CN110642534A - Vacuum glass with composite layer sealing structure and anodic bonding packaging method thereof - Google Patents
Vacuum glass with composite layer sealing structure and anodic bonding packaging method thereof Download PDFInfo
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- CN110642534A CN110642534A CN201911104976.2A CN201911104976A CN110642534A CN 110642534 A CN110642534 A CN 110642534A CN 201911104976 A CN201911104976 A CN 201911104976A CN 110642534 A CN110642534 A CN 110642534A
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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
- C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
- C03C27/06—Joining glass to glass by processes other than fusing
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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
- C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
- C03C27/06—Joining glass to glass by processes other than fusing
- C03C27/08—Joining glass to glass by processes other than fusing with the aid of intervening metal
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Abstract
The invention relates to the technical field of vacuum glass manufacturing, in particular to vacuum glass with a composite layer sealing structure and an anodic bonding packaging method thereof. The method is characterized in that glass slurry coatings are printed and sprayed on the surfaces to be sealed of the upper glass substrate and the lower glass substrate, then the low-melting-point metal edge sealing material is connected with one of the glass substrates by ultrasonic welding, the low-melting-point metal edge sealing material is a sheet or strip metal material, the melting point is low, the low-temperature sealing requirement can be met, the anodic bonding vacuum glass is used for further reducing the sealing temperature, the sealing quality is improved, and the low-temperature high-strength edge sealing process is realized. The sealing method can finish the sealing of the vacuum glass at the sealing temperature of 250-350 ℃, and the sealing quality is good. The invention provides a novel composite sealing method and a technical scheme for the edge sealing of the vacuum glass, improves the sealing process of the vacuum glass and provides a novel solution for preparing the vacuum glass with excellent performance.
Description
Technical Field
The invention relates to the technical field of vacuum glass manufacturing, in particular to vacuum glass with a composite layer sealing structure and an anodic bonding packaging method thereof.
Background
Collins and the original physical system professor Tangjian of Beijing university cooperate positively in the university of Sydney professor R.E. Collins in 1989, and the vacuum glass is successfully developed for the first time. Then, Japan plate glass society (NSG) obtains the patent right of vacuum glass of Sydney university, and establishes the first vacuum glass production line in the world in Kyoto, Japan, thereby realizing the industrialization of the vacuum glass. In 1998, the vacuum glass research in China started from the professor of Tangjian Zheng and Hui nationality. Then, a Beijing New foundational vacuum glass technology company Limited is created, and becomes a second enterprise in the world which masters the vacuum glass manufacturing technology. The new foundational company applies for a plurality of Chinese patents, solves some technical problems in the development of vacuum glass, wherein the technical problems comprise selection of vacuum glass support materials, edge sealing, vacuum pumping and the like, and promotes the research and development of the vacuum glass.
The vacuum glass is composed of two pieces of flat glass, the flat glass is uniformly separated by a support, the periphery of the flat glass is sealed by melting low-melting-point glass or metal solder, and the vacuum glass is vacuumized through air holes reserved on the flat glass. In order to achieve the best heat preservation and heat insulation performance, at least one of the two pieces of flat glass of the vacuum glass is low-emissivity glass. The heat transfer of the central part of the vacuum glass is composed of radiation heat transfer, support heat transfer and residual gas heat transfer 3 parts. The vacuum glass is used as new-generation energy-saving glass, has wide market prospect in the field of energy conservation and environmental protection due to excellent heat preservation, heat insulation and sound insulation performance, and can be widely applied to a plurality of fields such as building doors, windows and curtain walls, refrigerating cabinets, photovoltaic solar power generation, vehicles, ships and the like.
The sealing material of vacuum glass can be roughly classified into a metal material, an organic material and an inorganic material in terms of chemical composition. The metal sealing material mainly comprises silver, aluminum, soldering tin and indium alloy solder. The organic material includes high molecular materials such as silicone rubber, butyl rubber, silicone resin and the like. The organic sealing material has simple process, does not need to be sealed at higher temperature, can meet the use conditions of most of Low-E films, but is easy to age, Low in sealing strength and poor in air tightness. The inorganic material is mainly low-melting-point glass powder, but generally contains lead element, and is not friendly to the environment. The metal material can be sealed at a lower temperature, and is firm in sealing and good in air tightness.
