阅读说明：本技术 真空玻璃内置吸气剂的激活方法及包覆结构及封装结构 (Activation method of built-in getter of vacuum glass, coating structure and packaging structure ) 是由 蒋毅 孙景春 刘谦 于 2020-11-25 设计创作，主要内容包括：本发明公开了一种真空玻璃内置吸气剂的激活方法及包覆结构及激活结构,解决了现有真空玻璃内置吸气剂激活方法步骤繁琐的问题。本发明将吸气剂的激活工艺与真空玻璃的抽真空排气工艺相结合,在真空玻璃排气的同时对吸气剂进行激活,设置抽真空时加热炉温度为200℃至300℃,设置抽真空的时间为25min至110min,采用非蒸散型吸气剂,吸气剂的激活温度为200℃至300℃,激活时间为25min至110min。本发明具有简化工艺流程,工艺简单易行,提高生产效率,降低生产成本等优点。(The invention discloses an activation method, a coating structure and an activation structure of a built-in getter of vacuum glass, and solves the problem that the conventional activation method of the built-in getter of vacuum glass has complicated steps. The method combines the activation process of the getter with the vacuumizing and exhausting process of vacuum glass, activates the getter while exhausting the vacuum glass, sets the temperature of a heating furnace to be 200-300 ℃ during vacuumizing, sets the vacuumizing time to be 25-110 min, adopts a non-evaporable getter, sets the activation temperature of the getter to be 200-300 ℃ and the activation time to be 25-110 min. The invention has the advantages of simplifying the process flow, being simple and easy to operate, improving the production efficiency, reducing the production cost and the like.)

1. An activation method of a getter arranged in vacuum glass is characterized in that,

in the process of manufacturing the vacuum glass, the activation process of the getter (1) is combined with the vacuumizing and exhausting process of the vacuum glass, and the getter (1) is activated while the vacuum glass is vacuumized and exhausted;

setting the temperature of the heating furnace to be 200-300 ℃ during vacuumizing, and setting the vacuumizing time to be 25-110 min;

the method is characterized in that a non-evaporable getter (1) is adopted, the activation temperature of the non-evaporable getter (1) is 200-300 ℃, the activation time is 25-110 min, and the non-evaporable getter (1) is a zirconium vanadium iron type solid substance.

2. The method for activating the getter built in the vacuum glass according to claim 1, comprising the following steps:

step 1), putting the vacuum glass component with the getter (1) into a heating furnace;

step 2), heating the heating furnace, and carrying out sealing welding on the periphery of the vacuum glass component to form a vacuum glass cavity;

step 3), cooling the heating furnace, maintaining the temperature at 200-300 ℃, and vacuumizing the sealed and welded vacuum glass cavity from the air extraction opening (7);

step 4), keeping the vacuumizing time to be 25-110 min until the vacuum degree in the vacuum glass cavity reaches 0.01-0.001 Pa, and completing the activation of the getter (1);

and 5), keeping vacuumizing the sealed and welded vacuum glass cavity, and welding the sealing sheet (8) on the air extraction opening (7).

3. A coating structure of a getter built in vacuum glass, which is characterized in that the coating structure is used for the activation method of the getter built in vacuum glass according to any one of claims 1 and 2, wherein the getter (1) is coated by the coating structure, the coating structure is an unsealed cavity, and gas is communicated between the getter (1) in the unsealed cavity and the vacuum glass cavity.

4. The coating structure of the getter built-in vacuum glass according to claim 3,

the cladding structure is formed by folding a planar structure (2);

the planar structure (2) is folded and coated along the surface of the getter (1) until the surface of the getter (1) is completely covered by the planar structure (2);

the folding part of the plane structure (2) is provided with an overlapping area, a gap (3) exists in the overlapping area, and gas in the vacuum glass cavity is in contact with the surface of the getter (1) through the gap (3).

