CN114105483A - Ultra-thin glass strengthening method, ultra-thin glass, display screen and touch display device - Google Patents
Ultra-thin glass strengthening method, ultra-thin glass, display screen and touch display device Download PDFInfo
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- CN114105483A CN114105483A CN202111410105.0A CN202111410105A CN114105483A CN 114105483 A CN114105483 A CN 114105483A CN 202111410105 A CN202111410105 A CN 202111410105A CN 114105483 A CN114105483 A CN 114105483A
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- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 24
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
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- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 235000011181 potassium carbonates Nutrition 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
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- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
-
- 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
-
- 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
Abstract
The application discloses a strengthening method of ultrathin glass, the ultrathin glass, a display screen and a touch display device. The method comprises the following steps: pretreating glass to remove dirt on the surface of the glass; determining a target cutting area of the glass, and protecting the area of the glass except the target cutting area by using a protective layer; chemically cutting the target cutting area by using etching solution to enable the section of the target cutting area to be in an arc shape; carrying out surface treatment on the cut glass; immersing the glass subjected to surface treatment into a strengthening solution for strengthening treatment; and (4) performing secondary surface treatment on the strengthened glass by using the repair liquid. The method has the advantages of simple process, convenience in operation and capability of batch processing, and the strength of the ultrathin glass is effectively improved, so that the damage effect of stress concentration on the surface of the glass is favorably overcome, and the strengthened glass has good flexibility properties such as bending or folding.
Description
Technical Field
The invention relates to the technical field of touch display screens, in particular to a strengthening method of ultrathin glass, the ultrathin glass, a display screen and a touch display device.
Background
The glass has the unique advantages of good transparency, high mechanical strength, uniform texture, smooth surface and the like, and is widely applied to display devices of intelligent terminals such as mobile phones, digital cameras, computers and the like. Although glass has high theoretical strength, glass needs to be lightweight (thinned) and have good flexibility such as bending or folding based on the demand of a display device of an existing electronic product, and also needs to meet the requirement that a user carelessly scratches a surface of a display screen during a long-time use, so that the glass is easily damaged due to stress concentration at the surface scratches.
The related art has been devoted to developing thinner, less fragile materials, and thus transparent PI, PES, PEN, and the like have been developed or applied as substitutes for glass. However, these materials still have low surface hardness and are easily scratched, and thus, they are difficult to be applied to display devices of electronic products. Therefore, it is difficult to provide ultra-thin glass with good flexibility such as bending or folding.
Disclosure of Invention
In view of the above-mentioned drawbacks and deficiencies of the prior art, it is desirable to provide a strengthening method for ultra-thin glass, a display screen and a touch display device.
In a first aspect, the present invention provides a method for strengthening ultra-thin glass, comprising:
pretreating glass to remove dirt on the surface of the glass;
determining a target cutting area of the glass, and protecting the area of the glass except the target cutting area by using a protective layer;
chemically cutting a target cutting area by using an etching solution to enable the section of the target cutting area to be in an arc shape;
carrying out surface treatment on the cut glass;
immersing the glass subjected to surface treatment into a strengthening solution for strengthening treatment;
carrying out secondary surface treatment on the strengthened glass by using a repair liquid; the repairing liquid consists of the following components: 2-15% by weight of hydrofluoric acid; 0.3 to 4% by weight of ammonium fluoride; 2-15 wt% of an inorganic acid; and the balance water.
According to the embodiment of the application, the etching solution consists of the following components: 10-30 wt% hydrofluoric acid; 0.3 to 4% by weight of ammonium fluoride; 10 to 40 wt% of an inorganic acid; and the balance water.
Further, the content of hydrofluoric acid is 15 to 20 wt%.
Further, the etching solution is composed of the following components: 15% by weight of hydrofluoric acid; 3% by weight of ammonium fluoride; 30% by weight of an inorganic acid; and the balance water.
According to an embodiment of the present application, a process of chemically cutting a target cutting region using an etching solution includes:
and immersing the glass into the etching solution or spraying the etching solution on two sides of the glass.
According to the embodiment of the application, the cut glass is subjected to surface treatment, which comprises the following steps:
and removing the protective layer on the glass except the target cutting area according to the property of the protective layer, and cleaning the surface of the glass.
According to the embodiment of the application, the cut glass is subjected to surface treatment, and the method further comprises the following steps:
after the glass surface is cleaned, the crack on the glass surface is treated by using the repairing liquid.
