress Layer).
  • CS Compressive Stress
  • DOL compressive stress layer depth
  • the strengthening treatment is divided into physical toughening and chemical strengthening.
  • the chemical strengthening method is also called the ion exchange chemical strengthening method. The principle is to immerse the glass in a molten alkali metal salt bath.
  • the alkali metal ions K + or Na + with a larger diameter in the glass exchange with the alkali metal ions Na + or Li + with a smaller diameter in the glass, and the "pinching effect" generated by the ion exchange forms a large compressive stress on the glass surface. Thereby enhancing the strength of the glass.
  • Chemical strengthening can produce several times the strength compared to physical tempering. For thin glass with a thickness less than 2mm, and glass with high requirements for strength and flatness, chemical strengthening can only be used.
  • the strength of chemically strengthened glass comes from the CS and DOL produced by ion exchange. Although the traditional single ion exchange strengthened glass can provide a certain impact strength, it is difficult for the internal central tensile stress (CT, Central Tension) generated during the ion exchange process. If not well controlled, the glass has the risk of self-explosion, thus becoming "unsafe" glass.
  • CT Central Tension
  • the present invention provides a crystallized glass and strengthened crystallized glass, specifically adopting the following technical solutions:
  • the crystallized glass contains the following components: 40-60% SiO 2 , 10-20% Al 2 O 3 , 0-20% Rn 2 O, 3- 20% MgO, 0-11% TiO 2 , 0-10% CaO, 0-5% SrO, 0-6% BaO, 0-1% Sb 2 O 3 , wherein Rn is selected from Li, Na, K Any one or more, and the sum of the contents of MgO, ZnO and TiO 2 is ⁇ 20%;
  • Rn 2 O is composed of the following components: Li 2 O 0%-5.0%, K 2 O 0%-20.0% and/or Na 2 O 0%-20.0%;
  • the crystallized glass also contains the following components: 0-15% Ta 2 O 5 , 0-1% P 2 O 5 , 0-1% B 2 O 3 , 0-15% ZnO, 0-5% Gd 2 O 3 , 0-2% Bi 2 O 3 , 0-2% Nb 2 O 5 , 0-2% La 2 O 3 , 0-5% WO 3 , 0-2% Y 2 O 3 , 0-1% TeO 2 , 0-2% SnO 2 , 0-2% CeO 2 ;
  • the lower limit of the sum of SiO 2 , Rn 2 O, Al 2 O 3 , MgO, ZnO, ZrO 2 , and TiO 2 in the crystallized glass is ⁇ 70.0%; preferably, In terms of oxides, the lower limit of the sum of SiO 2 , Rn 2 O, Al 2 O 3 , MgO, ZnO, ZrO 2 , and TiO 2 in the crystallized glass is ⁇ 85.0%; further preferably, in terms of oxides, the The lower limit of the sum of SiO 2 , Rn 2 O, Al 2 O 3 , MgO, ZnO, ZrO 2 , and TiO 2 in the crystallized glass is ⁇ 88.0%; more preferably, in terms of oxides, SiO 2 in the crystallized glass 2.
  • the lower limit of the sum of the contents of Rn 2 O, Al 2 O 3 , MgO, ZnO, ZrO 2 , and TiO 2 is ⁇
  • the main crystal image of the crystallized glass contains any one or two selected from enstatite (MgSiO 3 ) and spinel (MgAl 2 O 4 );
  • the grain diameter of the main crystal phase is 0.05 nm to 100 nm, preferably, the grain diameter of the main crystal phase is 0.1 nm to 10 nm; further preferably, the grain diameter of the main crystal phase is 0.1nm ⁇ 7nm;
  • the crystallinity of the main crystal phase is ⁇ 30%; more preferably, the crystallinity is ⁇ 25%;
  • the specific gravity of the main crystal phase is ⁇ 4.00, more preferably, the specific gravity is 2.50-3.10;
  • a strengthened crystallized glass which includes any one of the above-mentioned crystallized glass as a substrate and a compressive stress layer;
  • the compressive stress layer includes a compressive stress layer on the surface of the substrate and a compressive stress layer on the end surface of the substrate;
  • the compressive stress layer contains Na + and/or K + ions; more preferably, the compressive stress layer contains NaNO 3 and/or KNO 3 ;
  • the depth of the compressive stress layer of the strengthened crystallized glass is 0-150 ⁇ m
  • the surface compressive stress of the strengthened crystallized glass is 200.0-1400.0MPa; preferably 225-1000MPa;
  • the central compressive stress CT of the strengthened crystallized glass is 1.0-150.0 MPa.
