CN114436537A - Oled glass plate for display and preparation method thereof - Google Patents

Oled glass plate for display and preparation method thereof Download PDF

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CN114436537A
CN114436537A CN202210355551.4A CN202210355551A CN114436537A CN 114436537 A CN114436537 A CN 114436537A CN 202210355551 A CN202210355551 A CN 202210355551A CN 114436537 A CN114436537 A CN 114436537A
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oxide
percent
glass plate
whiskers
dioxide
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CN114436537B (en
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杨振邦
张云晓
王光祥
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Wuhan Rongjiada Photoelectric Technology Co ltd
Qingdao Fusion Photoelectric Technology Co Ltd
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Wuhan Rongjiada Photoelectric Technology Co ltd
Qingdao Fusion Photoelectric Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C14/00Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B17/00Forming molten glass by flowing-out, pushing-out, extruding or drawing downwardly or laterally from forming slits or by overflowing over lips
    • C03B17/06Forming glass sheets
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B25/00Annealing glass products
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C1/00Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C1/00Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • C03C1/004Refining agents
    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10KORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00Organic light-emitting devices
    • H10K50/80Constructional details
    • H10K50/84Passivation; Containers; Encapsulations
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C2214/00Nature of the non-vitreous component
    • C03C2214/06Whiskers ss
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C2214/00Nature of the non-vitreous component
    • C03C2214/30Methods of making the composites

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

Abstract

The invention discloses an oled glass plate for display and a preparation method thereof. The preparation of the oled glass plate comprises the following raw materials in percentage by weight: 55% -75% of silicon dioxide; 5% -15% of aluminum oxide; 2% -8% of diboron trioxide; 5% -12% of calcium oxide; 5% -15% of zinc oxide; 0.2 to 0.8 percent of magnesium oxide; 0.1 to 0.8 percent of zirconium dioxide; 0.1% -0.8% of tantalum oxide; 0.1 to 0.8 percent of niobium oxide; 0.05 to 0.5 percent of strontium oxide; 2% -5% of chromium oxide; 2% -5% of vanadium trioxide; 0.8 to 1.5 percent of calcium sulfate and 0.5 to 1.5 percent of cerium dioxide; 2% -3% of AlN whiskers; 1% -3% of TiN whiskers; the sum of the weight percentages of the raw materials is 100 percent. The oled glass plate prepared by the invention can meet the quality requirement of large-size glass plates for display.

Description

Oled glass plate for display and preparation method thereof
Technical Field
The invention relates to the field of glass manufacturing, in particular to an oled glass plate for display and a preparation method thereof.
Background
In recent years, the information industry has been rapidly developed, electronic display products are more and more commonly used, and electronic display products such as mobile phones, tablet computers and liquid crystal displays have become indispensable necessities in work or life of people. Ultra-thin glass is a basic material required for producing the flat panel display, and has excellent performance, so that the ultra-thin glass occupies a very important position in the information industry, particularly the electronic display industry, and no other material can be completely substituted at present. With the development of light weight and thinning of electronic display products, the market puts forward higher requirements on the process and products of ultrathin electronic glass.
Generally, glass is classified into ultra-thin glass, general glass, ultra-thick glass, and the like according to its thickness. Ultra-thin glass refers to glass having a thickness of 0.1-1.1 mm. The thickness of the ultrathin glass substrate for electronic information ranges from 0.1 mm to 1.1mm, and is a core component of a display panel. With the development of display technology, the OLED display technology is developed vigorously, and higher requirements are put on glass. The performance of the OLED carrier plate glass has a remarkable influence on the performance of the OLED display product, key technical indexes such as resolution, light transmittance, thickness, weight and visual angle of the display are closely related to the performance of the OLED carrier plate, and the performance and quality of the OLED display panel depend on the carrier plate glass to a great extent, so that the OLED display panel also becomes a main restriction factor for the development of the OLED. Therefore, from the performance perspective, the OLED carrier plate glass needs to satisfy higher thermal stability, good chemical corrosion resistance, few surface and internal defects, proper thermal expansion coefficient, light weight, high strength, and the like.
With the development of the information industry, display panel production will gradually expand in size from Gen 1 to Gen 10.5. Under the condition that the area of the carrier plate glass is enlarged, the quality requirement on the carrier plate glass is improved year by year, and the manufacturing of the carrier plate glass is difficult to reach the required quality level.
