KR20130109754A - Seal composition for exhaust pipe of vacuum glazing - Google Patents

Seal composition for exhaust pipe of vacuum glazing Download PDF

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Publication number
KR20130109754A
KR20130109754A KR1020120031756A KR20120031756A KR20130109754A KR 20130109754 A KR20130109754 A KR 20130109754A KR 1020120031756 A KR1020120031756 A KR 1020120031756A KR 20120031756 A KR20120031756 A KR 20120031756A KR 20130109754 A KR20130109754 A KR 20130109754A
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KR
South Korea
Prior art keywords
weight
frit
forming
exhaust pipe
vacuum glass
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KR1020120031756A
Other languages
Korean (ko)
Inventor
정효성
정우만
이상호
김경진
정승화
Original Assignee
주식회사 휘닉스소재
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Priority to KR1020120031756A priority Critical patent/KR20130109754A/en
Publication of KR20130109754A publication Critical patent/KR20130109754A/en

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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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
    • C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
    • C03C3/066—Glass compositions containing silica with less than 40% silica by weight containing boron containing zinc
    • 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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
    • C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
    • C03C3/068—Glass compositions containing silica with less than 40% silica by weight containing boron containing rare earths
    • 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
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
    • C03C8/04—Frit compositions, i.e. in a powdered or comminuted form containing zinc
    • 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
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
    • 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
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/24—Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
    • E—FIXED CONSTRUCTIONS
    • E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
    • E06B—FIXED OR MOVABLE CLOSURES FOR OPENINGS IN BUILDINGS, VEHICLES, FENCES OR LIKE ENCLOSURES IN GENERAL, e.g. DOORS, WINDOWS, BLINDS, GATES
    • E06B3/00—Window sashes, door leaves, or like elements for closing wall or like openings; Layout of fixed or moving closures, e.g. windows in wall or like openings; Features of rigidly-mounted outer frames relating to the mounting of wing frames
    • E06B3/66—Units comprising two or more parallel glass or like panes permanently secured together
    • E06B3/6612—Evacuated glazing units

Abstract

A sealant composition for a vacuum glass exhaust pipe is provided. The sealant composition includes a frit for forming a support and a frit for forming a junction, wherein the frit for forming a support is 50 to 80 wt% of Bi 2 O 3 , 1 to 15 wt% of SiO 2, and 1 to 15 wt% of B 2 O 3. %, Al 2 O 3 1 to 10% by weight, ZnO 1 to 15% by weight and CeO 0.1 to 5% by weight, the junction forming frit is 70 to 90% by weight of PbO, 1 to 25% by weight of B 2 O 3 Base and filler comprising from 1% to 10% by weight of SiO 2 .
The seal manufactured by using the sealant composition may seal the vacuum glass exhaust pipe without leaking out of the vacuum between the panes and cracking of the plate glass itself when sealing the exhaust pipe of the building vacuum glass.

Description

Sealing composition for vacuum glass exhaust pipe {SEAL COMPOSITION FOR EXHAUST PIPE OF VACUUM GLAZING}

The present invention relates to a sealant composition for a vacuum glass exhaust pipe.

Architectural vacuum glass uses environmentally friendly materials that save energy, unlike single glazing. At the time when many environmentally friendly materials are on the rise due to global warming and resource depletion, vacuum glass is attracting attention as an environmentally friendly material that meets these requirements.

The vacuum glass introduces outdoor solar heat to the inside, and minimizes heat loss due to conduction and convection due to the vacuum present between the glass and the glass. Accordingly, it is important to maintain a constant vacuum in the glass through the exhaust pipe sealing process or the optimization of the sealing frit composition.

One embodiment of the present invention is to provide a sealant composition capable of sealing a vacuum glass exhaust pipe without leaking out of the vacuum between the plate glass and cracking of the plate glass itself when sealing the exhaust pipe of the building vacuum glass.

Another embodiment of the present invention is to provide a method for producing a seal manufactured by using the seal composition and a seal prepared therefrom.

Another embodiment of the present invention is to provide a vacuum glass manufactured using the seal.

According to an embodiment of the present invention, Bi 2 O 3 50 to 80% by weight, SiO 2 1 to 15% by weight, B 2 O 3 1 to 15% by weight, Al 2 O 3 1 to 10% by weight, ZnO 1 to A frit for forming a support comprising 15 wt% and 0.1-5 wt% CeO 2 ; And a sealant composition for a vacuum glass exhaust pipe including a mother phase comprising 70 to 90 wt% of PbO, 1 to 25 wt% of B 2 O 3, and 1 to 10 wt% of SiO 2 , and a frit for forming a joint including a filler. to provide.

