CN106986551A - A kind of preparation method of vacuum glass metal sealing metal layer - Google Patents
A kind of preparation method of vacuum glass metal sealing metal layer Download PDFInfo
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- CN106986551A CN106986551A CN201710280885.9A CN201710280885A CN106986551A CN 106986551 A CN106986551 A CN 106986551A CN 201710280885 A CN201710280885 A CN 201710280885A CN 106986551 A CN106986551 A CN 106986551A
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- metal
- glass
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- metal paste
- sealing
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Classifications
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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
- 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
-
- 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
Abstract
The invention discloses a kind of preparation method of vacuum glass metal sealing metal layer：Step 1, treat that the surface of sealing region prepares metal paste coating in glass sheet perimeter；Step 2, drying and processing is carried out to metal paste coating；Step 3, pre-add hot glass sheet keeps the temperature to 200 DEG C to 350 DEG C within the period of setting；Step 4, metal paste coating is heated using sintering process, it is consolidated with glass plate, form metal layer；Step 5, repeat step 1 to step 4 at least one times, complete vacuum glass sealing-in metal layer preparation.When solving vacuum glass using metal brazing process sealing-in, sealing-in side low intensity, the problem of air-tightness is bad can significantly improve the intensity and air-tightness on vacuum glass sealing-in side, and then improve the yield rate and service life of vacuum glass production.
Description
Technical field
The present invention relates to vacuum glass technical field, in especially a kind of vacuum glass metal sealing process, in glass base
The method that metal layer is prepared on plate.
Background technology
The vacuum glass of glass powder with low melting point edge sealing, the temperature needed for being melted because of low glass powder is used between 380 DEG C -450 DEG C
When safety glass makees substrate, lasting high temperature makes glass move back tempering during edge sealing, and this vacuum glass is not belonging to safe glass
Glass, using severely limited.The vacuum glass being combined with safety glass, because manufacturing cost is high, only on some top-grade buildings
Use.In order to reduce manufacturing cost, vacuum glass is made in the glass plate of Qingdao henry up to used tempering, using the glass of more low melting point
Powder, in relative lower temperature lower sealing edge；Beijing Xin Liji is used reaches lower edge sealing temperature than Qingdao henry, with reference to external pressure
Mode solves the problems, such as that toughened vacuum glass is made in low temperature edge sealing glass solder illiquidity.But, the glass dust of more low melting point
Mean that the ionic radius for constituting the material of this glass dust is bigger, its penetrating power is poor, and then sintering strength is low, air-tightness
Difference.Continuous high temperature during edge sealing, the tempering performance loss of substrate；The vacuum glass of completion represents the surface stress of tempering intensity
Only keep 75%.
The applicant proposes a kind of glass plate in the Chinese invention patent of Application No. 201010508421.7 and is combined
Method for sealing, the hermetic seal of vacuum glass is realized using low-melting-point metal, is concretely comprised the following steps：(1) in each glass to be composite
Predetermined sealing region surface on plate, prepares the metal layer being consolidated with glass plate body respectively；(2) metal pricker is used
Welding, will it is compound after the metal layer of mutually corresponding sealing region welds together on glass plate two-by-two, realize two glass
Plate is tightly connected sealing region.It is envelope that the metal layer being consolidated with glass plate body how is prepared in the above method
The key connect, be this in that patent, applicant also describes the detailed step for preparing metal layer.Later, with research, reality
That tests deepens continuously, applicants have discovered that：Solder etch transition zone occurs in the glass plate of metalized, brazing process
Phenomenon, directly translates into sealing-in side intensity decreases, solder is commonly called as silverskin and torn along silverskin transition zone cracking phenomena after edge sealing completion
Split, ultimately result in vacuum glass directly cracking or the chronic permeation of sealing-in completion, the final product quality and later stage of vacuum glass are made
Totally unfavorable influence is produced with the life-span.
The content of the invention
For problems of the prior art, it is an object of the invention to provide a kind of vacuum glass metal sealing metal
Change the preparation method of layer.
