Glass sealing material, sealing method for glass container, glass product, and tempered glass product

By using a slurry composed of low softening point glass powder and solvent for sealing glass containers, the problems of insufficient sealing and appearance durability are solved, and the process is simplified and energy-saving sealing is achieved.

WO2025252222A1PCT designated stage Publication Date: 2025-12-11WEIDALI IND CHIBI CO LTD
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Patent Information

Application Number
PCT/CN2025/099694
Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
Priority Date
2024-06-07
Filing Date
2025-06-06
Publication Date
2025-12-11

AI Technical Summary

Technical Problem

Existing glass container sealing technologies suffer from insufficient sealing and appearance durability, especially polymer sealing materials which have poor temperature resistance, and metal sealing processes which are complex and energy-intensive.

Method used

A first slurry and a second slurry composed of low softening point glass powder and solvent are used for sealing. The sealing is achieved by heating to soften the glass powder, avoiding a transition layer, simplifying the process and improving sealing performance and appearance.

Benefits of technology

It achieves a good appearance and high sealing performance for glass containers, while reducing sealing temperature and energy consumption, simplifying the process and improving the yield.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present application relates to a glass sealing material, a sealing method for a glass container, a glass product, and a tempered glass product. The glass sealing material comprises a first slurry and a second slurry. On the basis of the total mass percentage of the first slurry being 100%, the first slurry comprises: 75-90% of a first low-softening-point glass powder, and 10-25% of a first solvent. On the basis of the total mass percentage of the second slurry being 100%, the second slurry comprises: 50-75% of a second low-softening-point glass powder, and 25-50% of a second solvent. The softening temperatures of the first low-softening-point glass powder and the second low-softening-point glass powder are each independently lower than 700°C.
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Description

Glass sealing material, sealing method of glass container, glass product and tempered glass product

[0001] Cross-reference to related applications

[0002] The present disclosure is based on and claims priority to Chinese Patent Application No. 202410739622.X, filed on June 7, 2024, entitled “Glass sealing material, sealing method of glass container, glass product and tempered glass product”, the entire contents of which are incorporated herein by reference. TECHNICAL FIELD

[0003] The present application relates to the field of glass sealing, in particular to a glass sealing material, a sealing method of a glass container, a glass product and a tempered glass product. BACKGROUND

[0004] The current sealing technology of glass containers mainly includes: (1) using polymer sealing. Polymer materials can be applied to various shapes of glass containers and have good corrosion resistance. However, polymer materials have poor temperature resistance and will age after long-term use, affecting the sealing performance and appearance of the container. (2) Using metal sealing. Since the adhesion performance of metal and glass is poor when they are directly sealed, at least one or more transition layers are required in the preparation process of metal sealing, which need to have good adhesion strength with both glass and metal, so as to ensure the sealing strength of the edge. The current metal sealing process is generally carried out in two steps, first, the transition layer is pre-prepared on the glass surface and sintered at about 700 DEG C to complete the adhesion of the transition layer and the glass, and then the adhesion of the sealing metal and the transition layer is completed, thereby ensuring the air tightness and strength of the edge sealing, and the process flow is complex.

[0005] Therefore, it is urgent to provide a sealing material and a sealing method which can ensure the appearance and sealing performance of the glass container and have a simple process. SUMMARY

[0006] Based on this, some embodiments of the present application provide a glass sealing material which can ensure good appearance of the glass container and good sealing performance.

[0007] In addition, some other embodiments of the present application also provide a glass sealing method, a glass product and a tempered glass product.

[0008] A glass sealing material comprises a first slurry and a second slurry;

[0009] The first slurry comprises, based on 100% of the total mass percentage of the first slurry: 75% to 90% of a first low-softening-point glass powder and 10% to 25% of a first solvent;

[0010] the second slurry comprises, based on 100% of the total mass percentage of the second slurry, 50% to 75% of the second low-softening-point glass powder and 25% to 50% of the second solvent;

[0011] wherein the softening temperature of the first low-softening-point glass powder and the second low-softening-point glass powder is each independently less than 700℃.

[0012] In some embodiments, the first slurry comprises, based on 100% of the total mass percentage of the first slurry, 80% to 85% of the first low-softening-point glass powder and 15% to 20% of the first solvent.

[0013] In some embodiments, the second slurry comprises, based on 100% of the total mass percentage of the second slurry, 60% to 70% of the second low-softening-point glass powder and 30% to 40% of the second solvent.

[0014] In some embodiments, the average particle size of the first low-softening-point glass powder is greater than the average particle size of the second low-softening-point glass powder.

[0015] In some embodiments, the average particle size of the first low-softening-point glass powder is 0.01mm to 0.5mm, and the average particle size of the second low-softening-point glass powder is less than or equal to 0.02mm.

[0016] In some embodiments, the average particle size of the second low-softening-point glass powder is 0.001mm to 0.02mm.

[0017] In some embodiments, the first low-softening-point glass powder and the second low-softening-point glass powder each independently comprise one or more of soda-lime glass powder, silicate glass powder, phosphate glass powder, borate glass powder, bismuthate glass powder or vanadate glass powder.

[0018] In some embodiments, the first solvent and the second solvent each independently comprise one or more of ink thinner, terpineol, butyl carbitol, butyl acetate or dibutyl phthalate.

[0019] A sealing method of a glass container, comprising the following steps:

[0020] obtaining the glass sealing material described above and two glass pieces to be sealed;

[0021] applying the first slurry to the sealing area of the two glass pieces to be sealed, and applying the second slurry to the surface of the first slurry and filling the sealing area, to obtain a glass container;

[0022] heating the glass container to soften the first low softening point glass powder in the first paste and the second low softening point glass powder in the second paste to seal the glass container.

[0023] In some embodiments, one end of the to-be-sealed surface of at least one of the glass pieces is inclined relative to the other end.

