CN112499963A - Self-cleaning TFT-LCD substrate glass and preparation method thereof - Google Patents
Self-cleaning TFT-LCD substrate glass and preparation method thereof Download PDFInfo
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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
- C03C3/11—Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen
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- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B18/00—Shaping glass in contact with the surface of a liquid
- C03B18/02—Forming sheets
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- 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/001—General methods for coating; Devices therefor
- C03C17/002—General methods for coating; Devices therefor for flat glass, e.g. float glass
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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
- 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
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- 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
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/29—Mixtures
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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
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
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Abstract
The invention relates to self-cleaning TFT-LCD substrate glass and a preparation method thereof, which are characterized by being prepared from the following raw materials in percentage by mass: 59 to 63% SiO2、16～18.5%Al2O3、0.5～1.5%P2O5、3.5～5.5CaO、6～7.5%B2O3、1.5～4MgO、6～7%SrO、0～0.2%ZrO2、0.01～0.08％CaX2，SiO2+P2O5The value is 60 to 63 percent, and SiO is2+Al2O3+ZrO2The value is 75.5-77%; (1) mixing the raw materials according to the proportion, melting at 1580-1630 ℃, carrying out float forming at 1380-1180 ℃, and annealing to obtain TFT-LCD substrate glass; (2) TFT-LCDThe substrate glass is immersed in molten silver salt and ion exchange is carried out for 4-20h at the temperature of 350-420 ℃, and an Ag/AgX film is formed on the surface of the glass. The invention has the advantages that: the strain point of the glass is higher than 650 ℃, the melting temperature is lower than 1630 ℃, and the forming temperature interval is higher than 150 ℃; the Ag/AgX film is prepared on the surface of the glass by using an ion exchange method, the process is simple, and the cost is low; strong absorption in the visible light range, high sunlight utilization rate and excellent pollutant decomposing performance.
Description
Technical Field
The invention belongs to the field of special glass production, and particularly relates to self-cleaning TFT-LCD substrate glass and a preparation method thereof.
Background
At present, the substrate glass of the glass for electronic information display is mainly alkali-free aluminosilicate glass, because the glass material does not contain alkali metal oxides and has high alumina content, the glass melting process is more difficult than that of the conventional soda-lime silicate glass, the surface tension of the glass is high under the same temperature condition, the characteristic of high viscosity is embodied, the transverse fluidity of the glass liquid is poor under the influence of the surface tension, the difficulty of horizontal thinning forming of the glass liquid by the vertical gravity is increased, and the uniformity of the product density is poor, which is the disadvantage of float forming.
The self-cleaning glass is prepared by coating a film on the surface of the glass, and degrading most pollutants through photocatalysis, so that the surface of the glass is kept clean. At present, the preparation methods of self-cleaning glass mainly comprise a chemical vapor deposition method, an electrostatic spinning method, a magnetron sputtering method, a sol-gel method and the like, and although the preparation methods are various, most of the preparation methods have the problems of high preparation cost, complex process, unsuitability for large-scale production and the like.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides self-cleaning TFT-LCD substrate glass and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the self-cleaning TFT-LCD substrate glass is characterized by being prepared from the following raw materials in percentage by mass: 59-63% of SiO216 to 18.5% of Al2O30.5 to 1.5% of P2O53.5 to 5.5 percent of CaO, 6 to 7.5 percent of B2O31.5 to 4% of MgO, 6 to 7% of SrO, and 0 to 0.2% of ZrO20.01 to 0.08% of CaX2Wherein X is Cl, Br or I, SiO2+P2O5The value is 60 to 63 percent, and SiO is2+Al2O3+ZrO2The value is 75.5 to 77%.
Further, the self-cleaning TFT-LCD substrate glass is characterized by being prepared from the following raw materials in percentage by massThe composition is as follows: 59-61.5% SiO216-17% of Al2O30.5 to 0.8% of P2O53.5 to 3.8 of CaO, 6 to 6.5 percent of B2O31.5 to 2.3 MgO, 6 to 6.4% SrO, 0.03 to 0.05% ZrO20.01 to 0.03% of CaX2Wherein X is Cl, Br or I, SiO2+P2O5The value is 60 to 61.5 percent, SiO2+Al2O3+ZrO2The value is 75.5 to 75.8%.