5. The coating structure of the getter built-in vacuum glass according to claim 3,

the coating structure comprises a polyhedral shell structure and a plurality of covering structures, wherein at least one side surface of the polyhedral shell structure is provided with an opening;

the covering structure covers the opening of the polyhedral shell structure, a gap (3) is formed at the contact position of the covering structure and the polyhedral shell structure, and gas in the vacuum glass cavity is in contact with the surface of the getter (1) through the gap (3);

the covering structure is a plane structure (2) or a polyhedral shell structure, and at least one side surface of the polyhedral shell structure is provided with an opening.

6. The structure of claim 4 or 5, wherein the planar structure (2) and the polyhedral shell structure are made of a material having a heat resistance temperature higher than 200 ℃, such as tin foil or aluminum foil.

7. A vacuum glass getter packaging structure, which is used in the activation method of a vacuum glass getter according to any one of claims 1 and 2;

comprises a vacuum glass component, a sealing sheet (8) and a getter (1);

the vacuum glass component comprises two glass substrates (4), a support (6) is arranged between the two glass substrates (4), glass solders (5) are arranged at the peripheral edges of the two glass substrates (4), the air exhaust port (7) is arranged on one of the glass substrates (4), and the getter (1) is placed in the air exhaust port (7);

the sealing sheet (8) is placed on the outer side of the air extraction opening (7).

Technical Field

The invention relates to the technical field of vacuum application, in particular to an activation method, a coating structure and a packaging structure of a built-in getter of vacuum glass.

Background

In the use of the vacuum glass, the surface outgassing phenomenon of the glass substrate and the edge sealing welding material and the inherent gas permeability of each component material of the vacuum glass can cause the vacuum degree attenuation phenomenon of the vacuum glass in the long-term use process, and a getter needs to be placed in a cavity of the vacuum glass in order to maintain the service life of the vacuum glass.

One method is to activate the getter in advance and tightly enclose it in a metal or glass closed container to isolate it from the atmosphere. And putting the encapsulated getter into the cavity of the vacuum glass or the exhaust hole in advance, and opening the encapsulating container after the vacuum glass is manufactured. This method not only requires an additional vacuum brazing apparatus for encapsulating the getter but also requires a complicated process and an additional apparatus for opening the encapsulating case, which increases the production cost.

The other method is that the getter is put into a cavity of the vacuum glass or an exhaust hole before the vacuum glass is manufactured, and the getter is contacted with the atmosphere at the moment, so that the getter loses the air suction function and needs to be activated after the vacuum glass is manufactured.

The getter with high activation temperature is usually activated by adopting a high-frequency heating method, the method not only needs to use high-frequency heating equipment, but also is easy to cause local severe temperature rise of glass to generate thermal stress while heating the getter, and is very unfavorable for the strength and the service life of the glass; the getter with low activation temperature is oxidized by atmosphere in the heating process of sealing and connecting the edges of the vacuum glass due to strong activity of the getter, so that the getter fails and can not be reversed after reactivation.

After the vacuum glass is manufactured, the getter is activated, gas molecules adsorbed on the surface of the getter are released into the vacuum layer, the vacuum degree of the vacuum glass is reduced to a certain degree, and the gas molecules released from the surface of the getter are adsorbed by the getter again in the later use process of the vacuum glass, so that the gas absorption capacity of the getter is reduced, the vacuum degree of the vacuum glass is reduced, and the service life of the vacuum glass is shortened.

Disclosure of Invention

The technical problem to be solved by the invention is as follows: the steps of the conventional method for activating the built-in getter in the vacuum glass are complicated, and the invention provides a method for activating the built-in getter in the vacuum glass, a coating structure and a packaging structure, which solve the problems.

The invention is realized by the following technical scheme:

an activation method of a getter built in vacuum glass is characterized in that in the process of manufacturing the vacuum glass, the activation process of the getter is combined with the vacuumizing and exhausting process of the vacuum glass, and the getter is activated while the vacuum glass exhausts; setting the temperature of a heating furnace to be 200-300 ℃ during vacuumizing, and keeping the vacuumizing time to be 25-110 min; the method is characterized in that a non-evaporable getter is adopted, the activation temperature of the non-evaporable getter is 200-300 ℃, the activation time is 25-110 min, and the non-evaporable getter is zirconium vanadium iron and is a solid substance.

