CN115448586A - Foldable glass and preparation method thereof - Google Patents
Foldable glass and preparation method thereof Download PDFInfo
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- CN115448586A CN115448586A CN202211327977.5A CN202211327977A CN115448586A CN 115448586 A CN115448586 A CN 115448586A CN 202211327977 A CN202211327977 A CN 202211327977A CN 115448586 A CN115448586 A CN 115448586A
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- Prior art keywords
- glass
- etching
- bending
- foldable
- hole
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B33/00—Severing cooled glass
- C03B33/02—Cutting or splitting sheet glass or ribbons; Apparatus or machines therefor
- C03B33/0222—Scoring using a focussed radiation beam, e.g. laser
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B33/00—Severing cooled glass
- C03B33/02—Cutting or splitting sheet glass or ribbons; Apparatus or machines therefor
- C03B33/04—Cutting or splitting in curves, especially for making spectacle lenses
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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
- 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
Abstract
The invention discloses foldable glass and a preparation method thereof, wherein the preparation method comprises the following steps: punching a target bending area of the glass, and then carrying out chemical etching, toughening treatment and surface etching treatment; the preparation method can process the glass with the thickness of 100-500 mu m into the foldable glass, and the bending times of the foldable glass prepared by the method can reach more than 20w times under the condition of high impact resistance.
Description
Technical Field
The invention belongs to the technical field of foldable glass, particularly relates to foldable glass and a preparation method thereof, and particularly relates to a preparation method of foldable glass with the thickness of more than or equal to 100 mu m.
Background
With the rapid development of flexible display technology and the upgrading of electronic products, foldable, stretchable and rollable flexible display products gradually enter the field of view of consumers. However, in the trend of the flexible display products toward being lighter, thinner and more portable, the demand for the lighter, thinner outer cover plate is also higher. However, when the cover plate of the flexible display folding product is made of Ultra-Thin Glass (UTG) with a thickness thinner than 100 μm, the Glass has a flexible bending capability, but the Glass has a low thickness, which causes poor impact resistance against the outside, and reduces reliability and stability of the product.
Conventional flexible ultra-thin glass cover plates, in which the thickness of the glass is controlled to 30-70 μm as required for the foldability, result in that the impact strength and scratch resistance of the glass cover plate become poor as the plate thickness is reduced. Because the thickness of ultra-thin glass (UTG) is directly proportional to its impact resistance and inversely proportional to its ultimate bending capability.
In the prior art, the high impact resistance and excellent scratch resistance of UTG cannot be guaranteed, and the bending capability of UTG can be considered, namely the target bending radius and the target bending times cannot be achieved. When UTG is compatible with the bending capability, UTG is inferior in impact resistance (ball/pen drop) as the thickness of the plate becomes smaller, which increases the risk of process chipping and lowers the production yield.
Disclosure of Invention
In order to solve the technical problems, the invention provides foldable glass and a preparation method thereof, the preparation method can process the glass with the thickness of 100-500 mu m into the foldable glass, and the bending times of the foldable glass prepared in the way can reach more than 20w times under the condition of high impact resistance.
The technical scheme adopted by the invention is as follows:
a method of making foldable glass, the method comprising the steps of:
(1) Punching a target bending area of the glass;
(2) Chemically etching the glass treated in the step (1);
(3) Tempering the glass treated in the step (2);
(4) And (4) performing surface etching on the glass treated in the step (3).
In the step (1), the thickness of the glass is 100-500 μm, so that the glass with the thickness is ultrathin compared with the glass with the thickness of 30-70 μm, and has higher strength, high impact resistance and excellent scratch resistance.
In the step (1), the target bending area of the glass is more than one, so that foldable glass with different bending forms can be prepared. The width of the target bending area is 20-40mm.
In the step (1), during punching, the punched holes are distributed in the target bending area of the glass in an array arrangement mode, so that the stress generated by the glass during bending can be effectively released.
