WO2011103798A1 - Verre chimiquement renforcé susceptible d'être postérieurement découpé - Google Patents

Verre chimiquement renforcé susceptible d'être postérieurement découpé Download PDF

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Publication number
WO2011103798A1
WO2011103798A1 PCT/CN2011/071155 CN2011071155W WO2011103798A1 WO 2011103798 A1 WO2011103798 A1 WO 2011103798A1 CN 2011071155 W CN2011071155 W CN 2011071155W WO 2011103798 A1 WO2011103798 A1 WO 2011103798A1
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Prior art keywords
glass
subsequent cutting
cutting according
less
chemically
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PCT/CN2011/071155
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English (en)
Chinese (zh)
Inventor
王冲
乔斯·西默
巴塞尔·马蒂亚斯
Original Assignee
肖特玻璃科技(苏州)有限公司
尚光强
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Publication of WO2011103798A1 publication Critical patent/WO2011103798A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • 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
    • 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
    • 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
    • C03C3/093—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium containing zinc or zirconium
    • 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
    • C03C3/095—Glass compositions containing silica with 40% to 90% silica, by weight containing rare earths
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/097—Glass compositions containing silica with 40% to 90% silica, by weight containing phosphorus, niobium or tantalum

Definitions

  • the present invention relates to a thin glass that can be cut after chemical tempering.
  • the present invention relates to a silicate glass having high strength, high fracture toughness, and high wear resistance, which has chemical tempering properties and can be laser cut after tempering.
  • the present invention relates to glass which can be used in electronic product screens and other fields involving high-strength thin glass, and which can perform subsequent laser cutting after chemical tempering.
  • the invention also relates to a chemical tempering process for the silicate glass. Background technique
  • Thin glass typically less than 2 mm thick, cannot be physically tempered. Therefore, thin glass having a thickness of less than 2 mm is usually selected from chemical tempering.
  • Chemically tempered glass is known in the art and is described, for example, in the patents US 4,156,755 and DE 4,206,268 A1.
  • the chemically tempered glass is machined such as edging, cutting, etc., which has a high defect rate or cannot be processed at all. This is because the higher internal stresses in the glass product during processing can lead to unpredictable cracking.
  • cutting tempered glass can bring significant economic benefits. In special cases, it is advantageous to cut the tempered thin glass because it can temper large pieces of flat glass and then cut it to increase the yield.
  • the most common methods of glass cutting are, for example, mechanical cutter cutting, water jet or laser cutting.
  • Laser cutting has the advantages of no chipping, difficulty in peeling and high boundary quality.
  • the high quality of the boundary after laser cutting can eliminate the subsequent processing of the boundary, and the good surface quality can improve the scratch resistance of the glass, thereby eliminating the need for subsequent surface treatment. It is therefore necessary to obtain such high-strength glass that can be subjected to subsequent mechanical or laser cutting.
  • the conventional glass cutting method uses mechanical force to cut the glass surface, and introduces an external force to separate the glass and complete the cutting. Using this method, microcracks remain on the edges of the glass, peeling, the glass surface is destroyed, and glass debris remains.
  • laser cutting is widely used in the field of glass cutting with its excellent cutting quality.
  • the glass is separated by the tension introduced by the laser.
  • CO 2 laser cutting As an example, the CO 2 laser can theoretically be completely absorbed by various glasses.
  • the glass is directly melted by a laser to separate the glass. At this time, the temperature of the glass is much greater than the transition point T g of the glass.
  • the second method pulsed laser heating of the glass a slight dot-like areas to a portion slightly larger than the temperature, T g, the glass removed in these regions of the glass breaking.
  • the glass is heated to a temperature slightly below the T g, and then rapidly cooled. A crack caused by tension will separate the glass.