Further, the self-cleaning TFT-LCD substrate glass is characterized by being prepared from the following raw materials in percentage by mass: 62-62.8% of SiO217.5 to 18.5% of Al2O31 to 1.5% of P2O54 to 4.5 of CaO, 7.2 to 7.5 percent of B2O33.5 to 4 MgO, 6.5 to 7% SrO, 0.05 to 0.15% ZrO20.03 to 0.05 percent of CaX2Wherein X is Cl, Br or I, SiO2+P2O5The value is 62 to 62.5 percent, SiO2+Al2O3+ZrO2The value is 76.5 to 77%.
Further, the self-cleaning TFT-LCD substrate glass is characterized in that: and 0.1-0.2% of SnO.
Further, the self-cleaning TFT-LCD substrate glass is characterized in that: the strain point is higher than 650 ℃, the melting temperature is lower than 1630 ℃, and the forming temperature interval is higher than 150 ℃.
A preparation method of self-cleaning TFT-LCD substrate glass is characterized by comprising the following steps:
(1) selecting raw materials according to the proportion, mixing the raw materials, melting at 1580-1630 ℃, carrying out float forming at 1380-1180 ℃, and annealing to obtain TFT-LCD substrate glass;
(2) and (2) immersing the TFT-LCD substrate glass prepared in the step (1) into molten silver salt at the temperature of 350-420 ℃ for 4-20h, and performing ion exchange to form an Ag/AgX film on the surface of the glass.
Further, the temperature of the molten salt in the step (2) is 360-400 ℃, and the ion exchange time is 8-15 h.
Further, the temperature of the molten salt in the step (2) is 370-.
The self-cleaning TFT-LCD substrate glass comprises the following components:
SiO in the glass component2The content is increased, so that the light weight, the low thermal expansion coefficient and the chemical resistance of the glass are improved, but the high viscosity is not beneficial to production, and the proper range is 59-63%;
al in the glass component2O3With [ AlO ]4]The tetrahedral form enters the network and has a repairing effect on broken network, so that the structural compactness of the glass network is favorably enhanced, the characteristic viscosity point of the glass is increased, the high content is favorable for improving the strain point and the bending strength of the glass, but the glass is easy to crystallize when the content is too high, and the proper range is 16-18.5%;
p in the glass component2O5It is advantageous to lower the melting temperature of the glass because of P2O5Small viscous activation energy of the melt, it and B2O3Has a viscosity activation energy close to that of P2O5Into a glass structure to form [ PO ]4]One of the double-bonded oxygen atoms and the double-bonded phosphorus-oxygen tetrahedron is an asymmetric center, which can cause the viscosity of the glass to be reduced, thereby reducing the high-temperature characteristic viscosity point of the glass and being beneficial to the control of a float forming process, but the P is too high2O5The chemical stability of the glass is deteriorated, and the proper range is 0.5-1.5%;
the MgO and CaO in the glass components have similar effects, the high-temperature viscosity can be adjusted and reduced, the melting performance of the glass can be obviously improved, the strain point can not be reduced, but the chemical resistance of the glass can be reduced when the content is too high, and the proper ranges are 1.5-4 and 3.5-5.5 respectively;
in the glass component B2O3Can be used alone as a glass former and can form [ BO ] under high temperature conditions4]With decreasing temperature, B has free oxygen abstraction to form [ BO4]The tendency of (B) to make the structural region compact, increase the low-temperature viscosity of the glass, prevent devitrification, but too high of (B)2O3Is suitable for lowering the strain point of the glassThe range is 6-7.5%;
in the glass component, SrO is taken as a network exosome, so that the crystallization tendency and the crystallization speed can be reduced, the chemical stability and the mechanical strength of the glass are improved, but the excessive introduction of SrO can cause the glass to be loose, the density to be reduced and the hardness to be reduced, and the proper range is 6-7%;
ZrO in the glass component2Can effectively improve the chemical stability of the glass, reduce the expansion coefficient of the glass and obviously improve the elastic modulus of the glass, but ZrO2The solubility in glass is low, the glass crystallization tendency is increased, and the proper range is 0-0.2%;
CaX is introduced into the glass component2Then mixing with Ag in molten salt+Ion exchange is generated, a layer of Ag/AgX structure is formed on the surface of the glass, the photocatalysis effect is achieved, and the self-cleaning performance is generated, wherein X is Cl, Br or I, and the external doping amount is 0.01-0.08 wt%.