  • the Vickers hardness Hv of the strengthened crystallized glass is 700-1400; more preferably, the Vickers hardness Hv is 800-1350.
  • the present invention adjusts the content and composition of each component in the crystallized glass, especially can change the degree of crystallization of the crystallized glass and the size of the precipitated particles, so that the ions of the crystallized glass can reach the nanometer level (0.1-10nm), and can make the crystallized glass The crystallization rate of the glass is improved.
  • the compressive stress layer is formed, the surface and the side can be ion-exchanged through the control of the preparation method and parameters, so that the degree of ion exchange is deeper than the existing technology, reaching 0-150 ⁇ m.
  • the implementation Example 1 obtained 124.5 ⁇ m, thereby obtained following beneficial effect: first, improve the hardness of crystallized glass, obtain the stronger crystallized glass of impact resistance; In addition, can guarantee certain plasticity while improving hardness, its degree of wear (Aa ) is relatively high, which is good for processing, so it can be widely used in vehicle lenses, short-focus projector lenses, wearable devices, decorations (vehicles, buildings, smart keys, etc.), touch panels, and dielectric filters;
  • the crystallized glass of the present invention has higher light transmittance, light transmittance ⁇ 90%, and is easy to realize thin film and light weight, and can also be used as optical components such as optical filters and cameras (such as lenses, substrates, etc.);
  • the crystallized glass of the present invention has a high dielectric constant and a low dielectric loss rate, so it has a high sensitivity, thereby making it more suitable for use as a cover for smart phones, tablet computers, and PCs.
  • Plate glass or shell which can facilitate the signal transmission of 5G and 6G products.
  • composition and preparation method of the present invention will be further described in detail below in conjunction with specific examples, but the present invention is not limited by the following embodiments and examples, and can be implemented with appropriate changes within the scope of the purpose of the present invention .
  • the content of each component is represented by the mass % of oxide conversion.
  • “in terms of oxides” refers to the amount of each oxide contained in the crystallized glass when the total mass of the oxides is assumed to be 100% by mass, assuming that all the constituent components of the crystallized glass are decomposed and changed into oxides. The amount of is expressed in mass%. In this specification, 0% means that the content is 0%.
  • SiO 2 is a glass-forming component that forms a network structure of glass and is an essential component.
  • the upper limit of the content of the SiO 2 component may be less than 60.0%, 58.0% or less, 56.0% or less, or 55.0% or less.
  • the lower limit of the content of the SiO2 component may be equal to or greater than 40.0%, equal to or greater than 45.0%, equal to or greater than 50.0%, or equal to or greater than 54.0%;
  • Rn 2 O (Rn is selected from one or more of Li, Na, and K) is a component that participates in ion exchange during chemical strengthening. On the other hand, if it is contained in excess, chemical durability or devitrification resistance will deteriorate. Poor ingredients. Therefore, the upper limit of the content of Rn 2 O may be 25.0% or less, 23.0% or less, 20.0% or less, or 18.0% or less.
