CN110655304A - Glass capable of effectively improving chemical strengthening warping property - Google Patents
Glass capable of effectively improving chemical strengthening warping property Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B18/00—Shaping glass in contact with the surface of a liquid
- C03B18/02—Forming sheets
- C03B18/20—Composition of the atmosphere above the float bath; Treating or purifying the atmosphere above the float bath
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B18/00—Shaping glass in contact with the surface of a liquid
- C03B18/02—Forming sheets
- C03B18/18—Controlling or regulating the temperature of the float bath; Composition or purification of the float bath
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B18/00—Shaping glass in contact with the surface of a liquid
- C03B18/02—Forming sheets
- C03B18/20—Composition of the atmosphere above the float bath; Treating or purifying the atmosphere above the float bath
- C03B18/22—Controlling or regulating the temperature of the atmosphere above the float tank
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B27/00—Tempering or quenching glass products
- C03B27/02—Tempering or quenching glass products using liquid
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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
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
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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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
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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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
- C03C17/245—Oxides by deposition from the vapour phase
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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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
- C03C17/25—Oxides by deposition from the liquid phase
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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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Abstract
The invention discloses glass for effectively improving chemical strengthening warping performance, wherein the side surface of the glass, namely the distribution of CS & ltDOL & gt in the thickness direction, meets | (. integral & gt CS & ltDOLdT, T is more than or equal to 0 and less than or equal to D/2)/(. integral & gt CS & ltDOLdT, -D/2 and less than or equal to 0) -1| and less than or equal to 10T%, T is corresponding thickness, the center of the glass is taken as the origin of coordinates, a tin surface is-D/2, and an air surface is D/2; in addition, the central tensile stress (CT) = CS × DOl/(T-2 DOL). The controllable chemical strengthening warping performance of the float glass is realized.
Description
Technical Field
The invention belongs to the field of glass, relates to float glass, and provides glass capable of effectively improving chemical strengthening warping performance and a preparation method thereof.
Background
In recent years, displays having a touch panel, such as tablet computers, smart phones, car screens, and the like, have been essential for electronic information products. The outermost layer of the touch screen display is provided with a layer of protective Glass, also known as Cover Glass. Cover glass is required to have good mechanical strength (bending resistance, impact resistance, and drop resistance) as an outer screen of a mobile phone. At present, the method for improving the mechanical property of cover glass mainly adopts a low-temperature chemical ion exchange strengthening method, and the principle is as follows: in the temperature region below the strain point of the glass, alkali ions (such as Na) are used for the surface layer+) Monovalent cations with large ionic radii (e.g. K)+) With Na+Ion exchange of K+A method of accessing a skin layer. In short, a Na-containing glass is immersed in a melt containing a high concentration of K in a certain temperature range. However, the strengthening method requires that the components, thermal history and other properties of the two surfaces of the glass are close to each other, otherwise, the strengthened glass is poor in flatness (warpage value) which affects the bonding effect of the glass, and thus the overall machine dropping effect of products such as smart phones is affected.
The current mainstream production mode of cover glass comprises an overflow method (such as Corning, NEG, rainbow and koshidi), a float process (AGC-asahi glass, asahi rainbow and south glass), wherein the two surfaces of the overflow method are basically consistent in environment and basically similar in thermal history when the glass is formed, the warping value is generally far lower than the required standard (a smart phone is generally 0.25mm) after chemical strengthening, the float glass is formed on the surface of molten metal Sn, the surface in contact with the metal surface is called a tin liquid surface, and the surface not in contact with the metal surface is called an air surface. During molding, the air surface and the tin liquid surface are in different environments, so that chemical components and structures have certain differences. Chemical components and structures of an air surface and a tin surface of float glass are asymmetrical, so that CS and DOL (CS-surface compressive stress and DOL-ion exchange depth) of two surfaces after chemical strengthening are inconsistent, the warping amount of the chemically strengthened glass exceeds the standard, and the product bonding and the whole machine falling are influenced.
