CN115073020A - Chemical tempering method for ultrathin foldable non-equal-thickness glass and ultrathin foldable non-equal-thickness tempered glass - Google Patents
Chemical tempering method for ultrathin foldable non-equal-thickness glass and ultrathin foldable non-equal-thickness tempered glass Download PDFInfo
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- CN115073020A CN115073020A CN202210713588.XA CN202210713588A CN115073020A CN 115073020 A CN115073020 A CN 115073020A CN 202210713588 A CN202210713588 A CN 202210713588A CN 115073020 A CN115073020 A CN 115073020A
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- 239000011521 glass Substances 0.000 title claims abstract description 87
- 238000000034 method Methods 0.000 title claims abstract description 44
- 238000005496 tempering Methods 0.000 title claims abstract description 40
- 239000000126 substance Substances 0.000 title claims abstract description 20
- 239000005341 toughened glass Substances 0.000 title claims abstract description 11
- 238000005530 etching Methods 0.000 claims abstract description 50
- 230000001681 protective effect Effects 0.000 claims abstract description 18
- 239000002253 acid Substances 0.000 claims description 8
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 3
- 239000004323 potassium nitrate Substances 0.000 claims description 3
- 235000010333 potassium nitrate Nutrition 0.000 claims description 3
- 238000005260 corrosion Methods 0.000 claims description 2
- 230000007797 corrosion Effects 0.000 claims description 2
- 229920002635 polyurethane Polymers 0.000 claims description 2
- 239000004814 polyurethane Substances 0.000 claims description 2
- 238000005452 bending Methods 0.000 abstract description 20
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 3
- 235000011130 ammonium sulphate Nutrition 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 238000005243 fluidization Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
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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
-
- 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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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
The invention discloses a chemical toughening method of ultrathin foldable non-equal-thickness glass and the ultrathin foldable non-equal-thickness toughened glass; the chemical toughening method comprises the following steps: tempering the non-equal-thickness glass integrally according to the tempering process of the equal-thickness area; covering a protective film on the surface of the equal-thickness area of the toughened non-equal-thickness glass; etching the non-equal-thickness area of the toughened non-equal-thickness glass to ensure that the stress difference value between the non-equal-thickness area and the equal-thickness area is-80 MPa to-150 MPa and the stress depth difference value is-2 mu m to-6 mu m; the protective film in the equal-thickness area is removed, then the whole etching is carried out to remove the problem of light and shadow on the surface of the glass, the method can ensure that the bending area has a smaller bending R angle and higher bending times, 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 toughening method of ultrathin foldable non-equal-thickness glass and the ultrathin foldable non-equal-thickness toughened glass.
Background
With the update of electronic products, people tend to thin and light the glass cover plate, the appearance of the folding screen attracts more and more extensive attention of all social circles, and the appearance of the ultrathin glass cover plate is popular among more and more listed companies in the electronic display industry. The Samsung Galaxy series are applied to the mobile phone cover plate for the first time in 2020, and due to the fact that the Samsung Galaxy series are small in size, thin in thickness, high in strength and good in rebound resilience, the using effects of the mobile phone and the Ipad can be considered simultaneously, a new direction is provided for a foldable computer and a scroll, and the Samsung Galaxy series are popular with consumers.
Ultra-Thin Glass (UTG) refers to Glass with the thickness of less than 100 microns and flexibility, 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, a great milestone is drawn for the folding display screen industry, the Ultra-Thin Glass becomes a CPI Cover plate and has an important position in the field of folding flexibility, a folding display terminal with UTG as a protective Cover plate (Cover window) is appeared, the display terminal shape is not limited to a plane straight plate machine or a conventional Cover turning machine any more, the development trend of diversified fluidization is presented, and the Ultra-Thin Glass is easier to carry.
But the non-equal-thickness glass has the toughening bottleneck problem, if chemical toughening is carried out according to the non-equal-thickness area process, the equal-thickness area can not be fully toughened, and the impact strength is lower; if tempering is carried out according to the equal-thickness area process, the glass in the non-equal-thickness area has the problem of excessive tempering, so that the central stress value is large, and the impact strength is low; if the equal-thickness area and the non-equal-thickness area are respectively tempered step by step according to different processes, the tempering treatment is hardly realized on the same piece of glass, the conventional process is shielded and blocked by coating or high-temperature-resistant ink, but the operation steps are complicated, and the protection is required to be carried out in a subarea mode during tempering, but even if the protection is carried out, the performance of the glass is degraded by repeated high-temperature heating.
