CN113698112B - Preparation method of tailless vacuum glass - Google Patents
Preparation method of tailless vacuum glass Download PDFInfo
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- CN113698112B CN113698112B CN202111136096.0A CN202111136096A CN113698112B CN 113698112 B CN113698112 B CN 113698112B CN 202111136096 A CN202111136096 A CN 202111136096A CN 113698112 B CN113698112 B CN 113698112B
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Images
Classifications
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Joining Of Glass To Other Materials (AREA)
Abstract
The invention discloses a preparation method of tailless vacuum glass in the field of vacuum glass production, which comprises the following steps: A. metallization treatment, namely coating metal slurry on the areas to be sealed of the upper glass and the lower glass and sintering, wherein the metal slurry comprises a glass phase, an organic phase and a metal phase; B. laying a support and metal solder; C. carrying out plasma bombardment treatment on the surface of the glass in vacuum; D. the two pieces of glass are butted in vacuum; E. heating and sealing the area where the metal solder is distributed; F. cooling to obtain the tailless vacuum glass. The invention can overcome the problem of air leakage risk caused by the arrangement of the air extraction opening on the vacuum glass in the prior art.
Description
Technical Field
The invention relates to the field of vacuum glass production, in particular to a preparation method of tailless vacuum glass.
Background
The vacuum glass is a new generation of energy-saving and environment-friendly glass, and has obvious product performance advantages compared with commonly used glass products such as common single-layer toughened glass, double-layer hollow glass and the like. The composite material has the advantages of sound insulation performance, heat preservation performance and anti-condensation function, has high-efficiency energy-saving effect and environment pollution reduction effect in wide fields of buildings, refrigeration and heating electric appliances, traffic and the like, and has very large potential and application market.
The vacuum glass is essentially formed by packaging two pieces of common toughened glass through an airtight sealing material, wherein the airtight sealing mostly adopts low-temperature glass powder or flexible metal soft solder, a vacuum layer with the thickness of 0.3-0.4 mm is formed between the two pieces of glass through vacuum, metal supports are arranged between the two pieces of glass in an array manner to offset atmospheric pressure, and an air suction opening is reserved on one piece of glass so as to conveniently suck air from the vacuum layer to form vacuum. In the prior art, the low-temperature glass powder sealing technology for vacuum glass is less adopted due to the problems of overhigh temperature and reduced mechanical property of the vacuum glass, and the flexible metal soft solder sealing technology has the defects that the components of a sealing layer are complex because metal materials and glass are different from homogeneous materials and extra materials are required to be added into the sealing layer, so that the thermal expansion coefficients of all layers of the sealing material are not matched, great residual thermal stress can be generated in the sealing treatment process, and the mechanical strength of the vacuum glass can be influenced. In the vacuumizing process, an air pumping opening with the thickness ranging from a few millimeters to 1-2 millimeters is reserved in the prior art, or the vacuum degree of a vacuum layer of the vacuum glass is realized by vacuumizing through a glass tube or slowly exhausting the vacuum glass in a vacuum environment, and finally the air pumping opening is sealed off. The process is an important reason for the low production speed of the traditional vacuum glass, the extraction opening is too small, the flow conductance is very large during the extraction, the extraction speed is very small, the production period of the single vacuum glass is very long, even the extraction time is calculated by hours, and the process is not suitable for large-scale production. Meanwhile, after the vacuum degree of the vacuum layer is reduced to a certain value, the free path of gas molecules is large, the gas molecules are difficult to diffuse out from a small air suction opening, the vacuum degree far away from the air suction opening is greatly different from the vacuum degree near the air suction opening, and the vacuum degree of the vacuum layer cannot be reached, so that the product performance of the vacuum glass is greatly influenced. The reserved air extraction opening is obtained by mechanically drilling the common float glass before tempering, and microcracks inevitably occur at the edge of the air extraction opening, so that the air leakage risk is great in the later period.
Disclosure of Invention
The invention aims to provide a preparation method of tailless vacuum glass, which aims to solve the problem of air leakage risk caused by the arrangement of an air extraction opening on the vacuum glass in the prior art.
