Sealing glass film and its preparation method and application

Abstract

The invention discloses a sealing glass film and a preparation method and application thereof. The preparation method comprises the following steps: mixing polyvinyl butyral and ethanol and ball milling them to obtain a mixed slurry; pouring the mixed slurry into a tape casting machine; preparing a layer of PVB film on a PET release film tape; mixing glass powder, a dispersant and a solvent and ball milling them; the solvent is one or more of terpineol, diethylene glycol monobutyl ether and alcohol ester twelve; when D 50 =10μm-12μm, add a binder and a plasticizer, ball mill, vacuum degassing, obtain a casting slurry, cast the casting slurry on a PET release film with a PVB film, dry and demold, and obtain a sealing glass film. The preparation method of the invention has simple process and strong universality. The prepared sealing glass film can achieve high-strength sealing of ceramic parts, has good airtightness, and is easy to store.

Description

Technical Field

[0001] The invention belongs to the technical field of new materials and relates to a sealing glass film and a preparation method and application thereof. Background Art

[0002] Advanced ceramic materials have excellent properties such as high temperature resistance, wear resistance, corrosion resistance, high specific modulus and specific strength, and have been widely used in cutting-edge technology fields such as aerospace, new energy and semiconductors. However, with the continuous development of science and technology, higher and higher requirements are put forward for precision ceramic components, including the following characteristics: First, large size and complex shape, some parts have reached meter-level size; second, some ceramic parts need to design functional hollow closed-cell structures to integrate their structure and function; in addition, in order to reduce the impact on products such as wafers, silicon carbide ceramic parts may have fine and precise structures. Based on this, many structural parts with complex cavity structures, such as laser transmitter ceramic cavity shells and ceramic arms, often adopt "modular manufacturing", that is, the structural parts are split into two separate parts for processing, and then bonded into one with resin or sealing glass. Due to the poor heat resistance, corrosion resistance and mechanical properties of resin, sealing glass has become the mainstream choice for high-performance ceramic structural parts.

[0003] In the existing production process, a scraper is often used in conjunction with a screen printing process to apply sealing glass paste to the bonding area, and then it is bonded to other modules through the bonding area, fixed in an oven with a tooling, and then transferred to a sintering furnace for sintering after drying to melt the sealing glass. After cooling, the modules can be bonded. However, this process has the following problems:

[0004] (1) The screen printing process requires a customized template for each specific ceramic component, which increases costs and is inefficient. In addition, the long-term preservation of the sealing glass paste is also difficult.

[0005] (2) The slurry applied to the bonding area is often squeezed during the bonding process. On the one hand, the thickness of the sealing glass cannot be guaranteed. On the other hand, the shrinkage of the slurry during the drying process will cause uneven glue coating in the bonding area, ultimately resulting in low bonding strength or insufficient airtightness.

[0006] Based on this, it is necessary to develop new processes to solve the above technical problems. Summary of the invention

[0007] The technical problem to be solved by the present invention is to overcome the deficiencies of the prior art and to provide a sealing glass film which has simple process, strong universality, is easy to store, can achieve high-strength sealing of ceramic parts and good airtightness, and a preparation method and application thereof.

[0008] In order to solve the above technical problems, the present invention adopts the following technical solutions.

[0009] A method for preparing a sealing glass film comprises the following steps:

[0010] (1) mixing polyvinyl butyral and ethanol and ball milling them, wherein the mass ratio of polyvinyl butyral to ethanol is 1:5-20, to obtain a mixed slurry;

[0011] (2) pouring the mixed slurry obtained in step (1) into a tape casting machine, wherein the tape casting machine is provided with a PET release film tape, and preparing a layer of PVB film on the PET release film tape to form a PET release film tape with PVB film;

[0012] (3) Mixing glass powder, dispersant and solvent for ball milling, wherein the solvent is one or more of pineol, diethylene glycol monobutyl ether and alcohol ester twelve, and testing the particle size of the glass powder. 50 =10μm~12μm, adding a binder and a plasticizer, continuing ball milling, vacuum degassing the ball milled slurry to obtain a casting slurry;

[0013] (4) pouring the casting slurry obtained in step (3) into the casting machine, the casting slurry is cast through the PET release film tape with PVB film, and after drying and demolding, a sealing glass film is obtained.