Furthermore, the holes are distributed in the target bending area of the glass in an array arrangement mode in a staggered mode, so that stress generated by the glass during bending can be uniformly and effectively released.
Furthermore, the shape and the size of each hole are completely the same, so that the uniformity of the stress distribution of the glass in the bending area can be ensured.
The shape of each hole is a waist hole, and each waist hole is arranged perpendicular to the bending direction of the glass; the strength of the bent area glass in the bending direction is weaker than that of the non-bending direction due to the arrangement of the waist holes, so that the bent area glass can be kept to have higher strength in the non-bending direction under the condition of ensuring good bending performance of the glass.
Furthermore, the width of the waist hole is 50-200 μm, the length-width ratio is 20-100, the distance between the upper hole and the lower hole is 100-300 μm, and the distance between the left hole and the right hole is 300-500 μm.
In the step (1), because the glass which is not subjected to strengthening treatment is brittle and fragile, the aperture size of the holes to be punched is small, and the distance between the holes is extremely small, the bending area of the glass is cut and punched by adopting an infrared picosecond-level laser cutting machine, the laser power is 5-50w, and the wavelength is 1000-1500, so that the glass cannot be broken during punching.
In the step (2), during chemical etching treatment, the acid etching rate is controlled to be 1-4 μm/min, the etching time is 500-3000s, and the etching time is specifically determined according to the target plate thickness; in the process, the cutting waste materials remained in the holes can be completely peeled off, and the thinning of different thicknesses of the glass can be realized by controlling the etching time.
In the step (2), ultrasonic treatment is carried out while etching is carried out, and a chamfering process is adopted in the process of etching to half of the target plate thickness, so that the uniformity of the plate thickness is ensured, the uniformity of the concentration of etching acid liquid and the uniform falling of cutting waste materials in the etching process are ensured, and the accumulation of reactants after etching is effectively prevented.
In the step (2), the etching solution used for the chemical etching comprises the following components 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.
In the step (3), the toughening treatment conditions are as follows: preheating for 30-60min at 370-400 deg.c, and tempering at 380-410 deg.c for 30-90min to control the stress value of the tempered glass in the non-bending area to 500-900MPa and the stress layer depth to 8-16 micron.
In the step (3), the toughening liquid used in the toughening treatment is a potassium nitrate solution with the mass fraction of 99.99%.
In the step (4), the surface etching amount is controlled to be 4-8 μm, the etching rate is 0.5-0.8 μm/min, and the surface roughness of the foldable glass after the surface etching process is 0.2-0.40 μm.
In the step (4), the etching solution used for surface etching comprises the following components 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.
Further, before the step (1), the method also comprises a step of carrying out laser cutting on the glass, wherein the glass is cut into the size and the shape required by a use scene; the laser cutting adopts an infrared picosecond level laser cutting machine, the laser power is between 5 and 50w, the wavelength is between 1000 and 1500, the picosecond level laser cutting mode can effectively control the edge breakage of the glass to be less than 10 micrometers, and the picosecond level laser cutting machine has the processing capacity for special-shaped glass, and meanwhile, the laser cutting is not limited by the material and the size of a sample.
Further, the steps (1) and (4) are followed by a step of ultrasonic cleaning.
And (3) after the step (2), sequentially carrying out ultrasonic cleaning and slow drawing treatment to remove residual water drops on the surface of the glass, wherein the slow drawing speed is 30 s/time, and finally carrying out a baking step at the temperature of 60-80 ℃.
The invention also provides the foldable glass prepared by the preparation method, and the bending times of the foldable glass can reach more than 20w times under the condition of high impact resistance.