In order to achieve the purpose, the basic technical scheme of the invention is as follows: a preparation method of tailless vacuum glass comprises the following steps:
A. metallization treatment, namely coating metal slurry on the to-be-sealed areas of the upper glass and the lower glass and sintering, wherein the metal slurry comprises 3-7 parts by mass of a glass phase, 5-20 parts by mass of an organic phase and 50-90 parts by mass of a metal phase;
B. laying a support on one glass sheet, and laying metal solder on the region to be sealed;
C. two pieces of glass are sent into a two-stage vacuum cavity, and after vacuumizing, plasma bombardment treatment is carried out on the upper surface of the lower glass and the lower surface of the upper glass;
D. after vacuumizing in the two-stage vacuum cavity, closing the two pieces of glass;
E. heating to seal the area where the metal solder is distributed;
F. cooling to obtain the tailless vacuum glass.
The invention adopts the complete glass plate for production, adopts the metal slurry with specific components, wherein the glass is connected with the glass plate and the metal phase, ensures the stable and reliable connection, adopts the dosage range to ensure the bonding strength, avoids falling, and cannot influence the subsequent heating welding, adopts the dosage range to ensure the slurry to have good printing performance, adopts the dosage range to ensure the fluidity, ensures that the metal slurry can be stably coated on the glass to form regular distribution, cannot influence the content of the glass phase and the metal phase, adopts the dosage range to ensure the welding effect, avoids the welding, and cannot influence the content of the glass phase and the organic phase. Adopt two-stage vacuum chamber body processing method, wash and the degasification with plasma in the preceding stage vacuum chamber body, get rid of debris such as greasy dirt on glass surface and adsorbed multilayer gas molecule, can effectively cover the whole area of glass, wash, the quality and the efficiency of degasification are higher, need not carry out the degasification through the extraction opening, carry out the piece that closes of whole piece glass in vacuum environment, ensure to close piece back vacuum cavity sealed reliable, do not have the risk of extraction opening gas leakage.
Further, in the step A, the distance between the outer edge of the metal paste and the edge of the glass is 1-5 mm. This is preferred to avoid the metal paste coming off the metallization layer formed by the metal paste as a result of the paste being too close to the glass edge.
Further, the coating width of the metal slurry in the step A is 6-15 mm. It is preferable that the coating width is less than 6mm, the welding area is insufficient, the welding strength is reduced, and the risk of air leakage is increased, and more than 15mm, the heat insulating property of the glass is deteriorated due to the good heat transfer property of the metal paste.
Further, the coating thickness of the metal slurry in the step A is 10-50 μm. Preferably, the coating thickness is less than 10 mu m, the metal slurry layer reacts quickly during welding, over-welding occurs, the glass fails, and the coating thickness is more than 50 mu m, and the metal slurry layer cracks and falls off during welding due to large difference of thermal expansion coefficients of metal and glass.
Further, the sintering temperature in step A is 450-. Preferably, the sintering temperature is lower than 450 ℃, organic components in the slurry can not be completely oxidized and volatilized, the organic components are remained in the metal layer to influence the vacuum in the glass, and the temperature is higher than 800 ℃, the glass is softened and can not be tempered. The sintering at the temperature of 680-800 ℃ can be carried out simultaneously with the glass tempering, and the tempered vacuum glass can be prepared.
Further, the metal solder in step B is tin or a tin-based alloy in a ribbon or wire shape. Preferably, the glass can be easily paved on the periphery of the glass to meet the requirement of the width of the sealing edge.
Further, the step C is completed in a front-stage vacuum cavity of the two-stage vacuum cavity, the vacuum degree of the front-stage vacuum cavity is 100Pa-0.1Pa, and the glass plate is heated at the heating temperature of 150-. Preferably, the gas molecules are too much below the vacuum range to affect the plasma degassing effect, and the time for reaching the vacuum degree is longer above the vacuum range, so that the process time is increased, and the efficiency is reduced. The heating temperature interval is adopted to heat the overflowed gas at most, so that a better auxiliary effect is achieved, and the risk of damaging equipment is caused when the temperature is higher than 200 ℃.
