CN110981220A - Chemical toughening method for glass - Google Patents
Chemical toughening method for glass Download PDFInfo
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- CN110981220A CN110981220A CN201911389904.7A CN201911389904A CN110981220A CN 110981220 A CN110981220 A CN 110981220A CN 201911389904 A CN201911389904 A CN 201911389904A CN 110981220 A CN110981220 A CN 110981220A
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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
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Abstract
The invention discloses a chemical toughening method for glass, which mainly comprises the following steps: preheating aluminosilicate glass at 100-300 ℃ for 1-3 h; immersing the primary preheating piece into first molten salt, and carrying out primary ion exchange for 5-6h at the temperature of 410-; lifting the first tempering piece and dripping salt for 10-20 min; annealing the first toughened part for 2-3h to reduce the temperature to below 100 ℃; standing the first annealing piece for 10-30min, and preheating again at 100-300 ℃ for 1-3 h; immersing the second preheating part into second molten salt, and carrying out first ion exchange for 10-20min at the temperature of 380-; lifting the second tempering piece for 10-20 min; and (5) performing direct-falling annealing on the secondary toughened part to finish toughening. According to the invention, the thickness of the stress layer is increased by adopting higher temperature in the first toughening, and the surface stress is increased by adopting lower temperature and annealing direct-falling mode in the second toughening, so that the strength is ensured, meanwhile, the time required by toughening is greatly shortened, the frequent replacement of molten salt is avoided, the cost is reduced, and the efficiency is improved.
Description
Technical Field
The invention relates to a chemical toughening method for glass, and belongs to the technical field of glass preparation.
Background
With the continuous increase of smart phone screens, glass becomes one of important structural members in the structural design of the whole smart phone. In a destructive experiment process, the condition that the touch glass cover plate is broken frequently occurs in a complete machine drop test, the theoretical strength of common plate glass is more than 10000MPa, but a test result shows that the actual strength of the glass is only 30-80 MPa. Factors influencing the actual strength of the glass, such as storage environment, surface machining, sample size, mechanical scratches, and internal defects such as bubbles, stones, and the like, wherein the existence of microcracks has the greatest influence on the actual strength of the glass, particularly microcracks on the outer surface of the glass. The causes of microcrack generation can be summarized as internal defects, surface reactions, and surface wear. The occurrence of microcracks can affect the surface strength of the whole machine and cause the defects of the glass such as cracking, chipping and the like. The existing method for enhancing the strength of glass adopts a physical toughening method or a chemical toughening method, and the chemical toughening method is mainly used for immersing the glass into a chemical solution, so that ions with smaller radius in the glass exchange with ions with larger radius in the chemical solution, and the pressure stress is formed in the glass by utilizing the difference of the ion volume, so that the pressure resistance is enhanced. The existing chemical toughening method is long in time consumption, and used chemical solution needs to be replaced frequently.
Disclosure of Invention
The invention aims to solve the problem of providing a chemical toughening method for glass, which is used for enhancing the surface strength of the glass and reducing the defects of micro-cracks and the like during toughening; meanwhile, the molten salt replacement is reduced, and the tempering time is shortened.
The technical scheme of the invention is as follows: a chemical toughening method for glass mainly comprises the following steps:
(1) preheating for the first time: placing the aluminosilicate glass in a preheating furnace in automatic toughening furnace equipment, and preheating for 1-3h at the temperature of 100-300 ℃ to obtain a first preheating piece;
(2) first tempering: immersing the primary preheating piece into first molten salt of a toughening furnace of automatic toughening furnace equipment, and carrying out primary ion exchange for 5-6h at the temperature of 410-420 ℃ to obtain a primary toughening piece;
(3) first salt dropping: lifting the first tempering piece and dripping salt for 10-20 min;
(4) first annealing: after salt dripping is finished, the first tempered piece is moved into an annealing furnace of tempering furnace equipment, annealing is carried out for 2-3h, the temperature is reduced to be below 100 ℃, and the first tempered piece is obtained after discharging;
(5) preheating for the second time: standing the first annealing piece for 10-30min, placing the first annealing piece into a preheating furnace in automatic toughening furnace equipment again, and preheating for 1-3h at the temperature of 100-300 ℃ to obtain a second preheating piece;
(6) and (3) tempering for the second time: immersing the secondary preheating piece into a second molten salt of a toughening furnace of the automatic toughening furnace equipment, and performing primary ion exchange for 10-20min at the temperature of 380-;
(7) and (4) dripping salt for the second time: lifting the second tempering piece for 10-20 min;
(8) and (3) second annealing: and after the salt dripping is finished, moving the secondary toughening piece to an annealing furnace of toughening furnace equipment for direct falling annealing, and finishing the toughening operation.