[0024] The step of applying the first paste to the sealing area of the two glass pieces to be sealed and applying the second paste to the surface of the first paste to fill the sealing area to obtain the glass container comprises:

[0025] The to-be-sealed surfaces of the two glass pieces are fitted together, and a V-shaped groove is formed between the other to-be-sealed surfaces, the depth of the V-shaped groove is 0.2mm-2mm, and the opening angle of the V-shaped groove is 15°-75°.

[0026] The first paste is applied to the V-shaped groove.

[0027] The second paste is applied to the surface of the first paste to fill the V-shaped groove to obtain the glass container.

[0028] In some embodiments, the depth of the V-shaped groove is 0.3mm-1mm, and the opening angle of the V-shaped groove is 30°-60°.

[0029] In some embodiments, the peak temperature of the heating in the step of heating the glass container does not exceed 800℃.

[0030] In some embodiments, the step of heating the glass container comprises: performing a sintering treatment at 500℃-800℃ for 10min-60min.

[0031] In some embodiments, the temperature of the sintering treatment is 600℃-700℃, and the time is 20min-40min.

[0032] In some embodiments, the step of heating the glass container further comprises: performing a degassing treatment at 250℃-400℃ for 10min-60min before the sintering treatment.

[0033] In some embodiments, the temperature of the degassing treatment is 300℃-350℃, and the time is 20min-40min.

[0034] In some embodiments, the heating in the step of heating the glass container comprises one or a combination of convective heating, infrared radiation heating, microwave heating, and laser heating.

[0035] A glass product is prepared by the sealing method of the glass container.

[0036] A tempered glass product is prepared by tempering the glass product.

[0037] The glass sealing material includes a first paste and a second paste, both of which include low-softening-point glass powder. The use of low-softening-point glass powder for sealing helps to reduce the sealing temperature, so that the glass container is less likely to deform and the appearance is good. In addition, the first paste has a high content of low-softening-point glass powder, so that the first paste has almost no flowability, so that the first paste does not flow into the glass container during sealing and affect the appearance of the glass container. The second paste has a low content of low-softening-point glass powder and has a certain flowability, so that it can fill the micropores of the first paste and improve the sealing performance and appearance. Therefore, in some embodiments of the present application, low-softening-point glass powder is used as the sealing material, and the first paste and the second paste are optimized for sealing, so that the glass container has a good appearance and good sealing performance.

[0038] The sealing method of the glass container provided in some embodiments of the present application uses the above-mentioned glass sealing material for sealing. The first paste is applied to the sealing area of the two glass pieces to be sealed, and the second paste is applied to the surface of the first paste and fills the sealing area. The first paste is first applied to the sealing area, and since the first paste has almost no flowability, the paste does not flow into the glass container. The second paste is then applied to the surface of the first paste, and the second paste can fill the micropores of the first paste, which helps to improve the sealing performance and appearance. In addition, the sealing method of the glass container uses glass powder as the sealing material, which is simpler than the metal sealing method and does not require a transition layer. BRIEF DESCRIPTION OF DRAWINGS

[0039] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the following will briefly introduce the drawings needed in the embodiment description. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative labor.

[0040] FIG. 1 is a process flow diagram of a glass sealing method according to some embodiments of the present application;

[0041] FIG. 2 is a schematic diagram of a glass piece in step S110 of the process flow diagram shown in FIG. 1;

[0042] FIG. 3 is a schematic diagram of step S120 of the process flow diagram shown in FIG. 1;

[0043] FIG. 4 is a schematic diagram showing the depth of the V-shaped groove and the opening angle;

[0044] FIG. 5 is a schematic diagram of a glass sealing process in some embodiments of the present application. DETAILED DESCRIPTION

[0045] For the purpose of understanding the present application, a more complete description of the present application will be rendered by reference to specific embodiments thereof which are shown in the accompanying drawings. The preferred embodiments of the present application are shown in the drawings as follows:

[0046] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used in the description herein is for describing specific embodiments only and is not intended to be limiting of the present application. As used herein, the term "and / or" includes any and all combinations of one or more of the associated listed items.

[0047] Unless otherwise indicated, or unless the context clearly indicates otherwise, terms or phrases used in this application have the following meanings:

[0048] In the present application, "first", "second" are used only for the purpose of description, and can not be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined with "first", "second" can explicitly or implicitly include at least one of the features.

[0049] In the description of the present application, "a plurality of" means at least two, for example, two, three, etc., unless otherwise specifically limited.

[0050] In the present application, "one or more" refers to any one, any two or any two or more of the listed items. Among them, "several" refers to any two or more.

[0051] In the present application, the percentage concentration involved, unless otherwise specified, refers to the final concentration. The final concentration refers to the proportion of the added ingredient in the system after the ingredient is added.

[0052] The word "optionally" and the like in the present application means that the embodiments of the present application can provide certain beneficial effects in some cases. However, in the same or other cases, other embodiments can also be optional. In addition, the description of one or more optional embodiments does not imply that other embodiments are not available, nor is it intended to exclude other embodiments from the scope of the present application.

[0053] When a range of values is disclosed, the disclosure is intended to encompass the end points of the range as well as each and every intervening value. Further, when a range of values is provided, it is intended to encompass all ranges of values whether the stated range is explicitly recited or not. Additionally, it is intended that when a limit of a range is stated, e.g., 7-9, that any number falling within the range is also specifically recited. Further, it is intended that when a range of values is provided, it is intended to encompass any and all sub-ranges of values falling within the range, even if the sub-range is not explicitly recited. The disclosure of a single value of a parameter or characteristic, however, is intended to encompass at least that single value, as well as any and all sub-ranges of the value unless otherwise indicated.

[0054] In the present application, the technical features described in an open way include both the closed technical solutions consisting of the listed features and the open technical solutions containing the listed features.

[0055] The terms "comprises", "comprising", "includes", "including", "has", "having" and their conjugates, as used herein, are intended to cover the meaning of "consists of, "consisting of", "consists essentially of", and "consisting essentially of", as well as the meaning of "includes", "including", "has", "having", "comprises", "comprising", "is" and "are", "are" and "is" when used in a listing of elements or components.