Compared with the prior art, the invention has the following advantages:
1. the preparation method provided by the invention can realize that the foldable glass is prepared from the glass with the thickness of 100-500 mu m, the thickness of the foldable glass can be controlled by controlling the time of chemical etching, the external dimension of the target foldable glass to be prepared is not limited, the foldable glass can be used as cover plate glass for various foldable display devices such as folding mobile phones, folding notebook computers and the like, and the problems of CPI crease and low strength of UTG can be effectively solved by using the rigidity of the glass;
2. according to the invention, the hole patterns of the glass bending area are cut by laser, etching waste materials in the holes are removed in a chemical etching mode, the bending performance and the impact strength of the glass are ensured by toughening treatment, and finally surface micro-cracks are removed by surface etching to improve the strength of the glass, so that the steps are simple and convenient to operate, and the industrial batch production of the foldable glass can be realized;
3. the bent glass prepared by the preparation method provided by the invention can realize inward bending and outward bending of the glass at the same time, and the bending direction of the glass is not limited;
4. the preparation method provided by the invention can realize polymorphic bending of the glass according to the bending requirement of the glass, and effectively solves the problems of crease and low strength of UTG which replace a CPI material;
5. the foldable glass provided by the invention not only has high impact resistance, but also has higher process yield and lower production cost and is more beneficial to commercialization because the thickness of the glass adopted in the processing process is more than or equal to 100 mu m.
Drawings
FIG. 1 is a flow chart of a process for manufacturing foldable glass in accordance with the present invention;
FIG. 2 is a schematic view of the spacing between the holes in the bending region of the foldable glass in accordance with the present invention;
FIG. 3 is a plot of a bend region array of holes in a foldable glass of the present invention.
Detailed Description
The present invention will be described in detail with reference to examples.
Examples
A method of making foldable glass comprising the steps of: glass laser cutting, laser hole digging, ultrasonic cleaning, chemical etching, ultrasonic cleaning, chemical tempering and surface etching optimization;
the glass laser cutting adopts a picosecond infrared laser machine cutting machine to cut original glass with the thickness of 100-500 mu m into a shape required by a use scene, the laser power is 5-50w, the wavelength is 1000-1500, the cutting power is different according to the glass material and the plate thickness, the picosecond laser cutting mode can effectively control the edge breakage of the glass to be less than 10 mu m, and has the processing capacity (including an R angle) for special-shaped glass, and meanwhile, the laser cutting is not limited by the material and the size of a sample.
And the laser hole digging is also carried out by adopting a picosecond infrared laser machine cutting machine. The holes are distributed in the bending area of the glass in a staggered mode in an array mode, so that stress generated by the glass during bending can be uniformly and effectively released.
The shape and the size of each hole are completely the same, so that the uniformity of the stress distribution of the glass in the bending area can be ensured.
The shape of each hole is a waist hole, and each waist hole is arranged perpendicular to the bending direction of the glass; the strength of the bent area glass in the bending direction is weaker than that of the non-bending direction due to the arrangement of the waist holes, so that the bent area glass can be kept to have higher strength in the non-bending direction under the condition of ensuring good bending performance of the glass.
The width of the waist hole is 50-200 μm, the length-width ratio is 20-100, the distance between the upper hole and the lower hole is 100-300 μm, and the distance between the left hole and the right hole is 300-500 μm.
When the size of the foldable glass product is set to be 8 inches, the length L of the cutting pattern of the bending area is 4000-5000 microns, the width d of the hole is 50-200 microns, the vertical distance a between the two holes is 100-300 microns, and the horizontal distance b is 300-500 microns, as shown in FIG. 2.
And ultrasonically cleaning the cut glass so as to remove glass powder generated in the cutting process and prevent the residual glass powder in the next etching process from reacting with hydrofluoric acid to generate fluosilicic acid, so that the fluosilicic acid is accumulated in the pores to influence etching.
The glass cleaned by ultrasonic is etched, the acid etching rate of the etching treatment is controlled to be 1-4 mu m/min, an ultrasonic foaming device is arranged in an etching tank body to ensure the uniformity of the concentration of etching acid liquor and the uniform falling of cutting waste materials in a pattern area in the etching process, and a beveling process is adopted in the etching process to effectively prevent reactants from being accumulated after etching. After the etching process is finished, all glass in the aperture of the sample punched in the bending area falls off and is peeled off, and the bending area forms staggered array stepped waist holes.