The support forming frit may have a thermal expansion coefficient of 70 × 10 −7 / K to 100 × 10 −7 / K and a transition point of 390 ° C. to 470 ° C.

The filler may be selected from the group consisting of alumina, cordierite, spodumene, willemite, mullite, and mixtures thereof.

The joining part forming frit may include 5 to 20 parts by weight of filler based on 100 parts by weight of base.

The junction forming frit may have a thermal expansion coefficient of 70 × 10 −7 / K to 95 × 10 −7 / K and a transition point of 310 ° C. to 360 ° C.

According to another embodiment of the present invention, Bi 2 O 3 50 to 80% by weight, SiO 2 1 to 15% by weight, B 2 O 3 1 to 15% by weight, Al 2 O 3 1 to 10% by weight, ZnO 1 A support comprising from 15 wt% to 0.1 wt% CeO 2 ; And a bonding portion including a filler, positioned below the support, to seal the exhaust pipe, the base including 70 to 90 wt% of PbO, 1 to 25 wt% of B 2 O 3, and 1 to 10 wt% of SiO 2 , and a filler. Provided is a seal for a vacuum glass exhaust pipe.

The filler may be selected from the group consisting of alumina, cordierite, spodumene, willemite, mullite, and mixtures thereof.

The bonding portion may include 5 to 20 parts by weight of the filler with respect to 100 parts by weight of the base.

According to another embodiment of the present invention, Bi 2 O 3 50 to 80% by weight, SiO 2 1 to 15% by weight, B 2 O 3 1 to 15% by weight, Al 2 O 3 1 to 10% by weight, ZnO 1 Preparing a support using a frit for forming a support comprising from about 15 wt% to about 0.1 wt% to about 5 wt% CeO 2 ; Forming a junction using a frit for forming a junction comprising a 70-90 wt% PbO, 1-25 wt% B 2 O 3, and 1-10 wt% SiO 2 , and a filler; And it provides a method for producing a seal for the vacuum glass exhaust pipe comprising the step of heat-treating and then positioning the bonding portion on the support.

The frit for forming the support part may have a thermal expansion coefficient of 70 to 100 × 10 −7 / K and a transition point of 390 to 470 ° C.

The supporting part forming process may be performed by applying a load of 180 kgf or more to a supporting part forming frit to form a molded body, and then heating the temperature to 460 to 480 ° C. at a speed of 5 to 10 ° C. per minute for 10 minutes and then cooling the same.

The junction forming frit may have a thermal expansion coefficient of 70 × 10 −7 / K to 95 × 10 −7 / K and a transition point of 310 ° C. to 360 ° C.

The joining part forming process may be performed by applying a load for forming the joining part to a molded body by applying a load of 180 kgf or more.

The heat treatment process may be carried out by increasing the temperature to 370 to 390 ℃ at a rate of 5 to 7 ℃ per minute to maintain for 10 to 15 minutes.

According to another embodiment of the present invention, there is provided a vacuum glass manufactured using the above-mentioned seal.

Other details of the embodiments of the present invention are included in the following detailed description.

The vacuum glass sealing body may seal the vacuum glass exhaust pipe without leaking out of the vacuum between the plate glass and cracking of the plate glass itself when sealing the exhaust pipe of the building vacuum glass.

1 is a structural diagram schematically showing the structure of the jinyong glass sealing body according to an embodiment of the present invention.
2 is a structural diagram schematically showing a structure of a vacuum glass according to another embodiment of the present invention.

Hereinafter, embodiments of the present invention will be described in detail. However, this is presented as an example, by which the present invention is not limited and the present invention is defined only by the scope of the claims to be described later.

In general, in the case of building vacuum glass, the outside air is blocked through the joining of the plate glass and the plate glass, and the vacuum is set through the exhaust pipe at the top of the plate glass, and the vacuum inside the vacuum glass is maintained by sealing the exhaust pipe and the sealing body. .

In one embodiment of the present invention, when manufacturing the seal for the vacuum glass exhaust pipe, the seal is divided into a support portion for the exhaust pipe and a junction for sealing the exhaust pipe in contact with the vacuum glass, using a frit optimized with a composition suitable for each of these By forming the sealing body of the heterojunction, the vacuum glass exhaust pipe can be sealed without leaking to the outside of the vacuum between the plate glass and cracking of the plate glass itself when sealing the exhaust pipe of the vacuum glass.