[0056] Reference throughout this specification to "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment can be included in at least one embodiment of the application. The appearances of the phrase "in an embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are they necessarily mutually exclusive of one another. It is expressly understood that any of the embodiments described herein can be combined with any of the other embodiments unless explicitly stated otherwise.

[0057] A first aspect of the present application provides a glass sealing material, comprising a first slurry and a second slurry;

[0058] The first slurry comprises, with the total mass percentage of the first slurry being 100%, 75%-90% of a first low softening point glass powder and 10%-25% of a first solvent;

[0059] The second slurry comprises, with the total mass percentage of the second slurry being 100%, 50%-75% of a second low softening point glass powder and 25%-50% of a second solvent;

[0060] The softening temperature of the first low softening point glass powder and the second low softening point glass powder is independently less than 700°C.

[0061] Optionally, the softening temperature of the first low softening point glass powder and the second low softening point glass powder is independently less than 500°C, and the sintering has less impact on the shape of the container when the softening point temperature of the glass powder is lower.

[0062] In some embodiments, when the glass sealing material is used to seal glass, the softening temperature of the first low softening point glass powder and the second low softening point glass powder is lower than the Tg (glass transition temperature) of the glass to be sealed.

[0063] In this context, the softening temperature has the same meaning as the softening point, which refers to the temperature at which a material begins to soften and lose its strength under certain conditions.

[0064] In some embodiments, the first low softening point glass powder and the second low softening point glass powder each independently comprises one or more of a soda-lime glass powder, a silicate glass powder, a phosphate glass powder, a borate glass powder, a bismuthate glass powder, and a vanadate glass powder. It can be understood that the first low softening point glass powder can be the same as or different from the second low softening point glass powder, as long as each of them has a softening temperature lower than 700°C. In one example, the first low softening point glass powder is a soda-lime glass powder, and the second low softening point glass powder is a borate glass powder. In another example, the first low softening point glass powder and the second low softening point glass powder are both borate glass powders. In yet another example, the first low softening point glass powder and the second low softening point glass powder are both a mixture of borate glass powders and bismuthate glass powders.

[0065] In some embodiments, the first solvent and the second solvent each independently comprises one or more of an ink thinner, a terpineol, a butyl carbitol, a butyl acetate, and a dibutyl phthalate. It can be understood that the first solvent and the second solvent can be the same or different, and are not particularly limited.

[0066] In one example, in the first slurry, the mass percentage of the first low softening point glass powder and the first solvent can be, but is not limited to, 75% and 25%, 78% and 22%, 80% and 20%, 81% and 19%, 82% and 18%, 83% and 17%, 84% and 16%, 85% and 15%, 86% and 14%, 88% and 12%, 90% and 10%. Alternatively, the first slurry comprises, by mass percentage, 80%-85% of the first low softening point glass powder and 15%-20% of the first solvent. Further, the first slurry consists of, by mass percentage, 80%-85% of the first low softening point glass powder and 15%-20% of the first solvent.

[0067] In one example, the mass percentage of the second low softening point glass powder and the second solvent in the second slurry can be, but not limited to, 50% and 50%, 55% and 45%, 58% and 42%, 60% and 40%, 62% and 38%, 64% and 36%, 66% and 34%, 68% and 32%, 70% and 30%, 72% and 28%, 75% and 25%. Alternatively, the second slurry comprises, by mass percentage, 60% to 70% of the second low softening point glass powder and 30% to 40% of the second solvent. Further, the second slurry consists of, by mass percentage, 60% to 70% of the second low softening point glass powder and 30% to 40% of the second solvent.

[0068] It can be understood that, since the first slurry is different from the second slurry, when the mass percentage of the first low softening point glass powder in the first slurry is 75%, the mass percentage of the second low softening point glass powder in the second slurry cannot be 75%, i.e. less than 75%. Therefore, the above implies that the mass percentage of the first low softening point glass powder in the first slurry is greater than the mass percentage of the second low softening point glass powder in the second slurry.

[0069] In some embodiments, the glass sealing material comprises the first slurry and the second slurry, the first slurry comprises, by total mass percentage of the first slurry, 75% to 90% of the first low softening point glass powder and 10% to 25% of the first solvent, and the second slurry comprises, by total mass percentage of the second slurry, 60% to 70% of the second low softening point glass powder and 30% to 40% of the second solvent.

[0070] In other embodiments, the glass sealing material comprises the first slurry and the second slurry, the first slurry comprises, by total mass percentage of the first slurry, 80% to 85% of the first low softening point glass powder and 15% to 20% of the first solvent, and the second slurry comprises, by total mass percentage of the second slurry, 50% to 75% of the second low softening point glass powder and 25% to 50% of the second solvent.

[0071] In yet other embodiments, the glass sealing material comprises the first slurry and the second slurry, the first slurry comprises, by total mass percentage of the first slurry, 80% to 85% of the first low softening point glass powder and 15% to 20% of the first solvent, and the second slurry comprises, by total mass percentage of the second slurry, 60% to 70% of the second low softening point glass powder and 30% to 40% of the second solvent.

[0072] In some embodiments, the glass sealing material is composed of a first paste and a second paste, the first paste is composed of a first low softening point glass powder and a first solvent, and the second paste is composed of a second low softening point glass powder and a second solvent. The glass sealing material is composed of a low softening point glass powder and a solvent without introducing metal materials or other substances, which can improve the appearance transparency of the glass container, and the pure glass composition does not affect the use range of the glass container. After the sealing of the glass container is completed, the glass container can be tempered to improve the glass strength, and the stress consumption of the sealing process on the glass container does not need to be considered. In addition, the metal sealing process is generally carried out in two steps. First, a transition layer is pre-prepared on the surface of the glass, and sintering is performed at about 700°C to complete the bonding of the transition layer and the glass. Then, the bonding of the sealing metal and the transition layer is completed, thereby ensuring the air tightness and strength of the edge sealing. The process flow is complex, the yield is low, and the energy consumption of repeated temperature rising and falling is large. In some embodiments of the present application, the glass sealing material includes a low softening point glass powder and a solvent. Compared with metal sealing, the sealing process is less, and the cost rate is high. Repeated temperature rising and falling is not required, and the energy consumption is reduced.

