CN107793039B - Impact-resistant toughened glass, preparation method thereof and display terminal - Google Patents

Impact-resistant toughened glass, preparation method thereof and display terminal Download PDF

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Publication number
CN107793039B
CN107793039B CN201711115154.5A CN201711115154A CN107793039B CN 107793039 B CN107793039 B CN 107793039B CN 201711115154 A CN201711115154 A CN 201711115154A CN 107793039 B CN107793039 B CN 107793039B
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glass
impact
resistant
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toughened
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CN107793039A (en
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田鹏
李俊锋
张广涛
闫冬成
王丽红
郑权
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Dongxu Optoelectronic Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/28Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
    • C03C17/30Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material with silicon-containing compounds
    • GPHYSICS
    • G06COMPUTING; CALCULATING OR COUNTING
    • G06FELECTRIC DIGITAL DATA PROCESSING
    • G06F3/00Input arrangements for transferring data to be processed into a form capable of being handled by the computer; Output arrangements for transferring data from processing unit to output unit, e.g. interface arrangements
    • G06F3/01Input arrangements or combined input and output arrangements for interaction between user and computer
    • G06F3/03Arrangements for converting the position or the displacement of a member into a coded form
    • G06F3/041Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C2217/00Coatings on glass
    • C03C2217/70Properties of coatings
    • C03C2217/78Coatings specially designed to be durable, e.g. scratch-resistant

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  • Engineering & Computer Science (AREA)
  • Theoretical Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Human Computer Interaction (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Glass Compositions (AREA)

Abstract

The invention relates to the field of glass processing, and discloses impact-resistant tempered glass, a preparation method thereof and a display terminal. The preparation method of the shock-resistant toughened glass comprises the steps of contacting the toughened glass with silicone oil, then cleaning the glass with a solution, and drying. The impact-resistant glass prepared by the method improves the toughening property and the impact resistance of the glass on the basis of not influencing the light transmittance of the glass, and has the advantages of simple preparation method and low cost of raw materials.