That is, the sealing composition for a vacuum glass exhaust pipe according to an embodiment of the present invention is Bi 2 O 3 50 to 80% by weight, SiO 2 1 to 15% by weight, B 2 O 3 1 to 15% by weight, Al 2 O 3 A frit for forming a support comprising 1 to 10 wt%, ZnO 1 to 15 wt% and CeO 2 0.1 to 5 wt%; And a frit for forming a junction comprising 70 to 90 wt% PbO, 1 to 25 wt% B 2 O 3 and 1 to 10 wt% SiO 2 , and a filler.

Preferably the frit for forming the support portion is 60 to 80% by weight of Bi 2 O 3 , 3 to 15% by weight of SiO 2 , 5 to 15% by weight of B 2 O 3 , 1 to 5% by weight of Al 2 O 3 , ZnO 10 to 15 weight percent and 0.1-1 weight percent CeO 2 .

The frit for forming the support part having the composition as described above has a coefficient of thermal expansion and a transition point equivalent to that of the plate glass, so that there is no fear of cracking during the manufacture of the plate glass, and may exhibit excellent adhesion strength to the plate glass with excellent cold heat. Specifically, the frit for forming the support part has a thermal expansion coefficient of 70 × 10 −7 / K to 100 × 10 −7 / K and a transition point of 390 ° C. to 470 ° C.

Preferably, the junction forming frit may include a matrix containing 75 to 90% by weight of PbO, 5 to 25% by weight of B 2 O 3, and 1 to 5% by weight of SiO 2 , and a filler.

The filler may be selected from the group consisting of alumina, cordierite, spodumene, willemite, mullite, and mixtures thereof.

In addition, the bonding part forming frit includes 5 to 20 parts by weight of a filler, and more preferably 5 to 18 parts by weight, based on 100 parts by weight of the base. By including the mother phase and the filler in the above content range, it has the same level of thermal expansion coefficient and transition point as that of the plate glass, so that there is no fear of cracking during the production of the plate glass, and exhibits excellent adhesion strength to the plate glass with excellent cold heat.

The frit for junction formation having the composition as described above specifically exhibits a thermal expansion coefficient of 70 × 10 −7 / K to 95 × 10 −7 / K and a transition point of 310 ° C. to 360 ° C.

According to another embodiment of the present invention provides a seal manufactured by using the seal composition.

Specifically, the seal is Bi 2 O 3 50 to 80% by weight, SiO 2 1 to 15% by weight, B 2 O 3 1 to 15% by weight, Al 2 O 3 1 to 10% by weight, ZnO 1 to 15 A support comprising from 0.1 wt% to 5 wt% CeO 2 ; And it is located below the support to seal the exhaust pipe, and includes a bonding phase including a filler phase and a filler comprising 70 to 90% by weight of PbO, 1 to 25% by weight of B 2 O 3 and 1 to 10% by weight of SiO 2 .

1 is a structural diagram schematically showing the structure of a seal for a vacuum glass exhaust pipe according to an embodiment of the present invention. The seal shown in FIG. 1 has a structure including a ring-shaped support having a groove formed in the center, and a ring-shaped joint formed with a groove formed in the lower portion of the support, which is an example for describing the present invention. However, the present invention is not limited to FIG. 1.

Hereinafter, referring to FIG. 1, the vacuum glass exhaust pipe sealing body 10 may be a support part 11 serving as a support part of the exhaust pipe joint and a joint part 12 which is positioned below the support part and is bonded to the plate glass to seal the exhaust pipe. ).

In the center of the seal 10, a groove 13 penetrating the support 11 and the junction 12 is formed. At the same time as the plate glass bonding to form a vacuum to seal the plate glass with a sealing body, wherein the groove 13 serves to serve as an air outlet by extracting air to form a vacuum in the plate glass.

The height, the inner diameter and the outer diameter of the support portion 11 and the bonding portion 12 are preferably adjusted in consideration of the thickness and width of the plate glass used as the vacuum glass.

Specifically, when the thickness of the plate glass is 2 to 3mm, the support portion 11 may be 3mm or less in height, 2 to 3mm in inner diameter and 4 to 5mm in outer diameter, and the junction portion 12 is 0.5 to 1mm in height and 3 to 5mm in inner diameter. And an outer diameter of 4 to 5 mm.

