CN110818251A - Glass composition and preparation method of glass - Google Patents
Glass composition and preparation method of glass Download PDFInfo
- Publication number
- CN110818251A CN110818251A CN201911134491.8A CN201911134491A CN110818251A CN 110818251 A CN110818251 A CN 110818251A CN 201911134491 A CN201911134491 A CN 201911134491A CN 110818251 A CN110818251 A CN 110818251A
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- glass
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Classifications
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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
- 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
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
Abstract
The invention relates to a glass composition and a preparation method of glass, which are characterized by comprising the following raw materials in percentage by weight: 55-74% SiO212-18% of Al2O30.5-4.5% of B2O32.5-5% of MgO, 6.5-12% of CaO, 1-3% of SrO, 0.1-1.5% of ZnO and 0.01-1.5% of ZrO2. The invention has the advantages that: the glass composition is substantially free of alkali metal oxides, free of BaO, and free of As2O3、Sb2O3And the like, belonging to an environment-friendly formula; has the characteristics of higher chemical stability, low thermal shrinkage, high strain point, high Young's modulus, low density and the like, is suitable for a float forming manufacturing process, accords with the development trend of the flat panel display industry, is suitable for large-scale industrial production, and can be applied to the production of the flat panel displayThe glass substrate is particularly suitable for preparing glass substrates for LCD/OLED displays.
Description
Technical Field
The invention belongs to the field of glass, relates to the field of glass substrates for displays, and particularly relates to a glass composition and a preparation method of glass.
Background
With the development of the electro-optical display technology and the popularization of electronic products, the liquid crystal display is continuously updated, the performance requirements of people on the display are continuously improved, and the display market is gradually occupied by the lightness, thinness, high resolution and ultra high definition, so that the liquid crystal display becomes a mainstream characteristic. Therefore, the technology of the glass substrate for the display is also continuously updated, so that the characteristic requirements of the glass substrate are more and more strict.
In the process of manufacturing a flat panel display panel, a metal or oxide film needs to be plated on the surface of a glass substrate, alkali metal ions in the substrate glass diffuse into the film to damage the film characteristics, and the glass does not contain alkali metal oxide. With the increasing resolution of display images, the deformation of the glass substrate is required to be lower and lower during the thermal treatment process of panel printing and coating, and the thermal shrinkage rate of the glass substrate needs to be strictly controlled.
The amorphous silicon (a-Si) TFT technology has the treatment temperature of 300-450 ℃ in the production process, the low-temperature polysilicon TFT technology needs higher heat treatment temperature in the panel manufacturing process, and the glass substrate cannot deform in multiple high-temperature treatment processes, so that the glass substrate needs high strain point and has the heat shrinkage rate as small as possible. Meanwhile, the expansion coefficient of the glass substrate needs to be close to that of silicon, so the linear thermal expansion coefficient of the glass substrate should be lower than 38 x 10-7/℃。
With the large size of the glass substrate, the sag and warpage of the glass become important research points, the carrying capacity of the glass substrate is affected in each process after the glass substrate is formed, and in the panel process, the greater sag or warpage can cause the increase of the fragment rate and the alarm of the CF process technology, which seriously affects the product yield. Therefore, the substrate glass should have a low density and a high elastic modulus.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, provides a glass composition and a preparation method of glass, and provides a glass product with lower density, higher strain point, higher Young modulus, lower heat shrinkage rate and good surface flatness, which is suitable for large-scale industrial production.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the glass composition is characterized by comprising the following raw materials in percentage by weight:
55-74% SiO212-18% of Al2O30.5-4.5% of B2O32.5-5% of MgO, 6.5-12% of CaO, 1-3% of SrO, 0.1-1.5% of ZnO and 0.01-1.5% of ZrO2。
Further, the glass composition can also comprise the following raw materials in percentage by weight:
62.5-72.6% SiO212-16.55% of Al2O31.55-3.75% of B2O32.65-4.65% of MgO, 8-10% of CaO, 1.5-2.5% of SrO, 0.45-1.35% of ZnO and 0.1-1.3% of ZrO2。
Further, the glass composition also contains SnO with the weight of 0.1-0.5 percent of the composition2As a clarifying agent.
Further, it is preferable that MgO + CaO + SrO + ZnO is 11.2 to 21%.
Further, it is preferable that (MgO + CaO + SrO + ZnO)/Al2O30.8-1.2%.
Further, it is preferable that the MgO/CaO is 0.2 to 0.75%.
Further, it is preferable that the MgO/SrO is 0.9 to 4.6%.