  • the third laser cutting method can reduce edge defects. It is enough to increase the mechanical strength of the glass.
  • laser cutting is not limited by the shape of the cut, there is no mechanical wear, and it does not come into contact with the processed object, so that the laser cutting hardly produces glass debris, which is suitable for use in a clean room. Summary of the invention
  • the present invention relates to a chemically toughened glass that can be cut.
  • the glass is a silicate glass comprising aluminosilicate glass, borosilicate glass or the like.
  • the cutting method is performed by mechanical force or laser cutting.
  • the present invention provides a glass article which is capable of laser cutting after chemical tempering.
  • the glass article may be a flat glass.
  • the glass product may be a glass tube.
  • the thickness of the glass sheet is between 0.3 and 2.0 mm.
  • the invention also provides a method of tempering in which the tempered glass is cleavable.
  • the glass is a silicate glass.
  • the surface stress of the tempered glass is less than 1200 MPa. Further, the surface stress of the tempered glass is less than 900 MPa.
  • the surface stress of the tempered glass is less than 800 MPa. Further, the center stress of the tempered glass is less than 600 MPa. After tempering, the center stress of the glass is less than 60 MPao. Further, the center stress of the tempered glass is less than 40 MPa. Further, the center stress of the tempered glass is less than 20 MPao. Further, the center stress of the tempered glass is less than 15 MPa.
  • the depth of the ion exchange layer of the tempered glass is less than 50 ⁇ m. Further, the depth of the ion exchange layer of the tempered glass is less than 30 ⁇ m. Further, the ion exchange of the tempered glass The layer depth is less than 20 ⁇ m.
  • the depth of the ion exchange layer of the tempered glass is less than 15 ⁇ m.
  • the ratio of the ion exchange layer depth to the glass thickness of the tempered glass is less than 0.08.
  • the ratio of the depth of the ion exchange layer to the thickness of the glass after the tempered glass is less than 0.05.
  • the ratio of the depth of the ion exchange layer to the thickness of the glass of the tempered glass is less than 0.03.
  • the ratio of the ion exchange layer depth to the glass thickness of the tempered glass is less than 0.02.
  • the value of the tempered glass (ion exchange layer depth X surface compressive stress ⁇ glass thickness) should be less than 30.
  • the value of the tempered glass should be less than 20. Further, the value of the tempered glass (ion exchange layer depth X surface compressive stress + glass thickness) should be less than 10. Further, the value of the tempered glass (ion exchange layer depth X surface compressive stress ⁇ glass thickness) should be less than 5.
  • the invention also provides a method of cutting chemically tempered glass. Further, this method uses (0 2 laser for cutting. Further, the power of the CO 2 laser beam is 50-1000 watts. Further, the power of the CO 2 laser beam is in the range of 60-800 watts. the power of the laser beam 02. further, the power CO 2 laser beam.
  • the moving speed of the laser beam is 20-1500 mm / sec in the range of 80-300 watts in the range 80-500 watts. Further, the moving speed of the laser beam is between 40 and 1200 mm/sec. Further, the moving speed of the laser beam is between 60 and 800 mm/sec. Further, the moving speed of the laser beam is 80-500 mm/ Other laser cutting methods such as YAG: Nd laser, green laser, etc. can be used for the cutting of the chemically strengthened glass of the present invention.
  • Figure 1 Relationship between surface compressive stress, tensile stress, stress layer depth, and glass thickness (surface compressive stress is fixed at 800 MPa).
  • FIG. 1 The photo shows the edge of a laser-cut chemically tempered glass.
  • Figure 3 The photo shows the edge of a chemically tempered glass cut by a common cutter wheel.
  • the alkali metal ions with a large radius in the salt bath penetrate into the network structure of the glass by ion exchange, and exchange the alkali metal ions with a small radius in the glass to form a layer of tens of microns deep on the surface of the glass. Compressive stress layer. Glass strength is enhanced during this process.
  • Protective cover glass for use in touch screen products such as smart phones, tablets, etc. typically requires chemical tempering to increase its strength and scratch resistance.
