CN115073020B - Chemical tempering method of ultrathin foldable non-uniform thickness glass and ultrathin foldable non-uniform thickness tempered glass - Google Patents
Chemical tempering method of ultrathin foldable non-uniform thickness glass and ultrathin foldable non-uniform thickness tempered glass Download PDFInfo
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- CN115073020B CN115073020B CN202210713588.XA CN202210713588A CN115073020B CN 115073020 B CN115073020 B CN 115073020B CN 202210713588 A CN202210713588 A CN 202210713588A CN 115073020 B CN115073020 B CN 115073020B
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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
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
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Abstract
The invention discloses a chemical tempering method of ultrathin foldable non-uniform thickness glass and ultrathin foldable non-uniform thickness tempered glass; the chemical tempering method comprises the following steps: tempering the whole non-uniform-thickness glass according to a tempering process of the uniform-thickness region; covering a protective film on the surface of the equal-thickness area of the non-equal-thickness glass after the tempering treatment; etching the non-uniform thickness region of the non-uniform thickness glass after the tempering treatment to ensure that the stress difference between the non-uniform thickness region and the uniform thickness region is-80 MPa to-150 MPa and the stress depth difference is-2 mu m to-6 mu m; the method can ensure that the glass has smaller bending R angle and higher bending times in the bending area, the equal-thickness area has higher impact and scratch resistance, and the appearance of the glass is good.
Description
Technical Field
The invention belongs to the technical field of optical ultrathin foldable glass, and particularly relates to a chemical tempering method of ultrathin foldable non-uniform thickness glass and ultrathin foldable non-uniform thickness tempered glass.
Background
With the updating of electronic products, people tend to be lighter and thinner, the appearance of folding screens is more widely focused on all communities, and the appearance of ultrathin glass covers is more and more popular in the electronic display industry. The ultra-thin glass is firstly adopted in the Samsung Galaxy series in 2020 to be applied to the mobile phone cover plate, and the ultra-thin glass has small volume, thin thickness, high strength and good rebound resilience, can simultaneously give consideration to the using effects of the mobile phone and the Ipad, shows the provided new direction for the foldable computer and the scroll, and is favored by wide consumers.
Ultra-Thin Glass (UTG) is Glass with the thickness of less than 100 μm and flexibility, and the Ultra-Thin Glass after surface processing and edge treatment is widely applied to various electronic industries due to the advantages of high impact resistance, bending performance and the like, so that a significant milestone is marked for the folding display screen industry, the Ultra-Thin Glass becomes an important place in the field of folding flexibility after being connected with a CPI Cover plate, and a folding display terminal with UTG serving as a protective Cover plate (Cover window) appears, so that the form of the display terminal is not limited to a plane plate straightener or a conventional flip machine any more, and the display terminal has the development trend of various flow and is easier to carry.
However, if the non-uniform thickness glass is chemically tempered according to the non-uniform thickness region technology, the uniform thickness region cannot be sufficiently tempered, and the impact strength is low; if the glass is tempered according to the equal thickness area technology, the glass in the non-equal thickness area has the problem of excessive tempering, so that the central stress value is larger and the impact strength is lower; if the equal-thickness area and the non-equal-thickness area are toughened step by step according to different processes, the realization is almost difficult on the same glass, and the shielding and blocking are conventionally carried out through coating films or high-temperature resistant ink, but the operation steps are more complicated, and the areas are required to be protected during toughening, but even if the protection is carried out, the performance of the glass is deteriorated by repeated high-temperature heating.
Disclosure of Invention
In order to solve the technical problems, the invention provides a chemical tempering method of ultrathin foldable non-uniform thickness glass and the ultrathin foldable non-uniform thickness tempered glass; firstly, tempering the whole non-uniform-thickness glass, then etching the non-uniform-thickness region of the glass, and finally etching the whole non-uniform-thickness glass to remove the shadow problem on the surface of the glass, and meanwhile, the stress concentration on the surface of the tempered glass can be effectively relieved, and the strength of the glass is improved; the method can ensure that the glass has higher bending performance in non-equal thickness areas, higher impact and scratch resistance in equal thickness areas and good appearance of the glass.
