WO2023053786A1 - Procédé de production de verre renforcé - Google Patents

Procédé de production de verre renforcé Download PDF

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Publication number
WO2023053786A1
WO2023053786A1 PCT/JP2022/031820 JP2022031820W WO2023053786A1 WO 2023053786 A1 WO2023053786 A1 WO 2023053786A1 JP 2022031820 W JP2022031820 W JP 2022031820W WO 2023053786 A1 WO2023053786 A1 WO 2023053786A1
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WIPO (PCT)
Prior art keywords
glass
tempered glass
stress layer
chemical strengthening
compressive stress
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PCT/JP2022/031820
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English (en)
Japanese (ja)
Inventor
一嘉 中島
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日本電気硝子株式会社
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Publication of WO2023053786A1 publication Critical patent/WO2023053786A1/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 present invention relates to a method for manufacturing tempered glass having a compressive stress layer.
  • glass products such as cover glass for smartphones and windshields of automobiles sometimes use tempered glass with a reinforced surface for the purpose of preventing cracking and improving mechanical strength.
  • tempered glass In such tempered glass, a compressive stress layer is formed on the surface of the glass by a method such as chemical strengthening treatment, thereby suppressing the occurrence of scratches and the extension of cracks.
  • An object of the present invention is to provide a method for producing tempered glass that can reliably and stably produce tempered glass having a compressive stress layer.
  • the method for producing tempered glass according to the present invention includes a forming step of obtaining tempered glass by thermoforming glass, and chemically tempering the tempered glass to obtain tempered glass having a compressive stress layer on the surface.
  • the tempered glass has a first main surface and a second main surface facing each other, and in the determining step, a compressive stress layer is formed on the first main surface of the tempered glass. and confirming that a tensile stress layer is formed on the second main surface, and the non-stress layer existing between the compressive stress layer and the tensile stress layer in the thickness direction of the tempered glass It is preferable to determine the presence or absence of chemical strengthening by checking the position.
  • chemical strengthening is performed by confirming that the center position in the thickness direction of the non-stress layer exists on the compressive stress layer side of the center position in the thickness direction of the tempered glass. It is preferable to determine that
  • the present invention further comprises a confirmation step of confirming the position of the stress-free layer inside the tempered glass before the chemical strengthening by cross Nicols observation with a polarizing microscope, and in the determination step, the inside of the tempered glass confirming that the center position in the thickness direction of the stress-free layer in is shifted to the compressive stress layer side from the center position in the thickness direction of the stress-free layer inside the tempering glass before the chemical strengthening. It is preferable to determine that chemical strengthening has been performed.
  • thermoform the glass by a redraw method in the forming step.
  • the tempered glass is a glass tube, and in the tempering step, the tempering glass is chemically tempered so that the compressive stress layer is formed on the outer surface of the glass tube.
  • a tempered glass manufacturing method capable of reliably and stably manufacturing tempered glass having a compressive stress layer.
  • FIG. 1 is a schematic cross-sectional view showing tempering glass before chemical strengthening in the case of manufacturing a glass tube as tempered glass.
  • FIG. 2 is a schematic cross-sectional view showing tempered glass after chemical strengthening in the case of manufacturing a glass tube as tempered glass.
  • FIG. 3 is a photograph showing the tempering glass before chemical strengthening obtained by crossed Nicols observation with a polarizing microscope.
  • FIG. 4 is a photograph showing tempered glass after chemical strengthening obtained by crossed Nicols observation with a polarizing microscope.
  • tempered glass is obtained by thermoforming glass (forming step).
  • the tempered glass obtained in the molding step is chemically tempered to obtain tempered glass having a compressive stress layer on its surface (strengthening step).
  • stress layer was formed on the surface of the tempered glass obtained in the tempering process, and the position of the stress-free layer inside the tempered glass was confirmed. , to discriminate the presence or absence of chemical strengthening (discrimination step).
  • the method for producing tempered glass of the present invention has the above configuration, so that tempered glass having a compressive stress layer can be produced reliably and stably. This point can be explained as follows.
  • the compressive stress layer in tempered glass can be confirmed by cross-Nicol observation using a polarizing microscope. In the crossed nicols observation with a polarizing microscope, it can be determined that the high-brightness portion in the obtained image is the compressive stress layer.
  • the tempered glass that has undergone the thermoforming process is chemically strengthened, in the crossed Nicols observation with a polarizing microscope, the tempered glass before chemical strengthening sometimes has a high brightness portion. In this case, it was difficult to distinguish the difference in brightness before and after chemical strengthening, and it was sometimes impossible to confirm the presence or absence of the formation of a compressive stress layer. Therefore, there is a problem that it is difficult to reliably and stably obtain tempered glass having a compressive stress layer.
