阅读说明：本技术 一种全钢化态真空玻璃及其制备方法 (All-tempered vacuum glass and preparation method thereof ) 是由 蔡邦辉 刘勇江 龚有来 王国焦 鲜华 于 2021-09-27 设计创作，主要内容包括：本发明涉及真空玻璃领域,公开了一种全钢化态真空玻璃,包括两块玻璃板,两块玻璃板之间设置有封接结构,玻璃板与封接结构之间围成真空腔,玻璃板的内侧面设置有盲孔,全钢化态真空玻璃的钢化应力值≥90MPa。全钢化态真空玻璃的制备方法,包括S1,玻璃板预处理：盲孔加工、金属浆料的涂覆与固化；S2,物理钢化：采用整体加热方式对玻璃板及金属浆料进行烧结；S3,支撑物及焊料的布放；S4,在盲孔内放置吸气剂；S5,合片及封接：将两块玻璃板送入真空腔合片后进行等离子轰击处理；S6,二次封接后激活吸气剂即得全钢化态真空玻璃。本发明解决了真空玻璃预留抽气孔或封接后再在封接区域进行制孔抽真空导致的封接强度下降及存在漏气隐患的问题。(The invention relates to the field of vacuum glass, and discloses all-tempered vacuum glass which comprises two glass plates, wherein a sealing structure is arranged between the two glass plates, a vacuum cavity is enclosed between the glass plates and the sealing structure, a blind hole is formed in the inner side surface of each glass plate, and the tempering stress value of the all-tempered vacuum glass is more than or equal to 90 MPa. The preparation method of the fully tempered vacuum glass comprises the steps of S1, glass plate pretreatment: blind hole processing, coating and curing of metal slurry; s2, physical tempering: sintering the glass plate and the metal slurry in an integral heating mode; s3, laying the support and the solder; s4, placing getters in the blind holes; s5, sheet combination and sealing: conveying the two glass plates into a vacuum cavity for laminating and then carrying out plasma bombardment treatment; and S6, activating the getter after secondary sealing to obtain the fully tempered vacuum glass. The invention solves the problems of reduced sealing strength and hidden air leakage caused by reserving an air suction hole in vacuum glass or drilling and vacuumizing a sealing area after sealing.)

1. The utility model provides a full tempering attitude vacuum glass, includes two piece at least glass boards, and the glass board is the whole piece formula glass of sclausura, is provided with sealing structure between the at least glass board, encloses into the vacuum cavity between glass board and the sealing structure, its characterized in that: the inner side surface of the glass plate is provided with a blind hole, and the tempering stress value of the all-tempered vacuum glass is more than or equal to 90 MPa.

2. The all-tempered vacuum glass as claimed in claim 1, wherein: the sealing structure comprises a metallization layer and an outer sealing adhesive, wherein the outer sealing adhesive is arranged on one side, far away from the vacuum cavity, of the metallization layer.

3. The all-tempered vacuum glass as claimed in claim 2, wherein: the metallization layer is arranged in the edge area of the glass plate, and the distance between the outer edge of the metallization layer and the outer edge of the glass plate is 1.5-4 mm.

4. The all-tempered vacuum glass as claimed in claim 3, wherein: the metallization layer comprises metal paste arranged on the inner side surface of the glass plate and solder arranged between the two layers of metal paste.

5. The all-tempered vacuum glass as claimed in claim 4, wherein: the blind holes are arranged in the areas of 15-25mm of equal distance on the two side edges of the glass plate, the diameter of each blind hole is 8-16mm, and the depth of each blind hole is 20-33% of the thickness of the glass plate.

6. The all-tempered vacuum glass as claimed in claim 5, wherein: a plurality of support columns are arranged in the vacuum cavity.

7. The preparation method of the all-tempered vacuum glass is characterized by comprising the following steps of:

s1, glass plate pretreatment:

(1) processing blind holes, namely prefabricating the blind holes on one glass plate;

(2) coating and curing the metal slurry, coating and curing the metal slurry on the region to be sealed of the glass plate, wherein the metal slurry and the blind hole are positioned at the same side of the glass plate;

s2, physical tempering: sintering the glass plate and the metal slurry in an integral heating mode;

s3, laying of supports and solder: fixing a support on a glass plate with a prefabricated blind hole and distributing alloy solder, wherein the thickness of the alloy solder is greater than the height of the support;

s4, placing getters in the blind holes;

s5, sheet combination and sealing: conveying the two glass plates into a vacuum cavity for laminating, then carrying out plasma bombardment treatment, and then sealing the positions where the alloy welding materials are distributed;

s6, secondary sealing: and gluing the periphery of the alloy solder for secondary sealing, and activating the getter to obtain the fully tempered vacuum glass.