The current methods for treating warpage are mainly as follows: 1) the cover plate glass processing factory carries out certain grinding to glass both sides to reach the purpose that glass both sides composition is unanimous, this kind of mode influences processing rate, processing cost. 2) For on-line processing of glass raw sheets, for example, in patent CN201280064392, inorganic source gas, oxygen, carrier gas, etc. are used as raw materials to form inorganic oxide film on the glass surface by chemical vapor deposition, which requires control of chemical reaction process and high control of gas flow. 3) The chemical tempering warpage of float glass is regulated and controlled by adjusting the alkali metal content of an air surface and a tin surface, for example, in patent CN201380068423, acidic gas and liquid containing atoms such as F, Cl and S are used to perform dealkalization reaction with the glass surface, the acidic gas used in the method has a corrosion effect on a kiln body, the service life of the kiln body is influenced, and in addition, the acidic gas and liquid containing atoms such as F, Cl and S have great harm to the environment.
Disclosure of Invention
The invention provides glass capable of effectively improving the chemical strengthening warping performance, so that the chemical strengthening warping performance of float glass can be controlled.
The technical scheme provided by the invention is that the glass effectively improves the chemical strengthening warping performance, the side surface of the glass, namely the distribution of CS & ltDOL & gt in the thickness direction, meets | (& ltintegral & gt CS & ltDOLdT, T & ltSUB & gt 0 & lt/SUB & gt)/(& ltintegral & gt CS & ltintegral & gt DOLdT, T & ltSUB & gt/2 & lt/SUB & gt 0) & ltSUB & gt-1 & lt| & lt/SUB & gt & lt/10T & gt, T is the corresponding thickness, the center of the glass is taken as the origin of coordinates, the; further, the central tensile stress (CT) ═ CS DOl/(T-2 DOL).
Preferably, CS & ltSUP & gt DOL distribution satisfies | (. integral & ltSUP & gt CS & ltSUP & gt DOLdT,0 & ltSUP & gt, D/2 & ltSUP & gt, T & ltSUP & gt, & ltSUP & gt CS & ltSUP & gt, 0) -1 & ltSUP & gt, T.
Further preferably, the glass air surface is a, the tin surface is B, and the CS × DoL ratio | CS of the a surface and the B surfaceA*DOLA/CSB*DOLB-1∣≤T％。
Further, the glass is produced by an overflow method, a down-draw method or a float method.
Further, after the glass is polished, the CS and DOL value of the polished surface is larger than that of the non-polished surface.
The invention also relates to a method for preparing the glass, which comprises the steps of forming the glass and carrying out subsequent surface treatment to adjust the CS and DOL values so as to meet the distribution rule of CS and DOL on the side surface of the glass in the thickness direction.
Further, in the forming process, the CS and DOL values are adjusted by controlling the temperature of different areas of the glass or controlling the component distribution of the areas with different thicknesses of the glass by using an electric field or a magnetic field.
Further, the subsequent surface treatment comprises glass surface dealkalization treatment and glass surface coating treatment.
By constraining the distribution of CS × DOL, there was good warpage values not only on 2D products, but also on 2.5D cover glasses. The 2.5D product has an asymmetric structure, so that four corners of the 2.5D structure are easy to warp, namely, ship warp exists; in addition, an asymmetrical polishing process exists in the processing process of the 2.5D product, and the CS and DOL values of the surface of the product are not balanced, so that the problem of warpage control is brought. For a 2.5D product, the precision is limited due to the stress detector, and the side face of the product is a frosted surface, so that only CS and DOL values of an upper plane and a lower plane can be detected, and the stress distribution of the side face cannot be directly measured. Therefore, the stress distribution condition of the side surface can be indirectly reflected only according to the CS and DOL values of the upper plane and the lower plane.
The glass prepared by the method provided by the invention has good reinforced warping, and does not need to be ground in a subsequent cover plate processing factory.