  • the present inventors found that, when producing tempered glass by thermoforming by a method such as the redraw method, the stress remains inside due to quenching and air-cooling tempering is performed. It was found that a stress layer may be formed, and this is the cause of the observation of high brightness areas even in tempered glass before chemical strengthening. Therefore, even if a compressive stress layer is formed on the surface of this tempered glass by subsequent chemical strengthening, it is difficult to determine whether it is a compressive stress layer formed by thermoforming or a compressive stress layer formed by chemical strengthening. There was a problem that it was difficult to determine.
  • the inventor of the present invention confirms the position of the stress-free layer inside the obtained tempered glass, thereby confirming the chemical strengthening. It was found that the presence or absence can be determined.
  • the presence or absence of chemical strengthening can be determined as follows.
  • the following embodiment demonstrates the case where the glass for strengthening before chemical strengthening is obtained by the redraw method.
  • FIG. 1 is a schematic cross-sectional view showing tempering glass before chemical strengthening in the case of manufacturing a glass tube as tempered glass.
  • FIG. 1 is a schematic diagram of a cross section of the tempering glass 1 perpendicular to the tube length direction.
  • a compressive stress layer 2 is formed by quenching on the outer surface 1a of the tempering glass 1 that has been thermoformed by the redraw method before being chemically tempered.
  • a tensile stress layer 3 is formed on the inner surface 1b of the tempering glass 1 .
  • stress-free layers 4 are formed between the compressive stress layers 2 and the tensile stress layers 3 in the thickness direction T of the tempering glass 1 by canceling each other's stresses.
  • FIG. 2 is a schematic cross-sectional view showing tempered glass after chemical strengthening in the case of manufacturing a glass tube as tempered glass.
  • the tempered glass 10 shown in FIG. 2 is tempered glass obtained by chemically strengthening the outer surface 1a side of the tempering glass 1 shown in FIG.
  • FIG. 2 is a schematic diagram of a cross section of the tempered glass 10 perpendicular to the tube length direction.
  • the center position T2 in the thickness direction of the stress-free layer 4 exists in the tempered glass 10 obtained by chemically strengthening the outer surface 1a side of the tempering glass 1 shown in FIG. .
  • the position of the stress-free layer 4 can be confirmed by cross Nicols observation with a polarizing microscope.
  • FIG. 3 is a photograph showing the tempering glass before chemical strengthening obtained by cross-Nicol observation with a polarizing microscope.
  • FIG. 4 is a photograph showing tempered glass after chemical strengthening obtained by crossed Nicols observation with a polarizing microscope.
  • the high-brightness (bright) portion is the stress layer
  • the low-brightness (dark) portion sandwiched between the high-brightness stress layers is the non-stress layer 4 .
  • the compressive stress layer 2 is a bright (bright) portion of the outer surface 1a
  • the tensile stress layer 3 is a bright (bright) portion of the inner surface 1b.
  • the direction of the arrow is a diagonal position.
  • the thickness direction center position T2 of the stress-free layer 4 exists on the side of the compressive stress layer 2 that is closer to the outer surface 1a than the thickness direction center position T1 of the tempered glass 10. It can be seen that 3 and 4, the center position T2 in the thickness direction of the stress-free layer 4 in the tempered glass 10 after chemical strengthening is closer to the center position T0 in the thickness direction of the stress-free layer 4 in the tempered glass 1 before chemical strengthening. It can be seen that there is a shift toward the compressive stress layer 2 side, which is the outer surface 1a side.
  • the distance L2 from the thickness direction central position T2 of the non-stress layer 4 to the compressive stress layer 2 and the distance from the thickness direction central position T1 of the tempered glass 10 to the compressive stress layer 2
  • the ratio (L2/L1) to L1 is preferably 0.9 or less, more preferably 0.8 or less.
  • the thickness direction center position T2 of the stress-free layer 4 exists on the compressive stress layer 2 side from the thickness direction center position T1 of the tempered glass 10. Therefore, it can be determined that chemical strengthening has been performed.
  • the stress-free layer 4 in the tempered glass 10 Chemical strengthening is performed by confirming that the center position T2 in the thickness direction of is shifted to the side of the compressive stress layer 2 from the center position T0 in the thickness direction of the non-stress layer 4 in the tempering glass 1 before chemical strengthening. It can be determined that However, in the present invention, the step of confirming the position of the stress-free layer 4 inside the tempering glass 1 before chemical strengthening may be omitted.
