CN110642535A - Method for preparing vacuum glass for vacuumizing and sealing in vacuum furnace - Google Patents

Method for preparing vacuum glass for vacuumizing and sealing in vacuum furnace Download PDF

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Publication number
CN110642535A
CN110642535A CN201911143468.5A CN201911143468A CN110642535A CN 110642535 A CN110642535 A CN 110642535A CN 201911143468 A CN201911143468 A CN 201911143468A CN 110642535 A CN110642535 A CN 110642535A
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CN
China
Prior art keywords
glass
vacuum
sealing
flat glass
vacuumizing
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CN201911143468.5A
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Chinese (zh)
Inventor
张方娥
温泽
张瑶
孙诗兵
田英良
呂锋
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Beijing University of Technology
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Beijing University of Technology
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Priority to CN201911143468.5A priority Critical patent/CN110642535A/en
Publication of CN110642535A publication Critical patent/CN110642535A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C27/00Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
    • C03C27/06Joining glass to glass by processes other than fusing
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C27/00Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
    • C03C27/06Joining glass to glass by processes other than fusing
    • C03C27/08Joining glass to glass by processes other than fusing with the aid of intervening metal

Abstract

The invention discloses a preparation method of vacuum glass for vacuumizing and sealing in a vacuum furnace, which comprises the following steps: arranging a wetting film at the corresponding position of the edge seals of the two pieces of flat glass; placing a sealing metal foil on the wetting film of the lower flat glass; arranging array support columns at corresponding positions of the lower piece of flat glass; placing the upper piece of flat glass on the lower piece of flat glass with the supporting columns, and combining the upper piece of flat glass and the lower piece of flat glass; placing the laminated plate glass in a vacuum furnace; vacuumizing the vacuum furnace, and heating to the sealing temperature for sealing the metal foil to seal the edges of the two pieces of flat glass; after cooling, vacuum glass was obtained. The invention can omit the hole aligning process of punching and vacuumizing, continuously carry out vacuumizing and sealing in a vacuum furnace, and change the prior process sequence of sealing edge and vacuumizing into the process sequence of vacuumizing and sealing edge; the method can improve the continuity of the process, shorten the vacuumizing time, avoid manual intervention in the process and create conditions for full-line continuity and automation.