[0014] In the above-mentioned method for preparing the sealing glass film, preferably, in step (1), the ball milling medium used in the ball milling is zirconium oxide ball, the mass ratio of the ball milling medium to the polyvinyl butyral is 5-20:1, the ball milling time is 2h-5h, and the ball milling speed is 200rad / min-300rad / min.

[0015] In the above-mentioned method for preparing the sealing glass film, preferably, the specific process of step (2) is: preparing a tape casting machine, the tape casting machine comprising a scraper, a PET release film tape and a slurry tank, pouring the mixed slurry into the slurry tank, driving the mixed slurry tank forward by the PET release film tape, and using the scraper to form a layer of PVB film on the PET release film tape, and after drying, obtaining a PET release film tape with PVB film, wherein the moving rate is 5 mm / s to 20 mm / s, the height of the scraper is 0.1 mm to 0.3 mm, and the thickness of the PVB film is ≤0.05 mm.

[0016] The above-mentioned method for preparing the sealing glass film, preferably, in step (3): the mass ratio of the glass powder to the solvent is 1:0.5~1, and the mass of the dispersant is 0.5%~1.5% of the mass of the glass powder; the dispersant is one or more of BYK series dispersants, polyethylene glycol 200 and polyethylene glycol 400; the ball milling medium used in the mixed ball milling is one of aluminum oxide balls, zirconium oxide balls and silicon nitride balls, the ball milling time is 6h~24h, the ball milling speed is 200rad / min~400rad / min, and the mass ratio of the ball milling medium to the glass powder is 1~3:1.

[0017] The above-mentioned method for preparing the sealing glass film, preferably, in step (3): the time of continued ball milling is 5h~10h, and the rotation speed of continued ball milling is 200rad / min~400rad / min; the binder is ethyl cellulose or polyvinyl butyral, and the mass of the binder is 3%~8% of the mass of the glass powder; the plasticizer is one or more phthalate plasticizers, and the mass of the plasticizer is 20%~60% of the mass of the binder; the time of vacuum degassing is 15min~30min, and the vacuum degree is 100Pa~1000Pa.

[0018] In the above-mentioned method for preparing the sealing glass film, preferably, the specific process of step (4) is: pouring the casting slurry obtained in step (3) into the slurry tank of the casting molding machine, driving the slurry tank forward by the PET release film tape with PVB film, and using the scraper to form a liquid film on the PET release film tape with PVB film, and obtaining the sealing glass film after drying and demolding; wherein the moving rate is 5 mm / s to 20 mm / s, the height of the scraper is 0.2 mm to 0.5 mm, and the drying temperature is 50°C to 80°C.

[0019] As a general technical concept, the present invention also provides a sealing glass film prepared by the above-mentioned method for preparing the sealing glass film.

[0020] As a general technical concept, the present invention also provides an application of the above-mentioned sealing glass film in sealing ceramic components.

[0021] The above application preferably comprises the following steps:

[0022] S1. Ultrasonic cleaning and drying of the ceramic parts to be sealed;

[0023] S2, cutting the sealing glass film according to the shape of the bonding area of ​​the ceramic component to be sealed;

[0024] S3. Firstly apply a layer of solvent on the surface of the bonding area of ​​the ceramic component to be sealed, wherein the solvent is consistent with the solvent used in the preparation process of the sealing glass film, and then adhere the cut sealing glass film to the bonding area. After assembling the obtained ceramic components to be sealed, fix them with tooling, and obtain the sealed ceramic components after drying and sintering.

[0025] In the above application, preferably, in step S3, the drying temperature is 60°C to 80°C; the sintering process conditions are: the heating rate is 0.5°C / min to 2°C / min, the sintering temperature is 600°C to 1000°C, the holding time is 1h to 4h, and the sintering atmosphere is a vacuum atmosphere or an air atmosphere.

