CN109369036A - Vacuum glass and preparation method thereof and vacuum glass production line - Google Patents
Vacuum glass and preparation method thereof and vacuum glass production line Download PDFInfo
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- CN109369036A CN109369036A CN201811384238.3A CN201811384238A CN109369036A CN 109369036 A CN109369036 A CN 109369036A CN 201811384238 A CN201811384238 A CN 201811384238A CN 109369036 A CN109369036 A CN 109369036A
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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
-
- 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/06—Surface treatment of glass, not in the form of fibres or filaments, by coating with metals
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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
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/25—Metals
- C03C2217/263—Metals other than noble metals, Cu or Hg
-
- 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
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/25—Metals
- C03C2217/27—Mixtures of metals, alloys
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Joining Of Glass To Other Materials (AREA)
Abstract
The invention discloses a kind of vacuum glass and preparation method thereof and vacuum glass production lines, the preparation method of the vacuum glass includes: after being vacuum-evacuated the first glass after cleaning, tin material is plated in the surrounding of the first glass again, forms the first tin layers connecting with the first glass air-tightness；It after the second glass after cleaning is vacuum-evacuated, then in the surrounding of the second glass plates tin material, forms the second tin layers connecting with the second glass air-tightness；First glass and the second glass are superimposed with each other and is placed on vacuum drying oven and vacuumizes, and pass through the first tin layers of vacuum stove heating and the second tin layers, so that the first tin layers and the second tin layers melt to form one, and first vacuum cavity for forming sealing between glass and the second glass, wherein, when first glass and the second glass are superimposed with each other, the first tin layers and the second tin layers are bonded to each other.This method simple process, strong operability, the vacuum glass produced have preferable compression strength and properties of product.
Description
Technical field
The present invention relates to glass arts, in particular to a kind of vacuum glass and preparation method thereof and vacuum glass
Production line.
Background technique
Vacuum glass can effectively completely cut off heat transmission with the characteristic of its vacuum, therefore have optimal insulation
Performance is the development trend of building energy conservation, reduces building energy consumption for China, realizes that low carbon development is significant.
The technology of existing vacuum glass mainly uses frit to carry out sealing-in, then carries out vacuumizing sealing-in and exhaust, such as specially
Benefit CN103588386 causes sealing temperature higher, will affect tempered glass in sealing-in since the fusing point of glass powder is high
Intensity.
Therefore, the low-temperature sealing of vacuum glass is development trend, and patent CN105541132 elaborates a kind of vacuum glass
Manufacture prepares metalization layer on glass first, then carries out tempering processing to glass, then will be metallized with brazing metal
Glass sealing get up, sealing-in process is complicated, higher cost, and secondly its vacuum evacuation and sealing-in are all complete in a vacuum chamber
At increasing the difficulty of realization.
Summary of the invention
The purpose of the present invention includes providing a kind of vacuum glass and preparation method thereof and vacuum glass production line, both can be with
Reduce sealing temperature, the intensity with preferable tempered glass, and it is innovative will vacuum evacuation link to be placed on glass tin plating
Before sealing-in, not only clean glass surface can be provided for glass is tin plating by being vacuum-evacuated, but also glass surface can be reduced
Adsorbed gas meets service life requirement, breaches vacuum glass without this difficult point of aspirating hole, to simplify production
Technique improves production efficiency.
The present invention solves its technical problem and adopts the following technical solutions to realize.
The present invention provides a kind of preparation methods of vacuum glass comprising: the first glass after cleaning is subjected to vacuum
It after exhaust, then in the surrounding of the first glass plates tin material, forms the first tin layers connecting with the first glass air-tightness；It will cleaning
It after the second glass afterwards is vacuum-evacuated, then in the surrounding of the second glass plates tin material, is formed and the second glass air-tightness
Second tin layers of connection；
First glass and the second glass are superimposed with each other and is placed on vacuum drying oven and vacuumizes, and passes through the vacuum stove heating
First tin layers and the second tin layers so that the first tin layers and the second tin layers melt to form one, and the first glass and the second glass it
Between form the vacuum cavity of sealing, wherein when the first glass and the second glass are superimposed with each other, the first tin layers and the second tin layers are mutual
Fitting.