In contrast, the following patents and documents mainly exist in China:
patent No. CN103373805A proposes uniformly coating the edges of flat glass with glass solder, curing the glass, laminating, and then heat sealing. However, the sealing temperature adopted by the method is 430 ℃, which exceeds the sealing limit temperature of the vacuum glass. Patent CN102079631A proposes sintering a metallized layer on a glass plate and hermetically sealing the edges of two glass plates based on the metallized layer. The sealing temperature of the method is less than 350 ℃, the air tightness is ensured, but the sealing strength cannot be greatly improved. Patent No. CN 105439480 a proposes to prefabricate a metallization layer on a glass substrate, place a metal solder on the metallization layer, locally heat the metallization layer to solidify the metal solder, and finally join the sheets to complete sealing by heating. Lujia, the university of harbin industry, proposed in the paper to seal vacuum glass with tin-aluminum alloy and to use anodic bonding techniques to achieve low temperature sealing. The specific patent conditions are shown in Table 1.
TABLE 1 comparison of edge sealing methods for vacuum glass
Disclosure of Invention
The invention aims to provide vacuum glass with a composite layer sealing structure and an anodic bonding packaging method thereof aiming at the technical problems of the existing vacuum glass.
In order to achieve the purpose, the invention adopts the following technical scheme: the vacuum glass of the composite layer sealing structure comprises a sealing structure layer and two glass substrates, wherein the sealing structure layer is positioned between the two glass substrates and is arranged along the edge parts of the glass substrates; the sealing structure layer is a composite layer sealing structure; the composite layer sealing structure consists of a low-melting-point metal edge sealing material and two glass slurry layers, wherein the upper surface and the lower surface of the low-melting-point metal edge sealing material are respectively provided with one glass slurry layer.
An anode bonding packaging method for vacuum glass with a composite layer sealing structure comprises the steps of printing and spraying a low-melting-point glass paste coating on the surface to be sealed of a glass substrate, wherein the spraying thickness is 0.02-0.05 mm; and then, pre-welding a low-melting-point metal edge sealing material (a low-melting-point metal sheet) on the coating by adopting ultrasonic welding, and finally carrying out anodic bonding packaging.
The anode bonding packaging method of the vacuum glass with the composite layer sealing structure is characterized by comprising the following steps of:
1) performing surface cleaning pretreatment on the glass substrate and the low-melting-point metal edge sealing material;
2) preparing low-melting-point glass slurry: coating low-melting-point glass slurry on the surfaces to be sealed of the upper and lower glass substrates by a printing and spraying technology, and heating the glass substrates to solidify the low-melting-point glass slurry coating to form a glass slurry layer;
3) fixing the low-melting-point metal edge sealing material on the glass slurry layer of one glass substrate by adopting ultrasonic welding;
4) overlapping two glass substrates, placing the two glass substrates into an anodic bonding device, vacuumizing, setting bonding temperature, bonding voltage and bonding time, and bonding; the bonding temperature is 250-350 ℃, the bonding voltage is 400-600V, and the bonding time is 20-60 min;
and closing the voltage and temperature switches after bonding is finished, cooling to room temperature, and taking out to finish sealing (the shear strength of the vacuum glass after sealing is not less than 2.0 MPa).
The low-melting-point glass powder can be one of a vanadate system, a phosphate system, a bismuthate system and a borate system or a glass system formed by compounding two or more of the vanadate system, the phosphate system, the bismuthate system and the borate system.
Glass transition temperature T of selected low-melting-point glass powderg230 to 400 ℃ and a glass softening temperature Tf300 to 500 ℃ and a thermal expansion coefficient alpha of 80 to 120 x 10-7/℃。
Preparing the low-melting-point glass slurry: mixing terpineol and ethyl cellulose according to the mass ratio of the terpineol to the ethyl cellulose of (94-98) to (2-6) to obtain a mixed solution; according to the method, the method comprises the following steps of: the mass ratio of the mixed solution is 1 (1-1.4), the low-melting-point glass powder and the mixed solution are mixed, magnetic stirring is carried out for 0.5h, and then low-melting-point glass slurry is obtained, wherein the spraying thickness of the low-melting-point glass slurry is 0.02-0.05 mm.
The low-melting-point metal edge sealing material can be in a strip shape or a sheet shape, and the thickness of the low-melting-point metal edge sealing material is 0.05-0.1 mm.
The melting point of the low-melting-point metal edge sealing material is 120-220 ℃.
The low-melting-point metal edge sealing material is one of indium tin alloy, tin bismuth alloy, indium silver alloy and tin indium silver alloy.
The glass substrate is common glass, coated glass or toughened glass.
The surface to be sealed of the glass substrate is etched with grains or has certain roughness, and the roughness is as follows: the sealing strength of the vacuum glass is further improved, wherein the Ra is less than 0.8 mu m and less than 3.2 mu m.