To achieve the above object, technical scheme is as follows：
A kind of preparation method of vacuum glass metal sealing metal layer, this method comprises the following steps：
Step 1, treat that the surface of sealing region prepares metal paste coating in glass sheet perimeter；
Step 2, drying and processing is carried out to metal paste coating；
Step 3, pre-add hot glass sheet keeps the temperature to 200 DEG C to 350 DEG C within the period of setting；
Step 4, metal paste coating is heated using sintering process, it is consolidated with glass plate, form metal layer；
Step 5, repeat step 1 to step 4 at least one times, complete vacuum glass sealing-in metal layer preparation.
Further, in the step 1, the metal paste coating is with dip-coating, spraying, silk-screen printing, manual application or machine
The mode of tool coating is prepared on the surface for treating sealing region in glass sheet perimeter.
Further, the metal paste coating uses silk screen plate to be prepared with silk-screen printing technique in glass pane surface, institute
The mesh number for stating silk screen plate is 180 mesh to 400 mesh.
Further, pre-add hot glass sheet, to 230 DEG C to 300 DEG C, and keeps the temperature 100 seconds to 120 in the step 3
Second.
Further, the sintering process of the step 4 is specially：The glass plate that preparation has metal paste coating is integrally heated
To sintering temperature, the tempering temperature that the sintering temperature is located at glass plate is interval interior.
Further, it is directly logical when described prepare has the glass plate of metal paste coating after the processing of multiple sintering process
Too fast quickly cooling but completes the tempering processing of glass plate.
Further, the sintering process of the step 4 is specially:The glass plate that preparation has metal paste coating is integrally heated
To 500 DEG C to 720 DEG C, and keep the temperature 90 seconds to 300 seconds.
Further, the sintering process of the step 4 is specially：Position where metal paste coating is heated, plus
Hot temperature is 500 DEG C to 720 DEG C, and keeps the temperature 90 seconds to 300 seconds.
Further, the metal paste is Ag metal pastes, Cu-Ag alloying metals slurry, Ni metal pastes, Ni-Ag conjunctions
Golden metal paste, Au metal pastes, Au alloying metals slurry, Zn metal pastes, Zn alloying metals slurry, Pd metal pastes or Pd
Alloying metal slurry.
Further, the metal paste is the Ag metal pastes that silver-colored weight content is 70% to 90%.
Further, the thickness of metal paste coating is 10 μm to 35 μm in the step 1.
Further, the thickness of the metal layer in the step 5 is 5 μm to 25 μm.
The preparation method of metal layer in the present invention, metal paste coating is in sintering process, surface of metal particles oxidation
Formation oxide-film, and the glass powder in metal paste, infiltrate surface of metal particles.Oxidized metal, which is partly dissolved, enters glass
Phase, glass is mutually penetrated into the pore of the metallized layer surface prepared for the first time, plugs solder into the logical of transition zone
Road.Metallic particles is grown up, rapider than surface to reduce, and glass more than needed enters under capillary pressure effect between metallic particles
Space, and enter together among space with coating metal particle, metallic particles is grown up rapidly in the horizontal direction, glass is mutually taken
In the pore for the metallized layer surface for entering first sintering formation with metallic particles, make metallic particles in first sintering shape
Into metal layer on continued growth, so as to be sintered together the metal layer for foring continuous sponge skeletal like.Make again
During standby metal layer, glass phase is further set to be sintered with substrate firm, integrated metal layer possesses good ductility, can
The thermal shock during Welding is resistant to, etch of the solder to transition zone has been blocked.Vacuum glass is solved using metal pricker
During Welding sealing-in, sealing-in side low intensity, the problem of air-tightness is bad, can significantly improve vacuum glass sealing-in side intensity and
Air-tightness, and then improve the yield rate and service life of vacuum glass production.
Brief description of the drawings
Fig. 1 is process chart of the invention.
Embodiment
Technical scheme is described in detail with combining embodiment below.The present invention can be presented as
A variety of multi-forms, are not construed as the exemplary embodiment for being confined to describe here.