The present invention also provides a kind of vacuum glass prepared by the preparation method comprising the first glass and
The surrounding of the sealing surface of two glass, the sealing surface of the first glass and the second glass melts consolidation by the first tin layers and the second tin layers
Integrated tin layers vacuum tight connection is formed afterwards.
The present invention also provides a kind of vacuum glass production lines comprising:
Cleaning equipment, for being cleaned to the first glass and the second glass；
First vacuum drying oven, for after cleaning the first glass and the second glass be vacuum-evacuated；
Tin equipment, for plating the first tin layers and the second tin respectively in the sealing surface surrounding of the first glass and the second glass
Layer；
Second vacuum drying oven for vacuumizing tin plating rear and the first glass being bonded to each other and the second glass, and adds
Heat makes the first tin layers and the second tin layers melt to form one, and the vacuum chamber of sealing is formed between the first glass and the second glass
Body.
By being first vacuum-evacuated to the first glass and the second glass, then respectively in the envelope of the first glass and the second glass
Junction surrounding the first tin layers of tin plating formation and the second tin layers, then first vacuumized and the first tin layers of heating and melting and the second tin layers
The operation being attached, to reach lower in sealing temperature, the first glass and the second glass can be bound to each other to form vacuum glass
Glass, and the intensity of tempered glass will not be had an impact, in the preparation process, carry out carrying out vacuum evacuation processing to glass,
It is different first to be consolidated with existing, the rear method that vacuumizing is carried out by aspirating hole, so that obtained vacuum glass is without pumping
Hole.In addition, as the tin layers of the first glass of connection and the second glass its due to the flexibility of metal, when cold and hot contraction, which can absorb, answers
Power, so that vacuum glass has preferable compression strength and excellent properties of product.
Detailed description of the invention
It, below will be to use required in embodiment in order to illustrate more clearly of the technical solution of embodiment of the present invention
Attached drawing be briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not to be seen as
It is the restriction to range, it for those of ordinary skill in the art, without creative efforts, can be with root
Other relevant attached drawings are obtained according to these attached drawings.
Fig. 1 is the schematic diagram of the preparation method of the vacuum glass of one embodiment of the present invention；
Fig. 2 is the structural schematic diagram of the vacuum glass of one embodiment of the present invention；
Fig. 3 is the structural schematic diagram of the vacuum glass of one embodiment of the present invention；
Fig. 4 is the structural schematic diagram of the vacuum glass production line of one embodiment of the present invention.
Icon: 100- vacuum glass；The first glass of 110-；The second glass of 120-；130- tin layers；140- support column；200-
Vacuum glass production line；210- cleaning equipment；The first vacuum drying oven of 220-；230- tin equipment；The second vacuum drying oven of 240-；250- is clean
Clean room；The first delivery track of 261-；The second delivery track of 262-.
Specific embodiment
It, below will be to embodiment party of the present invention to keep the purposes, technical schemes and advantages of embodiment of the present invention clearer
Technical solution in formula is clearly and completely described.The person that is not specified actual conditions in embodiment or embodiment, according to routine
The condition that condition or manufacturer suggest carries out.Reagents or instruments used without specified manufacturer, being can be by commercially available purchase
Buy the conventional products of acquisition.
A kind of vacuum glass of embodiment of the present invention being related to and preparation method thereof and vacuum glass are produced below
Line is specifically described.