The Low-melting-point material has lower melting temperature, so that the thermal stress generated in the heating edge sealing process is lower, the use performance requirement of the Low-e glass can be ensured, and the anodic bonding technology has the advantages of simple process, Low bonding temperature, small residual stress, high bonding strength, good sealing performance and the like.
The invention has the beneficial effects that:
1) the product of the invention has wide application range, can be used for sealing of various materials such as glass, ceramics, metal and the like, has good sealing performance, and the shear strength of vacuum glass after sealing is not less than 2.0 MPa.
2) The uniform combination is formed on the interface, the combination strength is high, the air tightness is good, and the method can be used for packaging vacuum glass.
3) The metal edge sealing material adopted by the invention can be used for sealing at 250-350 ℃, so that the performances of toughened glass and coated glass are ensured.
4) The invention applies the anodic bonding packaging technology to the vacuum glass packaging process, and can effectively improve the sealing quality while reducing the sealing temperature.
Drawings
FIG. 1 is a schematic view of the structure of the vacuum glass of the present invention.
FIG. 2 is a schematic view of anodic bonding sealing in accordance with the present invention.
Fig. 3 is a picture of a sample after anode bonding sealing and sealing performance test in example 1 of the present invention.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the sealing structure of the low melting point metal and glass composite layer for vacuum glass and the anodic bonding packaging method proposed by the present invention are described in detail below with reference to the accompanying drawings.
In the following examples: the vacuum glass of the composite layer sealing structure comprises the composite layer sealing structure and two glass substrates, wherein the composite layer sealing structure is positioned between the two glass substrates and is arranged along the edge parts of the glass substrates; the composite layer sealing structure consists of a low-melting-point metal edge sealing material (or called low-melting-point metal sheet, the same below) and two glass slurry layers, wherein the upper surface and the lower surface of the low-melting-point metal edge sealing material are respectively provided with one glass slurry layer.
Example 1
An anodic bonding packaging method for vacuum glass with a composite layer sealing structure comprises the steps of prefabricating a glass slurry coating on a glass substrate, then adopting ultrasonic welding on the coating of one glass substrate to enable the slurry coating to form welding combination with a low-melting-point metal sheet, and finally carrying out anodic bonding sealing on the vacuum glass. The preparation process comprises the following steps:
1) carrying out surface cleaning pretreatment on the glass substrate and the low-melting-point metal sheet, and etching lines on the surface to be sealed of the glass substrate;
2) prefabricating V on the surface of the glass substrate to be sealed by adopting a printing and spraying mode2O5-TeO2A glass paste coating having a thickness of 0.02 mm;
3) drying the slurry coating at 150 ℃ to enable the slurry coating to be solidified with the glass plate;
4) ultrasonic welding of sheet-like In52Sn48(low-melting-point metal edge sealing materials or low-melting-point metal sheets) are welded and combined with the slurry coating of one glass substrate, wherein the thickness of the metal sheets is 0.1 mm;
5) overlapping the glass substrate coated with the glass slurry and the glass substrate pre-welded with the metal sheet, putting the glass substrate and the glass substrate into an anodic bonding device for vacuum glass sealing, vacuumizing, and setting the bonding temperature at 280 ℃, the bonding voltage at 600V and the bonding time for 20 min; and closing the voltage and temperature switches after bonding is finished, cooling to room temperature, taking out, and finishing sealing.
In this example, the final sealing temperature was 250 ℃ and the shear strength after sealing was 2.1 MPa.
Example 2
An anodic bonding packaging method for vacuum glass with a composite layer sealing structure comprises the steps of prefabricating a glass slurry coating on a glass substrate, solidifying the slurry and the glass substrate, then adopting ultrasonic welding on the coating of one glass substrate to form firm bonding with a low-melting-point metal sheet, and finally carrying out anodic bonding sealing on the vacuum glass. The preparation process comprises the following steps:
1) carrying out surface cleaning pretreatment on the glass substrate and the low-melting-point metal sheet, and etching lines on the surface to be sealed of the glass substrate;
2) prefabricating V on the surface of the glass substrate to be sealed by adopting a printing and spraying mode2O5-P2O5-Li2An O glass paste coating layer with a thickness of 0.02 mm;
3) drying the slurry coating at 150 ℃ to enable the slurry coating to be solidified with the glass plate;
4) ultrasonic welding of band-shaped Sn42Bi58The glass substrate is welded and combined with the slurry coating of one glass substrate, wherein the thickness of the metal sheet is 0.1 mm;
5) overlapping the glass substrate coated with the glass slurry and the glass substrate pre-welded with the metal sheet, putting the glass substrate and the glass substrate into an anodic bonding device for vacuum glass sealing, vacuumizing, and setting the bonding temperature at 300 ℃, the bonding voltage at 400V and the bonding time for 20 min; and closing the voltage and temperature switches after bonding is finished, cooling to room temperature, taking out, and finishing sealing.