Further, the method comprises the following specific steps:

step 1), putting the vacuum glass component with the getter into a heating furnace;

step 2), heating the heating furnace, and carrying out sealing welding on the periphery of the vacuum glass component to form a vacuum glass cavity;

step 3), cooling the heating furnace, maintaining the temperature at 200-300 ℃, and vacuumizing the sealed and welded vacuum glass cavity from the air suction port;

step 4), keeping the vacuumizing time to be 25-110 min until the vacuum degree in the vacuum glass cavity reaches 0.1-0.001 Pa, and finishing the activation of the getter;

and 5), keeping vacuumizing the sealed and welded vacuum glass cavity, and welding the sealing sheet on the air extraction opening.

A coating structure of a built-in getter of vacuum glass is used in any one of the activation methods of the built-in getter of vacuum glass, the coating structure is a non-sealed cavity, and gas flows between the getter in the non-sealed cavity and the vacuum glass cavity.

Further, the coating structure is formed by folding a plane structure, and the plane structure is folded and coated along the surface of the getter until the surface of the getter is completely covered by the plane structure; the folded part of the planar structure has an overlapping region, a gap exists in the overlapping region, and gas in the vacuum glass cavity is in contact with the surface of the getter through the gap.

Furthermore, the coating structure comprises a polyhedral shell structure and a plurality of covering structures, and at least one side surface of the polyhedral shell structure is provided with an opening; the covering structure covers the opening of the polyhedral shell structure, a gap exists at the contact position of the covering structure and the polyhedral shell structure, and gas in the vacuum glass cavity is in contact with the surface of the getter through the gap; the covering structure is a plane structure or a polyhedral shell structure, and at least one side surface of the polyhedral shell structure is an opening surface; gaps exist at the contact parts of the covering structures and the polyhedral shell structures, and gas in the vacuum glass cavity can be in contact with the surfaces of the getters through the gaps.

Furthermore, the plane structure and the polyhedral shell structure are made of tin foil or aluminum foil and other foldable materials with the heat-resisting temperature higher than 200 ℃, and the aluminum foil or the tin foil has very strong plasticity and can be arbitrarily kneaded into various shapes so as to be convenient for coating the getter.

A packaging structure of a vacuum glass built-in getter is used in any one of the activation methods of the vacuum glass built-in getter, and comprises a vacuum glass component, a sealing sheet and a getter; the vacuum glass component comprises two glass substrates, a support is arranged between the two glass substrates, glass solders are arranged at the peripheral edges of the two glass substrates, the air exhaust port is arranged on one glass, and the getter is placed in the air exhaust port; the sealing piece is placed on the outer side of the air extraction opening.

The invention has the following advantages and beneficial effects:

the method combines the step of activating the getter with the step of vacuumizing the vacuum glass, and activates the getter when the vacuum glass is vacuumized and exhausted, so that the process flow is simplified, and the subsequent equipment and process for activating the getter are saved; the coating structure of the getter is simple and easy to implement, and the getter can be protected from being oxidized compared with the uncoated getter; compared with the existing getter tight encapsulation structure, the vacuum brazing equipment and the process for manufacturing the getter tight encapsulation structure can be reduced, the process and the equipment for unsealing the getter tight encapsulation structure after the vacuum glass is manufactured can be reduced, the production cost is obviously reduced, and the production efficiency is improved.

Drawings

The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention. In the drawings:

FIG. 1 is a view showing a structure of a getter incorporated in a vacuum glass.

Fig. 2 is a planar view of the coating structure of the getter.

FIG. 3 is a graph showing the change of a vacuum glass performance parameter (U value) with time during the use of a vacuum glass manufactured by a conventional method.