The technical scheme adopted by the invention is as follows:
the chemical tempering method of the ultrathin foldable non-uniform thickness glass is characterized by comprising the following steps of:
(1) Tempering the whole non-uniform-thickness glass according to a tempering process of the uniform-thickness region;
(2) Covering a protective film on the surface of the equal-thickness area of the non-equal-thickness glass after the tempering treatment;
(3) Etching the non-uniform thickness region of the non-uniform thickness glass after the tempering treatment to ensure that the stress difference between the non-uniform thickness region and the uniform thickness region is-80 MPa to-150 MPa and the stress depth difference is-2 mu m to-6 mu m;
(4) And removing the protective film of the equal-thickness region, and then performing integral etching to solve the problem of shadow on the surface of the glass.
In the step (1), the tempering treatment method comprises the following steps: preheating at 370-400deg.C for 30-45min, and tempering at 380-410 deg.C for 10-60min. The stress value of the equal thickness area and the unequal thickness area of the non-equal thickness glass after the tempering treatment is 500-750MPa, which is the stress value specified by common ultrathin glass, and the depth of the stress layer is 6-12m. The tempering process is suitable for the tempering process of the glass equal-thickness area, the unequal-thickness area of the unequal-thickness glass tempered by the tempering process is excessively tempered, the central stress value is larger, and the impact strength is lower, so that the etching step of the unequal-thickness area is carried out to remove the redundant stress value and the stress layer of the unequal-thickness area, and the bending performance of the unequal-thickness area is ensured.
In the step (1), the tempering liquid is potassium nitrate solution with the purity of 99.99 percent; the thickness of the non-uniform thickness region of the glass is 100-150 mu m, and the thickness of the non-uniform thickness region is 30-70 mu m.
In the step (2), the protective film is an acid corrosion-resistant protective film, so that the equal-thickness area is prevented from being etched in the process of etching the non-equal-thickness area.
In the step (2), the protective film is a protective film made of polyurethane or a protective film made of PET, and can be soaked for 10-30min in mixed acid of hydrofluoric acid, sulfuric acid, phosphoric acid, ammonium sulfate, acetic acid, nitric acid and deionized water, so that acid permeation and falling off can be avoided.
In the step (3), the etching conditions are as follows: the etching temperature is 25-35 ℃, the acid etching rate is 0.5-1 mu m/min, and the etching amount is 2-6 mu m.
In the step (4), the protective film of the equal-thickness area is removed by adopting a direct manual film tearing mode.
In the step (5), the conditions of the bulk etching are: the etching temperature is 25-35 ℃, the acid etching rate is 0.5-1 mu m/min, the etching amount is 2-4 mu m, and the problem of light shadow caused by film coating is removed.
In the step (2) and the step (5), the etching solution used for etching comprises the following raw materials in percentage by weight: 0.1 to 0.4 percent of hydrofluoric acid, 40 to 60 percent of sulfuric acid, 0.2 to 0.4 percent of phosphoric acid, 1 to 2 percent of ammonium sulfate, 1.0 to 20.0 percent of acetic acid, 2.0 to 10.0 percent of nitric acid and the balance of deionized water.
The invention also provides ultrathin foldable non-uniform thickness toughened glass, which is obtained by toughening the non-uniform thickness glass by adopting the chemical toughening method disclosed by the invention, wherein the non-uniform thickness region of the toughened glass has higher bending performance, and the uniform thickness region has higher impact and scratch resistance.
Compared with the prior art, the invention has the following advantages:
(1) According to the invention, the ultrathin foldable non-uniform thickness glass is only subjected to one-time tempering treatment, so that adverse effects on the glass caused by repeated high-temperature heating are avoided, the tempering steps are simple, and the operation is convenient;
(2) After the tempering treatment, the stress depth of the non-uniform thickness area is reduced only by an etching process, so that the stress value of the non-uniform thickness area is reduced, the etching depth can be controlled according to the requirement in the process, the stress value of the non-uniform thickness area is controlled, and different customer requirements are met.
(3) Finally, the invention carries out integral etching on the non-uniform thickness glass to remove the shadow problem left in the process of etching the stress layer of the non-uniform thickness region, thereby ensuring the appearance performance of the non-uniform thickness glass finished product; the invention can ensure that the equal thickness area and the non-equal thickness area can obtain corresponding toughening depth by the way of etching after toughening.