In this example, the final sealing temperature was 300 ℃ and the shear strength after sealing was 2.03 MPa.
Example 3
An anodic bonding packaging method for vacuum glass with a composite layer sealing structure comprises the steps of prefabricating a glass slurry coating on a glass substrate, then adopting ultrasonic welding on the coating of one glass substrate to enable the slurry coating to form welding combination with a low-melting-point metal sheet, and finally carrying out anodic bonding sealing on the vacuum glass. The preparation process comprises the following steps:
1) carrying out surface cleaning pretreatment on the glass substrate and the low-melting-point metal sheet, and etching lines on the surface to be sealed of the glass substrate;
2) prefabricating V on the surface of the glass substrate to be sealed by adopting a printing and spraying mode2O5-P2O5-B2O3Glass paste coatingA layer having a thickness of 0.05 mm;
3) drying the slurry coating at 150 ℃ to enable the slurry coating to be solidified with the glass plate;
4) ultrasonic welding of flaky Sn42Bi58The glass substrate is welded and combined with the slurry coating of one glass substrate, wherein the thickness of the metal sheet is 0.05 mm;
5) overlapping the glass substrate coated with the glass slurry and the glass substrate pre-welded with the metal sheet, putting the glass substrate and the glass substrate into an anodic bonding device for vacuum glass sealing, vacuumizing, and setting the bonding temperature at 300 ℃, the bonding voltage at 400V and the bonding time for 40 min; and closing the voltage and temperature switches after bonding is finished, cooling to room temperature, taking out, and finishing sealing.
In this example, the final sealing temperature was 300 ℃ and the shear strength after sealing was 2.12 MPa.
Example 4
An anodic bonding packaging method for vacuum glass with a composite layer sealing structure comprises the steps of prefabricating a glass slurry coating on a glass substrate, then adopting ultrasonic welding on the coating of one glass substrate to enable the slurry coating to form welding combination with a low-melting-point metal sheet, and finally carrying out anodic bonding sealing on the vacuum glass. The preparation process comprises the following steps:
1) carrying out surface cleaning pretreatment on the glass substrate and the low-melting-point metal sheet, and enabling the surface of the glass substrate to be sealed to have the roughness Ra of 0.8 mu m by adopting a machining method;
2) prefabricating V on the surface of the glass substrate to be sealed by adopting a printing and spraying mode2O5-B2O3-a ZnO glass paste coating with a thickness of 0.05 mm;
3) drying the slurry coating at 150 ℃ to enable the slurry coating to be solidified with the glass plate;
4) ultrasonic welding of flaky Sn77.2In20Ag2.8Welded to the paste coating of one of the glass substrates, the thickness of the metal sheetIs 0.05 mm;
5) overlapping the glass substrate coated with the glass slurry and the glass substrate pre-welded with the metal sheet, placing the glass substrate and the glass substrate into an anodic bonding device, vacuumizing, and setting the bonding temperature to be 320 ℃, the bonding voltage to be 600V and the bonding time to be 30 min; and after bonding is finished, closing the voltage and temperature switches, cooling to room temperature, and finishing sealing.
In this embodiment, a final sealing temperature of the vacuum glass with a composite layer sealing structure and an anodic bonding packaging method thereof is 300 ℃, and a shear strength after sealing is 2.2 MPa.
Example 5
An anodic bonding packaging method for vacuum glass with a composite layer sealing structure comprises the steps of prefabricating a glass slurry coating on a glass substrate, then adopting ultrasonic welding on the coating of one glass substrate to enable the slurry coating to form welding combination with a low-melting-point metal sheet, and finally carrying out anodic bonding sealing on the vacuum glass. The preparation process comprises the following steps:
1) carrying out surface cleaning pretreatment on the glass substrate and the low-melting-point metal sheet, and enabling the surface of the glass substrate to be sealed to have the roughness Ra of 1.2 mu m by adopting a machining method;
2) prefabricating B on the surface of the glass substrate to be sealed by adopting a printing and spraying mode2O3-a coating of BaO-ZnO glass paste with a thickness of 0.04 mm;
3) drying the slurry coating at 150 ℃ to enable the slurry coating to be solidified with the glass plate;
4) ultrasonic welding of flaky Sn77.2In20Ag2.8The glass substrate is welded and combined with the slurry coating of one glass substrate, and the thickness of the glass substrate is 0.1 mm;
5) overlapping the glass substrate coated with the glass slurry and the glass substrate pre-welded with the metal sheet, putting the glass substrate and the glass substrate into an anodic bonding device for vacuum glass sealing, vacuumizing, and setting the bonding temperature to be 320 ℃, the bonding voltage to be 400V and the bonding time to be 20 min; and closing the voltage and temperature switches after bonding is finished, cooling to room temperature, taking out, and finishing sealing.