The applicant has found that the prior art has at least the following technical problems:
in the prior art, the manufacturing of the carrier plate glass is difficult to reach the required quality level under the condition of enlarging the glass area.
Disclosure of Invention
The invention aims to provide an oled glass plate for display and a preparation method thereof, which have the characteristics of low density and high modulus and solve the technical problem that the manufacturing of carrier plate glass is difficult to achieve the required quality level under the condition of enlarging the area of the carrier plate glass in the prior art.
In order to realize the purpose, the invention provides the following technical scheme:
the invention provides an oled glass plate for display and a preparation method thereof, wherein the preparation comprises the following raw materials in percentage by weight: 55% -75% of silicon dioxide; 5% -15% of aluminum oxide; 2% -8% of boron trioxide; 5% -12% of calcium oxide; 5% -15% of zinc oxide; 0.2 to 0.8 percent of magnesium oxide; 0.1 to 0.8 percent of zirconium dioxide; 0.1% -0.8% of tantalum oxide; 0.1 to 0.8 percent of niobium oxide; 0.05 to 0.5 percent of strontium oxide; 2% -5% of chromium oxide; 2% -5% of vanadium trioxide; 0.8 to 1.5 percent of calcium sulfate and 0.5 to 1.5 percent of cerium dioxide; 2% -3% of AlN whiskers; 1% -3% of TiN whiskers; the sum of the weight percentages of the raw materials is 100 percent.
Further, the weight percentages of the raw materials are respectively as follows: 55% -65% of silicon dioxide; 7% -12% of aluminum oxide; 5% -7% of boron trioxide; 5% -7% of calcium oxide; 7% -12% of zinc oxide; 0.4 to 0.6 percent of magnesium oxide; 0.3 to 0.5 percent of zirconium dioxide; 0.3% -0.5% of tantalum oxide; 0.3 to 0.5 percent of niobium oxide; 0.2 to 0.4 percent of strontium oxide; 3% -4% of chromium oxide; 3% -4% of vanadium trioxide; 1 to 1.2 percent of calcium sulfate and 0.8 to 1.2 percent of cerium dioxide; 2.2% -2.8% of AlN whiskers; 1.2 to 2 percent of TiN crystal whisker; the sum of the weight percentages of the raw materials is 100 percent.
Further, the weight percentages of the raw materials are respectively as follows: 58% of silicon dioxide; 8% of aluminum oxide; 6% of boron trioxide; 6% of calcium oxide; 8% of zinc oxide; 0.5 percent of magnesium oxide; zirconium dioxide 0.4%; 0.4% of tantalum oxide; 0.4 percent of niobium oxide; 0.3 percent of strontium oxide; 3% of chromium oxide; 3% of vanadium trioxide; 1% of calcium sulfate and 1% of cerium dioxide; 2.5 percent of AlN whisker; 1.5 percent of TiN crystal whisker.
The invention provides a preparation method of an oled glass plate for display, which comprises the following steps:
s1, blending according to the proportion;
s2, adding silicon dioxide, aluminum oxide, boron trioxide, calcium oxide, zinc oxide, magnesium oxide, zirconium dioxide, tantalum oxide, niobium oxide, strontium oxide, chromium oxide, vanadium trioxide, calcium sulfate, cerium dioxide, AlN whiskers and TiN whiskers into a ball mill, and then carrying out ball milling for 10-15 h; after the ball milling is finished, obtaining a mixture;
s3, adding the mixture obtained in the step S2 into a crucible, then placing the crucible into a high-temperature furnace for melting, wherein the melting temperature is 1700-1900 ℃, and when the melting temperature is reached, preserving the heat for 3-6 h; obtaining molten glass;
s4, clarifying and homogenizing the molten glass obtained in the step S3 through a platinum channel, and cooling to 1200-1300 ℃;
s5, performing overflow forming on the molten glass processed in the step S4 through an overflow brick in a muffle furnace, controlling the thickness of the glass plate to be 0.3-1.1mm, and cooling to normal temperature to obtain a semi-finished glass plate;
and S6, annealing the semi-finished glass plate obtained in the step S5, and cooling to normal temperature to obtain a finished glass plate.
Further, in step S2, the AlN whiskers and the TiN whiskers are activated before ball milling.