[0026] In the present invention, the glass powder is commercially available glass powder and can be adapted according to the sealing body.

[0027] Compared with the prior art, the advantages of the present invention are:

[0028] The present invention adopts a sealing glass film prepared by a tape-casting process to replace the existing screen printing process for gluing, thereby ensuring the uniformity of the thickness of the sealing glass in the bonding area, avoiding the phenomena of empty glue, overflowing glue, bubbles, etc. to the greatest extent, and achieving high-efficiency and high-strength sealing.

[0029] In the present invention, a layer of PVB film is coated on the PET release film tape in the tape casting process, which can realize the preparation of ultra-thin sealing glass film on the one hand, and can realize safe demoulding of the sealing glass film on the other hand. The PVB film can be used to solve the problem that the solvent and the release film are incompatible. The release film is convenient for demoulding, but the surface tension between the solvent and the release film is large, and it is impossible to prepare a sealing glass film with uniform thickness. The PVB film is used as a transition layer, and the surface tension between the PVB film and the solvent is small, so that the two are compatible, which not only ensures the characteristic of easy demoulding, but also solves the problem of uneven thickness caused by excessive surface tension.

[0030] In the preparation method of the sealing glass film of the present invention, an organic substance with a relatively high boiling point (>150°C) such as pine alcohol is used as a solvent, which can achieve slow drying of the sealing glass film, thereby obtaining a sealing glass film with a flat surface and uniform thickness. When the sealing glass film of the present invention is applied to the bonding process of ceramic components, a homologous solvent is coated on the bonding area to ensure wettability with the sealing glass film, achieve close fitting, and also dissolve a portion of the adhesive in the sealing glass film, and achieve bonding strength between the sealing glass film and the ceramic component after drying.

[0031] In summary, the method for preparing the sealing glass film provided by the present invention has a simple process and strong universality. The prepared sealing glass film is easy to preserve and can be widely used in the sealing of various precision ceramic parts. DETAILED DESCRIPTION

[0032] The present invention is further described below in conjunction with specific preferred embodiments, but the protection scope of the present invention is not limited thereby. The materials and instruments used in the following embodiments are all commercially available, wherein the tape casting machine is the LYJ-253-3 tape casting machine of Beijing Dongfang Taiyang Technology Co., Ltd., but is not limited thereto.

[0033] Example 1

[0034] A method for preparing a sealing glass film of the present invention comprises the following steps:

[0035] (1) Weigh polyvinyl butyral (PVB), ethanol and zirconium oxide balls and place them in a ball mill for ball milling. The mass ratio of polyvinyl butyral: ethanol: zirconium oxide balls is 1:10:10. The ball milling time is 3 h and the rotation speed is 200 rad / min to obtain a mixed slurry.

[0036] (2) preparing a tape casting machine, which includes a scraper, a PET release film tape and a slurry tank, adjusting the height of the scraper of the tape casting machine, pouring the mixed slurry obtained in step (1) into the slurry tank, starting the power supply, and driving the slurry in the slurry tank to move forward by the parallel movement of the PET release film tape (i.e., the silicone oil-modified PET film), and using the scraper to form a layer of PVB film on the PET release film tape. After natural drying at room temperature, a layer of PVB film with a thickness of 0.02 mm is formed on the PET release film tape, wherein the movement rate is 10 mm / s and the height of the scraper is 0.2 mm.

[0037] (3) Weigh 400 g of glass powder (Gujing Technology, FJB-2915), 4 g of dispersant BYK-170, 400 g of pine alcohol and 800 g of zirconium oxide balls and place them in a ball mill for 6 h at a speed of 300 rad / min. Test the particle size of the glass powder. 50 =10μm, add 30g ethyl cellulose and 12g dibutyl phthalate, and continue ball milling for 5h at a rotation speed of 300rad / min. After ball milling, pour the resulting slurry into a vacuum degassing device for vacuum degassing. The degassing time is 20min and the vacuum degree is 1000Pa to obtain a casting slurry.