The invention has the advantages that:
(1) the self-cleaning TFT-LCD substrate glass has lower melting temperature, forming temperature and viscosity characteristic points, wider forming temperature range, improved glass liquid fluidity, reduced glass forming difficulty, and easy float forming (the strain point is higher than 650 ℃, the melting temperature is lower than 1630 ℃, and the forming temperature range is higher than 150 ℃);
(2) the invention uses ion exchange method, which has simple process and relatively low cost;
(3) the Ag/AgX film prepared on the glass surface of the self-cleaning TFT-LCD substrate has strong absorption in the visible light range and high sunlight utilization rate, and is compared with the traditional TiO film2Compared with the film, the film has greatly improved ultraviolet and visible absorption efficiency and excellent pollutant decomposition performance.
(4) The self-cleaning is applied to the TFT-LCD glass for electronic information display, thereby not only reducing the influence of environmental pollution on display devices, but also greatly prolonging the service life and prolonging the service life of products.
Drawings
FIG. 1 is a graph showing the UV-VIS absorption spectra of glasses according to examples 1 and 2 of the present invention.
Detailed Description
A self-cleaning TFT-LCD substrate glass formula suitable for float forming is formed by melting according to a glass preparation process and is fused with Ag+After salt ion exchange, self-cleaning TFT-LCD substrate glass for electronic information display is obtained; the specific implementation steps are as follows:
example 1
A self-cleaning TFT-LCD substrate glass formula suitable for float forming comprises 63 mass percent of SiO214% of Al2O30.5% of P2O56.5 percent of CaO, 5.5 percent of B2O34.5 percent of MgO, 5.8 percent of SrO, 0.2 percent of SnO and CaI doped outside2Amount 0.05%; the glass sample is obtained by batching and melting the glass according to the components, and the characteristic viscosity points in the float process are respectively as follows: the melting and clarifying temperature is 1598 ℃, the forming starting temperature is 1366 ℃ and the operating temperature is 1186 ℃, which are easy to control in the float forming process, and the silver salt and the Ag are immersed into the silver salt melt at 400 ℃ and are mixed+Ion exchange is carried out for 8h, self-cleaning glass is prepared, and the ultraviolet visible absorption spectrum is shown in figure 1.
Example 2
A self-cleaning TFT-LCD substrate glass formula suitable for float forming comprises 62% of SiO by mass215% of Al2O31% of P2O56 percent of CaO, 6 percent of B2O34% of MgO, 5.7% of SrO and 0.1% of ZrO20.2 percent of SnO and CaCl2Amount 0.05%; the glass sample is prepared by proportioning and melting the components, the characteristic viscosity points in the float process are respectively 1604 ℃ of melting and clarifying temperature, 1367 ℃ of forming starting temperature and 1190 ℃ of operating temperature, and the control of the float forming process is easy to realize by immersing 390 ℃ molten silver salt and Ag into the molten silver salt+Ion exchange is carried out for 10h, self-cleaning glass is prepared, and the ultraviolet visible absorption spectrum is shown in figure 1.