Embodiment 1
As shown in figure 1, the preparation method of the vacuum glass metal sealing metal layer of the present embodiment comprises the following steps：
Step 1, treat that the surface of sealing region prepares the Ag metal pastes that weight content is 70%-90% in glass sheet perimeter
Coating, the thickness of metal paste coating is 10 μm to 35 μm, and metal paste coating is with dip-coating, spraying, silk-screen printing, manual application
Or machinery coating mode prepare on the surface for treating sealing region in glass sheet perimeter, when metal paste coating use silk screen plate with
When silk-screen printing technique is prepared in glass pane surface, the mesh number of the silk screen plate used is 180 mesh to 400 mesh；
Step 2, drying and processing is carried out to metal paste coating；
Step 3, pre-add hot glass sheet is preferred to 200 DEG C to 350 DEG C with 230 DEG C to 300 DEG C, and is incubated 100 seconds to 120
Second；
Step 4, metal paste coating is heated using sintering process, concrete mode is：Glass plate is integrally heated to 500 DEG C
To 720 DEG C of sintering temperature, kept for 90 seconds to 300 seconds in sintering temperature, Ag metal paste coatings is sintered into and glass plate
The metal layer being consolidated；
Step 5, repeat step 1 to step 4 at least one times, above-mentioned steps prepare metallized layer surface prepare gold again
Categoryization layer, the thickness for making metal layer overall is reached after 5 μm to 25 μm, completes the system of vacuum glass metal sealing metal layer
It is standby.
In the present embodiment, if sintering temperature is located in the tempering temperature of glass plate interval, glass plate is by multiple
After sintering process processing, directly by quickly cooling down, for example, dry, the tempering processing of glass plate is completed, so as to meet making steel
Change the requirement of vacuum glass.Wherein, tempering temperature refers to：During the processing of glass plate tempering, it is heated and is reached according to technological requirement
Temperature.For example, can be 600 DEG C to 700 DEG C.
Certainly, the requirement of toughened vacuum glass is made in order to meet, in the present embodiment, can also have been prepared in metal layer
Tempering processing is carried out after, then to glass plate.
The present embodiment prepares metal layer using Ag metal pastes, and Ag has good Welding performance, and extends
Performance is good, ensures that Welding obtains the sealing-in side of firm, reliable, resistance to alternate stress.Ag metal paste coatings use silk screen plate
Prepared with silk-screen printing technique in glass pane surface, the mesh number of silk screen plate is 230 mesh.Preferably, in the present embodiment in order to protect
Hinder the good sintering effect of Ag metal paste coatings, heating glass plate is incubated 200 seconds to 300 seconds to after 680 DEG C.
Ag metal pastes are used during first sintering metal layer, are used and first time phase during second of sintering metalization layer
Same metal paste.During Ag metal paste coating first sinterings, Argent grain surface oxidation formation silver oxide, and Ag metals
Glass powder in slurry coating, infiltration Argent grain surface.Silver oxide is partly dissolved into glass phase, and glass is mutually penetrated into
Glass pane surface, forms the transition zone that glass mutually wraps up Argent grain.Argent grain is grown up, rapider than surface to reduce, glass more than needed
The space that glass enters between Argent grain under capillary pressure effect, and enter together among space with top layer Argent grain, make
Argent grain is grown up rapidly in the horizontal direction, forms the first metal layer of continuous sponge skeletal like.Second of sintering metal
Change layer to be continuing with and first time identical Ag metal paste.In sintering process, Argent grain surface oxidation formation silver oxide, and Ag
Glass powder in metal paste coating, infiltration Argent grain surface.Silver oxide is partly dissolved into glass phase, and glass mutually permeates
Into in the pore of the first metal layer, solder enters the passage of transition zone when plugging Welding.Argent grain is grown up, than
Surface reduces rapidly, the space that glass more than needed enters between Argent grain under capillary pressure effect, and with surface silver coating
Grain enters among space together, Argent grain is grown up rapidly in the horizontal direction, and glass mutually carries Argent grain into the first metallization
In the pore of layer, make Argent grain continued growth on the first metal layer, the metal layer of front and rear two-step sintering is combined one
Act the new metal layer for foring continuous sponge skeletal like.Further make glass phase and base after second of sintering metalization layer
Plate sintering is firm, formed by new metal layer there is good ductility, can tolerate the thermal shock in brazing process, block
Etch of the solder to transition zone.The metal layer of above-mentioned preparation technology formation is used for three layers, a. transition zones：Sintered with substrate
The Argent grain layer that glass phase and glass together is mutually wrapped up；B. silver layer：The metal layer of continuous sponge skeletal like；C. silver-colored oxygen
Change layer：During Welding, with solder bonds formation intermetallic compounds layer.
