CN111056749A - Chemical strengthening method for high-alumina glass - Google Patents
Chemical strengthening method for high-alumina glass Download PDFInfo
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- CN111056749A CN111056749A CN201911401764.0A CN201911401764A CN111056749A CN 111056749 A CN111056749 A CN 111056749A CN 201911401764 A CN201911401764 A CN 201911401764A CN 111056749 A CN111056749 A CN 111056749A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C21/00—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface
- C03C21/001—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions
- C03C21/002—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions to perform ion-exchange between alkali ions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B27/00—Tempering or quenching glass products
- C03B27/02—Tempering or quenching glass products using liquid
- C03B27/03—Tempering or quenching glass products using liquid the liquid being a molten metal or a molten salt
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
The invention relates to a chemical strengthening method of high-alumina glass, which comprises the following steps: 1. adding potassium nitrate into a tempering furnace to be melted into molten salt; 2. heating the glass sample to 380-450 ℃, immersing the glass sample into molten salt, preserving heat for 4-6 hours, and then putting the glass sample into hot water at 90 ℃ for quenching; 3. placing the glass sample in a muffle furnace, preserving heat for 0.5-1 h at 500-550 ℃, and then cooling to below 100 ℃; 5. and heating the glass sample to 380-450 ℃, immersing the glass sample into the potassium nitrate molten salt, keeping the temperature for 4-6 h, taking out the glass sample, and putting the glass sample into hot water at 90 ℃ for quenching. The invention has the beneficial effects that: the chemically strengthened glass of the present invention has a higher value of the depth of compressive stress layer by lowering the CS on the glass surface than in the prior art, and has a higher value of the CS at a deep position from the glass surface, and therefore has excellent scratch resistance and is less likely to crack. As a measure for reducing the breakage, it is effective to increase the stress depth of the end face so that the crack existing on the end face does not progress.
Description
Technical Field
The invention relates to chemically strengthened glass, in particular to chemically strengthened glass suitable for high-aluminum cover plate glass.
Background
In recent years, devices such as mobile phones (particularly smart phones), digital cameras, PDAs, touch panel displays, and large-sized televisions have been becoming increasingly popular.
Cover glass in these applications is mainly made of high alumina glass, which is chemically strengthened by ion exchange to improve strength. Such as: JP 2006-. In recent years, there have been increasing cases where chemically strengthened glass is used for exterior parts of digital signage, mice, smartphones, and the like, and in particular, chemically strengthened glass is used for cover glass of smartphones. However, there is no better solution for improving the impact resistance.
Disclosure of Invention
The invention aims to solve the problem that high-alumina glass in the prior art has insufficient impact resistance and is easy to damage, and provides a high-alumina glass chemical strengthening method.
The technical scheme provided by the invention for solving the technical problems is as follows:
the chemical strengthening method of the high-alumina glass is characterized by comprising the following steps:
(1) processing a glass sample into a preset size, edging, cleaning and drying;
(2) adding potassium nitrate with the purity of more than 95 percent into a tempering furnace, heating and melting into molten salt, and clarifying;
(3) heating the glass sample to 380-450 ℃ for preheating treatment;
(4) immersing the glass sample into the molten salt at 450-490 ℃, taking out after the heat preservation time is 4-6 h, and putting into water for quenching;
(5) putting the glass sample into a muffle furnace, preserving heat for 0.5-1 h at 500-550 ℃, and then cooling along with the furnace;
(6) heating the glass sample to 380-450 ℃ again for preheating treatment;
(7) and (3) immersing the glass sample into the potassium nitrate molten salt at the temperature of 400-490 ℃, keeping the temperature for 4-6 h, taking out, and placing into water for quenching.
The invention has the beneficial effects that:
the chemically strengthened glass of the present invention has a higher value of the depth of compressive stress layer by lowering the CS on the glass surface than in the prior art, and has a higher value of the CS at a deep position from the glass surface, and therefore has excellent scratch resistance and is less likely to crack. As a measure for reducing the breakage, it is effective to increase the stress depth of the end face so that the crack existing on the end face does not progress.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples
Example 1
Selecting high-alumina glass with the thickness of 0.7mm, cutting and edging the glass sheet, cleaning, putting the glass sheet into a preheating furnace for preheating treatment, wherein the preheating temperature is 380 ℃, heating along with the furnace and preserving heat for half an hour, then quickly transferring the glass sheet into molten salt, the molten salt comprises potassium nitrate with the purity of more than 95%, the molten salt temperature is 480 ℃, the ion exchange time is 4 hours, taking out the glass sheet after the exchange is finished, and testing the stress and stress layer depth value of the glass by using a stress tester.
