A production process of vacuum glass

Abstract

The present invention discloses a production process of vacuum glass, which comprises the following steps: 3 ~10 ﹣1 The assembled glass is hermetically sealed under an environment of Pa; the production process of the present invention can be sealed under low vacuum or medium vacuum, which can effectively reduce the requirements on equipment performance in the production process of vacuum glass, reduce the investment in vacuum glass production equipment, reduce the time of vacuuming in the production process, improve production efficiency, and reduce the production cost of vacuum glass.

Description

Technical Field

[0001] The invention relates to the technical field of vacuum glass preparation, and in particular to a production process of vacuum glass. Background Art

[0002] Vacuum Insulation Glass (VIG) is mainly composed of glass, support, getter and sealing material. Vacuum glass is a new energy-saving and environmentally friendly product with excellent light transmittance and high-efficiency heat and sound insulation performance. Vacuum glass is developed based on the principle of thermos bottle. The structure of vacuum glass is similar to that of hollow glass, but the difference is that the gas in the cavity of vacuum glass is very thin, and the internal air pressure P≤10 -1 Pa. In this vacuum environment, the heat conduction of gas molecules in the vacuum glass is very small, thus achieving efficient energy-saving performance. The heat transfer coefficient U is generally ≤0.7W·m -2 ·K -1 It is one of the most advanced and efficient thermal insulation materials in the world. It can be seen that the high vacuum environment (P≤10 -1 The acquisition and maintenance of 2.04 Pa) is the guarantee for the efficient thermal insulation and sound insulation performance of vacuum glass.

[0003] At present, the production process of vacuum glass can be roughly divided into two types: one-step method: prepare glass; place support, getter and sealing material; put two layers of glass together and place them in a vacuum chamber; draw high vacuum (P ≤10 -1 The vacuum degree of the vacuum process chamber is 10 -2 ~10 -5 Pa, the vacuum glass lamination process in the invention patent with application number CN202111536570 requires -3 ~7×10 -5 The two-step method is as follows: prepare the glass; place the support, getter and sealing material; seal the two layers of glass together; and evacuate the vacuum glass to a high vacuum (P≤10 -1 Pa); seal the vacuum hole; activate the getter to obtain vacuum glass. For example, in the vacuum glass production equipment of patent CN103570229A, high vacuum equipment including molecular pumps is used to convert vacuum glass into high vacuum (P≤10 -1 Pa) environment for airtight sealing.

[0004] In both of the above vacuum glass production processes, the vacuum glass needs to be evacuated to a high vacuum (P≤10 -1Pa) treatment requires high vacuum equipment including oil diffusion pumps, which requires large investment in production equipment and high production costs. In addition, the sealing of sealing materials under high vacuum in the one-step method is prone to bubbling of the sealing materials, resulting in a mismatch between the thermal expansion coefficient of the sealing materials and the glass, thereby causing airtight sealing defects. The two-step method of sealing first and then evacuating can avoid the problem of bubbling of the sealing materials, but the reserved evacuation port diameter is usually 0.2 to 2 mm. The vacuum degree of the vacuum glass is achieved by evacuating the glass tube, or placing the vacuum glass in a vacuum environment for slow exhaust, and finally sealing the evacuation port. The process has a low pumping speed, and the vacuum inside the vacuum glass reaches a high vacuum level (≤10 -1 Pa), which requires several hours of pumping time, resulting in low production efficiency and serious energy consumption, and high product costs.

[0005] In summary, in view of the problems of high investment, low production efficiency, low yield rate and high product cost of existing vacuum glass production equipment, a low vacuum (10 3 ~10 2 Pa) or medium vacuum (10 2 ~10 -1 The production process of preparing vacuum glass at 400 Pa has certain application significance. Summary of the invention

[0006] The purpose of the present invention is to provide a production process for vacuum glass, which can be sealed under low vacuum or medium vacuum, can effectively reduce the requirements on equipment performance in the production process of vacuum glass, reduce the investment in vacuum glass production equipment, reduce the time of vacuuming in the production process, improve production efficiency, and reduce the production cost of vacuum glass.