If the chemical deposition principle is adopted for coating, one side of the glass is coated with the Al-rich film2O3Solvent suspension, surface formation of SiO-rich2、Al2O3Layer, which can improve the hardness of the glass surface, improve the chemical resistance and surface scratch resistance of the glass, form a stress-free layer with certain thickness on one side of the glass, and simultaneously, the thickness of the stress-free layerIncreasing also changes the geometric center of the glass, thereby improving warpage. SiO 22、Al2O3Chemical composition is closer to that of glass, especially for aluminosilicate glass, SiO2、Al2O3The optical refractive index of the oxide layer is close to that of float glass, and the oxide layer basically has no influence on the optical performance of the original glass and does not deteriorate the original optical performance.
Drawings
Fig. 1 is a graph of the CS × DoL values of float glass as a function of the thickness direction T of the glass. Wherein T is the thickness, the center of the glass is taken as the origin of coordinates, A is the air surface, and B is the tin surface.
Fig. 2 is a schematic structural view of a 2.5D cover glass.
Detailed Description
The invention will be further elucidated with reference to the following examples.
The glass substrate composition may be aluminosilicate glass, boroaluminosilicate glass, lithium aluminosilicate glass, or the like. Because the chemical strengthening warpage of the glass produced by the processes of an overflow method, a down-draw method and the like generally meets the standard, the glass substrate selected by the invention is a float process product. The chemical strengthening process of the aluminosilicate glass is single, the processing influence is small, and the aluminosilicate glass with 13 percent (wt percent) of aluminum content is selected as the target in the specific embodiment of the invention.
Example 1:
the thickness of the glass substrate has no special requirements, and when the chemical strengthening process is fixed, the larger the thickness is, the smaller the chemical strengthening warpage is, and the product with the thickness of 0.7mm is selected.
In the preparation process of the glass, the obtained glass has good chemical strengthening warping performance through tin bath process adjustment, acid treatment, annealing kiln film coating and other controls.
Specifically, the tin bath process adjustment can firstly reduce the tin bath pressure properly, increase the temperature of partial tin bath area, increase the tin content in the atmosphere, secondly adjust the tin bath shielding gas composition, in the shielding gas mixing, add a certain amount of tin vapor, and introduce the shielding gas mixed with the tin vapor into the tin bath, so that the tin in the tin bath atmosphere is in a supersaturated state, deposit a layer of tin film on the non-tin surface of the glass, namely, form a tin infiltration layer on the air surface of the glass, reduce the composition difference between the tin surface and the air surface, and reduce the DOL value of the air surface after chemical strengthening. The temperature and the flow rate of the protective gas can be adjusted, the alkali volatilization on the surface is increased, so that an alkali-poor layer is formed on the air surface of the glass, and the CS value of the air surface after chemical strengthening is reduced.
Selecting HCl and SO during acidic treatment2And one or more of the acid gases are mixed, the mixture is guided into a kiln for advancing and retreating under the guide of carrier gases such as water vapor, compressed air and the like according to a certain flow rate, the basic surface of the glass is treated, the treatment temperature is in a range of 500-800 ℃, the acid treatment mainly shows micro-crack holes and reacts with Na on the surface layer of the air surface, the CS value after chemical strengthening is reduced, and the acid treatment area needs to be isolated by a baffle.
When the annealing kiln is coated with the film, the coating film can be an inorganic oxide film, and the inorganic oxide film can be SiO2、Al2O3Oxides of good chemical stability and high hardness, SiO2、Al2O3Is closer to the glass substrate and is between 1.50 and 1.52. The method mainly selects silica sol, alumina sol or a mixture of the silica sol and the alumina sol, atomizes by using a high-temperature spray head, an atomizing chamber and the like, enters an annealing kiln under the guidance of compressed air, and carries out chemical deposition coating on the surface of glass at the treatment temperature of 500-800 ℃.
The glass substrate is annealed, cut, CNC (shape processing), polished (0min, 5min, 10min, 15min, 20min), chemically strengthened and detected. Wherein the chemical strengthening is by K+Exchange of Na in glass+The method adopts the general cover plate processing plant process that the ion exchange temperature is 390-. The detection adopts conventional instruments in the industry: FSM6000le stress tester, warpage was tested using a plug gauge or laser tester.