According to the embodiment of the application, the temperature of the strengthening treatment is 340-400 ℃, and the time is 10-60 min.
According to an embodiment of the present application, a strengthening fluid includes: potassium nitrate which is melted at high temperature, wherein the purity of the potassium nitrate is more than or equal to 99.9 percent, and the melting temperature is equal to 334 ℃.
According to an embodiment of the present application, the method of strengthening ultra-thin glass further comprises:
preheating the glass before immersing the glass after surface treatment into a strengthening solution for strengthening treatment;
after the surface-treated glass is immersed in a strengthening liquid to be strengthened, the strengthened glass is cooled.
According to the examples of the present application, the conditions for performing the secondary surface treatment on the strengthened glass using the repair liquid are as follows: the temperature is 20-30 ℃, and the time is 1-10 min.
In a second aspect, the present application provides an ultra-thin glass made according to the method of the first aspect.
In a third aspect, the present application provides a display panel, at least a portion of which is made of the above ultra-thin glass.
In a fourth aspect, the present application provides a touch display device, including the display screen and/or the ultra-thin glass.
The manufacturing method of the ultrathin glass is simple in process, convenient to operate and capable of processing in batches, strength of the ultrathin glass is effectively improved, damage to the surface of the glass caused by stress concentration is overcome, the strengthened glass has good bending or folding flexibility and the like, and the manufacturing method of the ultrathin glass is suitable for manufacturing flexible screens and relevant equipment.
Drawings
Other features, objects and advantages of the present application will become more apparent upon reading of the following detailed description of non-limiting embodiments thereof, made with reference to the accompanying drawings in which:
FIG. 1 is a schematic flow chart of a method for strengthening ultra-thin glass;
FIG. 2 is a sectional view after chemical cutting;
FIG. 3 is a graph showing the stress distribution within the strengthened glass;
FIG. 4 is a graph showing the relationship between the concentration of the strengthening liquid, the thickness of the glass, and the bending radius and the compressive stress.
Detailed Description
The present application will be described in further detail with reference to examples. It is to be understood that the specific embodiments described herein are merely illustrative of the relevant invention and not restrictive of the invention. It should be noted that, for convenience of description, only the portions related to the invention are shown in the embodiments.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present application will be described in detail with reference to examples.
It is noted that the endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and that such ranges or values are understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
Cover substrates for consumer products (e.g., consumer electronics, including cell phones, tablets, computers, navigation systems, wearable devices, etc.) are used primarily to provide an easy-to-clean transparent surface and to protect sensitive components of the consumer product from mechanical damage (e.g., puncture and impact forces). The glass has the unique advantages of good transparency, high mechanical strength, uniform texture, smooth surface and the like, and is widely applied to intelligent terminals such as mobile phones, digital cameras, computers and the like.
At present, requirements of users on the beauty, performance and use comfort of various electronic products are higher and higher. In order to meet the demands of users, the display screens of existing electronic products, such as mobile phones, are as thin as possible, or are also required to have good foldability and/or curvature.
Thus, the ultra-thin glass makes it possible to design electronic products to meet the user's needs. However, the conventional ultra-thin glass is not ideal in terms of strength, flexibility such as bending or folding, and during a long time use, a Scratch (Scratch) is easily formed on the surface of the glass by a user without paying attention to the use of the glass, and a stress concentration phenomenon is easily generated at a fine surface Scratch, so that a display screen of an electronic product is easily broken and damaged.
In view of the above problems, an embodiment of the present invention provides a method for strengthening an ultra-thin glass, as shown in fig. 1, including:
s1, pretreating the glass to remove dirt on the surface of the glass;
s2, determining a target cutting area of the glass, and protecting the area of the glass except the target cutting area by using a protective layer;
s3, chemically cutting the target cutting area by using the etching solution to enable the section to be in an arc shape;
s4, performing surface treatment on the cut glass;
s5, immersing the glass with the surface treated into a strengthening solution for strengthening treatment;
s6, performing secondary surface treatment on the strengthened glass by using a repair liquid; the repairing liquid consists of the following components: 2-15% by weight of hydrofluoric acid; 0.3 to 4% by weight of ammonium fluoride; 2-15 wt% of an inorganic acid; and the balance water.
It should be noted that, in the following description,
the method for strengthening an ultra-thin glass according to the embodiment of the present application is applicable to various ultra-thin glasses, such as alkali aluminosilicate-based glasses and lithium alumino-alumina glasses. The ultra-thin glass is glass having a thickness of 0.2mm or less, preferably 0.1mm or less.