[0038] (4) Adjust the scraper height of the tape casting machine, pour the tape casting slurry obtained in step (3) into the slurry tank, start the power supply, and drive the slurry in the slurry tank to move forward by the parallel movement of the PET release film belt with the PVB film. Use the scraper to form a layer of liquid film with the tape casting slurry. The scraper height is 0.5 mm, and the moving speed is 10 mm / s. Adjust the temperature of the tape casting machine to 60°C to allow the liquid film to dry slowly. After demolding, a sealing glass film is obtained.

[0039] An application of the sealing glass film of this embodiment in sealing a ceramic component comprises the following steps:

[0040] S1. Clean the ceramic parts to be sealed using an ultrasonic cleaning device and dry them using hot air;

[0041] S2, cutting the sealing glass film according to the shape of the bonding area of ​​the ceramic component to be sealed;

[0042] S3. Coat a layer of pine oil on the bonding area of ​​the ceramic component to be sealed, attach the cut sealing glass film to the bonding area, assemble the ceramic components and fix them with tooling, then place them in an oven for drying at 80°C, transfer the bonded ceramic components to a sintering furnace for sintering at a heating rate of 1°C / min, a sintering temperature of 800°C, a holding time of 2h, and an air atmosphere. After sintering, a sealed ceramic component is obtained.

[0043] Example 2

[0044] A method for preparing a sealing glass film of the present invention comprises the following steps:

[0045] (1) Weigh polyvinyl butyral, ethanol and zirconium oxide balls and place them in a ball mill for ball milling. The mass ratio of polyvinyl butyral: ethanol: zirconium oxide balls is 1:10:10. The ball milling time is 3 h and the rotation speed is 200 rad / min to obtain a mixed slurry.

[0046] (2) preparing a tape casting machine, which includes a scraper, a PET release film tape and a slurry tank, adjusting the scraper height of the tape casting machine, pouring the mixed slurry obtained in step (1) into the slurry tank, starting the power supply, and driving the slurry in the slurry tank to move forward through the parallel movement of the PET release film tape, and using the scraper to form a layer of PVB film on the PET release film tape with a thickness of 0.02 mm. After natural drying at room temperature, a PET release film tape with a PVB film is obtained, wherein the scraper height is 0.2 mm and the moving speed is 10 mm / s.

[0047] (3) 800 g of glass powder (Lomat, LMT-P750W), 4 g of dispersant BYK-170, 400 g of pine alcohol and 800 g of zirconium oxide balls were weighed and placed in a ball mill for ball milling. The ball milling time was 12 h and the speed was 300 rad / min. The particle size of the glass powder was tested. When D 50 =10μm), add 30g ethyl cellulose and 12g dibutyl phthalate, and continue ball milling for 5h at a rotation speed of 300rad / min. After ball milling, pour the resulting slurry into a vacuum degassing device for vacuum degassing. The degassing time is 20min and the vacuum degree is 1000Pa to obtain a casting slurry.

[0048] (4) Adjust the scraper height of the tape casting machine, pour the tape casting slurry obtained in step (3) into the slurry tank, start the power supply, and drive the slurry in the slurry tank to move forward by the parallel movement of the PET release film belt with the PVB film. Use the scraper to form a layer of liquid film with the tape casting slurry. The scraper height is 0.5 mm, and the moving speed is 10 mm / s. Adjust the temperature of the tape casting machine to 60°C to allow the liquid film to dry slowly. After demolding, a sealing glass film is obtained.

[0049] An application of the sealing glass film of this embodiment in sealing a ceramic component comprises the following steps:

[0050] S1. Use an ultrasonic cleaning device to ultrasonically clean the ceramic parts to be sealed, and use hot air to blow them dry;

[0051] S2, cutting the sealing glass film according to the shape of the bonding area of ​​the ceramic component to be sealed;

[0052] S3. Coat a layer of pine oil on the surface of the bonding area of ​​the ceramic component to be sealed, attach the cut sealing glass film to the bonding area, assemble the ceramic components and fix them with tooling, and then place them in an oven for drying at a temperature of 80°C. Transfer the bonded ceramic components to a sintering furnace for sintering at a heating rate of 1°C / min, a sintering temperature of 780°C, a holding time of 2h, and an air atmosphere. After sintering, a sealed ceramic component is obtained.