Because the glass substrate is thin, the CS and DOL values in the thickness direction are not easy to grasp, the invention adopts the indirect representation of the CS and DOL values on the upper surface and the lower surface, and the CS and DOL values are not obvious after polishing for 15min through a double-sided polishing test, and the two surfaces are basically consistent. Specifically, the following table 1 shows.
TABLE 1
By SO2Introducing gas into the kiln at a certain flow rate, isolating the area with a curtain at 660 deg.C, and performing dealkalization treatment to chemically strengthen the air surface. Specific data are shown in table 2 below.
TABLE 2
On the basis of dealkalization, in the temperature region of 640 ℃, Al is plated2O3The film, specific data are shown in table 3 below.
TABLE 3
In addition, the change in warpage after chemical strengthening is shown in table 4 below:
TABLE 4
One side of the edge of the glass in the 2.5D product is an arc, the arc needs to be polished to have certain brightness, the polishing time is generally 10-15min, and the product structure is shown in figure 2. Due to the fact that the product structure is asymmetric, the 2.5D surface generates ship warping (the 2.5D surface is arranged on the upper portion, and four corners are warped). CS & ltDOL & gt close to the surface of the product is smaller than other regions, after polishing, the integral & ltCS & gtDOLdT & lt of the 2.5D surface is larger than the integral & ltCS & gtDOLdT & lt of the 2D surface, and tortoises and upwarping (2.5D surface is upward and arched) can be caused, so that the warpage generated by asymmetric structure is offset, and the glass capable of effectively improving the chemically-strengthened warping performance is obtained.
Example 2: in the embodiment, a sol-gel principle is adopted for coating, a stress-free layer with a certain thickness is formed on one surface of the glass, and the geometric center of the glass is changed due to the increase of the thickness, so that the warping is improved.
Experiment raw materials: 0.7mm, 2.5D product, silica sol.
The experimental process comprises the following steps: cutting glass, CNC and polishing to obtain a 2.5D unreinforced product, plating silica sol on a non-polished surface, and curing the silica sol in an oven. A multi-batch test was conducted in which the control piece was not coated with silica sol, and the test sample was treated with silica sol. Specific data are shown in table 5 below, and from the test data, the silica sol coating film is also beneficial to improving the warping.
TABLE 5
Example 3:
experiment raw materials: 0.7mm product, 10% solid content alumina sol suspension.
The experimental process comprises the following steps: putting a product of 300mm x 300mm into a tempering preheating furnace, heating to 500 ℃, atomizing the alumina sol by using a spray bottle, spraying a proper amount of the alumina sol to the air surface of the glass sheet, closing a furnace door, preserving heat for a period of time, and cooling along with the temperature of the furnace. And then carrying out CNC, cleaning, toughening and detection. Specific data are shown in table 6 below.
Coating a certain side of glass with Al-rich film2O3The solvent suspension forms a stress-free layer with a certain thickness on one surface of the glass, and the increase of the thickness also changes the geometric center of the glass, thereby improving the warping.
In the process of Al plating2O3In sol-gel process, the toughening warpage should be increased and then decreased theoretically, because when plating a trace amount of Al, the surface AlO is increased4]Increasing the tempering DOL value of the air surface, thereby increasing tempering warpage, [ AlO ] with increasing Al plating amount4]The gradual reduction, tempering warpage reduces, but does not find the process that tempering warpage increases in the experimentation, probably because the experimental facilities is too simple, and the coating film volume can't accurate management and control, also probably the coating film temperature is too low, does not destroy the original group structure composition of glass.