[0007] In order to achieve the above-mentioned purpose of the present invention, the following technical solutions are particularly adopted:

[0008] A first aspect of the present invention provides a production process for vacuum glass, the production process comprising the following steps:

[0009] In 10 3 ~10 ﹣1 Pa environment to hermetically seal the joined glass sheets.

[0010] Preferably, the production process comprises the following steps:

[0011] (a) preparing glass;

[0012] (b) placing a support, a getter and a sealing material on the glass surface;

[0013] (c) In 10 3 ~10 ﹣1 Pa environment for glass lamination and hermetic sealing;

[0014] (d) activating the getter to obtain the vacuum glass.

[0015] Preferably, the production process comprises the following steps:

[0016] (a) preparing glass;

[0017] (b) placing a support, a getter and a sealing material on the glass surface;

[0018] (c) Laminating the glass;

[0019] (d) Seal the assembled glass and reserve a vacuum hole. Then, evacuate the glass to 10 3 ~10 ﹣1 Pa after sealing the exhaust hole;

[0020] (e) activating the getter to obtain the vacuum glass.

[0021] Preferably, the getter is the vacuum getter in patent application number 202110368506.8.

[0022] Preferably, the sealing material is at least one of glass powder, alloy material, photosensitive colloid material and resin material.

[0023] Preferably, the airtight sealing method is heating sealing, metal brazing sealing or light sealing.

[0024] Preferably, the sealing method is heating sealing, metal brazing sealing or light sealing.

[0025] Preferably, the 10 3～10﹣1 The Pa vacuum environment is obtained by evacuating the air using a rotary vane vacuum pump, a sliding valve vacuum pump, a Roots vacuum pump, a dry vacuum pump, a water ring vacuum pump or a reciprocating vacuum pump.

[0026] Preferably, the activation of the getter is performed by using a laser to perform a hole-piercing process on the getter.

[0027] Compared with the prior art, the beneficial effects of the present invention include at least:

[0028] The production process of the present invention can perform sealing under low vacuum or medium vacuum, which can effectively reduce the requirements on equipment performance in the vacuum glass production process, reduce the investment in vacuum glass production equipment, reduce the time of vacuuming in the production process, improve production efficiency, and reduce the production cost of vacuum glass.

[0029] In the production process of the present invention, the getter can absorb the gas in the vacuum glass after being activated, so that the vacuum glass can achieve the purpose of high vacuum, and the prepared vacuum glass has excellent performance. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] In order to more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the following is a brief introduction to the drawings required for the specific embodiments or the description of the prior art. In all the drawings, similar elements or parts are generally identified by similar reference numerals. In the drawings, the elements or parts are not necessarily drawn according to the actual scale.

[0031] Figure 1 The aging comparison experimental data of the vacuum glass made in Examples 1 and 2 of the present invention and Comparative Example 1 are shown. DETAILED DESCRIPTION

[0032] The following embodiments of the technical solution of the present invention are described in detail in conjunction with the embodiments. The following embodiments are only used to more clearly illustrate the technical solution of the present invention, and are therefore only used as examples, and cannot be used to limit the protection scope of the present invention.

[0033] It should be noted that, unless otherwise specified, the technical terms or scientific terms used in this application should have the common meanings understood by those skilled in the art to which the invention belongs.

[0034] The raw materials used in the following examples are as follows:

[0035] Getter: The vacuum getter is prepared according to Example 1 in application number 202110368506.8.

[0036] Example 1

[0037] This embodiment is a production process of vacuum glass, which includes:

[0038] (a) Prepare glass with a size of 300mm*240mm;

[0039] (b) placing a support, a getter and a sealing material on the glass surface;

[0040] (c) putting two layers of glass together, placing them in a vacuum chamber and using a rotary vane vacuum pump to draw a vacuum (2 Pa) in the vacuum chamber, and then heating the sealing material to achieve hermetic sealing;

[0041] (d) Activating the getter by laser drilling to obtain the above-mentioned vacuum glass.