The first molten salt is potassium nitrate molten salt containing sodium ions, wherein the sodium ions account for 0-0.6 wt% of the total amount of metal ions; the second molten salt is potassium nitrate molten salt containing sodium ions, wherein the sodium ions account for 0wt% -0.2wt% of the total amount of the metal ions.
The toughening furnace equipment is a full-automatic integrated toughening furnace and comprises a preheating furnace, a toughening furnace and an annealing furnace.
And (4) the annealing furnace is directly exposed in air and cooled to normal temperature.
According to the traditional chemical strengthening method, after glass is placed in molten salt for ion exchange, small-radius ions in the glass replace large-radius ions in the molten salt, the large-radius ions in the molten salt are replaced in the glass, the small-radius ions in the glass are replaced out of the molten salt and enter the molten salt, the concentration of the small-radius ions in the molten salt is increased, the ion exchange speed is reduced after the concentration of the small-radius ions is increased, the efficiency is reduced, the surface stress of the glass is reduced by continuously using the molten salt, the requirement cannot be met, and usually, when the small-radius ions in the molten salt account for more than 0.3 wt% of the total amount of metal ions, the molten salt needs to be replaced. When ion exchange is carried out, the surface stress of the glass needs to be kept, the stress layer thickness of the glass needs to be ensured, and the tempering effect is achieved only when the stress layer thickness is larger than the depth of the surface crack of the glass. Certain temperature and ion exchange time need to be ensured to reach certain stress layer thickness, the higher the temperature is, the shorter the required time is, but the higher the temperature is, the more serious the stress relaxation is, and the product after molten salt decomposition at high temperature can erode the glass surface, thereby affecting the ion exchange effect.
By adopting the method, two times of toughening are respectively carried out in two kinds of molten salts, the first time of toughening is used for improving the depth of the stress layer, so that the exchange depth of sodium ions and potassium ions in the stress layer is deeper than the depth of microcracks, and the molten salts with the sodium ions accounting for more than 0.3 wt% of the total amount of metal ions can be continuously used without replacement. Performing first ion exchange in first molten salt with sodium ions accounting for 0-0.6 wt% of the total amount of metal ions to reach the required depth of the stress layer, transferring the glass to second molten salt with sodium ions accounting for 0-0.2 wt% of the total amount of metal ions for secondary toughening, wherein the second ion exchange is used for improving surface stress and increasing surface strength to meet the requirement of the surface stress strength.
Because the sodium ions are immersed into the second molten salt for the second ion exchange after the first ion exchange of the first molten salt, the concentration of the sodium ions entering the second molten salt is relatively low in the second ion exchange, and the service life of the second molten salt can be prolonged. In addition, when the total amount of the metal ions in the second molten salt is more than 0.2wt%, the sodium ions can be continuously used as the first molten salt, and the recycling rate of the molten salt is increased. That is, the molten salt in which the sodium ions account for less than 0.2wt% of the total amount of the metal ions can be used as the second molten salt, and after the molten salt is used for a period of time and the sodium ions account for more than 0.2wt% of the total amount of the metal ions, the molten salt can be used as the first molten salt until the sodium ions in the first molten salt account for more than 0.6wt% of the total amount of the metal ions, and then the molten salt can be replaced. Therefore, by adopting the method for carrying out two times of toughening in two kinds of molten salts, the service life of the molten salts is greatly prolonged while the toughening strength of the glass is ensured. After the cracks are reduced, the edge sand edge, the opening breakage and the poor splintering of the aluminosilicate glass are reduced. And (2) direct falling annealing, namely, after salt is dripped in the toughening furnace, the glass is moved to an annealing furnace and is directly exposed in the air, so that the outer layer of the glass shrinks less and the inner layer of the glass shrinks more in the cooling process, and after the glass is cooled to normal temperature, the glass is in a state that the inner layer is pulled and the outer layer is pressed, so that the glass has better strength.
According to the method, two times of toughening and direct-falling annealing after the second time of toughening are respectively carried out in two kinds of molten salts, namely the stress layer thickness is increased by adopting a higher temperature for the first time of toughening, and the surface stress is increased by adopting a lower temperature and annealing direct-falling mode for the second time of toughening, so that the strength of glass is effectively increased, frequent replacement of the molten salts is avoided, the cost is reduced, and the efficiency is improved. The required strength is ensured, the time required by one-time toughening is greatly shortened, and the working hour of toughening is integrally shortened.