[0053] Example 3

[0054] A method for preparing a sealing glass film of the present invention comprises the following steps:

[0055] (1) Weigh polyvinyl butyral, ethanol and zirconium oxide balls and place them in a ball mill for ball milling. The mass ratio of polyvinyl butyral: ethanol: zirconium oxide balls is 1:10:10. The ball milling time is 3 h and the rotation speed is 200 rad / min to obtain a mixed slurry.

[0056] (2) preparing a tape casting machine, which includes a scraper, a PET release film tape and a slurry tank, adjusting the scraper height of the tape casting machine, pouring the mixed slurry obtained in step (1) into the slurry tank, starting the power supply, and driving the mixed slurry in the slurry tank to move forward through the parallel movement of the PET release film tape, and using the scraper to form a layer of PVB film on the PET release film tape with a thickness of 0.02 mm. After natural drying at room temperature, a PET release film tape with a PVB film is obtained, wherein the scraper height is 0.2 mm and the moving speed is 10 mm / s.

[0057] (3) Weigh 500 g of glass powder (Lomat, LMT-S1000), 4 g of dispersant BYK-170, 300 g of pine alcohol, 100 g of alcohol ester dodecahydrate and 800 g of zirconium oxide balls and place them in a ball mill for 12 h at a speed of 300 rad / min. Test the particle size of the glass powder. When D 50 =10μm, add 30g of polyvinyl butyral and 15g of dibutyl phthalate, and continue ball milling for 5h at a rotation speed of 300rad / min. After ball milling, pour the resulting slurry into a vacuum degassing device for vacuum degassing. The degassing time is 20min and the vacuum degree is 1000Pa to obtain a casting slurry.

[0058] (4) Adjust the scraper height of the tape casting machine, pour the tape casting slurry obtained in step (3) into the slurry tank, start the power supply, and drive the slurry in the slurry tank to move forward by the parallel movement of the PET release film belt with the PVB film. Use the scraper to form a layer of liquid film with the tape casting slurry. The scraper height is 0.5 mm, and the moving speed is 10 mm / s. Adjust the temperature of the tape casting machine to 70°C to allow the liquid film to dry slowly. After demolding, a sealing glass film is obtained.

[0059] An application of the sealing glass film of this embodiment in sealing a ceramic component comprises the following steps:

[0060] S1. Use an ultrasonic cleaning device to ultrasonically clean the ceramic parts to be sealed, and use hot air to blow them dry;

[0061] S2, cutting the sealing glass film according to the shape of the bonding area of ​​the ceramic component to be sealed;

[0062] S3. Coat a layer of solvent containing pine oil alcohol and alcohol ester in a mass ratio of 3:1 on the surface of the bonding area of ​​the ceramic component to be sealed, adhere the cut sealing glass film to the bonding area, assemble the ceramic components and fix them with tooling, and then place them in an oven for drying at a temperature of 80°C. Transfer the bonded ceramic components to a sintering furnace for sintering at a heating rate of 1°C / min, a sintering temperature of 1000°C, a holding time of 2h, and a vacuum atmosphere. After sintering, a sealed ceramic component is obtained.

[0063] Comparative Example 1

[0064] A method for preparing a sealing glass film, which differs from Example 1 in that a PET film tape is used as a substrate instead of a PVB-coated PET release film tape, and comprises the following steps:

[0065] (1) Weigh 400 g of glass powder (Gujing Technology, FJB-2915), 4 g of dispersant BYK-170, 400 g of pine alcohol and 800 g of zirconium oxide balls and place them in a ball mill for 6 h at a speed of 300 rad / min. Test the particle size of the glass powder. When D 50 =10μm, add 30g ethyl cellulose and 12g dibutyl phthalate, continue ball milling for 5h, the speed is 300rad / min, pour the obtained slurry into a vacuum degassing device for vacuum degassing, the degassing time is 20min, the vacuum degree is 1000Pa, and the casting slurry is obtained;