Sealing body 10 having the structure as described above is Bi 2 O 3 50 to 80% by weight, SiO 2 1 to 15% by weight, B 2 O 3 1 to 15% by weight, Al 2 O 3 1 to 10% by weight, Preparing a support using a frit for forming a support comprising 1 to 15 wt% ZnO and 0.1 to 5 wt% CeO 2 ; Forming a junction using a frit for forming a junction comprising a 70-90 wt% PbO, 1-25 wt% B 2 O 3, and 1-10 wt% SiO 2 , and a filler; And it may be prepared by a manufacturing method comprising the step of placing a heat treatment on the support portion after the heat treatment.

Specifically, first, using the Bi 2 O 3 powder, SiO 2 powder, B 2 O 3 powder, Al 2 O 3 powder, ZnO powder and CeO 2 powder to prepare a frit for forming the support, the prepared frit for forming the support Using a mold to apply a load of 180kgf or more to produce a support part molded body of a predetermined form.

Bi 2 O 3 powder, SiO 2 powder, B 2 O 3 powder, Al 2 O 3 powder, ZnO powder and CeO 2 powder is Bi 2 O 3 50 to 80% by weight, SiO 2 1 It is preferable to mix in an amount of from 15 to 15% by weight, B 2 O 3 1 to 15% by weight, Al 2 O 3 1 to 10% by weight, ZnO 1 to 15% by weight and CeO 2 0.1 to 5% by weight, more preferably. Preferably 60 to 80 wt% of Bi 2 O 3 , 3 to 15 wt% of SiO 2, 5 to 15 wt% of B 2 O 3 , 1 to 5 wt% of Al 2 O 3 , 10 to 15 wt% of ZnO and 0.1 to CeO 2 0.1 It is preferably mixed at 1% by weight.

The frit for forming the support part may be prepared according to a conventional frit forming method, specifically, the mixture of the powders is heated to 900 to 1200 ° C. under an atmospheric atmosphere and then held for 10 to 30 minutes to melt, resulting in The melt can be prepared by quenching in air.

The frit for forming the support part prepared by the above method has a thermal expansion coefficient of 70 × 10 −7 / K to 100 × 10 −7 / K, and has a transition point of 390 ° C. to 470 ° C.

By having the thermal expansion coefficient and transition point in the above range, it has a transition point in the temperature range lower than the plate glass, there is no deformation of the plate glass when sealing, and also has a thermal expansion coefficient similar to the plate glass, there is no fear of cracks caused by the difference in thermal expansion. .

Subsequently, the manufactured support part forming frit is molded using a mold, wherein the mold can be appropriately selected according to the shape of the target sealing body. For example, in the case of the annular groove formed in the center of the seal, specifically, the support glass to be manufactured in the form of a ring with the center groove, specifically, when the thickness of the plate glass is 2 to 3mm in height 3mm or less, inner diameter 2 to 3mm And it is preferable to use the one having a form such that the annular support having an outer diameter of 4 to 5mm can be produced.

It is preferable to apply a load of 180 kgf or more at the time of molding using the mold to obtain a rigid molded body with high density, and more preferably to apply a load of 190 kgf or more.

The molded part of the support part produced as a result of molding may be used as it is, or the sintering process with respect to the said molded object may be further performed.

When performing the sintering process, the temperature of the support part molded body was raised to 460 to 480 ° C at a rate of 5 to 10 ° C per minute, maintained for 10 minutes, and then cooled by furnace. At this time, when the furnace temperature is 100 ° C. or less, the support part is made in the form of a plastic sintered body with convenient workability.

Apart from the above, PbO powder, B 2 O 3 powder and SiO 2 powder were mixed and melted to prepare a frit for forming a joint, and then mixed with a filler, and the mixed powder was put into a mold to apply a load of 180 kgf or more. The junction part molded object of a predetermined form is manufactured.

At this time, the PbO powder, B 2 O 3 powder and SiO 2 powder may be mixed with 70 to 90% by weight of PbO, 1 to 25% by weight of B 2 O 3 and 1 to 10% by weight of SiO 2 . Mixing in the content range is preferable because it can obtain an excellent effect of the adhesion strength due to the similar coefficient of thermal expansion with the plate glass, more preferably PbO 75 to 90% by weight, B 2 O 3 5 to 25% by weight and SiO 2 It is preferably mixed at 1 to 5% by weight.

The filler may be selected from the group consisting of alumina, cordierite, spodumene, willemite, mullite, and mixtures thereof.