Detailed Description
Example one
(1) Preheating for the first time: placing glass to be tempered with the thickness of 0.55mm in a preheating furnace in automatic tempering furnace equipment, and preheating for 1h at the temperature of 300 ℃ to obtain a first preheating piece;
(2) first tempering: immersing the first preheating piece into potassium nitrate molten salt of a toughening furnace of automatic toughening furnace equipment, wherein sodium ions account for 0wt% of the total amount of metal ions, and performing first ion exchange for 6 hours at the temperature of 410 ℃ to obtain a first toughening piece;
(3) first salt dropping: lifting the first tempering piece for 10 min;
(4) first annealing: after salt dripping is finished, the first tempered piece is moved into an annealing furnace of tempering furnace equipment, annealing is carried out for 2 hours, the temperature is reduced to be lower than 100 ℃, and the first tempered piece is obtained after discharging;
(5) preheating for the second time: standing the first annealing piece for 10min, placing the first annealing piece into a preheating furnace in automatic toughening furnace equipment again, and preheating for 3h at the temperature of 100 ℃ to obtain a second preheating piece;
(6) and (3) tempering for the second time: immersing the secondary preheating piece into a potassium nitrate molten salt of a toughening furnace of the automatic toughening furnace equipment, wherein sodium ions account for 0wt% of the total amount of metal ions, and performing primary ion exchange for 20min at the temperature of 380 ℃ to obtain a secondary toughening piece;
(7) and (4) dripping salt for the second time: lifting the second tempering piece for 20 min;
(8) and (3) second annealing: and after the salt dripping is finished, moving the secondary toughening piece to an annealing furnace of toughening furnace equipment for direct falling annealing, and finishing the toughening operation.
Example two
(1) Preheating for the first time: placing glass with the thickness of 0.55mm to be tempered in a preheating furnace in automatic tempering furnace equipment, and preheating for 3 hours at the temperature of 100 ℃ to obtain a first preheating piece;
(2) first tempering: immersing the first preheating piece into potassium nitrate molten salt of a toughening furnace of automatic toughening furnace equipment, wherein sodium ions account for 0.6wt% of the total amount of metal ions, and carrying out first ion exchange for 5 hours at the temperature of 420 ℃ to obtain a first toughening piece;
(3) first salt dropping: lifting the first tempering piece and dripping salt for 20 min;
(4) first annealing: after salt dripping is finished, the first tempered piece is moved into an annealing furnace of tempering furnace equipment, annealing is carried out for 3 hours, the temperature is reduced to be lower than 100 ℃, and the first tempered piece is obtained after discharging;
(5) preheating for the second time: standing the first annealing piece for 30min, placing the first annealing piece into a preheating furnace in automatic toughening furnace equipment again, and preheating for 1h at the temperature of 300 ℃ to obtain a second preheating piece;
(6) and (3) tempering for the second time: immersing the secondary preheating piece into a potassium nitrate molten salt of a toughening furnace of the automatic toughening furnace equipment, wherein sodium ions account for 0.2% of the total amount of metal ions, and carrying out primary ion exchange for 10min at the temperature of 400 ℃ to obtain a secondary toughening piece;
(7) and (4) dripping salt for the second time: lifting the secondary tempering piece for 10 min;
(8) and (3) second annealing: and after the salt dripping is finished, moving the secondary toughening piece to an annealing furnace of toughening furnace equipment for direct falling annealing, and finishing the toughening operation.
EXAMPLE III
This example is comparative example one
(1) Preheating: corning 2320 glass with the thickness of 0.55mm to be tempered is put into a preheating furnace and preheated for 3 hours at the temperature of 200 ℃.
(2) Tempering: the preheated Corning 2320 glass was transferred to a tempering furnace containing molten salt (potassium nitrate containing 0.1% of sodium ions), and ion-exchanged at 420 ℃ for 6h30 min.
(3) And (4) salt dropping: dripping salt into toughened Corning 2320 glass for 30min
(4) Annealing: the Corning 2320 glass after dropping salt is transferred to an annealing furnace, slowly cooled to 320 ℃, and discharged for salt washing test after 3.5 hours.
Example four
This example is comparative example No. 2
(1) Preheating: NEG T2X-1 glass with the thickness of 0.55mm to be toughened is put into a preheating furnace and preheated for 2 hours at the temperature of 300 ℃.
(2) Tempering: the preheated NEG T2X-1 glass was transferred to a tempering furnace containing molten salt (potassium nitrate containing 0.1% of sodium ions), and ion-exchanged at 430 ℃ for 5h30 min.
(3) And (4) salt dropping: adding salt into the toughened NEG T2X-1 glass for 30min
(4) Annealing: transferring the NEG T2X-1 glass after dropping the salt to an annealing furnace, slowly cooling to 320 ℃, discharging for 3h, and carrying out a salt washing test.