And (3) putting the glass sheet into a muffle furnace for heat treatment at 490 ℃, preserving the heat for 0.5 hour, cooling along with the furnace, and testing the stress and the stress layer depth value of the glass by using a stress tester.
And cutting and edging the glass sheet, cleaning, placing the glass sheet into a preheating furnace for preheating treatment, wherein the preheating temperature is 380 ℃, the temperature is increased along with the furnace, the temperature is kept for half an hour, then the glass sheet is quickly transferred into molten salt, the temperature of the molten salt is 450 ℃, the ion exchange time is 3 hours, the glass sheet is taken out for quenching and cooling after the exchange is finished, and a stress tester is used for testing the stress and stress layer depth value of the glass. The molten salt component is potassium nitrate with purity of more than 95%.
Example 2
The present embodiment is different from embodiment 1 in that: the third step is ion exchange temperature and time of 420 ℃ for 4 h.
Example 3
The present embodiment is different from embodiment 1 in that: the third step is ion exchange temperature and time of 390 ℃ for 5h
Example 4
The present embodiment is different from embodiment 1 in that: the ion exchange temperature and time of the first step are 480 ℃ for 5h, and the heat treatment temperature and time of the second step are 500 ℃ for 1h
Example 5
The present embodiment is different from embodiment 1 in that: the ion exchange temperature and time of the first step are 480 ℃, 5h, the second heat treatment temperature and time are 500 ℃, 1h, the ion exchange temperature and time of the third step are 420 ℃ and 4h
Example 6
The present embodiment is different from embodiment 1 in that: the ion exchange temperature and time of the first step are 480 ℃ for 5h, the heat treatment temperature and time of the second step are 500 ℃ for 1h, and the ion exchange temperature and time of the third step are 390 ℃ for 5h
Comparative example 1
Substantially the same as in example 1, the difference from example 1 is that: the ion exchange temperature and time of the first step are 400 ℃ for 6h, the heat treatment temperature and time of the second step are 510 ℃ for 1h, and the ion exchange temperature and time of the third step are 420 ℃ for 3 h.
Comparative example 2
Substantially the same as in example 1, the difference from example 1 is that: the ion exchange temperature and time of the first step are 400 ℃ for 6h, the heat treatment temperature and time of the second step are 510 ℃ for 1h, and the ion exchange temperature and time of the third step are 420 ℃ for 4 h.
The comparison of the properties of the examples is shown in the attached Table 1.
TABLE 1 comparison of Properties of various glass samples
At one step temperature/time Workshop | One step stress CS Mpa | One step depth Dol. mu. m | Two step temperature/time Workshop | Two-step stress CS Mpa | Two step depth Dol. mu. m | Three step temperature/time Workshop | Three step stress CS Mpa | Three step depth Dol. mu m | |
Comparative example 1 | 400℃ 6h | 934.71 | 33.3786 | 510℃ 1h | 196.251 | 72.2522 | 420℃ 3h | 782.9136 | 55.6944 |
Comparative example 2 | 400℃ 6h | 939.4104 | 34.7788 | 510℃ 1h | 184.8512 | 73.5812 | 420℃ 4h | 789.0116 | 57.6808 |
Examples 1 | 480℃ 4h | 738.5286 | 69.021 | 490℃ 0.5h | 385.4504 | 89.5144 | 450℃ 3h | 648.2046 | 82.5548 |
Examples 2 | 480℃ 4h | 728.778 | 69.2546 | 490℃ 0.5h | 391.1516 | 89.2224 | 420℃ 4h | 629.1698 | 84.1654 |
Examples 3 | 480℃ 4h | 734.572 | 69.4968 | 490℃ 0.5h | 389.1134 | 88.5078 | 390℃ 5h | 611.1502 | 82.0116 |
Examples 4 | 480℃ 5h | 736.791 | 67.1542 | 500℃ 1h | 360.1022 | 97.8078 | 450℃ 3h | 667.7944 | 82.8482 |
Examples 5 | 480℃ 5h | 747.7482 | 71.2564 | 500℃ 1h | 371.7828 | 96.8458 | 420℃ 4h | 655.9436 | 90.209 |
Examples 6 | 480℃ 5h | 743.0982 | 71.7422 | 500℃ 1h | 382.5098 | 95.2252 | 390℃ 5h | 633.0788 | 86.4556 |
Although the preferred embodiments and examples have been described in detail above, the present invention is not limited to the embodiments and examples described above, and various modifications and substitutions may be made thereto without departing from the scope of the claims. The above embodiments can be combined as appropriate.