8. The method for preparing the fully tempered vacuum glass according to claim 7, wherein the method comprises the following steps: in S1, the curing method is infrared or hot air treatment, the treatment temperature is 120-200 ℃, and the treatment time is 5-10 min.

9. The method for preparing the fully tempered vacuum glass according to claim 8, wherein the method comprises the following steps: in S1, the metal paste comprises 65-80% of Ag, 2-8% of Si, 5-15% of synthetic resin and 15-25% of solvent, the coating width of the metal paste is 6-14mm, and the coating thickness of the metal paste is 0.010-0.046 mm.

10. The method for preparing the fully tempered vacuum glass according to claim 9, wherein the method comprises the following steps: in S2, the sintering temperature is 660-720 ℃, and the sintering time is 2-7 min.

11. The method for preparing the fully tempered vacuum glass according to claim 10, wherein the method comprises the following steps: in S3, the distance between the two sides of the alloy solder and the two sides of the metal paste is more than or equal to 0.5 mm.

12. The method for preparing the fully tempered vacuum glass according to claim 11, wherein the method comprises the following steps: in S3, the solder alloy is distributed in single or multiple parallel lines, and when multiple parallel lines are distributed, a gap is arranged between two adjacent solder alloys.

13. The method for preparing the fully tempered vacuum glass according to claim 12, wherein the method comprises the following steps: in S3, a plurality of supports are arranged, and the distance between every two adjacent supports is 30-80 mm.

14. The method for preparing the fully tempered vacuum glass as claimed in claim 13, wherein the method comprises the following steps: at S4, the vacuum degree of the vacuum chamber was 10^-2-10^-5Pa。

15. The method for preparing the fully tempered vacuum glass as claimed in claim 13, wherein the method comprises the following steps: in S5, a heating process is performed before sealing, wherein the heating process is infrared heating, induction heating, heat conduction heating or laser heating, and the heating temperature is 100 ℃ and 250 ℃.

Technical Field

The invention relates to the field of vacuum glass, in particular to all-tempered vacuum glass and a preparation method thereof.

Background

The vacuum glass is glass obtained by sealing the peripheries of two pieces of flat glass and vacuumizing the gap between the two pieces of flat glass. The vacuum glass is a novel glass deep-processing product, is also a transparent and energy-saving green building material, integrates the technical advantages of coated glass and hollow glass, and has excellent performances in heat preservation, heat insulation, dewing prevention, sound insulation, wind pressure resistance and the like.

At present, the processing process of vacuum glass is generally to coat a metal slurry layer on the periphery of two or more glass plates (toughened glass), then to sinter in a local heating mode, and to weld the sintered plates. After the glass plates are combined, a vacuum layer with the thickness of 0.3 mm-0.4 mm can be formed between the two glass plates, metal supports are arranged between the two glass plates in an array mode to offset atmospheric pressure, and an air suction opening is reserved in one of the two glass plates to facilitate air suction of the vacuum layer to form vacuum; or hole making and vacuum pumping are carried out in the sealing area. However, the processing process of the vacuum glass has the following problems: after the metal slurry is coated, a local sintering mode is adopted, so that the process of local stress change of the glass is increased, the probability of dark collapse and fracture of the glass caused by stress change is increased, and the yield of the manufacturing process is reduced; secondly, reserving an air suction hole in the vacuum glass or performing hole making and vacuum pumping on a sealing area after sealing, wherein secondary damage of the sealing strength (for example, the release of glass stress caused by external force) on the product structure can be caused, and the process loss of the product is increased by reprocessing; and thirdly, reserving an air exhaust hole in the vacuum glass or performing hole making and vacuum pumping on the sealing area after sealing to form natural hidden trouble of air leakage hole for protecting the vacuum degree in the vacuum glass cavity.