Disclosure of Invention
In order to solve the technical problems, the invention provides a chemical toughening method of ultrathin foldable non-equal-thickness glass and the ultrathin foldable non-equal-thickness toughened glass; firstly, tempering the non-uniform-thickness glass integrally, etching the non-uniform-thickness area of the non-uniform-thickness glass, and finally etching the non-uniform-thickness glass integrally to remove the problem of light and shadow on the surface of the glass, and simultaneously effectively relieving the stress concentration on the surface of the tempered glass and improving the strength of the glass; the method can ensure that the glass has higher bending performance in a non-equal-thickness area, has higher impact and scratch resistance in an equal-thickness area, and has good appearance.
The technical scheme adopted by the invention is as follows:
a chemical toughening method of ultrathin foldable non-uniform-thickness glass is characterized by comprising the following steps:
(1) carrying out tempering treatment on the non-equal-thickness glass integrally according to the tempering process of the equal-thickness area;
(2) covering a protective film on the surface of the equal-thickness area of the toughened non-equal-thickness glass;
(3) etching the non-equal-thickness area of the toughened non-equal-thickness glass to ensure that the stress difference value between the non-equal-thickness area and the equal-thickness area is-80 MPa to-150 MPa and the stress depth difference value is-2 mu m to-6 mu m;
(4) and removing the protective film in the equal-thickness area, and then performing overall etching to remove the light shadow problem on the glass surface.
In the step (1), the toughening treatment method comprises the following steps: preheating at 400 ℃ for 30-45min at 370 ℃ and then toughening at 410 ℃ for 10-60min at 380 ℃. The stress value of the equal-thickness area and the unequal-thickness area of the non-equal-thickness glass after the toughening treatment is 500-750MPa, which is the specified stress value of the common ultrathin glass, and the depth of the stress layer is 6-12 m. The toughening process is suitable for the glass equal-thickness area, the non-equal-thickness area of the toughened non-equal-thickness glass is excessively toughened through the process, the central stress value is large, and the impact strength is low, so that the etching step of the non-equal-thickness area is carried out to remove the redundant stress value and the stress layer of the non-equal-thickness area, and the bending performance of the non-equal-thickness area is guaranteed.
In the step (1), the tempering liquid is a potassium nitrate solution with the purity of 99.99 percent; the thickness of the equal-thickness area of the unequal-thickness glass is 100-150 mu m, and the thickness of the unequal-thickness area is 30-70 mu m.
In the step (2), the protective film is resistant to acid corrosion, so that the equal-thickness area can be prevented from being etched in the process of etching the unequal-thickness area.
In the step (2), the protective film is made of polyurethane or PET, and can be soaked in mixed acid of hydrofluoric acid, sulfuric acid, phosphoric acid, ammonium sulfate, acetic acid, nitric acid and deionized water for 10-30min without acid seepage and falling off.
In the step (3), the etching conditions are as follows: the etching temperature is 25-35 deg.C, the acid etching rate is 0.5-1 μm/min, and the etching amount is 2-6 μm.
And (4) removing the protective film in the equal-thickness area by adopting a direct manual film tearing mode.
In the step (5), the conditions of the bulk etching are as follows: the etching temperature is 25-35 ℃, the acid etching rate is 0.5-1 μm/min, the etching amount is 2-4 μm, 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: 0.1-0.4% of hydrofluoric acid, 40-60% of sulfuric acid, 0.2-0.4% of phosphoric acid, 1-2% of ammonium sulfate, 1.0-20.0% of acetic acid, 2.0-10.0% of nitric acid and the balance of deionized water.
The invention also provides the ultrathin foldable non-equal-thickness toughened glass, which is obtained by toughening the non-equal-thickness glass by adopting the chemical toughening method, wherein the non-equal-thickness area of the toughened glass has higher bending performance, and the equal-thickness area of the toughened glass has higher impact and scratch resistance.
Compared with the prior art, the invention has the following advantages:
(1) according to the invention, the ultra-thin foldable non-uniform-thickness glass is only required to be toughened once, so that adverse effects on the glass caused by repeated high-temperature heating are avoided, and the toughening step is simple and convenient to operate;
(2) after the toughening treatment, the stress depth of the non-equal-thickness area is reduced through an etching process, so that the stress value of the non-equal-thickness area is reduced, the etching depth can be controlled according to the requirement in the process, the stress value of the non-equal-thickness area is controlled, and different customer requirements are met.