Description

Impact-resistant toughened glass, preparation method thereof and display terminal
Technical Field
The invention relates to the field of glass processing, in particular to impact-resistant toughened glass, a preparation method thereof and a display terminal.
Background
With the gradual popularization of notebook computers and mobile phones, in order to increase the touch feeling and the surface aesthetic property, the touch panel is gradually changed from the conventional PC material to the conventional glass material. The demand of the ultrathin glass adopted by the touch panel is rapidly increased, the touch mode puts forward higher requirements on the strength and the hardness of the glass, but the strength and the hardness of the ultrathin glass cannot meet the requirements of the touch technology on the performance of the touch screen, the surface hardness of the glass material is higher, and the transmittance and the scratch-resistant effect are good. But the characteristic of being easily broken by impact is the deadly characteristic of glass. In order to change the brittle nature of glass when subjected to impact, chemical tempering processes have been developed.
The reinforcement of ultra-thin glass is mainly achieved by chemical tempering. The glass is subjected to a series of processing processes such as cutting, grinding, polishing and the like before chemical tempering, the processed glass surface or subsurface has more or less micro cracks, and the depth, length, width, quantity and distribution of the micro cracks on the glass surface and the scratch and abrasion of the glass surface have great influence on the glass strength, particularly the impact strength of the glass.
The chemical strengthening is to soak the glass in a potassium nitrate solution, and to replace sodium ions on the surface of the glass with potassium ions in the potassium nitrate solution for a long time and at a high temperature, so that a replacement layer of potassium and sodium ions is formed on the surface of the glass, and the glass generates certain internal stress, commonly called surface stress value. The chemically strengthened glass can be used as touch screen glass (including OGS, In-Cell, On-Cell, G/G, G/F, G/F/F) of electronic devices such as smart phones, tablet computers, ultrabooks and the like.
However, the impact resistance effect of the glass formed by the existing chemical tempering is not good, for example, in a steel ball experiment: the glass is crushed by freely falling from the height of 500mm by using a steel ball with the diameter of 30mm and the weight of 120g, and the strength of the glass after chemical tempering is not high, namely the impact strength can not meet the test requirements of people.
In order to solve the problem of poor impact resistance, CN104400581A discloses a method for performing fine polishing on tempered glass to remove microcracks on the surface of the tempered glass, but because both sides of the tempered glass have large compressive stresses symmetrically distributed along the thickness direction, if the fine polishing process is not proper, the removal thicknesses of both sides of the glass are inconsistent, and the stress distribution of both sides of the processed glass is asymmetric, so that the glass is deformed or even broken, thereby greatly reducing the yield of the glass.
CN103508674A discloses a method for removing micro-cracks on the surface of tempered glass by etching with hydrofluoric acid, but the method has the disadvantages of environmental pollution, dangerous operation, corrosion of the glass surface by the external environment after acid treatment, reduced surface hardness and ineffective strength maintenance.
CN102643033A discloses coating the surface of toughened glass with an organic glue layer and subjecting it to a high temperature treatment, said organic glue layer being converted into a protective layer, thereby improving the impact resistance. Although the organic glue layer has simple manufacturing process and low cost, the organic glue layer is easily influenced by the external environment, and once the organic glue layer is damaged, the glass strength is obviously reduced.
Disclosure of Invention
The invention aims to overcome the problem of poor impact resistance of toughened glass in the prior art, and provides impact-resistant toughened glass, a preparation method thereof and a display terminal.
In order to achieve the above object, a first aspect of the present invention provides a method for producing impact-resistant tempered glass, wherein the method comprises: and (3) contacting the toughened glass with silicone oil, then washing the glass with the solution, and drying.
Preferably, the contacting is by dipping.
Preferably, the temperature of the silicone oil is 150-.
Preferably, the contact time of the toughened glass and the silicone oil is 0.5-2 h.
Preferably, the tempered glass is tempered sodium aluminosilicate glass.
Preferably, the soda-aluminosilicate glass contains 55 to 70 wt.% SiO210-25% by weight of Al2O310-20 wt% of Na2O, 0-6% by weight of K2O, 0-5 wt% CaO, 0-10 wt% MgO, 0-2 wt% ZrO20 to 10% by weight of B2O3And 0-15% by weight of P2O5
Preferably, the thickness of the tempered glass is 0.1-3 mm.
Preferably, the solution is carbon tetrachloride.
The second aspect of the invention provides the impact-resistant toughened glass prepared by the method, wherein the impact-resistant toughened glass is subjected to a ball drop test by using a steel ball with the diameter of 30mm and the mass of 120g, and the measured breaking height is more than or equal to 615 mm; the surface stress of the impact-resistant toughened glass is more than or equal to 768 psi.
Preferably, the crushing height is 615mm to 625 mm; the surface stress is 768-.
Preferably, the thickness of the impact-resistant toughened glass is 0.1-3 mm.
The invention provides a display terminal, which comprises a touch screen made of the impact-resistant toughened glass.
The silicone oil forms a silica film on the surface of the glass, is similar to a Si-O tetrahedral framework structure in the glass, can fill microcracks on the surface of the glass, plays a role in healing the microcracks on the surface of the glass, eliminates a fracture layer on the surface of the glass, and improves the impact strength of the glass. Furthermore, in a ball drop experiment, the glass is still intact when freely dropped from a height of 600mm by using a steel ball with the diameter of 30mm (the diameter is 30mm) and the mass of 120g, and fine cracks on the surface of the chemically strengthened glass are filled, so that the glass has the advantages of strong impact resistance, small warping degree, stable surface structure and increased surface stress of a product.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be 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.
The invention provides a preparation method of impact-resistant toughened glass, which comprises the following steps: and (3) contacting the toughened glass with silicone oil, then washing the glass with the solution, and drying.
In the invention, the silicon oil forms a silicon-oxygen film on the surface of the toughened glass, which is similar to the Si-O tetrahedral framework structure in the glass, can fill the microcracks on the surface of the glass, plays a role in healing the microcracks on the surface of the glass and eliminates the fracture layer on the surface of the glass. The impact strength of the glass is improved.
In the present invention, the contacting may be, but not limited to, a dipping method.
In the present invention, the temperature of the silicone oil may be 150-.
In the invention, the contact time of the toughened glass and the silicone oil can be 0.5-2 h.
In the invention, the toughened glass is toughened sodium aluminosilicate glass. Toughened sodium aluminosilicateThe glass refers to sodium aluminosilicate glass which is chemically tempered by a method which is conventional in the field, for example, the sodium aluminosilicate glass can be put into KNO3Ion exchange was performed at 440 ℃ for 6 hours, and washing and drying were performed.
Further, the soda-aluminosilicate glass may contain 55 to 70 wt% of SiO210-25% by weight of Al2O310-20 wt% of Na2O, 0-6% by weight of K2O, 0-5 wt% CaO, 0-10 wt% MgO, 0-2 wt% ZrO20 to 10% by weight of B2O3And 0-15% by weight of P2O5
In the present invention, the thickness of the tempered glass may be 0.1mm or more, preferably 0.1 to 3 mm.