Disclosure of Invention

The invention aims to provide all-tempered vacuum glass and a preparation method thereof, and aims to solve the problems of reduced sealing strength and hidden air leakage caused by hole making and vacuumizing in a sealing area in order to eliminate gas residues after vacuum glass is sealed in the prior art.

In order to achieve the purpose, the invention adopts the following technical scheme: the full-tempered vacuum glass comprises at least two glass plates, wherein the glass plates are non-porous whole glass, a sealing structure is arranged between the at least two glass plates, a vacuum cavity is enclosed between the glass plates and the sealing structure, blind holes are formed in the inner side faces of the glass plates, and the tempering stress value of the full-tempered vacuum glass is larger than or equal to 90 MPa.

The technical scheme also provides a preparation method of the all-tempered vacuum glass, which comprises the following steps:

s1, glass plate pretreatment:

(1) processing blind holes, namely prefabricating the blind holes on one glass plate;

(2) coating and curing the metal slurry, coating and curing the metal slurry on the region to be sealed of the glass plate, wherein the metal slurry and the blind hole are positioned at the same side of the glass plate;

s2, physical tempering: sintering the glass plate and the metal slurry in an integral heating mode;

s3, laying of supports and solder: fixing a support on a glass plate with a prefabricated blind hole and distributing alloy solder, wherein the thickness of the alloy solder is greater than the height of the support;

s4, placing getters in the blind holes;

s5, sheet combination and sealing: conveying the two glass plates into a vacuum cavity for laminating, then carrying out plasma bombardment treatment, and then sealing the positions where the alloy welding materials are distributed;

s6, secondary sealing: and gluing the periphery of the alloy solder for secondary sealing, and activating the getter to obtain the fully tempered vacuum glass.

The principle and the advantages of the scheme are as follows: according to the all-tempered vacuum glass in the technical scheme, the blind hole is prefabricated on the glass plate, the getter is placed in the blind hole, the getter is activated after sealing, residual oxyhydrogen gas in the vacuum cavity can be eliminated, a gas suction hole does not need to be reserved, or hole making and vacuumizing are carried out in a sealing area after sealing, the integrity of the glass plate is ensured, and the sealing strength can be ensured; on the other hand, the hidden danger problem of air leakage of the air exhaust hole is avoided.

In the preparation process of the full tempered glass in the technical scheme, the non-perforated complete glass plate is processed, and before solder is distributed, the physical tempering of the glass plate is realized in an integral heating mode, so that the stress change of the glass plate caused by local heating can be avoided, and the sintering of metal slurry and the glass plate surface can be realized. After the sheet combination, plasma is used for cleaning and degassing, impurities such as oil stains on the surface of the glass and adsorbed multilayer gas molecules are removed, the sealing effect in the later period is ensured, and the amount of residual gas in the vacuum cavity can be reduced. When in sealing, firstly, the metal slurry and the alloy solder are used cooperatively, so that compared with the method of directly utilizing the alloy solder, the usage amount is reduced by about 60 percent, and the solder cost is further reduced by 60 percent; in addition, by the cooperative sealing mode of the two layers of metal slurry and the alloy solder, the sealing temperature is reduced during sealing, the change degree of stress in the annealing process of the glass is reduced due to the reduction of the sealing temperature, and the bad phenomena of film tearing of a metal layer and self-breaking of a glass plate are reduced; moreover, after the welding material is sealed, secondary sealing is realized by utilizing peripheral gluing, double protection of vacuum degree is realized, sealing strength can be enhanced, the service life of the vacuum glass is prolonged, the peripheral gluing of the vacuum glass also plays a role in flexible protection, the strength of resisting external impact is improved, the extensibility of stress release of the glass in the temperature change process is reduced, and the spontaneous explosion risk of the vacuum glass is avoided. After sealing, only the getter in the blind hole needs to be activated, and the hidden danger problem of air leakage of the air suction hole is avoided.

Preferably, as an improvement, the sealing structure includes a metallization layer and an outer sealant, and the outer sealant is disposed on a side of the metallization layer away from the vacuum cavity.

In the technical scheme, secondary sealing of the vacuum glass is realized by using the external sealing adhesive, so that double protection of vacuum degree is realized, the sealing strength can be enhanced, and the service life of the vacuum glass is prolonged; in addition, the periphery of the vacuum glass is coated with glue to play a role in flexible protection, so that the strength of resisting external impact is improved, the extensibility of the glass for releasing stress in the temperature change process is reduced, and the spontaneous explosion risk of the vacuum glass is avoided.

