High-entropy glass-ceramic sealing material for GIS partial discharge monitoring device and preparation method thereof

Abstract

The application discloses a GIS partial discharge monitoring device high-entropy microcrystalline glass sealing material and a preparation method thereof, and belongs to the technical field of sealing. The sealing material is a double-main-crystal-phase and glass-phase combined structure, and the material is Bi2O3-MgO-SiO2-Al2O3-Na2O-B2O3-ZrO2 microcrystalline glass. The application has the beneficial effect that: a plurality of oxides are used as main compounds, the comprehensive performance of the microcrystalline glass is improved by using the high-entropy effect, the condition that the microcrystalline glass is mainly composed of a single compound is changed, the connection between copper and stainless steel is realized in the GIS system, and the application field of the microcrystalline glass is well expanded.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of sealing, in particular to a high-entropy glass-ceramic sealing material for GIS partial discharge monitoring device and a preparation method thereof. BACKGROUND

[0002] The GIS partial discharge on-line monitoring device can timely understand the operation condition of the equipment, reduce the economic loss caused by power failure, find the insulation defects that cannot be found in preventive test under the operating voltage, and locate the internal hidden danger of the insulation monitoring equipment. The GIS maintenance work can be carried out in a planned manner, the maintenance time is shortened, the maintenance cost is saved, and thus the operation reliability of the GIS is improved. The GIS combined with the on-site operation results shows that the partial discharge monitoring is necessary when the high-voltage electrical equipment is operated, the GIS partial discharge on-line monitoring system can effectively detect the partial discharge phenomenon, lays a foundation for in-depth analysis of the partial discharge, and the monitoring equipment is easy to install, the cost is moderate, and the work is stable.

[0003] The GIS partial discharge box is an important device for realizing partial discharge monitoring, but the sealing between the GIS partial discharge box and the GIS system is a prerequisite for determining whether the GIS partial discharge box can normally and stably work, and is an important guarantee for the service life of the GIS partial discharge box. The research on the sealing material has important value for the research and development of the GIS partial discharge box.

[0004] The sealing material generally refers to a material embedded in the building joint to achieve air-tightness and water-tightness. The sealing material has metal materials (aluminum, lead, indium, stainless steel, etc.), non-metal materials (rubber, plastic, ceramic, graphite, etc.), and composite materials, but the most commonly used is the rubber elastomer material. The silicone rubber sealant can withstand high temperature and low temperature, resist radiation, resist vacuum, be pollution-free and non-toxic; the polysulfide rubber sealant has excellent aviation fuel resistance, and also has high temperature resistance, high pressure resistance, friction resistance, pressure resistance and other properties, which are the development direction of the sealing industry.

[0005] Glass-ceramic, also known as glass ceramic, is a kind of polycrystalline solid material containing a large amount of microcrystalline phase and glass phase, which is prepared by controlling crystallization in the heating process of a base glass with a specific composition. Glass is a non-crystalline solid, and from the viewpoint of thermodynamics, it is a metastable state with higher internal energy than the crystalline state, and can be converted into a crystalline state under certain conditions. From the viewpoint of dynamics, the rapid increase of viscosity in the cooling process of glass melt inhibits the formation and growth of crystal nuclei, making it difficult to convert into a crystalline state. Glass-ceramic is a new material obtained by fully utilizing the favorable conditions of glass in thermodynamics.

[0006] The difference between glass-ceramics and ceramics is that the crystalline phase in glass-ceramics is generated from a single homogeneous glass phase or a phase-separated region through nucleation and crystal growth, while the crystalline phase in ceramics is mostly introduced directly during the preparation of the ceramics in addition to recrystallization or new crystalline phase generated through solid phase reaction. The difference between glass-ceramics and glass is that glass-ceramics is a composite material composed of microcrystals and residual glass, while glass is a non-crystalline or amorphous body. Although the structure, performance and production method of glass-ceramics are different from those of glass and ceramics, glass-ceramics has the basic performance of glass and the polycrystalline characteristics of ceramics, and combines the characteristics of glass and ceramics, becoming a unique new type of material.