  • the lower limit of the content of Rn 2 O can be greater than 0%, greater than or equal to 1.0%, greater than or equal to 4.0%, greater than or equal to 10.0%, or greater than or equal to 15.0%;
  • the exchange reaction between the component (K + ions) and the sodium component (Na + ions) in the substrate with a small ionic radius results in the formation of compressive stress on the surface of the substrate, so it is preferably an essential component. Therefore, the upper limit of the content of Na 2 O may be 20.0% or less, 18.0% or less, or 16.0% or less; in addition, the lower limit of the Na 2 O content may be greater than 0%, greater than or equal to 1.0%, or greater than 4.0%. or greater than or equal to 10.0%;
  • Al 2 O 3 is a component suitable for improving the mechanical strength, but on the other hand, if it is contained in excess, it will deteriorate meltability and devitrification resistance. Therefore, the upper limit of the content of Al 2 O 3 may be 20.0% or less. In addition, the lower limit of the content of Al 2 O 3 may be greater than or equal to 0%, or greater than or equal to 10.0%;
  • TiO 2 is an important constituent of crystalline particles contributing to mechanical strength. Therefore, the upper limit of the MgO content is 20.0% or less, 15.0% or less, and 10.0% or less, and the lower limit of the MgO content is 0% or more, 4.0% or more, and 8.0% or more;
  • MgO is a component that raises the refractive index and contributes to mechanical strength. On the other hand, if it is contained in excess, the devitrification resistance will deteriorate. Therefore, the upper limit of the content of the MgO component is 18.0% or less. In addition, the lower limit of the content of MgO is 0% or more, 3.0% or more, 5.0% or more, 10.0% or more, or 15.0% or more;
  • the total amount of MgO and TiO 2 is greater than or equal to 20%, preferably greater than or equal to 25%;
  • the crystallized glass also contains the following components: 0-15% Ta 2 O 5 , 0-1% P 2 O 5 , 0-1% B 2 O 3 , 0-15% ZnO, 0-5% Gd 2 O 3 , 0-2% Bi 2 O 3 , 0-2% Nb 2 O 5 , 0-2% La 2 O 3 , 0-5% WO 3 , 0-2% Y 2 O 3 , 0-1% TeO 2 , 0-2% SnO 2 , 0-2% CeO 2 ;
  • the lower limit of the sum of SiO 2 , Rn 2 O, Al 2 O 3 , MgO, ZnO, ZrO 2 , and TiO 2 in the crystallized glass is ⁇ 70.0%; preferably, In terms of oxides, the lower limit of the sum of SiO 2 , Rn 2 O, Al 2 O 3 , MgO, ZnO, ZrO 2 , and TiO 2 in the crystallized glass is ⁇ 85.0%; further preferably, in terms of oxides, the The lower limit of the sum of SiO 2 , Rn 2 O, Al 2 O 3 , MgO, ZnO, ZrO 2 , and TiO 2 in the crystallized glass is ⁇ 88.0%; more preferably, in terms of oxides, SiO 2 in the crystallized glass 2.
  • the lower limit of the sum of the contents of Rn 2 O, Al 2 O 3 , MgO, ZnO, ZrO 2 , and TiO 2 is ⁇
  • the strengthened crystallized glass of the present invention has a high Vickers hardness. When the hardness is high, it is difficult to be scratched or broken.
  • the Vickers hardness Hv of the strengthened crystallized glass is 700-1400; more preferably, the Vickers hardness Hv is 800-1350.
  • the thickness of the crystallized glass substrate is ⁇ 0.1mm; further preferably, the thickness of the crystallized glass substrate is ⁇ 0.15mm; further preferably, the thickness of the crystallized glass substrate is ⁇ 0.20mm; further preferably, The thickness of the crystallized glass substrate is ⁇ 0.40mm.
  • the thickness of the crystallized glass substrate is ⁇ 10.0mm; further preferably, the thickness of the crystallized glass substrate is ⁇ 6.0mm; further preferably, the thickness of the crystallized glass substrate is ⁇ 2.0mm; further preferably, The thickness of the crystallized glass substrate is ⁇ 1.0mm.
  • Another aspect of the present invention provides the preparation method of above-mentioned crystallized glass, comprises the following steps:
  • the present invention also provides a method for preparing a strengthened crystallized glass, comprising the steps of preparing the above crystallized glass S1, S2, and the following steps:
  • S3 Using the crystallized glass described in S2 as a substrate, performing chemical strengthening to obtain a strengthened crystallized glass including a compressive stress layer.