Some embodiments of the present invention provide a kind of preparation method of vacuum glass comprising:
After the first glass after cleaning is vacuum-evacuated, then in the surrounding of the first glass plate tin material, formed with
First tin layers of the first glass air-tightness connection；After the second glass after cleaning is vacuum-evacuated, then in the second glass
Surrounding plates tin material, forms the second tin layers connecting with the second glass air-tightness；
First glass and the second glass are superimposed with each other and is placed on vacuum drying oven and vacuumizes, and passes through institute's vacuum stove heating
First tin layers and the second tin layers so that the first tin layers and the second tin layers melt to form one, and the first glass and the second glass it
Between form the vacuum cavity of sealing, wherein when the first glass and the second glass are superimposed with each other, the first tin layers and the second tin layers are mutual
Fitting.
In embodiments of the present invention, the first glass and sealing-in that sealing surface surrounding is coated with the first tin layers are used first
Face surrounding is coated with the second glass with matched second tin layers of the first tin layers, is distinguished on the first glass and the second glass by elder generation
Plate the first tin layers and the second tin layers, can be realized the first tin layers and the second tin layers respectively with the first glass and the second glass
Good air-tightness connection.Then after being again bonded to each other the first glass and the second glass, so that the first tin layers and second
Tin layers can occur to melt the sealing-in for being formed and integrally realizing the first glass and the second glass at a lower temperature, thus the first tin
Layer can also be closely joined together with the second tin layers and realize that airtight sealing connects.Therefore, pass through the first tin layers and the second tin
Air-tightness between layer and glass connects, along with the air-tightness between the first tin layers and the second tin layers connects, to reach first
Firm be tightly connected is formed between glass and the second glass.
Meanwhile embodiment of the present invention changes the mode of operation vacuumized after existing first sealing-in, does not have to reserved pumping
Hole is first vacuum-evacuated the first glass and the second glass, and the first glass and are removed by way of vacuumizing and heating
The gas of two glass surfaces, then vacuumized and heated in a vacuum furnace, so that the first glass and the second glass are before sealing-in
Therebetween it is just first in vacuum state, then the first tin layers and the second tin layers are melted at a certain temperature, so that the two connects
Solidification, so that self-assembling formation vacuum cavity between the first glass and the second glass.Since the first tin layers and the second tin layers all belong to
In low-temperature metal solder, therefore, during above-mentioned sealing-in, since temperature is lower, glass is carried out so as to avoid high temperature
Thermal shock, to reduce the loss of strength of glass.Meanwhile first is connected using metal material between glass and the second glass
It connects, the flexibility of metal material enables glass to absorb stress when receiving and expanding with heat and contract with cold, so that it has more preferably
Service performance.
According to some embodiments, it is coated with the first glass of the first tin layers and second glass for being coated with the second tin layers is logical
It crosses following steps to be prepared: after the first glass after cleaning is vacuum-evacuated, then in the surrounding of the first glass plating tin
Material forms the first tin layers connecting with the first glass air-tightness；After the second glass after cleaning is vacuum-evacuated, then
The surrounding of second glass plates tin material, forms the second tin layers connecting with the second glass air-tightness.
The surface of glass is easy containing some spots and dust etc., can the transparency to glass itself and tin material with
The binding ability on its surface impacts, and therefore, needs first to clean glass before progress is tin plating.Of the invention is some
In embodiment, the cleaning of glass includes but is not limited to be rinsed and dried with deionized water again after being cleaned with cleaning solution or vacuum
Plasma cleaning or ultraviolet rays cleaning.
Further, a large amount of steam and organic matter are generally adsorbed in the surface of glass, these steam and organic matter will lead to
Energy-saving effect is lost because of the rising of vacuum degree in its service life, how to remove low temperature sealing glass table well
The steam and organic matter in face become a problem.In some embodiments of the present invention, also needed after being cleaned to glass
First glass and the second glass are vacuum-evacuated.Above-mentioned vacuum evacuation mode can remove glass surface to a certain extent
Steam and organic matter, advantageously ensure that the energy-saving effect of vacuum glass.