[0042] The vacuum glass is coded as VIG-1 and placed in a heat transfer coefficient test bench for thermal insulation performance testing. The initial value of the heat transfer coefficient of the vacuum glass is 0.623 W·m-2 ·K -1 .

[0043] Afterwards, the vacuum glass was subjected to an accelerated aging test. The aging conditions were as follows: the sample was aged in a constant temperature and humidity chamber at a temperature of 90°C, a humidity of 80RH, and an ultraviolet radiation intensity of 100μW / cm 2 The test results are shown in Table 1. Figure 1 Table 1 is the aging comparison experimental data of the vacuum glass made in Examples 1, 2, 3 and Comparative Example 1 of the present application. Figure 1 This is a comparison chart of the thermal conductivity U of the vacuum glasses made in Examples 1, 2, 3 of the present application and Comparative Example 1 after accelerated aging tests.

[0044] Example 2

[0045] This embodiment is a production process of vacuum glass, which includes:

[0046] (a) Prepare glass with a size of 400mm*300mm;

[0047] (b) placing a support, a getter and a sealing material on the glass surface;

[0048] (c) Laminating two layers of glass;

[0049] (d) heating the sealing material to hermetically seal the assembled glass and leaving a vacuum hole, then using a slide valve vacuum pump to pump a vacuum (1 Pa) through the reserved vacuum hole and then sealing the vacuum hole;

[0050] (e) Activating the getter by laser drilling to obtain the above-mentioned vacuum glass.

[0051] The vacuum glass is codenamed VIG-2 and placed in a heat transfer coefficient test bench for thermal insulation performance testing. The initial value of the heat transfer coefficient of the vacuum glass is 0.647 W·m -2 ·K -1 .

[0052] The vacuum glass was subjected to an aging test. The aging method is shown in Example 1. The test results are shown in Tables 1 and 2. Figure 1 .

[0053] Example 3

[0054] This embodiment is a production process of vacuum glass, which includes:

[0055] (a) Prepare glass with a size of 300mm*300mm;

[0056] (b) placing a support, a getter and a sealing material on the glass surface;

[0057] (c) Laying the two layers of glass together, placing them in a vacuum chamber, and using a Roots vacuum pump-water ring pump two-stage unit to evacuate a low vacuum (300 Pa) in the vacuum chamber, and then heating the sealing material to achieve hermetic sealing;

[0058] (d) Activating the getter by laser drilling to obtain the above-mentioned vacuum glass.

[0059] The vacuum glass is codenamed VIG-3 and placed in a heat transfer coefficient test bench for thermal insulation performance testing. The initial value of the heat transfer coefficient of the vacuum glass is 0.619 W·m -2 K-1.

[0060] The vacuum glass was subjected to an aging test. The aging method is shown in Example 1. The test results are shown in Tables 1 and 2. Figure 1 .

[0061] Comparative Example 1

[0062] This comparative example is a production process of vacuum glass, which includes:

[0063] (a) Prepare glass with a size of 300mm*300mm;

[0064] (b) Placing a support, a Zr alloy getter (from Italy's CESI) and a sealing material on the glass surface;

[0065] (c) Put the two layers of glass together, place them in the vacuum chamber and use the rotary vane vacuum pump-oil diffusion pump vacuum unit to draw a high vacuum of 3*10 -3 Pa, then, the sealing material is heated to achieve airtight sealing;

[0066] (d) The Zr alloy getter is subjected to a heating activation treatment to obtain the above-mentioned vacuum glass.

[0067] The code of the vacuum glass is set as the standard sample (corresponding to the standard value), and it is placed in the heat transfer coefficient test bench for thermal insulation performance testing. The initial value of the heat transfer coefficient of the vacuum glass is 0.635 W·m -2 K-1.

[0068] The vacuum glass was subjected to an aging test. The aging test method is shown in Example 1. The test results are shown in Tables 1 and 2. Figure 1 .