The filler is preferably included in an amount of 5 to 20 parts by weight based on 100 parts by weight of the mother phase. When included in the content may exhibit an effect having a similar coefficient of thermal expansion to the plate glass, more preferably may be included in 5 to 18 parts by weight.

The joint forming frit may also be prepared by a conventional frit forming method, specifically, the mixture of the powders is heated to 900 to 1200 ° C. under an atmospheric atmosphere and then held for 10 to 30 minutes to melt, resulting in Prepared melt may be prepared by quenching in air.

The frit for joining portions produced by the method as described above has a thermal expansion coefficient of 70 × 10 −7 / K to 95 × 10 −7 / K and a transition point of 310 ° C. to 360 ° C. By having a coefficient of thermal expansion and a transition point in the above range, it has a coefficient of thermal expansion similar to that of plate glass, showing excellent adhesion strength.

Subsequently, the manufactured joint forming frit is molded using a mold, wherein the mold can be appropriately selected in accordance with the shape of the sealing body as the target. For example, when the groove is formed in the center of the sealing ring, and the thickness of the plate glass is 2 to 3mm, the shape so that the annular joint having a height of 0.5 to 1mm, an inner diameter of 3 to 5mm and an outer diameter of 4 to 5mm can be produced It is good to use a mold having a.

The molding process using the mold is the same as the supporting part forming process.

The junction part molded body obtained after the said molding process may be used for a subsequent process as it is, or the sintering process with respect to the said junction part molded object may further be performed. The sintering process for the junction molded body may be performed in the same manner as the molding process for the support molded body.

Next, the joint is placed on the prepared support and then heat treated.

The heat treatment process may be carried out by increasing the temperature to 370 to 390 ℃ at a rate of 5 to 7 ℃ per minute to maintain for 10 to 15 minutes.

After the heat treatment, by cooling to a furnace temperature of 100 ° C. or lower, a seal body in the form of a heterojunction of the support portion and the junction portion is produced.

As described above, in the method of manufacturing the seal according to the present invention, since the sintering temperature of the support and the joint is low, the seal may be manufactured by one heat treatment after the manufacture of the molded body of the support and the joint, or each of the molded parts of the support and the joint may be After the sintering process, a heat treatment process for forming the sealing body may be performed.

The sealing body produced by the above method is a heterojunction manufactured using frits having different compositions, and has a coefficient of thermal expansion and transition point similar to that of glass, showing excellent adhesion strength and heat resistance, and consequently a vacuum between the glass. It can effectively prevent leakage and prevent cracking of the pane itself when sealing the pane. Accordingly, the sealing body according to the present invention is useful in the manufacture of vacuum glass, and particularly in the manufacture of vacuum glass for construction.

Accordingly, according to another embodiment of the present invention provides a vacuum glass and a manufacturing method using the sealing body.

2 is a structural diagram schematically showing a structure of a vacuum glass according to an embodiment of the present invention. 2 is only an example of the present invention and the present invention is not limited thereto.

Referring to FIG. 2, the vacuum glass 100 includes an upper plate glass 101 on which an exhaust pipe 104 is formed, a lower plate glass 102 positioned to face the upper plate glass at a predetermined interval, and the upper plate and the lower plate glass. The adhesive layer 103 which interposes between 101 and 102 and bonds upper and lower plate glass, and the sealing body (not shown) which seals the said exhaust pipe 104 are included.

In addition, the manufacturing method of the vacuum glass can be carried out according to a conventional method except that the sealing body produced in the present invention, a detailed description thereof will be omitted. However, the sealing process of the exhaust pipe after vacuum formation between the plate glass is preferable because it can seal the exhaust pipe with excellent adhesion strength without the occurrence of cracks carried out by firing at a sealing temperature lower than the softening point of the plate glass, specifically about 500 to 580 ℃.

Hereinafter, specific embodiments of the present invention are presented. However, the embodiments described below are merely for illustrating or explaining the present invention in detail, and thus the present invention is not limited thereto.

(Examples 1 to 8)

After mixing to the ingredients and contents shown in Table 1, and then heated to 1100 ℃ under an atmospheric atmosphere to maintain a melt for 10 minutes to prepare a melt, and quenched with air while discharging the melt to prepare a frit for forming a support. After forming the molded body by applying a load of 190kgf or more to the manufactured frit forming frit by using a cylindrical mold, the temperature was raised to 470 ° C at a rate of 5 ° C per minute and maintained for 10 minutes, followed by quenching to prepare a support in the form of a plasticized body. Height 3mm, inner diameter 2.5mm and outer diameter 4.5mm).