In this embodiment, the final sealing temperature of the vacuum glass with a composite layer sealing structure and the anodic bonding packaging method thereof is 320 ℃, and the shear strength after sealing is 2.15 MPa.
Example 6
An anodic bonding packaging method for vacuum glass with a composite layer sealing structure comprises the steps of prefabricating a glass slurry coating on a glass substrate, then adopting ultrasonic welding on the coating of one glass substrate to enable the slurry coating to form welding combination with a low-melting-point metal sheet, and finally carrying out anodic bonding sealing on the vacuum glass. The preparation process comprises the following steps:
1) carrying out surface cleaning pretreatment on the glass substrate and the low-melting-point metal sheet, and enabling the surface of the glass substrate to be sealed to have the roughness Ra of 1.6 mu m by adopting a machining method;
2) prefabricating the glass substrate B on the surface to be sealed by adopting a printing and spraying mode2O3-ZnO-Bi2O3Glass slurry coating, the thickness of the metal sheet is 0.05 mm;
3) drying the slurry coating at 150 ℃ to enable the slurry coating to be solidified with the glass plate;
4) ultrasonic welding of flaky Sn42Bi58The glass substrate is welded and combined with the slurry coating of one glass substrate, and the thickness of the glass substrate is 0.07 mm;
5) overlapping the glass substrate coated with the glass slurry and the glass substrate pre-welded with the metal sheet, placing the glass substrate and the glass substrate into an anodic bonding device, vacuumizing, and setting the bonding temperature to be 350 ℃, the bonding voltage to be 600V and the bonding time to be 20 min; and closing the voltage and temperature switches after bonding is finished, cooling to room temperature, taking out, and finishing sealing.
In this embodiment, a final sealing temperature of the vacuum glass with a composite layer sealing structure and an anodic bonding packaging method thereof is 340 ℃, and a shear strength after sealing is 2.3 MPa.
Example 7
An anodic bonding packaging method for vacuum glass with a composite layer sealing structure comprises the steps of prefabricating a glass slurry coating on a glass substrate, then adopting ultrasonic welding on the coating of one glass substrate to enable the slurry coating to form welding combination with a low-melting-point metal sheet, and finally carrying out anodic bonding sealing on the vacuum glass. The preparation process comprises the following steps:
1) carrying out surface cleaning pretreatment on the glass substrate and the low-melting-point metal sheet, and enabling the surface of the glass substrate to be sealed to have the roughness Ra of 1.2 mu m by adopting a machining method;
2) prefabricating the glass substrate B on the surface to be sealed by adopting a printing and spraying mode2O3-SnO-ZnO glass slurry coating, the thickness of the metal sheet being 0.05 mm;
3) drying the slurry coating at 150 ℃ to enable the slurry coating to be solidified with the glass plate;
4) ultrasonic welding of flaky Sn42Bi58The glass substrate is welded and combined with the slurry coating of one glass substrate, wherein the thickness of the metal sheet is 0.07 mm;
5) overlapping the glass substrate coated with the glass slurry and the glass substrate pre-welded with the metal sheet, placing the glass substrate and the glass substrate into an anodic bonding device, vacuumizing, and setting the bonding temperature to be 350 ℃, the bonding voltage to be 600V and the bonding time to be 20 min; and closing the voltage and temperature switches after bonding is finished, cooling to room temperature, taking out, and finishing sealing.
In this embodiment, a final sealing temperature of the vacuum glass with a composite layer sealing structure and an anodic bonding packaging method thereof is 310 ℃, and a shear strength after sealing is 2.3 MPa.