Description

Method for preparing vacuum glass for vacuumizing and sealing in vacuum furnace
Technical Field
The invention relates to the technical field of vacuum glass, in particular to a preparation method of vacuum glass for vacuumizing and sealing in a vacuum furnace, which is suitable for manufacturing flat plate type vacuum glass.
Background
The two pieces of plate glass are supported in an array arrangement by using tiny support columns to form a gap with a certain height; the peripheries of the two pieces of flat glass are sealed by sealing solders, and the gap is vacuumized to form flat vacuum glass, which is called vacuum glass for short. The vacuum glass can block heat conduction and convection heat transfer in three basic heat transfer modes, so that the vacuum glass has good heat insulation performance and is widely used for heat insulation of building doors and windows, curtain walls and industrial transparent bodies (such as refrigerators).
The vacuum glass should have good perspective effect, so the supporting column should be as small as possible to avoid causing discomfort in perspective. The diameter of the vacuum glass supporting column is about 0.2mm, and the existence of the supporting column is difficult to detect without carefully recognizing; the height of the support columns is also typically about 0.2mm because thin and tall support columns are easily unstable and the vacuum thermal resistance characteristics are independent of vacuum thickness. Usually, the support columns are made of metal materials, and are too dense to form a large number of support column heat bridges for heat transfer; if the support columns are too thin, the two pieces of plate glass may form deflection deformation between the support columns, and the plate glass may contact with each other to lose the vacuum effect. The optimized result at present is that the spacing between the support columns is 30 mm-50 mm, and the support columns are arranged in an array.
The largest application of the vacuum glass is doors, windows and curtain walls of buildings, and the flat glass of the vacuum glass required in the building safety design specification must be safety glass with higher strength, and generally adopts physical toughened glass. The physical tempered glass is formed with a surface compressive stress (pre-set stress) inside the glass by heating the glass and then forcibly cooling the glass with cold air to achieve an enhanced effect. After reheating and tempering, the structure of the glass can be relaxed, the preset stress is subsided, and the requirement of safe glass can not be met. The strain point temperature is set as the lower limit of the annealing temperature of the glass, and the preset stress in the glass is gradually relieved below the strain point temperature. That is, the strain point temperature is the upper limit of the glass sealing temperature. In fact, when the sealing temperature is lower than the strain point temperature, the preset stress in the glass is also reduced, and the reduction speed is only reduced. Therefore, in order to protect the preset stress of the tempered glass, the vacuum glass should use as low a sealing temperature as possible during the manufacturing process.
The process of sealing the perimeter of a vacuum glass with a material and process is called edge sealing, and the resulting configuration is also called edge sealing. Strict air tightness is a necessary condition for obtaining a vacuum, and the material of the edge seal should be capable of bonding two pieces of flat glass together and forming a certain bonding strength. Glass sealing solders are commonly used edge sealing materials because glass generally has good wetting and bonding strength; meanwhile, the metal material has excellent processability, and the melting point of the metal can be reduced to be lower than the strain point temperature of the glass in an alloy mode, so that the metal is also an ideal material for glass sealing and welding.
At present, the common manufacturing process of vacuum glass is to punch a hole (air extraction hole) on a piece of flat glass, seal the periphery of the vacuum glass, extract vacuum from the air extraction hole, and then seal the air extraction hole to form vacuum.
The manufacturing process has the following defects:
the hole is punched in advance before vacuum pumping, manual operation is needed for hole alignment in the vacuum pumping process, and the precision required for hole alignment operation is high; the pumping hole is not suitable to be too large (generally the diameter is 5-7mm), otherwise the appearance is influenced, and the efficiency of pumping vacuum is low; the air exhaust holes are easy to fail, and the failure of the air exhaust holes is a main factor causing the failure of the manufacture or use of the vacuum glass. The edge sealing process is firstly carried out, and the vacuum pumping process is switched to after the edge sealing process is finished, so that manual intervention is needed, the process is not convenient to be continuous, and the production cost is increased. The process is the main reason that the vacuum glass can not be continuously produced at present, and the product cost is difficult to reduce.
Disclosure of Invention
Aiming at the defects in the problems, the invention provides a preparation method of vacuum glass for vacuumizing and sealing in a vacuum furnace.
The invention discloses a preparation method of vacuum glass for vacuumizing and sealing in a vacuum furnace, which comprises the following steps:
arranging a wetting film at the corresponding position of the edge seals of the two pieces of flat glass;
placing a sealing metal foil on the wetting film of the lower flat glass;
arranging array support columns at corresponding positions of the lower piece of flat glass;
placing the upper piece of flat glass on the lower piece of flat glass with the supporting columns, and combining the upper piece of flat glass and the lower piece of flat glass;
placing the laminated plate glass in a vacuum furnace;
vacuumizing the vacuum furnace, and heating to the sealing temperature of the sealing metal foil to seal edges of the two pieces of flat glass;
after cooling, vacuum glass was obtained.
