A sealed glass preform, method of making and use thereof

CN117776504BActive Publication Date: 2026-09-18CHINA BUILDING MATERIALS ACADEMY CO LTD +1
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Patent Information

Application Number
CN202311655322.5
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-12-05
Publication Date
2026-09-18
Estimated Expiration
2043-12-05

AI Technical Summary

Technical Problem

其中,模压法难以制得薄壁管状玻璃预制件;拉拔法经济效应差,多用于单一尺寸玻璃件的大批量生产

Benefits of technology

[0024] This invention proposes a method for preparing sealed glass preforms. It creatively uses paper tubes as molds, and through the preparation of a special glass slurry, the slurry is adsorbed onto the paper tube. After cutting, drying, and pre-sintering, sealed glass preforms are obtained. This method can economically and quickly produce a variety of thin-walled tubular sealed glass preforms of specific sizes in small to medium batches. The sealed glass preforms prepared using this invention significantly improve the sealing pass rate and sealing efficiency. Compared to the traditional glass slurry sealing method with a pass rate of approximately 50% and a sealing efficiency of 20 pieces/person/day (taking a 36-array as an example), the sealing glass preforms of this invention achieve a pass rate of approximately 90% and a sealing efficiency of 100 pieces/person/day. This facilitates standardized product delivery, improves production efficiency, and shortens the production cycle.

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Abstract

This invention provides a sealing glass preform, its preparation method, and its application. The preparation method involves: preparing a paper tube according to sealing requirements, with the inner diameter of the paper tube being the same as the outer diameter of the sealing glass preform; preparing a glass slurry by mixing glass powder, dispersant, defoamer, ammonia, binder, and water; immersing the paper tube in the glass slurry to allow its inner surface to absorb the slurry, then removing it, cutting it, and drying it to obtain a blank; and pre-sintering the blank to obtain the sealing glass preform. The pre-sintering process includes an ablation process and a heat preservation process. During the ablation process, components other than glass are removed from the blank; during the heat preservation process, the glass in the blank is sintered into a whole. The sealing glass preform preparation method proposed in this invention can economically and quickly produce a variety of thin-walled tubular sealing glass preforms of specific sizes in small to medium batches, with a high sealing qualification rate of approximately 90%.
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Description

Technical Field

[0001] This invention relates to the field of high-performance ceramic technology for the electronics industry, and in particular to a sealing glass preform, its preparation method, and its application. Background Technology

[0002] Composite ceramic substrates, due to their excellent mechanical properties, electrical properties, heat resistance, and chemical stability, are widely used in high-tech fields such as aerospace, lasers, high-energy physics, new energy vehicles, semiconductors, and pyrotechnics. Glass brazing filler metals, due to their excellent compatibility and bonding capabilities with ceramics, metals, and semiconductors, are widely used in ceramic-metal and ceramic-ceramic bonding, and are an important component of composite ceramic substrate bonding.

[0003] In composite ceramic substrates, nested glass solder is the most widely used. Due to the small size of the nested glass solder required for composite ceramic substrates (typically 0.5mm thick), traditional glass paste sealing methods cannot guarantee sealing pass rates and efficiency: too little filler leads to a lower pass rate; too much filler leads to waste and reduced sealing efficiency. Existing technology addresses this problem by using sealing glass preforms as nested glass solders. Sealing of the composite ceramic substrate is achieved by nesting sealing glass preforms of corresponding sizes into the gaps to be sealed. With the continuous rise of my country's manufacturing industry, the requirements for precision composite ceramic substrate materials are constantly increasing, and sealing glass preforms are now required to meet multiple criteria such as "thin, stable, well-matched, and strong." Among these, controlling the thickness of the sealing glass preform is a core parameter in the processing, directly affecting sealing strength and airtightness.

[0004] Existing methods for preparing sealed glass preforms are mostly molding and melt drawing. Among them, molding is difficult to produce thin-walled tubular glass preforms; drawing is not economically efficient and is mostly used for mass production of single-size glass parts. Summary of the Invention

[0005] The main objective of this invention is to provide a sealing glass preform, its preparation method, and its application. The technical problem to be solved is how to economically and quickly obtain a variety of thin-walled tubular sealing glass preforms with specific specifications and sizes in small to medium batches, thereby making them more suitable for practical use.