Further, the step D is completed in a vacuum process cavity of the two-stage vacuum cavity, and the vacuum degree of the vacuum process cavity is 10-2-10-5Pa. Preferably, the vacuum degree of the vacuum process cavity is the same as the internal vacuum degree of the vacuum glass product, so that the tailless vacuum glass after the whole piece is combined is reliable in quality, the heat preservation effect is poor below the range, and the product fracture risk is higher above the range.
Further, the heating temperature in the step E is 180-350 ℃. Preferably, the temperature range can effectively melt the solder, and defects such as insufficient soldering, missing soldering, and over soldering can be avoided.
Further, the height of the metal solder in the step B is 1-2mm higher than that of the support. Preferably, the solder melting and welding are ensured to be stable and reliable, if the range is lower than the range, the amount of the molten solder is insufficient, and the phenomenon of poor welding is easy to occur, if the range is higher than the range, the metal layer is torn off due to excessive edge stress.
Drawings
FIG. 1 is a top view of example 14 of the present invention.
Detailed Description
The following is further detailed by way of specific embodiments:
reference numerals in the drawings of the specification include: glass plate 1, sealing layer 2, solid getter 3.
Embodiment 1, a method for preparing tailless vacuum glass, comprising the steps of:
1. metallization treatment, namely coating metal slurry on the to-be-sealed areas of the upper glass and the lower glass and sintering, wherein the coating width of the metal slurry is 6mm, the distance between the outer edge of the metal slurry and the edge of the glass is 1mm, the coating thickness of the metal slurry is 10 mu m, the metal slurry can be Ag, Cu, Ni, Au and other metals and any mixed component slurry thereof, the metal slurry comprises 5 parts by mass of glass phase, 5 parts by mass of organic phase and 90 parts by mass of metal phase, and the glass phase is glass component Bi2O3-SiO2-B2O3-ZnO, wherein Bi is calculated in parts by mass2O3Content 30 parts, SiO2Content 10 parts, B2O325 parts of ZnO and 15 parts of ZnO; the organic phase comprises 28 parts by mass of ethylene glycol monobutyl ether, 28 parts by mass of terpineol, 28 parts by mass of butyl carbite, 7 parts by mass of ethyl cellulose, 6 parts by mass of hydrogenated castor oil and 4 parts by mass of lecithin; the metal phase is one or a mixture of several of metal powders such as Ag, Cu, Ni, Au and the like, and Ag is preferred in the embodiment; the sintering temperature is 450-800 ℃, the glass can be sintered locally or integrally, when the sintering temperature is 650-800 ℃, the slurry sintering and the glass tempering can be carried out simultaneously, and the tempered vacuum glass is prepared;
2. laying a support on one piece of glass, laying a metal solder on a region to be sealed, wherein the metal solder is strip or filiform tin or tin-based alloy, the height of the metal solder is 1-2mm higher than that of the support, and the metal solder can be laid on the edge to be sealed of one piece of glass or the edges to be sealed of two pieces of glass;
3. two pieces of glass are sent into a two-stage vacuum cavity, after the vacuum degree is controlled to be 0.1-100 Pa in a preceding stage vacuum cavity of the two-stage vacuum cavity, plasma bombardment treatment is carried out on the upper surface of the lower glass and the lower surface of the upper glass, a plasma gas source is nitrogen, the glass plate is heated while the plasma bombardment treatment is carried out, and the heating temperature is 150-;
4. vacuumizing the vacuum process cavity of the two-stage vacuum cavity until the vacuum degree is 10-2-10-5After Pa, the two pieces of glass are involuted;
5. heating to seal the area where the metal solder is distributed at the temperature of 180-350 ℃, wherein the heating mode can be infrared heating, induction heating, heat conduction heating, laser heating and the like, and can be local heating or integral heating;
6. cooling to obtain the tailless vacuum glass.
Example 2 in this example the outer edge of the sealing layer was spaced 5mm from the outer edge of the glass sheet.
Example 3 in this example the outer edge of the sealing layer was spaced 3mm from the outer edge of the glass sheet.
Example 4, the width of the sealing layer in this example was 15 mm.
Example 5, the width of the sealing layer in this example was 11 mm.
Example 6, the thickness of the slurry layer in this example was 50 μm.
Example 7 the thickness of the slurry layer in this example was 30 μm.
