KR20130003579A - Manufacturing method of strengthed glass and strengthed glass thereby - Google Patents

Manufacturing method of strengthed glass and strengthed glass thereby Download PDF

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Publication number
KR20130003579A
KR20130003579A KR1020110065016A KR20110065016A KR20130003579A KR 20130003579 A KR20130003579 A KR 20130003579A KR 1020110065016 A KR1020110065016 A KR 1020110065016A KR 20110065016 A KR20110065016 A KR 20110065016A KR 20130003579 A KR20130003579 A KR 20130003579A
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South Korea
Prior art keywords
glass
thin glass
potassium nitrate
high pressure
compressive stress
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KR1020110065016A
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Korean (ko)
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KR101302664B1 (en
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정상기
박만금
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정상기
박만금
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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
    • C03C21/00Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface
    • C03C21/001Treatment 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
    • C03C21/002Treatment 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
    • 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
    • C03C23/00Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/007Other surface treatment of glass not in the form of fibres or filaments by thermal treatment
    • 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
    • C03C23/00Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/0075Cleaning of glass
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00Technologies relating to the processing of minerals
    • Y02P40/50Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57Improving the yield, e-g- reduction of reject rates

Abstract

The present invention promotes the ion exchange reaction rate of sodium ions and potassium ions in the glass surface layer by ion exchange in a high pressure atmosphere to significantly reduce the time required to obtain a practical surface compressive stress and to strengthen the depth of the compressive stress layer deeply. Disclosed is a glass manufacturing method. The method of manufacturing tempered glass according to the present invention includes a chemical strengthening treatment step of forming a compressive stress layer on the surface of the thin glass by immersing the thin glass preheated to a transition temperature below 200 to 400 ° C. in a potassium nitrate solution. The chemical strengthening treatment step is characterized in that it is carried out in a high pressure atmosphere (about 2Kg / ㎠ to 1000Kg / ㎠) above atmospheric pressure. Here, the preheating temperature of the thin glass is 300 ~ 450 ℃, the tempering time of the thin glass is a few minutes to several tens of minutes.

Description

Method for manufacturing tempered glass and tempered glass manufactured therefrom {MANUFACTURING METHOD OF STRENGTHED GLASS AND STRENGTHED GLASS THEREBY}

The present invention relates to a method of manufacturing tempered glass, and more particularly, to a method of manufacturing tempered glass used in liquid crystal display windows of various display devices such as mobile phones, portable information terminals, navigation, and the like.

In general, the strengthening of glass is largely divided into physical strengthening and chemical strengthening.

Physical reinforcement is mainly used in the production of tempered glass doors, automotive glass, etc. in a manner of strengthening the internal strength of the glass by heating the glass of 5 mm or more thickness to a temperature between 550 ° C and 700 ° C and then quenching. However, this physical reinforcement is not applicable to thin glass (less than 3mm), which cannot make a sufficient temperature difference between the glass surface layer and the center layer. There is a disadvantage that each part does not have a uniform temperature difference, and there is a possibility of deformation since the operation is performed at a relatively high temperature (near softening temperature).

On the other hand, chemical strengthening is to strengthen the glass by substituting the sodium ions in the glass and the potassium ions in the potassium nitrate solution by immersing the thin glass in the potassium nitrate solution at 450 ° C. for at least 3 hours. Used to reinforce.

The chemical strengthening is to strengthen the glass through ion exchange, it is possible to strengthen both thin glass and glass of complex shape, there is no fear of deformation during operation, it is superior to the physical strengthening in terms of strength with the advantage of high precision, after strengthening There is an advantage in that cutting and the like are possible.

In the above-described chemical glass strengthening method, first, the glass to be strengthened is heated below the transition temperature in the range of 300 to 450 ° C., on the other hand, the potassium nitrate salt is melted at a temperature of 380 ° C. or higher to preheat the molten salt. It is a method of forming and strengthening a predetermined compressive stress layer on the surface of the glass by immersing the prepared glass for a predetermined time or more.

However, the above conventional chemical glass strengthening method requires a long time of several hours to several tens of hours in order to obtain a practical surface compressive stress, which leads to a problem that the productivity is lowered. As the depth of the glass is not deep, there is a limit in improving the strength and hardness of the tempered glass.