  • Chemical tempered glass has different compressive stress range of 200-1500 MPa and ion exchange layer depth range of 10-150 micrometers due to different types of glass, chemical tempering salt bath composition, exchange time and temperature.
  • the tensile stress In order to balance the compressive stress of the surface, the tensile stress accumulates in the middle of the glass.
  • the magnitude of the tensile stress is related to the thickness of the glass, the surface compressive stress, and the depth of the ion exchange layer.
  • the tensile stress of chemically tempered glass ranges from a few MPa to 100 MPa.
  • Conventional glass cutting methods have difficulty scratching the surface of the tempered glass, or the depth of the scratch is not sufficient to cut the glass. As long as the depth of the ion exchange layer is greater than a certain limit, even if scratches are formed on the surface, since the ion exchange layer is not scratched, the externally applied tensile stress cannot be concentrated on the edge of the scratch, so that the entire glass cannot be broken along the scratch.
  • the glass article described above may be a flat glass.
  • the tempered glass may have a size greater than 50 cm 2 , may be greater than 100 cm 2 , may be greater than 1000 cm 2 , or may be greater than 2000 cm 2 .
  • the tempered glass may also have a size of less than 50 cm 2 .
  • 500-800 Kg/mm 2 more preferably 550-750 Kg/mm 2 , and the optimum range is 550-700 Kg/mm 2 .
  • CTE is the most important parameter for the tensile stress generated during the cooling of glass after heating. Large CTE glass will produce large tensile stress during the cutting process, making the glass easier to cut. However, if the CTE is too large, the glass will be susceptible to uncontrollable cracking due to thermal shock during cutting and chemical tempering. To meet these requirements, a preferred CTE range for glass 5.0-11.0xlO- 6 / ° C, more preferably in the range of 5.0-10.0xlO '6 / ° C, the optimal range of 5.0-9.0xlO- 6 / ° C.
  • the mechanical properties of glass products after chemical tempering are defined by the surface compressive stress (CS), central tensile stress (CT) and ion exchange layer depth (DoL) of the glass.
  • CS surface compressive stress
  • CT central tensile stress
  • DoL ion exchange layer depth
  • the central tensile stress should be less than 60 MPa, more preferably less than 40 MPa, more preferably less than 20 MPa, and most preferably less than 15 MPa.
  • the surface compressive stress of the chemically tempered glass should be less than 1200 MPa, more preferably less than 900 MPa, preferably less than 800 MPa, preferably less than 600 MPao.
  • the depth of the ion exchange layer is in the range of 0-50 microns, preferably in the range of 0- 30 microns, more preferably 0-20 microns, with an optimum range of 0-15 microns.
  • the chemically tempered glass must also satisfy the ion exchange layer depth and the glass thickness ratio of less than 0.08, more preferably less than 0.05, and preferably less than 0.03. , preferably less than 0.02.
  • laser-cut chemically tempered glass must meet a range of conditions such as thickness, surface compressive stress, and ion exchange layer depth:
  • the value of (ion exchange layer depth X surface compressive stress ⁇ glass thickness) should be less than 30, more preferably less than 20, preferably less than 10, and most preferably less than 5.
  • the central tensile stress of different thicknesses of glass varies with the depth of the ion exchange layer as shown. If the central tensile stress layer is required to be equal to 40 MPa, the depth of the ion exchange layer should be: 0.3 mm of glass of about 15 ⁇ m, 0.5 mm of glass of about 25 ⁇ m, 0.7 mm of glass of about 35 ⁇ m, and 1.0 mm of glass of about 50 ⁇ m.
  • the chemically tempered glass was subjected to CO 2 laser cutting.
  • CO 2 laser beam power Within the range of 50-1000 watts, the power of the optimized CO 2 laser beam is in the range of 60-800 watts, and the power of the better CO 2 laser beam is in the range of 80-500 watts, the optimal CO 2 laser The power of the beam is in the range of 80-300 watts.
  • the moving speed of the laser beam is between 20 and 1500 mm/sec
  • the moving speed of the optimized laser beam is between 40 and 1200 mm/sec
  • the moving speed of the better laser beam is 60-800 mm/sec.
  • the optimal movement speed of the laser beam is
  • Sodium aluminosilicate glass contains Na+ ions and is a typical glass that can be chemically tempered. This glass has a coefficient of thermal expansion between 4 and 15 ppm.
  • the ion exchange between Na + o K+ was carried out in a KNO 3 salt bath.
