CN114262163A - Chemical strengthening method for inhibiting microcracks on surface of flexible glass - Google Patents
Chemical strengthening method for inhibiting microcracks on surface of flexible glass Download PDFInfo
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- CN114262163A CN114262163A CN202111651042.8A CN202111651042A CN114262163A CN 114262163 A CN114262163 A CN 114262163A CN 202111651042 A CN202111651042 A CN 202111651042A CN 114262163 A CN114262163 A CN 114262163A
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Abstract
The invention provides a chemical strengthening method for inhibiting microcracks on the surface of flexible glass, which is characterized by comprising the following steps of: (a) preparing a film material; (b) preparing a film on flexible glass; (c) chemical strengthening of flexible glass. The method provided by the invention can effectively inhibit the generation and the diffusion of the surface cracks of the glass, improve the chemical strengthening efficiency and improve the strength of the glass.
Description
The technical field is as follows:
the invention relates to the field of glass strengthening, in particular to a chemical strengthening method for inhibiting microcracks on the surface of flexible glass.
Background art:
with the development of electronic display products towards light weight, thin thickness and special shape, glass materials are also correspondingly changed, and flexible glass appears, wherein the glass is flat glass with the thickness of less than 100 mu m and good flexibility. The flexible glass has good flexibility, and still maintains the inherent characteristics of high hardness, high transparency, high thermal stability, chemical resistance and the like of the glass, so the flexible glass plays an important role in the fields of displays, touch sensors, flexible photovoltaic products, illumination and the like.
As glass becomes thinner, internal and surface defects of the glass are magnified. The cutting method of the flexible glass is most commonly mechanical cutting and laser cutting, but in the cutting process, the surface and the edge of the glass are easy to generate micro cracks, which greatly reduces the strength of the glass and prevents the glass from being bent, and the micro cracks are broken under the action of stress in a high-temperature environment in the chemical strengthening process. And because the glass is too thin, the micro-cracks are difficult to remove by adopting a mechanical polishing or chemical method, so that the glass is easy to crack in the whole production and processing process and hidden troubles are caused to the safety performance of the product. This directly causes the mechanical performance indexes of the flexible glass, such as breaking strength, surface hardness, etc., to be obviously reduced, which brings great difficulty to the application of the flexible glass.
There is therefore a need in the art for a method by which microcracks on the surface or edges of glass can be protected from cracking during chemical strengthening, while further repairing the microcracks and increasing the strength of the glass.
The invention content is as follows:
the invention aims to overcome the defects in the prior art and provides a chemical strengthening method for inhibiting microcracks on the surface of flexible glass.
The application provides the following technical scheme:
a chemical strengthening method for inhibiting microcracks on the surface of flexible glass is characterized by comprising the following steps: (a) the preparation of the film material comprises (a 1) the preparation of a base material and (a 2) the mixing of the base material and nano-scale silicon dioxide, (a 1) stage, the weighed aluminum powder is dispersed in N, N-dimethylformamide, polydimethylsiloxane or imide is added, the mixture is placed in a reaction kettle and reacts for 24 hours at the temperature of 100 ℃, and the base material is obtained after cooling, filtering and vacuum drying; (a2) mixing the base material, the dispersing agent and the nano-scale silicon dioxide to obtain a mixed transparent film material, and sealing for later use;
(b) preparing at least one layer of film on flexible glass: uniformly coating a film material on the surface of the flexible glass, solidifying the surface of the film material to form a transparent film by adopting laser evaporation, placing the coated flexible glass in an oven, and drying to remove a dispersion medium;
(c) and (3) chemically strengthening the flexible glass, namely immersing the flexible glass after the step (b) in high-temperature molten salt for a period of time to obtain the chemically strengthened flexible glass with the surface coated with the film, wherein the high-temperature molten salt is composed of potassium nitrate and additives.
On the basis of the technical scheme, the following further technical scheme can be provided:
the additive in step (c) is composed of one or more of metasilicic acid, diatomaceous earth and silica.
The flexible glass in the step (b) is prepared from the following raw materials in percentage by mass: 60.5% SiO217.5% of Al2O312.5% of Na2O, 5.5% of K2O, 3.5% of MgO and 0.5% of ZrO2。
The particle size of the nano-scale silicon dioxide in the step (a) is 10-80 nm.