Further, it is preferable that the MgO/ZnO ratio is 1.5 to 14.2%.
Further, ZrO is preferable2/ B2O30.01-1.95%.
A preparation method of glass is characterized by comprising the following steps:
(1) uniformly mixing the raw materials of the components according to the weight percentage;
(2) melting at high temperature (1560-;
(3) and (5) processing and performance testing.
The glass composition produced by the above method has a density of less than 2.6g/cm3Young's modulus higher than 75GPa, and thermal expansion coefficient lower than 37.5X 10 in 50-350 deg.C range-7The strain point is higher than 700 ℃, the melting temperature is lower than 1630 ℃, the working temperature is lower than 1340 ℃, the liquidus temperature is lower than 1150 ℃, the heat shrinkage rate is lower than 13ppm, the transmittance at 308nm is higher than 70%, and the 5wt% HCl erosion amount at 95 ℃ for 24 hours is lower than 0.58mg/cm2And the erosion amount of 10wt% HF acid buffer solution at 20 ℃ for 20min is lower than 1.85 mg/cm210wt% HF acid at 20 deg.c for 20min to reach etching amount lower than 8.89mg/cm2。
SiO in the glass composition2Is a glass former, the components constituting the glass skeleton are increased by SiO2And (3) the chemical resistance, mechanical strength and strain point are improved. If SiO2Too much, the high temperature viscosity of the glass increases, causing refractory behavior and aggravating the erosion of the refractory material. SiO 22When the content is low, glass is not easily formed, the strain point is reduced, the expansion coefficient is increased, and the acid resistance and the alkali resistance are reduced. Taking into account the properties of melting temperature, glass expansion coefficient, mechanical strength, glass frit properties, etc.
Al in the glass composition2O3Is intermediate oxide for improving the strength and strain point of glass structure, improving the chemical stability of glass, reducing the devitrification tendency of glass, and Al2O3Excessive content, difficult melting of glass, short material property, easy crystallization and Al2O3The content is low, the glass is easy to devitrify, the mechanical strength is low, and the molding is not facilitated.
In the glass composition B2O3Can produce glass independently, is a good fluxing agent, can reduce the viscosity, dielectric loss and vibration loss of glass, and improveGlass brittleness, toughness and light transmission. Having [ BO ] in glass4]Tetrahedron and [ BO3]Two structures of triangle, B under high temperature melting condition2O3Difficult to form [ BO4]Can reduce high temperature viscosity, and B can deprive free oxygen to form [ BO ] at low temperature4]The trend of the glass makes the structure tend to be compact, improves the low-temperature viscosity of the glass and prevents the occurrence of crystallization.
MgO in the glass composition has the effects of reducing high-temperature viscosity and increasing low-temperature viscosity, and can increase Young modulus and specific modulus of glass and inhibit the increase of brittleness of the glass.
The alkaline earth metal oxide RO (CaO, SrO, BaO) in the glass composition can improve the strain point and Young's modulus of the glass and reduce the thermal expansion coefficient. The high-temperature viscosity of the glass can be effectively reduced, so that the meltability and the formability of the glass are improved, the occurrence probability of devitrification and phase separation can be increased due to excessive content, and 7.55-15 wt% of RO is introduced into the glass.
ZnO is introduced into the glass composition, so that the high-temperature viscosity of the glass can be reduced, and bubbles can be eliminated; meanwhile, the glass has the effects of improving the strength and the hardness, increasing the chemical resistance of the glass and reducing the thermal expansion coefficient of the glass below the softening point. Too much ZnO content greatly lowers the strain point of the glass.
The glass composition is introduced with ZrO2The glass melting is promoted, the Young modulus and the breaking strength of the glass are improved, the high-temperature resistivity of the glass is reduced, the stability of the glass is promoted, and the density and the thermal expansion coefficient of the glass are increased too much.
The glass composition of the present invention, when used for preparing aluminosilicate glass, is characterized by the mutual coordination of the components of the composition, especially SiO2、Al2O3、B2O3、MgO、CaO、SrO、BaO、ZnO、ZrO2The combination of the components, more particularly the combination of the components in the specific content can ensure that the glass has excellent comprehensive properties.
The invention has the advantages that: the glass composition is substantially free of alkali metal oxides, free of BaO, and free of As2O3、Sb2O3And the like, belonging to an environment-friendly formula; the glass substrate has the characteristics of higher chemical stability, low thermal shrinkage rate, high strain point, high Young modulus, low density and the like, is suitable for a float forming manufacturing process, accords with the development trend of the flat panel display industry, is suitable for large-scale industrial production, can be applied to the preparation of display devices and/or photoelectric devices, and is particularly suitable for glass substrates for LCD/OLED displays.