[0073] In some embodiments, the average particle size of the first low softening point glass powder is greater than the average particle size of the second low softening point glass powder. During sealing, the first paste is used to fill the sealing area of the two glass pieces to be sealed, and the second paste is coated on the surface of the first paste. By setting the average particle size of the first low softening point glass powder to be greater than the average particle size of the second low softening point glass powder, the second paste is further filled in the first paste, and the sealing performance is improved.

[0074] In some embodiments, the average particle size of the first low softening point glass powder in the first paste is 0.01 mm to 0.5 mm. For example, the average particle size of the first low softening point glass powder can be, but is not limited to, 0.01 mm, 0.05 mm, 0.1 mm, 0.15 mm, 0.2 mm, 0.25 mm, 0.3 mm, 0.35 mm, 0.4 mm, 0.45 mm, 0.5 mm, or a range formed by any two of these values. By setting the above, the flowability of the first paste is further reduced, the flow into the interior of the glass container is avoided, and the appearance of the glass container is affected. At the same time, the sintering temperature is reduced, and the appearance of the glass container after sintering is improved.

[0075] Optionally, in the second slurry, the average particle size of the second low softening point glass powder is less than or equal to 0.02 mm. For example, the average particle size of the second low softening point glass powder can be, but is not limited to, 0.001 mm, 0.002 mm, 0.005 mm, 0.008 mm, 0.01 mm, 0.012 mm, 0.015 mm, 0.018 mm, 0.02 mm, or a range between any two of these values. Optionally, in the second slurry, the average particle size of the second low softening point glass powder is 0.001 mm to 0.02 mm. By setting the above, the second slurry is further facilitated to fill the pores of the first slurry, and the surface of the first slurry is smoothed, so as to further improve the appearance and sealing performance of the sealing part.

[0076] It can be understood that the first slurry and the second slurry are independent of each other before being used for sealing.

[0077] The second aspect of the present application provides a glass sealing method, comprising the following steps:

[0078] obtaining the glass sealing material and the two glass pieces to be sealed as described above;

[0079] applying the first slurry to the sealing area of the two glass pieces to be sealed, and applying the second slurry to the surface of the first slurry and filling the sealing area, to obtain a glass container;

[0080] heating the glass container, so that the first low softening point glass powder in the first slurry and the second low softening point glass powder in the second slurry are softened to seal the glass container.

[0081] In some embodiments, the softening temperature of the first low softening point glass powder and the second low softening point glass powder is lower than the Tg (glass transition temperature) of the glass pieces.

[0082] The glass container sealing method provided by some embodiments of the present application uses the above-mentioned glass sealing material for sealing, and the first slurry and the second slurry are sequentially applied to the sealing area of the two glass pieces to be sealed, so that the second slurry is applied to the surface of the first slurry and fills the sealing area. The first slurry is applied to the sealing area first, and since the first slurry has almost no flowability, the slurry will not flow into the interior of the glass container. Then the second slurry is applied to the surface of the first slurry, and the second slurry can fill the micropores of the first slurry, which is conducive to improving the sealing performance and appearance. In addition, the glass container sealing method uses glass powder as the sealing material, which is simpler than the metal sealing method and does not need to set a transition layer.

[0083] In some embodiments, one end of the sealing surface of at least one glass piece is inclined relative to the other end.

[0084] The step of applying the first paste to the sealing area of the two glass pieces to be sealed and applying the second paste to the surface of the first paste to fill the sealing area to obtain the glass container comprises:

[0085] The part of the two glass pieces to be sealed is abutted, and a V-shaped groove is formed between the other part of the two glass pieces to be sealed, the depth of the V-shaped groove is 0.2mm-2mm, and the opening angle of the V-shaped groove is 15°-75°.

[0086] The first paste is applied to the V-shaped groove.

[0087] The second paste is applied to the surface of the first paste to fill the V-shaped groove to obtain the glass container.

[0088] Specifically, in some embodiments, referring to FIG. 1, the glass sealing method comprises the following steps:

[0089] Step S110: obtaining the glass sealing material and the two glass pieces to be sealed, and at least one end of the glass piece to be sealed is inclined relative to the other end.

[0090] Specifically, referring to FIG. 2, the glass piece has a sealing surface, and the first end 202 of the sealing surface is inclined relative to the second end 204.

[0091] Step S120: abutting the part of the two glass pieces to be sealed, and forming a V-shaped groove between the other part of the two glass pieces to be sealed to obtain the glass container, the depth of the V-shaped groove is 0.2mm-2mm, and the opening angle of the V-shaped groove is 15°-75°.

[0092] In some embodiments, one end of the glass piece to be sealed is inclined relative to the other end. The inclined surface has a depth of 0.2mm-2mm and an inclination angle of 7.5°-37.5°. Through the above arrangement, when the two glass pieces are in contact, the V-shaped groove formed has a depth of 0.2mm-2mm and an opening angle of 15°-75°. Optionally, the inclined surface of the glass piece has a depth of 0.3mm-1mm and an inclination angle of 15°-30°. The V-shaped groove formed has a depth of 0.3mm-1mm and an opening angle of 30°-60°.

[0093] In some embodiments, the thickness of the glass piece is 2mm-4mm. The thickness of the glass piece is too thin to be suitable for a glass container. Under the above thickness of the glass piece, the depth of the V-shaped groove is 0.2mm-2mm, which can make the sealing size as small as possible without affecting the sealing effect and reduce the influence on the appearance of the sealed glass product.

