CN103553354B - The preparation method of one side toughened glass - Google Patents
The preparation method of one side toughened glass Download PDFInfo
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- CN103553354B CN103553354B CN201310530154.7A CN201310530154A CN103553354B CN 103553354 B CN103553354 B CN 103553354B CN 201310530154 A CN201310530154 A CN 201310530154A CN 103553354 B CN103553354 B CN 103553354B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
Abstract
A preparation method for one side toughened glass, comprises the steps: to provide pending glass; Protective membrane is formed in a surface-coated layer of protecting liquid of described glass; By the glass preheating 15 ~ 100 minutes under 270 DEG C ~ 370 DEG C conditions being coated with protective membrane; Fused salt glass after preheating being put into 390 DEG C ~ 440 DEG C reacts 3 ~ 8 hours; Reacted glass is carried out anneal, obtains one side toughened glass.The preparation method of above-mentioned one side toughened glass; after a surface-coated protection liquid of pending glass forms protective membrane; protective membrane can prevent the surface of the glass being coated with protective membrane from the fused salt of high temperature, carrying out ion-exchange; ion exchange reaction can only be carried out on the surface of the glass of uncoated protective membrane, thus obtains one side toughened glass.The preparation method of above-mentioned one side toughened glass only needs can enter protection at a surface-coated layer protecting film of glass, does not need to carry out ion exchange reaction in the effect of extra electric field, lower to equipment requirements.
Description
Technical field
The present invention relates to toughened glass preparation field, particularly relate to a kind of preparation method of one side toughened glass.
Background technology
Along with the fast development of electronic information technology industry, the requirement of ultra-thin glass is increasing, is widely used and mobile phone and field of display.In order to solve the more weak problem of ultra-thin glass mechanical strength, toughened glass is widely used.The surface of toughened glass has one deck compressive stress layer, have higher ultimate compression strength, when glass is subject to External Force Acting, stressor layers effectively can avoid glass breaking.But toughened glass is when using, not easily processes, cut toughened glass, breakage that the technique such as grinding easily causes toughened glass, meanwhile, the intensity of glass can reduce a lot, reduces and processes yield.But one side toughened glass when not affecting glass outer surface tempering intensity, can be processed the one side of the non-tempering of glass, reducing difficulty of processing, improving product yield.
General, preparation method's persevering piezoelectric field assistant chemical tempering method, the non-uniform electric field assisting ion of one side toughened glass exchange tempering method etc.The method of electric field-assisted chemical tempering is adopted to need to add electric field at the two ends of fused salt groove, higher to equipment requirements.
Summary of the invention
Based on this, be necessary the preparation method that a kind of one side toughened glass lower to equipment requirements is provided.
A preparation method for one side toughened glass, comprises the steps:
Pending glass is provided;
Protective membrane is formed in a surface-coated layer of protecting liquid of described glass;
By the glass preheating 15 ~ 100 minutes under 270 DEG C ~ 370 DEG C conditions being coated with protective membrane;
Fused salt glass after preheating being put into 390 DEG C ~ 440 DEG C reacts 3 ~ 8 hours;
Reacted glass is carried out anneal, obtains one side toughened glass.
Wherein in an embodiment, a described surface-coated layer of protecting liquid at described glass is formed in the operation of protective membrane, adopts roller painting to apply described protection liquid.
Wherein in an embodiment, the thickness of described protective membrane is 3 μm ~ 8 μm.
Wherein in an embodiment, described fused salt is saltpetre fused salt.
Wherein in an embodiment, described protection liquid comprises each component of following mass percentage:
Wherein in an embodiment, described protection liquid comprises each component of following mass percentage:
Wherein in an embodiment, in the mixture of described metasilicic acid and two silicic acid, the mass ratio of metasilicic acid and two silicic acid is 1:1 ~ 10.
Wherein in an embodiment, described water soluble alkali is sodium hydroxide, potassium hydroxide, sodium carbonate or sodium bicarbonate.
Wherein in an embodiment, the thickness of described pending glass is 0.2mm ~ 1.1mm.
Wherein in an embodiment, the temperature of described preheating is 350 DEG C.
The preparation method of above-mentioned one side toughened glass; after a surface-coated protection liquid of pending glass forms protective membrane; protective membrane can prevent the surface of the glass being coated with protective membrane from the fused salt of high temperature, carrying out ion-exchange; ion exchange reaction can only be carried out on the surface of the glass of uncoated protective membrane, thus obtains one side toughened glass.The preparation method of above-mentioned one side toughened glass only needs can enter protection at a surface-coated layer protecting film of glass, does not need to carry out ion exchange reaction in the effect of extra electric field, lower to equipment requirements.