FIG. 4 is a graph showing the change of the vacuum glass performance parameter (U value) with time during the use of the vacuum glass manufactured by the method of the present invention.

FIG. 5 is a graph showing the change in the degree of vacuum when the vacuum glass chamber is evacuated at a temperature of 280 ℃ to 300 ℃ in the heating furnace.

FIG. 6 is a graph showing the change in the degree of vacuum when the vacuum glass chamber is evacuated at a temperature of 240 ℃ to 260 ℃ in the heating furnace.

FIG. 7 is a graph showing the change in the degree of vacuum when the vacuum glass chamber is evacuated at a temperature of 200 ℃ to 220 ℃ in the heating furnace.

Reference numbers and corresponding part names in the drawings:

1-getter, 2-planar structure, 3-gap, 4-glass substrate, 5-glass solder, 6-support, 7-pumping hole, 8-sealing piece and 9-protective cap.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples and accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not meant to limit the present invention.

Example 1

Referring to fig. 1, a getter packaging structure built in vacuum glass comprises a vacuum glass member, a sealing sheet and a getter; the vacuum glass component comprises two glass substrates, a support is arranged between the two glass substrates, glass solders are arranged at the peripheral edges of the two glass substrates, an air suction opening is formed in one of the two glass substrates, the getter is placed in the air suction opening, and a sealing sheet is placed on the outer side of the air suction opening; the getter is covered by a covering structure, as shown in fig. 2, the covering structure is formed by folding an aluminum foil, the getter is placed in the middle of the aluminum foil, the aluminum foil is folded and wrapped upwards along the edge of the getter until the surface of the getter is covered by the aluminum foil, the folding part of the aluminum foil has an overlapping area, a gap exists in the overlapping area, and gas in the vacuum glass cavity is in contact with the surface of the getter through the gap.

In the process of manufacturing the vacuum glass, the activation process of the getter is combined with the vacuumizing and exhausting process of the vacuum glass, and the getter is activated while the vacuum glass exhausts; the non-evaporable getter is a cylindrical solid structure, is a zirconium-vanadium-iron getter, has the activation temperature of 280-300 ℃, the activation time of 25-30 min, and the standard air suction amount of 17PaL/mg when the non-evaporable getter leaves a factory.

During the process of manufacturing the vacuum glass, the vacuum glass component with the getter is placed in a heating furnace, the heating furnace is heated to 340 ℃ to 400 ℃, the periphery of the vacuum glass component is subjected to sealing welding to form a vacuum glass cavity, after the welding is finished, the heating furnace is cooled to maintain 280 ℃ to 300 ℃, the vacuum glass cavity after the sealing welding is vacuumized from an air exhaust port, the vacuum degree is rapidly reduced, when the vacuumizing time is 25min to 30min, the vacuum degree in the vacuum glass cavity reaches 0.1Pa to 0.001Pa, at the moment, the getter is activated, after the getter is activated, the vacuum glass cavity is kept vacuumized, the sealing sheet is welded on the air exhaust port, a protective cap is arranged on the outer side of the sealing sheet, and the sealing sheet is further protected; the temperature required when the vacuum glass cavity is vacuumized is consistent with the activation of the getter, so that the getter is activated while vacuumizing.

When the getter is activated, gas molecules adsorbed on the surface of the getter are released into the vacuum layer and are pumped away by the vacuumizing and exhausting equipment, so that the vacuum degree of the vacuum glass is improved to a certain extent, the unit suction capacity of the getter is not influenced and reduced, and the getter can better play a role in the subsequent use of the vacuum glass.

When the vacuum is pumped, the change of the vacuum degree in the vacuum glass cavity is shown in fig. 5, the unit air suction amount of the adopted non-evaporable getter measured after the vacuum pumping is finished is 16.9PaL/mg, the error from the standard air suction amount is 0.59%, the getter can completely and normally work, and the getter is successfully activated.