[0066] (2) Adjust the height of the scraper of the tape casting machine, pour the slurry obtained in step (1) into the tape casting slurry tank, start the power supply, and drive the slurry in the slurry tank to move forward through the parallel movement of the PET film belt, and form a film through the tape casting scraper, wherein the scraper height is 0.5 mm and the moving speed is 10 mm / s; adjust the temperature of the tape casting machine to 60°C, so that the liquid film obtained in step (4) is slowly dried, and then it is demolded to obtain a sealing glass film.

[0067] An application of the sealing glass film of this comparative example in sealing ceramic components is carried out in the same process as in Example 1.

[0068] Comparative Example 2

[0069] A method for preparing a sealing glass film, which differs from Example 1 in that a PET release film tape is used as a substrate instead of a PVB-coated PET release film tape, and comprises the following steps:

[0070] (1) Weigh 400 g of glass powder (Gujing Technology, FJB-2915), 4 g of dispersant BYK-170, 400 g of pine alcohol and 800 g of zirconium oxide balls and place them in a ball mill for 6 h at a speed of 300 rad / min. Test the particle size of the glass powder. 50 =10μm, add 30g ethyl cellulose and 12g dibutyl phthalate, continue ball milling for 5h, the speed is 300rad / min, pour the obtained slurry into a vacuum degassing device for vacuum degassing, the degassing time is 20min, the vacuum degree is 1000Pa, and the casting slurry is obtained;

[0071] (2) Adjust the height of the scraper of the tape casting machine, pour the slurry obtained in step (1) into the tape casting slurry tank, start the power supply, and drive the slurry in the slurry tank to move forward through the parallel movement of the PET release film belt, and form a film through the tape casting scraper, wherein the scraper height is 0.5 mm and the moving speed is 10 mm / s; adjust the temperature of the tape casting machine to 60°C, so that the liquid film obtained in step (4) is slowly dried, and then it is demolded to obtain a sealing glass film.

[0072] An application of the sealing glass film of this comparative example in sealing ceramic components is carried out in the same process as in Example 1.

[0073] Comparative Example 3

[0074] A method for preparing a sealing glass paste, which is the same as the sealing glass raw material used in Example 1, except that a paste is prepared and a screen printing process is used to encapsulate ceramic parts. The preparation method comprises the following steps:

[0075] (1) Weigh 400 g of glass powder (Gujing Technology, FJB-2915), 4 g of dispersant BYK-170, 300 g of pine alcohol and 800 g of zirconium oxide balls and place them in a ball mill for 6 h at a speed of 300 rad / min. Test the particle size of the glass powder. 50 =10 μm, add 30 g of ethyl cellulose and 12 g of dibutyl phthalate, and continue ball milling for 5 h at a speed of 300 rad / min to obtain a slurry;

[0076] (2) Pour the ball-milled slurry in step (1) into a vacuum degassing device for degassing, the degassing time is 20 minutes, the vacuum degree is 1000 Pa, and a screen printing slurry is obtained.

[0077] An application of the sealing glass slurry of this comparative example in sealing a ceramic component comprises the following steps:

[0078] S1. Clean the ceramic parts to be sealed using an ultrasonic cleaning device and dry them using hot air;

[0079] S2. Place a screen printing mold in the bonding area, pour the slurry onto the mold, use a scraper to flatten it, remove the mold, assemble the ceramic parts to be sealed and fix them with a tooling, and then place them in an oven for drying at 80°C.

[0080] S3. The bonded ceramic components are transferred to a sintering furnace for sintering to obtain sealed ceramic components. The heating rate is 1°C / min, the sintering temperature is 800°C, the holding time is 2h, and the sintering atmosphere is air atmosphere.