[0094] Please refer to Fig. 3 for a schematic diagram of step S120. In Fig. 3, each glass piece has a to-be-sealed surface, and the first end 202 of the to-be-sealed surface is inclined relative to the second end 204. In step S120, part of the to-be-sealed surface of one glass piece is attached to part of the to-be-sealed surface of another glass piece, i.e., one glass piece is attached to another glass piece in a plane in which the second end 204 of the to-be-sealed surface of one glass piece is located and a plane in which the second end 204 of the to-be-sealed surface of another glass piece is located, and a V-shaped groove is formed between the planes in which the first ends 202 of the two glass pieces are located.

[0095] In some embodiments, the glass pieces to be sealed are processed by a Computerized Numerical Control (CNC) method so that one end of the to-be-sealed surface is inclined relative to the other end. The CNC processing includes two steps of roughing and finishing. In a specific example, in the roughing step, the rotating speed of the cutter wheel is 18000 r / min-22000 r / min, the feed rate is 0.9 m / min-1 m / min, and the cutting depth is 0.08 mm-0.11 mm. In the finishing step, the rotating speed of the cutter wheel is 22000 r / min-25000 r / min, the feed rate is 0.6 m / min-0.9 m / min, and the cutting depth is 0.03 mm-0.08 mm. It can be understood that the above only gives a more specific CNC processing method, but is not limited thereto, and other methods that can process the glass into an inclined surface and meet the above-mentioned angle and depth can also be used.

[0096] Optionally, the depth of the V-shaped groove is 0.2 mm-2 mm, and the opening angle is 15°-75°. For example, the depth of the V-shaped groove can be, but is not limited to, 0.2 mm, 0.3 mm, 0.5 mm, 0.6 mm, 0.7 mm, 0.8 mm, 0.9 mm, 1 mm, 1.2 mm, 1.5 mm, 1.8 mm, 2 mm, or a range formed by any two of these values. Optionally, the depth of the V-shaped groove is 0.3 mm-1 mm. For example, the opening angle of the V-shaped groove can be, but is not limited to, 15°, 20°, 25°, 30°, 35°, 40°, 45°, 50°, 55°, 60°, 65°, 70°, 75°, or a range formed by any two of these values. Optionally, the opening angle of the V-shaped groove is 30°-60°.

[0097] In some embodiments, the depth of the V-shaped groove is 0.2 mm-2 mm, and the opening angle is 30°-60°. In other embodiments, the depth of the V-shaped groove is 0.3 mm-1 mm, and the opening angle is 15°-75°. In yet other embodiments, the depth of the V-shaped groove is 0.3 mm-1 mm, and the opening angle is 30°-60°.

[0098] It can be understood that the depth of the V-shaped groove refers to the distance between the opening of the V-shaped groove and the bottom of the V-shaped groove. For details, refer to FIG. 4, in which h represents the depth of the V-shaped groove, and a represents the opening angle of the V-shaped groove.

[0099] Optionally, the glass piece to be sealed can be a glass container of various shapes, such as a cuboid, a sphere, etc.

[0100] Step S130: applying the first slurry into the V-shaped groove.

[0101] In some embodiments, the first slurry is applied into the V-shaped groove using a spatula.

[0102] In some embodiments, the thickness of the first slurry accounts for 50% to 95% of the depth of the V-shaped groove. For example, the thickness of the first slurry can account for 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, or a range formed by any two of these values, but is not limited thereto. Optionally, the thickness of the first slurry accounts for 90% to 95% of the depth of the V-shaped groove. It can be understood that the thickness of the first slurry refers to the thickness in the depth direction of the V-shaped groove.

[0103] Step S140: applying the second slurry to the surface of the first slurry and filling the V-shaped groove.

[0104] In some embodiments, the second slurry is applied to the surface of the first slurry using a syringe. Specifically, the needle opening of the syringe has a diameter of 0.4 mm to 0.8 mm.

[0105] In some embodiments, after the second slurry is applied to the surface of the first slurry, 1 min to 5 min is waited, and then the surface is wiped clean. Through the above arrangement, it is beneficial to make the second slurry fully fill the first slurry, and further improve the appearance and sealing performance of the glass.

[0106] Step S150: heating the glass container to make the first low-softening-point glass powder in the first slurry and the second low-softening-point glass powder in the second slurry soften to seal the glass container.

[0107] In some embodiments, in the step of heating the glass container, the peak temperature of the heating does not exceed 800°C. At the above heating temperature, the low-softening-point glass powder can be softened, while the glass container is not deformed. Optionally, in the step of heating the glass container, the peak temperature of the heating is 500°C to 800°C. Further, the peak temperature of the heating is 600°C to 700°C.

[0108] In some embodiments, the step of heating the glass container includes: performing sintering treatment at 500°C to 800°C for 10 min to 60 min.

[0109] Specifically, the temperature of the sintering process is 500-800°C. For example, the temperature of the sintering process can be, but is not limited to, 500°C, 550°C, 600°C, 650°C, 700°C, 750°C, 800°C, or a range defined by any two of these values. Alternatively, the temperature of the sintering process is 600-700°C.

[0110] Specifically, the time of the sintering process is 10-60 min. For example, the sintering time can be, but is not limited to, 10 min, 15 min, 20 min, 25 min, 30 min, 35 min, 40 min, 45 min, 50 min, 55 min, 60 min, or a range defined by any two of these values. Alternatively, the sintering time is 20-40 min.

[0111] Further, the step of heating the glass container comprises a sintering process at 600-700°C for 10-60 min.

[0112] In some embodiments, the heating rate in the sintering process is 0.2-20°C / min. For example, the heating rate can be, but is not limited to, 0.2°C / min, 1°C / min, 2°C / min, 5°C / min, 6°C / min, 7°C / min, 8°C / min, 9°C / min, 10°C / min, 12°C / min, 15°C / min, 18°C / min, 20°C / min, or a range defined by any two of these values. Alternatively, the heating rate in the sintering process is 5-10°C / min. With the above heating rate, the overall integrity of the glass container and the stress relief effect are ensured, and further optimization of the heating rate can further ensure that the glass container does not break due to thermal shock.