Further, the activation treatment is as follows: respectively soaking the AlN whiskers and the TiN whiskers in 1-3mol/L sulfuric acid solution for 2-3h, and then cleaning and drying.
Further, in the step S6, the annealing treatment is performed by heat preservation at 400 ℃ for 1-2h and then heating to 600 ℃ for 1-2 h.
Based on the technical scheme, the embodiment of the invention can at least produce the following technical effects:
(1) according to the oled glass plate for display and the preparation method thereof, the manufactured oled glass plate has high thermal stability, good chemical corrosion resistance, few surface and internal defects, proper thermal expansion coefficient, light weight and high strength under the condition that the area of a glass substrate is enlarged, and can meet the quality requirement of the glass plate for display.
(2) According to the oled glass plate for display and the preparation method thereof, the added tantalum oxide and niobium oxide, and the rare metal elements of tantalum and niobium are added, so that the overall thermal stability, chemical corrosion resistance and strength of the glass plate can be improved.
(3) According to the oled glass plate for display and the preparation method thereof, the added chromium oxide and vanadium trioxide can play a role of a grain inhibitor during melting, can inhibit the growth of grains, enables the glass liquid to achieve an initial homogenization effect before entering a platinum channel, and can achieve a best homogenization effect during platinum channel homogenization treatment, so that the strength of the glass plate is improved.
(4) According to the oled glass plate for display and the preparation method thereof, calcium sulfate and cerium dioxide are added to play a role of a clarifying agent, and the best clarifying effect can be achieved through the synergistic effect of the calcium sulfate and the cerium dioxide, so that the defects on the surface and the inside of the glass plate are reduced; therefore, the resolution, the light transmittance, the visual angle and the like of the display are improved, and the display can achieve a higher display effect.
(5) The added AlN whiskers and TiN whiskers are ground into dispersion strengthening particles during ball milling to inhibit the growth of grains, so that the uniformity and crack expansion resistance of the material can be enhanced, the strength and transverse fracture toughness of the material are further improved, and the material has synergistic action with chromium oxide and vanadium trioxide, so that the obtained oled glass plate is strengthened and toughened; and activation treatment is carried out before ball milling, so that the reactivity of AlN whiskers and TiN whiskers is increased, better reactivity can be exerted during melting,
(6) according to the oled glass plate for display and the preparation method thereof, the annealing treatment method adopts gradual temperature rise, and two temperature sections are subjected to heat preservation and annealing treatment, so that the strength of the glass plate can be further improved, and the requirements of light weight and high strength are met.
Detailed Description
First, preparation example:
an oled glass plate having a length and width dimension of 3370mm × 2940mm was prepared.
And raw materials:
the raw material formulations in examples 1-6 are shown in table 1 below:
table 1 examples raw material table
Raw materials Example 1 Example 2 Example 3 Example 4 Example 5 Example 6
Silicon dioxide 58.00% 55.00% 63.00% 74.00% 65.00% 55.00%
Aluminum oxide 8.00% 15.00% 5.00% 5.00% 6.00% 10.00%
Boron trioxide 6.00% 8.00% 2.00% 2.00% 5.00% 6.00%
Calcium oxide 6.00% 5.00% 5.00% 5.00% 5.00% 7.00%
Zinc oxide 8.00% 5.00% 5.00% 5.00% 6.00% 5.00%
Magnesium oxide 0.50% 0.20% 0.80% 0.20% 0.40% 0.60%
Zirconium dioxide 0.40% 0.10% 0.80% 0.10% 0.30% 0.50%
Tantalum oxide 0.40% 0.10% 0.80% 0.10% 0.30% 0.50%
Niobium oxide 0.40% 0.10% 0.80% 0.10% 0.30% 0.50%
Strontium oxide 0.30% 0.05% 0.50% 0.05% 0.20% 0.40%
Chromium oxide 3.00% 2.00% 5.00% 2.00% 3.00% 3.50%
Vanadium trioxide 3.00% 2.00% 5.00% 2.00% 3.00% 3.50%
Calcium sulfate 1.00% 0.80% 1.50% 0.80% 1.00% 1.20%
Cerium oxide 1.00% 0.50% 1.50% 0.50% 0.80% 1.20%
AlN whisker 2.50% 3.00% 2.00% 2.00% 2.20% 2.80%
TiN whisker 1.50% 3.00% 1.00% 1.00% 1.20% 2.00%
2. The preparation method comprises the following steps:
example 1:
the method comprises the following steps:
s1, blending according to the proportion;