Preferably, as a refinement, the metallization layer is arranged in the edge region of the glass plate, and the distance between the outer edge of the metallization layer and the outer edge of the glass plate is 1.5-4 mm.

In the technical scheme, different from the prior art that the metallization layer is arranged in the peripheral adjacent marginal area of the glass plate, the distance of 1.5-4mm is reserved between the metallization layer and the outer edge of the glass plate, and after sintering and laminating, the metallization layer cannot overflow to the outside of the glass plate, so that the vacuum glass can be ensured to be neat and attractive in appearance; and deep processing and grinding are not needed in the later stage, the surface layer of the glass is prevented from being damaged, and the problems of edge cracking, opening collapse, demoulding and the like of the glass plate caused by the change of the stress of the glass during heating and temperature rising in the later stage are avoided.

Preferably, as a refinement, the metallization layer comprises a metal paste arranged on the inner side of the glass plate and a solder arranged between the two layers of metal paste.

In the technical scheme, the metallization layer is set to be a mode of combining two layers of metal slurry and the solder, so that compared with the mode of directly utilizing the solder, the usage amount is reduced by nearly 60%, and the cost of the solder is further reduced by 60%; in addition, by the cooperative sealing mode of the two layers of metal slurry and the solder, the sealing temperature is reduced during sealing, the change degree of stress in the annealing process of the glass is reduced due to the reduction of the sealing temperature, and the bad phenomena of film tearing of the metal layer and self-breaking of the glass plate are reduced.

Preferably, as an improvement, the blind holes are arranged in the areas with the equal distance between two sides of the glass plate within the range of 15-25mm, the diameter of the blind holes is 8-16mm, and the depth of the blind holes is 20-33% of the thickness of the glass plate.

In the technical scheme, through the optimization of the setting position of the blind hole, the hole diameter and the depth, the influence of the blind hole on the stress of the tempered glass plate can be reduced as much as possible, the processing of the blind hole can be ensured to basically avoid the influence on the sealing strength and the impact strength of the glass, and the structural design is reasonable.

Preferably, as a modification, a plurality of support columns are provided in the vacuum chamber.

Among this technical scheme, the support column in the vacuum chamber plays the fixed effect of support to the glass board, can cushion dispersion part vacuum pressure, guarantees vacuum glass's two glass boards's stability.

Preferably, as an improvement, in S1, the curing method is infrared or hot air treatment, the treatment temperature is 120-200 ℃, and the treatment time is 5-10 min.

In the technical scheme, when the metal slurry is cured, the mode can be infrared heating or hot air heating, the metal slurry can be flexibly selected in practical use, the treatment temperature and the treatment time are the optimal curing conditions, the temperature is relatively low, and the glass performance is basically not adversely affected while the effective curing is ensured.

Preferably, as a modification, in S1, the metal paste includes Ag 65-80%, Si 2-8%, synthetic resin 5-15%, and solvent 15-25%, the coating width of the metal paste is 6-14mm, and the coating thickness of the metal paste is 0.010-0.046 mm.

Among this technical scheme, resin in the metal slurry can be in the same place Ag and the better bonding of Si, improves adnexed ropping agent, and the solvent can avoid appearing the sediment with the even suspension of components such as Ag, Si and resin, just does benefit to the defoaming, does benefit to the homogeneity of coating. The coating width and the coating thickness of the metal slurry are in the optimal range verified by tests, and the sealing effect can be ensured.

Preferably, as an improvement, in S2, the sintering temperature is 660-720 ℃, and the sintering time is 2-7 min.

In the technical scheme, the sintering temperature has great influence on the adhesive force of the metal slurry coated on the glass plate, and the adhesive force is reduced when the sintering temperature is too high or too low, so that poor sealing is caused. In addition, the sintering temperature range is an optimum temperature range in consideration of the annealing point of the glass itself and the adhesion of the metal paste.

Preferably, as a modification, in S3, the distance between the two sides of the alloy solder and the two sides of the metal paste is greater than or equal to 0.5 mm.

In the technical scheme, at least 0.5mm of allowance is arranged between the side edge of the alloy solder and the side edge of the metal slurry, so that the solder can be prevented from overflowing to form a solid metal pedicle knot on the surface of the glass plate.