Separately, after mixing with the ingredients and contents shown in Table 1, the mixture was formed by heating to 1100 ° C. in an air atmosphere, and then maintained for 10 minutes and rapidly cooled in air. Was made (height 1 mm, inner diameter 3 mm and outer diameter 5 mm).

After placing the junction on the support such that the groove formed in the support and the groove formed in the junction coincide with each other, the temperature is raised to 370 ° C. at a rate of 5 ° C. per minute and maintained for 10 minutes. Sieve was prepared.

Example One 2 3 4 5 6 7 8 Frit for forming support Bi 2 O 3 (% by weight) 62.8 68.8 74.8 78.8 74.8 74.8 74.8 74.8 SiO 2 (weight%) 10 10 5 3 5 5 5 5 B 2 O 3 (% by weight) 13 8 8 5 8 8 8 8 Al 2 O 3 (weight%) 4 2 One 2 One One One One ZnO (% by weight) 10 11 11 11 11 11 11 11 CeO 2 (weight%) 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 Frit for forming joints Motherhood
PbO
(weight%) 85.3 85.3 85.3 85.3 85.3 85 75 88 SiO 2
(weight%) 1.8 1.8 1.8 1.8 1.8 1.8 3 3 B 2 O
(% By weight) 3 12.9 12.9 12.9 12.9 12.9 12.9 22 9 filler
(Parts by weight based on 100 parts by weight of base) Cordierite 16 15 14 10 10 18 5 18

(Comparative Examples 1 to 4)

A sealing body was prepared by the same method as in Examples 1 to 8 except for using the ingredients and contents shown in Table 2 below.

Comparative Example One 2 3 4 Frit for forming support Bi 2 O 3 (% by weight) 74.8 74.8 59.5 81.2 SiO 2 (% by weight) 5 5 10 One B 2 O 3 (% by weight) 8 8 15.3 6.6 Al 2 O 3 (% by weight) One One 4 One ZnO (% by weight) 11 11 11 10 CeO 2 (% by weight) 0.2 0.2 0.2 0.2 Frit for forming joints Motherhood PbO (% by weight) - 85.3 85.3 85.3 SiO 2 (% by weight) - 1.8 1.8 1.8 B 2 O 3 (% by weight) - 12.9 12.9 12.9 filler
(Parts by weight based on 100 parts by weight of base) Cordierite - 3 14 14

Test Example 1

The coefficient of thermal expansion and the transition point of the frit for forming the supporting part and the joint part used in the manufacture of the seal according to the present invention were measured by the following method. The results are shown in Table 3.

1) Thermal expansion coefficient: After molding by applying a load of 190kgf or more to a cylindrical mold of 10 mm diameter, each of the support and the frit forming frit 2g prepared in Examples 1 to 8 and Comparative Examples 1 to 4 were molded, and the obtained molded body was box furnace. Using a box furnace to increase the temperature by 10 ℃ per minute, the temperature was raised to 50 ℃ or more than the transition point and maintained for 10 minutes, and cooled in the box furnace to prepare a molded body. After sintering, the thermal expansion coefficient was measured by increasing the temperature by 5 ° C. per minute using a TMA equipment (TA Instrument Q400) (measurement interval 50 to 250 ° C.).

2) Transition point: 30 mg of the frit for forming the support part and the junction part prepared in Examples 1 to 8 and Comparative Examples 1 to 4 were respectively measured using a differential thermal analyzer (TA Instrument Q100).

Frit for forming support Frit for forming joints Coefficient of thermal expansion
(10 -7 / K) Transition point
(℃) Coefficient of thermal expansion
(10 -7 / K) Transition point
(℃) Example 1 73 460 71.2 316.4 Example 2 77 440 73.6 316.4 Example 3 86 410 75.9 316.4 Example 4 96 395 83.9 316.4 Example 5 86 410 83.9 316.4 Example 6 86 410 70.1 316.4 Example 7 86 410 92.6 357.7 Example 8 86 410 72.9 311.6 Comparative Example 1 86 410 - - Comparative Example 2 86 410 97.8 316.4 Comparative Example 3 69 473 75.9 316.4 Comparative Example 4 105 356 75.9 316.4

As shown in Table 3, the seals of Examples 1 to 8 according to the present invention, the frit forming the bonding portion and the support portion can exhibit excellent adhesion properties to the plate glass by exhibiting a coefficient of thermal expansion equivalent to that of ordinary plate glass. . On the other hand, Comparative Examples 1 to 4 show a thermal expansion coefficient outside the range of the plate glass thermal expansion coefficient can be expected to decrease the adhesion strength to the plate glass.