The specific implementation mode is as follows:
the present invention will be further described with reference to examples, and each of the materials used in the present invention is commercially available, and the methods used are conventional in the art unless otherwise specified. The specific embodiments described herein are merely illustrative and explanatory of the invention and are not restrictive thereof.
The specific components of the glass composition are shown in the following tables 1, 2, 3 and 4:
the preparation method of the glass comprises the following specific implementation steps:
(1) fully mixing the raw materials of the components for 5-7 min according to the mixture ratio in each embodiment in the table;
(2) melting at the temperature of 1560-;
(3) and cooling the annealed glass to room temperature, and then carrying out various machining processing (cutting, grinding, polishing and the like).
The specific melting temperature and melting time can be determined by those skilled in the art according to actual conditions, and the temperature and time for clarifying homogenization, molding and annealing are also well known to those skilled in the art and are not described in detail herein.
Preferably, the glass composition of the present invention has a density of less than 2.6g/cm3The Young's modulus is higher than 75GPa,
the thermal expansion coefficient of the material is 34.5 x 10 in the range of 50-350 DEG C-7/℃-37.5×10-7between/deg.C, strain point is higher than 700 deg.C, melting temperature is lower than 1630 deg.C, working temperature is lower than 1340 deg.C, and liquid phaseThe line temperature is lower than 1150 c,
the transmittance at 308nm is higher than 70%, and the erosion amount of 5wt% HCl at 95 ℃ for 24h is lower than 0.58mg/cm2And the erosion amount of 10wt% HF acid buffer solution at 20 ℃ for 20min is lower than 1.85 mg/cm210wt% HF acid at 20 deg.c for 20min to reach etching amount lower than 8.89mg/cm2. A heat treatment having a heat shrinkage of less than 13ppm, the heat treatment comprising: the glass is heated to 600 ℃ from the room temperature at the heating rate of 10 ℃/min and is kept warm for 10min, and then the room temperature is cooled at the cooling rate of 10 ℃/min.
In the composition for glass, according to different glass preparation processes, the composition contains a clarifying agent, and a composite clarifying agent is adopted, wherein the clarifying agent comprises at least one of sulfate, nitrate and chloride; the specific selection of the clarifying agent is not particularly limited, and may be various ones commonly used in the art, such as calcium sulfate, strontium nitrate, calcium chloride.
It will be understood by those skilled in the art that in the composition for glass of the present invention, the composition contains SiO2、Al2O3、B2O3、MgO、CaO、SrO、BaO、ZnO、ZrO2The composition contains Si-containing compounds, Al-containing compounds, B-containing compounds, Mg-containing compounds, Ca-containing compounds, Sr-containing compounds, Ba-containing compounds, Zn-containing compounds and Zr-containing compounds, such as carbonates, nitrates, sulfates, oxides and the like containing the elements, and the contents of the components are calculated by the oxides of the elements, and the specific selection of the carbonates, nitrates, sulfates and oxides of the elements is well known to those skilled in the art and is not described herein again.
In the following examples and comparative examples:
the glass density was determined in g/cm with reference to ASTMC-6933。
The Young's modulus of the glass was measured in GPa using a mechanical testing machine with reference to ASTMC-623.
The coefficient of thermal expansion of the glass at 50-350 ℃ was measured in 10 units using a horizontal dilatometer with reference to ASTME-228-7/℃。
The annealing and strain points of the glasses were measured in degrees centigrade using a three-point tester with reference to astm c-336 and astm c-338.
Glass high temperature visco-temperature curves were determined using a rotary high temperature viscometer with reference to ASTMC-965, where the temperature T corresponds to a viscosity of 200P2.3In units of; molding temperature T corresponding to 40000P viscositywIn units of ℃.
The upper limit temperature of glass devitrification (liquidus temperature) was measured by the gradient temperature furnace method with reference to astm c-829, and the corresponding liquidus viscosity was obtained by calculation.
The heat shrinkage was calculated using the difference. A glass substrate without any defects, the initial length of which is marked as L0, after being subjected to heat treatment under certain conditions (for example, the heat treatment process conditions of the invention are that the glass is heated to 600 ℃ from room temperature at a heating rate of 10 ℃/min and is kept for 10min, and then the glass is cooled to room temperature at a cooling rate of 10 ℃/min), the length of the substrate is shrunk by a certain amount, the length of the substrate is measured again, the length is marked as Lt, and the heat shrinkage Yt is expressed as:
the glass transmittance was measured using an ultraviolet-visible spectrophotometer with a glass sample thickness of 0.5mm, and the transmittance was taken in units of% at 308 nm.