As a further improvement of the invention, two pieces of flat glass are continuously vacuumized and sealed in the vacuum furnace.
As a further improvement of the invention, the wetting film wets the sealing metal foil to form an adhesive strength.
As a further development of the invention, the wetting film has a thickness of not more than 50 μm and a width of the sealing edge.
As a further improvement of the invention, the thickness of the sealing metal foil is 2/5-1/2 of the height of the sealing edge, and the width is calculated according to the following formula:
the width of the sealing metal foil is [ W x (H-2 XH 1) ]/H2
Wherein W is the seal width, H is the seal height, H1 is the wetting film thickness, and H2 is the seal foil height.
As a further improvement of the invention, the sealing metal foil is flush with the outer side of the lower flat glass sheet.
As a further improvement of the invention, the vacuum degree of the vacuum glass prepared by the vacuum glass preparation method is not lower than the vacuum degree required by the vacuum glass.
As a further improvement of the invention, the wetting film is a silver film sintered or sputtered on the flat glass, the sealing metal foil is a tin foil or an alloy soldering lug, and the melting point of the sealing metal foil is lower than 350 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method of the vacuum glass can omit the prior hole punching and vacuumizing hole aligning processes, continuously carries out vacuumizing and sealing in a vacuum furnace, and changes the prior process sequence of sealing edge and vacuumizing, into the process sequence of vacuumizing and sealing edge; the method can improve the continuity of the process, shorten the vacuumizing time, avoid manual intervention in the process and create conditions for full-line continuity and automation.
Drawings
FIG. 1 is a flow chart of a method for manufacturing vacuum glass by performing vacuum-pumping and sealing in a vacuum furnace according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a vacuum glass before sealing according to an embodiment of the present invention;
fig. 3 is a schematic structural diagram of a vacuum glass before sealing according to an embodiment of the present invention.
In the figure:
1. discharging the flat glass; 2. wetting the membrane; 3. sealing the metal foil; 4. loading flat glass; 5. and (4) a support column.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
In the description of the present invention, it should also be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or chemically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
As shown in FIG. 1, the present invention provides a method for manufacturing vacuum glass by vacuum-pumping and sealing in a vacuum furnace, which comprises the following core steps:
arranging a wetting film at the corresponding position of the edge seals of the two pieces of flat glass;
placing a sealing metal foil on the wetting film of the lower flat glass;
arranging array support columns at corresponding positions of the lower piece of flat glass;
placing the upper piece of flat glass on the lower piece of flat glass with the supporting columns, and combining the upper piece of flat glass and the lower piece of flat glass;
placing the laminated plate glass in a vacuum furnace;
vacuumizing the vacuum furnace, and heating to the sealing temperature for sealing the metal foil to seal the edges of the two pieces of flat glass;
after cooling, vacuum glass was obtained.
In order to realize the preparation process of the core, the following embodiments will be further described with reference to the working mechanism:
as shown in FIGS. 1 to 3, the present invention provides a method for manufacturing vacuum glass for performing vacuum-pumping and sealing in a vacuum furnace, comprising:
s1, arranging a wetting film 2 at the corresponding position of the edge sealing of the two pieces of flat glass 1 and 4;
that is, as shown in fig. 2, a wetting film 2 is disposed on the upper edge of the sealed edge of the lower glass sheet 1, and a corresponding wetting film 2 is disposed on the lower edge of the sealed edge of the upper glass sheet 4. Wherein the content of the first and second substances,
the wetting film 2 is wetted with the two pieces of flat glass 1 and 4 to form bonding strength; the wetting film 2 has a thickness of not more than 50 μm and a width of the sealing edge.
S2, placing the sealing metal foil 3 on the wetting film 2 of the lower flat glass 1;
that is, as shown in fig. 2, a circle of sealing metal foil 3 is placed on the wetting film 2 of the lower flat glass 1 to ensure that the sealing metal foil 3 is melted to achieve complete sealing of the two flat glasses 1 and 4. Wherein the content of the first and second substances,
the wetting film 2 and the sealing metal foil 3 are wetted to form bonding strength;
the wetting film 2 in S1, S2 functions as: the wetting film 2, in addition to providing good wetting and adhesion between the sealing foil 3 and the sheet glass, is primarily responsible for positioning the edge seal. Lotus effect and wetting: the liquid is always concentrated towards the wet part, while the non-wet part is not easy to adhere; based on the lotus effect and the wetting principle, the molten sealing metal foil liquid is shrunk and concentrated to the wetting film which can be wetted, the wetting film is arranged at the corresponding position of the edge sealing of the two pieces of flat glass of the vacuum glass, and the molten sealing metal foil liquid can be concentrated between the upper wetting film and the lower wetting film which are preset. Under the action of no other external force, the molten sealing metal foil liquid reaches a certain thickness under the action of interfacial tension, gravity and melt surface tension, and the thickness is the natural thickness. Typically the natural thickness of the metal is in the order of a few millimeters. The thickness of the gap of the vacuum glass is about 0.2mm, and the vacuum glass can not spread to a non-wetting part any more.
The thickness of the sealing metal foil is 2/5-1/2 of the height of the sealing edge, and the width is calculated according to the following formula:
the width of the sealing metal foil is [ W x (H-2 XH 1) ]/H2
Wherein W is the seal width, H is the seal height, H1 is the wetting film thickness, and H2 is the seal metal foil height; the sealing metal foil is flush with the outer side of the lower flat glass.
S3, arranging array supporting columns 5 at corresponding positions of the lower piece of flat glass 1; wherein the content of the first and second substances,
the size and shape of the array support posts 5 may be conventional and conventional structures and methods, and therefore, will not be described in detail herein.
S4, placing the upper flat glass 4 on the lower flat glass 1 with the support columns 5, and combining the sheets; as shown in fig. 2.
S5, placing the laminated plate glass in a vacuum furnace; wherein the content of the first and second substances,
the vacuum furnace adopted by the invention is equipment for heating in a vacuum environment, and the vacuum furnace can be a single body, such as a vacuum furnace adopted by an electric vacuum device, vacuum sintering and the like; or continuous, such as continuous large-area vacuum glass coating production. The strain point temperature of the plate glass is about 450 ℃, and the sealing temperature of the sealing metal foil is lower than 400 ℃, preferably lower than 350 ℃;
meanwhile, the sealing metal foil can prevent the sealing metal foil from being oxidized when being heated and melted in a vacuum state.
S6, vacuumizing in a vacuum furnace, and heating to the sealing temperature of the sealing metal foil to seal edges of the two pieces of flat glass; wherein the content of the first and second substances,
the two pieces of flat glass are continuously vacuumized and sealed in a vacuum furnace, and can be continuously pumped out before sealing metal foils are melted and sealed; and after the sealing metal foil is melted and the edge sealing is finished, vacuumizing is finished.
And S7, cooling to obtain the vacuum glass, as shown in figure 3.
Further, the choice of the wetting film and the sealing foil according to the invention may be:
the wetting film of the present invention is a silver film sintered or sputtered on a plate glass, and other components satisfying the above-described wetting film function may be selected similarly. The sealing metal foil is a tin foil or an alloy soldering lug, and the melting point of the sealing metal foil is lower than 350 ℃. Wherein the content of the first and second substances,
1. the commercially available nano silver powder is coated by screen printing before tempering the plate glass, then is sintered on the plate glass during tempering, and the sealing metal foil adopts tin foil (the melting point is 232 ℃);
2. sputtering silver plating below 350 ℃, and adopting low-melting-point alloy for sealing the metal foil. There are many commercially available low-melting-point metal alloys, and a low-melting-point alloy solder material contains silver-series SAC305, SAC387, SAC405, and the like, in which SAC305 is sn96.5ag3.0cu0.5, and the solid/liquid phase temperature is 217/218. Pb60In40 without silver, solid/liquid phase temperature 197/231; pb90Sn10, solid/liquid phase temperature 275/302, and the like.
Further, the purpose of wetting the membrane can theoretically be achieved by a monolayer, so that the wetting membrane is not too thick, the thickness is not more than 50 μm, and the cross-sectional area of the vacuum pumping is affected by too thick. The wetting film positions the width of the seal edge so that the wetting film width is the width of the seal edge. The sealing width is wide to meet the mechanical property and air tightness requirements of the vacuum glass, and the sealing width is too narrow, which may affect the satisfaction of the requirements. The sealing edge is too wide, the non-transparent sealing edge influences lighting and attractiveness, and the width of the sealing edge is generally 8-10 mm.
Further, the sealing foil can form a bond strength with the wetting film. The invention does not need to arrange a separate air exhaust hole. If the gap between the two flat glass sheets is 0.2mm, the height of the sealing foil is 1/2, i.e. 0.1mm, and the thickness of the wetting film is 50 μm, i.e. 0.01mm, then there is still a gap of 0.09 between the sheets to provide the evacuation. Assuming that the size of the vacuum glass is 1200mm × 400mm, the sectional area in which vacuum can be drawn is 288mm2. If the diameter of the air suction hole is 7mm, the cross section area is 38.5mm2. Because the gap space is reserved for vacuumizing, the sealing metal foil automatically shrinks and fills the reserved gap space after being melted.
Further, the vacuum degree of the vacuum glass prepared according to the vacuum glass preparation method is not lower than the vacuum degree required by the vacuum glass. Wherein the vacuum degree of the vacuum glass is usually not more than 0.1 Pa; obviously, reaching a certain vacuum degree is the first requirement of vacuum glass and also the requirement of a vacuum furnace. The vacuum glass standard does not directly require the vacuum degree, but stipulates the heat preservation performance (K value) and the sound insulation performance. The two properties are application properties, and are related to factors such as the design of the vacuum glass, such as the material and the density of the support pillars, besides the vacuum degree. This patent is when implementing, can combine specific vacuum glass according to the requirement of heat preservation performance in the standard, selects the vacuum requirement of vacuum furnace through the experiment.
The invention has the advantages that:
the vacuum glass preparation method can omit the prior punching and hole aligning processes, continuously carries out vacuumizing and sealing in a vacuum furnace by the process and equipment, and changes the prior process sequence of edge sealing and vacuumizing into the process sequence of vacuumizing and edge sealing; the method can improve the continuity of the process, shorten the vacuumizing time, avoid manual intervention in the process and create conditions for full-line continuity and automation.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (8)