However, the present inventor it has been investigated that, in sealing-in vacuum glass, due to using low melting point tin solder,
Fusing point is lower, therefore sealing temperature cannot be too high, leads to not more fully remove above-mentioned steam and organic matter, easily certain
The energy-saving effect of vacuum glass is reduced in degree.The present inventor it has been investigated that, the vacuum evacuation of high temperature is first carried out before sealing-in
Operation removes steam and organic matter, more can fully remove the steam and organic matter of glass surface, and this method is not only key
It closes and provides clean surface, also achieve thorough exhaust, specifically, in some embodiments of the present invention, vacuum evacuation is
Temperature in vacuum drying oven is warming up to 200~400 DEG C, keeps the temperature 25~60min, while vacuum degree being kept to be less than 10Pa.Study table
Bright, above-mentioned condition is conducive to completely remove the steam and organic matter of glass surface；If heating temperature is too low, then can not effectively remove
These steam and organic matter；And heating temperature is excessively high to adversely affect to the intensity of glass.
It should be noted that during aforesaid operations, cleaning process can be by the first glass and the second glass into
It goes while cleaning, then be vacuum-evacuated simultaneously；It is also possible to that the first glass and the second glass are carried out individually cleaning, true respectively
Idle discharge gas.
In addition, the present inventor it has been investigated that, although sealing temperature can reduce using low-temperature metal solder, but deposit
It is difficult to soak glass to be difficult to form the problems such as air-tightness is connect with glass in brazing metal；The present inventor it has been investigated that,
It can reinforce the wetting of brazing metal and glass by applying ultrasonic wave, to overcome the above problem well.Therefore, in this hair
In bright some embodiments, plated on the sealing surface of the first glass and the second glass tin material be respectively formed the first tin layers and
Second tin layers are carried out by way of applying ultrasonic wave.The equipment used sets for supersonic bonding equipment, supersonic bonding
It is standby have the characteristics that quickly, energy conservation, fuse intensity height, be good conductivity, no-spark, excellent close to cool grinding, enable to tin material
Material can be bonded together with the surface of glass well, to reach good air-tightness connection effect.Further,
In some embodiments, the frequency of ultrasonic wave used can be 20~80kHz, and power can be 5~60w.In said frequencies and
Under the action of power, tin material uniformly and stably can form tin layers in glass surface, and be bonded well, and adhesion effect is excellent.
It should be noted that tin equipment is also possible to thermal spraying apparatus, such as supersonic flame spraying, plasma spraying.
Further, in order to increase wetting and bond strength of the tin layers to glass, in the first He by way of thermal spraying
The surface of second glass surrounding is pre-formed copper or copper alloy layer, then plates tin material, shape in copper or copper alloy layer surface again
At the first and second tin layers.
Further, during tin plating in order to avoid the oxidation of tin material, it is therefore preferable that the first tin layers of tin plating is formationed with
Second tin layers carry out under an inert atmosphere.Inert atmosphere can be the atmosphere of the rare gas such as nitrogen or argon gas.
The tin material of the first tin layers of formation, the second tin layers described here is the well known solder containing tin, such as pure
At least one of tin, tin bismuth, tin indium, tin zinc, tin-lead, tin silver.In some embodiments, the tin of the first tin layers and the second tin layers
Material may be the same or different, and preferably the first tin layers are identical with the material of the second tin layers.In some embodiments, in order to
The thickness of the performance requirement of guarantee vacuum glass, the first tin layers and the second tin layers is 1mm hereinafter, for example can be about
0.8mm, 0.7mm, 0.6mm, 0.5mm or 0.4mm.