The surface of the glass is contaminated by a plurality of organic and inorganic particles during transportation, and the contaminants may scratch the surface of the glass during subsequent processes, cause damage to the glass and affect the strengthening effect. Therefore, S1, the glass is pretreated to remove organic or inorganic residues such as dust, impurities, dirt, oil stains and the like on the surface of the glass, so that the strengthening effect is avoided, and the strengthening effect and the yield are improved; wherein, the glass pretreatment can be rolling adhesion by using a viscous rolling rod or cleaning by using ultrasonic waves; of course, the glass pretreatment can also be carried out by washing with an alkaline detergent and pure water (DI); the cleaning mode can be spray rinsing by a high-pressure gun or directly entering into a lotion; the alkaline detergent may be sodium hydroxide, potassium hydroxide, etc., and this is not particularly limited in the present application.
According to the actual processing requirement, after the target cutting area of the glass is determined, other areas except the target cutting area on the glass need to be protected by using a protective layer (Masking). The material of the protective layer may be a material having acid resistance, including but not limited to polytetrafluoroethylene, polyimide, polyvinyl chloride, polyethylene terephthalate, polypropylene, polyethylene, acrylic series mixture, polyurethane series mixture, and epoxy series mixture, for example, in practical use, a film to which organic substances such as polyvinyl chloride (PVC), polytetrafluoroethylene (Teflon) and the like are attached is included, and the film protection includes two modes: one is to cut the film into a desired shape and then attach the film to glass; one is that after the whole glass is completely pasted with a film, the film of the target cutting area on the glass is cut off through procedures such as a needle knife and the like, and only the area needing to be protected is reserved; the protective layer can also be an organic coating material, such as photoresist and the like, and when the organic coating material is used, the region needing to be protected can be coated by a screen printing or printing process and then dried or hardened by ultraviolet; if the whole glass is organically coated, the protective layer of the target cutting area can be removed through the procedures of exposure, development and the like; of course, if a liquid organic coating material is used, a procedure such as VCD, drying, etc. may be used in order to remove the solvent and improve the adhesion.
In S3, the target region is chemically cut with an etching solution so that the cut surface thereof is circular-arc-shaped. The etching solution is mainly a mixture solution containing HF, the target region without the protection of the protective layer is cut into a desired shape by chemical etching, and the cut section is made to be circular arc by controlling the composition of the etching solution, the treatment temperature and the treatment time, as shown in fig. 2. In actual processing, the shape of the section can be changed by regulating the composition of the etching solution, the treatment temperature and the treatment time according to the actual requirements of users, and the ideal section is C-shaped. When a flaw portion such as a scratch is formed on a cut surface of a glass, if stress is concentrated on the flaw portion of the cut surface, the glass is likely to be broken. Therefore, in order to prevent the strength of the glass from being reduced, the tip of the defect portion such as the cut surface and the scratch is sufficiently rounded in the embodiment of the present application, which is advantageous for enhancing the strength of the glass.
The embodiment of the application adopts the etching solution to carry out chemical cutting, has simple process and controllable conditions, does not generate any micro-crack on the section of the glass, does not generate stress concentration phenomenon under the action of external force, and does not need to carry out secondary grinding or polishing and other processes on the section.
For S4, the surface treatment is performed on the cut glass, mainly to remove the protective layer on the glass except the target cutting area, and to remove other contaminants on the glass surface.
In S5, the glass after surface treatment is immersed in the strengthening solution to be strengthened, and the alkali metal ions in the glass containing alkali metal ions are ion-exchanged with other alkali metal ions having a larger ionic radius than the alkali metal ions mainly by the ion exchange process, so that the ion exchange process is advantageous in forming a compressive stress on the glass surface, and improving the bending strength, impact strength, and abrasion and scratch resistance.
Specifically, the chemical strengthening treatment is a treatment of replacing alkali metal ions (Li ions and/or Na ions) having a small ionic radius on the glass surface with other alkali metal ions (K ions) having a larger ionic radius by ion exchange at a temperature equal to or lower than the glass transition point. This causes a compressive stress to remain on the glass surface, thereby improving the strength of the glass.
The strengthening treatment process in the examples of the present application is carried out by bringing the above-mentioned glass containing alkali metal ions into contact with an inorganic salt composition containing other alkali metal ions having a larger ion radius than the alkali metal ions contained in the glass to carry out ion exchange.