[0007] Glass-ceramics has many excellent properties, and its performance indicators are often better than those of similar glass and ceramics. For example, the thermal expansion coefficient can be adjusted in a wide range; the mechanical strength is high, the hardness is large, and the wear resistance is good; it has good chemical stability and thermal stability, and can adapt to harsh use environments; the softening temperature is high, and it can maintain high mechanical strength even in high temperature environments; and glass-ceramics can also obtain special optical, electrical, magnetic, thermal and biological functions through composition design, so that it can be widely used as various technical materials, structural materials or other special materials. The most widely used glass-ceramics is the melting method, in which various raw materials and additives are uniformly mixed, melted at high temperature, homogenized, and then the glass melt is formed, annealed, and then nucleated and crystallized at a certain temperature to obtain glass-ceramics with fine and uniform grains and overall crystallization. The biggest feature of the melting method is that it can use any glass forming method, such as pressing, calendering, blowing, drawing and casting. Compared with the usual ceramic forming process, this method is suitable for preparing products with complex shape and precise size, and is convenient for mechanization and automation production. The obtained glass-ceramics products have high density, uniform composition and no pores.

[0008] High-entropy oxides have many ideal properties different from single oxides, so they are very important in material science and engineering. Although glass-ceramics have been studied for many years, the study of high-entropy glass-ceramics is relatively less, especially there is no related record of its application in the sealing structure of GIS.

[0009] Therefore, the present inventors carried out in-depth research on this demand, and thus the present case was produced. SUMMARY

[0010] In order to overcome the problem that high-entropy glass-ceramics is not applied to the sealing structure of GIS in the prior art, so as to realize the connection of copper and stainless steel, the sealing structure obtained has the characteristics of high bonding strength, high and low temperature resistance, impact resistance and excellent sealing performance, and has good application prospect in GIS system in harsh environment. The specific technical scheme is as follows:

[0011] The application discloses a GIS partial discharge monitoring device high-entropy microcrystalline glass sealing material, the sealing material is a double-main-crystal-phase and glass-phase combined structure, and the material is Bi2O3-MgO-SiO2-Al2O3-Na2O-B2O3-ZrO2 microcrystalline glass.

[0012] The application adopts multiple oxides as main compounds, uses the high-entropy effect to improve the comprehensive performance of the microcrystalline glass, changes the current single-compound main component condition of the microcrystalline glass, realizes the connection of copper and stainless steel in the GIS system, and well expands the application field of the microcrystalline glass.

[0013] ZrO2 is used as a nucleating agent in the high-entropy microcrystalline glass, the crystallization ability of the main crystal phase is improved, Bi2O3 and B2O3 are added into the microcrystalline glass, the melting point of the microcrystalline glass is reduced, and the forming performance is improved.

[0014] Preferably, the double main crystal phases in the sealing material are NaAlSiO4 and Bi 24 B2O 39 , and the remaining phase is a Bi2O3-MgO-SiO2-Al2O3-Na2O-B2O3 glass phase. The double main crystal phases NaAlSiO4 and Bi 24 B2O 39 are formed in the microcrystalline glass, and the crystallization difficulty is reduced.

[0015] Preferably, the particle size of the main crystal phase NaAlSiO4 is 0.1-0.6 microns, and the particle size of the main crystal phase Bi 24 B2O 39 is 0.2-0.8 microns.

[0016] Preferably, the hardness of the sealing material is 6-10 GPa, and the thermal expansion coefficient is (3.0-6.5) x 10 -6 / ℃.

[0017] The application further provides a preparation method of the high-entropy microcrystalline glass sealing material, and the high-entropy microcrystalline glass sealing material is prepared from at least the following powder raw materials in percentage by mass: 25-30% of Bi2O3, 15-25% of MgO, 15-25% of SiO2, 10-15% of Al2O3, 5-15% of Na2O, 15-25% of B2O3 and 5-10% of ZrO2.

[0018] Preferably, the powder raw materials are mixed and high-temperature melted in proportion, the glass melt obtained after melting is poured into a sealing structure and cooled, then the semi-finished product after cooling is put into a vacuum chamber and subjected to high-temperature crystallization treatment and is cooled again. The crystallization process in the vacuum can overcome the oxidation problem of the surface of the copper material.

[0019] The nano materials of Bi2O3, MgO, SiO2, Al2O3, Na2O, B2O3 and ZrO2 are mechanically mixed, then high-temperature melting is carried out and pouring between stainless steel and copper is carried out, and then low-temperature crystallization treatment is carried out, so that the connection between high-temperature-resistant stainless steel and low-melting-point copper is realized, the process flow is simple, and the defects of complex manufacturing process and high melting temperature of the existing microcrystalline glass are overcome.

[0020] The low-melting-point Bi2O3 and B2O3 materials are added into the microcrystalline glass to reduce the melting point, so that the connection between the low-melting-point copper material and the stainless steel can be realized.