The present invention has been made in view of the above, and by ion exchange in a high pressure atmosphere to accelerate the ion exchange reaction rate of sodium and potassium ions in the glass surface layer to significantly reduce the time required to obtain a practical surface compressive stress and compression It is an object of the present invention to provide a method for producing tempered glass that can form a deep depth of the stress layer, and a tempered glass produced by the method.

In the method for producing tempered glass according to the present invention for achieving the above object, the chemical strengthening treatment to form a compressive stress layer on the surface of the thin glass by immersing the thin glass preheated to the transition temperature below 200 ~ 400 ℃ potassium nitrate solution And the chemical strengthening step is performed in a high pressure atmosphere at a pressure above atmospheric pressure.

According to a preferred embodiment of the present invention, the high pressure is preferably 2Kg / ㎠ to 1000Kg / ㎠.

In addition, the preheating temperature of the thin glass is 300 ~ 450 ℃, the immersion time of the thin glass is a few minutes to several tens of minutes. That is, when performing the chemical strengthening treatment in the atmospheric pressure atmosphere should be immersed for at least several tens of hours, according to the present invention, even if only a few minutes to several tens of minutes to immerse in the atmosphere at atmospheric pressure dozens of hours to obtain a compressive stress layer of the same depth and depth You can get it.

According to a preferred embodiment of the present invention, a method of manufacturing tempered glass, comprising: preparing a thin glass having a predetermined thickness; Preheating the thin glass to 300 to 450 ° C. in a preheating furnace; Filling with potassium nitrate in a high temperature salt bath followed by heating to 200-400 ° C .; Immersing the preheated thin glass in the potassium nitrate solution and performing a high pressure chemical strengthening treatment for a predetermined time while maintaining an internal pressure of a high temperature salt bath at 2 Kg / cm 2 to 1000 Kg / cm 2; And a cooling and washing step of cooling the high pressure chemically strengthened thin glass and removing potassium nitrate remaining on the surface of the thin glass.

According to the present invention, since the chemical strengthening treatment of immersing the thin glass in the potassium nitrate solution to form a compressive stress layer on the surface of the thin glass is carried out in a high pressure atmosphere of at least atmospheric pressure, preferably 2Kg / ㎠ to 1000Kg / ㎠, The rate of ion exchange reaction between sodium ions and potassium ions in the glass surface layer is accelerated, which can drastically reduce the time required to obtain a practical surface compressive stress.

In other words, according to the present invention, assuming that the compressive stress layer having the same depth as the method of forming the compressive stress layer by immersing the thin glass in the potassium nitrate solution in the atmospheric pressure as in the general method, the strengthening time is several minutes to It can be reduced by tens of minutes.

In addition, according to the present invention, not only can reduce the strengthening time compared to the existing method, but also can form a deeper depth of the compressive stress layer, it is possible to improve the strength and hardness of the tempered glass.

Therefore, according to the present invention, since the tempered glass with improved strength and hardness can be manufactured in a shorter time than the existing chemical strengthening method, it is possible to improve the quality and productivity, and to reduce the manufacturing cost according to the productivity. We can plan.

1 is a process diagram of a method of manufacturing tempered glass according to an embodiment of the present invention, and
2 is a view schematically showing an example of accommodating a plurality of thin glass in a high temperature salt bath to process a high pressure chemical strengthening.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. The present invention may be variously modified and may have various forms, and exemplary embodiments will be described in detail. However, this is not intended to limit the present invention to the specific form disclosed, it should be understood to include all modifications, equivalents, and substitutes included in the spirit and scope of the present invention.

The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The singular expressions include plural expressions unless the context clearly dictates otherwise.

Also, unless otherwise defined, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Terms such as those defined in commonly used dictionaries are to be interpreted as having a meaning consistent with the meaning of the context in the relevant art and, unless explicitly defined herein, are to be interpreted as ideal or overly formal Do not.

As shown in Figure 1, the tempered glass manufacturing method according to an embodiment of the present invention, the step of preparing a thin glass having a predetermined thickness (S110), the step of preheating the thin glass at 300 ~ 450 ℃ in the preheating furnace (S120), after filling potassium nitrate in a high temperature salt bath and heating to 200 ~ 400 ℃ (S130), immersing the preheated thin glass in the potassium nitrate solution and the internal pressure of the high temperature salt bath above atmospheric pressure, preferably Preferably, the step of maintaining a high pressure chemically strengthened glass for a predetermined time in a state of maintaining 2Kg / ㎠ to 1000Kg / ㎠ (S140) and cooling the high pressure chemically strengthened thin glass and potassium nitrate remaining on the surface of the thin glass Cooling and washing step to remove (S150).

