WO2019134133A1 - Procédé de renforcement de vitrocéramique et procédé de fabrication d'une plaque de couverture en vitrocéramique - Google Patents

Procédé de renforcement de vitrocéramique et procédé de fabrication d'une plaque de couverture en vitrocéramique Download PDF

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WO2019134133A1
WO2019134133A1 PCT/CN2018/071629 CN2018071629W WO2019134133A1 WO 2019134133 A1 WO2019134133 A1 WO 2019134133A1 CN 2018071629 W CN2018071629 W CN 2018071629W WO 2019134133 A1 WO2019134133 A1 WO 2019134133A1
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glass
ion exchange
weight
glass ceramic
ceramic
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PCT/CN2018/071629
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English (en)
Chinese (zh)
Inventor
刘伟
李火增
唐彬
李亚
张芳
王晓凤
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南昌欧菲光学技术有限公司
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Priority to PCT/CN2018/071629 priority Critical patent/WO2019134133A1/fr
Publication of WO2019134133A1 publication Critical patent/WO2019134133A1/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
    • 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 production and manufacture, in particular to a method for strengthening glass ceramics and a method for manufacturing a glass ceramic cover.
  • Glass-ceramics are widely used in the manufacture of astronomical telescopes, high-temperature electric light source glass, induction cooktop panels, and microelectronics substrates for their low expansion, high strength, wear resistance, good electrical insulation, and impact resistance. Since the glass-ceramic products need to be ground and polished, the strength of the milled glass-ceramics is lowered, thereby affecting the performance of the glass-ceramic products.
  • Embodiments of the present invention provide a method for strengthening glass ceramics and a method for fabricating a glass ceramic cover.
  • the method for strengthening the glass ceramic according to the embodiment of the present invention includes: providing a first ion exchange bath including a potassium nitrate and a sodium nitrate, and a second ion exchange bath comprising potassium nitrate; Putting the crystallized glass to be intensively treated into the first ion exchange bath to perform a primary salt bath to obtain a primary strengthened glass ceramic; and placing the primary strengthened crystallized glass into the second ion exchange bath A secondary salt bath was performed to obtain a secondary strengthened glass ceramic.
  • the method for strengthening the glass ceramics according to the embodiment of the present invention improves the linear expansion coefficient of the glass ceramic by performing the two salt baths by sequentially placing the glass ceramics to be strengthened into the first ion exchange bath and the second ion exchange bath. Hardness, bending stress and strength, and reduced dielectric loss.
  • the first ion exchange bath comprises 0% by weight to 20% by weight of potassium nitrate, and 0% by weight to 10% by weight of sodium nitrate, and the temperature of the first ion exchange bath is 400 ° C - 600 °C, the time of the first salt bath is from 300 minutes to 720 minutes.
  • the first ion exchange bath can increase the exchange rate of the plurality of ions in the glass ceramics with the potassium ions and the sodium ions in the first ion exchange bath at the above temperature, and at the same time, the first ion exchange time in the first salt bath time
  • the potassium ions and sodium ions in the bath can be sufficiently exchanged with a plurality of ions in the glass ceramics.
  • the second ion exchange bath comprises 5% by weight to 20% by weight of potassium nitrate, and the temperature of the second ion exchange bath is between 400 ° C and 500 ° C, the time of the secondary salt bath It is 5 minutes to 30 minutes.
  • the second ion exchange bath can increase the exchange rate of the plurality of ions in the glass ceramics with the potassium ions in the second ion exchange bath at the above temperature, and at the same time, in the first salt bath time, in the second ion exchange bath Potassium ions can be sufficiently exchanged with a plurality of ions in the glass-ceramic.
  • the method of strengthening the glass ceramic further comprises: washing the primary strengthened glass ceramic. Since the glass ceramic to be strengthened is firstly strengthened by the first ion exchange bath, the surface of the first strengthened glass ceramic adheres to the first ion exchange bath and the ions displaced into the first ion exchange bath, and is first strengthened by washing. The glass ceramics can reduce the influence of impurities on the second ion exchange bath.
  • first ion exchange bath comprising potassium nitrate and sodium nitrate
  • second ion exchange bath comprising potassium nitrate
  • a film is coated on the electrode layer to form the glass-ceramic cover.
  • the method for fabricating a glass-ceramic cover plate according to an embodiment of the present invention improves the surface of the glass-ceramic cover by sequentially placing the glass-ceramic to be strengthened into the first ion exchange bath and the second ion exchange bath to perform two salt baths. Linear expansion coefficient, hardness, bending stress and strength, and reduced dielectric loss.
  • the first ion exchange bath comprises 0% by weight to 20% by weight of potassium nitrate, and 0% by weight to 10% by weight of sodium nitrate, and the temperature of the first ion exchange bath is 400 ° C - 600 °C, the time of the first salt bath is from 300 minutes to 720 minutes.