Further, it is specifically included by the first tin layers of vacuum stove heating and the second tin layers: by the temperature liter in vacuum drying oven
Temperature is to 232~350 DEG C, and preferably 240~300 DEG C, more preferable 245~255 DEG C, such as 250 DEG C.And 4 are kept the temperature at the temperature disclosed above
~7min, such as 4min, 5min, 6min or 7min.Further, the first tin layers and the second tin are heated under the conditions of above-mentioned temperature
When layer, the vacuum degree in vacuum drying oven is less than or equal to 0.1Pa, that is, vacuum drying oven is evacuated to vacuum degree when vacuumizing and is less than or waits
In 0.1Pa.
In certain embodiments of the present invention, also there is air-breathing between the first glass and the second glass being bonded to each other
Agent and support column.It is added and inhales between the first glass and the second glass i.e. between being bonded the first glass and the second glass
Gas agent and support column, wherein support column can be multiple, be uniformly distributed, which can be metal support column,
When the first glass and the second glass are bonded to each other, the both ends of support column are abutted with the first glass and the second glass respectively.In addition
In some embodiments, support column may be the glass support being sintered to fix on the sealing surface of the first glass or the second glass
Column, material are glass glaze, are to be sintered together in glass manufacture with glass.
In some embodiments, getter can be evaporable, be also possible to non-evaporable, be also possible to compound.It inhales
Gas agent include but is not limited to containing Zr element, containing Ti element, contain one of transition metal element or a variety of or containing dilute
One of earth metal element is a variety of.In some embodiments, getter can be Zr system getter, such as Zr-Al type,
Zr-Ni type, Zr-C type, Zr-Co-RE type (RE is rare earth element) or Zr-V-Fe type.In some embodiments, getter Ti
It is getter, such as Ti-Mo type or Ti-Zr-V type getter.It can be placed according to the size of vacuum glass cavity the desired amount of
Getter, such as place 1g/cm3Above getter.It is preferred that getter is nonevaporable getter without steaming through high-frequency heating
It is used after hair, does not form metal film in vitreous surface, the transparency of vacuum glass influenced small.
In some embodiments of the present invention, above-mentioned first glass and the second glass can be ordinary glass, can also
Think the tempered glass for being coated with low-E film.
The preparation method for the vacuum glass that some embodiments of the present invention provide, integrated operation process such as 1 institute of attached drawing
Show, specifically include:
A. the first glass and the second glass are cleaned；
B. by the first glass and the second glass 200-400 DEG C at a temperature of be vacuum-evacuated；
C. the first tin plating, formation is connect with the first glass air-tightness tin layers are carried out in the sealing surface surrounding of the first glass；
The second tin plating, formation is connect with the second glass air-tightness tin layers are carried out in the sealing surface surrounding of the second glass；
D. first piece is superimposed together with the second sheet glass, and places getter between, so that the first tin
Layer is bonded to each other with the second tin layers；
F. the glass of overlapping is moved into vacuum drying oven, vacuumized, and the first tin layers and the second tin layers are heated, after being allowed to thawing
One is formed, first piece is connect with the second sheet glass air-tightness.
Some embodiments of the present invention additionally provide a kind of vacuum glass prepared by the preparation method 100,
The vacuum glass is without aspirating hole, and referring to attached drawing 2, which includes the first glass 110 and the second glass 120, the first glass
The surrounding of the sealing surface of the sealing surface of glass 110 and the second glass 120 is formed after melting consolidation by the first tin layers and the second tin layers
130 vacuum tight of the tin layers connection of one.Wherein, due to the sealed connection of tin layers 130 in the first glass 110 and the second glass
It is formed between 120 in closed vacuum cavity and is additionally provided with support column 140.Further, referring to attached drawing 3, in order to increase tin layers
Wetting and bond strength to glass, it is pre- on the surface of 120 surrounding of the first glass 110 and the second glass by way of thermal spraying
It is initially formed copper or copper alloy layer, then tin material is plated in copper or copper alloy layer surface again, forms the first tin layers and the second tin layers,
First tin layers and the second tin layers form tin layers 130 after melting.