  • the original glass is first heat-treated, and then the crystals are precipitated inside the glass;
  • the heat treatment is completed in one step, including: completing the nucleation process and the crystal growth process at a constant temperature, that is, first raising the temperature to a specified temperature, then heating at a constant temperature, and then cooling down;
  • the heat treatment is completed in two steps, including: (1) performing a nucleation process at a constant temperature at the first temperature; (2) after the nucleation process, by performing heat treatment at a second temperature to perform the crystal growth process;
  • the first temperature is 600°C-750°C; further preferably, the holding time of the first temperature is 30-2000 minutes; preferably 180-1440 minutes;
  • the second temperature is 650°C-850°C; further preferably, the holding time of the second temperature is 30-600 minutes; preferably 60-300 minutes;
  • the crystallized glass is first prepared into a substrate-shaped crystallized glass by using a process including grinding and grinding, and then a compressive stress layer is formed on the crystallized glass substrate by using a chemical strengthening method;
  • the chemical strengthening method includes: ion exchange method, heat strengthening method, ion implantation method and air cooling strengthening method;
  • the chemical strengthening method includes: contacting or immersing the crystallized glass substrate in a salt containing potassium or sodium, such as potassium nitrate (KNO 3 ), sodium nitrate (NaNO 3 ) and/or a mixed salt thereof or Molten salt of its compound salt;
  • a salt containing potassium or sodium such as potassium nitrate (KNO 3 ), sodium nitrate (NaNO 3 ) and/or a mixed salt thereof or Molten salt of its compound salt;
  • the chemical strengthening method includes: (1) at 400° C. to 550° C., contacting or immersing the crystallized glass substrate in a solution containing KNO 3 and NaNO 3 at a weight ratio of 1:(1 to 3) Immerse in the mixed molten salt for 100 to 1440 minutes; preferably 200 to 1000 minutes; (2) at 450°C to 550°C, immerse the crystallized glass substrate impregnated according to step (1) in a solution containing KNO 3 and NaNO 3 Immerse in mixed molten salt with a weight ratio of (40-100):1 for 10-100 minutes; preferably 20-90 minutes;
  • the chemical strengthening method includes: (1) at 400°C to 550°C, then immersing the crystallized glass substrate in a mixture containing KNO 3 and NaNO 3 at a weight ratio of 2 to 5:1. Immersing in molten salt for 500-1000 minutes; (2) immersing the crystallized glass substrate impregnated according to step (1) in KNO 3 molten salt at 450°C-550°C for 20-60 minutes;
  • the thermal strengthening method is not particularly limited, for example, after heating the crystallized glass substrate to 300-600°C, rapid cooling such as water cooling and/or air cooling can be used to utilize the strength of the glass substrate.
  • rapid cooling such as water cooling and/or air cooling can be used to utilize the strength of the glass substrate.
  • the temperature difference between the surface and the interior forms a compressive stress layer.
  • the compressive stress layer can also be formed more effectively by combining with the above-mentioned chemical treatment method;
  • the ion implantation method is not particularly limited, for example, by causing arbitrary ions to collide with the acceleration energy and acceleration voltage on the surface of the crystallized glass substrate to the extent that the substrate surface is not damaged, the ions are implanted on the substrate surface, and then, if necessary, By heat treatment, a compressive stress layer can be formed on the surface similarly to other methods.
  • the mixed raw materials are put into a platinum crucible, and melted in an electric furnace at 1200° C. to 1600° C. for 2 hours to 72 hours depending on the melting difficulty of the glass component. Then, stir the molten glass for homogenization, then lower the temperature to 1000°C-1450°C, then cast it into a mold and cool it down slowly to make the original glass;
  • the obtained original glass is heat-treated (650-730 degreeC, 5 hours) in step 1 for nucleation and crystallization, and the crystallized glass used as a base material is produced.
  • the crystallized glass used as a base material is produced.
  • FE-TEM field emission type transmission electron microscope
  • precipitated crystals having an average crystal diameter of 0.1 nm to 10 nm were observed.
  • Enstatite was further confirmed by lattice images based on electron diffraction images and analyzed by EDX, and crystal phases of enstatite (MgSiO 3 ) and spinels (MgAl 2 O 4 ) were confirmed.
  • the average crystal diameter was obtained by obtaining the crystal diameters of crystal particles in the range of 180 ⁇ 180 nm 2 using a transmission electron microscope and calculating the average value.