The results of the surface stress CS, the stress layer depth Dol, the central layer tension CT, the tempering area per KG of potassium nitrate, the tempering time per sheet, and the B10 bending strength test of the first and third examples are shown in table 1.
The results of the surface stress CS, the stress layer depth Dol, the central layer tension CT, the tempering area per KG of potassium nitrate, the tempering time per sheet and the B10 bending strength test of the second and fourth examples are shown in table 1.
The CS/Dol/CT test is carried out by adopting a stress tester, and the B10 bending strength test is carried out by adopting a 4PB tester. In tables 1 and 2, CS means surface stress, DOL means stress layer depth, CT means center tension, and B10 means four-bar bending strength.
It can be seen from tables 1 and 2 that the CS value, DOL value, CT value, and B10 value of the glass of either example one or example two, after the secondary tempering and down annealing treatment, are all greater than those of the comparative example in which only the primary tempering treatment was performed. The strength of the glass is greatly improved after the secondary tempering.
The first molten salt of the first embodiment and the second embodiment has the sodium ion content of more than 0.4 percent, and can achieve good strengthening effect, while the sodium ion content of the molten salt of the comparative example 1 and the comparative example 2 needs to be controlled within 0.2 percent, and the molten salt of the comparative example 1 and the comparative example 2 needs to be replaced after a batch of glass is treated.
In the first embodiment, the second embodiment, the third embodiment and the fourth embodiment, the toughening time of the former is at least 30% higher than that of the latter.
TABLE 1
TABLE 2
Claims (4)
1. A chemical toughening method for glass is characterized in that: the method mainly comprises the following steps:
(1) preheating for the first time: placing the aluminosilicate glass in a preheating furnace in automatic toughening furnace equipment, and preheating for 1-3h at the temperature of 100-300 ℃ to obtain a first preheating piece;
(2) first tempering: immersing the primary preheating piece into first molten salt of a toughening furnace of automatic toughening furnace equipment, and carrying out primary ion exchange for 5-6h at the temperature of 410-420 ℃ to obtain a primary toughening piece;
(3) first salt dropping: lifting the first tempering piece and dripping salt for 10-20 min;
(4) first annealing: after salt dripping is finished, the first tempered piece is moved into an annealing furnace of tempering furnace equipment, annealing is carried out for 2-3h, the temperature is reduced to be below 100 ℃, and the first tempered piece is obtained after discharging;
(5) preheating for the second time: standing the first annealing piece for 10-30min, placing the first annealing piece into a preheating furnace in automatic toughening furnace equipment again, and preheating for 1-3h at the temperature of 100-300 ℃ to obtain a second preheating piece;
(6) and (3) tempering for the second time: immersing the secondary preheating piece into a second molten salt of a toughening furnace of the automatic toughening furnace equipment, and performing primary ion exchange for 10-20min at the temperature of 380-;
(7) and (4) dripping salt for the second time: lifting the second tempering piece for 10-20 min;
(8) and (3) second annealing: and after the salt dripping is finished, moving the secondary toughening piece to an annealing furnace of toughening furnace equipment for direct falling annealing, and finishing the toughening operation.
2. A method of chemically tempering glass according to claim 1, wherein: the first molten salt is potassium nitrate molten salt containing sodium ions, wherein the sodium ions account for 0-0.6 wt% of the total amount of metal ions; the second molten salt is potassium nitrate molten salt containing sodium ions, wherein the sodium ions account for 0wt% -0.2wt% of the total amount of the metal ions.
3. A method of chemically tempering glass according to claim 2, wherein: the toughening furnace equipment is a full-automatic integrated toughening furnace and comprises a preheating furnace, a toughening furnace and an annealing furnace.
4. A method of chemically tempering glass according to claim 3, wherein: and (4) the annealing furnace is directly exposed in air and cooled to normal temperature.
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| CN112745016A (en) * | 2020-12-24 | 2021-05-04 | 安徽立光电子材料股份有限公司 | Pretreatment method before film coating of 0.10mm glass |
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| CN113213776A (en) * | 2021-06-22 | 2021-08-06 | 东莞市亮成电子有限公司 | Strengthening method for strong glass |
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Cited By (6)
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| CN113060943A (en) * | 2021-03-23 | 2021-07-02 | 蓝思科技（长沙）有限公司 | Ultra-thin glass strengthening method, ultra-thin glass, flexible screen and equipment |
| CN113213776A (en) * | 2021-06-22 | 2021-08-06 | 东莞市亮成电子有限公司 | Strengthening method for strong glass |
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Application publication date: 20200410 |