Embodiment 2
The preparation method of the vacuum glass metal sealing metal layer of the present embodiment comprises the following steps：
Step 1, treat that the surface of sealing region prepares the Ag metal pulps that weight content is 70%-90% on glass edges of boards periphery
Expect coating, metal paste coating is prepared in glass plate in the way of dip-coating, spraying, silk-screen printing, manual application or machinery coating
Periphery is treated on the surface of sealing region, when metal paste coating uses silk screen plate to be prepared with silk-screen printing technique in glass pane surface
When upper, the mesh number of the silk screen plate used is 180 mesh to 400 mesh；
Step 2, drying and processing is carried out to metal paste coating；
Step 3, the temperature of pre-add hot glass sheet to 200 DEG C to 350 DEG C, is preferred with 230 DEG C to 300 DEG C, and is incubated 100 seconds
To 120 seconds, glass plate is preheated made metal paste coating further solidify simultaneously；
Step 4, metal paste coating is heated using sintering process, concrete mode is：Glass plate is integrally heated to 500 DEG C
To 720 DEG C of sintering temperature, kept for 90 seconds to 300 seconds in sintering temperature, Ag metal paste coatings is sintered into and glass plate
The metal layer being consolidated；
Step 5, using Cu-Ag alloying metals slurry as new metal paste, the processing method of repeat step 1 to step 4
At least one times, Cu-Ag alloy metallizations layer is repeatedly sintered on Ag metal layers, vacuum glass metal sealing metal layer is completed
Preparation.
In this embodiment, if the method for the present invention is used to make toughened vacuum glass, glass plate is by multiple
After sintering process processing, the tempering that glass plate is directly completed by quickly cooling down is handled.
Ag metal pastes are used during first sintering metal layer, Cu-Ag alloys are used during second of sintering metalization layer
Metal paste.Metallic particles is still Argent grain in slurry, and its slurry is substantially Cu-Ag alloying metal slurries.Ag in the present embodiment
Metal paste sinter to be formed the first metal layer technical process it is identical with embodiment 1, therefore not to repeat here.And in Cu-
In Ag alloying metal slurry sintering processes, the silver oxidation on alloying pellet surface forms silver oxide, and in Cu-Ag alloying metal slurries
Glass powder, infiltration Argent grain surface.Silver oxide is partly dissolved into glass phase, and glass mutually penetrates into the first metallization
In the pore of layer, solder enters the passage of transition zone when plugging Welding.The silver on alloying pellet surface makes alloying pellet
Grow up, rapider than surface to reduce, the space that glass more than needed enters between alloy Argent grain under capillary pressure effect, and band
Top layer alloy Argent grain together to enter among space, alloy Argent grain is grown up rapidly in the horizontal direction, glass mutually carries conjunction
Gold grain enters in the pore of the first metal layer, makes alloying pellet continue to give birth on the first metal layer by the silver on surface
Long, the first metal layer sinters the metal layer to be formed with Cu-Ag alloying metal slurries and together form continuous sea
The new metal layer of continuous skeletal like.Second sintering metalization layer uses Cu-Ag alloying metal slurries, it is to avoid erosion silver is existing
As the peak temperature duration can be extended during Welding, and the sealing-in side intensity of acquisition is higher.Formed using above-mentioned preparation technology
Metal layer be three layers, a. transition zones：The Argent grain layer that the glass phase and glass being sintered together with substrate are mutually wrapped up；B. it is silver-colored
Layer：The metal layer (silver-bearing copper composite film) of continuous sponge skeletal like；C. silver-colored oxide layer：Silver-colored oxide layer, Welding process
In, with solder bonds formation intermetallic compounds layer.