The corrosion amount of the glass in a 5% hydrochloric acid solution is detected by using a weight loss method, and the detection conditions comprise: putting the defect-free glass into a hydrochloric acid solution with the concentration of 5wt% at 95 ℃, eroding for 24 hours under a shaking state, and calculating the erosion amount, wherein the calculation formula is (before the M sample is eroded-after the M sample is eroded)/the S sample surface area, and the unit is mg/cm2The smaller the value, the stronger the acid resistance.
Detecting the erosion amount of the glass in a 10% hydrofluoric acid buffer solution by using a weight loss method, wherein the detection conditions comprise: the defect-free glass was placed in a 10wt% hydrofluoric acid buffer solution (NH) at 20 deg.C4In the volume ratio of HF to HF of 6: 1), eroding for 20min under the oscillation state, and calculating the erosion amount, wherein the calculation formula is (before M sample erosion-after M sample erosion)/S sample surface area, and the unit is mg/cm2The smaller the value, the stronger the acid resistance.
The corrosion amount of the glass in a 10% hydrofluoric acid solution is detected by using a weight loss method, and the detection conditions comprise:placing defect-free glass into 10wt% hydrofluoric acid solution at 20 deg.C, eroding for 20min under oscillation state, and calculating erosion amount by using (before erosion of M sample-after erosion of M sample)/S sample surface area with unit of mg/cm2The smaller the value, the stronger the acid resistance.
Claims (10)
1. The glass composition is characterized by comprising the following raw materials in percentage by weight:
55-74% SiO212-18% of Al2O30.5-4.5% of B2O32.5-5% of MgO, 6.5-12% of CaO, 1-3% of SrO, 0.1-1.5% of ZnO and 0.01-1.5% of ZrO2。
2. The glass composition of claim 1, wherein: the glass composition comprises the following raw materials in percentage by weight:
62.5-72.6% SiO212-16.55% of Al2O31.55-3.75% of B2O32.65-4.65% of MgO, 8-10% of CaO, 1.5-2.5% of SrO, 0.45-1.35% of ZnO and 0.1-1.3% of ZrO2。
3. The glass composition of claim 1, wherein: the glass composition also contains SnO in an amount of 0.1-0.5% by weight of the composition2As a clarifying agent.
4. A glass composition according to claim 1, 2 or 3, wherein: 11.2 to 21 percent of MgO + CaO + SrO + ZnO.
5. A glass composition according to claim 1, 2 or 3, wherein: (MgO + CaO + SrO + ZnO)/Al2O30.8-1.2%.
6. A glass composition according to claim 1, 2 or 3, wherein: MgO/CaO is 0.2-0.75%.
7. A glass composition according to claim 1, 2 or 3, wherein: MgO/SrO is 0.9-4.6%.
8. A glass composition according to claim 1, 2 or 3, wherein: the ratio of MgO/ZnO is 1.5-14.2%.
9. A glass composition according to claim 1, 2 or 3, wherein: ZrO (ZrO)2/ B2O30.01-1.95%.
10. A preparation method of glass is characterized by comprising the following steps:
(1) uniformly mixing the raw materials of the components according to the weight percentage;
(2) melting at the temperature of 1560-;
(3) and (5) processing and performance testing.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109231816A (en) * | 2018-10-09 | 2019-01-18 | 成都中光电科技有限公司 | A kind of glass substrate and preparation method thereof can be used for LTPS |
| CN112225462A (en) * | 2020-08-13 | 2021-01-15 | 航天特种材料及工艺技术研究所 | Low-expansion-coefficient low-dielectric-constant microcrystalline glass powder for electronic paste and preparation method thereof |
| WO2023051190A1 (en) * | 2021-09-29 | 2023-04-06 | 成都光明光电股份有限公司 | Glass composition |
| TWI838857B (en) | 2021-09-29 | 2024-04-11 | 大陸商成都光明光電股份有限公司 | Glass composition |
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| CN112225462A (en) * | 2020-08-13 | 2021-01-15 | 航天特种材料及工艺技术研究所 | Low-expansion-coefficient low-dielectric-constant microcrystalline glass powder for electronic paste and preparation method thereof |
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| TWI838857B (en) | 2021-09-29 | 2024-04-11 | 大陸商成都光明光電股份有限公司 | Glass composition |
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