[0081] Comparative Example 4

[0082] A method for preparing a sealing glass paste is the same as the preparation method of comparative example 3, except that the sealing glass paste is dried before being combined after screen printing during application. The method comprises the following steps:

[0083] (1) Weigh 400 g of glass powder (Gujing Technology, FJB-2915), 4 g of dispersant BYK-170, 300 g of pine alcohol and 800 g of zirconium oxide balls and place them in a ball mill for 6 h at a speed of 300 rad / min. Test the particle size of the glass powder. When D 50 =10 μm, add 30 g of ethyl cellulose and 12 g of dibutyl phthalate, and continue ball milling for 5 h at a speed of 300 rad / min to obtain a slurry;

[0084] (2) Pour the ball-milled slurry in step (1) into a vacuum degassing device for degassing. The degassing time is 20 minutes and the vacuum degree is 1000 Pa to obtain a sealing glass slurry.

[0085] An application of the sealing glass slurry of this comparative example in sealing a ceramic component comprises the following steps:

[0086] S1. Clean the ceramic parts to be sealed using an ultrasonic cleaning device and dry them using hot air;

[0087] S2. Place a screen printing mold on the bonding area, pour the slurry onto the mold, scrape it flat with a scraper, remove the mold, and then place it in an oven to dry at 80°C.

[0088] S3, coating a layer of pineol on the surface of the ceramic component to be sealed, combining it with the ceramic component with the sealing glass printed on the surface, fixing it with a tooling, and then drying it in an oven at a temperature of 80°C;

[0089] S4. The bonded ceramic components are transferred to a sintering furnace for sintering to obtain sealed ceramic components. The heating rate is 1°C / min, the sintering temperature is 800°C, the holding time is 2h, and the sintering atmosphere is air atmosphere.

[0090] Table 1 Forming and sealing conditions of Examples 1-3 and Comparative Examples 1-4

[0091]

[0092] As shown in Table 1, the sealing glass film prepared in Examples 1-3 has a thin and uniform thickness, good airtightness after sealing and only slight glue overflow, strong universality, and a minimum sealing strength of 83MPa. When a PET film tape is used instead of a PET release film tape covered with PVB, film stripping is more difficult, and the sealing strength decreases slightly. When a PET release film tape is used instead of a PET release film tape covered with PVB, due to the surface tension of the solvent, a film with a thickness of 0.2 mm cannot be prepared, and serious glue overflow occurs during sealing, and the sealing strength decreases. When bonding using a silk screen process, if combined before drying, the sealing strength decreases significantly and obvious air leakage occurs. If combined again after drying, serious glue overflow occurs and the sealing strength decreases. From the above content, it can be seen that the sealing glass film preparation process provided by the present invention is simple, easy to preserve, and can achieve high-strength sealing and high airtightness of ceramic parts.

[0093] The above is only a preferred embodiment of the present invention and does not limit the present invention in any form. Although the present invention has been disclosed as above in the preferred embodiment, it is not used to limit the present invention. Any technician familiar with the art can make many possible changes and modifications to the technical solution of the present invention by using the methods and technical contents disclosed above without departing from the spirit and technical solution of the present invention, or modify it into an equivalent embodiment of equivalent changes. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention without departing from the content of the technical solution of the present invention, still fall within the scope of protection of the technical solution of the present invention.

Claims

1. A method for preparing a sealing glass film, characterized in that: The following steps are involved: (1) mixing polyvinyl butyral and ethanol and ball milling them, wherein the mass ratio of polyvinyl butyral to ethanol is 1:5-20, to obtain a mixed slurry; (2) pouring the mixed slurry obtained in step (1) into a tape casting machine, wherein the tape casting machine is provided with a PET release film tape, and preparing a layer of PVB film on the PET release film tape to form a PET release film tape with PVB film; (3) Mixing glass powder, dispersant and solvent for ball milling, wherein the solvent is one or more of pineol, diethylene glycol monobutyl ether and alcohol ester twelve, and testing the particle size of the glass powder. 50 =10μm~12μm, adding a binder and a plasticizer, continuing ball milling, vacuum degassing the ball milled slurry to obtain a casting slurry; (4) pouring the casting slurry obtained in step (3) into the casting machine, the casting slurry is cast through the PET release film tape with PVB film, and after drying and demolding, a sealing glass film is obtained.