Step S110 is a step of preparing a thin glass having a predetermined thickness determined according to the product to be applied to the tempered glass. At this time, the thin glass may have a thickness of about 0.5 to 3.0mm, but slightly different for each product such as mobile (cell phone, smart phone, PDA), LCD TV, LCD monitor, navigation, MP3, PMP, notebook, and the like.

The step S120 is a step of preheating the thin glass prepared as described above in the preheating furnace to 300 ~ 450 ℃. The preheating temperature and time vary depending on the thickness of the thin glass, but the preheating treatment is performed for about 30 minutes to 1 hour 30 minutes. Here, when the preheating temperature is 300 ° C. or below, the thin glass is not sufficiently preheated, and thus, it is difficult to transfer the ion ionization reaction with the potassium nitrate solution or the reaction time since sodium ions on the surface of the thin glass are difficult to transfer in a high temperature salt bath. If the temperature is higher than 450 ℃, there is a risk of damage due to thermal shock during preheating, and rapid ion exchange reaction of sodium ions and potassium ions occurs in a high temperature salt bath, resulting in deterioration of the elasticity of the thin glass. Will adversely affect.

On the other hand, the pre-heating furnace is to prevent the thin glass because it may cause damage and damage to the tissue of the thin glass when heated to a high temperature in a high temperature salt bath to be described later. Although not illustrated in detail, such a preheating furnace may be configured to alternately include a pipe heater and a far infrared heater, and to adjust the temperature by using a blower. In addition, by installing a temperature sensor inside the preheating furnace for precise temperature control, it may be configured to increase the blower volume of the blower if the temperature exceeds the set value, and decrease the blower volume if the temperature is lower.

The step S130 is a step of liquefying the chemicals to be used for glass strengthening, that is, potassium nitrate into a high temperature salt bath and heating to about 200 ~ 400 ℃. In addition to potassium nitrate, sodium nitrate may be used as the chemical agent.

As the high temperature salt bath according to the characteristics of the present invention, as shown in Figure 2, a cover for sealing the main body 10 and the main body 10 in which the potassium nitrate 30 and a plurality of laminated glass 40 is accommodated ( 11). In addition, the main body 10 is connected to a pressure generating unit 20 for maintaining the inside of the high temperature salt bath in a predetermined pressure state. The cover 11 can be opened and closed with respect to the main body 10.

The step S140 is a step of performing an indirect heat treatment for a predetermined time by immersing the thin glass 40 in the potassium nitrate solution 30 accommodated in the high temperature salt bath. This step S140 is carried out in a high pressure atmosphere of pressure above atmospheric pressure, preferably about 2 Kg / cm 2 to about 1000 Kg / cm 2 in accordance with a feature of the present invention. Here, the pressure in the high temperature salt bath may be generated at an appropriate pressure by the pressure generating unit (20).

Specifically, put the potassium nitrate powder for producing the thin glass into tempered glass in the high temperature salt bath, and heated to a temperature of about 200 ~ 400 ℃ to liquefy potassium nitrate and immers the thin glass in the liquefied potassium nitrate solution In this case, sodium ions having a small ionic radius distributed on the surface of the thin glass and potassium ions having a large ionic radius of the potassium nitrate solution are substituted with each other to form a compressive stress layer formed by ion exchange reaction on the surface of the thin glass. Large tempered glass is formed.

At this time, in the present invention, the high-temperature salt bath is tempered for the thin glass while maintaining a high pressure of about 2Kg / ㎠ to 1000Kg / ㎠. As described above, when the chemical strengthening treatment is performed in a pressure atmosphere higher than atmospheric pressure, the ion replacement reaction rate is accelerated, thereby greatly reducing the strengthening time.