  • crossed Nicols observation with a polarizing microscope can be performed by vertically illuminating the cross-section, which is the observation surface of the tempered glass 10, with polarized light through a polarizing microscope and observing with crossed Nicols.
  • a polarizing microscope for example, product number "BX53-P" manufactured by Olympus can be used.
  • the tempered glass 10 may be subjected to observation after etching or polishing the cross section, which is the observation surface of the tempered glass 10 .
  • the high-brightness (bright) part is the stress layer
  • the low-brightness (dark) part is the non-stress layer. Therefore, in cross Nicols observation with a polarizing microscope, the thickness of the stress layer can be obtained from the area where the high-brightness (bright) part is provided, and the thickness of the non-stress layer can be obtained from the area where the low-brightness (dark) part is provided. can be asked for.
  • the thickness of the compressive stress layer 2 in the tempering glass 1 can be, for example, 0.05 mm or more and 0.3 mm or less. Moreover, the thickness of the compressive stress layer 2 in the tempered glass 10 can be, for example, 0.01 mm or more and 0.25 mm or less.
  • the thickness of the non-stress layer 4 in the tempered glass 1 can be, for example, 0.3 mm or more and 0.6 mm or less. Moreover, the thickness of the non-stress layer 4 in the tempered glass 10 can be, for example, 0.1 mm or more and 0.4 mm or less.
  • the thickness of the tensile stress layer 3 in the tempering glass 1 can be, for example, 0.05 mm or more and 0.3 mm or less. Moreover, the thickness of the tensile stress layer 3 in the tempered glass 10 can be, for example, 0.1 mm or more and 0.4 mm or less.
  • the compressive stress value of the compressive stress layer 2 in the tempered glass 10 after chemical strengthening is preferably 3 MPa or more, more preferably 5 MPa or more.
  • the mechanical strength of the tempered glass 10 can be further enhanced.
  • the compressive stress value of the compressive stress layer 2 can be calculated, for example, by observing the number of interference fringes and their intervals using a surface stress meter.
  • borosilicate glass has an optical elastic constant of 34.0 [(nm/cm)/MPa]
  • aluminosilicate glass has an optical elastic constant of 29.0 [(nm/cm)/MPa]. (nm/cm)/MPa].
  • FSM-6000 manufactured by Toshiba Corporation can be used as a surface stress meter.
  • the tensile stress value of the tensile stress layer 3 in the tempered glass 10 after chemical strengthening can be, for example, 1 MPa or more and 3 MPa or less.
  • the tensile stress value of the tensile stress layer 3 can be derived, for example, by calculating the stress from the results of birefringence measurements.
  • the stress value of the non-stress layer 4 in the tempered glass 1 and tempered glass 10 is preferably 1 MPa or less, more preferably 0.5 MPa or less, even more preferably 0.2 MPa or less, and particularly preferably 0 MPa.
  • the tempered glass 10 is a glass tube.
  • the tempered glass 10 may be glass having another shape such as a glass plate, and the shape is not particularly limited. However, from the viewpoint of obtaining the effects of the present invention more reliably, it is preferable that the tempered glass 10 is a glass tube.
  • the thickness of the tempered glass 10 is not particularly limited, it is preferably 0.3 mm or more, more preferably 0.5 mm or more, preferably 10 mm or less, and more preferably 5 mm or less. When the thickness of the tempered glass 10 is within the above range, it is possible to further increase the mechanical strength while maintaining the production efficiency of the tempered glass 10 .
  • the inner diameter of the tempered glass 10 is not particularly limited, but is preferably 0.1 mm or more, more preferably 0.8 mm or more, still more preferably 1 mm or more, preferably 10 mm or less, more preferably 5 mm or less, and still more preferably 3 mm. It is below.
  • thermoforming may be performed by blow molding, Danner molding, or the like, and is not particularly limited. Any method may be used as long as a stress layer or a non-stress layer is formed on the glass for strengthening 1 before chemical strengthening. However, from the viewpoint of obtaining the effects of the present invention more reliably, it is desirable to obtain the tempering glass 1 by thermoforming by a redraw method.
  • tempering glass for example, a glass having a known composition that enables chemical strengthening by ion exchange can be used.
  • the glass composition is SiO 2 50% to 80%, Al 2 O 3 1% to 20%, B 2 O 3 0% to 20%, and Na 2 O 1% in terms of mass %. 20%, K 2 O 0%-15%, Li 2 O 0%-10%.