Example 3
A self-cleaning TFT-LCD substrate glass formula suitable for float forming comprises 61% of SiO by mass216% of Al2O31.5% of P2O55.5 percent of CaO, 6.5 percent of B2O33.5 percent of MgO, 5.65 percent of SrO and 0.15 percent of ZrO20.2 percent of SnO and CaI doped outside2Amount 0.05%; the glass sample is obtained by batching and melting the glass according to the components, and the characteristic viscosity points in the float process are respectively as follows: the melting and clarifying temperature is 1608 ℃, the forming starting temperature is 1370 ℃, the operating temperature is 1195 ℃, which is easy to control the floating forming process, and the silver salt and the Ag are immersed into the molten silver salt at 380 ℃ and are mixed+Ion exchange is carried out for 112h, and self-cleaning glass is prepared.
Example 4
A self-cleaning TFT-LCD substrate glass formula suitable for float forming comprises 60% of SiO by mass percentage217% of Al2O32% of P2O5、5% of CaO, 7% of B2O33% of MgO, 5.6% of SrO and 0.2% of ZrO20.2 percent of SnO and CaBr added2Amount 0.05%; the glass sample is prepared by mixing and melting the components, the characteristic viscosity points in the float process are respectively 1613 ℃ of melting and clarifying temperature, 1366 ℃ of forming starting temperature and 1201 ℃ of operating temperature, and the glass sample is easy to control in the float forming process and is immersed into 400 ℃ of molten silver salt and Ag+Ion exchange is carried out for 6 hours, and self-cleaning glass is prepared.
Example 5
A self-cleaning TFT-LCD substrate glass formula suitable for float forming comprises 59% of SiO by mass218% of Al2O32.5% of P2O54.5 percent of CaO, 7.5 percent of B2O32.5% of MgO, 5.55% of SrO and 0.25% of ZrO20.2 percent of SnO and CaI doped outside2Amount 0.05%; the glass sample is obtained by batching and melting the glass according to the components, and the characteristic viscosity points in the float process are respectively as follows: the melting and clarifying temperature is 1625 ℃, the forming starting temperature is 1373 ℃, the operating temperature is 1207 ℃, which is easy to control the floating forming process, and the silver salt and the Ag are immersed into the silver salt melted at 370 DEG C+Ion exchange is carried out for 15h, and self-cleaning glass is prepared.
Example 6
A self-cleaning TFT-LCD substrate glass formula suitable for float forming comprises 58% by massSiO219% of Al2O33% of P2O54% of CaO, 8% of B2O32% of MgO, 5.5% of SrO and 0.3% of ZrO20.2 percent of SnO and CaI doped outside2Amount 0.05%; the glass sample is obtained by batching and melting the glass according to the components, and the characteristic viscosity points in the float process are respectively as follows: the melting and clarifying temperature is 1623 ℃, the forming starting temperature is 1378 ℃, the operating temperature is 1207 ℃, which is easy to control the floating forming process, and the silver salt and the Ag are immersed into the molten silver salt at 400 ℃ and are mixed+Ion exchange is carried out for 18h, and self-cleaning glass is prepared.
Float characteristic points of the glasses obtained in examples 1 to 6 are shown in table 1.
TABLE 1 float characteristic points of examples 1 to 6
| Component (wt.%) | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 |
| SiO2 | 63 | 62 | 61 | 60 | 59 | 58 |
| Al2O3 | 14 | 15 | 16 | 17 | 18 | 19 |
| P2O5 | 0.5 | 1 | 1.5 | 2 | 2.5 | 3 |
| CaO | 6.5 | 6 | 5.5 | 5 | 4.5 | 4 |
| B2O3 | 5.5 | 6 | 6.5 | 7 | 7.5 | 8 |
| MgO | 4.5 | 4 | 3.5 | 3 | 2.5 | 2 |
| SrO | 5.8 | 5.7 | 5.65 | 5.6 | 5.55 | 5.5 |
| ZrO2 | 0 | 0.1 | 0.15 | 0.2 | 0.25 | 0.3 |
| SnO | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| SiO2+ P2O5 | 63.5 | 63 | 62.5 | 62 | 61.5 | 61 |
| SiO2+ Al2O3+ ZrO2 | 77 | 77.1 | 77.15 | 77.2 | 77.25 | 77.3 |
| Doped CaX2 | 0.05 | 0.05 | 0.05 | 0.05 | 0.05 | 0.05 |
| Melting clarification temperature (. degree.C.) | 1598 | 1604 | 1608 | 1613 | 1625 | 1623 |
| Temperature for onset of Molding (. degree. C.) | 1366 | 1367 | 1370 | 1366 | 1373 | 1378 |
| Operating temperature (. degree.C.) | 1186 | 1190 | 1195 | 1201 | 1207 | 1207 |
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; those skilled in the art can make numerous possible variations and modifications to the present teachings, or modify equivalent embodiments to equivalent variations, without departing from the scope of the present teachings, using the methods and techniques disclosed above. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention.