In the specific implementation mode of the invention, the chemical toughened glass can be put into 150-300 ℃ silicon oil for 0.5-2h for glass strengthening treatment, the silicon oil on the surface of the glass is cleaned by carbon tetrachloride solution, and the shock-resistant toughened glass is obtained by drying.
The second aspect of the invention provides the impact-resistant toughened glass prepared by the method, wherein the impact-resistant toughened glass is subjected to a ball drop test by using a steel ball with the diameter of 30mm and the mass of 120g, and the measured breaking height is more than or equal to 615 mm; preferably 615mm to 625 mm. The breaking height is the average height, the test method is that a steel ball with the diameter of 30mm and the weight of 120g is used for impacting the glass product from the height of 250mm, the glass product is impacted for 3 times at the same height without breaking, and then the height is raised by 50mm until the glass product is broken, and the height is the breaking height of the glass.
In the invention, according to JC-T977-789 method, FSM-6000 glass stress meter is adopted to test the surface stress of the glass, and the surface stress of the impact-resistant toughened glass is determined to be more than or equal to 768psi, preferably 768-789 psi.
In the present invention, the thickness of the impact-resistant tempered glass may be 0.1mm or more, preferably 0.1 to 3 mm.
The invention provides a display terminal, which comprises a touch screen made of the impact-resistant toughened glass.
In the invention, the display terminal can be, but is not limited to, an electronic device such as a smart phone, a tablet computer, a super notebook, and the like.
The present invention will be described in detail below by way of examples.
Preparation example 1
20 pieces of a material having a size of 100mm (length) x 100mm (width) x 0.7mm (thickness) and containing 61% by weight of SiO213% by weight of Al2O314% by weight of Na2O, 3% by weight of K2O, 4 wt% CaO, 4 wt% MgO, and 1 wt% ZrO2Putting the sodium aluminosilicate glass into high-quality KNO3Ion exchange is carried out for 6 hours at 440 ℃, and then the toughened glass A is obtained by washing with deionized water and drying.
Preparation example 2
20 pieces of a material having a size of 100mm (length) x 100mm (width) x 0.7mm (thickness) and containing 58% by weight of SiO29% by weight of Al2O317% by weight of Na2O, 1.5% by weight of K2O, CaO 3 wt%, MgO 3 wt%, ZrO 0.5 wt%2And 8% by weight of B2O3Putting the sodium aluminosilicate glass into high-quality KNO3And performing ion exchange at 440 ℃ for 6 hours, then washing with deionized water, and drying to obtain toughened glass B.
Preparation example 3
20 pieces of a material having a size of 100mm (length) x 100mm (width) x 0.7mm (thickness) and containing 56% by weight of SiO210% by weight of Al2O313% by weight of Na2O, 1% by weight of K2O, 3 wt% CaO, 4 wt% MgO, 1 wt% ZrO2And 12% by weight of B2O3Putting the sodium aluminosilicate glass into high-quality KNO3And performing ion exchange at 440 ℃ for 6 hours, then washing with deionized water, and drying to obtain the toughened glass C.
Example 1
Examples 1-3 serve to illustrate the process of the invention.
And (2) putting 20 pieces of toughened glass A (obtained in preparation example 1) into a silicone oil solution at 150 ℃, treating for 2 hours, cooling, cleaning the silicone oil on the surface by using a carbon tetrachloride solution, and drying at 50 ℃ to obtain the shock-resistant toughened glass A.
The light transmittance of the impact-resistant tempered glass A was measured by an ultraviolet spectrophotometer (model UV-2501PC, manufactured by Shimadzu corporation, Japan) according to Lambert-beer's law, and the results are shown in Table 1.
The warpage test was carried out using a glass warpage test apparatus (model Excel 200U, manufactured by U.S. micro vision corporation) for impact-resistant tempered glass A, and the results are shown in Table 1
The surface inspection was carried out using a surface inspection machine (model CSB1600, manufactured by Shenke, Germany) for the impact-resistant tempered glass A, and the results are shown in Table 1.
The glass product was impacted from 250mm height using a steel ball of 30mm diameter and 120g mass, 3 times at the same height without shattering, and then raised by 50mm until shattered, this height being the shattered height of the piece of glass, and the results are given in Table 1.
According to JC-T977-2005 method, a surface stress test was performed on impact-resistant tempered glass A using a glass stress meter (model FSM-6000, manufactured by NIPPON FANYAO Co., Ltd.) and the results are shown in Table 1.
Example 2
And (2) putting 20 pieces of toughened glass B (obtained in preparation example 2) into a silicone oil solution at 200 ℃, treating for 1h, cooling, cleaning the silicone oil on the surface by using a carbon tetrachloride solution, and drying at 50 ℃ to obtain the impact-resistant toughened glass A.
The light transmittance, warpage, surface inspection yield and height of fracture were measured according to the method of example 1, and the results are shown in Table 1.
Example 3
And (2) putting 20 pieces of toughened glass C (obtained in preparation example 3) into a silicone oil solution at 300 ℃, treating for 0.5h, cooling, cleaning the silicone oil on the surface by using a carbon tetrachloride solution, and drying at 50 ℃ to obtain the impact-resistant toughened glass A.
The light transmittance, warpage, surface inspection yield and height of fracture were measured according to the method of example 1, and the results are shown in Table 1.
Comparative example
Comparative examples 1 to 3 are for explaining the method of using tempered glass without carrying out the method of putting into silicone oil of the present invention.
Comparative examples 4-6 are intended to illustrate the use of a soda-aluminosilicate glass, without tempering, and without the method of the present invention in silicone oil.
Comparative example 1
20 pieces of tempered glass a (obtained in production example 1) were tested for light transmittance, warpage, surface inspection yield, and fracture height according to the method of example 1, and the results are shown in table 1.
Comparative example 2
20 pieces of tempered glass B (obtained in preparation example 2) were tested for light transmittance, warpage, surface inspection yield, and fracture height according to the method of example 1, and the results are shown in table 1.
Comparative example 3
20 pieces of tempered glass C (obtained in production example 3) were tested for light transmittance, warpage, surface inspection yield, and fracture height according to the method of example 1, and the results are shown in table 1.
Comparative example 4
20 pieces of a material having a size of 100mm (length) x 100mm (width) x 0.7mm (thickness) and containing 61% by weight of SiO213% by weight of Al2O314% by weight of Na2O, 3% by weight of K2O, 4 wt% CaO, 4 wt% MgO, and 1 wt% ZrO2The soda-aluminosilicate glass obtained was measured for light transmittance, warpage, surface inspection yield and fracture height by the method of example 1, and the results are shown in Table 1.
Comparative example 5
20 pieces of a material having a size of 100mm (length) x 100mm (width) x 0.7mm (thickness) and containing 58% by weight of SiO29% by weight of Al2O317% by weight of Na2O, 1.5% by weight of K2O, CaO 3 wt%, MgO 3 wt%, ZrO 0.5 wt%2And 8% by weight of B2O3The soda-aluminosilicate glass obtained was measured for light transmittance, warpage, surface inspection yield and fracture height by the method of example 1, and the results are shown in Table 1.
Comparative example 6
20 pieces of a material having a size of 100mm (length) x 100mm (width) x 0.7mm (thickness) and containing 56% by weight of SiO210 by weight% of Al2O313% by weight of Na2O, 1% by weight of K2O, 3 wt% CaO, 4 wt% MgO, 1 wt% ZrO2And 12% by weight of B2O3The soda-aluminosilicate glass obtained was measured for light transmittance, warpage, surface inspection yield and fracture height by the method of example 1, and the results are shown in Table 1.
TABLE 1
Figure BDA0001466022810000091
The results in table 1 show that the impact-resistant toughened glass prepared by the method improves the toughening property and the impact resistance of the glass on the basis of not influencing the warping degree and the light transmittance of the glass, the surface stress of the glass is improved by more than 10%, the impact strength is improved by more than 30%, and the method is environment-friendly.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.