[0069] Table 1 Aging comparison experimental data of vacuum glass made in Examples 1, 2, 3 and Comparative Example 1

[0070]

[0071] From Table 1 and Figure 1 It can be seen that:

[0072] Compared with the standard sample of comparative example 1, the initial heat transfer coefficients of the vacuum glasses of Examples VIG-1, VIG-2, and VIG-3 are comparable to those of comparative example 1, indicating that the low vacuum (10 3 ~10 2 Pa) or medium vacuum (10 2 ~10 -1 The production process of preparing vacuum glass under high vacuum (≤10 Pa) can produce vacuum glass with the same -1 Pa) vacuum glass with comparable process performance, and after the accelerated aging test, the increase in heat transfer coefficient is small; indicating that the thermal insulation performance of the vacuum glass in the embodiment of the present application is better.

[0073] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein by equivalents. These modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present invention, and they should all be included in the scope of the claims and specification of the present invention.

Claims

1. A production process of vacuum glass, characterized in that: The production process comprises the following steps: (a) preparing glass; (b) placing a support, a getter and a sealing material on the glass surface; (c) Glass lamination and airtight sealing under 300Pa environment; (d) activating the getter to obtain the vacuum glass; The getter is a room temperature vacuum getter, which comprises an external airtight tube shell and internal getter powder; Ultrafine silica is used as internal getter powder; Weigh 2 g of silicon dioxide powder with a particle size of 2-5 microns and put it into a cylindrical copper alloy shell; wherein the copper alloy shell has a diameter of 10 mm and a height of 75 mm; The opening of the copper alloy tube shell is extruded and closed, and then placed in an argon atmosphere furnace for heating at a rate of 30°C / min to 370°C for insulation activation for 2 hours. The opening of the copper alloy tube shell is then heated and sealed in the atmosphere furnace at a sealing temperature of 1020°C for 1 hour, and then cooled to room temperature to obtain the room temperature vacuum getter.

2. The production process according to claim 1, characterized in that: The sealing material is at least one of glass powder, alloy material, photosensitive colloid material and resin material.

3. The production process according to claim 1, characterized in that: The hermetic sealing method is heating sealing, metal brazing sealing or light sealing.

4. The production process according to claim 1, characterized in that: The 300Pa vacuum environment is obtained by evacuating with a rotary vane vacuum pump, a sliding valve vacuum pump, a Roots vacuum pump, a dry vacuum pump, a water ring vacuum pump or a reciprocating vacuum pump.

5. The production process according to claim 1, characterized in that: The activation of the getter is to perform a hole-piercing process on the getter using a laser.

6. A production process of vacuum glass, characterized in that: The production process comprises the following steps: (a) preparing glass; (b) placing a support, a getter and a sealing material on the glass surface; (c) Laminating the glass; (d) The assembled glass is sealed and a vacuum hole is reserved, and then the vacuum hole is evacuated to 300 Pa and then the vacuum hole is sealed; (e) activating the getter to obtain the vacuum glass; The getter is a room temperature vacuum getter, which comprises an external airtight tube shell and internal getter powder; Ultrafine silica is used as internal getter powder; Weigh 2 g of silicon dioxide powder with a particle size of 2-5 microns and put it into a cylindrical copper alloy shell; wherein the copper alloy shell has a diameter of 10 mm and a height of 75 mm; The opening of the copper alloy tube shell is extruded and closed, and then placed in an argon atmosphere furnace for heating at a rate of 30°C / min to 370°C for insulation activation for 2 hours. The opening of the copper alloy tube shell is then heated and sealed in the atmosphere furnace at a sealing temperature of 1020°C for 1 hour, and then cooled to room temperature to obtain the room temperature vacuum getter.

7. The production process according to claim 6, characterized in that: The sealing material is at least one of glass powder, alloy material, photosensitive colloid material and resin material.

8. The production process according to claim 6, characterized in that: The sealing method is heating sealing, metal brazing sealing or light sealing.

9. The production process according to claim 6, characterized in that: The 300Pa vacuum environment is obtained by evacuating with a rotary vane vacuum pump, a sliding valve vacuum pump, a Roots vacuum pump, a dry vacuum pump, a water ring vacuum pump or a reciprocating vacuum pump.

10. The production process according to claim 6, characterized in that: The activation of the getter is to perform a hole-piercing process on the getter using a laser.

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