  • the first ion exchange bath can increase the exchange rate of the plurality of ions in the glass ceramics with the potassium ions and the sodium ions in the first ion exchange bath at the above temperature, and at the same time, the first ion exchange time in the first salt bath time
  • the potassium ions and sodium ions in the bath can be sufficiently exchanged with a plurality of ions in the glass ceramics.
  • the second ion exchange bath comprises 5% by weight to 20% by weight of potassium nitrate, and the temperature of the second ion exchange bath is between 400 ° C and 500 ° C, the time of the secondary salt bath It is 5 minutes to 30 minutes.
  • the second ion exchange bath can increase the exchange rate of the plurality of ions in the glass ceramics with the potassium ions in the second ion exchange bath at the above temperature, and at the same time, in the first salt bath time, in the second ion exchange bath Potassium ions can be sufficiently exchanged with a plurality of ions in the glass-ceramic.
  • the method of fabricating the glass-ceramic cover further comprises: washing the primary strengthened glass ceramic. Since the glass ceramic to be strengthened is firstly strengthened by the first ion exchange bath, the surface of the first strengthened glass ceramic adheres to the first ion exchange bath and the ions displaced into the first ion exchange bath, and is first strengthened by washing. The glass ceramics can reduce the influence of impurities on the second ion exchange bath.
  • the manufacturing method further includes:
  • the refined glass ceramic is washed to obtain the glass ceramic to be strengthened.
  • the refined glass ceramics obtainable by the present embodiment have a suitable size and structure, a smooth surface quality, and a finer grain size.
  • the step of cutting the crystallized glass ceramic to obtain a refined glass ceramic comprises:
  • the sheet glass ceramic is cut to obtain the refined glass ceramic.
  • the manufacturing method further includes: providing a glass-ceramic material; crystallizing the glass-ceramic material to obtain crystallized glass-ceramic; cutting the crystallized glass-ceramic And obtaining the refined glass ceramic; grinding the refined glass ceramic; and cleaning the refined glass ceramic to obtain the glass ceramic to be strengthened.
  • a glass ceramic of a suitable shape can be obtained by refining the glass ceramic by hot bending.
  • the temperature of the refined glass ceramic is 650 ° C - 850 ° C
  • the time for refining the glass ceramic is 10 seconds - 60 seconds
  • the thinning is performed by hot bending.
  • the pressure of the crystal glass is from 0.1 MPa to 0.5 MPa. The glass ceramic obtained under the above bending pressure, temperature and time has a high strength, and the glass ceramic does not return to its original shape.
  • the temperature of the refined glass ceramic is 700 ° C - 750 ° C
  • the time for refining the glass ceramic is 20 seconds - 40 seconds
  • the thinning is performed by hot bending.
  • the pressure of the crystal glass is 0.2 MPa to 0.3 MPa. The glass ceramic obtained under the above bending pressure, temperature and time has a high strength, and the glass ceramic does not return to its original shape.
  • FIG. 1 is a schematic flow chart of a method for strengthening a glass ceramic according to some embodiments of the present invention.
  • FIG. 2 is a schematic diagram showing the principle of a method for strengthening a glass ceramic according to some embodiments of the present invention.
  • FIG. 3 is a schematic flow chart of a method for strengthening a glass ceramic according to some embodiments of the present invention.
  • FIG. 4 is a schematic diagram showing the principle of a method for strengthening a glass ceramic according to some embodiments of the present invention.
  • FIG. 5 is a schematic flow chart of a method for fabricating a glass-ceramic cover according to some embodiments of the present invention.
  • FIG. 6 is a schematic diagram showing the principle of a method for fabricating a glass-ceramic cover according to some embodiments of the present invention.
  • FIG. 7 is a schematic flow chart of a method of fabricating a glass-ceramic cover according to some embodiments of the present invention.
  • FIG. 8 is a schematic diagram showing the principle of a method for fabricating a glass-ceramic cover according to some embodiments of the present invention.
  • FIG. 9 is a schematic flow chart of a method of fabricating a glass-ceramic cover according to some embodiments of the present invention.
  • FIG. 10 is a schematic diagram showing the principle of a method for fabricating a glass-ceramic cover according to some embodiments of the present invention.
  • FIG. 11 is a schematic flow chart of a method of fabricating a glass-ceramic cover according to some embodiments of the present invention.
  • FIG. 12 is a schematic flow chart of a method of fabricating a glass-ceramic cover according to some embodiments of the present invention.
  • FIG. 13 is a schematic diagram showing the principle of a method for fabricating a glass-ceramic cover according to some embodiments of the present invention.
  • first and second are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated.