The rotation speed of the mixing in the step (a) is 700 to 1100 rmp.
In step (b) 1-3 layers of film are prepared on flexible glass.
In the step (b), the thickness of the flexible glass is 0.03-0.1 mm.
In the step (b), the laser wavelength is 360nm and the laser power is 1000W during laser evaporation.
In the step (b), the thickness of the film is 0.04-0.1 mm.
In the step (c), the temperature of the high-temperature molten salt is 380-400 ℃, and the soaking time is 5-15 min.
The invention has the advantages that:
the invention utilizes the chemical strengthening process to enhance the adhesive force between the film and the glass and effectively inhibit the generation and the diffusion of cracks on the surface of the glass; releasing nano SiO2Entering the glass to fill the crack gap and promote the chemical exchange of sodium ions and potassium ions; the additive in the high-temperature mixed molten salt has the functions of removing impurities, protecting and repairing microcracks, further inhibits the generation of microcracks on the surface of the glass in the chemical strengthening process, effectively inhibits the generation and the diffusion of the cracks on the surface of the glass, improves the chemical strengthening efficiency and improves the strength of the glass.
In addition, aluminum powder of an inorganic material is dispersed in organic N, N-dimethylformamide in the film, so that the inorganic material is used as a center, the organic material is used as a ligand, and the coordination and the extension are continuously carried out, so that a porous frame structure is formed, and the strength and the adhesive force of the film are effectively ensured.
The specific implementation mode is as follows:
example 1:
a chemical strengthening method for inhibiting microcracks on the surface of flexible glass is characterized by comprising the following steps: the preparation of the a film material comprises the steps of preparing an a1 base material and mixing an a2 base material with nano-scale silicon dioxide, in the stage a1, weighing 0.5mol of aluminum powder, dispersing the aluminum powder in 500ml of N, N-dimethylformamide, adding 1mol of polydimethylsiloxane, placing the mixture in a reaction kettle, reacting for 24 hours at 100 ℃, cooling, filtering, and drying in vacuum to prepare the base material.
and a2, mixing the base material, the dispersing agent and the nano-scale silicon dioxide at the mixing speed of 700 rmp to obtain a fully mixed transparent film material, and sealing for later use. The particle size of the silicon dioxide is 60 nm.
b preparing a film on flexible glass: the film material is uniformly coated on the surface of the flexible glass, the laser wavelength is 360nm by adopting laser evaporation, the laser power is 1000W, so that the surface of the film material is cured to form a transparent film layer, the thickness of the film is 0.04mm, and then the film-coated flexible glass is placed in an oven and dried, so that the dispersion medium is removed. The flexible glass is prepared from the following raw materials in percentage by mass: 60.5% SiO217.5% of Al2O312.5% of Na2O, 5.5% of K2O, 3.5% of MgO and 0.5% of ZrO2. The thickness of the flexible glass is 0.07 mm.
c, chemically strengthening the flexible glass, namely soaking the flexible glass subjected to the step b into high-temperature KNO3In the solution for 5min, the temperature of the solution is 380 ℃, thus obtaining the chemically strengthened flexible glass with a surface coating, and the KNO3Metasilicic acid and diatomite are also added into the solution as additives.
Example 2:
a chemical strengthening method for inhibiting microcracks on the surface of flexible glass is characterized by comprising the following steps: the preparation of the a film material comprises the steps of preparing an a1 base material and mixing an a2 base material with nano-scale silicon dioxide, in the stage a1, weighing 0.5mol of aluminum powder, dispersing the aluminum powder in 500ml of N, N-dimethylformamide, adding 1mol of polydimethylsiloxane, placing the mixture in a reaction kettle, reacting for 24 hours at 100 ℃, cooling, filtering, and drying in vacuum to prepare the base material.
and a2, mixing the base material, the dispersing agent and the nano-scale silicon dioxide at the rotating speed of 900 rmp to obtain a fully mixed transparent film material, and sealing for later use. The particle size of the silicon dioxide is 50 nm.
b preparing a film on flexible glass: the film material is uniformly coated on the surface of the flexible glass, the laser wavelength is 360nm by adopting laser evaporation, the laser power is 1000W, so that the surface of the film material is solidified to form a transparent film layer, then the steps are repeated to sequentially prepare a second film layer on the film, and then the coated flexible glass is placed in an oven and dried, so that the dispersion medium is removed. The thickness of the first layer of film is 0.04mm, and the thickness of the second layer of film is 0.04 mm.