s2, AlN whiskers and TiN whiskers are subjected to activation treatment before ball milling; the activation treatment comprises the following steps: respectively soaking AlN whiskers and TiN whiskers in 2mol/L sulfuric acid solution for 2.5 hours, and then cleaning and drying for later use; adding silicon dioxide, aluminum oxide, boron trioxide, calcium oxide, zinc oxide, magnesium oxide, zirconium dioxide, tantalum oxide, niobium oxide, strontium oxide, chromium oxide, vanadium trioxide, calcium sulfate, cerium dioxide, AlN whiskers and TiN whiskers into a ball mill, and carrying out ball milling for 12 hours; after the ball milling is finished, obtaining a mixture;
s3, adding the mixture obtained in the step S2 into a crucible, then placing the crucible into a high-temperature furnace to be melted, wherein the melting temperature is 1800 ℃, and preserving heat for 5 hours when the melting temperature is reached; obtaining molten glass;
s4, clarifying and homogenizing the molten glass obtained in the step S3 through a platinum channel, and cooling to 1250 ℃;
s5, performing overflow forming on the molten glass processed in the step S4 through an overflow brick in a muffle furnace, controlling the thickness of the glass plate to be 0.3mm, and cooling to normal temperature to obtain a semi-finished glass plate;
s6, annealing the semi-finished glass plate obtained in the step S5, wherein the annealing is performed by keeping the temperature at 360 ℃ for 1.5h, and then heating to 550 ℃ and keeping the temperature for 1.5 h; and cooling to normal temperature to obtain a finished glass plate.
Example 2:
the method comprises the following steps:
s1, blending according to the proportion;
s2, AlN whiskers and TiN whiskers are subjected to activation treatment before ball milling; the activation treatment comprises the following steps: respectively soaking AlN whiskers and TiN whiskers in a 3mol/L sulfuric acid solution for 2 hours, and then cleaning and drying for later use; adding silicon dioxide, aluminum oxide, boron trioxide, calcium oxide, zinc oxide, magnesium oxide, zirconium dioxide, tantalum oxide, niobium oxide, strontium oxide, chromium oxide, vanadium trioxide, calcium sulfate, cerium dioxide, AlN whiskers and TiN whiskers into a ball mill, and carrying out ball milling for 10 hours; after the ball milling is finished, obtaining a mixture;
s3, adding the mixture obtained in the step S2 into a crucible, then placing the crucible into a high-temperature furnace to be melted, wherein the melting temperature is 1700 ℃, and preserving heat for 6 hours when the melting temperature is reached; obtaining molten glass;
s4, clarifying and homogenizing the molten glass obtained in the step S3 through a platinum channel, and cooling to 1200 ℃;
s5, performing overflow forming on the molten glass processed in the step S4 through an overflow brick in a muffle furnace, controlling the thickness of the glass plate to be 0.5mm, and cooling to normal temperature to obtain a semi-finished glass plate;
s6, annealing the semi-finished glass plate obtained in the step S5, wherein the annealing is carried out by keeping the temperature at 320 ℃ for 2h, and then heating to 500 ℃ and keeping the temperature for 2 h; and cooling to normal temperature to obtain a finished glass plate.
Example 3:
the method comprises the following steps:
s1, blending according to the proportion;
s2, AlN whiskers and TiN whiskers are subjected to activation treatment before ball milling; the activation treatment comprises the following steps: respectively soaking AlN whiskers and TiN whiskers in 1mol/L sulfuric acid solution for 3 hours, and then cleaning and drying for later use; adding silicon dioxide, aluminum oxide, boron trioxide, calcium oxide, zinc oxide, magnesium oxide, zirconium dioxide, tantalum oxide, niobium oxide, strontium oxide, chromium oxide, vanadium trioxide, calcium sulfate, cerium dioxide, AlN whiskers and TiN whiskers into a ball mill, and carrying out ball milling for 15 hours; after the ball milling is finished, obtaining a mixture;
s3, adding the mixture obtained in the step S2 into a crucible, then placing the crucible into a high-temperature furnace for melting, wherein the melting temperature is 1900 ℃, and when the melting temperature is reached, preserving the heat for 3 hours; obtaining glass liquid;
s4, clarifying and homogenizing the molten glass obtained in the step S3 through a platinum channel, and cooling to 1300 ℃;
s5, performing overflow forming on the molten glass processed in the step S4 through an overflow brick in a muffle furnace, controlling the thickness of the glass plate to be 0.6mm, and cooling to normal temperature to obtain a semi-finished glass plate;
s6, annealing the semi-finished glass plate obtained in the step S5, wherein the annealing is performed by keeping the temperature at 400 ℃ for 1h, and then heating to 600 ℃ and keeping the temperature for 1 h; and cooling to normal temperature to obtain a finished glass plate.