  • SiO2 is a component that forms the network of glass.
  • the content of SiO2 is preferably 53% or more, more preferably 55% or more, still more preferably 60% or more, preferably 78% or less, more preferably 75% or less, even more preferably 72% or less.
  • the content of SiO 2 is equal to or higher than the above lower limit, vitrification is further facilitated, and acid resistance can be further enhanced.
  • the content of SiO 2 is equal to or less than the above upper limit, the meltability and formability can be further improved. Also, since the coefficient of thermal expansion does not become too low, it is possible to more easily match the coefficient of thermal expansion of the surrounding materials.
  • Al 2 O 3 is a component that increases the ion exchange rate, and also a component that increases the Young's modulus and hardness.
  • the content of Al 2 O 3 is preferably 3% or more, more preferably 4% or more, still more preferably 5% or more, preferably 18% or less, more preferably 15% or less, further preferably 12% or less. is.
  • the content of Al 2 O 3 is at least the above lower limit, the ion exchange rate and Young's modulus can be further improved, the acid resistance can be further improved, and the acid treatment process can be applied more easily. can do.
  • the content of Al 2 O 3 is equal to or less than the above upper limit, the high-temperature viscosity can be lowered, and the meltability can be further improved.
  • B 2 O 3 is a component that lowers high-temperature viscosity and density and increases devitrification resistance.
  • the content of B 2 O 3 is not particularly limited, but is preferably 18% or less, more preferably 16% or less, still more preferably 14% or less, and particularly preferably 12% or less.
  • the ion exchange rate can be further increased.
  • coloration of the glass surface due to ion exchange can be further suppressed, and acid resistance and water resistance can be further improved.
  • Na 2 O is an ion-exchange component and also a component that lowers high-temperature viscosity and enhances meltability and moldability. Na 2 O is also a component that enhances devitrification resistance.
  • the content of Na 2 O is not particularly limited, and is preferably 2% or more, more preferably 3% or more, still more preferably 5% or more, preferably 18% or less, more preferably 15% or less, and even more preferably. is 12% or less.
  • the meltability and thermal expansion coefficient can be further increased, and the ion exchange rate can be further increased.
  • acid resistance and devitrification resistance can be further improved.
  • K 2 O is a component that lowers high-temperature viscosity and improves meltability and moldability. It is also a component that increases devitrification resistance and Vickers hardness.
  • the content of K 2 O is not particularly limited, and is preferably 0.1% or more, more preferably 1% or more, still more preferably 2% or more, preferably 10% or less, more preferably 5% or less, More preferably less than 3%. When the K 2 O content is within the above range, the acid resistance and devitrification resistance can be further improved.
  • Li 2 O is an ion-exchange component that lowers high-temperature viscosity and improves meltability and moldability. It is also a component that increases Young's modulus. Furthermore, Li 2 O is also a component that elutes out during the ion exchange treatment and deteriorates the ion exchange solution. Therefore, the content of Li 2 O is preferably 0.01% or more, preferably 2% or less, more preferably 1% or less, and still more preferably 0.1% or less.
  • the following components can be included in the glass as components other than the above.
  • MgO is a component that lowers high-temperature viscosity and improves meltability and moldability. It is also a component that increases Young's modulus to increase Vickers hardness and acid resistance.
  • the content of MgO is preferably 0.1% or more, more preferably 1% or more, still more preferably 2% or more, preferably 4.5% or less, more preferably 3% or less, further preferably 2.0% or more. 5% or less. When the content of MgO is within the above range, the ion exchange rate can be further increased, and the devitrification of the glass can be made more difficult.
  • P 2 O 5 is a component that increases the ion exchange rate while maintaining the compressive stress value.
  • the content of P 2 O 5 is preferably 2% or more, more preferably 3.5% or more, still more preferably 4.5% or more, preferably 8% or less, more preferably 6% or less, still more preferably is 5% or less.
  • water resistance can be further improved.
  • Cl, SO 3 or CeO 2 may be added as a refining agent to the glass constituting the tempered glass, and Cl or SO 3 is preferably added.
  • the content of the clarifier can be, for example, 0% or more and 3% or less.
  • the glass constituting the tempering glass may contain SnO 2 .
  • SnO2 has the effect of enhancing the ion exchange performance.
  • the SnO 2 content is preferably 0.01% or more, more preferably 0.05% or more, still more preferably 0.1% or more, and preferably 3% or less.
  • the content of Fe 2 O 3 in the glass constituting the tempering glass is preferably less than 1000 ppm (less than 0.1%), more preferably less than 400 ppm, still more preferably less than 300 ppm.