(3) The invention finally carries out integral etching on the non-uniform thickness glass to remove the problem of light and shadow left in the process of etching the stress layer of the non-uniform thickness area and ensure 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 in an etching mode after toughening.
(4) The method can ensure that the bending area has a smaller bending R angle and a higher bending frequency, and the non-bending area has higher impact resistance and scratch resistance.
(5) The ultrathin foldable non-equal-thickness glass treated by the method disclosed by the invention can realize inward bending and outward bending, has excellent bending performance, high impact resistance and scratch resistance, and effectively replaces the problem of wrinkling caused by excessive bending times of the existing product.
Drawings
FIG. 1 is a schematic diagram of the process of tempering ultra-thin foldable non-uniform-thickness glass in the present invention.
Detailed Description
The present invention will be described in detail with reference to examples.
The tempering liquid used in each example is a potassium nitrate solution with the concentration of 99.99 percent; 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 toughening method of ultrathin foldable non-uniform-thickness glass comprises the following steps:
(1) tempering the whole non-equal-thickness glass with the thickness of 100 mu m in the equal-thickness area and the thickness of 30 mu m in the non-equal-thickness area, wherein the stress value of the equal-thickness area and the non-equal-thickness area of the non-equal-thickness glass after the tempering treatment is 732MPa and the stress layer depth is 10.8 mu m; the toughening treatment conditions are as follows: preheating at 370 deg.C for 45min, and tempering at 380 deg.C for 50 min;
(2) covering a PET protective film on the surface of the equal-thickness area of the toughened non-equal-thickness glass;
(3) placing the non-equal-thickness glass into an etching solution for etching for 8min so as to enable the stress difference between the non-equal-thickness area and the equal-thickness area to be-140 MPa and the stress depth difference to be-4 mu m;
(4) and removing the protective film in the equal-thickness area, then putting the non-equal-thickness glass into the etching solution for etching for 6min, and etching for 3 mu m to remove the light shadow problem on the surface of the glass.
Example 2
A chemical toughening method of ultrathin foldable non-uniform-thickness glass comprises the following steps:
(1) tempering the whole non-equal-thickness glass with the thickness of 80 microns in the equal-thickness area and the thickness of 40 microns in the non-equal-thickness area, wherein the stress value of the equal-thickness area and the non-equal-thickness area of the non-equal-thickness glass after tempering is 716MPa, and the stress layer depth is 9.7 microns; the toughening treatment conditions are as follows: preheating at 370 deg.C for 45min, and then tempering at 370 deg.C for 40 min;
(2) covering a PET protective film on the surface of the equal-thickness area of the toughened non-equal-thickness glass;
(3) placing the non-equal-thickness glass into an etching solution for etching for 6min so that the stress difference between the non-equal-thickness area and the equal-thickness area is-90 MPa and the stress depth difference is-3 mu m;
(4) and removing the protective film in the equal-thickness area, then putting the non-equal-thickness glass into the etching solution for etching for 6min, and etching for 3 mu m to remove the light shadow problem on the surface of the glass.
Example 3
A chemical toughening method of ultrathin foldable non-uniform-thickness glass comprises the following steps:
(1) tempering the whole non-equal-thickness glass with the thickness of 70 mu m in the equal-thickness area and the thickness of 30 mu m in the non-equal-thickness area, wherein the stress value of the equal-thickness area and the non-equal-thickness area of the non-equal-thickness glass after tempering is 706MPa, and the stress layer depth is 9.2 mu m; the toughening treatment conditions are as follows: preheating at 370 deg.C for 45min, and tempering at 380 deg.C for 35 min;
(2) covering a PET protective film on the surface of the equal-thickness area of the toughened non-equal-thickness glass;
(3) placing the non-equal-thickness glass into an etching solution for etching for 4min so as to enable the stress difference between the non-equal-thickness area and the equal-thickness area to be-85 MPa and the stress depth difference to be-2 mu m;
(4) and removing the protective film in the equal-thickness area, then putting the non-equal-thickness glass into the etching solution for etching for 6min, and etching for 3 mu m to remove the light shadow problem on the surface of the glass.