  • features defining “first” or “second” may include one or more of the described features either explicitly or implicitly.
  • the meaning of "a plurality” is two or more unless specifically and specifically defined otherwise.
  • connection In the description of the present invention, it should be noted that the terms “installation”, “connected”, and “connected” are to be understood broadly, and may be fixed or detachable, for example, unless otherwise explicitly defined and defined. Connected, or integrally connected; may be mechanically connected, may be electrically connected or may communicate with each other; may be directly connected, or may be indirectly connected through an intermediate medium, may be internal communication of two elements or interaction of two elements relationship.
  • Connected, or integrally connected may be mechanically connected, may be electrically connected or may communicate with each other; may be directly connected, or may be indirectly connected through an intermediate medium, may be internal communication of two elements or interaction of two elements relationship.
  • the specific meanings of the above terms in the present invention can be understood on a case-by-case basis.
  • the first feature "on” or “under” the second feature may include direct contact of the first and second features, and may also include first and second features, unless otherwise specifically defined and defined. It is not in direct contact but through additional features between them.
  • the first feature "above”, “above” and “above” the second feature includes the first feature directly above and above the second feature, or merely indicating that the first feature level is higher than the second feature.
  • the first feature “below”, “below” and “below” the second feature includes the first feature directly below and below the second feature, or merely the first feature level being less than the second feature.
  • a method for strengthening the glass ceramic 10 includes:
  • the first ion exchange bath 101 comprises potassium nitrate and sodium nitrate
  • the second ion exchange bath 102 comprises potassium nitrate
  • the glass ceramics 10 to be intensified are placed in the first ion exchange bath 101 for a primary salt bath to obtain the primary strengthened glass ceramics 20;
  • the primary strengthened glass ceramics 20 is placed in the second ion exchange bath 102 to perform a secondary salt bath to obtain the secondary strengthened glass ceramics 30.
  • the glass ceramics of the embodiment of the present invention may be a boron-based glass ceramic or an aluminum-based glass ceramic.
  • the first ion exchange bath 101 is formed by dissolving potassium nitrate and sodium nitrate with a solvent.
  • the solvent may be a protic polar solvent, for example, the solvent may be any one of water, methanol, ethanol, isopropanol, nitromethane, formic acid, acetic acid, ethylene glycol, 1,3-propanediol, glycerin or A variety of combinations are formed.
  • the solvent may also be an aprotic polar solvent, for example, the solvent may be formed by any one or a combination of acetone, ethyl acetate, acetonitrile, dimethyl sulfoxide, tetrahydrofuran, dimethylformamide. Further, the solvent may be formed in a combination of protic solvents and aprotic solvents in different ratios.
  • the second ion exchange bath 102 is formed of potassium nitrate and a solvent which may be the same as the solvent component in the first ion exchange bath 101, and the content of the solvent component may be different.
  • exchange means introducing a cation (potassium ion, sodium ion) from the first ion exchange bath 101 into the glass ceramics 10 (or a surface portion of the glass ceramic 10) and making it in the first ion exchange bath 101.
  • the cation replaces the cation having the same valence state/charge/oxidation state in the glass-ceramics 10; alternatively, "exchange” may also mean introducing the cation (potassium ion, sodium ion) from the first ion exchange bath 101 into the glass-ceramic 10 (or the surface portion of the glass-ceramics 10) and the cations in the first ion exchange bath 101 are substituted for cations having different valence/charge/oxidation states in the glass-ceramics 10.
  • the primary strengthened glass ceramics 20 When the primary strengthened glass ceramics 20 is placed in the second ion exchange bath 102 for the secondary salt bath, the plurality of ions in the first strengthened glass ceramics 20 are exchanged with the potassium ions in the second ion exchange bath 102.
  • the strengthening method of the glass ceramics 10 according to the embodiment of the present invention can increase the linear expansion coefficient and hardness of the glass ceramics 10 under the premise that the light transmittance of the glass ceramics 10 is greater than or equal to 88%. , bending stress and strength, and reducing dielectric loss.
  • the method for strengthening the glass-ceramics 10 of the present invention enhances the line of the glass-ceramics 10 by sequentially placing the glass-ceramics 10 to be strengthened into the first ion exchange bath 101 and the second ion exchange bath 102 in two salt baths. Expansion coefficient, hardness, bending stress and strength, and reduced dielectric loss.
  • the first ion exchange bath 101 comprises 0% by weight to 20% by weight of potassium nitrate, and 0% by weight to 10% by weight of sodium nitrate, of the first ion exchange bath 101.
  • the temperature is from 400 ° C to 600 ° C, and the initial salt bath time is from 300 minutes to 720 minutes.
  • the first ion exchange bath 101 further includes a solvent, which may be a protic polar solvent or an aprotic polar solvent.