In general, the alkali metal ion contained in the glass is a Na ion, and from the viewpoint of enabling the inorganic salt to have a long life, the inorganic salt composition is more preferably an inorganic salt composition containing a potassium ion, for example, at least one of potassium nitrate, potassium carbonate, potassium hydrogen carbonate, and potassium phosphate.
Under sufficient heating conditions, the heat activation energy of ion diffusion is increased, larger potassium ions and relatively smaller sodium ions in the glass are exchanged and permeated, and the exchanged potassium ions form compressive stress on the surface of the glass due to attraction; according to the penetration depth and distribution density of potassium ions on the glass, the surface hardness, strength and bending property of the glass are improved. The step of ion-exchanging the glass may be a method of coating a paste-like inorganic salt composition on the surface of the glass, a method of spraying an aqueous solution of the inorganic salt composition on the surface of the glass, a method of immersing the glass in a salt bath of a molten salt heated to a melting point or higher, or the like.
In actual processing, the temperature and time of the strengthening treatment are adjusted depending on the type and thickness of the glass, and the method of the embodiment of the present application can strengthen most glasses, preferably in the vicinity of the softening point of each glass composition.
S6, the strengthened glass is subjected to secondary surface treatment by using a repair liquid, on one hand, the residual inorganic salt ions on the surface of the strengthened glass are mainly cleaned, and the strengthened glass can be immersed in pure water or the surface of the glass is cleaned by spraying the pure water as the inorganic salt is easily dissolved in the pure water; on the other hand, fine scratches are caused on the surface of the glass in the strengthening treatment process, and the repair treatment is carried out by using the repair liquid containing HF, so that the scratches on the surface of the glass become smooth and soft, the strength of the glass is further ensured, the surface of the glass is thoroughly cleaned after the repair is finished, and the glass can be cleaned by using an alkaline detergent, but the residual detergent needs to be fully cleaned by using pure water after the cleaning by using the alkaline detergent is finished; in a specific embodiment, the repair liquid is composed of 5 wt% hydrofluoric acid; 0.9% by weight of ammonium fluoride; 7% by weight of mineral acid and the balance water.
The method for strengthening the ultrathin glass solves the problem that the existing ultrathin glass is poor in flexibility such as bending or folding. According to the embodiment of the application, the glass section is arc-shaped by adopting a chemical cutting method, the ultra-thin glass is strengthened by the strengthening liquid, and the compressive stress is formed on the surface of the glass, so that the strength, bending or folding flexibility and other flexibility properties of the ultra-thin glass are effectively improved, and the ultra-thin glass can meet the processing and design requirements of other components such as the display screen of the existing electronic product.
In some embodiments, the etching solution consists of: 10-30 wt% hydrofluoric acid; 0.3 to 4% by weight of ammonium fluoride; 10 to 40 wt% of an inorganic acid; and the balance water. Wherein the hydrofluoric acid contains extremely strong electrophilic particles H+And medium electrophilic particles F-The silicon fluoride has strong decomposition capability on glass, can react with oxides on the surface of the glass to form fluosilicate, and can be well dissolved in an etching solution. Based on the total weight of the etching solution, the content of hydrofluoric acid is 10-30%, the amount of hydrofluoric acid is less than 10%, it is difficult to form an arc-shaped section, the bending strength of the glass cannot be increased, and the amount of hydrofluoric acid is greater than 30%, so that the etching amount is too large, the size of the glass is affected, the section is sharp, the shape is not uniform, and the etching rate is too high, the forming degree of the section is difficult to control, and safety and environmental problems may be caused. Ammonium fluoride is basic and forms a buffer solution with hydrofluoric acid, and NH4+Will influence F-The activation degree of the glass is reduced, so that the reaction rate of the glass and hydrofluoric acid can be reduced, the control of the shape of the section is realized through the regulation of the etching speed, over-etching is avoided, the slow etching speed is favorable for improving the flatness of the edge of the section, and the glass strength is favorably improved. Based on the total weight of the etching solution, the content of ammonium fluoride is 0.3-4%, the amount of ammonium fluoride is less than 0.3%, the purpose of controlling the etching rate is difficult to achieve, and the amount of ammonium fluoride is more than 4%, so that the etching rate is too low to influence the repair efficiency. The inorganic acid can provide H+So as to regulate and control the etching rate and exert a synergistic effect with hydrofluoric acid and/or ammonium fluoride to improve the repairing effect. Based on the total weight of the etching solution, the content of the inorganic acid is 10-40%, the amount of the inorganic acid is less than 10%, the etching rate is reduced, an expected arc-shaped section cannot be formed, the amount of the inorganic acid is more than 40%, on one hand, the etching rate is too high, the shape and the size of the section are not controlled, and on the other hand, the H in the etching solution is measured+The concentration reaches a critical saturation state when the content of the inorganic acid is 40%, and if the content of the inorganic acid is continuously increased, the etching solution contains excessive inorganic acid, so that the cost is increased, and the acid-containing wastewater is more discharged. Wherein the inorganic acid is at least one of nitric acid, sulfuric acid, phosphoric acid and hydrochloric acid. Nitric acid can increase acidity of the acid solution and enhance etching effect; the viscosity of the sulfuric acid is high, so that the surface of the glass can be covered and protected, and new defects are prevented from being generated in the cutting process; the addition of phosphoric acid can ensure the glassSiO of (2)2The layer is not over-etched but only in-plane defects are repaired; the hydrochloric acid can effectively remove metal impurities contained in the glass, and the dissolved glass components can not be condensed to form a water glass state; the water is preferably deionized or pure water.