Some embodiments of the present invention additionally provide a kind of vacuum glass production line 200, referring to attached drawing 4 comprising:
Cleaning equipment 210, for being cleaned to the first glass 110 and the second glass 120；
First vacuum drying oven 220, for after cleaning the first glass 110 and the second glass 120 be vacuum-evacuated；
Tin equipment 230, for plating the first tin respectively in the sealing surface surrounding of the first glass 110 and the second glass 120
Layer and the second tin layers；
Second vacuum drying oven 240, for taking out tin plating rear and the first glass 110 being bonded to each other and the second glass 120
Vacuum, and heating makes the first tin layers and the second tin layers melt to form one, and shape between the first glass 110 and the second glass 120
At the vacuum cavity of sealing.
Further, it is connected between cleaning equipment 210 and the first vacuum drying oven 220 by the first delivery track 261, the first glass
Glass 110 and the second glass 120 are delivered to by delivery track cleaned in cleaning equipment 210 after, then pass through the first conveyor track
Road is delivered in the first vacuum drying oven 220 and is vacuum-evacuated.First vacuum drying oven 220 and the second vacuum drying oven 240 pass through the second conveying
Track 262 connects, and the second delivery track 262 is set in toilet 250, and tin plating operation is operated in toilet 250.
Tin equipment 230 is set in toilet 250, the first glass 110 and the second glass that can be transmitted to the second delivery track 262
Glass 120 carries out tin plating operation.It is exported again through delivery track by the vacuum glass that 240 vacuum seal of the second vacuum drying oven has been formed.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
The preparation method of vacuum glass provided in this embodiment comprising:
Firstly, by cleaning solution to being rinsed and dried with deionized water again after the first glass and the second glass cleaning；Again will
First glass and the second glass are placed in the first vacuum drying oven, and it is 6Pa that vacuum drying oven, which is evacuated to vacuum degree, then temperature is heated up
To at 200 DEG C, 35min is kept the temperature.
Secondly, first glass and the second glass are removed the first vacuum drying oven after cooling, respectively in the first glass and the second glass
The sealing surface surrounding progress of glass is tin plating, forms the first tin layers and the second tin layers on the first glass and the second glass respectively.It is tin plating
Mode is tin plating to be carried out by supersonic bonding equipment, and the frequency of ultrasonic wave used is 20kHz, power 10w.Wherein, first
Tin layers and the second tin thickness are 0.5mm；First glass and the second glass are ordinary glass；Carry out tin plating tin material
Material is pure tin.
Then, first piece and the second sheet glass are superimposed together, and place Zr-Ni type air-breathing between
Agent, so that the first tin layers are bonded to each other with the second tin layers.The glass of overlapping is moved into the second vacuum drying oven again, is evacuated to vacuum degree
For 0.05Pa, and being heated to temperature to the first tin layers and the second tin layers is 232 DEG C, keeps the temperature 7min, both makes shape after melting
Integrally, first piece is connect with the second sheet glass air-tightness, is removed after cooling, obtains vacuum glass.
Embodiment 2
The preparation method of vacuum glass provided in this embodiment comprising:
Firstly, after being dried by vacuum plasma cleaning equipment to the first glass and the second glass cleaning；Again by the first glass
Glass and the second glass are placed in the first vacuum drying oven, and it is 8Pa that vacuum drying oven, which is evacuated to vacuum degree, then temperature is warming up to
400 DEG C, keep the temperature 25min.
Secondly, first glass and the second glass are removed the first vacuum drying oven after cooling, respectively in the first glass and the second glass
The sealing surface surrounding progress of glass is tin plating, forms the first tin layers and the second tin layers on the first glass and the second glass respectively.It is tin plating
Mode is tin plating to be carried out by supersonic bonding equipment, and the frequency of ultrasonic wave used is 80kHz, power 60w.Wherein, first
Tin layers and the second tin thickness are 0.6mm；First glass and the second glass are ordinary glass；Carry out tin plating tin material
Material is the Sn-Zn solder that Zn mass content is 4%.