The flexible glass is prepared from the following raw materials in percentage by mass: 60.5% SiO217.5% of Al2O312.5% of Na2O, 5.5% of K2O, 3.5% of MgO and 0.5% of ZrO2. The thickness of the flexible glass is 0.03 mm.
c, chemically strengthening the flexible glass, namely soaking the flexible glass subjected to the step b into high-temperature KNO3In the solution for 10min, the temperature of the solution is 390 ℃, thereby obtaining the chemically strengthened flexible glass with a surface coating, and the KNO3Metasilicic acid and diatomite are also added into the solution as additives.
Example 3:
a chemical strengthening method for inhibiting microcracks on the surface of flexible glass is characterized by comprising the following steps: the preparation of the a film material comprises the steps of preparing an a1 base material and mixing an a2 base material with nano-scale silicon dioxide, in the stage a1, weighing 0.5mol of aluminum powder, dispersing the aluminum powder in 500ml of N, N-dimethylformamide, adding 1mol of polydimethylsiloxane, placing the mixture in a reaction kettle, reacting for 24 hours at 100 ℃, cooling, filtering, and drying in vacuum to prepare the base material.
and a2, mixing the base material, the dispersing agent and the nano-scale silicon dioxide at the rotating speed of 1100rmp to obtain a fully mixed transparent film material, and sealing for later use. The particle size of the silicon dioxide is 70 nm.
b preparing a film on flexible glass: uniformly coating a film material on the surface of the flexible glass, solidifying the surface of the film material to form a transparent film by adopting laser evaporation with the laser wavelength of 360nm and the laser power of 1000W, then repeating the steps to sequentially prepare a second film and a third film on the film, then placing the coated flexible glass in a baking oven, and drying to remove the dispersion medium. The thickness of the first layer of film is 0.04mm, the thickness of the second layer of film is 0.05mm, and the thickness of the third layer of film is 0.04 mm.
The flexible glass is prepared from the following raw materials in percentage by mass: 60.5% SiO217.5% of Al2O312.5% of Na2O, 5.5% of K2O, 3.5% of MgO and 0.5% of ZrO2. The thickness of the flexible glass is 0.05 mm.
c, chemically strengthening the flexible glass, namely soaking the flexible glass subjected to the step b into high-temperature KNO3In the solution for 15min, the temperature of the solution is 400 ℃, thus obtaining the chemically strengthened flexible glass with a surface coating, and the KNO3Diatomite and silicon dioxide are also added into the solution as additives.
Example 4:
a chemical strengthening method for inhibiting microcracks on the surface of flexible glass is characterized by comprising the following steps: the preparation of the a film material comprises the steps of preparing an a1 base material and mixing an a2 base material with nano-scale silicon dioxide, in the stage a1, weighing 0.5mol of aluminum powder, dispersing the aluminum powder in 500ml of N, N-dimethylformamide, adding 1mol of polydimethylsiloxane, placing the mixture in a reaction kettle, reacting for 24 hours at 100 ℃, cooling, filtering, and drying in vacuum to prepare the base material.
and a2, mixing the base material, the dispersing agent and the nano-scale silicon dioxide at the rotating speed of 900 rmp to obtain a fully mixed transparent film material, and sealing for later use. The particle size of the silicon dioxide is 65 nm.
b preparing a film on flexible glass: uniformly coating a film material on the surface of the flexible glass, solidifying the surface of the film material to form a transparent film by adopting laser evaporation with the laser wavelength of 360nm and the laser power of 1000W, then repeating the steps to sequentially prepare a second film and a third film on the film, then placing the coated flexible glass in a baking oven, and drying to remove the dispersion medium. The thickness of the first layer of film is 0.05mm, the thickness of the second layer of film is 0.05mm, and the thickness of the third layer of film is 0.06 mm.