For example, the depth of the compressive stress layer of the tempered glass is generally formed about 3 ~ 4㎛, although there is a slight difference depending on the manufacturer and the product to be applied, according to the conventional method (reinforcement treatment at atmospheric pressure atmosphere) In order to form a compressive stress layer of such a depth, the thin glass should be immersed in potassium nitrate solution for 3 to 5 hours. However, when the chemical reinforcement treatment is performed in a pressure atmosphere higher than atmospheric pressure as in the present invention, assuming that a compressive stress layer having the same depth is formed, the reinforcement time is shortened to within 1 hour. That is, according to this invention, productivity improvement of about 4 to 5 times can be aimed at.

In addition, when the chemical strengthening treatment is performed in the high pressure atmosphere as described above, it is possible to significantly shorten the strengthening time and to obtain a strengthened glass with improved strength and hardness by forming a deeper compressive stress layer on the thin glass surface.

Here, the pressure in the high temperature salt bath can be appropriately adjusted according to the thickness and / or degree of strengthening of the thin glass. In other words, when a large strength and hardness are required, the pressure may be increased to deepen the depth of the compressive stress layer.

As described above, after performing the chemical strengthening treatment for the thin glass, and performing cooling and washing step (S150) to remove the potassium nitrate remaining in the thin glass while cooling the tempered glass.

Although the cooling and washing step (S150) is not specifically illustrated, for example, in the slow cooling furnace to cool the temperature of the heated thin glass to about 100 ℃ in the ion replacement process with potassium nitrate ions. This slow cooling can prevent deformation of the ion-substituted thin glass and at the same time remove residual stresses.

Next, the temperature of the thin glass transferred by cooling in the slow cooling furnace is kept at a constant temperature for a few minutes. In this way, the surface of the thin glass is strengthened chemically stable structure, such that the physical properties and chemical properties such as strength of the tempered glass does not change for a long time.

Finally, the potassium nitrate remaining on the surface of the thin glass is washed while keeping the internal temperature at a constant temperature in the cold water furnace.

According to the method of manufacturing tempered glass according to the present invention as described above, compared to the case of manufacturing the same thickness of tempered glass, the time required for chemical strengthening can be reduced to 1/3 to 1/5 of the conventional level. In addition, the tempered glass prepared by the present invention is about 3 to 5 times the bending strength, impact resistance about 6 to 8 times stronger than conventional tempered glass of the same thickness, excellent in physical and chemical properties such as hardness, heat resistance, transparency Effect.

While the invention has been described with respect to specific embodiments thereof, it will be apparent to one skilled in the art that the invention may be embodied in other specific forms without departing from the essential characteristics thereof. Accordingly, the described embodiments are to be considered in all respects as illustrative and not restrictive, and therefore, all modifications apparent to those skilled in the art are included therein.

10: Body 11; cover with high temperature salt bath
20; pressure generating unit 30; potassium nitrate solution
40; thin glass

Claims (5)

In the tempered glass manufacturing method comprising a chemical strengthening treatment step of forming a compressive stress layer on the surface of the thin glass by immersing the thin glass preheated to the transition temperature below 200 ~ 400 ℃ potassium nitrate solution,
The chemical strengthening step is tempered glass manufacturing method characterized in that carried out in a high pressure atmosphere of atmospheric pressure or more.
The method of claim 1,
The high pressure range above the atmospheric pressure is 2Kg / ㎠ to 1000Kg / ㎠ characterized in that the tempered glass manufacturing method.
The method of claim 1,
The preheating temperature of the thin glass is 300 ~ 450 ℃, the tempering time of the thin glass is tempered glass manufacturing method, characterized in that several minutes to several tens of minutes.
Preparing a thin glass having a predetermined thickness;
Preheating the thin glass to 300 to 450 ° C. in a preheating furnace;
Filling with potassium nitrate in a high temperature salt bath followed by heating to 200-400 ° C .;
Immersing the preheated thin glass in the potassium nitrate solution and performing a high pressure chemical strengthening treatment for a predetermined time while maintaining an internal pressure of a high temperature salt bath at 2 Kg / cm 2 to 1000 Kg / cm 2; And
And cooling and washing to cool the high pressure chemically strengthened thin glass, and to remove potassium nitrate remaining on the surface of the thin glass.
The tempered glass for touch panels manufactured by the method in any one of Claims 1-4.
KR1020110065016A 2011-06-30 2011-06-30 Manufacturing method of strengthed glass and strengthed glass thereby KR101302664B1 (en)

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