  • the glass is usually treated in a salt bath furnace at a temperature of 390-460 ° C for 1-8 hours.
  • the ion exchange layer of the glass thus treated has a depth of between 10 and 120 microns. Shorter processing times and lower processing temperatures are advantageous for laser cutting.
  • the temperature of the salt bath ranges from 380 to 440 ° C, more preferably from 380 to 420 ° C, and most preferably from 380 to 400 ° C.
  • the treatment time is 1 to 4 hours, more preferably 1 to 3 hours, and preferably 1 to 2 hours.
  • Lithium aluminosilicate glass is an aluminosilicate glass containing Li 2 0. Since the inclusion of Li 2 O means that such a glass can be treated with a NaNO 3 salt bath, and because Li + ⁇ Na+ diffuses rapidly in the salt bath, it has a fast ion exchange rate.
  • the surface compressive stress of NaN0 3 treated glass is usually lower than that of KNO 3 treated glass, but the depth of ion exchange layer can be easily reached.
  • the cutting of the glass can be achieved by controlling the chemical tempering conditions.
  • the time and temperature for tempering with NaNO 3 are: 1-60 minutes, preferably 1-30 minutes, preferably 1-15 minutes, temperature 360-390 ° C, better at 360-380 ° C, most Good for 360-370 ° C.
  • the glass is treated with KNO 3 , since the diffusion speed of Li + ⁇ K + is low, the depth of the ion exchange layer is small, that is,
  • Borosilicate glass is a silicate glass containing a certain amount of B 2 O 3 as a network structure. This glass tends to have a lower coefficient of thermal expansion. Because of the presence of B 2 O 3 , the network structure of the glass is denser than ordinary silicate glass. Dense structure leads to the exchange of alkali metal ions The velocity into the glass structure is relatively slow and the depth of the ion exchange layer is not deep. Therefore, after chemical tempering, the glass can be laser cut.
  • the optimized temperature range for chemical tempering is
  • the optimum range is 420-480 ° C
  • the tempering time is optimized in the range of 1-30 hours, more preferably in the range of 1-20 hours, the most preferred range is 1-15 hours.
  • the depth of the ion exchange layer should be less than 15, 20, 30, 50 microns, and the fracture strength should be at least 100% higher than that of the untempered glass.
  • other elements may be added to the composition of the glass to increase the absorption of the laser.
  • the above laser wavelengths may be in the ultraviolet UV, visible VIS and infrared IR bands. Usually, but not necessarily, rare earth elements such as barium are added.
  • the composition of the relevant glass ranges as follows:
  • the sodium aluminosilicate glass comprises the following components, and the percentage of each component is (wt%) based on the total weight of the glass composition:
  • Lithium aluminosilicate glass comprising the following components, based on the total weight of the glass composition, the percentage of each component is (wt%):
  • the following amount of the following refining agent can be added, but there is no limitation.
  • the borosilicate glass comprises the following components, and the percentage of each component is (wt%) based on the total weight of the glass composition:
  • ZnO 0 ⁇ 8%.
  • a general amount of the following refining agent can be added, but there is no limitation.
  • AI2O3 0 ⁇ 5%.
  • a general amount of the following refining agent can be added, but there is no limitation.
  • the above glass components may each include CeO 2 0-l%. In the following examples, all component amounts are calculated by weight percent unless otherwise stated.
  • the FSM6000 cannot measure the surface compressive stress and the depth of the stress layer. It can be measured by the principle of stress birefringence using a polarizing microscope.
  • the main components of the glass are SiO 2 63%, ⁇ 1 2 ⁇ 3 16%, Na 2 O 13%, K 2 O 3.55%, MgO 3.95%, and the balance is SnO 2 .
  • the corresponding raw materials are compounded, and the raw materials are melted through platinum crucible at 1600-1640 ° C for 5 to 15 hours, and then clarified at 1640-1660 ° C, followed by Cool down to around 1600 °C.
  • the platinum crucible was taken out from the high temperature furnace, and the glass melt was poured into a cold stainless steel mold to obtain a bulk glass having a size of approximately 50 x 50 x 40 mm.
  • the glass is then annealed in an annealing furnace at about 600 ° C for 2 to 8 hours.
  • the annealed glass is polished, then cut, edging, and finely diced to the desired sample size, i.e., 40 x 40 x 0.7 mm.
  • the surface roughness after polishing is below 1 nm.