[0021] Preferably, the preparation method of the high-entropy microcrystalline glass sealing material comprises the following steps:

[0022] Step one, in a room temperature environment, the nano powder raw materials are put into a nano powder mixing machine in proportion and stirred and mixed for 10-30 min;

[0023] Step two, the mixed powder is high-temperature melted at 800-1350 DEG C for 1-3 h, the melted glass melt is poured into a preheated 200-250 DEG C sealing structure and cooled in air;

[0024] Step three, the cooled sample is put into a vacuum chamber for high-temperature crystallization treatment, the treatment temperature is 400-800 DEG C, the treatment time is 1-3 h, and then natural cooling is carried out.

[0025] Preferably, the particle size of the nano powder in the nano powder mixing machine in step one is 30-100 nanometers.

[0026] Preferably, the sealing structure in step two is a sealing structure composed of stainless steel material and copper material.

[0027] Preferably, in step three, the high-temperature crystallization treatment has a treatment temperature of 400-500 DEG C, a vacuum degree of 3-10 Pa and a treatment time of 1-3 h.

[0028] Beneficial effects:

[0029] The beneficial effects of the technical scheme of the present application are as follows:

[0030] (1) A plurality of oxides are used as main compounds to construct high-entropy microcrystalline glass, the high-entropy effect is used to improve the comprehensive performance of the microcrystalline glass, the current situation of using single compound as the main component of the microcrystalline glass is changed, the connection between copper and stainless steel in the GIS system is realized, and the application field of the microcrystalline glass is well expanded.

[0031] (2) The nano-materials of Bi2O3, MgO, SiO2, Al2O3, Na2O, B2O3 and ZrO2 are mechanically mixed for the first time, then high-temperature melting is carried out and pouring between stainless steel and copper is carried out, and then low-temperature crystallization treatment is carried out, so that the connection between high-temperature-resistant stainless steel and low-melting-point copper is realized, the process flow is simple, and the defects of the existing microcrystalline glass manufacturing process, such as complex process and high melting temperature, are overcome.

[0032] (3) The double main crystal phases NaAlSiO4 and Bi 24 B2O 39 are formed in the microcrystalline glass, and the crystallization difficulty is reduced.

[0033] (4) In the high-entropy microcrystalline glass, ZrO2 is used as a nucleating agent to improve the crystallization ability of the main crystal phase, Bi2O3 and B2O3 are added to the microcrystalline glass to reduce the melting point of the microcrystalline glass and improve its forming performance. BRIEF DESCRIPTION OF DRAWINGS

[0034] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed to be used in the embodiments will be briefly introduced below, and it should be understood that the following drawings only show some embodiments of the present application, and therefore should not be regarded as a limitation on the scope, and for those skilled in the art, other related drawings can also be obtained without creative labor on the basis of these drawings.

[0035] Figure 1 is a preferred high-entropy microcrystalline glass structure diagram of the present application;

[0036] Figure 2 is a preferred preparation process flow diagram of the high-entropy microcrystalline glass sealing material of the present application;

[0037] Figure 3 is a preferred GIS partial discharge box monitoring device sealing structure diagram of the present application.

[0038] In the figure, 1 is a high-entropy microcrystalline glass sealing material; 2 is a copper probe; and 3 is a stainless steel flange. DETAILED DESCRIPTION

[0039] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of the present invention, not all of them. Therefore, the following detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the claimed invention, but merely to represent selected embodiments of the invention. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without inventive effort are within the scope of protection of the present invention.

[0040] This implementation method uses multiple oxides as the main compounds to construct high-entropy glass-ceramics, leveraging the high-entropy effect to enhance the overall performance of the glass-ceramics. This changes the current practice of using a single compound as the main component in glass-ceramics, enabling the connection of copper and stainless steel in a GIS system and significantly expanding the application areas of glass-ceramics. The specific implementation method is as follows:

[0041] A high-entropy microcrystalline glass sealing material for a GIS partial discharge monitoring device, wherein the sealing material has a dual main crystalline phase and glass phase combination structure, and its material is Bi2O3-MgO-SiO2-Al2O3-Na2O-B2O3-ZrO2 microcrystalline glass.

[0042] Using ZrO2 as a nucleating agent in high-entropy glass-ceramics enhances the crystallization ability of the main crystalline phase. Adding Bi2O3 and B2O3 to glass-ceramics lowers their melting point and improves their forming performance.