  • the weight percentage of potassium nitrate in the first ion exchange bath 101 may be 0% by weight, 2% by weight, 4% by weight, 5% by weight, 6% by weight, 8% by weight, 10% by weight, 12% by weight, and 14% by weight. Any one of 15% by weight, 16% by weight, 18% by weight, and 20% by weight, or a value between any of the above.
  • the weight percentage of sodium nitrate in the first ion exchange bath 101 may be 0% by weight, 1% by weight, 2% by weight, 3% by weight, 4% by weight, 5% by weight, 6% by weight, 7% by weight, and 8% by weight. Any one of 9% by weight and 10% by weight, or a value between any of the above.
  • the temperature of the first ion exchange bath 101 is any one of 400 ° C, 425 ° C, 450 ° C, 475 ° C, 500 ° C, 525 ° C, 550 ° C, 575 ° C, 600 ° C, or between any two of the above. .
  • the initial salt bath time is 300 minutes, 330 minutes, 360 minutes, 390 minutes, 400 minutes, 425 minutes, 450 minutes, 475 minutes, 500 minutes, 525 minutes, 550 minutes, 575 minutes, 600 minutes, 630 minutes, 660 minutes. Any one of 690 minutes, 700 minutes, and 720 minutes, or between any two of the above.
  • the first ion exchange bath 101 can increase the exchange rate of the plurality of ions in the glass ceramics 10 with the potassium ions and the sodium ions in the first ion exchange bath 101 at the above temperature, and at the same time, in the first salt bath time, The potassium ions and sodium ions in the ion exchange bath 101 can be sufficiently exchanged with a plurality of ions in the glass ceramics 10.
  • the first ion exchange bath 101 comprises 5% by weight to 15% by weight potassium nitrate, and 0.5% by weight to 5% by weight sodium nitrate, of the first ion exchange bath 101.
  • the temperature is from 450 ° C to 500 ° C, and the initial salt bath time is from 400 minutes to 600 minutes.
  • the first ion exchange bath 101 further includes a solvent, which may be a protic polar solvent or an aprotic polar solvent.
  • the weight percentage of potassium nitrate in the first ion exchange bath 101 may be 5% by weight, 6% by weight, 7% by weight, 8% by weight, 9% by weight, 10% by weight, 11% by weight, 12% by weight, and 13% by weight. Any one of 14% by weight and 15% by weight, or a value between any of the above.
  • the weight percentage of sodium nitrate in the first ion exchange bath 101 may be 0.5% by weight, 1% by weight, 1.5% by weight, 2% by weight, 2.5% by weight, 3% by weight, 3.5% by weight, 4% by weight, 4.5% by weight.
  • the temperature of the first ion exchange bath 101 is any one of 450 ° C, 460 ° C, 470 ° C, 475 ° C, 480 ° C, 490 ° C, and 500 ° C, or a value between any of the above.
  • the time of the first salt bath is any one of 400 minutes, 425 minutes, 450 minutes, 475 minutes, 500 minutes, 525 minutes, 550 minutes, 575 minutes, 600 minutes, or a value between any two of the above.
  • the first ion exchange bath 101 can increase the exchange rate of the plurality of ions in the glass ceramics 10 with the potassium ions and the sodium ions in the first ion exchange bath 101 at the above temperature, and at the same time, in the first salt bath time, The potassium ions and sodium ions in the ion exchange bath 101 can be sufficiently exchanged with a plurality of ions in the glass ceramics 10.
  • the second ion exchange bath 102 includes 5% by weight to 20% by weight of potassium nitrate, and the second ion exchange bath 102 has a temperature of 400 ° C to 500 ° C.
  • the time of the secondary salt bath is 5 minutes to 30 minutes.
  • the second ion exchange bath 102 further includes a solvent, which may be a protic polar solvent or an aprotic polar solvent.
  • the weight percentage of potassium nitrate in the first ion exchange bath 101 may be 5% by weight, 6% by weight, 7% by weight, 8% by weight, 9% by weight, 10% by weight, 11% by weight, 12% by weight, and 13% by weight. Any one of 14% by weight, 15% by weight, 16% by weight, 17% by weight, 18% by weight, 19% by weight, or 20% by weight, or a value between any of the above.
  • the temperature of the first ion exchange bath 101 is any one of 400 ° C, 410 ° C, 420 ° C, 425 ° C, 430 ° C, 440 ° C, 450 ° C, 460 ° C, 470 ° C, 475 ° C, 480 ° C, 490 ° C, 500 ° C.
  • the time of the first salt bath is any one of 5 minutes, 10 minutes, 12 minutes, 15 minutes, 18 minutes, 20 minutes, 22 minutes, 25 minutes, 30 minutes, or a value between any two of the above.