  • the prepared crystallized glass substrate (colorless and transparent) is cut and ground to prepare a substrate with a thickness of 0.60mm, and then its surface is parallel ground; the parallel ground substrate is chemically strengthened to obtain a crystallized glass substrate.
  • the parallel ground substrate is chemically strengthened to obtain a crystallized glass substrate.
  • the chemical strengthening condition of embodiment 5,12,15 is in mixing ratio KNO 3 : NaNO 3 weight ratio is in the mixed molten salt of 1: 1.5 (weight ratio), after immersing at 470 °C for 400 minutes, when mixing ratio is It was immersed at 400° C. for 90 minutes in a molten salt having a KNO 3 :NaNO 3 ratio of 80:1 (weight ratio).
  • the chemical strengthening conditions of Examples 1, 13, and 14 were in a mixed molten salt with a mixing ratio of KNO 3 : NaNO 3 weight ratio of 1:2 (weight ratio), after immersion at 470°C for 270 minutes, when the mixing ratio was 50 : 1 (weight ratio) in molten salt and immersed at 450° C. for 30 minutes.
  • the refractive index (nd) is represented by the measured value of the d-line (587.56nm) of a helium lamp in accordance with the V-block method specified in JISB7071-2:2018.
  • a 136° diamond quadrangular pyramidal indenter is indented with a load of 980.7 mN for 10 seconds, and is obtained by dividing by the surface area (mm2) calculated from the length of the indentation depression.
  • the measurement was performed using a micro Vickers hardness meter HMV-G manufactured by Shimadzu Corporation.
  • CS surface compressive stress value
  • stress depth DOLzero thickness of the compressive stress layer
  • the value of the refractive index at a wavelength of 596nm is based on the measured value of the refractive index at the wavelength of the C-line, d-line, F-line, and g-line using the quadratic approximation formula according to the V-block method specified in JISB7071-2:2018 figured out.
  • the central compressive stress value (CT) is obtained by curve analysis (Curve analysis). In addition, in Example 11, stress streaks were not confirmed, and the numerical value was 0.
  • Example 5 of patent document 1 As comparative example 1, the crystallized glass of Example 5 of patent document 1 was used, and it evaluated similarly to an Example. The results are shown in Table 1.
  • Example 6 As comparative example 2, the crystallized glass of Example 6 of patent document 2 was used, and it evaluated similarly to an Example. The results are shown in Table 1.

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

Abstract

La présente invention concerne du verre cristallin et du verre cristallin renforcé et leurs procédés de préparation. Le verre cristallin comprend les composants suivants, en termes de teneurs en pourcentage en masse d'oxydes : 40-60 % de SiO2, 1-20 % d'Al2O3, 0-20 % de Rn2O, 1-20 % de MgO, 0,5-20 % de ZnO, 0-20 % de TiO2, 0-20 % de CaO, 0-10 % de SrO, 0-10 % de BaO et 0-10 % de Sb2O3, Rn étant choisi parmi un ou plusieurs des éléments Li, Na et K, et la somme des teneurs en MgO, ZnO et TiO2 étant supérieure ou égale à 20 %. Le verre cristallin et le verre cristallin renforcé de la présente invention ont des particules cristallines jusqu'à l'échelle nanométrique, et présentent ainsi de meilleures propriétés de dureté, de facteur de transmission de la lumière et de constante diélectrique, un taux de perte diélectrique plus faible et des perspectives d'application plus larges.
PCT/CN2022/125285 2021-11-11 2022-10-14 Verre cristallin et verre cristallin renforcé et leurs procédés de préparation WO2023082936A1 (fr)

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CN114262155A (zh) * 2021-11-11 2022-04-01 深圳旭安光学有限公司 一种结晶玻璃、强化结晶玻璃及其制备方法
CN117886514B (zh) * 2024-03-12 2024-06-11 蒙娜丽莎集团股份有限公司 一种ZnO基抗菌晶种材料及其制备方法

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CN101905952A (zh) * 2009-06-04 2010-12-08 株式会社小原 信息记录媒体用晶化玻璃基板及其制造方法
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