Example 8
An anodic bonding packaging method for vacuum glass with a composite layer sealing structure comprises the steps of prefabricating a glass slurry coating on a glass substrate, then adopting ultrasonic welding on the coating of one glass substrate to enable the slurry coating to form welding combination with a low-melting-point metal sheet, and finally carrying out anodic bonding sealing on the vacuum glass. The preparation process comprises the following steps:
1) carrying out surface cleaning pretreatment on the glass substrate and the low-melting-point metal sheet, and enabling the surface of the glass substrate to be sealed to have the roughness Ra of 2.0 mu m by adopting a machining method;
2) prefabricating the glass substrate B on the surface to be sealed by adopting a printing and spraying mode2O3-ZnO-Bi2O3A glass paste coating, wherein the thickness of the metal sheet is 0.03 mm;
3) drying the slurry coating at 150 ℃ to enable the slurry coating to be solidified with the glass plate;
4) ultrasonic welding of flaky Sn88Ag3.5Bi0.5In8.0The glass substrate is welded and combined with the slurry coating of one glass substrate, and the thickness of the glass substrate is 0.1 mm;
5) overlapping the glass substrate coated with the glass slurry and the glass substrate pre-welded with the metal sheet, putting the glass substrate and the glass substrate into an anodic bonding device for vacuum glass sealing, vacuumizing, and setting the bonding temperature to be 340 ℃, the bonding voltage to be 500V and the bonding time to be 30 min; and closing the voltage and temperature switches after bonding is finished, cooling to room temperature, taking out, and finishing sealing.
In this embodiment, the final sealing temperature of the vacuum glass with a composite layer sealing structure and the anodic bonding packaging method thereof is 340 ℃, and the shear strength after sealing is 2.06 MPa.
Example 9
An anodic bonding packaging method for vacuum glass with a composite layer sealing structure comprises the steps of prefabricating a glass slurry coating on a glass substrate, then adopting ultrasonic welding on the coating of one glass substrate to enable the slurry coating to form welding combination with a low-melting-point metal sheet, and finally carrying out anodic bonding sealing on the vacuum glass. The preparation process comprises the following steps:
1) carrying out surface cleaning pretreatment on the glass substrate and the low-melting-point metal sheet, and enabling the surface of the glass substrate to be sealed to have the roughness Ra of 2.2 mu m by adopting a machining method;
2) prefabricating P on the surface of the glass substrate to be sealed by adopting a printing and spraying mode2O5-a ZnO-SnO glass slurry coating having a thickness of 0.05 mm;
3) drying the slurry coating at 150 ℃ to enable the slurry coating to be solidified with the glass plate;
4) ultrasonic welding of flaky Sn77.2In20Ag2.8The glass substrate is welded and combined with the slurry coating of one glass substrate, and the thickness of the metal sheet in the thickness is 0.05 mm;
5) overlapping the glass substrate coated with the glass slurry and the glass substrate pre-welded with the metal sheet, placing the glass substrate and the glass substrate into an anodic bonding device, vacuumizing, and setting the bonding temperature to be 320 ℃, the bonding voltage to be 400V and the bonding time to be 20 min; and closing the voltage and temperature switches after bonding is finished, cooling to room temperature, taking out, and finishing sealing.
In this embodiment, the final sealing temperature of the vacuum glass with a composite layer sealing structure and the anodic bonding packaging method thereof is 320 ℃, and the shear strength after sealing is 2.3 MPa.
Example 10
An anodic bonding packaging method for vacuum glass with a composite layer sealing structure comprises the steps of prefabricating a glass slurry coating on a glass substrate, then adopting ultrasonic welding on the coating of one glass substrate to enable the slurry coating to form welding combination with a low-melting-point metal sheet, and finally carrying out anodic bonding sealing on the vacuum glass. The preparation process comprises the following steps:
1) carrying out surface cleaning pretreatment on the glass substrate and the low-melting-point metal sheet, and enabling the surface of the glass substrate to be sealed to have the roughness Ra of 2.6 mu m by adopting a machining method;
2) prefabricating P in the region of the glass substrate to be sealed by adopting a printing and spraying mode2O5-ZnO-B2O3A glass paste coating having a thickness of 0.05 mm;
3) drying the slurry coating at 150 ℃ to enable the slurry coating to be solidified with the glass plate;
4) ultrasonic welding of flaky Sn77.2In20Ag2.8The glass substrate is welded and combined with the slurry coating of one glass substrate, and the thickness of the metal is 0.05 mm;
5) overlapping the glass substrate coated with the glass slurry and the glass substrate pre-welded with the metal sheet, putting the glass substrate and the glass substrate into an anodic bonding device for vacuum glass sealing, vacuumizing, and setting the bonding temperature to be 320 ℃, the bonding voltage to be 400V and the bonding time to be 20 min; and closing the voltage and temperature switches after bonding is finished, cooling to room temperature, taking out, and finishing sealing.