The properties of the non-uniform thickness glass after the tempering treatment in the step (1) and the etching treatment in the step (4) in each example are shown in table 1.
TABLE 1
As can be seen from the table, the non-uniform thickness area of the ultrathin foldable non-uniform thickness glass treated by the method has a bending area with a smaller bending R angle and a higher bending frequency, and the uniform thickness area has higher impact and scratch resistance.
If the non-equal-thickness glass with the equal-thickness area thickness of 70-100 and the non-equal-thickness area thickness of 30-40 is toughened according to the toughening process of the non-equal-thickness area, namely the toughening condition is 380-400 ℃, the toughening time is 20-60min, and the pen falling impact strength (cm) of the equal-thickness area and the non-equal-thickness area of the non-equal-thickness glass after toughening is respectively 30-40 and 10-15; the pencil hardness (H) equal-thickness area and the non-equal-thickness area are respectively 6-7 and 1-2; the bending R angle (mm) is R1.5-R3, and the bending times is less than 50K; it can be seen that the equal-thickness zone has poorer impact resistance and scratch resistance than the tempered zone in the examples.
The above detailed description of the method for chemically tempering ultra-thin foldable non-equal thickness glass and the ultra-thin foldable non-equal thickness tempered glass with reference to the embodiments is illustrative and not restrictive, and several embodiments may be cited within the scope defined thereby, and thus, variations and modifications may be made without departing from the general concept of the present invention and within the scope of the present invention.
Claims (10)
1. A chemical toughening method of ultrathin foldable non-uniform-thickness glass is characterized by comprising the following steps:
(1) carrying out tempering treatment on the non-equal-thickness glass integrally according to the tempering process of the equal-thickness area;
(2) covering a protective film on the surface of the equal-thickness area of the toughened non-equal-thickness glass;
(3) etching the non-equal-thickness area of the toughened non-equal-thickness glass to ensure that the stress difference value between the non-equal-thickness area and the equal-thickness area is-80 MPa to-150 MPa and the stress depth difference value is-2 mu m to-6 mu m;
(4) and removing the protective film in the equal-thickness area, and then performing overall etching to remove the light shadow problem on the glass surface.
2. The chemical tempering method of ultra-thin foldable non-uniform thickness glass according to claim 1, wherein in the step (1), the tempering method is: preheating at 400 ℃ for 30-45min at 370 ℃ and then toughening at 410 ℃ for 10-60min at 380 ℃.
3. The chemical tempering method of ultra-thin foldable non-uniform thickness glass according to claim 1 or 2, wherein in the step (1), said tempering liquid is potassium nitrate solution with purity of 99.99%.
4. The chemical tempering method for ultra-thin foldable non-uniform thickness glass according to claim 1 or 2, wherein in the step (1), the thickness of the non-uniform thickness glass equal thickness area is 100-150 μm, and the thickness of the non-uniform thickness area is 30-70 μm.
5. The chemical tempering method for ultra-thin foldable non-uniform thickness glass according to claim 1 or 2, wherein in the step (1), the stress value of the uniform thickness region and the non-uniform thickness region of the non-uniform thickness glass after the tempering treatment is 500-750MPa, and the depth of the stress layer is 6-12 μm.
6. The method for chemically tempering ultra-thin foldable non-uniform thickness glass according to claim 1, wherein in the step (2), said protective film is a protective film resistant to acid corrosion.
7. The method for chemically tempering ultra-thin foldable non-uniform thickness glass according to claim 1, 2 or 5, wherein in the step (2), said protection film is polyurethane protection film or PET protection film.
8. The chemical tempering method of ultra-thin foldable non-uniform thickness glass according to claim 1, wherein in the step (3), the etching condition is: the etching temperature is 25-35 deg.C, the acid etching rate is 0.5-1 μm/min, and the etching amount is 2-6 μm.
9. The method for chemical tempering of ultra-thin foldable non-uniform thickness glass according to claim 1, wherein in step (5), said global etching condition is: the etching temperature is 25-35 ℃, the acid etching rate is 0.5-1 μm/min, and the etching amount is 2-4 μm.
10. An ultrathin foldable non-uniform-thickness tempered glass, which is characterized by being obtained by tempering the non-uniform-thickness glass by using the chemical tempering method of any one of claims 1 to 9.
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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 |
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