Accompanying drawing explanation
Fig. 1 is the schema of the preparation method of the one side toughened glass of an embodiment.
Embodiment
For enabling above-mentioned purpose of the present invention, feature and advantage become apparent more, are described in detail the specific embodiment of the present invention below in conjunction with accompanying drawing.Set forth a lot of detail in the following description so that fully understand the present invention.But the present invention can be much different from alternate manner described here to implement, those skilled in the art can when without prejudice to doing similar improvement when intension of the present invention, therefore the present invention is by the restriction of following public concrete enforcement.
As shown in Figure 1, the preparation method of the one side toughened glass of an embodiment, comprises the steps:
S10, provide pending glass.
Pending glass can be ultra-thin glass or sheet glass.The thickness of ultra-thin glass can be 0.2mm ~ 1.1mm.The surface of pending glass can deposit one deck conductive layer.The material of conductive layer can be tin indium oxide (IndiumTinOxides, ITO) etc.First glass was carried out cleaning and drying before painting protection liquid.
S20, form protective membrane in surface-coated layer of protecting liquid of glass.
In the present embodiment, protect liquid to comprise each component of following mass percentage: the metasilicic acid of 0.7% ~ 42% and the mixture of two silicic acid, 0.1% ~ 48% disilicic acid, 0.1% ~ 5% water soluble alkali, the acetone of 0.5% ~ 30%, the ethanol of 0.5% ~ 40% and surplus water.Wherein, in the mixture of metasilicic acid and two silicic acid, the mass ratio of metasilicic acid and two silicic acid can be 1:1 ~ 10, in actual applications, can regulate the mass ratio of metasilicic acid and two silicic acid as required.In the present embodiment, water soluble alkali is sodium hydroxide.In other embodiments, water soluble alkali can also be potassium hydroxide, sodium carbonate or sodium bicarbonate.
In one embodiment, protect liquid to comprise each component of following mass percentage: the metasilicic acid of 0.9% ~ 15% and the mixture of two silicic acid, 0.9% ~ 15% disilicic acid, 0.1% ~ 3% water soluble alkali, the acetone of 18% ~ 30%, the ethanol of 15% ~ 30% and surplus water.
In a preferred embodiment, protect liquid to comprise each component of following mass percentage: the metasilicic acid of 0.9% and the mixture of two silicic acid, 0.3% disilicic acid, 0.1% water soluble alkali, the acetone of 5%, the ethanol of 18% and surplus water.Now, the reaction of metasilicic acid, two silicic acid, disilicic acid and water soluble alkali is comparatively complete, and the viscosity of the protection liquid obtained is better.
In the present embodiment, roller painting can be adopted to form protective membrane in a surface-coated layer of protecting liquid of glass.The quality of protective membrane adopting roller painting coating to be formed is good, homogeneous, and roller painting to have working efficiency high, the advantages such as environmental pollution is little.Certainly, in other embodiments, additive method can also be adopted to form protective membrane in a surface-coated layer of protecting liquid of glass.
In the present embodiment, the thickness of the protective membrane of formation can be 3 μm ~ 8 μm.
S30, glass preheating 15 ~ 100 minutes under 270 DEG C ~ 370 DEG C conditions that will protective membrane be coated with.
In one embodiment, glass preheating 30 minutes under 350 DEG C of conditions that can will be coated with protective membrane.The glass being coated with protective membrane is carried out preheating to be cured protective membrane.
S40, the glass after preheating put into the fused salt reaction 3 ~ 8 hours of 390 DEG C ~ 440 DEG C.
In the present embodiment, fused salt can be saltpetre fused salt.In other embodiments, according to the character of the one side toughened glass that will prepare, in fused salt, appropriate potassium hydroxide and aluminium sesquioxide etc. can also be added.Glass after preheating is put into the fused salt of 390 DEG C ~ 440 DEG C, do not have the potassium ion in the metal ion on the surface of the glass of coating protective film and fused salt to carry out ion-exchange.Utilize the difference on basic ion volume to form embedded squeezing stress on the top layer of glass, form compressive stress layer on the surface of glass, thus reduce the impact of glass surface crackle, improve the intensity of glasswork.
S50, reacted glass is carried out anneal, obtain one side toughened glass.
After glass carries out ion exchange reaction, slowly taken out by glass from fused salt, the annealing furnace putting into temperature identical or close with temperature of molten salt is annealed to room temperature.
The preparation method of above-mentioned one side toughened glass; after a surface-coated protection liquid of pending glass forms protective membrane; protective membrane can prevent the surface of the glass being coated with protective membrane from the fused salt of high temperature, carrying out ion-exchange; ion exchange reaction can only be carried out on the surface of the glass of uncoated protective membrane, thus obtains one side toughened glass.The preparation method of above-mentioned one side toughened glass only needs can enter protection at a surface-coated layer protecting film of glass, does not need to carry out ion exchange reaction in the effect of extra electric field, lower to equipment requirements.Meanwhile, this preparation method is simple to operate, is easy to realize.