2. The method for preparing a sealing glass film according to claim 1, characterized in that: In step (1), the ball milling medium used in the ball milling is zirconium oxide ball, the mass ratio of the ball milling medium to the polyvinyl butyral is 5-20:1, the ball milling time is 2h-5h, and the ball milling speed is 200rad / min-300rad / min.

3. The method for preparing a sealing glass film according to claim 1, characterized in that: The specific process of step (2) is as follows: preparing a tape casting machine, the tape casting machine comprising a scraper, a PET release film tape and a slurry tank, pouring the mixed slurry into the slurry tank, driving the mixed slurry tank forward by the PET release film tape, and using the scraper to form a layer of PVB film on the PET release film tape, and obtaining a PET release film tape with PVB film after drying, wherein the moving rate is 5 mm / s to 20 mm / s, the height of the scraper is 0.1 mm to 0.3 mm, and the thickness of the PVB film is ≤0.05 mm.

4. The method for preparing a sealing glass film according to any one of claims 1 to 3, characterized in that: In step (3): the mass ratio of the glass powder to the solvent is 1:0.5-1, the mass of the dispersant is 0.5%-1.5% of the mass of the glass powder; the dispersant is one or more of BYK series dispersants, polyethylene glycol 200 and polyethylene glycol 400; the ball milling medium used in the mixed ball milling is one of alumina balls, zirconium oxide balls and silicon nitride balls, the ball milling time is 6h-24h, the ball milling speed is 200rad / min-400rad / min, and the mass ratio of the ball milling medium to the glass powder is 1-3:

1.

5. The method for preparing a sealing glass film according to any one of claims 1 to 3, characterized in that: In step (3), the time of continuing ball milling is 5 hours to 10 hours, the rotation speed of continuing ball milling is 200 rad / min to 400 rad / min; the binder is ethyl cellulose or polyvinyl butyral, and the mass of the binder is 3% to 8% of the mass of the glass powder; the plasticizer is one or more phthalate plasticizers, and the mass of the plasticizer is 20% to 60% of the mass of the binder; the time of vacuum degassing is 15 minutes to 30 minutes, and the vacuum degree is 100Pa to 1000Pa.

6. The method for preparing a sealing glass film according to any one of claims 1 to 3, characterized in that: The specific process of step (4) is as follows: pouring the cast slurry obtained in step (3) into the slurry tank of the cast molding machine, driving the slurry tank forward by the PET release film tape with PVB film, and using the scraper to form a liquid film on the PET release film tape with PVB film, and obtaining a sealing glass film after drying and demolding; wherein the moving speed is 5 mm / s to 20 mm / s, the height of the scraper is 0.2 mm to 0.5 mm, and the drying temperature is 50°C to 80°C.

7. A sealing glass film prepared by the method for preparing a sealing glass film according to any one of claims 1 to 6.

8. Use of the sealing glass film according to claim 7 in sealing ceramic components.

9. The use according to claim 8, characterized in that: The following steps are involved: S1. Ultrasonic cleaning and drying of the ceramic parts to be sealed; S2, cutting the sealing glass film according to the shape of the bonding area of ​​the ceramic component to be sealed; S3. Firstly apply a layer of solvent on the surface of the bonding area of ​​the ceramic component to be sealed, wherein the solvent is consistent with the solvent used in the preparation process of the sealing glass film, and then adhere the cut sealing glass film to the bonding area. After assembling the obtained ceramic components to be sealed, fix them with tooling, and obtain the sealed ceramic components after drying and sintering.

10. The use according to claim 9, characterized in that: In step S3, the drying temperature is 60°C to 80°C; the sintering process conditions are: a heating rate of 0.5°C / min to 2°C / min, a sintering temperature of 600°C to 1000°C, a holding time of 1h to 4h, and a sintering atmosphere of a vacuum atmosphere or an air atmosphere.

Images