Example 8, the metal paste in this example includes 5 parts by mass of a glass phase, 15 parts by mass of an organic phase, and 80 parts by mass of a metal phase.
Example 9, the metal paste in this example includes 5 parts by mass of a glass phase, 20 parts by mass of an organic phase, and 75 parts by mass of a metal phase.
Example 10, the metal paste in this example includes 3 parts by mass of a glass phase, 15 parts by mass of an organic phase, and 82 parts by mass of a metal phase.
Example 11, the metal paste in this example includes 7 parts by mass of a glass phase, 15 parts by mass of an organic phase, and 78 parts by mass of a metal phase.
EXAMPLE 12 Bi is calculated as the mass fraction in the glass phase of this example2O3Content 60 parts, SiO2Content 20 parts, B2O3The content is 55 parts;
example 13 in this example Bi is present in the glass phase in parts by mass2O3Content 45 parts, SiO2Content 15 parts, B2O3The content is 35 parts, and the ZnO content is 8 parts;
comparative example 1, the metal paste included 5 parts by mass of a glass phase, 3 parts by mass of an organic phase, and 92 parts by mass of a metal phase.
Comparative example 2, the metal paste included 5 parts by mass of a glass phase, 30 parts by mass of an organic phase, and 65 parts by mass of a metal phase.
Comparative example 3, the metal paste included 1 part by mass of a glass phase, 15 parts by mass of an organic phase, and 84 parts by mass of a metal phase.
Comparative example 4, the metal paste included 9 parts by mass of a glass phase, 15 parts by mass of an organic phase, and 76 parts by mass of a metal phase.
Comparative example 5, the metal paste included 45 parts by mass of a glass phase, 15 parts by mass of an organic phase, and 40 parts by mass of a metal phase.
Comparative example 6, the metal paste included 35 parts by mass of a glass phase, 15 parts by mass of an organic phase, and 50 parts by mass of a metal phase.
Comparative example 7, the metal paste included 2 parts by mass of a glass phase, 3 parts by mass of an organic phase, and 95 parts by mass of a metal phase.
The experiments of the examples 1 and 8-11 and the comparative examples 1-7 are compared, the printing performance (viscosity), the adhesion and the welding performance of the metal paste are evaluated, and the evaluation method and the standard refer to the specification of the noble metal paste for the microelectronic technology GB/T17472-:
| numbering | Organic phase | Glass phase | Metallic phase | Printing performance | Adhesion force | Welding performance |
| Example 1 | 5 | 5 | 90 | Good wine | 14 | Good wine |
| Example 8 | 15 | 5 | 80 | Superior food | 16 | Youyou (an instant noodle) |
| Example 9 | 20 | 5 | 75 | Good wine | 17 | Superior food |
| Example 10 | 15 | 3 | 82 | Superior food | 10 | Superior food |
| Example 11 | 15 | 7 | 78 | Superior food | 17 | Good wine |
| Comparative example 1 | 3 | 5 | 92 | Difference (D) | - | - |
| Comparative example 2 | 30 | 5 | 65 | Difference (D) | - | - |
| Comparative example 3 | 15 | 1 | 84 | Superior food | 5 | - |
| Comparative example 4 | 15 | 9 | 76 | Superior food | 17 | Difference (D) |
| Comparative example 5 | 15 | 45 | 40 | Superior food | 9 | Difference (D) |
| Comparative example 6 | 15 | 35 | 50 | Superior food | 7 | Difference (D) |
| Comparative example 7 | 3 | 2 | 95 | Difference (D) | - | - |
In the table, "-" indicates that the previous test result does not reach the standard, and the measurement is not carried out in the subsequent test.
As can be seen from the above table, when the metal paste proportioning range value provided by the invention is used for processing, the printing performance of the metal paste is better than that of the metal paste, the adhesion is excellent, the welding performance is better, and one or more of the metal pastes beyond the proportioning range provided by the invention are not up to the standard in three aspects, so that the production requirement of the tailless vacuum glass cannot be met, the stable and reliable sealing of the vacuum cavity after the sealing of the tailless vacuum glass sheet cannot be ensured, and the risk of air leakage of the sealing layer exists.