Example 4:
the method comprises the following steps:
s1, blending according to the proportion;
s2, AlN whiskers and TiN whiskers are subjected to activation treatment before ball milling; the activation treatment comprises the following steps: respectively soaking AlN whiskers and TiN whiskers in 1.5mol/L sulfuric acid solution for 2.8 hours, and then cleaning and drying for later use; adding silicon dioxide, aluminum oxide, boron trioxide, calcium oxide, zinc oxide, magnesium oxide, zirconium dioxide, tantalum oxide, niobium oxide, strontium oxide, chromium oxide, vanadium trioxide, calcium sulfate, cerium dioxide, AlN whiskers and TiN whiskers into a ball mill, and carrying out ball milling for 14 hours; after the ball milling is finished, obtaining a mixture;
s3, adding the mixture obtained in the step S2 into a crucible, then placing the crucible into a high-temperature furnace for melting, wherein the melting temperature is 1750 ℃, and preserving heat for 5 hours when the melting temperature is reached; obtaining molten glass;
s4, clarifying and homogenizing the molten glass obtained in the step S3 through a platinum channel, and cooling to 1280 ℃;
s5, performing overflow forming on the molten glass processed in the step S4 through an overflow brick in a muffle furnace, controlling the thickness of the glass plate to be 0.7mm, and cooling to normal temperature to obtain a semi-finished glass plate;
s6, annealing the semi-finished glass plate obtained in the step S5, wherein the annealing is performed by keeping the temperature at 380 ℃ for 1.2h, and then heating to 580 ℃ and keeping the temperature for 1.2 h; and cooling to normal temperature to obtain a finished glass plate.
Example 5:
the method comprises the following steps:
s1, blending according to the proportion;
s2, AlN whiskers and TiN whiskers are subjected to activation treatment before ball milling; the activation treatment comprises the following steps: respectively soaking AlN whiskers and TiN whiskers in 2.5mol/L sulfuric acid solution for 2.2 hours, and then cleaning and drying for later use; adding silicon dioxide, aluminum oxide, boron trioxide, calcium oxide, zinc oxide, magnesium oxide, zirconium dioxide, tantalum oxide, niobium oxide, strontium oxide, chromium oxide, vanadium trioxide, calcium sulfate, cerium dioxide, AlN whiskers and TiN whiskers into a ball mill, and carrying out ball milling for 13 hours; after the ball milling is finished, obtaining a mixture;
s3, adding the mixture obtained in the step S2 into a crucible, then placing the crucible into a high-temperature furnace for melting, wherein the melting temperature is 1850 ℃, and preserving heat for 4 hours when the melting temperature is reached; obtaining molten glass;
s4, clarifying and homogenizing the molten glass obtained in the step S3 through a platinum channel, and cooling to 1280 ℃;
s5, performing overflow forming on the molten glass processed in the step S4 through an overflow brick in a muffle furnace, controlling the thickness of the glass plate to be 0.9mm, and cooling to normal temperature to obtain a semi-finished glass plate;
s6, annealing the semi-finished glass plate obtained in the step S5, wherein the annealing is performed by keeping the temperature at 340 ℃ for 1.8h, and then heating to 520 ℃ and keeping the temperature for 1.2 h; and cooling to normal temperature to obtain a finished glass plate.