FIG. 3 is a graph showing the change of a vacuum glass performance parameter (U value) with time during the use of a vacuum glass manufactured by a conventional method.

FIG. 4 is a graph showing the change of the vacuum glass performance parameter (U value) with time during the use of the vacuum glass manufactured by the method of the present invention.

Comparing fig. 3 and fig. 4, it can be clearly observed that the performance parameter (U value) of the vacuum glass manufactured by the method of the present invention is the same as that of fig. 3, and in the subsequent use, the performance parameter (U value) of the vacuum glass of fig. 3 and fig. 4 is changed consistently, although the present invention simplifies the production process of the vacuum glass, the performance of the vacuum glass is not changed.

In the embodiment, the activation process of the getter is combined with the vacuumizing and exhausting process of the vacuum glass, so that the production process of the vacuum glass is simplified, and the production cost is reduced.

Example 2

The difference between the embodiment and the embodiment 1 is that the non-evaporable getter is adopted, the activation temperature is 240-260 ℃, and the activation time is 60-80 min; the standard gas absorption amount of the non-evaporable getter at the time of shipment from the factory was 17 PaL/mg.

Forming a vacuum glass cavity after the periphery of the vacuum glass component is sealed and welded, reducing the temperature of the heating furnace, maintaining the temperature to be 240-260 ℃, starting to vacuumize the vacuum glass cavity from the air suction port, rapidly reducing the vacuum degree in the vacuum glass cavity when the vacuum time reaches 25-30 min, ensuring that the vacuum degree in the vacuum glass cavity reaches 0.1-0.001 Pa when the getter is not fully activated, continuously keeping the vacuum, continuously activating the getter, releasing gas molecules adsorbed on the surface of the getter into the vacuum glass cavity, pumping away the getter by a vacuum pumping device, completing the activation of the getter when the total vacuum time is 60-80 min, ensuring that the vacuum degree in the vacuum glass changes as shown in figure 6, and ensuring that the unit volume of the adopted non-evaporable getter after the vacuum pumping is finished is 16.8PaL/mg and the error from the standard suction volume is 1.2%, the getter can work normally and the activation of the getter is successful.

Example 3

The difference between the embodiment and the embodiment 1 is that the non-evaporable getter is adopted, the activation temperature is 200-220 ℃, and the activation time is 90-110 min; the standard gas absorption amount of the non-evaporable getter at the time of shipment from the factory was 17 PaL/mg.

Forming a vacuum glass cavity after the periphery of the vacuum glass component is sealed and welded, reducing the temperature of the heating furnace, maintaining the temperature of the heating furnace to be 200-220 ℃, starting to vacuumize the vacuum glass cavity from the air suction port, rapidly reducing the vacuum degree in the vacuum glass cavity when the vacuum time reaches 25-30 min, ensuring that the vacuum degree in the vacuum glass cavity reaches 0.1-0.001 Pa when the getter is not fully activated, continuously keeping the vacuum, continuously activating the getter, releasing gas molecules adsorbed on the surface of the getter into the vacuum glass cavity, pumping away the getter by a vacuum pumping device, completing the activation of the getter when the total vacuum time is 90-110 min, ensuring that the vacuum degree in the vacuum glass changes as shown in figure 7, and ensuring that the unit volume of the adopted non-evaporable getter after the vacuum pumping is completed is 16.9PaL/mg and the error of the standard suction volume is 0.59%, the getter can work normally and the activation of the getter is successful.

The performance coefficient of the vacuum glass manufactured by the method is the same as that of the vacuum glass manufactured by the prior art, and the performance coefficient of the vacuum glass is basically unchanged in the subsequent use process; the invention reduces the process flow for manufacturing the vacuum glass, and reduces the equipment used in the manufacturing process of the vacuum glass, such as equipment for activating the getter, vacuum brazing equipment used for manufacturing the getter tight encapsulation structure, and equipment for unsealing the getter tight encapsulation structure, thereby obviously simplifying the production flow, improving the production efficiency and reducing the production cost.

The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.