  • the coefficient of thermal expansion and the conversion point were determined by the following methods. That is, the measurement is performed by a dilatometer. The sample was processed into a cylinder having a diameter of 5 mm. The amount of change in length from 20 to 300 ° C was recorded to calculate the coefficient of linear expansion.
  • the density of the glass was determined by the Archimedes principle.
  • the volume of the sample is obtained by placing the glass sample in a container filled with water and accurately measuring the volume change of the water in the container. Density data is obtained by dividing the weight of the sample that can be accurately measured by the volume.
  • the polished sample was chemically tempered. The tempering is carried out in a laboratory-scale small salt bath furnace (diameter 250x250mm, depth 400mm). The sample is placed on a special corrosion-resistant stainless steel sample holder. Pass 390 in a KNO 3 salt bath.
  • a glass sample was prepared in the same manner as in Example 1.
  • the glass sample has a thickness of 0.7 mm.
  • the chemical tempering was carried out in a pure KNO 3 salt bath at 440 ° C for 6 hours.
  • the surface stress is 700 MPa
  • the center stress is 45 MPa
  • the stress layer depth is 40 ⁇ m.
  • Cutting with a C0 2 laser, the laser beam power and moving speed are adjusted, and the glass cannot be cut smoothly. The reason is that the stress layer depth and the central tensile stress are too large.
  • a glass sample was prepared in the same manner as in Example 1.
  • the glass sample has a thickness of 1.0 mm.
  • Chemical tempering was carried out in a pure KNO 3 salt bath at 390 ° C for 8 hours.
  • the surface stress is 1000 Mpa
  • the center stress is 10 Mpa
  • the stress layer depth is 10 ⁇ m.
  • Cutting with a CO 2 laser with a laser power of 100 W and a laser beam moving speed of 180 mm/sec the glass can be cut smoothly.
  • the edge quality is good.
  • the quality of the glass edge can be seen in Figure 2.
  • the glass can be cut by a conventional glass cutting table with a cutter wheel, as shown in Figure 3.
  • a large number of small gaps are generated at the edge, and large-scale production cannot be performed.
  • a glass sample was prepared in the same manner as in Example 1.
  • the glass sample has a thickness of 0.5 mm.
  • the chemical tempering was carried out in a pure NaNO 3 salt bath at 380 ° C for 10 minutes.
  • the surface stress is 650 Mpa
  • the center stress is 10 Mpa
  • the stress layer depth is 14 ⁇ m.
  • the laser beam moving speed is 200mm/sec, and the glass can be cut smoothly.
  • the edge quality is good.
  • a glass sample was prepared in the same manner as in Example 1.
  • the sample thickness is 0.3 mm.
  • the chemical tempering was carried out in a pure KNO 3 salt bath at 420 ° C for 3 hours.
  • the surface stress is 500 Mpa
  • the center stress is 14 Mpa
  • the stress layer depth is 8 ⁇ .
  • a glass sample was prepared in the same manner as in Example 1.
  • the sample thickness was 1.0 mm.
  • Chemical tempering was carried out in a pure KNO 3 salt bath at 460 ° C for 8 hours.
  • the surface stress is 300 Mpa
  • the center stress is 5 Mpa
  • the stress layer depth is 16 ⁇ m.
  • Cutting with a CO 2 laser with a laser power of 120 W and a laser beam moving speed of 150 mm/sec the glass can be cut smoothly.
  • the edge quality is good.
  • Applications include display glass for consumer electronics and optics.
  • the cutting method may be any cutting method, but it is preferably laser cutting such as CO 2 , Nd-YAG laser or femtosecond laser. It can also be cut with a water knife and a mechanical cutter wheel.

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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)
  • Ceramic Engineering (AREA)
  • Glass Compositions (AREA)

Abstract

L'invention concerne un verre chimiquement renforcé susceptible d'être postérieurement découpé caractérisé en ce que le module d'élasticité de Young dudit verre est compris entre 70 et 100 GPa, la microdureté Knoop (0,1/20, 100 gramme-force, 20 secondes) est comprise entre 500 et 800 kg/mm2 et le CTE est compris entre 5,0 et 11,0x1O-6/°C.
PCT/CN2011/071155 2010-02-26 2011-02-22 Verre chimiquement renforcé susceptible d'être postérieurement découpé WO2011103798A1 (fr)

Applications Claiming Priority (2)

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CN201010126367.X 2010-02-26
CN201010126367XA CN102167509A (zh) 2010-02-26 2010-02-26 能进行后续切割的化学钢化玻璃

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WO2011103798A1 true WO2011103798A1 (fr) 2011-09-01

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