TABLE 6
Claims (9)
1. A glass effective in improving the warpage properties of chemically strengthened glass, characterized in that: the side surface of the glass, namely the distribution of CS & ltDOL & gt in the thickness direction meets | (& ltintegral & gt CS & ltDOLdT & gt, T & ltintegral & gt 0 & lt & gtD/2 & lt & gtT & ltintegral & gt CS & ltDOLdT & gt, -D/2 & lt & gtT & lt & gt 0) -1| & lt & gtT & lt & gt 10T & lt & gtT is the corresponding thickness, the center of the glass is taken as the origin of coordinates, the tin surface is-D/2, and the air surface is D/2; further, the central tensile stress (CT) ═ CS DOl/(T-2 DOL).
2. The glass according to claim 1, wherein: CS & ltSUB & gt DOL distribution satisfies | (. integral | (. CS & ltSUB & gt DOLdT,0 & ltSUB & gt) D/2)/(. integral | (. CS & ltSUB & gt DOLdT, -D/2 & ltSUB & gt 0) -1| & ltSUB & gt.
3. The glass according to claim 1, wherein: the glass has air surface A, tin surface B, and CS-DoL ratio | CS of the surfaces A and BA*DOLA/CSB*DOLB-1∣≤T％。
4. The glass according to claim 1, wherein: the glass is produced by an overflow process, a down-draw process or a float process.
5. The glass according to claim 1, wherein: after the glass is polished, the CS DOL value of the polished surface is larger than that of the non-polished surface.
6. The glass according to claim 1, wherein: the glass is 2D and/or 2.5D glass.
7. A method of making a glass according to any one of claims 1 to 6, wherein: the method comprises the steps of forming glass and subsequent surface treatment, and the values of CS and DOL are adjusted to meet the distribution rule of the side surface of the glass, namely the thickness direction CS and DOL.
8. The method of claim 7, wherein: in the forming process, the CS and DOL values are adjusted by controlling the temperature of different areas of the glass or controlling the component distribution of the areas with different thicknesses of the glass by using an electric field or a magnetic field.
9. The method of claim 7, wherein: the subsequent surface treatment comprises glass surface dealkalization treatment and glass surface coating treatment.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111333348A (en) * | 2020-03-10 | 2020-06-26 | 醴陵旗滨电子玻璃有限公司 | Chemical strengthening method, chemical strengthening device and chemically strengthened glass |
| CN111592233A (en) * | 2020-05-29 | 2020-08-28 | 醴陵旗滨电子玻璃有限公司 | Chemically strengthened glass, float glass raw sheet, preparation method and production line thereof |
| CN114656815A (en) * | 2022-03-31 | 2022-06-24 | 醴陵旗滨电子玻璃有限公司 | Coating liquid, preparation method thereof and chemical strengthening method |
| CN115028357A (en) * | 2022-06-17 | 2022-09-09 | 四川虹科创新科技有限公司 | Low-warpage scratch-resistant sodium-aluminum-silicon glass and preparation method and application thereof |
| CN115925280A (en) * | 2022-11-25 | 2023-04-07 | 安徽繁盛显示科技有限公司 | Asymmetric toughened ultrathin glass, manufacturing method and display panel |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111333348A (en) * | 2020-03-10 | 2020-06-26 | 醴陵旗滨电子玻璃有限公司 | Chemical strengthening method, chemical strengthening device and chemically strengthened glass |
| CN111592233A (en) * | 2020-05-29 | 2020-08-28 | 醴陵旗滨电子玻璃有限公司 | Chemically strengthened glass, float glass raw sheet, preparation method and production line thereof |
| CN114656815A (en) * | 2022-03-31 | 2022-06-24 | 醴陵旗滨电子玻璃有限公司 | Coating liquid, preparation method thereof and chemical strengthening method |
| CN115028357A (en) * | 2022-06-17 | 2022-09-09 | 四川虹科创新科技有限公司 | Low-warpage scratch-resistant sodium-aluminum-silicon glass and preparation method and application thereof |
| CN115925280A (en) * | 2022-11-25 | 2023-04-07 | 安徽繁盛显示科技有限公司 | Asymmetric toughened ultrathin glass, manufacturing method and display panel |
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