Then, first piece and the second sheet glass are superimposed together, and place Zr-Ni type air-breathing between
Agent, so that the first tin layers are bonded to each other with the second tin layers.The glass of overlapping is moved into the second vacuum drying oven again, is evacuated to vacuum degree
For 0.06Pa, and being heated to temperature to the first tin layers and the second tin layers is 350 DEG C, keeps the temperature 4min, both makes shape after melting
Integrally, first piece is connect with the second sheet glass air-tightness, is removed after cooling, obtains vacuum glass.
Embodiment 3
The preparation method of vacuum glass provided in this embodiment comprising:
Firstly, by cleaning solution to being rinsed and dried with deionized water again after the first glass and the second glass cleaning；Again will
First glass and the second glass are placed in the first vacuum drying oven, and it is 2Pa that vacuum drying oven, which is evacuated to vacuum degree, then temperature is heated up
To at 300 DEG C, 30min is kept the temperature.
Secondly, first glass and the second glass are removed the first vacuum drying oven after cooling, respectively in the first glass and the second glass
The sealing surface surrounding thermal spraying copper alloy layer of glass, then copper alloy surface progress is tin plating again, thus in the first glass and the second glass
The first tin layers and the second tin layers are formed on glass.Tin plating mode is tin plating to be carried out by supersonic bonding equipment, ultrasonic wave used
Frequency is 50kHz, power 35w.Wherein, the first tin layers and the second tin thickness are 0.6mm；First glass and the second glass
It is ordinary glass；Carrying out tin plating tin material is the Sn-Cu solder that Cu mass content is 0.7%.
Then, first piece and the second sheet glass are superimposed together, and place Zr-Ni type air-breathing between
Agent, so that the first tin layers are bonded to each other with the second tin layers.The glass of overlapping is moved into the second vacuum drying oven again, is evacuated to vacuum degree
For 0.03Pa, and being heated to temperature to the first tin layers and the second tin layers is 250 DEG C, keeps the temperature 5min, both makes shape after melting
Integrally, first piece is connect with the second sheet glass air-tightness, is removed after cooling, obtains vacuum glass.
Comparative example 1
Firstly, by cleaning solution to being rinsed and dried with deionized water again after the first glass and the second glass cleaning；Again will
First glass and the second glass are placed in the first vacuum drying oven, and it is 2Pa that vacuum drying oven, which is evacuated to vacuum degree, then temperature is heated up
To at 300 DEG C, 30min is kept the temperature.
Then, first piece and the second sheet glass are superimposed together, and the first glass and the second glass sealing face four
Week places the lead-free glass powder with low melting point after 1.2mm, and places Zr-Ni type getter between.Again by the glass of overlapping
The second vacuum drying oven is moved into, being evacuated to vacuum degree is 0.03Pa, and being heated to temperature is 500 DEG C, 5min is kept the temperature, after cooling
It removes, obtains vacuum glass.
By Examples 1 to 3 and the resulting vacuum glass of comparative example 1 according to the test of glass strain in GB/T18144-2008
Method carries out stress test, and the results are shown in Table 1.
| Group | Average edge stress (MPa) |
| Embodiment 1 | 95.3 |
| Embodiment 2 | 98.4 |
| Embodiment 3 | 105.6 |
| Comparative example 1 | 61.5 |
In conclusion the preparation method of the vacuum glass of embodiment of the present invention, product structure is simple, production efficiency
Height, production line can also be assembled by existing traditional equipment, value with higher.And preparation process difference expects pumping
Hole, the vacuum glass produced intensity with higher and excellent properties of product.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of vacuum glass, characterized in that it comprises:
After the first glass after cleaning is vacuum-evacuated, then in the surrounding of first glass plate tin material, formed with
First tin layers of the first glass air-tightness connection；After the second glass after cleaning is vacuum-evacuated, then described
The surrounding of two glass plates tin material, forms the second tin layers connecting with the second glass air-tightness；
First glass and second glass are superimposed with each other and is placed on vacuum drying oven and vacuumizes, and passes through the vacuum
First tin layers described in stove heating and second tin layers, so that first tin layers and second tin layers melt to form one,
And the vacuum cavity of sealing is formed between first glass and second glass, wherein first glass and described
When two glass are superimposed with each other, first tin layers and second tin layers are bonded to each other.