[0006] The objective of this invention and the technical problem it solves are achieved by the following technical solution. A method for preparing a sealing glass preform according to this invention includes the following steps:

[0007] (1) Prepare a paper tube according to the sealing requirements; the inner diameter of the paper tube is the same as the outer diameter of the sealing glass preform to be prepared;

[0008] (2) Glass powder, dispersant, defoamer, ammonia, binder and water are used to prepare glass slurry;

[0009] (3) Immerse the paper tube in the glass slurry so that the glass slurry is adsorbed on its inner surface; take out the paper tube with the glass slurry adsorbed on its inner surface, cut it, and then dry it to obtain a blank.

[0010] (4) The blank is pre-sintered to obtain the sealed glass preform;

[0011] The pre-sintering process includes an ablation process and a heat preservation process; during the ablation process, components other than glass are removed from the green body; during the heat preservation process, the glass in the green body is sintered into a whole.

[0012] The objectives of this invention and the technical problems it addresses can be further achieved by the following technical measures.

[0013] In some embodiments, in the aforementioned method for preparing the sealed glass preform, the paper tube is made of kraft paper, and the single-sided wall thickness of the paper tube is 1-5 mm.

[0014] In some embodiments, in the aforementioned method for preparing sealed glass preforms, the glass powder accounts for 40-60% of the glass slurry by volume percentage, with the glass slurry volume being 100%.

[0015] In some embodiments, in the aforementioned method for preparing sealed glass preforms, the viscosity of the glass slurry is 0.3–1.5 Pa·s, and the pH is 9–11.

[0016] In some embodiments, in the aforementioned method for preparing sealed glass preforms, the glass powder, the dispersant, the defoamer, the binder, ammonia, and water are mixed and then ground to obtain the glass slurry.

[0017] The particle size D of the glass powder 50 The range is 0.1–5.0 μm or D 90 The range is 0.5–5.0 μm, and the grinding time is 20–60 h.

[0018] In some embodiments, in the aforementioned method for preparing the sealing glass preform, the immersion time in step (3) is 10 to 120 minutes, the single-sided wall thickness of the glass slurry adsorbed on the inner surface of the paper tube is 0.2 to 2.5 mm, and the glass slurry is dried at 60°C to 100°C for 2 to 5 hours.

[0019] In some embodiments, in the aforementioned method for preparing sealed glass preforms, the ablation process during pre-sintering is carried out at a temperature of 200°C to 400°C for a time of 0.5 to 3 hours; the heat preservation process is carried out at a temperature of 400°C to 500°C for a time of 15 to 60 minutes.

[0020] The objective of this invention and the technical problem it solves are also achieved by the following technical solution. A sealing glass preform according to this invention is prepared using the aforementioned method, and its single-sided wall thickness is 0.1–2.0 mm.

[0021] The objective of this invention and the technical problem it solves are also achieved by the following technical solution. A composite ceramic substrate according to this invention is sealed using the aforementioned sealing glass preform.

[0022] The objectives of this invention and the solutions to its technical problems are also achieved through the following technical solutions. The composite ceramic substrate proposed in this invention has applications in aerospace, high-energy physics, and laser devices.

[0023] Through the above technical solution, the sealing glass preform, its preparation method, and its application of the present invention have at least the following advantages:

[0024] This invention proposes a method for preparing sealed glass preforms. It creatively uses paper tubes as molds, and through the preparation of a special glass slurry, the slurry is adsorbed onto the paper tube. After cutting, drying, and pre-sintering, sealed glass preforms are obtained. This method can economically and quickly produce a variety of thin-walled tubular sealed glass preforms of specific sizes in small to medium batches. The sealed glass preforms prepared using this invention significantly improve the sealing pass rate and sealing efficiency. Compared to the traditional glass slurry sealing method with a pass rate of approximately 50% and a sealing efficiency of 20 pieces / person / day (taking a 36-array as an example), the sealing glass preforms of this invention achieve a pass rate of approximately 90% and a sealing efficiency of 100 pieces / person / day. This facilitates standardized product delivery, improves production efficiency, and shortens the production cycle.