  • the second ion exchange bath 102 can increase the exchange rate of the plurality of ions in the glass ceramics 10 with the potassium ions in the second ion exchange bath 102 at the above temperature, and at the same time, during the first salt bath time, the second ion exchange The potassium ions in the bath 102 can be sufficiently exchanged with a plurality of ions in the glass ceramics 10.
  • the strengthening method of the glass ceramic 10 further includes:
  • the glass ceramics 10 to be strengthened are subjected to initial strengthening by the first ion exchange bath 101, the surface of the first strengthened glass ceramic 20 adheres to the first ion exchange bath 101 and the ions displaced into the first ion exchange bath 101.
  • the effect of impurities on the second ion exchange bath 102 can be reduced by cleaning the primary strengthened glass ceramics 20.
  • the liquid used to clean the gas-enriched glass ceramics 20 may be the same as or different from the solute in the second ion exchange bath 102.
  • a method for fabricating a glass-ceramic cover 100 according to an embodiment of the present invention includes:
  • the first ion exchange bath 101 comprises potassium nitrate and sodium nitrate
  • the second ion exchange bath 102 comprises potassium nitrate
  • the glass ceramics 10 to be strengthened is placed in the first ion exchange bath 101 for the initial salt bath to obtain the primary strengthened glass ceramics 20;
  • the first strengthened glass-ceramic glass 20 is placed in the second ion exchange bath 102 for secondary salt bath to obtain secondary strengthened glass-ceramics 30;
  • the electrode layer 40 is screen printed on the surface of the second strengthened glass ceramic 30.
  • a film 50 is coated on the electrode layer 40 to form a glass-ceramic cover 100.
  • the glass ceramics of the embodiment of the present invention may be a boron-based glass ceramic or an aluminum-based glass ceramic.
  • the first ion exchange bath 101 is formed by dissolving potassium nitrate and sodium nitrate with a solvent.
  • the solvent may be a protic polar solvent, for example, the solvent may be any one of water, methanol, ethanol, isopropanol, nitromethane, formic acid, acetic acid, ethylene glycol, 1,3-propanediol, glycerin or A variety of combinations are formed.
  • the solvent may also be an aprotic polar solvent, for example, the solvent may be formed by any one or a combination of acetone, ethyl acetate, acetonitrile, dimethyl sulfoxide, tetrahydrofuran, dimethylformamide. Further, the solvent may be formed in a combination of protic solvents and aprotic solvents in different ratios.
  • the second ion exchange bath 102 is formed of potassium nitrate and a solvent which may be the same as the solvent component in the first ion exchange bath 101, and the content of the solvent component may be different.
  • exchange means introducing a cation (potassium ion, sodium ion) from the first ion exchange bath 101 into the glass ceramics 10 (or a surface portion of the glass ceramic 10) and making it in the first ion exchange bath 101.
  • the cation replaces the cation having the same valence state/charge/oxidation state in the glass-ceramics 10; alternatively, "exchange” may also mean introducing the cation (potassium ion, sodium ion) from the first ion exchange bath 101 into the glass-ceramic 10 (or the surface portion of the glass-ceramics 10) and the cations in the first ion exchange bath 101 are substituted for cations having different valence/charge/oxidation states in the glass-ceramics 10.
  • the primary strengthened glass ceramics 20 When the primary strengthened glass ceramics 20 is placed in the second ion exchange bath 102 for the secondary salt bath, the plurality of ions in the first strengthened glass ceramics 20 are exchanged with the potassium ions in the second ion exchange bath 102.
  • the strengthening method of the glass ceramics 10 according to the embodiment of the present invention can increase the linear expansion coefficient and hardness of the glass ceramics 10 under the premise that the light transmittance of the glass ceramics 10 is greater than or equal to 88%. , bending stress and strength, and reducing dielectric loss.
  • the electrode layer 40 can be a touch electrode layer.
  • the electrode layer 40 includes a touch electrode and an electrode lead.
  • the film 50 may be an insulating film for insulating the electrode layer 40 from contact with air to prevent the electrode layer 40 from being oxidized.
  • the method for fabricating the glass-ceramic cover 100 of the present invention improves the glass-ceramic by sequentially placing the glass-ceramics 10 to be strengthened into the first ion exchange bath 101 and the second ion exchange bath 102 in two salt baths.
  • the coefficient of linear expansion, hardness, bending stress, and strength of the cap plate 100, and dielectric loss are reduced.
  • the first ion exchange bath 101 comprises 0% by weight to 20% by weight of potassium nitrate, and 0% by weight to 10% by weight of sodium nitrate, and the temperature of the first ion exchange bath 101 is 400 ° C to 600 ° C,
  • the initial salt bath time is between 300 minutes and 720 minutes.