[0113] In some embodiments, the cooling rate in the sintering process is 0.2-10°C / min. For example, the cooling rate can be, but is not limited to, 0.2°C / min, 0.5°C / min, 1°C / min, 2°C / min, 3°C / min, 4°C / min, 5°C / min, 6°C / min, 8°C / min, 10°C / min, or a range defined by any two of these values. Alternatively, the cooling rate in the sintering process is 0.5-5°C / min. With the above cooling rate, the stress is further relieved and the glass container is ensured not to break.

[0114] In some embodiments, the heating the glass container further comprises: performing a degassing treatment at 250-400 °C for 10-60 min before the sintering process. Specifically, the degassing temperature is 250-400 °C. For example, the degassing temperature can be, but is not limited to, 250 °C, 280 °C, 300 °C, 310 °C, 320 °C, 330 °C, 340 °C, 350 °C, 360 °C, 380 °C, 400 °C, or a range between any two of these values. Alternatively, the degassing temperature is 300-350 °C. The degassing time is 10-60 min. For example, the degassing time can be, but is not limited to, 10 min, 15 min, 20 min, 22 min, 25 min, 28 min, 30 min, 32 min, 35 min, 38 min, 40 min, 50 min, 60 min, or a range between any two of these values. Alternatively, the degassing time is 20-40 min.

[0115] Further, the heating the glass container further comprises: performing a degassing treatment at 300-350 °C for 20-40 min before the sintering process.

[0116] In some embodiments, the heating rate in the degassing treatment is 0.2-20 °C / min. For example, the heating rate can be, but is not limited to, 0.2 °C / min, 1 °C / min, 2 °C / min, 5 °C / min, 6 °C / min, 7 °C / min, 8 °C / min, 9 °C / min, 10 °C / min, 12 °C / min, 15 °C / min, 18 °C / min, 20 °C / min, or a range between any two of these values. Alternatively, the heating rate in the degassing treatment is 5-10 °C / min.

[0117] In some embodiments, the cooling rate in the degassing treatment is 0.2-10 °C / min. For example, the cooling rate can be, but is not limited to, 0.2 °C / min, 0.5 °C / min, 1 °C / min, 2 °C / min, 3 °C / min, 4 °C / min, 5 °C / min, 6 °C / min, 8 °C / min, 10 °C / min, or a range between any two of these values. Alternatively, the cooling rate in the degassing treatment is 0.5-5 °C / min.

[0118] It can be understood that, in some embodiments, the glue removal treatment and the sintering treatment can be performed in steps, i.e., first heating to the glue removal temperature, performing the glue removal treatment at the glue removal temperature, then heating to the sintering treatment temperature after the glue removal treatment, performing the sintering treatment at the sintering treatment temperature, and then cooling after the sintering treatment. In other embodiments, the glue removal treatment and the sintering treatment can also be combined, i.e., heating at a certain heating rate, so that the glue removal treatment is performed simultaneously during the heating process, and then heating to the sintering treatment temperature, performing the sintering treatment at the sintering treatment temperature, and then cooling after the sintering treatment. The above two methods do not affect the implementation effect of the present application.

[0119] In some embodiments, the heating method includes one or a combination of several ways of convection heating, infrared radiation heating, microwave heating, and laser heating.

[0120] In some embodiments, in step S150, the glass piece is placed in a horizontal position, an inverted position, or supported by a high-temperature resistant rack.

[0121] The sealing method of the glass container provided by some embodiments of the present application forms a V-shaped groove between the glass pieces to be sealed, which facilitates the embedding of the paste into the sealing part. The first paste is applied in the V-shaped groove, and since the first paste has almost no flowability, the paste will not flow into the interior of the glass container. The second paste is then applied on the surface of the first paste, and the second paste can fill the micropores of the first paste, which facilitates the improvement of the sealing performance. Through the design of the V-shaped groove structure and the cooperation with the paste, the paste in the V-shaped groove is a thin line after sintering, which does not affect the overall appearance of the glass container and ensures the sealing performance.

[0122] In addition, the sealing method of the glass container solves the problems of complex process flow, high energy consumption, environmental pollution, and influence on glass stress in the conventional sealing method using metal as the sealing material, and has the advantages of simple process flow, environmental protection and energy saving, and the ability to strengthen the glass container after sealing.

[0123] FIG. 1 is a flowchart of the sealing method of the glass container according to an embodiment of the present application. It should be understood that, although each step in the flowchart shown in FIG. 1 is displayed in sequence according to the arrow, these steps are not necessarily performed in the order indicated by the arrow, unless otherwise specified herein. The execution of these steps is not necessarily limited in sequence, and they can be executed in other orders. At least part of the steps in FIG. 1 can include multiple sub-steps or multiple stages, which are not necessarily executed at the same time, but can be executed at different times. The execution sequence is not necessarily sequential, but can be executed in rotation or alternation with at least part of other steps or other sub-steps or stages.

[0124] Referring to Fig. 5, which is a schematic diagram of the sealing process of the glass container, in Fig. 5, 14 is the V-shaped groove backfilled with glass powder. It can be understood that the glass piece used in Fig. 5 is a double-layer glass, so the partial enlarged view is the V-shaped groove part of the entire glass container end face, and the flatly attached part is not shown, and there will be a part of the other glass inside. In other embodiments, the glass piece is a single-layer glass, and the end face of the sealing part shows not only the V-shaped groove part but also the flatly attached part.

[0125] The third aspect of the present application provides a glass product prepared by the sealing method of the glass container of the second aspect.

[0126] The glass product has good appearance and good sealing performance.

[0127] The fourth aspect of the present application provides a tempered glass product obtained by tempering the glass product of the third aspect.

[0128] The existing glass sealing method is difficult to be tempered after the glass is sealed, so it is mostly sealed after the glass is tempered, but high-temperature sealing will dissipate the stress of the glass, affecting the strength of the glass. The sealing method of the glass described above uses glass powder as the sealing material, which can be tempered after sealing to prepare tempered glass and improve the strength of the glass, while avoiding the stress dissipation caused by tempering before sealing.

[0129] It can be understood that the specific tempering process can be commonly used in the art, which is not particularly limited here.