[0025] The above description is merely an overview of the technical solution of the present invention. In order to better understand the technical means of the present invention and to implement it in accordance with the contents of the specification, the preferred embodiments of the present invention are described in detail below with reference to the accompanying drawings. Detailed Implementation

[0026] To further illustrate the technical means and effects adopted by the present invention to achieve its intended purpose, the following, in conjunction with the accompanying drawings and preferred embodiments, provides a detailed description of the specific implementation methods, structures, features, and effects of a sealing glass preform and its preparation method according to the present invention. In the following description, different "embodiments" or "embodiments" do not necessarily refer to the same embodiment. Furthermore, specific features, structures, or characteristics in one or more embodiments can be combined in any suitable manner.

[0027] These embodiments are provided to make the invention thorough and complete, and to fully express the scope of the invention to those skilled in the art. It should be noted that, unless otherwise specifically stated, the relative arrangement of components and steps, material composition, numerical expressions, and values ​​set forth in these embodiments should be interpreted as merely exemplary and not as limiting.

[0028] This invention proposes a method for preparing a sealing glass preform, the steps of which include:

[0029] (1) Prepare a paper tube according to the sealing requirements; the inner diameter of the paper tube is the same as the outer diameter of the sealing glass preform to be prepared;

[0030] (2) Glass powder, dispersant, defoamer, ammonia, binder and water are used to prepare glass slurry;

[0031] (3) Immerse the paper tube in the glass slurry so that the glass slurry is adsorbed on its inner surface; take out the paper tube with the glass slurry adsorbed on its inner surface, cut it, and then dry it to obtain the blank;

[0032] (4) The blank is pre-sintered to remove components other than glass from the blank, so that the glass in the blank is sintered into a whole.

[0033] Specifically, in step (1), the paper used to make the paper tube must have a certain thickness, hardness, and good water permeability, so that it can absorb a certain amount of glass slurry and maintain its shape after absorbing the glass slurry. The shape of the inner wall of the paper tube is the same as the shape of the glass preform to be sealed, and it is suitable for different shapes such as cylindrical holes, elliptical holes, or tapered holes; the inner diameter of the paper tube is the same as the outer diameter of the glass preform to be prepared.

[0034] In step (2), glass powder, dispersant, defoamer, ammonia, binder, and water are prepared into a glass slurry. The glass slurry must have a certain viscosity so that it can be adsorbed onto the inner wall of the paper tube.

[0035] The purpose of adding a dispersant is to ensure that the glass powder is uniformly dispersed in the glass slurry. The dispersant can be polyacrylamide, carboxylic acid amine, polyethylene glycol, or other commercially available dispersants, and the amount added depends on the mass of the glass powder and the type of dispersant. Preferably, the dispersant has a mass fraction of 0.5% to 2.0% based on the mass of the glass powder (100%).

[0036] The purpose of adding defoamer is to eliminate foam in the prepared glass slurry, increase the viscosity of the glass slurry, and eliminate air bubbles in the prepared glass sealing preforms, thereby improving the sealing qualification rate. The defoamer can be any commercially available defoamer, and can be added according to the total volume of the glass slurry and the type of defoamer.

[0037] The purpose of adding ammonia is to adjust the pH of the glass slurry, making it weakly alkaline, ionizing the dispersant, increasing the absolute value of the zeta potential of the glass powder, improving the rheological properties of the slurry, and the ammonia can be completely removed during the subsequent sintering process without changing the composition of the glass.

[0038] The purpose of adding a binder is to increase the viscosity of the glass slurry, allowing it to adhere to the inner wall of the paper tube. The binder can be gum arabic, gelatin, carboxymethyl cellulose, or other commercially available binders, added according to the mass of the glass powder and the type of dispersant. Preferably, the glass powder constitutes 100% of the total volume, and the binder comprises 0.1% to 0.5% of the total volume.

[0039] The height of the paper tube after cutting should be 0.1 to 1.0 mm higher than the required sealing height, preferably 0.2 to 0.5 mm.