[0043] In a preferred embodiment, the sealing material contains two main crystalline phases, NaAlSiO4 and Bi. 24 B2O 39 ,like Figure 1 As shown in the figure, NaAlSiO4 and Bi are present in the high-entropy glass-ceramic. 24 B2O 39 The glass-ceramic structure consists of two main crystalline phases, with the remainder being a Bi₂O₃-MgO-SiO₂-Al₂O₃-Na₂O-B₂O₃ glassy phase. The dual-principal-phase structure increases its crystallization ability, making it prone to forming microcrystalline structures. In microcrystalline glass, the dual-principal-phase structures NaAlSiO₄ and Bi₂O₃ are formed. 24 B2O 39 This reduces the difficulty of crystallization.

[0044] In a preferred embodiment, the main crystalline phase NaAlSiO4 has a particle size of 0.1-0.6 micrometers, and the main crystalline phase Bi... 24 B2O 39 The particle size is 0.2-0.8 micrometers.

[0045] As a preferred embodiment, the hardness of the sealing material is 6-10 GPa, and the thermal expansion coefficient is (3.0-6.5) x 10 -6 / ℃.

[0046] The present embodiment also provides a preparation method of the high-entropy glass-ceramic sealing material. The high-entropy glass-ceramic sealing material is prepared from at least the following powder raw materials in percentage by mass: 25-30% of Bi2O3, 15-25% of MgO, 15-25% of SiO2, 10-15% of Al2O3, 5-15% of Na2O, 15-25% of B2O3, and 5-10% of ZrO2.

[0047] As a preferred embodiment, the powder raw materials are mixed in proportion and high-temperature melted. The obtained glass melt is poured into a sealing structure and cooled. Then, the cooled semi-finished product is placed in a vacuum chamber for high-temperature crystallization treatment and cooled again. The crystallization process in vacuum can overcome the oxidation problem of the copper material surface.

[0048] The nano materials of Bi2O3, MgO, SiO2, Al2O3, Na2O, B2O3, and ZrO2 are mechanically mixed, and then high-temperature melted and poured between stainless steel and copper, and then low-temperature crystallization treatment is performed, realizing the connection between high-temperature-resistant stainless steel and low-melting-point copper, and overcoming the shortcomings of the existing glass-ceramic manufacturing process, such as complicated process and high melting temperature.

[0049] The low-melting-point Bi2O3 and B2O3 materials are added into the glass-ceramic to reduce the melting point, so that the connection between the low-melting-point copper material and the stainless steel can be realized.

[0050] As shown in Figure 2 , the preferred preparation method of the high-entropy glass-ceramic sealing material includes the following steps:

[0051] In step S101, the nano powder raw materials are placed in a nano powder mixing machine in proportion at room temperature and stirred and mixed for 10-30 min.

[0052] In step S102, the mixed powder is high-temperature melted at 800-1350℃ for 1-3 h. The melted glass melt is poured into a preheated 200-250℃ sealing structure and cooled in air.

[0053] In step S103, the cooled sample is placed in a vacuum chamber for high-temperature crystallization treatment at 400-800℃ for 1-3 h, and then naturally cooled.

[0054] As a preferred embodiment, the nano-powder particle size in the nano-powder mixing machine in step S101 is 30-100 nanometers.

[0055] As a preferred embodiment, the sealing structure in step S102 is a sealing structure composed of stainless steel and copper. As shown in the figure, the sealing structure includes a copper probe 2 and a stainless steel flange 3. The high-entropy glass-ceramic sealing material 1 involved in the embodiment is located between the copper probe 2 and the stainless steel flange 3, has high bonding strength, is resistant to high and low temperatures, and has excellent impact resistance and sealing performance, and has good application prospects in GIS systems in harsh environments. Figure 3

[0056] As a preferred embodiment, the treatment temperature of high-temperature crystallization treatment in step S103 is 400-500°C, the vacuum degree is 3-10 Pa, and the treatment time is 1-3 hours.

[0057] The beneficial effects of the high-entropy glass-ceramic sealing material and the preparation method thereof in the embodiment will be further commented on through examples and comparative examples.

[0058] Example 1:

[0059] In a room temperature environment, Bi2O3, MgO, SiO2, Al2O3, Na2O, B2O3 and ZrO2 nano-powder were put into a nano-powder mixing machine for 10 minutes of stirring and mixing, and the nano-powder particle size was 30 nanometers; the mixing ratio of each powder raw material was 25% Bi2O3, 15% MgO, 25% SiO2, 10% Al2O3, 5% Na2O, 15% B2O3 and 5% ZrO2 by mass percentage; the mixed powder was subjected to high-temperature melting at 800°C for 3 hours, the molten glass melt was poured into a preheated 200°C stainless steel and copper sealing structure and cooled in air, and the cooled sample was placed in a vacuum chamber for high-temperature crystallization treatment, the treatment temperature was 400°C, the vacuum degree was 3 Pa, and the treatment time was 1 hour.