  • the first ion exchange bath 101 further includes a solvent, which may be a protic polar solvent or an aprotic polar solvent.
  • the weight percentage of potassium nitrate in the first ion exchange bath 101 may be 0% by weight, 2% by weight, 4% by weight, 5% by weight, 6% by weight, 8% by weight, 10% by weight, 12% by weight, and 14% by weight. Any one of 15% by weight, 16% by weight, 18% by weight, and 20% by weight, or a value between any of the above.
  • the weight percentage of sodium nitrate in the first ion exchange bath 101 may be 0% by weight, 1% by weight, 2% by weight, 3% by weight, 4% by weight, 5% by weight, 6% by weight, 7% by weight, and 8% by weight. Any one of 9% by weight and 10% by weight, or a value between any of the above.
  • the temperature of the first ion exchange bath 101 is any one of 400 ° C, 425 ° C, 450 ° C, 475 ° C, 500 ° C, 525 ° C, 550 ° C, 575 ° C, 600 ° C, or between any two of the above. .
  • the initial salt bath time is 300 minutes, 330 minutes, 360 minutes, 390 minutes, 400 minutes, 425 minutes, 450 minutes, 475 minutes, 500 minutes, 525 minutes, 550 minutes, 575 minutes, 600 minutes, 630 minutes, 660 minutes. Any one of 690 minutes, 700 minutes, and 720 minutes, or between any two of the above.
  • the first ion exchange bath 101 can increase the exchange rate of the plurality of ions in the glass ceramics 10 with the potassium ions and the sodium ions in the first ion exchange bath 101 at the above temperature, and at the same time, in the first salt bath time, The potassium ions and sodium ions in the ion exchange bath 101 can be sufficiently exchanged with a plurality of ions in the glass ceramics 10.
  • the first ion exchange bath 101 comprises 5% by weight to 15% by weight potassium nitrate, and 0.5% by weight to 5% by weight sodium nitrate, and the temperature of the first ion exchange bath 101 is 450 ° C to 500 ° C.
  • the initial salt bath time is between 400 minutes and 600 minutes.
  • the first ion exchange bath 101 further includes a solvent, which may be a protic polar solvent or an aprotic polar solvent.
  • the weight percentage of potassium nitrate in the first ion exchange bath 101 may be 5% by weight, 6% by weight, 7% by weight, 8% by weight, 9% by weight, 10% by weight, 11% by weight, 12% by weight, and 13% by weight. Any one of 14% by weight and 15% by weight, or a value between any of the above.
  • the weight percentage of sodium nitrate in the first ion exchange bath 101 may be 0.5% by weight, 1% by weight, 1.5% by weight, 2% by weight, 2.5% by weight, 3% by weight, 3.5% by weight, 4% by weight, 4.5% by weight.
  • the temperature of the first ion exchange bath 101 is any one of 450 ° C, 460 ° C, 470 ° C, 475 ° C, 480 ° C, 490 ° C, and 500 ° C, or a value between any of the above.
  • the time of the first salt bath is any one of 400 minutes, 425 minutes, 450 minutes, 475 minutes, 500 minutes, 525 minutes, 550 minutes, 575 minutes, 600 minutes, or a value between any two of the above.
  • the first ion exchange bath 101 can increase the exchange rate of the plurality of ions in the glass ceramics 10 with the potassium ions and the sodium ions in the first ion exchange bath 101 at the above temperature, and at the same time, in the first salt bath time, The potassium ions and sodium ions in the ion exchange bath 101 can be sufficiently exchanged with a plurality of ions in the glass ceramics 10.
  • the second ion exchange bath 102 comprises from 5% by weight to 20% by weight potassium nitrate, the second ion exchange bath 102 has a temperature of from 400 ° C to 500 ° C, and the secondary salt bath has a time of 5 Minutes - 30 minutes.
  • the second ion exchange bath 102 further includes a solvent, which may be a protic polar solvent or an aprotic polar solvent.
  • the weight percentage of potassium nitrate in the first ion exchange bath 101 may be 5% by weight, 6% by weight, 7% by weight, 8% by weight, 9% by weight, 10% by weight, 11% by weight, 12% by weight, and 13% by weight. Any one of 14% by weight, 15% by weight, 16% by weight, 17% by weight, 18% by weight, 19% by weight, or 20% by weight, or a value between any of the above.
  • the temperature of the first ion exchange bath 101 is any one of 400 ° C, 410 ° C, 420 ° C, 425 ° C, 430 ° C, 440 ° C, 450 ° C, 460 ° C, 470 ° C, 475 ° C, 480 ° C, 490 ° C, 500 ° C.