Test Example 2

Two sheets of soda-lime silicate glass (manufactured by Korea Glass Co., Ltd.) having a thickness of 3 mm are faced to each other, and then attached using a Bi 2 O 3 -ZnO-B 2 O 3 -based glass adhesive, and the air between the plate glass is passed through the exhaust pipe formed in the plate glass. After evacuating and evacuating, the exhaust pipe was blocked with the seals prepared in Examples 1 to 8 and Comparative Examples 1 to 4, respectively, and sealed at the sealing temperature shown in Table 4 to prepare a vacuum glass.

After sealing the glass, the presence of cracks in the glass was visually observed.

In addition, the cold heat resistance and the adhesive strength of the sealing body were evaluated for the vacuum glass prepared as described below. The results are shown in Table 4 below.

1) Coolability evaluation: The cold glass test was performed by increasing the temperature from Δ60 ° C. to the temperature at which cracks were generated.

2) Adhesion strength evaluation: The adhesion strength at the time of breakage was measured when the vacuum glass produced by the push and pull gage was pulled vertically by pulling 30 mm from the end of the exhaust pipe in the vertical direction. .

Sting
Temperature
(℃) Plate glass cracks after sealing Cold heat evaluation (℃) Adhesion strength
(kgf / ㎠) Boxed / Cold Water ΔT Example 1 530 none 112 ℃ / 25 ℃ 87 ℃ 4.6 Example 2 510 none 120 ℃ / 25 ℃ 95 ℃ 4.6 Example 3 500 none 130 ℃ / 25 ℃ 105 ℃ 4.7 Example 4 500 none 125 ℃ / 25 ℃ 100 ℃ 4.3 Example 5 500 none 125 ℃ / 25 ℃ 100 ℃ 4.3 Example 6 500 none 128 ℃ / 25 ℃ 103 ℃ 4.6 Example 7 500 none 115 ℃ / 25 ℃ 90 ° C 3.9 Example 8 500 none 125 ℃ / 25 ℃ 100 ℃ 4.6 Comparative Example 1 500 none 125 ℃ / 25 ℃ 100 ℃ 3.1 Comparative Example 2 500 Cracking 110 ℃ / 25 ℃ 85 ℃ 3.7 Comparative Example 3 550 Cracking 125 ℃ / 25 ℃ 100 ℃ 4.4 Comparative Example 4 480 Cracking 125 ℃ / 25 ℃ 100 ℃ 2.8

As shown in Table 4, the seals of Examples 1 to 8 according to the present invention showed excellent adhesion strength and cold heat resistance, and also showed excellent strength characteristics because there was no crack in plate glass during vacuum glass manufacturing. Can be.

Although the preferred embodiments of the present invention have been described in detail above, the scope of the present invention is not limited thereto, and various modifications and improvements of those skilled in the art using the basic concepts of the present invention defined in the following claims are also provided. It belongs to the scope of rights.

10 seals
11 support
12 connections
100 vacuum glass
101 102 flat glass
103 adhesive layer
104 exhaust pipe

Claims (15)