Example 6:
the method comprises the following steps:
s1, blending according to the proportion;
s2, AlN whiskers and TiN whiskers are subjected to activation treatment before ball milling; the activation treatment comprises the following steps: respectively soaking AlN whiskers and TiN whiskers in 2mol/L sulfuric acid solution for 3 hours, and then cleaning and drying for later use; adding silicon dioxide, aluminum oxide, boron trioxide, calcium oxide, zinc oxide, magnesium oxide, zirconium dioxide, tantalum oxide, niobium oxide, strontium oxide, chromium oxide, vanadium trioxide, calcium sulfate, cerium dioxide, AlN whiskers and TiN whiskers into a ball mill, and carrying out ball milling for 15 hours; after the ball milling is finished, obtaining a mixture;
s3, adding the mixture obtained in the step S2 into a crucible, then placing the crucible into a high-temperature furnace for melting, wherein the melting temperature is 1900 ℃, and when the melting temperature is reached, preserving the heat for 3 hours; obtaining molten glass;
s4, clarifying and homogenizing the molten glass obtained in the step S3 through a platinum channel, and cooling to 1200 ℃;
s5, performing overflow forming on the molten glass processed in the step S4 through an overflow brick in a muffle furnace, controlling the thickness of the glass plate to be 1.1mm, and cooling to normal temperature to obtain a semi-finished glass plate;
s6, annealing the semi-finished glass plate obtained in the step S5, wherein the annealing is performed by keeping the temperature at 400 ℃ for 2h, and then heating to 600 ℃ and keeping the temperature for 2 h; and cooling to normal temperature to obtain a finished glass plate.
Second, experimental example:
1. the glass sheets prepared in examples 1 to 6 were examined for their properties.
(1) The detection method comprises the following steps:
density: glass Density is determined according to ASTM C-693-93 (2013) in g/cm3
Coefficient of thermal expansion: the coefficient of thermal expansion of the glass at 50-350 ℃ is measured according to ASTM E-228 using a horizontal dilatometer and has the unit 10-7/℃。
Melting temperature: the glass high temperature viscosity temperature curve was determined according to ASTM C-965-96 (2017) using a rotary high temperature viscometer, where the 200P viscosity corresponds to the melting temperature Tm in degrees Celsius.
Transmittance: the transmittance of the glass at a wavelength of 550nm and 308nm was measured by a UV-2600 UV-visible spectrophotometer.
Chemical resistance: the chemical resistance test was carried out according to the test method for chemical durability of glass of a substrate for a flat panel display of GB/T32644-2016.
Young's modulus: the Young's modulus of glass was measured in GPa according to ASTM C-623-92 (2015) using a Material mechanical tester.
Bending strength: the bending strength test method of the GB/T37781-2019 glass material measures the bending strength, and the unit is MPa.
(2) The results are shown in table 2 below:
table 2 results of testing the properties of the glass sheets in the examples
Figure 994274DEST_PATH_IMAGE002
As is clear from Table 2, of the glass sheets prepared in the examples of the present inventionThe density of the glass is less than 2.4 g/cm3(ii) a Young's modulus greater than 75 Gpa; expansion coefficient of less than 38 x 10 in the range of 50-350 deg.C-7/° c; chemical resistance less than 5.0; a melting temperature (200P) of less than 1650 ℃; the strain point is higher than 670 ℃; the transmittance of UV550nm is more than 92 percent, the transmittance of UV308nm is more than 78 percent, and the bending strength is more than 120 MPa. There is a significant advantage in manufacturing a large-sized panel and a high-performance display panel.

Claims (7)

1. An oled glass plate for display, characterized in that it is prepared from the following raw materials in weight percent: 55% -75% of silicon dioxide; 5% -15% of aluminum oxide; 2% -8% of boron trioxide; 5% -12% of calcium oxide; 5% -15% of zinc oxide; 0.2 to 0.8 percent of magnesium oxide; 0.1 to 0.8 percent of zirconium dioxide; 0.1% -0.8% of tantalum oxide; 0.1 to 0.8 percent of niobium oxide; 0.05 to 0.5 percent of strontium oxide; 2% -5% of chromium oxide; 2% -5% of vanadium trioxide; 0.8 to 1.5 percent of calcium sulfate and 0.5 to 1.5 percent of cerium dioxide; 2% -3% of AlN whiskers; 1% -3% of TiN whiskers; the sum of the weight percentages of the raw materials is 100 percent.