Embodiment 3
The preparation method of the vacuum glass metal sealing metal layer of the present embodiment comprises the following steps：
Step 1, treat that the surface of sealing region prepares the Ag metals that weight content is 70% to 90% on glass edges of boards periphery
Slurry coating, metal paste coating is prepared in glass in the way of dip-coating, spraying, silk-screen printing, manual application or machinery coating
Plate periphery is treated on the surface of sealing region, when metal paste coating uses silk screen plate to be prepared with silk-screen printing technique in glass plate table
On face, the mesh number of silk screen plate is 180 mesh to 400 mesh；
Step 2, drying and processing is carried out to metal paste coating；
Step 3, the temperature of pre-add hot glass sheet to 200 DEG C to 350 DEG C, is preferred with 230 DEG C to 300 DEG C, and is incubated 100 seconds
To 120 seconds；
Step 4, metal paste coating is heated using sintering process, concrete mode is：Using the mode of sensing heating by gold
Position where category slurry coating is heated to 500 DEG C to 720 DEG C of sintering temperature, is kept for 90 seconds to 300 seconds in sintering temperature,
Ag metal paste coatings are made to sinter the metal layer being consolidated with glass plate into；
Step 5, using Ni-Ag alloying metals slurry as new metal paste, repeat step 1 to step 4 at least one times,
Ag metallized layer surfaces prepared by above-mentioned steps repeatedly sinter Ni-Ag alloy metallizations layer, complete vacuum glass metal sealing gold
The preparation of categoryization layer.
Due to the present embodiment by the way of local heating sintering metalization layer, therefore, when make toughened vacuum glass when,
Metal layer directly can be prepared on armorplate glass, can also be after metal layer prepare completion, then glass plate is entered
The processing of row tempering.
Certainly, in step 4 can also using laser heating, flame heating, electric current heating or microwave heating by the way of pair
Position heat-agglomerating where metal paste coating.
Metal paste can also be：Ni metal pastes, Au metal pastes, Au alloying metals slurry, Zn metal pastes, Zn are closed
Golden metal paste, Pd metal pastes or Pd alloying metal slurries.Deng.
Ag metal pastes are used during first sintering metal layer, Ni-Ag alloys are used during second of sintering metalization layer
Metal paste.Metallic particles is still Argent grain in slurry, and its slurry is substantially Ni-Ag alloying metal slurries.Ag in the present embodiment
Metal paste sinter to be formed the first metal layer technical process it is identical with embodiment 1, therefore not to repeat here.And in Ni-
In Ag alloying metal slurry sintering processes, the silver oxidation on alloying pellet surface forms silver oxide, and in Ni-Ag alloying metal slurries
Glass powder, infiltration Argent grain surface.Silver oxide is partly dissolved into glass phase, and glass mutually penetrates into the first metallization
In the pore of layer, solder enters the passage of transition zone when plugging Welding.The silver on alloying pellet surface makes alloying pellet
Grow up, rapider than surface to reduce, the space that glass more than needed enters between alloy Argent grain under capillary pressure effect, and band
Top layer alloy Argent grain together to enter among space, alloy Argent grain is grown up rapidly in the horizontal direction, glass mutually carries conjunction
Gold grain enters in the pore of the first metal layer, makes alloying pellet continue to give birth on the first metal layer by the silver on surface
Long, the first metal layer sinters the metal layer knot to be formed with alloying metal slurry in Ni-Ag alloying metal slurry sintering processes
It is combined the new metal layer for foring continuous sponge skeletal like.Second of sintering metalization layer uses Ni-Ag alloys
Metal paste, it is to avoid the silver-colored phenomenon of erosion, can extend the peak temperature duration during Welding, but the wellability of nickel and tin compares copper
Wellability with tin is strong, and therefore, the sealing-in side intensity of acquisition is higher.The metal layer of above-mentioned preparation technology formation is used for three
Layer, a. transition zones：The Argent grain layer that the glass phase and glass being sintered together with substrate are mutually wrapped up；B. silver layer：Continuous sponge
The silver-colored nickel composite membrane of skeletal like；C. silver-colored oxide layer：During silver-colored oxide layer, Welding, change between solder bonds formation metal
Compound layer.