(4) The method can ensure that the bending area has smaller bending R angle and higher bending times, and the non-bending area has higher pen impact resistance and better scratch resistance.
(5) The ultrathin foldable unequal-thickness glass treated by the method can realize inward bending and outward bending, has excellent bending performance, high impact resistance and scratch resistance, and effectively replaces the problem of wrinkles caused by excessive bending times of the existing product.
Drawings
FIG. 1 is a schematic diagram of the tempering step of the ultrathin foldable non-uniform thickness glass.
Detailed Description
The present invention will be described in detail with reference to examples.
The tempering liquid used in each example was a 99.99% potassium nitrate solution; the etching solution comprises the following components in percentage by weight: 0.3% of hydrofluoric acid, 50% of sulfuric acid, 0.3% of phosphoric acid, 1.5% of ammonium sulfate, 10% of acetic acid, 6% of nitric acid and the balance of deionized water.
Example 1
A chemical tempering method of ultrathin foldable non-uniform thickness glass comprises the following steps:
(1) Tempering the whole non-uniform thickness glass with the thickness of the uniform thickness area being 100 mu m and the thickness of the non-uniform thickness area being 30 mu m, wherein the stress value of the uniform thickness area and the non-uniform thickness area of the non-uniform thickness glass after tempering is 732MPa, and the depth of the stress layer is 10.8 mu m; the tempering treatment conditions are as follows: preheating at 370deg.C for 45min, and tempering at 380deg.C for 50min;
(2) Covering PET protective films on the surfaces of the equal-thickness areas of the non-equal-thickness glass after the tempering treatment;
(3) Etching the non-uniform thickness glass in etching solution for 8min to ensure that the stress difference between the non-uniform thickness region and the uniform thickness region is-140 MPa and the stress depth difference is-4 mu m;
(4) And removing the protective film of the equal thickness region, and then placing the non-equal thickness glass into etching solution to etch for 6min and 3 mu m so as to solve the problem of shadow on the surface of the glass.
Example 2
A chemical tempering method of ultrathin foldable non-uniform thickness glass comprises the following steps:
(1) Tempering the whole non-uniform thickness glass with the thickness of 80 mu m in the uniform thickness region and the thickness of 40 mu m in the non-uniform thickness region, wherein the stress value of the uniform thickness region and the non-uniform thickness region of the non-uniform thickness glass after tempering is 716MPa, and the depth of the stress layer is 9.7 mu m; the tempering treatment conditions are as follows: preheating at 370 ℃ for 45min, and tempering at 370 ℃ for 40min;
(2) Covering PET protective films on the surfaces of the equal-thickness areas of the non-equal-thickness glass after the tempering treatment;
(3) Etching the non-uniform thickness glass in etching solution for 6min to ensure that the stress difference between the non-uniform thickness region and the uniform thickness region is-90 MPa and the stress depth difference is-3 mu m;
(4) And removing the protective film of the equal thickness region, and then placing the non-equal thickness glass into etching solution to etch for 6min and 3 mu m so as to solve the problem of shadow on the surface of the glass.
Example 3
A chemical tempering method of ultrathin foldable non-uniform thickness glass comprises the following steps:
(1) Tempering the whole non-uniform thickness glass with the thickness of 70 mu m in the uniform thickness region and the thickness of 30 mu m in the non-uniform thickness region, wherein the stress value of the uniform thickness region and the non-uniform thickness region of the non-uniform thickness glass after tempering is 706MPa, and the depth of the stress layer is 9.2 mu m; the tempering treatment conditions are as follows: preheating at 370deg.C for 45min, and tempering at 380deg.C for 35min;
(2) Covering PET protective films on the surfaces of the equal-thickness areas of the non-equal-thickness glass after the tempering treatment;
(3) Etching the non-uniform thickness glass in etching solution for 4min to ensure that the stress difference between the non-uniform thickness region and the uniform thickness region is-85 MPa and the stress depth difference is-2 mu m;
(4) And removing the protective film of the equal thickness region, and then placing the non-equal thickness glass into etching solution to etch for 6min and 3 mu m so as to solve the problem of shadow on the surface of the glass.
The properties of the non-uniform thickness glass after the tempering treatment in step (1) and after the etching treatment in step (4) in each example are shown in table 1.