1. A method for preparing vacuum glass for vacuumizing and sealing in a vacuum furnace is characterized by comprising the following steps:
arranging a wetting film at the corresponding position of the edge seals of the two pieces of flat glass;
placing a sealing metal foil on the wetting film of the lower flat glass;
arranging array support columns at corresponding positions of the lower piece of flat glass;
placing the upper piece of flat glass on the lower piece of flat glass with the supporting columns, and combining the upper piece of flat glass and the lower piece of flat glass;
placing the laminated plate glass in a vacuum furnace;
vacuumizing the vacuum furnace, and heating to the sealing temperature of the sealing metal foil to seal edges of the two pieces of flat glass;
after cooling, vacuum glass was obtained.
2. The method for producing vacuum glass according to claim 1, wherein two sheets of flat glass are continuously evacuated and sealed in the vacuum furnace.
3. The vacuum glass manufacturing method according to claim 1, wherein the wetting film wets the sealing metal foil to form an adhesive strength.
4. The method of making vacuum glass according to claim 1 or claim 3, wherein the wetting film has a thickness of no greater than 50 μm and a width that is the width of the edge seal.
5. The method of making vacuum glass according to claim 1, wherein the sealed metal foil has a thickness of 2/5-1/2 of the seal height and a width calculated according to the formula:
the width of the sealing metal foil is [ W x (H-2 XH 1) ]/H2
Wherein W is the seal width, H is the seal height, H1 is the wetting film thickness, and H2 is the seal foil height.
6. The method of claim 1 or 5, wherein the sealing foil is flush with the outer side of the lower glass sheet.
7. The method for producing vacuum glass according to claim 1, wherein the vacuum glass produced by the method for producing vacuum glass has a degree of vacuum not lower than a degree of vacuum required for vacuum glass.
8. The vacuum glass manufacturing method according to claim 1, wherein the wetting film is a silver film sintered or sputtered on the plate glass, the sealing metal foil is a tin foil or an alloy tab, and the melting point of the sealing metal foil is lower than 350 ℃.
CN201911143468.5A 2019-11-20 2019-11-20 Method for preparing vacuum glass for vacuumizing and sealing in vacuum furnace Pending CN110642535A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102249560A (en) * 2010-11-03 2011-11-23 洛阳兰迪玻璃机器有限公司 Method for sealing vacuum glass and vacuum glass product
CN102951787A (en) * 2012-03-21 2013-03-06 戴长虹 Vacuum glass edge sealing method by utilizing metal solders and product manufactured by method
CN104003628A (en) * 2013-02-26 2014-08-27 中国建材检验认证集团股份有限公司 Vacuum glass with metal edge-sealing structure and making method thereof
CN105621902A (en) * 2015-12-28 2016-06-01 太仓耀华玻璃有限公司 Packaging method for vacuum glass
JP2018058709A (en) * 2016-10-03 2018-04-12 日立化成株式会社 Vacuum heat-insulation member, sealing material for use therein, and method for producing vacuum heat-insulation member

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102249560A (en) * 2010-11-03 2011-11-23 洛阳兰迪玻璃机器有限公司 Method for sealing vacuum glass and vacuum glass product
CN102951787A (en) * 2012-03-21 2013-03-06 戴长虹 Vacuum glass edge sealing method by utilizing metal solders and product manufactured by method
CN104003628A (en) * 2013-02-26 2014-08-27 中国建材检验认证集团股份有限公司 Vacuum glass with metal edge-sealing structure and making method thereof
CN105621902A (en) * 2015-12-28 2016-06-01 太仓耀华玻璃有限公司 Packaging method for vacuum glass
JP2018058709A (en) * 2016-10-03 2018-04-12 日立化成株式会社 Vacuum heat-insulation member, sealing material for use therein, and method for producing vacuum heat-insulation member

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Application publication date: 20200103