Preferably, as an improvement, in S3, the solder alloy is laid in a single strip or in parallel with multiple strips, and when multiple strips are laid in parallel, a gap is formed between two adjacent solder alloys.

In the technical scheme, in the actual processing process, if the size of the vacuum glass is smaller, a single alloy solder can be adopted for laying, and the vacuum degree in the vacuum cavity can be effectively protected after sealing and sealing; if the size of the vacuum glass is larger, two or more vacuum glass strips can be arranged in parallel, and then two or more sealing belts are formed after sealing, so that multiple sealing is realized, and the sealing and sealing effect is ensured.

Preferably, as a modification, in S3, the supports are provided in plurality, and the spacing between adjacent supports is 30-80 mm.

In the technical scheme, the supports are arranged to be a plurality of, so that the stress can be dispersed, the stress of each part of the glass plate is uniform, and the distance between the supports is more suitable.

Preferably, as a modification, in S4, the vacuum chamber has a degree of vacuum of 10^-2-10^-5Pa。

In the technical scheme, when the vacuum degree in the vacuum cavity is lower than a standard value, an invalid vacuum state can be formed, and the heat insulation effect is influenced; the vacuum degree is higher than the standard value, so that the glass is increased under the external pressure and is easy to break.

Preferably, as an improvement, in S5, before sealing, heating treatment is performed, wherein the heating manner is infrared heating, induction heating, heat conduction heating or laser heating, and the heating temperature is 100-250 ℃.

In the technical scheme, the whole glass is heated before being sealed, so that a better degassing effect can be obtained before sealing, and the heating mode can be flexibly selected according to actual needs.

Drawings

FIG. 1 is a longitudinal sectional view of a fully tempered vacuum glass according to an embodiment of the present invention.

Fig. 2 is an enlarged view at a1 in fig. 1.

FIG. 3 is a top view of a glass plate and a sealing structure.

Detailed Description

The following is further detailed by way of specific embodiments:

reference numerals in the drawings of the specification include: the glass plate comprises a glass plate 1, a vacuum cavity 2, blind holes 3, support pillars 4, a metallization layer 5, a metal slurry layer 51, alloy solder 52 and external sealing glue 6.

Example one

In this embodiment, as shown in fig. 1-3, a fully tempered vacuum glass includes two glass plates 1, a sealing structure is disposed between the two glass plates 1, and a vacuum cavity 2 is enclosed between the glass plates 1 and the sealing structure.

The inner side surface of one glass plate 1 is provided with blind holes 3, the blind holes 3 are arranged in regions of two side edges of the glass plate 1 within the range of 15-25mm at equal intervals, the diameter of each blind hole 3 is 12mm, the depth of each blind hole 3 is 30% of the thickness of the glass plate 1, and getters (not shown in the figure) are arranged in the blind holes 3. A plurality of support columns 4 are arranged in the vacuum cavity 2, the distance between every two adjacent support columns 4 is 50mm, and two ends of each support column 4 are respectively abutted against the two glass plates 1.

The sealing structure is arranged in the edge area near the periphery of the two glass plates 1 and comprises a metallization layer 5 and outer sealing glue 6. Referring to fig. 2 and 3, the metallization layer 5 includes metal paste layers 51 respectively sintered and fixed on the inner side surfaces of the glass plate 1 and a flexible alloy solder 52 arranged between the two metal paste layers 51, the width of the metal paste layer 51 is 12mm, the thickness of the metal paste layer 51 is 0.03mm, and the distance between the outer edge of the metal paste layer 51 and the outer edge of the glass plate 1 is 2 mm. The outer sealing compound 6 is disposed outside the metallization layer 5, and the outer sealing compound 6 in this embodiment is a UV compound, and the UV compound is bonded between the two glass plates 1. The tempering stress value of the all-tempered vacuum glass of the technical scheme is more than or equal to 90 MPa.

A preparation method of all-tempered glass comprises the following steps:

s1, glass plate pretreatment: comprises prefabricating blind holes on a glass plate, coating and curing metal slurry, wherein the glass plate comprises a glass plate A and a glass plate B,

(1) processing blind holes, namely prefabricating circular blind holes on the glass plate B, wherein the blind holes are arranged in the range of being 20mm away from two straight edges of the plate surface of the glass plate B at equal distance, and the diameter of each blind hole12mm, and the depth of the blind hole is 30% of the thickness of the glass plate.