[0040] In step (3), the paper tube is immersed in the glass slurry, causing its inner surface to absorb the slurry. The paper tube with the slurry absorbed is then removed and dried to obtain a preform. The required thickness of the glass slurry absorbed on the inner surface of the paper tube is adjusted according to the wall thickness of the glass preform to be sealed. The thickness of the glass slurry absorbed by the paper tube is related to various factors, including the glass powder particle size, the material of the paper tube, the wall thickness of the paper tube, and the immersion time of the paper tube in the glass slurry. Adjustments are made based on actual practical conditions.

[0041] The paper tubes that adsorb the glass slurry can be dried using any existing drying technology; no restrictions are imposed here. The purpose of this step is to facilitate the subsequent sintering of the green body.

[0042] In step (4), the preform is sintered to obtain a sealed glass preform. The sintering process includes an ablation process and a pre-sintering process; during the ablation process, components other than glass are removed from the preform; during the pre-sintering process, the glass in the preform is sintered into a whole, so that the sealed glass preform has a certain strength.

[0043] The aforementioned preform is placed in a sintering furnace. The ablation temperature is determined based on the ignition point of the raw materials used in the paper tube and the melting temperature of the glass powder. The ablation temperature should be higher than the combustion temperature of the paper tube but lower than the melting point of the glass. The pre-sintering temperature is determined based on the melting point of the glass. The pre-sintering temperature should be higher than the melting point of the glass, but not too high, lest the sealing glass preform melt and deform. The duration of the ablation and pre-sintering processes is determined based on the temperature, preform size, and glass slurry thickness.

[0044] The single-sided wall thickness of the sintered sealing glass is preferably 0.1–1.2 mm; its height is 0.1–0.8 mm higher than the ceramic substrate to be sealed, preferably 0.1–0.4 mm higher, which corresponds to the aforementioned length range of the paper tube. If the height of the sealing glass preform is too low, it may affect the airtightness of the seal; if the height is too high, production efficiency will decrease, costs will increase, and more glass filler metal will easily overflow during sealing.

[0045] In some embodiments, the paper tube is made of kraft paper; kraft paper is flexible and strong, has high burst strength, good water permeability, and is readily available in various sizes on the market. The single-sided wall thickness of the paper tube is preferably 1-5mm. If the paper tube is too thin, it can only absorb a small amount of glass slurry; if the paper tube is too thick, it is not conducive to drying and increases costs.

[0046] In some embodiments, with the volume of the glass slurry as 100%, the glass powder accounts for 40-60% of the glass slurry by volume percentage. When the volume fraction of glass powder is less than 40%, the low solid content can easily lead to cracking or even breakage of the glass preform during the pre-sintering process; when the volume fraction of glass powder is greater than 60%, the viscosity of the prepared glass slurry is too high, making it difficult to control the thickness of the preform, and it is easy to form a circular piece rather than a ring preform in the inner diameter of the paper tube, and air bubbles are easily retained during the pre-sintering process, affecting the quality of the preform.

[0047] In some embodiments, the viscosity of the glass slurry is 0.3–1.5 Pa s, and the pH is 9–11. When the viscosity is below 0.3 Pa s, it is not easily adsorbed, and the glass slurry tends to flow down the paper tube wall, causing irregular deformation; if the viscosity is too high, the thickness of the preform is difficult to control, and it is easy to form a circular piece rather than a ring preform in the inner diameter of the paper tube, and air bubbles are easy to remain during the pre-sintering process, affecting the quality of the preform.

[0048] A pH below 9 is unfavorable for dispersant dissociation, further limiting the fluidity of the glass slurry. Adjusting the pH above 11 with ammonia requires adding a large amount of ammonia, making it impossible to guarantee the volume fraction of glass powder in the slurry, which can easily cause the green body to crack or even break during pre-sintering. If other inorganic dispersants are used, it is difficult to avoid the presence of metal cations in the slurry, and they cannot be removed during the pre-sintering process.