The etching solution used for chemical etching comprises the following components 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.
Performing performance strengthening process treatment on the chemically etched glass, performing ultrasonic cleaning and slow-pulling baking at 60-80 ℃, and performing chemical toughening on the foldable glass, wherein the chemical toughening principle is as follows: the sodium-potassium ion exchange process can be carried out in the glass under the high-temperature condition, and the surface strength and the flexibility of the glass are improved by utilizing the extrusion effect generated by the volume difference of the sodium-potassium ion exchange process and the glass; and (3) chemical toughening process: and (2) putting the chemically etched glass into a preheating furnace for heating, wherein the preheating temperature is 370-400 ℃, the preheating time is 30-60min, after the preheating is finished, putting the glass into a chemical tempering tank, the temperature of molten salt liquid in the tempering tank is 380-410 ℃, the temperature of the molten salt liquid is close to that of the preheating furnace, the tempering time is set to be 30-90mi, the stress value range of the tempered glass is controlled to be 500-900MPa, and the depth of a stress layer is 8-16 mu m.
The tempering liquid used for the tempering treatment is a potassium nitrate solution with the mass fraction of 99.99%.
Performing surface etching treatment on the toughened glass, and mainly aiming at repairing the problems of microcracks generated in the processing procedure of the glass, amplified defects after the toughening process and the like; in the surface etching process, the surface etching amount of the foldable glass is controlled to be 4-8 mu m, the etching rate is 0.5-0.8 mu m/min, the surface roughness of the flexible foldable glass after the surface etching process is 0.2-0.40 mu m, the surface strength of the glass is improved, finally, the finished product is cleaned and dried by ultrasonic cleaning to obtain the finished product, and the appearance of the array holes in the bending area of the finished product is shown in figure 3.
The etching solution used for surface etching comprises the following components 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 impact performance and the bending performance of the foldable glass prepared by the preparation method are tested, and the test process is as follows:
and (3) impact performance test: sequentially attaching OCA optical cement and a PET film to the upper surface and the lower surface of a hole digging sample to be detected respectively to form an attaching structure, and placing a marble at the lower end of the attaching structure, wherein the layer structure of the attaching structure from top to bottom is respectively PET-OCA-sample-OCA-PET-marble. And (3) freely falling at different heights by using a morning light pen with the pen point diameter of 0.5mm and the weight of 12-13g, falling in the jointed test sample, and observing that the appearance of the non-bending area of the y sample is crack-free and judging OK, wherein at the moment, the distance between the pen point and the jointed structure is a physical quantity for representing the pen-falling impact strength of the sample, and the larger the distance is, the stronger the impact resistance of the sample is. The falling impact strength of the non-bending area of the foldable glass prepared by the preparation method is measured to be 120-200cm.
And (3) bending performance test: the UTG sample is pasted on a U-shaped dynamic bending machine jig by using an adhesive tape, the bending speed is set for 2s for one cycle, the bending radius is 1-5 mm, the sample is bent for 20w times at room temperature, appearance defects such as cracks and creases are not determined to be OK after bending, the corresponding bending radius and bending frequency are physical quantities representing the bending performance of the sample, the smaller the bending radius is, the more the bending frequency is, the stronger the bending performance of the sample is, the bending radius of the bending area of the foldable glass prepared by the preparation method is 1-2mm, and the bending frequency is 200k times without fracture.
Compared with ultrathin glass with the thickness less than 100 mu m, the foldable glass prepared by the preparation method disclosed by the invention not only has high impact resistance, but also has higher process yield and lower production cost and is more favorable for commercialization because the thickness of the glass adopted in the processing process is more than or equal to 100 mu m. Secondly, the foldable glass cover plate provided by the invention can realize inward bending and outward bending of glass at the same time, and the bending direction of the glass is not limited. The treatment can be simultaneously carried out at a plurality of positions according to the bending requirement of the glass, so that the treated glass has a polymorphic bending effect, and the problems of crease and UTG with too low strength of a CPI material are effectively solved.