In some embodiments, the hydrofluoric acid is present in an amount of 15 to 20 wt%. The section of the glass cut by the etching solution with the content has the best arc shape.
In some of these embodiments, the etching solution is composed of 15 wt% hydrofluoric acid, 3 wt% ammonium fluoride, 30 wt% inorganic acid, and the balance water. By optimizing the content of the three key components, the section of the glass cut by the etching solution of the embodiment is smooth and soft.
In a preferred embodiment, the step of performing chemical cutting of the target cutting region using an etching solution in step S3 includes: and immersing the glass into the etching solution or spraying the etching solution on two sides of the glass. According to the mode, the uniform contact between the glass and the etching solution is favorably ensured, so that the section is flat.
In some embodiments, S4, subjecting the cut glass to a surface treatment, comprising: and removing the protective layer on the glass except the target cutting area according to the property of the protective layer, and cleaning the surface of the glass.
Wherein, if the protective layer is a film attached on the surface of the glass, the protective layer can be directly peeled and removed by manpower or machines, if an adhesive is used in the film attaching process, the film is peeled and removed in low temperature, high temperature or solvent according to the property of the adhesive; if the protective layer is organic coating liquid, the glass can be immersed in alkaline agent or the alkaline agent is sprayed on the glass to remove the organic coating, and the surface of the glass is washed clean by using clear water. According to the verification of practical experiments, the temperature of the alkaline medicament is 45-85 ℃, so that the organic coating can be removed more conveniently.
In some embodiments, S4, performing surface treatment on the cut glass, further comprising:
after the glass surface is cleaned, the crack on the glass surface is treated by using the repairing liquid.
According to the mode, the formation of fine scratches on the glass surface in the process can be avoided, and the strengthening effect of the ultrathin glass can be ensured.
As a preferable embodiment, experimental optimization verifies that in the process of immersing the glass after surface treatment in the strengthening solution for strengthening treatment at S5, the temperature of the strengthening treatment is 340-400 ℃ and the time is 10-60 min. The strengthening treatment temperature and time disclosed in the present embodiment are suitable for alkali aluminosilicate-based or lithium bauxite-based glasses, can obtain a higher depth of a compressive stress layer, can obtain chemically strengthened glasses having an excellent balance between strength and depth of the compressive stress layer, and ensure formation of a uniform compressive stress layer on the glass surface, thereby improving the properties of the glass, such as flexural strength, abrasion resistance, and scratch resistance. FIG. 3 is a graph showing the stress distribution within the strengthened glass. It should be noted that, as the strengthening temperature and time increase, the penetration and diffusion depth dol (depth of layer) of K ions increases, and the hardness of the glass increases; as the strengthening temperature and time increase, the compressive stress will decrease, and thus the strength of the glass will decrease; as the "thermally activated energy" that contributes to ion diffusion increases with increasing strengthening temperature and time, the DOL increases deeper. However, since the stress relaxation phenomenon occurs due to the Annealing (Annealing) effect, and the compressive stress on the glass surface tends to be reduced, it is necessary to determine the temperature and time for strengthening in actual processing according to the kind and thickness of the glass and the user's request. Wherein, the DOL can be detected by a DOL testing instrument.