[0049] In some embodiments, glass powder, dispersant, defoamer, binder, ammonia, and water are mixed and then ground to obtain a glass slurry; the particle size D of the glass powder is... 50 The range is 0.1–5.0 μm or D 90 The particle size range is 0.5–5.0 μm, and the grinding time is 20–60 h. If the glass powder used is at the nanoscale, grinding is not necessary, but this method is too costly. Therefore, a particle size D is used. 50 The range is 0.1–5.0 μm or D 90 Glass powder with a particle size ranging from 0.5 to 5.0 μm, after being mixed with other substances, requires a grinding time of 20 to 60 hours. Ball milling can be used for grinding. If the glass powder particle size is too large, the required grinding time is too long, resulting in poor cost-effectiveness; if the glass powder particle size is too small, the raw material cost is high. If the grinding time is less than 20 hours, the glass particle size in the glass slurry will be too large, which is not conducive to the adsorption of the glass slurry; if the grinding time is greater than 60 hours, the quality of the slurry cannot be further improved, reducing the cost-effectiveness.

[0050] In some embodiments, in step (3), the immersion time of the paper tube is 10-120 min, the single-sided wall thickness of the glass slurry adsorbed on the inner surface of the paper tube is 0.2-2.5 mm, and the drying method is to dry it in a constant temperature oven at 60℃-100℃ for 2-5 hours. The immersion time of the paper tube in the glass slurry is 10-120 min, preferably 20-60 min. If the immersion time of the paper tube in the glass slurry is too short, less glass slurry will be adsorbed or the glass slurry adsorbed on its surface will not be uniform, affecting the sealing qualification rate; if the immersion time of the paper tube in the glass slurry is too long, it will affect the strength of the paper tube, and the paper tube may deform in subsequent processes. The single-sided wall thickness of the glass slurry adsorbed on the inner wall of the paper tube is 0.2-2.5 mm, preferably 0.2-1.3 mm. The single-sided wall thickness of the sealing glass preform obtained within this range is 0.1-1.2 mm, which is suitable for most sealing environments.

[0051] In some embodiments, the ablation process is carried out at a temperature of 200℃ to 400℃ for a time of 0.5 to 3 hours; the pre-sintering process is carried out at a temperature of 400℃ to 500℃ for a time of 15 to 60 minutes. The sealing temperature of commonly used sealed glass preforms is around 600℃. Based on this, the temperature ranges for the ablation and pre-sintering processes are determined. If the ablation process temperature is below 200℃ or the time is less than 0.5 hours, substances other than glass in the preform are difficult to burn completely and be completely removed. If the ablation process temperature is above 400℃, the glass in the preform easily softens and encapsulates impurities, making it impossible to completely remove the impurities. If the ablation process time is greater than 3 hours, heat is wasted. If the pre-sintering process temperature is below 400℃ or the time is less than 10 minutes, the resulting sealed glass preform has poor strength and is difficult to handle and install. If the pre-sintering process temperature is above 500℃ or the time is greater than 60 minutes, the sealed glass preform is prone to softening and deformation during preparation, increasing costs.

[0052] This invention proposes a sealing glass preform, prepared using the aforementioned method, with a single-sided wall thickness of 0.1–2.0 mm. The sealing glass preform proposed in this invention can seal various composite ceramic substrates, such as ceramic-ceramic, ceramic-metal, and ceramic-metal oxide substrates.

[0053] This invention proposes a composite ceramic substrate, which is sealed using the aforementioned sealing glass preform. Specifically, according to the sealing requirements of the composite ceramic substrate, a corresponding sealing glass preform is prepared using the method described in this invention. After removing preforms with pores or chipped edges, the unsealed composite ceramic substrate and the sealing glass preform are assembled on a sealing tray and then placed in a sealing furnace for sealing to obtain the composite ceramic substrate.

[0054] The present invention also proposes applications of the aforementioned composite ceramic substrate in aerospace, high-energy physics, laser devices, new energy vehicles, semiconductors, or pyrotechnics.

[0055] The present invention will be further described below with reference to specific embodiments, but this should not be construed as a limitation on the scope of protection of the present invention. Some non-essential improvements and adjustments made by those skilled in the art based on the above description of the present invention still fall within the scope of protection of the present invention.

[0056] Unless otherwise specified, all materials and reagents mentioned below are commercially available products well known to those skilled in the art; unless otherwise specified, all methods described are methods known in the art. Unless otherwise defined, the technical or scientific terms used should have the ordinary meaning understood by those skilled in the art to which this invention pertains.