The above detailed description of a foldable glass and its method of manufacture with reference to the examples is illustrative and not restrictive, and several examples are set forth with the limits of the invention, so that variations and modifications may be made without departing from the general inventive concept and scope thereof.
Claims (10)
1. A method of making foldable glass, comprising the steps of:
(1) Punching a target bending area of the glass;
(2) Chemically etching the glass treated in the step (1);
(3) Tempering the glass treated in the step (2);
(4) And (4) performing surface etching on the glass treated in the step (3).
2. The production method according to claim 1, wherein in the step (1), the glass has a thickness of 100 to 500 μm; during punching, the punched holes are distributed in the target bending area of the glass in an array arrangement mode.
3. The method of claim 2, wherein the holes are staggered in an array in the intended bending area of the glass.
4. The method according to claim 2 or 3, wherein the shape and size of each hole are identical.
5. The production method according to claim 1 or 2, wherein each hole is shaped as a waist hole, and each waist hole is arranged perpendicularly to a direction in which the glass is bent.
6. The manufacturing method according to any one of claims 1 to 3, wherein in the step (1), a picosecond laser cutting machine is used for cutting and punching the bending region of the glass.
7. The production method according to any one of claims 1 to 3, wherein in the step (2), the acid etching rate is controlled to 1 to 4 μm/min during the chemical etching treatment; ultrasonic treatment is carried out while etching, and chamfering is carried out in the process of etching to half of the target plate thickness.
8. The production method according to any one of claims 1 to 3, wherein in the step (3), the tempering treatment conditions are: preheating for 30-60min at 370-400 ℃, and then toughening for 30-90min at 380-410 ℃.
9. The manufacturing method according to any one of claims 1 to 3, wherein in the step (4), the surface etching amount is controlled to be 4 to 8 μm, the etching rate is 0.5 to 0.8 μm/min, and the surface roughness of the flexible foldable glass after the surface etching process is 0.2 to 0.40 μm.
10. Foldable glass produced according to the production method of any one of claims 1 to 9.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211327977.5A CN115448586A (en) | 2022-10-27 | 2022-10-27 | Foldable glass and preparation method thereof |
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| CN202211327977.5A CN115448586A (en) | 2022-10-27 | 2022-10-27 | Foldable glass and preparation method thereof |
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| WO2015093356A1 (en) * | 2013-12-17 | 2015-06-25 | 株式会社村田製作所 | Method for manufacturing piezoelectric sensor |
| CN107241904A (en) * | 2013-12-17 | 2017-10-10 | 康宁股份有限公司 | The 3D shapings of glass |
| CN109843819A (en) * | 2016-09-08 | 2019-06-04 | 康宁股份有限公司 | The product and its manufacturing method in the hole with tool morphological properties |
| CN112264725A (en) * | 2020-10-30 | 2021-01-26 | 深圳市青虹激光科技有限公司 | Method for processing embossed glass hole |
| CN114671624A (en) * | 2022-05-09 | 2022-06-28 | 芜湖东信光电科技有限公司 | Treatment process of flexible glass with high impact resistance |
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2022
- 2022-10-27 CN CN202211327977.5A patent/CN115448586A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015093356A1 (en) * | 2013-12-17 | 2015-06-25 | 株式会社村田製作所 | Method for manufacturing piezoelectric sensor |
| CN107241904A (en) * | 2013-12-17 | 2017-10-10 | 康宁股份有限公司 | The 3D shapings of glass |
| CN109843819A (en) * | 2016-09-08 | 2019-06-04 | 康宁股份有限公司 | The product and its manufacturing method in the hole with tool morphological properties |
| CN112264725A (en) * | 2020-10-30 | 2021-01-26 | 深圳市青虹激光科技有限公司 | Method for processing embossed glass hole |
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