In a preferred embodiment, in the step of immersing the surface-treated glass in the strengthening solution to be strengthened in S5, the strengthening solution used is potassium nitrate melted at a high temperature, wherein the purity of potassium nitrate is 99.9% or more and the melting temperature is 334 ℃. According to experimental verification, the potassium nitrate has low melting point and better strengthening effect.
Since the strengthening temperature is relatively high, if glass is directly put into the high-temperature strengthening liquid at normal temperature or the glass is directly taken out from the high-temperature strengthening liquid and exposed to normal temperature, the glass is cracked or bent badly due to the rapid change of temperature. Thus, in some embodiments, the method further comprises:
preheating the glass before immersing the glass after surface treatment into a strengthening solution for strengthening treatment;
after the surface-treated glass is immersed in a strengthening liquid to be strengthened, the strengthened glass is cooled.
In a preferred embodiment, in the second surface treatment of the strengthened glass using the repair liquid at S6, the treatment temperature is 20 ℃ to 30 ℃ for 1min to 10 min. According to the mode, the method is beneficial to treating the fine scratches on the surface of the strengthened glass to be smooth and soft by using the repairing liquid, and the strength of the strengthened glass is ensured.
In a second aspect, the present application provides an ultra-thin glass made according to the strengthening method of the first aspect. Therefore, the ultrathin glass has the characteristics of high strength, good bending or folding performance and the like. It will be understood by those skilled in the art that the ultra-thin glass has all the features and advantages of the above-described ultra-thin glass strengthening method, and thus, will not be described in excessive detail herein.
In some embodiments, as shown in fig. 4, in the case that the penetration depth of potassium ions is the same for ultra-thin glasses with different thicknesses, the bending radius of the ultra-thin glass increases with the increase of the thickness, and correspondingly, the compressive stress of the ultra-thin glass also increases with the increase of the thickness of the ultra-thin glass; for ultra-thin glass of the same thickness, as the penetration depth of potassium ions increases, the bending radius and the compressive stress of the ultra-thin glass both decrease. As can be seen from fig. 4: for the ultra-thin glass with the thickness of 70 mu m, the bending radius can reach 1.5mm, and the compressive stress can reach 750 MPa; for the ultrathin glass with the thickness of 50 mu m, the bending radius can reach up to 1.0mm, and the compressive stress can reach up to 710 MPa; for ultra-thin glass with a thickness of 30 μm, the bending radius can be as high as 0.5mm and the compressive stress can be as high as 650 MPa. It is thus seen that the ultra-thin glass is excellent in bending characteristics, particularly, has a large bending radius.
In a third aspect, embodiments of the present application provide a display screen, at least a portion of which is formed of the ultra-thin glass of the second aspect. It will be understood by those skilled in the art that the ultra-thin glass has all the features and advantages of the above-described ultra-thin glass strengthening method, and thus, will not be described in excessive detail herein.
In a fourth aspect, embodiments of the present application provide a touch display device, which includes the display screen of the third aspect and/or the ultra-thin glass of the second aspect. Those skilled in the art will appreciate that the touch display device has all the features and advantages of the above-mentioned ultra-thin glass strengthening method, and will not be described in detail herein. The touch display device is not limited to a Personal Digital Assistant (PDA), a Tablet Computer (Tablet Computer), a wireless handheld device, a mobile phone, and the like.
Additional aspects and advantages of the present application will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the present application.
The present invention is illustrated below by way of specific examples, which are intended to be illustrative only and not to limit the scope of the present invention in any way, and reagents and materials used therein are commercially available, unless otherwise specified, and conditions or steps thereof are not specifically described.
Example 1
S1, removing dirt on the surface of the glass by using sodium hydroxide liquid medicine and clear water on the ultrathin glass with the thickness of 70 mu m;
s2, determining a target cutting area of the glass, and protecting the area of the glass except the target cutting area by using a PVC film;
s3, chemically cutting the target cutting area by using an etching solution composed of 15 wt% of hydrofluoric acid, 3 wt% of ammonium fluoride, 30 wt% of inorganic acid and the balance of water to make the section of the target cutting area be in a circular arc shape;
s4, removing the PVC film artificial glass on the cut glass surface, and then cleaning the glass surface by using pure water;
s5, preheating the glass after surface treatment, immersing the glass in molten potassium nitrate for strengthening treatment, controlling the temperature and strengthening time of the molten potassium nitrate to ensure that the penetration depth of potassium ions is 4 mu m, then controlling the temperature of the molten potassium nitrate to be reduced according to a certain rate, taking out the strengthened glass when the temperature is cooled to room temperature, and cleaning residual potassium nitrate on the surface of the glass by using pure water;
s6, immersing the strengthened glass in 5 wt% hydrofluoric acid; 0.9% by weight of ammonium fluoride; treating the glass surface at room temperature for about 5min in a repair liquid composed of 7 wt% of inorganic acid and the balance of water to eliminate fine scratches on the glass surface, and then sequentially cleaning the glass with alkaline liquid medicine and pure water.