2. The oled glass sheet as claimed in claim 1, wherein the raw materials comprise, in weight percent: 55% -65% of silicon dioxide; 7% -12% of aluminum oxide; 5% -7% of boron trioxide; 5% -7% of calcium oxide; 7% -12% of zinc oxide; 0.4 to 0.6 percent of magnesium oxide; 0.3 to 0.5 percent of zirconium dioxide; 0.3% -0.5% of tantalum oxide; 0.3 to 0.5 percent of niobium oxide; 0.2 to 0.4 percent of strontium oxide; 3% -4% of chromium oxide; 3% -4% of vanadium trioxide; 1 to 1.2 percent of calcium sulfate and 0.8 to 1.2 percent of cerium dioxide; 2.2% -2.8% of AlN whiskers; 1.2 to 2 percent of TiN crystal whisker; the sum of the weight percentages of the raw materials is 100 percent.
3. The oled glass sheet as claimed in claim 1, wherein the raw materials comprise, in weight percent: 58% of silicon dioxide; 8% of aluminum oxide; 6% of boron trioxide; 6% of calcium oxide; 8% of zinc oxide; 0.5 percent of magnesium oxide; 0.4 percent of zirconium dioxide; 0.4% of tantalum oxide; 0.4 percent of niobium oxide; 0.3 percent of strontium oxide; 3% of chromium oxide; 3% of vanadium trioxide; 1% of calcium sulfate and 1% of cerium dioxide; 2.5 percent of AlN whisker; 1.5 percent of TiN crystal whisker.
4. The method of manufacturing a low density high modulus oled glass sheet for display as claimed in any one of claims 1 to 3, comprising the steps of:
s1, blending according to the proportion;
s2, adding silicon dioxide, aluminum oxide, boron trioxide, calcium oxide, zinc oxide, magnesium oxide, zirconium dioxide, tantalum oxide, niobium oxide, strontium oxide, chromium oxide, vanadium trioxide, calcium sulfate, cerium dioxide, AlN whiskers and TiN whiskers into a ball mill, and then carrying out ball milling for 10-15 h; after the ball milling is finished, obtaining a mixture;
s3, adding the mixture obtained in the step S2 into a crucible, then placing the crucible into a high-temperature furnace for melting, wherein the melting temperature is 1700-1900 ℃, and when the melting temperature is reached, preserving the heat for 3-6 h; obtaining molten glass;
s4, clarifying and homogenizing the molten glass obtained in the step S3 through a platinum channel, and cooling to 1200-1300 ℃;
s5, performing overflow forming on the molten glass processed in the step S4 through an overflow brick in a muffle furnace, controlling the thickness of the glass plate to be 0.3-1.1mm, and cooling to normal temperature to obtain a semi-finished glass plate;
and S6, annealing the semi-finished glass plate obtained in the step S5, and cooling to normal temperature to obtain a finished glass plate.
5. The method of claim 4, wherein the AlN whiskers and the TiN whiskers are activated before the ball milling in step S2.
6. The method of manufacturing a low density high modulus oled glass sheet as claimed in claim 5, wherein the activation treatment is: respectively soaking the AlN whiskers and the TiN whiskers in 1-3mol/L sulfuric acid solution for 2-3h, and then cleaning and drying.
7. The method as claimed in claim 4, wherein the annealing treatment in step S6 is performed by heat preservation at 400 ℃ for 1-2h, and then heating to 600 ℃ for 1-2 h.
CN202210355551.4A 2022-04-06 2022-04-06 Oled glass plate for display and preparation method thereof Active CN114436537B (en)

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CN109678341A (en) * 2018-12-11 2019-04-26 东旭科技集团有限公司 Alkali-free glass compositions and alkali-free glass and application
CN111087175A (en) * 2019-12-17 2020-05-01 深圳市东丽华科技有限公司 Rare earth doped reinforced glass ceramic and preparation method and application thereof
CN113165946A (en) * 2018-11-29 2021-07-23 康宁股份有限公司 High refractive index silicate glass compositions with reduced devitrification kinetics

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04104921A (en) * 1990-08-18 1992-04-07 Mitsubishi Electric Corp Case unit material for display element, its production and display element
US5374595A (en) * 1993-01-22 1994-12-20 Corning Incorporated High liquidus viscosity glasses for flat panel displays
US20020123420A1 (en) * 2000-12-25 2002-09-05 Nippon Sheet Glass Co., Ltd. Alkali free glass, production method therefor, and flat display panel using the same
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CN113165946A (en) * 2018-11-29 2021-07-23 康宁股份有限公司 High refractive index silicate glass compositions with reduced devitrification kinetics
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