  • the transmittance (400 nm to 770 nm) at a plate thickness of 1 mm can be further improved.
  • the content of rare earth oxides such as Nb 2 O 5 and La 2 O 3 in the glass constituting the tempered glass is preferably 3% or less, more preferably 1% or less, and still more preferably 0.1% or less. be. In this case, devitrification resistance can be further improved.
  • the glass constituting the tempering glass does not substantially contain As 2 O 3 , Sb 2 O 3 and PbO in terms of the glass composition.
  • substantially no Bi 2 O 3 or F is contained from environmental considerations.
  • the glass to be tempered can be obtained by heat-melting the glass prepared so as to have the glass composition described above and thermoforming the melt by a redraw method or the like.
  • the heating and melting of the frit can be performed, for example, by putting the frit into a continuous melting furnace and heating it at 1500°C to 1600°C. It can be carried out.
  • the tempered glass can be produced by chemically tempering the tempered glass thus obtained.
  • the chemical strengthening method is a method of introducing alkali ions having a large ionic radius to the surface of the glass for strengthening by ion exchange treatment at a temperature below the strain point of the glass. With the chemical strengthening method, a compressive stress layer can be formed satisfactorily even if the thickness of the glass to be strengthened is thin, so that desired mechanical strength can be obtained.
  • the conditions for the ion exchange treatment are not particularly limited, and may be determined in consideration of the viscosity characteristics of the tempering glass.
  • the ion exchange treatment can be performed by immersing the tempering glass in a potassium nitrate solution at 400° C. to 550° C. for 1 hour to 8 hours.
  • composition of the tempered glass obtained by subjecting the tempering glass to ion exchange treatment can be the same as the composition of the tempering glass before the ion exchange treatment.

Abstract

L'invention concerne un procédé de production de verre renforcé grâce auquel du verre renforcé ayant une couche de contrainte de compression peut être produit de manière fiable et stable.　Ce procédé de production de verre renforcé 10 comprend : une étape de moulage pour obtenir, par thermoformage du verre, un verre à renforcer ; une étape de renforcement pour obtenir du verre renforcé 10 comprenant une couche de contrainte de compression 2 sur une surface 1a par renforcement chimique du verre à renforcer ; et une étape de détermination pour déterminer si un renforcement chimique s'est produit en confirmant, par observation Nicol croisée à l'aide d'un microscope polarisant, que les couches de contrainte 2, 3 ont été formées sur les surfaces 1a, 1b du verre renforcé 10, et confirmant la position d'une couche sans contrainte 4 à l'intérieur du verre renforcé 10.
PCT/JP2022/031820 2021-09-28 2022-08-24 Procédé de production de verre renforcé WO2023053786A1 (fr)

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JP2021157664A JP2023048384A (ja) 2021-09-28 2021-09-28 強化ガラスの製造方法
JP2021-157664 2021-09-28

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001294442A (ja) * 2000-02-10 2001-10-23 Sony Corp 陰極線管用ガラスパネルおよびこれを用いた陰極線管ならびに陰極線管の製造方法
JP2005174500A (ja) * 2003-12-12 2005-06-30 Hoya Corp 情報記録媒体用ガラス基板の製造方法
JP2014028730A (ja) * 2012-07-31 2014-02-13 Asahi Glass Co Ltd 化学強化ガラスの製造方法およびガラスの応力測定方法
JP2014040353A (ja) * 2012-08-23 2014-03-06 Nippon Electric Glass Co Ltd 化学強化結晶化ガラス物品
JP2016536650A (ja) * 2013-09-17 2016-11-24 コーニング インコーポレイテッド イオン交換可能なフュージョンドローガラス板を用いた広帯域偏光子

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001294442A (ja) * 2000-02-10 2001-10-23 Sony Corp 陰極線管用ガラスパネルおよびこれを用いた陰極線管ならびに陰極線管の製造方法
JP2005174500A (ja) * 2003-12-12 2005-06-30 Hoya Corp 情報記録媒体用ガラス基板の製造方法
JP2014028730A (ja) * 2012-07-31 2014-02-13 Asahi Glass Co Ltd 化学強化ガラスの製造方法およびガラスの応力測定方法
JP2014040353A (ja) * 2012-08-23 2014-03-06 Nippon Electric Glass Co Ltd 化学強化結晶化ガラス物品
JP2016536650A (ja) * 2013-09-17 2016-11-24 コーニング インコーポレイテッド イオン交換可能なフュージョンドローガラス板を用いた広帯域偏光子

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