Claims (8)
1. The self-cleaning TFT-LCD substrate glass is characterized by being prepared from the following raw materials in percentage by mass: 59-63% of SiO216 to 18.5% of Al2O30.5 to 1.5% of P2O53.5 to 5.5 percent of CaO, 6 to 7.5 percent of B2O31.5 to 4% of MgO, 6 to 7% of SrO, and 0 to 0.2% of ZrO20.01 to 0.08% of CaX2Wherein X is Cl, Br or I, SiO2+P2O5The value is 60 to 63 percent, and SiO is2+Al2O3+ZrO2The value is 75.5 to 77%.
2. The self-cleaning TFT-LCD substrate glass according to claim 1, which is characterized by being prepared from the following raw materials in percentage by mass: 59-61.5% SiO216-17% of Al2O30.5 to 0.8% of P2O53.5 to 3.8 of CaO, 6 to 6.5 percent of B2O31.5 to 2.3 MgO, 6 to 6.4% SrO, 0.03 to 0.05% ZrO20.01 to 0.03% of CaX2Wherein X is Cl or BrOr I, SiO2+P2O5The value is 60 to 61.5 percent, SiO2+Al2O3+ZrO2The value is 75.5 to 75.8%.
3. The self-cleaning TFT-LCD substrate glass according to claim 1, which is characterized by being prepared from the following raw materials in percentage by mass: 62-62.8% of SiO217.5 to 18.5% of Al2O31 to 1.5% of P2O54 to 4.5 of CaO, 7.2 to 7.5 percent of B2O33.5 to 4 MgO, 6.5 to 7% SrO, 0.05 to 0.15% ZrO20.03 to 0.05 percent of CaX2Wherein X is Cl, Br or I, SiO2+P2O5The value is 62 to 62.5 percent, SiO2+Al2O3+ZrO2The value is 76.5 to 77%.
4. The self-cleaning TFT-LCD substrate glass according to claim 1, wherein: and 0.1-0.2% of SnO.
5. The self-cleaning TFT-LCD substrate glass according to any one of claims 1 to 4, wherein: the strain point is higher than 650 ℃, the melting temperature is lower than 1630 ℃, and the forming temperature interval is higher than 150 ℃.
6. A method for producing a self-cleaning TFT-LCD substrate glass using the glass raw material according to any one of claims 1 to 4, characterized by comprising the steps of:
(1) selecting raw materials according to the proportion, mixing the raw materials, melting at 1580-1630 ℃, carrying out float forming at 1380-1180 ℃, and annealing to obtain TFT-LCD substrate glass;
(2) and (2) immersing the TFT-LCD substrate glass prepared in the step (1) into molten silver salt at the temperature of 350-420 ℃ for 4-20h, and performing ion exchange to form an Ag/AgX film on the surface of the glass.
7. The method of producing a self-cleaning TFT-LCD substrate glass according to claim 6, wherein: the temperature of the molten salt in the step (2) is 360-400 ℃, and the ion exchange time is 8-15 h.
8. The method of producing a self-cleaning TFT-LCD substrate glass according to claim 6, wherein: the temperature of the molten salt in the step (2) is 370-380 ℃, and the ion exchange time is 10-12 h.
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