(2) Coating and curing the metal slurry, namely coating the metal slurry in peripheral areas around the glass plate A and the glass plate B, wherein the coating frequency of the metal slurry is 2 times, the coating width of the metal slurry is 12mm, the coating thickness of the metal slurry is 0.03mm, and the distance from the outer edge of the metal slurry to the outer edge of the glass plate is 2 mm; wherein the metal slurry of the glass plate B and the blind hole are arranged at the same side; the metal paste in this embodiment includes 65-80% of Ag, 2-8% of Si, 5-15% of synthetic resin, and 15-25% of a solvent.

After the metal slurry is coated, infrared heating is used for curing, wherein the heating temperature is 180 ℃, and the heating time is 5 min; the screen with 300 meshes is selected, and the positioning printing is carried out by using mechanical automation and manual operation.

S2, physical tempering: and sintering the glass plate and the metal slurry by adopting an integral heating mode, wherein the sintering temperature is 660 ℃, and the sintering time is 5 min.

S3, laying of supports and solder: fixing a support on the glass plate B and distributing alloy solder;

the vacuum chamber is internally provided with a plurality of supporting columns, the distance between every two adjacent supporting columns is 50mm, and two ends of each supporting column respectively abut against the glass plate A and the glass plate B.

And laying the alloy solder on the metal slurry coating area, wherein the distance between two side edges of the alloy solder and two side edges of the metal slurry is more than or equal to 0.5mm, so that the solder is prevented from overflowing to form a solid metal base knot on the surface of the glass plate. The alloy solder in the embodiment is flexible solder, in particular to banded or filiform tin or tin-based alloy; if the size of the vacuum glass is smaller, a single alloy solder can be adopted for laying, and the vacuum degree in the vacuum cavity can be effectively protected after sealing and sealing; if the size of the vacuum glass is larger, two or more pieces of vacuum glass can be arranged in parallel, and then two or more sealing belts are formed after sealing, so that multiple sealing is realized; the thickness of the alloy solder is larger than the height of the support.

S4, placing a getter in the blind hole, wherein the getter is a solid cylinder and has a diameter10mm and the thickness of the getter 1.0 mm.

S5, sheet combination and sealing: and (3) conveying the two glass plates into a vacuum cavity for orderly laminating, and performing plasma bombardment treatment on the upper surface of the lower glass and the lower surface of the upper glass in a vacuum environment. Then the obtained product is sent into a vacuum process chamber, and the heating is carried out to seal the positions where the alloy welding flux is distributed at the edges. The vacuum degree of the vacuum process cavity is 10^-2-10^-5Pa, the heating temperature is 150 ℃, and the heating mode is infrared heating. The whole glass plate is heated, so that a better degassing effect can be obtained before sealing.

S6, secondary sealing: and after S5 is finished, the glass flows out of the vacuum process cavity, and the glass is annealed and cooled after the glass flows out of the cavity. And then, coating the peripheral groove parts of the vacuum glass by using ultraviolet UV glue at the periphery of the alloy solder to realize secondary sealing, and activating a getter by using an ultraviolet light or heating mode to obtain the fully tempered vacuum glass.

Example two

The difference between the present embodiment and the first embodiment is: in this example, the coating and curing of the metal paste and the coating and curing of the solder paste were performed on the corresponding surfaces of the glass plates a/B, and two different component pastes were used. Thereby eliminating the process of laying solid solder strips on the alloy paste coated areas.

Coating metal slurry for 1 time in peripheral areas around the glass plate A and the glass plate B, then coating a layer of solder slurry in the coating area of the metal slurry, wherein the coating width of the solder slurry is 8mm, the coating area of the solder slurry has a glass edge of 3mm, and the coating thickness of the solder slurry is 0.5 mm. And after the solder paste is coated, carrying out infrared heating curing. The rest of the steps are the same as the first embodiment.

EXAMPLE III

The difference between the present embodiment and the first embodiment is: in this example, the sintering temperature was 670 ℃.

Example four

The difference between the present embodiment and the first embodiment is: in this example, the sintering temperature was 680 ℃.

EXAMPLE five

The difference between the present embodiment and the first embodiment is: in this example, the sintering temperature was 690 ℃.