[0130] In order to make the purpose and advantages of the present application clearer, the glass sealing method and its effects of the present application will be further described in detail below in combination with specific examples. It should be understood that the specific examples described herein are only used to explain the present application and should not be used to limit the present application. The following examples do not include other components except unavoidable impurities if not specifically stated. The materials and instruments used in the examples are commonly selected in the art if not specifically stated. The experimental methods not specified in the examples are implemented according to the conventional conditions, such as the conditions described in the literature, books or the methods recommended by the manufacturer.

[0131] The low-softening-point glass powder used in the following examples and comparative examples is as follows: the softening temperature of the soda-lime glass powder is 554℃; the softening temperature of the borate glass powder is 510℃; the softening temperature of the bismuthate glass powder is 520℃. The borate glass powder + bismuthate glass powder refers to a mixture of borate glass powder and bismuthate glass powder, and the mass ratio of the two is 1:1. The solvent used in the first slurry and the second slurry is ink thinner. The glass piece used in the examples is high-alumina silicate glass.

[0132] Examples 1-8

[0133] Embodiments 1-8 each provide a glass sealing method, comprising the following steps:

[0134] (1) The first slurry and the second slurry are prepared according to the compositions and solid contents of the first slurry and the second slurry in Table 1, wherein the solid content refers to the content of the low-softening-point glass powder in the first slurry or the second slurry, and the remaining part is the solvent.

[0135] (2) Two glass pieces to be sealed are obtained, one end of the sealing surface of each glass piece is inclined relative to the other end, part of the sealing surface of each glass piece is attached, and a V-shaped groove is formed between the other part of the sealing surface, thereby obtaining a glass container, the depth and opening angle of the V-shaped groove are shown in Table 1.

[0136] (3) The first slurry is applied to the V-shaped groove using a scraper, the thickness of the first slurry accounts for 95% of the depth of the V-shaped groove, the second slurry is injected onto the surface of the first slurry and fills the V-shaped groove using a syringe, after the injection is completed, 3 minutes are waited, and then the surface of the glass container is wiped clean.

[0137] (4) The glass container wiped clean is placed upside down in a muffle furnace, and the degassing and sintering are performed according to the temperature processes in Table 1, respectively.

[0138] Table 1

[0139] Comparative Examples 1-12

[0140] Comparative Examples 1-12 each provide a glass sealing method, comprising the following steps:

[0141] (1) The first slurry and the second slurry are prepared according to the compositions and solid contents of the first slurry and the second slurry in Table 2, wherein the solid content refers to the content of the low-softening-point glass powder in the first slurry or the second slurry, and the remaining part is the solvent.

[0142] (2) Two glass pieces to be sealed are obtained, one end of the sealing surface of each glass piece is inclined relative to the other end, part of the sealing surface of each glass piece is attached, and a V-shaped groove is formed between the other part of the sealing surface, thereby obtaining a glass container, the depth and opening angle of the V-shaped groove are shown in Table 2.

[0143] (3) The first slurry is applied to the V-shaped groove using a scraper, the thickness of the first slurry accounts for 95% of the depth of the V-shaped groove, the second slurry is injected onto the surface of the first slurry and fills the V-shaped groove using a syringe, after the injection is completed, 3 minutes are waited, and then the surface of the glass container is wiped clean.

[0144] (4) The cleaned glass container was placed upside down in a muffle furnace, and degassing and sintering were performed according to the temperature process in Table 2.

[0145] Table 2

[0146] The glass products prepared by the glass sealing methods of the above examples and comparative examples were tested, as follows:

[0147] 1. Sealing place transmittance test

[0148] According to GB / T 5433-2008, a transmittance tester (VMS-1S) was used to test the sealing place of the glass products prepared by the glass sealing methods of the above examples and comparative examples. The scanning wavelength range was 400nm-900nm, and the transmittance of the sealing place of the glass product at 550nm was recorded.

[0149] 2. Glass bottle airtightness test

[0150] According to GB / T 13521, an intelligent sealing instrument (MFY-06S) was used to test the sealing of the glass products prepared by the glass sealing methods of the above examples and comparative examples. Specifically, a gas gun was used to blow the outer sealing place of the glass product filled with water, and if bubbles were observed, i.e. water leakage or air leakage, the sealing test was unqualified, otherwise, the sealing test was qualified.

[0151] The test results of the glass products prepared by the glass sealing methods of the above examples and comparative examples are shown in Table 3 below.

[0152] Table 3

[0153] In Table 3, OK indicates that the sealing test is qualified, NG indicates that the sealing test is unqualified, and complete sealing is not achieved.

[0154] As can be seen from Table 3, the sealing place of the glass products prepared by the glass sealing methods of Examples 1-8 has a transmittance of 85%-90% at 550nm, has a good appearance, and all achieve sealing of the glass container.

[0155] As can be seen from the comparison of Comparative Example 1-Comparative Example 2 and Example 1, if the content of the first low-softening-point glass powder in the first slurry is too high or too low, the transmittance of the sealing part of the prepared glass product is low, which affects the appearance of the glass product. As can be seen from the comparison of Comparative Example 3-Comparative Example 4 and Example 1, if the content of the second low-softening-point glass powder in the second slurry is too high or too low, the transmittance of the sealing part of the prepared glass product is low, which affects the appearance of the glass product, and when the content of the second low-softening-point glass powder is high, the packaging effect is also affected. As can be seen from the comparison of Comparative Example 5-Comparative Example 6 and Example 1, if the depth of the V-shaped groove is too low, although the transmittance of the sealing part of the prepared glass product is good, the sealing performance is unqualified and complete sealing is not achieved; if the depth of the V-shaped groove is too large, although the sealing performance is good, the transmittance is low, which affects the appearance of the glass product. As can be seen from the comparison of Comparative Example 7-Comparative Example 8 and Example 1, if the degassing temperature is too low or too high, the transmittance of the sealing part of the prepared glass product is affected, and the appearance of the prepared glass product is poor. As can be seen from the comparison of Comparative Example 9-Comparative Example 10 and Example 1, if the sintering temperature is too low, the transmittance of the sealing part of the prepared glass product is low, which makes the appearance of the prepared glass product poor, and at the same time, the sealing performance is poor and complete sealing is not achieved; if the sintering temperature is too high, although complete sealing is achieved, the prepared glass product is deformed due to the too high sealing temperature. As can be seen from the comparison of Comparative Example 11 and Example 1, if the angle of the V-shaped groove is too large, the appearance and transmittance of the sealing part are affected. As can be seen from the comparison of Comparative Example 12 and Example 1, if the average particle size of the first low-softening-point glass powder in the first slurry is too large, the transmittance of the glass product is affected, which makes the appearance of the prepared glass product poor, and at the same time, the sealing performance is poor.