[0057] In the following embodiments, the sealing temperature of the glass powder used is 600°C. The sealing pass rate is specified as follows: the airtightness detected by the helium leak detector is not higher than 10%. -7 pa·m 3 / s; and the concentricity measurement deviation of the image instrument does not exceed 0.02mm.

[0058] Example 1

[0059] (1) Prepare a kraft paper tube with a single-sided wall thickness of 1.5 mm, an inner diameter of 2.2 mm, and a height of 10 cm.

[0060] (2) In deionized water with the same volume fraction as the glass powder, add 0.23wt% gum arabic, 1wt% polyacrylamide, 4d / 100g defoamer, and 5d / 100g ammonia water, with the glass powder as 100% of its mass. Add the glass powder in two batches, and ball mill for 40 hours to obtain a glass slurry with a viscosity of 1 Pa·s and pH = 9.0; wherein the particle size D of the glass powder is... 50 =0.5μm.

[0061] (3) Immerse the kraft paper tube from step one vertically into the glass slurry from step two, keep it for 60 minutes, take it out of the slurry, cut it to a height of about 0.9 mm, and put it into a 60°C oven to dry for 2 hours to obtain the blank.

[0062] (4) The blank from step three is placed in a sintering furnace for sintering to obtain a sealed glass preform with a single-sided wall thickness of 1.0 mm, an outer diameter of 1.1 mm, and a height of 0.5 mm. The sintering temperature profile is as follows:

[0063]

[0064] After removing obvious pores and chipped edges from the sealing glass preform, a 0.4mm thick dielectric ceramic substrate, ferrite, and sealing glass preform are assembled on a sealing tray, and then placed in a sealing furnace for sealing to obtain a composite ceramic substrate. The sealing temperature profile is as follows:

[0065]

[0066] The sealing pass rate of the composite ceramic substrate was found to be 92% after testing.

[0067] Example 2

[0068] (1) Prepare a kraft paper tube with a single-sided wall thickness of 4 mm, an inner diameter of 2.2 mm, and a height of 10 cm.

[0069] (2) In deionized water with the same volume fraction as the glass powder, add 0.23wt% gum arabic, 1wt% polyacrylamide, 4d / 100g defoamer, and 5d / 100g ammonia water, with the glass powder as 100% of its mass. Add the glass powder in two batches, and ball mill for 40 hours to obtain a glass slurry with a viscosity of 1 Pa·s and pH = 9.0; wherein the particle size D of the glass powder is... 90 =0.5μm.

[0070] (3) Immerse the kraft paper tube from step one vertically into the glass slurry from step two, keep it for 60 minutes, take it out of the slurry, cut it to a height of about 0.7 mm, and put it into a 60°C oven to dry for 2 hours to obtain the blank.

[0071] (4) The blank from step three is placed in a sintering furnace for sintering to obtain a sealed glass preform with a single-sided wall thickness of 1.5 mm, an outer diameter of 2.0 mm, and a height of 0.6 mm. The sintering temperature profile is as follows:

[0072]

[0073] After removing obvious pores and chipped edges from the sealing glass preform, a 0.5mm thick dielectric ceramic substrate, ferrite, and sealing glass preform are assembled on a sealing tray, and then placed in a sealing furnace for sealing to obtain a composite ceramic substrate. The sealing temperature profile is as follows:

[0074]

[0075] The sealing pass rate of the composite ceramic substrate was found to be 88% after testing.

[0076] In this embodiment, D 90 The particle size of the glass powder is represented by the selection of thicker kraft paper tubes, which effectively improves the adsorption rate and ultimately yields a blank that can be sintered to produce a sealed glass preform with a single-sided wall thickness of 1.5 mm.

[0077] Example 3

[0078] The difference from Example 1 is that the amount of ammonia added is 1 d / 100g. A glass slurry with a viscosity of 1 Pa·s and pH = 7.0 is obtained. The single-sided wall thickness of the sealing glass preform prepared in this example is 1.5 mm.

[0079] The sealing pass rate of the composite ceramic substrate was found to be 88% after testing.