  • the time of the first salt bath is any one of 5 minutes, 10 minutes, 12 minutes, 15 minutes, 18 minutes, 20 minutes, 22 minutes, 25 minutes, 30 minutes, or a value between any two of the above.
  • the second ion exchange bath 102 can increase the exchange rate of the plurality of ions in the glass ceramics 10 with the potassium ions in the second ion exchange bath 102 at the above temperature, and at the same time, during the first salt bath time, the second ion exchange The potassium ions in the bath 102 can be sufficiently exchanged with a plurality of ions in the glass ceramics 10.
  • the method for manufacturing the glass-ceramic cover 100 further includes:
  • the glass ceramics 10 to be strengthened are subjected to initial strengthening by the first ion exchange bath 101, the surface of the first strengthened glass ceramic 20 adheres to the first ion exchange bath 101 and the ions displaced into the first ion exchange bath 101.
  • the effect of impurities on the second ion exchange bath 102 can be reduced by cleaning the primary strengthened glass ceramics 20.
  • the liquid used to clean the gas-enriched glass ceramics 20 may be the same as or different from the solute in the second ion exchange bath 102.
  • the method for fabricating the glass-ceramic cover 100 of the embodiment of the present invention further includes:
  • the fine glass ceramics 80 are cleaned to obtain the glass ceramics 10 to be strengthened.
  • the material of the glass-ceramic material 60 may include a nucleating agent (for example, titanium dioxide, zirconium dioxide), and the crystallized glass material 60 is nucleated and crystallized at a certain temperature (for example, 830 ° C).
  • the crystallization treatment can obtain crystallized glass ceramics 70 having finer crystal grains and more uniform structure.
  • Cutting the crystallized glass-ceramics 70 can obtain a fine-grained glass-ceramic 80 of a suitable size and structure.
  • a suitable structure can be understood as refining the structure of holes, grooves, chamfers and the like formed on the glass-ceramics 80. Grinding and refining the crystallized glass 80 can make the surface of the refined glass ceramic 80 smoother.
  • the cleaning and refining of the glass ceramics 90 can remove fine particles generated after grinding and refining the glass ceramics 80.
  • the refined glass ceramics 80 obtained after cleaning and refining the glass ceramics 80 may be the glass ceramics 10 to be strengthened.
  • the refined glass-ceramic 80 that can be obtained in the present embodiment has a suitable size and structure, a smooth surface quality, and a finer grain size.
  • the step of cutting the crystallized glass ceramic 70 to obtain the refined glass ceramics 80 includes:
  • the sheet glass ceramic 90 is cut to obtain a refined glass ceramic 80.
  • the sheet-like glass ceramic 90 obtained by cutting the crystallized glass ceramic 70 is a suitable size required by the user.
  • the dicing of the sheet-like glass-ceramics 90 can obtain a fine-grained glass-ceramic 80 of a suitable structure, and a suitable structure can be understood as a structure of refining pores, grooves, chamfers and the like formed on the glass-ceramics 80.
  • the fine crystallized glass 80 having an appropriate size and structure can be obtained.
  • the method for manufacturing the glass-ceramic cover 100 further includes:
  • the glass ceramics 80 are thermally bent and refined to obtain the glass ceramics 10 to be strengthened.
  • the thermally curved refining glass ceramic 80 includes thermally bending the edges of the glass ceramic 80 to form an edge of the glass ceramic 10 into a curved structure.
  • the glass ceramics 10 to be reinforced by a suitable shape can be obtained by refining the glass ceramics 80 by thermal bending.
  • the temperature of the hot-bending and refining glass ceramics 80 is 650° C. to 850° C., and the time for thermally bending and refining the glass ceramics 80 is 10 seconds to 60 seconds.
  • the pressure of the curved and refined glass-ceramics 80 is 0.1 MPa to 0.5 MPa.
  • the temperature of the hot-bending refining glass-ceramics 80 may be 650 ° C, 660 ° C, 680 ° C, 700 ° C, 720 ° C, 740 ° C, 760 ° C, 780 ° C, 800 ° C, 820 ° C, 840 ° C, 850 ° C One, or between any two.
  • the time for hot bending to refine the glass ceramic 80 may be one of 10 seconds, 15 seconds, 20 seconds, 25 seconds, 30 seconds, 35 seconds, 40 seconds, 45 seconds, 50 seconds, 55 seconds, 60 seconds, or Take a value between any two.
  • the pressure of the hot bending and refining glass ceramics 80 may be one of 0.1 MPa, 0.15 MPa, 0.2 MPa, 0.25 MPa, 0.3 MPa, 0.35 MPa, 0.4 MPa, 0.45 MPa, 0.5 MPa, or between any two. value.
  • the glass ceramics 10 obtained under the above-mentioned hot bending pressure, temperature and time have high strength, and the glass ceramics 10 does not return to its original shape.