[0060] After the preparation was completed, the sample was naturally cooled to obtain a glass-ceramic sealing GIS partial discharge box monitoring device sealing structure, the high-entropy glass-ceramic sealing material included 0.1 microns of NaAlSiO4 and 0.8 microns of Bi 24 B2O 39 Two main crystal phases, the hardness is 6GPa, the thermal expansion coefficient is 3.0×10 -6 / ℃.

[0061] Example 2:

[0062] ​In the room temperature environment, Bi2O3, MgO, SiO2, Al2O3, Na2O, B2O3 and ZrO2 nano-powder are put into the nano-powder mixing machine for 20 minutes of stirring and mixing, and the nano-powder particle size is 100 nanometers; the mixing ratio of each powder raw material is 25% of Bi2O3, 15% of MgO, 15% of SiO2, 15% of Al2O3, 5% of Na2O, 15% of B2O3 and 10% of ZrO2 in terms of mass percentage; the mixed powder is high-temperature melted at 1350℃ for 3 hours, the melted glass melt is poured into the preheated 250℃ stainless steel and copper sealing structure and cooled in air, and the cooled sample is put into a vacuum chamber for high-temperature crystallization treatment, the treatment temperature is 500℃, the vacuum degree is 10Pa, and the treatment time is 2 hours.

[0063] After the preparation is completed, natural cooling is performed, and the obtained microcrystalline glass sealed GIS partial discharge box monitoring device sealing structure, the high-entropy microcrystalline glass sealing material includes 0.2 microns of NaAlSiO4 and 0.7 microns of Bi 24 B2O 39 Two main crystal phases, the hardness is 10GPa, and the thermal expansion coefficient is 6.5x10 -6 / ℃.

[0064] Example 3:

[0065] In the room temperature environment, Bi2O3, MgO, SiO2, Al2O3, Na2O, B2O3 and ZrO2 nano-powder are put into the nano-powder mixing machine for 30 minutes of stirring and mixing, and the nano-powder particle size is 50 nanometers; the mixing ratio of each powder raw material is 25% of Bi2O3, 15% of MgO, 25% of SiO2, 10% of Al2O3, 5% of Na2O, 15% of B2O3 and 5% of ZrO2 in terms of mass percentage; the mixed powder is high-temperature melted at 1200℃ for 3 hours, the melted glass melt is poured into the preheated 250℃ stainless steel and copper sealing structure and cooled in air, and the cooled sample is put into a vacuum chamber for high-temperature crystallization treatment, the treatment temperature is 450℃, the vacuum degree is 5Pa, and the treatment time is 2 hours.

[0066] After the preparation is completed, natural cooling is performed, and the obtained microcrystalline glass sealed GIS partial discharge box monitoring device sealing structure, the high-entropy microcrystalline glass sealing material includes 0.3 microns of NaAlSiO4 and 0.5 microns of Bi 24 B2O 39 Two main crystal phases, the hardness is 9GPa, and the thermal expansion coefficient is 5.0x10 -6 / ℃.

[0067] Example 4:

[0068] In the room temperature environment, Bi2O3, MgO, SiO2, Al2O3, Na2O, B2O3 and ZrO2 nano-powder are put into the nano-powder mixing machine for 30 minutes of stirring and mixing, and the nano-powder particle size is 70 nanometers; the mixing ratio of each powder raw material is 25% of Bi2O3, 15% of MgO, 15% of SiO2, 10% of Al2O3, 5% of Na2O, 25% of B2O3 and 5% of ZrO2 according to the mass percentage; the mixed powder is high-temperature melted at 1000℃ for 2 hours, the melted glass melt is poured into the sealed structure of preheated 200℃ stainless steel and copper and cooled in air, and the cooled sample is put into a vacuum chamber for high-temperature crystallization treatment, the treatment temperature is 400℃, the vacuum degree is 3Pa, and the treatment time is 3 hours.

[0069] After the preparation is completed, natural cooling is carried out, and the obtained microcrystalline glass sealed GIS partial discharge box monitoring device sealing structure, high-entropy microcrystalline glass sealing material includes 0.5 microns of NaAlSiO4 and 0.6 microns of Bi 24 B2O 39 Two main crystal phases, the hardness is 7GPa, and the thermal expansion coefficient is 4.0×10 -6 / ℃.