[0080] Compared with Example 1, the pH value of the slurry was adjusted in this example. The pH value affects the suspension performance of the glass powder, which in turn affects the viscosity of the glass slurry and changes the adsorption effect.

[0081] Example 4

[0082] The difference from Example 1 is that the kraft paper tube is immersed in the glass slurry for 30 minutes. The single-sided wall thickness of the sealing glass preform prepared in this example is 0.8 mm.

[0083] The sealing pass rate of the composite ceramic substrate was found to be 90% after testing.

[0084] Compared with Example 1, this example shortens the soaking time of the kraft paper tube in the glass slurry, which directly affects the adsorption thickness of the glass slurry on the inner wall of the paper tube.

[0085] Example 5

[0086] The difference from Example 1 is that the ball milling time was 20 hours, resulting in a glass slurry with a viscosity of 1.4 Pa·s and a pH of 9. The single-sided wall thickness of the sealing glass preform prepared in this example is 1.5 mm.

[0087] The sealing pass rate of the composite ceramic substrate was found to be 88% after testing.

[0088] Compared with Example 1, the ball milling time was changed from 40h to 20h, which resulted in lower fluidity of the glass slurry, a thicker adsorption thickness of the glass slurry on the inner wall of the paper tube, and a thicker single-sided wall thickness of the resulting sealed glass preform.

[0089] The technical features in the claims and / or specification of this invention can be combined, and the combination is not limited to the combinations obtained through reference in the claims. Technical solutions obtained by combining the technical features in the claims and / or specification are also within the scope of protection of this invention.

[0090] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Any simple modifications, equivalent changes, and alterations made to the above embodiments based on the technical essence of the present invention shall still fall within the scope of the technical solution of the present invention.

Claims

1. A method for preparing a sealing glass preform, characterized in that, The steps include: (1) Prepare a paper tube according to the sealing requirements; the paper tube is made of kraft paper and the single-sided wall thickness of the paper tube is 1~5mm; The inner diameter of the paper tube is the same as the outer diameter of the sealing glass preform to be prepared; (2) Glass slurry is prepared by mixing glass powder, dispersant, defoamer, ammonia, binder and water; the viscosity of the glass slurry is 0.3~1.5 Pa·s and the pH is 9~11. (3) Immerse the paper tube in the glass slurry so that the glass slurry is adsorbed on its inner surface; The paper tube with the glass slurry adsorbed on its inner surface is removed, cut, and then dried to obtain a blank. (4) The blank is pre-sintered to obtain the sealed glass preform; The pre-sintering process includes an ablation process and a heat preservation process; during the ablation process, components other than glass are removed from the blank; during the heat preservation process, the glass in the blank is sintered into a whole.

2. The preparation method according to claim 1, characterized in that, With the volume of the glass slurry as 100%, the glass powder accounts for 40-60% of the glass slurry by volume percentage.

3. The preparation method according to claim 1, characterized in that, The glass powder, the dispersant, the defoamer, the binder, ammonia, and water are mixed and then ground to obtain the glass slurry. The particle size D of the glass powder 50 The range is 0.1~5.0μm or D 90 The range is 0.5~5.0μm, and the grinding time is 20~60h.

4. The preparation method according to claim 1, characterized in that, In step (3), the immersion time is 10~120min, and the single-sided wall thickness of the glass slurry adsorbed on the inner surface of the paper tube is 0.2~2.5mm; and it is dried at 60℃~100℃ for 2h~5h.

5. The preparation method according to claim 1, characterized in that, The ablation process in the pre-sintering is carried out at a temperature of 200℃~400℃ for 0.5~3h; the heat preservation process is carried out at a temperature of 400℃~500℃ for 15~60min.

6. A pre-fabricated sealed glass component, characterized in that, The material is prepared by any one of the preparation methods described in claims 1-5, and its single-sided wall thickness is 0.1~2.0 mm.

7. A composite ceramic substrate, characterized in that, The sealing is performed using the sealing glass preform as described in claim 6.

8. The application of the composite ceramic substrate according to claim 7 in the fields of aerospace, high-energy physics, laser devices, new energy vehicles, semiconductors or pyrotechnics.

Citation Information

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