Example 2
This example is different from example 1 in that the thickness of the ultra-thin glass is 50 μm.
Example 3
This example is different from example 1 in that the thickness of the ultra-thin glass is 30 μm.
Example 4
This example differs from example 1 in that the penetration depth of potassium ions was 5 μm;
example 5
This example differs from example 1 in that the penetration depth of potassium ions was 6 μm;
example 6
This example differs from example 1 in that the penetration depth of potassium ions was 7 μm;
example 7
This example differs from example 1 in that the penetration depth of potassium ions was 8 μm;
example 8
This example differs from example 1 in that the penetration depth of potassium ions was 9 μm;
example 9
This example is different from example 1 in that the penetration depth of potassium ions was 10 μm;
example 10
This example differs from example 1 in that the penetration depth of potassium ions was 11 μm;
example 11
This example is different from example 1 in that the penetration depth of potassium ions was 12 μm;
example 12
This example is different from example 1 in that the thickness of the ultra-thin glass is 50 μm and the penetration depth of potassium ions is 5 μm;
example 13
This example is different from example 1 in that the thickness of the ultra-thin glass is 50 μm and the penetration depth of potassium ions is 6 μm;
example 14
This example is different from example 1 in that the thickness of the ultra-thin glass is 50 μm and the penetration depth of potassium ions is 7 μm;
example 15
This example is different from example 1 in that the thickness of the ultra-thin glass is 50 μm and the penetration depth of potassium ions is 8 μm;
example 16
This example is different from example 1 in that the thickness of the ultra-thin glass is 50 μm and the penetration depth of potassium ions is 9 μm;
example 17
This example is different from example 1 in that the thickness of the ultra-thin glass is 50 μm and the penetration depth of potassium ions is 10 μm;
example 18
This example is different from example 1 in that the thickness of the ultra-thin glass is 50 μm and the penetration depth of potassium ions is 11 μm;
example 19
This example is different from example 1 in that the thickness of the ultra-thin glass is 50 μm and the penetration depth of potassium ions is 12 μm;
example 20
This example is different from example 1 in that the thickness of the ultra-thin glass is 30 μm and the penetration depth of potassium ions is 5 μm;
example 21
This example is different from example 1 in that the thickness of the ultra-thin glass is 30 μm and the penetration depth of potassium ions is 6 μm;
example 22
This example is different from example 1 in that the thickness of the ultra-thin glass is 30 μm and the penetration depth of potassium ions is 7 μm;
example 23
This example is different from example 1 in that the thickness of the ultra-thin glass is 30 μm and the penetration depth of potassium ions is 8 μm;
example 24
This example is different from example 1 in that the thickness of the ultra-thin glass is 30 μm and the penetration depth of potassium ions is 9 μm;
example 25
This example is different from example 1 in that the thickness of the ultra-thin glass is 30 μm and the penetration depth of potassium ions is 10 μm;
example 26
This example is different from example 1 in that the thickness of the ultra-thin glass is 30 μm and the penetration depth of potassium ions is 11 μm;
example 27
This example is different from example 1 in that the thickness of the ultra-thin glass is 30 μm and the penetration depth of potassium ions is 12 μm.
The results of testing the bend radius and compressive stress of the ultra-thin glasses obtained in examples 1 to 27 above are shown in table 1 and fig. 4:
table 1 test results for examples 1-27
Combining the results of table 1 and fig. 4, one can see that:
the test results of example 1 to example 27 are combined to show that: the strengthening method of the ultrathin glass disclosed by the embodiment of the application can effectively improve the strength of the ultrathin glass, so that the damage effect of stress concentration on the surface of the glass can be overcome, the strengthened glass has good flexible properties such as bending or folding, and the strengthening method is suitable for manufacturing flexible screens and related equipment.