Claims (1)
1. The chemical strengthening method of the high-alumina glass is characterized by comprising the following steps:
(1) processing a glass sample into a preset size, edging, cleaning and drying;
(2) adding potassium nitrate with the purity of more than 95 percent into a tempering furnace, heating to 400 ℃, melting into molten salt, clarifying and keeping the temperature;
(3) heating the glass sample to 380-450 ℃ for preheating treatment;
(4) heating the molten salt to 450-490 ℃ and keeping the temperature;
(5) immersing the glass sample into the molten salt at 450-490 ℃, keeping the temperature for 4-6 h, taking out, and putting into hot water at 90 ℃ for quenching;
(6) putting the glass sample into a muffle furnace, preserving heat for 0.5-1 h at 500-550 ℃, and then cooling to below 100 ℃ along with the furnace;
(7) heating the glass sample to 380-450 ℃ again for preheating treatment;
(8) adjusting the temperature of the molten salt to 400-490 ℃ and keeping the temperature;
(9) and (3) immersing the glass sample into the potassium nitrate molten salt again, keeping the temperature for 4-6 h, taking out, and putting into hot water at 90 ℃ for quenching.
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Cited By (2)
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CN111995261A (en) * | 2020-08-12 | 2020-11-27 | 咸宁南玻光电玻璃有限公司 | Method for manufacturing ultrathin glass substrate |
CN115159857A (en) * | 2022-07-27 | 2022-10-11 | 河北视窗玻璃有限公司 | Manufacturing method of concave display curved glass with AG function |
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CN106007405A (en) * | 2015-03-27 | 2016-10-12 | 旭硝子株式会社 | Chemically strengthened glass manufacturing method and chemically strengthened glass |
CN106608713A (en) * | 2015-10-27 | 2017-05-03 | 蓝思科技股份有限公司 | Method for removing surface compressive stress of toughened glass through chemical ion exchange |
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CN107840570A (en) * | 2017-10-26 | 2018-03-27 | 中国南玻集团股份有限公司 | Alumina silicate glass and preparation method thereof, electronic equipment |
CN108069624A (en) * | 2016-11-11 | 2018-05-25 | 蓝思科技股份有限公司 | A kind of reinforcing process method of glass |
CN109502991A (en) * | 2018-12-18 | 2019-03-22 | 北京工业大学 | A kind of method that air heating condition improves chemically reinforced glass ion exchange depth |
CN110316974A (en) * | 2019-05-31 | 2019-10-11 | 彩虹集团(邵阳)特种玻璃有限公司 | One kind alumina silicate glass containing alkali and its product, intensifying method and application |
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2019
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Patent Citations (8)
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US20130202715A1 (en) * | 2009-12-11 | 2013-08-08 | Schott Glass Technologies (Suzhou) Co., Ltd. | Aluminosilicate glass for touch screen |
CN106007405A (en) * | 2015-03-27 | 2016-10-12 | 旭硝子株式会社 | Chemically strengthened glass manufacturing method and chemically strengthened glass |
CN106608713A (en) * | 2015-10-27 | 2017-05-03 | 蓝思科技股份有限公司 | Method for removing surface compressive stress of toughened glass through chemical ion exchange |
CN108069624A (en) * | 2016-11-11 | 2018-05-25 | 蓝思科技股份有限公司 | A kind of reinforcing process method of glass |
CN107324649A (en) * | 2017-06-29 | 2017-11-07 | 四川旭虹光电科技有限公司 | Glass through chemical enhanced anti-dazzle glas and non-glare treated |
CN107840570A (en) * | 2017-10-26 | 2018-03-27 | 中国南玻集团股份有限公司 | Alumina silicate glass and preparation method thereof, electronic equipment |
CN109502991A (en) * | 2018-12-18 | 2019-03-22 | 北京工业大学 | A kind of method that air heating condition improves chemically reinforced glass ion exchange depth |
CN110316974A (en) * | 2019-05-31 | 2019-10-11 | 彩虹集团(邵阳)特种玻璃有限公司 | One kind alumina silicate glass containing alkali and its product, intensifying method and application |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111995261A (en) * | 2020-08-12 | 2020-11-27 | 咸宁南玻光电玻璃有限公司 | Method for manufacturing ultrathin glass substrate |
CN115159857A (en) * | 2022-07-27 | 2022-10-11 | 河北视窗玻璃有限公司 | Manufacturing method of concave display curved glass with AG function |
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