Claims (7)

1. A method for preparing impact-resistant toughened glass is characterized by comprising the following steps: contacting toughened glass with silicone oil, then cleaning the glass with a solution, and drying; the temperature of the silicone oil is 200-300 ℃; the contact time of the toughened glass and the silicone oil is 0.5-1 h; the thickness of the toughened glass is 0.1-3 mm; the toughened glass is toughened sodium aluminosilicate glass; the soda-aluminosilicate glass contains 56 wt.% SiO210% by weight of Al2O313% by weight of Na2O, 1% by weight of K2O, 3 wt% CaO, 4 wt% MgO, 1 wt% ZrO2And 12% by weight of B2O3
2. The method of claim 1, wherein the contacting is by immersion.
3. The method of claim 1, wherein the solution is carbon tetrachloride.
4. The impact-resistant tempered glass prepared by the method of any one of claims 1 to 3, wherein the impact-resistant tempered glass is subjected to a ball drop test using a steel ball having a diameter of 30mm and a mass of 120g, and the measured breaking height is not less than 615 mm; the surface stress of the impact-resistant toughened glass is more than or equal to 768 psi.
5. The impact-resistant tempered glass of claim 4, wherein the breaking height is 615mm to 630 mm; the surface stress was 768-.
6. The impact-resistant tempered glass of claim 4, wherein the impact-resistant tempered glass has a thickness of 0.1 to 3 mm.
7. A display terminal comprising a touch screen made of the impact-resistant tempered glass of any one of claims 4 to 6.
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Assignee: Xinjiang Huiguang Photoelectric Technology Co.,Ltd.

Assignor: DONGXU OPTOELECTRONIC TECHNOLOGY Co.,Ltd.

Contract record no.: X2024990000431

Denomination of invention: Impact resistant tempered glass and its preparation method and display terminal

Granted publication date: 20210323

License type: Common License

Record date: 20240828