[0070] Example 5:

[0071] In the room temperature environment, Bi2O3, MgO, SiO2, Al2O3, Na2O, B2O3 and ZrO2 nano-powder are put into the nano-powder mixing machine for 10 minutes of stirring and mixing, and the nano-powder particle size is 90 nanometers; the mixing ratio of each powder raw material is 25% of Bi2O3, 15% of MgO, 15% of SiO2, 15% of Al2O3, 5% of Na2O, 20% of B2O3 and 5% of ZrO2 according to the mass percentage; the mixed powder is high-temperature melted at 900℃ for 2 hours, the melted glass melt is poured into the sealed structure of preheated 250℃ stainless steel and copper and cooled in air, and the cooled sample is put into a vacuum chamber for high-temperature crystallization treatment, the treatment temperature is 450℃, the vacuum degree is 8Pa, and the treatment time is 3 hours.

[0072] After the preparation is completed, natural cooling is carried out, and the obtained microcrystalline glass sealed GIS partial discharge box monitoring device sealing structure, high-entropy microcrystalline glass sealing material includes 0.6 microns of NaAlSiO4 and 0.3 microns of Bi 24 B2O 39 Two main crystal phases, the hardness is 7GPa, and the thermal expansion coefficient is 5.0×10 -6 / ℃.

[0073] The above merely describes the preferred embodiments of the present application and is not used to limit the present application. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A high-entropy glass-ceramic sealing material for GIS partial discharge monitoring devices, characterized in that, The sealing material is a combination of double main crystal phase and glass phase, and is made of Bi2O3-MgO-SiO2-Al2O3-Na2O-B2O3-ZrO2 microcrystalline glass. The double main crystal phases in the sealing material are NaAlSiO4 and Bi respectively 24 B2O 39 , and the remaining phase is Bi2O3-MgO-SiO2-Al2O3-Na2O-B2O3 glass phase. 2.The GIS partial discharge monitoring device high-entropy glass-ceramic sealing material of claim 1, characterized in that, wherein the particle size of the main crystal phase NaAlSiO4 is 0.1-0.6 microns and the particle size of the main crystal phase Bi 24 B2O 39 is 0.2-0.8 microns. 3.The GIS partial discharge monitoring device high-entropy glass-ceramic sealing material of claim 1, characterized in that, The sealing material has a hardness of 6-10 GPa and a thermal expansion coefficient of (3.0-6.5)×10-6 / ℃.

4. The method for preparing the high-entropy microcrystalline glass sealing material according to any one of claims 1-3, characterized in that, The sealing material is prepared from the following powder raw materials by mass percentage: 25-30% of Bi2O3, 15-25% of MgO, 15-25% of SiO2, 10-15% of Al2O3, 5-15% of Na2O, 15-25% of B2O3 and 5-10% of ZrO2.

5. The method for preparing the high-entropy microcrystalline glass sealing material according to claim 4, characterized in that, The powder raw materials are mixed in proportion and high-temperature melted, and the obtained glass melt is poured into a sealing structure and cooled; then the cooled semi-finished product is put into a vacuum chamber for high-temperature crystallization treatment and cooled again.

6. The method for preparing the high-entropy microcrystalline glass sealing material according to claim 5, characterized in that, The method comprises the following steps: Step one, at room temperature, the nano-powder raw materials are put into a nano-powder mixing machine in proportion and stirred and mixed for 10-30 min; Step two, the mixed powder is high-temperature melted at 800-1350℃ for 1-3 h, and the melted glass melt is poured into a preheated 200-250℃ sealing structure and cooled in air; Step three, the cooled sample is put into a vacuum chamber for high-temperature crystallization treatment at a temperature of 400-800℃ for 1-3 h, and then naturally cooled.

7. The method for preparing the high-entropy microcrystalline glass sealing material according to claim 6, characterized in that, The nano-powder in the nano-powder mixing machine in step one has a particle size of 30-100 nm.

8. The method for preparing the high-entropy microcrystalline glass sealing material according to claim 6, characterized in that, The sealing structure in step two is made of stainless steel and copper.

9. The method for preparing the high-entropy microcrystalline glass sealing material according to claim 6, characterized in that, The high-temperature crystallization treatment in step three is carried out at a temperature of 400-500℃, a vacuum degree of 3-10 Pa and a treatment time of 1-3 h.

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