Be specific embodiment part below.
Embodiment 1
The mixture of 3g metasilicic acid and two silicic acid, 0.5g disilicic acid, 0.2g sodium hydroxide, 20g acetone, 30g ethanol and 110g water are mixed, wherein, the mixture of metasilicic acid and two silicic acid comprises the metasilicic acid of 1g and two silicic acid of 2g, obtains protecting liquid.
Dry after being had by a surface deposition Asahi glass cleaning of conductive layer clean, then form protective membrane at the above-mentioned protection liquid of surface-coated one deck of depositing conducting layer that do not have of glass.Then, the glass preheating 30 minutes under 350 DEG C of conditions will protective membrane being coated with.Afterwards glass after preheating is put into the fused salt reaction 3 hours of 400 DEG C, then glass is slowly taken out from fused salt, put into temperature and the close annealing furnace of temperature of molten salt is annealed to room temperature, obtain one side toughened glass.
The protective membrane on removing one side toughened glass surface and other pollutents are then clean by ultrasonic cleaning.The one side toughened glass cleaned up is adopted two interference technique test surfaces stress and exchanges the degree of depth, the instrument used is FSM-60LE measuring stress instrument.The experimental data obtained is as follows:
The test result of the glass surface of non-depositing conducting layer:
Exchange stress (Cs): 519Mpa.
The exchange degree of depth (DOL) of stressor layers: the upper limit: 10.3 μm, lower limit: 9.8 μm.
, without interference fringe, not there is chemical exchange, there is no tempering in the test result on the surface of conductive layer: test less than data.
Embodiment 2
The mixture of 1.1g metasilicic acid and two silicic acid, 37.5g disilicic acid, 7.5g sodium carbonate, 0.75g acetone, 60g ethanol and 46.2g water are mixed; wherein; the mixture of metasilicic acid and two silicic acid comprises the metasilicic acid of 0.3g and two silicic acid of 0.8g, obtains protecting liquid.
Dry after being had by a surface deposition Asahi glass cleaning of conductive layer clean, then form protective membrane at the above-mentioned protection liquid of surface-coated one deck of conductive layer.Then, the glass preheating 100 minutes under 270 DEG C of conditions will protective membrane being coated with.Afterwards glass after preheating is put into the fused salt reaction 8 hours of 390 DEG C, then glass is slowly taken out from fused salt, put into temperature and the close annealing furnace of temperature of molten salt is annealed to room temperature, obtain one side toughened glass.
The protective membrane on removing one side toughened glass surface and other pollutents are then clean by ultrasonic cleaning.The one side toughened glass cleaned up is adopted two interference technique test surfaces stress and exchanges the degree of depth, the instrument used is FSM-60LE measuring stress instrument.The experimental data obtained is as follows:
The test result on the surface of conductive layer:
Exchange stress (Cs): 516Mpa.
The exchange degree of depth (DOL) of stressor layers: the upper limit: 10.5 μm, lower limit: 9.7 μm.
, without interference fringe, not there is chemical exchange, there is no tempering in the test result of the glass surface of non-depositing conducting layer: test less than data.
Embodiment 3
The mixture of 63g metasilicic acid and two silicic acid, 0.15g disilicic acid, 0.15g potassium hydroxide, 45g acetone, 0.75g ethanol and 41g water are mixed; wherein; the mixture of metasilicic acid and two silicic acid comprises the metasilicic acid of 31.5g and two silicic acid of 31.5g, obtains protecting liquid.
Dry after being had by a surface deposition SodaLime glass cleaning of conductive layer clean, then form protective membrane at the above-mentioned protection liquid of surface-coated one deck of conductive layer.Then, the glass preheating 15 minutes under 370 DEG C of conditions will protective membrane being coated with.Afterwards glass after preheating is put into the fused salt reaction 5 hours of 440 DEG C, then glass is slowly taken out from fused salt, put into temperature and the close annealing furnace of temperature of molten salt is annealed to room temperature, obtain one side toughened glass.
The protective membrane on removing one side toughened glass surface and other pollutents are then clean by ultrasonic cleaning.The one side toughened glass cleaned up is adopted two interference technique test surfaces stress and exchanges the degree of depth, the instrument used is FSM-60LE measuring stress instrument.The experimental data obtained is as follows:
The test result on the surface of conductive layer:
Exchange stress (Cs): 523Mpa.
The exchange degree of depth (DOL) of stressor layers: the upper limit: 10.6 μm, lower limit: 10.0 μm.