[0156] The technical features of the above-described embodiments can be combined in any manner. In order to make the description concise, all possible combinations of the technical features in the above-described embodiments are not described, but it should be considered that any combination of the technical features is within the scope of the present disclosure.

[0157] The above-described embodiments only express several implementation manners of the present application, facilitate specific and detailed understanding of the technical solutions of the present application, but should not be considered as limiting the protection scope of the patent. It should be pointed out that, for ordinary skilled persons in the art, some modifications and improvements can be made without departing from the concept of the present application, and these all belong to the protection scope of the present application. It should be understood that, the technical solutions obtained by ordinary skilled persons in the art through logical analysis, reasoning or limited experiments on the basis of the technical solutions provided by the present application all belong to the protection scope of the appended claims of the present application. Therefore, the protection scope of the patent of the present application should be subject to the contents of the appended claims, and the description and drawings can be used to explain the contents of the claims. Industrial applicability

[0158] The embodiments of the present disclosure provide a glass sealing material. In the glass sealing material of the present disclosure, a low softening point glass powder is used as a sealing material, and through optimization of a first slurry and a second slurry, the glass container has a good appearance and good sealing performance when used for sealing.

Claims

1. A glass sealing material, comprising a first paste and a second paste; the first paste comprises, with the total mass percentage of the first paste being 100%, 75%-90% of a first low-softening-point glass powder and 10%-25% of a first solvent; the second paste comprises, with the total mass percentage of the second paste being 100%, 50%-75% of a second low-softening-point glass powder and 25%-50% of a second solvent; wherein the softening temperature of the first low-softening-point glass powder and the second low-softening-point glass powder is independently less than 700℃.

2. The glass seal material of claim 1, wherein, the first paste comprises, with the total mass percentage of the first paste being 100%, 80%-85% of a first low-softening-point glass powder and 15%-20% of a first solvent.

3. The glass seal material of claim 1 or 2, wherein, the second paste comprises, with the total mass percentage of the second paste being 100%, 60%-70% of a second low-softening-point glass powder and 30%-40% of a second solvent.

4. The glass seal material of any one of claims 1-3, wherein, the average particle size of the first low-softening-point glass powder is greater than the average particle size of the second low-softening-point glass powder.

5. The glass seal material of any one of claims 1-4, wherein, the average particle size of the first low-softening-point glass powder is 0.01mm-0.5mm, and the average particle size of the second low-softening-point glass powder is less than or equal to 0.02mm.

6. The glass seal material of any one of claims 1-5, wherein, the first low-softening-point glass powder and the second low-softening-point glass powder independently comprise one or more of a soda-lime glass powder, a silicate glass powder, a phosphate glass powder, a borate glass powder, a bismuthate glass powder or a vanadate glass powder.

7. The glass seal material of any one of claims 1-6, wherein, the first solvent and the second solvent independently comprise one or more of an ink thinner, a terpineol, a butyl carbitol, a butyl acetate or a dibutyl phthalate. 8.A sealing method of a glass container, comprising the following steps: obtaining the glass sealing material according to any one of claims 1-7 and two glass pieces to be sealed; applying the first paste to the sealing area of the two glass pieces to be sealed, and applying the second paste to the surface of the first paste and filling the sealing area to obtain a glass container; heating the glass container to soften the first low-softening-point glass powder in the first paste and the second low-softening-point glass powder in the second paste to seal the glass container.

9. The method of sealing a glass container of claim 8, wherein, one end of the sealing surface of at least one of the glass pieces is inclined relative to the other end; the step of applying the first paste to the sealing area of the two glass pieces to be sealed, and applying the second paste to the surface of the first paste and filling the sealing area to obtain a glass container comprises: adhering part of the sealing surface of the two glass pieces, and forming a V-shaped groove between the other part of the sealing surface, the depth of the V-shaped groove is 0.2mm-2mm, and the opening angle is 15°-75°; applying the first paste to the V-shaped groove; applying the second paste to the surface of the first paste and filling the V-shaped groove to obtain a glass container.

10. The method of sealing a glass container of claim 9, wherein, the depth of the V-shaped groove is 0.3mm-1mm, and the opening angle is 30°-60°.

11. The method of sealing a glass container according to any one of claims 8 to 10, wherein, in the step of heating the glass container, the peak temperature of the heating is not more than 800℃.

12. The method of sealing a glass container according to any one of claims 8 to 11, wherein, The step of heating the glass container comprises sintering treatment at 500-800℃ for 10-60 minutes.

13. The method of sealing a glass container of claim 12, wherein, The step of heating the glass container further comprises degassing treatment at 250-400℃ for 10-60 minutes before the sintering treatment.

14. A glass article prepared by the sealing method of any one of claims 8-13.

15. A tempered glass article prepared by tempering the glass article of claim 14.

Citation Information

Patent Citations

  • Preparation method of composite structural member, composite structural member and electronic equipment

    CN110635816A

  • Glass sealing method and vacuum glass

    CN114804661A

  • Glass powder, laser sealing glass slurry, vacuum glass and sealing process thereof

    CN116675435A

  • Manufacture of plane display

    JP1989300224A

  • Method for producing glass substrate with sealing material layer

    JP2013049614A