2. the preparation method of vacuum glass according to claim 1, which is characterized in that it is tin plating formed first tin layers and
Second tin layers carry out under an inert atmosphere.
3. the preparation method of vacuum glass according to claim 1, which is characterized in that first glass and described
It is to heat first glass and/or second glass under vacuum conditions that two glass, which carry out vacuum evacuation,；It is preferred that
Ground, heating temperature are 200~400 DEG C, and heating time is 25~60min；Preferably, vacuum degree is less than 10Pa.
4. the preparation method of vacuum glass according to claim 1, which is characterized in that in first glass and described
It is plated on the sealing surface of two glass when tin material is respectively formed first tin layers and second tin layers and is applied with ultrasonic wave；It is excellent
Selection of land, the frequency of ultrasonic wave used are 20~80kHz.
5. the preparation method of vacuum glass according to claim 1, which is characterized in that in first glass and described
Before plating tin material on the sealing surface of two glass, first glass and second glass first pass through heat in tin plating position in advance
Spraying method forms copper or copper alloy layer, then plates tin material in copper or copper alloy layer surface.
6. the preparation method of vacuum glass according to claim 1, which is characterized in that by described in the vacuum stove heating
First tin layers and second tin layers specifically include: the temperature in the vacuum drying oven being warming up to 180~350 DEG C, tin layers is allowed to melt
Change；Preferably, when heating first tin layers and second tin layers, the vacuum degree in the vacuum drying oven is less than or equal to
0.1Pa。
7. the preparation method of vacuum glass according to claim 1, which is characterized in that first glass being superimposed with each other
Also there is getter and support column between second glass, the support column is to be set to first glass and the second glass
Metal support column or the support column between glass are the sealing surface being sintered to fix in first glass or second glass
On glass support column.
8. the preparation method of vacuum glass according to claim 1, which is characterized in that first glass and described
The cleaning of two glass includes washing and/or plasma cleaning and/or ultraviolet rays cleaning.
9. a kind of vacuum glass being prepared by preparation method according to any one of claims 1 to 8, which is characterized in that institute
Vacuum glass is stated without aspirating hole comprising first glass and second glass, the sealing surface of first glass and institute
The surrounding of the sealing surface of the second glass is stated by forming integrated tin after first tin layers and second tin layers thawing consolidation
Layer vacuum tight connection.
10. a kind of vacuum glass production line, characterized in that it comprises:
Cleaning equipment, for being cleaned to the first glass and the second glass；
First vacuum drying oven, for after cleaning the first glass and the second glass be vacuum-evacuated；
Tin equipment, for plating the first tin layers and respectively in the sealing surface surrounding of first glass and second glass
Two tin layers；
Second vacuum drying oven, for tin plating rear and first glass being bonded to each other and second glass to be vacuumized,
And heating makes first tin layers and second tin layers melt to form one, and first glass and second glass it
Between form the vacuum cavity of sealing.
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| CN201811384238.3A CN109369036A (en) | 2018-11-20 | 2018-11-20 | Vacuum glass and preparation method thereof and vacuum glass production line |
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| CN201811384238.3A CN109369036A (en) | 2018-11-20 | 2018-11-20 | Vacuum glass and preparation method thereof and vacuum glass production line |
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| CN111499223A (en) * | 2020-04-24 | 2020-08-07 | 李长征 | Tempered vacuum glass and manufacturing method thereof |
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