The flexible glass is prepared from the following raw materials in percentage by mass: 60.5% SiO217.5% of Al2O312.5% of Na2O, 5.5% of K2O, 3.5% of MgO and 0.5% of ZrO2. The thickness of the flexible glass is 0.05 mm.
c, chemically strengthening the flexible glass, namely soaking the flexible glass subjected to the step b into high-temperature KNO3In the solution for 10min, the temperature of the solution is 390 ℃, thereby obtaining the chemically strengthened flexible glass with a surface coating, and the KNO3Metasilicic acid, diatomite and silicon dioxide are also added into the solution as additives.
Example 5:
a chemical strengthening method for inhibiting microcracks on the surface of flexible glass is characterized by comprising the following steps: the preparation of the a film material comprises the steps of preparing an a1 base material and mixing an a2 base material with nano-scale silicon dioxide, in the stage a1, weighing 0.5mol of aluminum powder, dispersing the aluminum powder in 500ml of N, N-dimethylformamide, adding 1mol of polydimethylsiloxane, placing the mixture in a reaction kettle, reacting for 24 hours at 100 ℃, cooling, filtering, and drying in vacuum to prepare the base material.
and a2, mixing the base material, the dispersing agent and the nano-scale silicon dioxide at the rotating speed of 900 rmp to obtain a fully mixed transparent film material, and sealing for later use. The particle size of the silicon dioxide is 75 nm.
b preparing a film on flexible glass: uniformly coating a film material on the surface of the flexible glass, solidifying the surface of the film material to form a transparent film by adopting laser evaporation with the laser wavelength of 360nm and the laser power of 1000W, then repeating the steps to sequentially prepare a second film and a third film on the film, then placing the coated flexible glass in a baking oven, and drying to remove the dispersion medium. The thickness of the first layer of film is 0.04mm, the thickness of the second layer of film is 0.04mm, and the thickness of the third layer of film is 0.04 mm.
The flexible glass is prepared from the following raw materials in percentage by mass: 60.5% SiO217.5% of Al2O312.5% of Na2O, 5.5% of K2O, 3.5% of MgO and 0.5% of ZrO2. The thickness of the flexible glass is 0.05 mm.
c, chemically strengthening the flexible glass, namely soaking the flexible glass subjected to the step b into high-temperature KNO3In the solution for 10min, the temperature of the solution is 400 ℃, thereby obtaining the chemically strengthened flexible glass with a surface coating, and the KNO3Metasilicic acid, diatomite and silicon dioxide are also added into the solution as additives.
And (3) testing:
glass stress depth of layer and surface layer stress: according to ASTM C1422/C1422M-20 "Standard Specification for chemically tempered Flat glass", chapter 9, SLP-2000 scattered light stress Meter was used for the test. Height of pen drop: and (3) enabling a ball-point pen with a ball core diameter of 0.7 mm and a ball point of 8 +/-0.5 g to impact 9 points on the surface of the glass in a free falling mode in a vertical state, and after the impact is finished, increasing the ball point pen by 10mm each time until a crack and a damage appear at an impact test point, and recording the ball point pen falling impact height.
The performance of the flexible glass prepared by the method 1-5 is directly strengthened on the premise of no film coating, and the strengthening conditions are the same as those of the data of the comparative example obtained in the example 2 in the test, and are shown in the table 1.
TABLE 1 examples 1 to 5 float characteristic points
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example | |
| Surface compressive stress CS (MPa) | 313.37 | 318.31 | 305.77 | 317.41 | 303.67 | 317.13 |
| Depth of stress layer DOL (mum) | 18.034 | 22.832 | 23.027 | 21.987 | 21.476 | 22.535 |
| Pen drop height (mm) | 28.74 | 30.82 | 31.87 | 31.65 | 30.92 | 25.15 |
From examples 1 to 5, it can be found that the prepared flexible glass has a surface compressive stress of more than 300MPa, a DOL of 18 μm and a stroke height of more than 20mm, indicating that the prepared flexible glass has excellent performance. Among them, the surface compressive stress and the depth of stress layer of example 2 are most excellent depending on the heat treatment temperature, time and additives, and thus, it can be seen that the preferable heat treatment temperature is 390 ℃ for 10min and the additives are metasilicic acid, diatomaceous earth and silica. The pen-fall performance of the example 3 is the most excellent, and the pen-fall performance of the comparative example is the worst, which shows that the film coating effect is obvious, and the 3-layer effect is optimal.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; those skilled in the art can make numerous possible variations and modifications to the present teachings, or modify equivalent embodiments to equivalent variations, without departing from the scope of the present teachings, using the methods and techniques disclosed above. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention.