Specifically, as shown in fig. 4, in the case where the penetration depth of potassium ions is the same for ultra-thin glasses of different thicknesses, the bending radius of the ultra-thin glass increases with the increase of the thickness, and correspondingly, the compressive stress of the ultra-thin glass also increases with the increase of the thickness of the ultra-thin glass; for ultra-thin glass of the same thickness, as the penetration depth of potassium ions increases, the bending radius and the compressive stress of the ultra-thin glass both decrease. It can also be derived from table 1 and fig. 4: for the ultra-thin glass with the thickness of 70 mu m, the bending radius can reach 1.5mm, and the compressive stress can reach 750 MPa; for the ultrathin glass with the thickness of 50 mu m, the bending radius can reach up to 1.0mm, and the compressive stress can reach up to 710 MPa; for ultra-thin glass with a thickness of 30 μm, the bending radius can be as high as 0.5mm and the compressive stress can be as high as 650 MPa. It is thus seen that the ultra-thin glass is excellent in bending characteristics, particularly, has a large bending radius. It is thus seen that the ultra-thin glass is excellent in bending characteristics, particularly, has a large bending radius.
The above description is only a preferred embodiment of the application and is illustrative of the principles of the technology employed. It will be appreciated by a person skilled in the art that the scope of the invention as referred to in the present application is not limited to the embodiments with a specific combination of the above-mentioned features, but also covers other embodiments with any combination of the above-mentioned features or their equivalents without departing from the inventive concept. For example, the above features may be replaced with (but not limited to) features having similar functions disclosed in the present application.
Claims (14)
1. A method for strengthening ultra-thin glass, comprising:
pretreating glass to remove dirt on the surface of the glass;
determining a target cutting area of the glass, and protecting the area of the glass except the target cutting area by using a protective layer;
chemically cutting the target cutting area by using etching solution to enable the section of the target cutting area to be in an arc shape;
carrying out surface treatment on the cut glass;
immersing the glass subjected to surface treatment into a strengthening solution for strengthening treatment;
carrying out secondary surface treatment on the strengthened glass by using a repair liquid, wherein the repair liquid comprises the following components: 2-15% by weight of hydrofluoric acid; 0.3 to 4% by weight of ammonium fluoride; 2-15 wt% of an inorganic acid; and the balance water.
2. The method of claim 1, wherein the etching solution consists of: 10-30 wt% hydrofluoric acid; 0.3 to 4% by weight of ammonium fluoride; 10 to 40 wt% of an inorganic acid; and the balance water.
3. The method according to claim 2, wherein the hydrofluoric acid content is 15 to 20 wt.%.
4. The method of claim 2, wherein the etching solution consists of: 15% by weight of hydrofluoric acid; 3% by weight of ammonium fluoride; 30% by weight of an inorganic acid; and the balance water.
5. The method according to any one of claims 1 to 4, wherein the chemically cutting the target cutting region using the etching solution comprises:
and immersing the glass into the etching solution or spraying the etching solution on two sides of the glass.
6. The method according to any one of claims 1 to 4, wherein the cut glass is subjected to a surface treatment comprising:
and removing the protective layer on the glass except the target cutting area according to the property of the protective layer, and cleaning the surface of the glass.
7. The method of claim 6, wherein the cut glass is surface treated, further comprising:
after the glass surface is cleaned, the crack on the glass surface is treated by the repair liquid.
8. The method according to any one of claims 1 to 4, wherein the temperature of the strengthening treatment is 340 ℃ to 400 ℃ for 10min to 60 min.
9. The method according to any one of claims 1 to 4, wherein the strengthening liquid is potassium nitrate molten at a high temperature, wherein the purity of the potassium nitrate is 99.9% or more, and the melting temperature is 334 ℃.
10. The method according to any one of claims 1-4, further comprising:
preheating the glass before immersing the glass after surface treatment into a strengthening solution for strengthening treatment;
after the surface-treated glass is immersed in a strengthening liquid to be strengthened, the strengthened glass is cooled.
11. The method according to any one of claims 1 to 4, wherein the conditions for performing the secondary surface treatment on the strengthened glass using the repair liquid are as follows: the temperature is 20-30 ℃, and the time is 1-10 min.
12. An ultra-thin glass produced by the method of any one of claims 1 to 11.
13. A display screen, wherein at least a portion of the display screen is comprised of the ultra-thin glass of claim 12.
14. Touch display device, characterized in that, includes the display screen of claim 13 and/or the ultra-thin glass of any one of claim 12.
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