Example 14, as shown in figure 1: this example provides a tailless vacuum glass produced by the process of example 1, comprising two rectangular glass sheets 1, preferably one of the glass sheets is regular glass and the other glass sheet is LOW-E glass, wherein both glass sheets 1 are non-porous monolithic glass. A sealing layer 2 is arranged between the two glass plates 1, the sealing layer 2 encloses a vacuum cavity, and a disk-shaped solid getter 3 is embedded on the surface of common glass serving as the inner wall of the vacuum cavity. The distance between the outer edge of the sealing layer 2 and the outer edge of the glass plate 1 is 1mm, and the width of the sealing layer 2 is 6 mm. The sealing layer 2 comprises a paste layer coated on the glass plate 1 and a solder layer located between the two paste layers, the paste layers having a thickness of 10 μm.
The invention adopts the method of plating the metalized layer on the surface of the glass to realize the connection of the glass and the metal, and the adopted metal slurry can effectively connect two glass plates to form a vacuum cavity and has stable and reliable sealing to the vacuum cavity. The process is suitable for producing the vacuum glass without the air exhaust port, and compared with the vacuum glass with the air exhaust port, the process has the advantages that no drilling is performed, the risk of crushing is reduced, and the process is safer; the process of sealing off the pumping hole is omitted, the risk of microcrack air leakage is avoided, and the vacuum service life is longer. Compared with the existing preparation process, the two-stage vacuum cavity treatment mode is adopted, and plasma is used for cleaning and degassing in the front-stage vacuum cavity to remove impurities such as oil stains on the surface of glass and adsorbed multilayer gas molecules. And the glass sheets are laminated in a vacuum process cavity with high vacuum degree, and the whole glass surface is exposed in the high vacuum environment, so that residual gas on the surface is easier to desorb. Compared with the prior art, the sheet combining device has the advantages that degassing is performed in the atmosphere through the uneven gaps of the welding materials, and degassing efficiency is greatly improved.
The foregoing is merely an example of the present invention and common general knowledge in the art of specific structures and/or features of the invention has not been set forth herein in any way. It should be noted that, for those skilled in the art, without departing from the structure of the present invention, several changes and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (6)
1. A preparation method of tailless vacuum glass is characterized in that: the method comprises the following steps:
A. metallization treatment, namely coating metal slurry on the to-be-sealed areas of the upper glass and the lower glass and sintering, wherein the sintering temperature is 450-800 ℃, and the metal slurry comprises 3-7 parts by mass of a glass phase, 5-20 parts by mass of an organic phase and 50-90 parts by mass of a metal phase;
B. laying a support on one glass sheet, and laying metal solder on the region to be sealed;
C. two pieces of glass are sent into a two-stage vacuum cavity, after vacuumizing, plasma bombardment treatment is carried out on the upper surface of the lower glass and the lower surface of the upper glass, the treatment is completed in a front-stage vacuum cavity of the two-stage vacuum cavity, the vacuum degree of the front-stage vacuum cavity is 0.1-100 Pa, the glass plate is heated while the plasma bombardment treatment is carried out, and the heating temperature is 150-;
D. is finished in a vacuum process cavity of a two-stage vacuum cavity, and the vacuum degree of the vacuum process cavity is 10-2-10-5Pa, closing the two pieces of glass after vacuumizing;
E. heating and sealing the area where the metal solder is distributed at the heating temperature of 180-350 ℃;
F. cooling to obtain the tailless vacuum glass.
2. The method for preparing tailless vacuum glass according to claim 1, wherein the method comprises the following steps: and in the step A, the distance between the outer edge of the metal paste and the edge of the glass is 1-5 mm.
3. The method for preparing tailless vacuum glass according to claim 1, wherein the method comprises the following steps: and in the step A, the coating width of the metal slurry is 6-15 mm.
4. The method for preparing tailless vacuum glass according to claim 1, wherein the method comprises the following steps: the coating thickness of the metal slurry in the step A is 10-50 μm.
5. The method for preparing tailless vacuum glass according to claim 1, wherein the method comprises the following steps: the metal solder in the step B is strip-shaped or wire-shaped tin or tin-based alloy.
6. The method for preparing tailless vacuum glass according to claim 1, wherein the method comprises the following steps: and in the step B, the height of the metal solder is 1-2mm higher than that of the support.
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