Claims (10)
1. A chemical strengthening method for inhibiting microcracks on the surface of flexible glass is characterized by comprising the following steps: (a) the preparation of the film material comprises (a 1) the preparation of a base material and (a 2) the mixing of the base material and nano-scale silicon dioxide, (a 1) stage, the weighed aluminum powder is dispersed in N, N-dimethylformamide, polydimethylsiloxane or imide is added, the mixture is placed in a reaction kettle and reacts for 24 hours at the temperature of 100 ℃, and the base material is obtained after cooling, filtering and vacuum drying; (a2) mixing the base material, the dispersing agent and the nano-scale silicon dioxide to obtain a mixed transparent film material, and sealing for later use;
(b) preparing at least one layer of film on flexible glass: uniformly coating a film material on the surface of the flexible glass, solidifying the surface of the film material to form a transparent film by adopting laser evaporation, placing the coated flexible glass in an oven, and drying to remove a dispersion medium;
(c) and (3) chemically strengthening the flexible glass, namely immersing the flexible glass after the step (b) in high-temperature molten salt for a period of time to obtain the chemically strengthened flexible glass with the surface coated with the film, wherein the high-temperature molten salt is composed of potassium nitrate and additives.
2. A method of chemically strengthening a flexible glass surface to suppress microcracks in the surface according to claim 1, wherein: the additive in step (c) is composed of one or more of metasilicic acid, diatomaceous earth and silica.
3. A method of chemically strengthening a flexible glass surface to suppress microcracks in the surface according to claim 1, wherein: the flexible glass in the step (b) is prepared from the following raw materials in percentage by mass: 60.5% SiO217.5% of Al2O312.5% of Na2O, 5.5% of K2O, 3.5% of MgO and 0.5% of ZrO2。
4. A method of chemically strengthening a flexible glass surface to suppress microcracks in the surface according to claim 1, wherein: the particle size of the nano-scale silicon dioxide in the step (a) is 10-80 nm.
5. A method of chemically strengthening a flexible glass surface to suppress microcracks in the surface according to claim 1, wherein: the rotation speed of the mixing in the step (a) is 700 to 1100 rmp.
6. A method of chemically strengthening a flexible glass surface to suppress microcracks in the surface according to claim 1, wherein: in step (b) 1-3 layers of film are prepared on flexible glass.
7. A method of chemically strengthening a flexible glass surface to suppress microcracks in the surface according to claim 1, wherein: in the step (b), the thickness of the flexible glass is 0.03-0.1 mm.
8. A method of chemically strengthening a flexible glass surface to suppress microcracks in the surface according to claim 1, wherein: in the step (b), the laser wavelength is 360nm and the laser power is 1000W during laser evaporation.
9. A method of chemically strengthening a flexible glass surface to suppress microcracks in the surface according to claim 1, wherein: in the step (b), the thickness of the film is 0.04-0.1 mm.
10. A method of chemically strengthening a flexible glass surface to suppress microcracks in the surface according to claim 1, wherein: in the step (c), the temperature of the high-temperature molten salt is 380-400 ℃, and the soaking time is 5-15 min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115818981A (en) * | 2022-12-23 | 2023-03-21 | 中建材玻璃新材料研究院集团有限公司 | Preparation method of high-strength antibacterial flexible glass |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105142900A (en) * | 2012-10-12 | 2015-12-09 | 康宁股份有限公司 | Articles with a low-elastic modulus layer and retained strength |
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- 2021-12-31 CN CN202111651042.8A patent/CN114262163A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105142900A (en) * | 2012-10-12 | 2015-12-09 | 康宁股份有限公司 | Articles with a low-elastic modulus layer and retained strength |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115818981A (en) * | 2022-12-23 | 2023-03-21 | 中建材玻璃新材料研究院集团有限公司 | Preparation method of high-strength antibacterial flexible glass |
| CN115818981B (en) * | 2022-12-23 | 2024-04-16 | 中建材玻璃新材料研究院集团有限公司 | Preparation method of high-strength antibacterial flexible glass |
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