In this embodiment, the final sealing temperature of the vacuum glass with a composite layer sealing structure and the anodic bonding packaging method thereof is 320 ℃, and the shear strength after sealing is 2.3 MPa.
Example 11
An anodic bonding packaging method for vacuum glass with a composite layer sealing structure comprises the steps of prefabricating a glass slurry coating on a glass substrate, then adopting ultrasonic welding on the coating of one glass substrate to enable the slurry coating to form welding combination with a low-melting-point metal sheet, and finally carrying out anodic bonding sealing on the vacuum glass. The preparation process comprises the following steps:
1) carrying out surface cleaning pretreatment on the glass substrate and the low-melting-point metal sheet, and enabling the surface of the glass substrate to be sealed to have the roughness Ra of 3.0 mu m by adopting a machining method;
2) prefabricating P on the surface of the glass substrate to be sealed by adopting a printing and spraying mode2O5-ZnO-Sb2O3A glass paste coating having a thickness of 0.05 mm;
3) drying the slurry coating at 150 ℃ to enable the slurry coating to be solidified with the glass plate;
4) ultrasonic welding of flaky Sn77.2In20Ag2.8The glass substrate is welded and combined with the slurry coating of one glass substrate, and the thickness of the metal sheet is 0.05 mm;
5) overlapping the glass substrate coated with the glass slurry and the glass substrate pre-welded with the metal sheet, putting the glass substrate and the glass substrate into an anodic bonding device for vacuum glass sealing, vacuumizing, and setting the bonding temperature to be 320 ℃, the bonding voltage to be 400V and the bonding time to be 20 min; and closing the voltage and temperature switches after bonding is finished, cooling to room temperature, taking out, and finishing sealing.
In this embodiment, the final sealing temperature of the vacuum glass with a composite layer sealing structure and the anodic bonding packaging method thereof is 320 ℃, and the shear strength after sealing is 2.3 MPa.
Example 12
An anodic bonding packaging method for vacuum glass with a composite layer sealing structure comprises the steps of prefabricating a glass slurry coating on a glass substrate, then adopting ultrasonic welding on the coating of one glass substrate to enable the slurry coating to form welding combination with a low-melting-point metal sheet, and finally carrying out anodic bonding sealing on the vacuum glass. The preparation process comprises the following steps:
1) carrying out surface cleaning pretreatment on the glass substrate and the low-melting-point metal sheet, and enabling the surface of the glass substrate to be sealed to have the roughness Ra of 3.2 mu m by adopting a machining method;
2) bi is prefabricated on the surface of the glass substrate to be sealed by adopting a printing and spraying mode2O3-ZnO-B2O-glass paste coatingThe thickness of the film is 0.03 mm;
3) drying the slurry coating at 150 ℃ to enable the slurry coating to be solidified with the glass plate;
4) ultrasonic welding of flaky Sn42Bi58The glass substrate is welded and combined with the slurry coating of one glass substrate, wherein the thickness of the metal sheet is 0.1 mm;
5) overlapping the glass substrate coated with the glass slurry and the glass substrate pre-welded with the metal sheet, putting the glass substrate and the glass substrate into an anodic bonding device for vacuum glass sealing, vacuumizing, and setting the bonding temperature to be 320 ℃, the bonding voltage to be 600V and the bonding time to be 60 min; and closing the voltage and temperature switches after bonding is finished, cooling to room temperature, taking out, and finishing sealing.
In this embodiment, a final sealing temperature of the vacuum glass with a composite layer sealing structure and an anodic bonding packaging method thereof is 320 ℃, and a shear strength after sealing is 2.1 MPa.
Example 13
An anodic bonding packaging method for vacuum glass with a composite layer sealing structure comprises the steps of prefabricating a glass slurry coating on a glass substrate, then adopting ultrasonic welding on the coating of one glass substrate to enable the slurry coating to form welding combination with a low-melting-point metal sheet, and finally carrying out anodic bonding sealing on the vacuum glass. The preparation process comprises the following steps:
1) carrying out surface cleaning pretreatment on the glass substrate and the low-melting-point metal sheet, and enabling the surface of the glass substrate to be sealed to have the roughness Ra of 3.2 mu m by adopting a machining method;
2) bi is prefabricated on the surface of the glass substrate to be sealed by adopting a printing and spraying mode2O3-B2O3-a coating of BaO glass paste with a thickness of 0.03 mm;
3) drying the slurry coating at 150 ℃ to enable the slurry coating to be solidified with the glass plate;
4) ultrasonic welding of flaky Sn42Bi58With one of the sheets of glassThe slurry coating of the substrate is welded and combined, wherein the thickness of the metal sheet is 0.1 mm;
5) overlapping the glass substrate coated with the glass slurry and the glass substrate pre-welded with the metal sheet, putting the glass substrate and the glass substrate into an anodic bonding device for vacuum glass sealing, vacuumizing, and setting the bonding temperature to be 320 ℃, the bonding voltage to be 600V and the bonding time to be 60 min; and closing the voltage and temperature switches after bonding is finished, cooling to room temperature, taking out, and finishing sealing.