  • the temperature of the hot-bending and refining glass ceramics 80 is 700° C. to 750° C.
  • the time for thermally bending and refining the glass ceramics 80 is 20 seconds to 40 seconds.
  • the pressure of the curved and refined glass-ceramics 80 is 0.2 MPa to 0.3 MPa.
  • the temperature of the hot bending refining glass ceramics 80 may be one of 700 ° C, 705 ° C, 710 ° C, 715 ° C, 720 ° C, 725 ° C, 730 ° C, 735 ° C, 740 ° C, 745 ° C, 750 ° C, Or take a value between any two.
  • the time for hot bending to refine the glass ceramic 80 may be 20 seconds, 22 seconds, 24 seconds, 25 seconds, 26 seconds, 28 seconds, 30 seconds, 32 seconds, 34 seconds, 35 seconds, 36 seconds, 38 seconds, 40 seconds. One of them, or a value between any two.
  • the pressure of the hot bending and refining glass ceramics 80 may be one of 0.2 MPa, 0.22 MPa, 0.24 MPa, 0.25 MPa, 0.26 MPa, 0.28 MPa, and 0.3 MPa, or a value between any two.
  • the glass ceramics 10 obtained under the above-mentioned hot bending pressure, temperature and time have high strength, and the glass ceramics 10 does not return to its original shape.
  • first and second are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated.
  • features defining “first” or “second” may include at least one of the features, either explicitly or implicitly.
  • the meaning of "a plurality” is at least two, such as two, three, etc., unless specifically defined otherwise.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

L'invention concerne un procédé de renforcement d'une vitrocéramique (10) et un procédé de fabrication d'une plaque de couverture en vitrocéramique (100), comprenant : (S11) la fourniture d'un premier bain d'échange d'ions (101) et d'un second bain d'échange d'ions (102), le premier bain d'échange d'ions (101) comprenant du nitrate de potassium et du nitrate de sodium, et le second bain d'échange d'ions (102) comprenant du nitrate de potassium ; (S12) le placement de la vitrocéramique (10) à renforcer dans le premier bain d'échange d'ions (101) pour un bain de sel primaire pour obtenir une vitrocéramique principalement renforcée (20) ; (S14) le placement de la vitrocéramique principalement renforcée (20) dans le second bain d'échange d'ions (102) pour un bain de sel secondaire pour obtenir une vitrocéramique secondairement renforcée (30). Le procédé augmente le coefficient de dilatation linéaire, la dureté, la contrainte de flexion et la résistance de la vitrocéramique, et réduit la perte diélectrique.
PCT/CN2018/071629 2018-01-05 2018-01-05 Procédé de renforcement de vitrocéramique et procédé de fabrication d'une plaque de couverture en vitrocéramique WO2019134133A1 (fr)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103553306A (zh) * 2013-10-25 2014-02-05 江苏铁锚玻璃股份有限公司 一种高速列车专用高强度钢化玻璃的制备方法
WO2015008763A1 (fr) * 2013-07-19 2015-01-22 旭硝子株式会社 Procédé de fabrication de verre chimiquement renforcé
WO2016117476A1 (fr) * 2015-01-20 2016-07-28 旭硝子株式会社 Verre chimiquement renforcé et son procédé de production
CN105837031A (zh) * 2016-03-03 2016-08-10 深圳市力沣实业有限公司 高强度化学强化玻璃、玻璃强化方法
CN106608713A (zh) * 2015-10-27 2017-05-03 蓝思科技股份有限公司 一种通过化学离子交换消除强化玻璃表面压应力的方法
CN107216032A (zh) * 2017-05-16 2017-09-29 东旭科技集团有限公司 一种玻璃用组合物和铝硅酸盐玻璃及其制备方法和应用

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015008763A1 (fr) * 2013-07-19 2015-01-22 旭硝子株式会社 Procédé de fabrication de verre chimiquement renforcé
CN103553306A (zh) * 2013-10-25 2014-02-05 江苏铁锚玻璃股份有限公司 一种高速列车专用高强度钢化玻璃的制备方法
WO2016117476A1 (fr) * 2015-01-20 2016-07-28 旭硝子株式会社 Verre chimiquement renforcé et son procédé de production
CN106608713A (zh) * 2015-10-27 2017-05-03 蓝思科技股份有限公司 一种通过化学离子交换消除强化玻璃表面压应力的方法
CN105837031A (zh) * 2016-03-03 2016-08-10 深圳市力沣实业有限公司 高强度化学强化玻璃、玻璃强化方法
CN107216032A (zh) * 2017-05-16 2017-09-29 东旭科技集团有限公司 一种玻璃用组合物和铝硅酸盐玻璃及其制备方法和应用

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