Several preferred embodiments of the application, but the application not limited to this, every ability are only described above in association with accompanying drawing
Domain those of ordinary skill is not in the case where departing from spirit herein, and any improvement and/or deformation made belong to the guarantor of the application
Protect scope.
Claims (10)
1. a kind of preparation method of vacuum glass metal sealing metal layer, it is characterised in that this method comprises the following steps：
Step 1, treat that the surface of sealing region prepares metal paste coating in glass sheet perimeter；
Step 2, drying and processing is carried out to metal paste coating；
Step 3, pre-add hot glass sheet keeps the temperature to 200 DEG C to 350 DEG C within the period of setting；
Step 4, metal paste coating is heated using sintering process, it is consolidated with glass plate, form metal layer；
Step 5, repeat step 1 to step 4 at least one times, complete vacuum glass sealing-in metal layer preparation.
2. preparation method as claimed in claim 1, it is characterised in that in the step 1, the metal paste coating is to soak
The mode that painting, spraying, silk-screen printing, manual application or machinery are coated is prepared on the surface for treating sealing region in glass sheet perimeter.
3. preparation method as claimed in claim 2, it is characterised in that the metal paste coating uses silk screen plate with screen printing
Dataller's skill is prepared in glass pane surface, and the mesh number of the silk screen plate is 180 mesh to 400 mesh.
4. preparation method as claimed in claim 1, it is characterised in that in the step 3 pre-add hot glass sheet to 230 DEG C extremely
300 DEG C, and keep the temperature 100 seconds to 120 seconds.
5. preparation method as claimed in claim 1, it is characterised in that the sintering process of the step 4 is specially：Preparation is had
The glass plate of metal paste coating is integrally heated to sintering temperature, and the tempering temperature that the sintering temperature is located at glass plate is interval interior.
6. preparation method as claimed in claim 5, it is characterised in that when the glass plate warp for preparing and having metal paste coating
Cross after multiple sintering process processing, the tempering that glass plate is directly completed by quickly cooling down is handled.
7. preparation method as claimed in claim 1, it is characterised in that the sintering process of the step 4 is specially:Preparation is had
The glass plate of metal paste coating is integrally heated to 500 DEG C to 720 DEG C, and keeps the temperature 90 seconds to 300 seconds.
8. preparation method as claimed in claim 1, it is characterised in that the sintering process of the step 4 is specially：To metal pulp
Position where material coating is heated, and heating-up temperature is 500 DEG C to 720 DEG C, and keeps the temperature 90 seconds to 300 seconds.
9. preparation method as claimed in claim 1, it is characterised in that the metal paste is Ag metal pastes, Cu-Ag alloys
Metal paste, Ni metal pastes, Ni-Ag alloying metals slurry, Au metal pastes, Au alloying metals slurry, Zn metal pastes, Zn
Alloying metal slurry, Pd metal pastes or Pd alloying metal slurries.
10. preparation method as claimed in claim 1, it is characterised in that the metal paste be silver-colored weight content be 70% to
90% Ag metal pastes.
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| CN201710280885.9A CN106986551A (en) | 2017-04-26 | 2017-04-26 | A kind of preparation method of vacuum glass metal sealing metal layer |
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| CN201710280885.9A CN106986551A (en) | 2017-04-26 | 2017-04-26 | A kind of preparation method of vacuum glass metal sealing metal layer |
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| CN110642534A (en) * | 2019-11-06 | 2020-01-03 | 武汉理工大学 | Vacuum glass with composite layer sealing structure and anodic bonding packaging method thereof |
| CN113698112A (en) * | 2021-09-27 | 2021-11-26 | 重庆英诺维节能环保科技有限公司 | Preparation method of tailless vacuum glass |
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Application publication date: 20170728 |