In this embodiment, a final sealing temperature of the vacuum glass with a composite layer sealing structure and an anodic bonding packaging method thereof is 320 ℃, and a shear strength after sealing is 2.1 MPa.
Claims (10)
1. The vacuum glass of the composite layer sealing structure comprises a sealing structure layer and two glass substrates, wherein the sealing structure layer is positioned between the two glass substrates and is arranged along the edge parts of the glass substrates; the sealing structure layer is a composite layer sealing structure; the composite layer sealing structure consists of a low-melting-point metal edge sealing material and two glass slurry layers, wherein the upper surface and the lower surface of the low-melting-point metal edge sealing material are respectively provided with one glass slurry layer.
2. The anode bonding packaging method of the vacuum glass with the composite layer sealing structure is characterized by comprising the following steps of:
1) performing surface cleaning pretreatment on the glass substrate and the low-melting-point metal edge sealing material;
2) preparing low-melting-point glass slurry: coating low-melting-point glass slurry on the surfaces to be sealed of the upper and lower glass substrates by a printing and spraying technology, and heating the glass substrates to solidify the low-melting-point glass slurry coating to form a glass slurry layer;
3) fixing the low-melting-point metal edge sealing material on the glass slurry layer of one glass substrate by adopting ultrasonic welding;
4) overlapping two glass substrates, placing the two glass substrates into an anodic bonding device, vacuumizing, setting bonding temperature, bonding voltage and bonding time, and bonding; the bonding temperature is 250-350 ℃, the bonding voltage is 400-600V, and the bonding time is 20-60 min;
and closing the voltage and temperature switches after bonding is finished, cooling to room temperature, taking out, and finishing sealing.
3. The method as claimed in claim 2, wherein the low-melting glass frit is selected from a vanadate system, a phosphate system, a bismuthate system, and a borate system, and a glass system formed by combining two or more of them.
4. The anodic bonding packaging method for vacuum glass with composite layer sealing structure as claimed in claim 2 or 3, wherein the glass transition temperature T of the selected low melting point glass powderg230 to 400 ℃ and a glass softening temperature Tf300 to 500 ℃ and a thermal expansion coefficient alpha of 80 to 120 x 10-7/℃。
5. The anodic bonding packaging method for vacuum glass with a composite layer sealing structure according to claim 2, wherein the preparation of the low-melting-point glass paste comprises the following steps: mixing terpineol and ethyl cellulose according to the mass ratio of the terpineol to the ethyl cellulose of (94-98) to (2-6) to obtain a mixed solution; according to the method, the method comprises the following steps of: the mass ratio of the mixed solution is 1 (1-1.4), the low-melting-point glass powder and the mixed solution are mixed, magnetic stirring is carried out for 0.5h, and then low-melting-point glass slurry is obtained, wherein the spraying thickness of the low-melting-point glass slurry is 0.02-0.05 mm.
6. The anodic bonding packaging method for vacuum glass with a composite layer sealing structure according to claim 2, wherein the low melting point metal edge sealing material is in a strip shape or a sheet shape, and the thickness is 0.05-0.1 mm.
7. The anodic bonding packaging method for vacuum glass with a composite layer sealing structure according to claim 2, wherein the melting point of the low-melting-point metal edge sealing material is 120-220 ℃.
8. The anodic bonding packaging method for vacuum glass with a composite layer sealing structure according to claim 2, wherein the low melting point metal edge sealing material is one of indium tin alloy, tin bismuth alloy, indium silver alloy and tin indium silver alloy.
9. The anodic bonding packaging method for vacuum glass with a composite layer sealing structure as claimed in claim 2, wherein the glass substrate is made of common glass, coated glass or toughened glass.
10. The anodic bonding packaging method for vacuum glass with a composite layer sealing structure as claimed in claim 2, wherein the surface to be sealed of the glass substrate is textured or made to have a certain roughness, and the roughness is: 0.8 μm < Ra <3.2 μm.
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