EXAMPLE six

The difference between the present embodiment and the first embodiment is: in this example, the sintering temperature was 700 ℃.

EXAMPLE seven

The difference between the present embodiment and the first embodiment is: in this example, the sintering temperature was 710 ℃.

Example eight

The difference between the present embodiment and the first embodiment is: in this example, the sintering temperature was 720 ℃.

Comparative example 1

The comparative example differs from the first example in that: in this example, the sintering temperature was 640 ℃.

Comparative example No. two

The comparative example differs from the first example in that: in this example, the sintering temperature was 650 ℃.

Comparative example No. three

The comparative example differs from the first example in that: in this example, the sintering temperature was 730 ℃.

Comparative example No. four

The comparative example differs from the first example in that: in this example, the sintering temperature was 740 ℃.

The first experimental example: adhesion strength test of alloy slurry

The test method comprises the following steps: sintering of alloy slurry and glass surface on a 300X 5.0mm glass plate and physical tempering of the whole glass plate are carried out by using the sintering conditions of the examples 1-8 and the comparative examples 1-4.

The inspection method and the judgment standard are as follows:

(1) the test method comprises the following steps: marking small grids of 1mm multiplied by 1mm in a sintering test area of the glass and alloy slurry, pressing the grids with a 3M810 adhesive tape and quickly pulling the grids along the 45-degree direction, wherein the number of the grids is more than or equal to 40 in principle.

(2) And (4) checking the position: 4 edges were measured for each 1 piece and analyzed at 4 points per piece.

(3) And (3) judging standard: calculating the falling proportion of the sintering layer in the grid after the 3M810 adhesive tape is pulled up, wherein A: judging the product is qualified if the product is less than 3 percent; b: slight disqualification is judged at 3-5%; c: judging the serious disqualification at more than 5 percent; the detection results are shown in Table 1, and the yield and the sealing effect are better when the sintering temperature is 660-720 ℃.

TABLE 1

Experiment example two: vacuum glass stress variation test

(1) The test mode is as follows: taking the product as a sample, the method is carried out according to the method specified in GB/T18144, 2 parallel lines parallel to the long side are led at the distance of 100mm from the long side and intersect with the diagonal line at 4 points, and the 4 points and the geometric center point of the product are measuring points. The test comprises a coating layer sintering and physical tempering stage, a sheet-combination solder sealing and sealing stage and a finished product test stage, and the specific test method of each stage is as follows:

coating layer sintering and physical tempering: the method is characterized in that the sintering of the alloy slurry on the A/B surface of the glass plate and the glass surface and the physical tempering preparation of the whole glass plate are completed by utilizing the strengthening process of the glass plate and adopting integral heating. The temperature setting range is as follows: 660-720 ℃.

Sealing and sealing the bonding solder: and (3) delivering the mixture into a vacuum process cavity, heating the position where the solder is distributed at the edge to seal, and controlling the temperature to be within the range of 100 ℃ and 250 ℃.

And (3) a finished product testing stage: and after the sealing of the vacuum glass structure is finished, the glass flows out of the vacuum cavity, annealing and cooling are carried out after the glass flows out of the cavity by using a device with a temperature capable of being raised and lowered, and the temperature is controlled to be in a range of-40-80 ℃.

(2) And (4) testing standard: according to the second tempered glass requirement of the safety glass GB 15763.2-2005, the surface stress of the tempered glass should not be less than 90 MPa.

And (3) judging standard: the results were measured using a surface stress tester (JF-1E) and three replicates were run per treatment group and expressed as mean values. Description of the drawings: stress value 1: sintering and physically toughening the coating layer; stress value 2: sealing and sealing the sheet-combination welding flux; stress value 3: a finished product testing stage; the results are shown in Table 2, the temperature of the coating layer sintering and physical toughening stage is 660-720 ℃, the temperature of the sheet-combination solder sealing and sealing stage is 100-250 ℃, the temperature of the finished product testing stage is-40-80 ℃, and the stress value of the product is more than 90MPa of the standard requirement.

TABLE 2

The foregoing is merely an example of the present invention and common general knowledge in the art of designing and/or characterizing particular aspects and/or features is not described in any greater detail herein. It should be noted that, for those skilled in the art, without departing from the technical solution of the present invention, several variations and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.