TABLE 1
As can be seen from the table, the non-isopachous region of the ultra-thin foldable non-isopachous glass treated by the method of the invention has smaller R angle and higher bending times in the bending region, and the isopachous region has higher impact and scratch resistance.
If the thickness of the equal thickness area is 70-100 and the thickness of the unequal thickness area is 30-40, tempering is carried out on the unequal thickness glass according to the tempering technology of the unequal thickness area, namely the tempering condition is 380-400 ℃, the tempering time is 20-60min, and the impact strength (cm) of the equal thickness area and the unequal thickness area of the unequal thickness glass after tempering is respectively 30-40 and 10-15; the pencil hardness (H) is respectively 6-7 and 1-2 in the equal thickness area and the unequal thickness area; the bending R angle (mm) is R1.5-R3, and the bending times are less than 50K; it can be seen that the equal thickness area has poor impact resistance and scratch resistance after the tempering treatment in the examples.
The foregoing detailed description of a chemical tempering method for ultra-thin foldable non-uniform thickness glass and ultra-thin foldable non-uniform thickness tempered glass with reference to the embodiments is illustrative and not restrictive, and several embodiments may be listed according to the defined scope, thus, variations and modifications without departing from the general inventive concept shall fall within the scope of protection of the present invention.
Claims (5)
1. The chemical tempering method of the ultrathin foldable non-uniform thickness glass is characterized by comprising the following steps of:
(1) Tempering the whole non-uniform-thickness glass according to a tempering process of the uniform-thickness region;
(2) Covering a protective film on the surface of the equal-thickness area of the non-equal-thickness glass after the tempering treatment;
(3) Etching the non-uniform thickness region of the non-uniform thickness glass after the tempering treatment to ensure that the stress difference between the non-uniform thickness region and the uniform thickness region is-80 MPa to-150 MPa and the stress depth difference is-2 mu m to-6 mu m;
(4) Removing the protective film of the equal-thickness region, and then performing integral etching to solve the problem of shadow on the surface of the glass;
in the step (1), the thickness of the non-uniform thickness glass uniform thickness region is 100-150 mu m, and the thickness of the non-uniform thickness region is 30-70 mu m;
in the step (1), the stress value of the equal thickness area and the unequal thickness area of the non-equal thickness glass after the tempering treatment is 500-750MPa, and the depth of the stress layer is 6-12 mu m;
in the step (1), the tempering treatment method comprises the following steps: preheating at 370-400deg.C for 30-45min, and tempering at 380-410 deg.C for 10-60min;
in the step (3), the etching conditions are as follows: the etching temperature is 25-35 ℃, the acid etching rate is 0.5-1 mu m/min, and the etching amount is 2-6 mu m;
in the step (5), the conditions of the bulk etching are: the etching temperature is 25-35 ℃, the acid etching rate is 0.5-1 mu m/min, and the etching amount is 2-4 mu m.
2. The method for chemically tempering ultra-thin foldable non-uniform thickness glass according to claim 1, wherein in the step (1), the tempering liquid is a potassium nitrate solution with a purity of 99.99%.
3. The method for chemically tempering ultra-thin foldable non-uniform thickness glass according to claim 1, wherein in step (2), the protective film is an acid corrosion resistant protective film.
4. The method for chemically toughening ultra-thin foldable non-uniform thickness glass according to claim 1, wherein in the step (2), the protective film is a protective film made of polyurethane or a protective film made of PET.
5. An ultra-thin foldable non-uniform thickness tempered glass, characterized in that the non-uniform thickness tempered glass is obtained by tempering by the chemical tempering method according to any one of claims 1 to 4.
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| CN115636594A (en) * | 2022-10-27 | 2023-01-24 | 芜湖东信光电科技有限公司 | Microporous foldable glass and preparation method thereof |
| CN115849690B (en) * | 2022-11-17 | 2024-12-06 | 芜湖东信光电科技有限公司 | Chemical tempering device for ultra-thin glass of unequal thickness and tempering method thereof |
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| CN109153599A (en) * | 2016-05-19 | 2019-01-04 | 苹果公司 | Asymmetric chemical strengthening |
| CN112135803A (en) * | 2018-05-18 | 2020-12-25 | 肖特玻璃科技(苏州)有限公司 | Ultra-thin glass with high impact resistance |
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