50 to 80 wt% Bi 2 O 3 , 1 to 15 wt% SiO 2, 1 to 15 wt% B 2 O 3, 1 to 10 wt% Al 2 O 3 , 1 to 15 wt% ZnO and 0.1 to 5 CeO 2 A frit for forming a support comprising a weight percent; And
A frit for forming a junction comprising 70 to 90% by weight of PbO, 1 to 25% by weight of B 2 O 3 and 1 to 10% by weight of SiO 2 , and a filler
Sealing composition for a vacuum glass exhaust pipe comprising a. The method of claim 1,
The frit for forming the support portion has a thermal expansion coefficient of 70 × 10 -7 / K to 100 × 10 -7 / K and a transition point of 390 ℃ to 470 ℃ seal composition for vacuum glass exhaust pipe. The method of claim 1,
Wherein the filler is selected from the group consisting of alumina, cordierite, spodumene, willemite, mullite and mixtures thereof. The method of claim 1,
The joining portion forming frit is a sealing composition for a vacuum glass exhaust pipe containing 5 to 20 parts by weight of filler with respect to 100 parts by weight of the mother phase. The method of claim 1,
The joint forming frit has a thermal expansion coefficient of 70 × 10 -7 / K to 95 × 10 -7 / K and a transition point of 310 ℃ to 360 ℃ sealing composition for vacuum glass. 50 to 80 wt% Bi 2 O 3 , 1 to 15 wt% SiO 2, 1 to 15 wt% B 2 O 3, 1 to 10 wt% Al 2 O 3 , 1 to 15 wt% ZnO and 0.1 to 5 CeO 2 A support comprising weight percent; And
Located at the bottom of the support to seal the exhaust pipe, the bonding portion including a filler, and a filler phase comprising 70 to 90% by weight of PbO, 1 to 25% by weight of B 2 O 3 and 1 to 10% by weight of SiO 2 , and a filler
Sealing body for a vacuum glass exhaust pipe comprising a. The method according to claim 6,
The filler is selected from the group consisting of alumina, cordierite, spodumene, willemite, mullite, and mixtures thereof. The method according to claim 6,
The joint portion sealing body for a vacuum glass exhaust pipe comprising 5 to 20 parts by weight of filler with respect to 100 parts by weight of the base. 50 to 80 wt% Bi 2 O 3 , 1 to 15 wt% SiO 2, 1 to 15 wt% B 2 O 3, 1 to 10 wt% Al 2 O 3 , 1 to 15 wt% ZnO and 0.1 to 5 CeO 2 Preparing a support using a frit for forming a support comprising a weight percent;
Forming a junction using a frit for forming a junction comprising a 70-90 wt% PbO, 1-25 wt% B 2 O 3, and 1-10 wt% SiO 2 , and a filler; And
The method of manufacturing a seal for a vacuum glass exhaust pipe comprising the step of heat-treating after placing the bonding portion on the support. 10. The method of claim 9,
The frit for forming the support portion has a thermal expansion coefficient of 70 × 10 -7 / K to 100 × 10 -7 / K and a transition point of 390 ℃ to 470 ℃ manufacturing method for a seal for a vacuum glass exhaust pipe. 10. The method of claim 9,
The supporting part forming process is to produce a molded body by applying a load of 180kgf or more frit for forming the support part, the temperature is raised to 460 to 480 ℃ at a rate of 5 to 10 ℃ per minute and maintained for 10 minutes to be cooled by vacuum for exhaust pipe Method for producing a seal. 10. The method of claim 9,
The joint forming frit has a thermal expansion coefficient of 70 × 10 -7 / K to 95 × 10 -7 / K and a transition point of 310 ℃ to 360 ℃ manufacturing method for a seal for a vacuum glass exhaust pipe. 10. The method of claim 9,
The joining part forming step is a manufacturing method of a sealing body for a vacuum glass exhaust pipe that is carried out by producing a molded body by applying a load of 180kgf or more frit for joining. 10. The method of claim 9,
The heat treatment step is a method for producing a sealing body for a vacuum glass exhaust pipe that is carried out by heating up to 370 ℃ to 390 ℃ at a rate of 5 ℃ to 7 ℃ per minute for 10 to 15 minutes. Vacuum glass manufactured using the sealing body according to claim 6.
KR1020120031756A 2012-03-28 2012-03-28 Seal composition for exhaust pipe of vacuum glazing KR20130109754A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108033684A (en) * 2017-12-13 2018-05-15 海南中航特玻科技有限公司 A kind of back of the body silver glass powder used for solar batteries and preparation method
US10358861B2 (en) 2017-02-17 2019-07-23 Vkr Holding A/S Vacuum insulated glazing unit
GB2587074A (en) * 2019-07-15 2021-03-17 Johnson Matthey Plc Composition, paste and methods

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10358861B2 (en) 2017-02-17 2019-07-23 Vkr Holding A/S Vacuum insulated glazing unit
EP3363982B1 (en) * 2017-02-17 2019-07-31 VKR Holding A/S Vacuum insulated glazing unit
CN108033684A (en) * 2017-12-13 2018-05-15 海南中航特玻科技有限公司 A kind of back of the body silver glass powder used for solar batteries and preparation method
GB2587074A (en) * 2019-07-15 2021-03-17 Johnson Matthey Plc Composition, paste and methods
GB2587074B (en) * 2019-07-15 2022-01-12 Johnson Matthey Advanced Glass Tech B V Composition, paste and methods

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