, without interference fringe, not there is chemical exchange, there is no tempering in the test result of the glass surface of non-depositing conducting layer: test less than data.
Embodiment 4
The mixture of 0.15g metasilicic acid and two silicic acid, 0.45g disilicic acid, 0.15g sodium bicarbonate, 7.5g acetone, 27g ethanol and 114.8g water are mixed; wherein; the mixture of metasilicic acid and two silicic acid comprises the metasilicic acid of 0.05g and two silicic acid of 0.1g, obtains protecting liquid.
Dry after being had by a surface deposition SodaLime glass cleaning of conductive layer clean, then form protective membrane at the above-mentioned protection liquid of surface-coated one deck of conductive layer.Then, the glass preheating 15 minutes under 370 DEG C of conditions will protective membrane being coated with.Afterwards glass after preheating is put into the fused salt reaction 5 hours of 440 DEG C, then glass is slowly taken out from fused salt, put into temperature and the close annealing furnace of temperature of molten salt is annealed to room temperature, obtain one side toughened glass.
The protective membrane on removing one side toughened glass surface and other pollutents are then clean by ultrasonic cleaning.The one side toughened glass cleaned up is adopted two interference technique test surfaces stress and exchanges the degree of depth, the instrument used is FSM-60LE measuring stress instrument.The experimental data obtained is as follows:
The test result on the surface of conductive layer:
Exchange stress (Cs): 509Mpa.
The exchange degree of depth (DOL) of stressor layers: the upper limit: 10.1 μm, lower limit: 9.2 μm.
, without interference fringe, not there is chemical exchange, there is no tempering in the test result of the glass surface of non-depositing conducting layer: test less than data.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (9)
1. a preparation method for one side toughened glass, is characterized in that, comprises the steps:
Pending glass is provided;
Protective membrane is formed in a surface-coated layer of protecting liquid of described glass;
By the glass preheating 15 ~ 100 minutes under 270 DEG C ~ 370 DEG C conditions being coated with protective membrane;
Fused salt glass after preheating being put into 390 DEG C ~ 440 DEG C reacts 3 ~ 8 hours;
Reacted glass is carried out anneal, obtains one side toughened glass;
Described protection liquid comprises each component of following mass percentage:
2. the preparation method of one side toughened glass according to claim 1, is characterized in that, a described surface-coated layer of protecting liquid at described glass is formed in the operation of protective membrane, adopts roller painting to apply described protection liquid.
3. the preparation method of one side toughened glass according to claim 1, is characterized in that, the thickness of described protective membrane is 3 μm ~ 8 μm.
4. the preparation method of one side toughened glass according to claim 1, is characterized in that, described fused salt is saltpetre fused salt.
5. the preparation method of one side toughened glass according to claim 1, is characterized in that, described protection liquid comprises each component of following mass percentage:
6. the preparation method of one side toughened glass according to claim 1, is characterized in that, in the mixture of described metasilicic acid and two silicic acid, the mass ratio of metasilicic acid and two silicic acid is 1:1 ~ 10.
7. the preparation method of one side toughened glass according to claim 1, is characterized in that, described water soluble alkali is sodium hydroxide, potassium hydroxide, sodium carbonate or sodium bicarbonate.
8. the preparation method of one side toughened glass according to claim 1, is characterized in that, the thickness of described pending glass is 0.2mm ~ 1.1mm.
9. the preparation method of one side toughened glass according to claim 1, is characterized in that, the temperature of described preheating is 350 DEG C.
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CN105814004A (en) | 2013-10-14 | 2016-07-27 | 康宁股份有限公司 | Ion exchange process and chemically strengthened glass substrates resulting therefrom |
DE102014113149A1 (en) * | 2014-09-12 | 2016-03-17 | Schott Ag | Thin glass roll and process for its production |
CN104445896A (en) * | 2014-11-28 | 2015-03-25 | 张家港市德力特新材料有限公司 | Method for preparing tempered glass |
CN109748518B (en) * | 2017-11-02 | 2022-12-27 | 重庆鑫景特种玻璃有限公司 | Tempered glass and manufacturing method thereof |
CN114656815A (en) * | 2022-03-31 | 2022-06-24 | 醴陵旗滨电子玻璃有限公司 | Coating liquid, preparation method thereof and chemical strengthening method |
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Effective date of registration: 20160127 Address after: 443005 No. 38, Dalian Road, Yichang, Hubei Patentee after: YICHANG NANBO DISPLAY DEVICES CO., LTD. Address before: 518000 Guangdong Province, Shenzhen high tech Zone of Nanshan District City, No. three North Road, CSG Electronics Building Patentee before: Shenzhen Nanbo Welllight Conductive Coating Co., Ltd. |