A solid-phase sintered sealing tube

By using the sealing and pressing components of a metal sealer to achieve sealing in test tubes, the problem of cumbersome high-temperature sintering sealing is solved, experimental efficiency and sealing performance are improved, and costs are reduced.

CN111609136BActive Publication Date: 2026-03-13SOUTHERN UNIVERSITY OF SCIENCE AND TECHNOLOGY
View PDF 3 Cites 0 Cited by

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2020-06-28
Publication Date
2026-03-13

AI Technical Summary

Technical Problem

Existing test tubes require high-temperature sintering and sealing during inorganic synthetic material experiments, which makes the operation cumbersome.

Method used

It adopts a tube body with a cavity and a metal sealer. The metal sealer includes a sealing element and a pressing element. The sealing element fits against the inner wall of the tube body, and the seal is achieved through the cooperation of the connecting hole and the pressing element, avoiding high-temperature operation.

Benefits of technology

It simplifies the sealing process, improves experimental efficiency, reduces experimental costs, and maintains sealing performance at high temperatures, preventing deformation and damage.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN111609136B_ABST
    Figure CN111609136B_ABST
Patent Text Reader

Abstract

This invention provides a solid-state sintered sealing tube, relating to the field of laboratory instrument technology. It comprises a tube body with a chamber and a metal sealer. One end of the tube body has an opening communicating with the chamber. The metal sealer includes a sealing element and a pressing element. A connecting hole is provided on the sealing element, and one end of the sealing element is fitted against the inner wall of the tube body through the opening. The connecting hole communicates with the chamber of the tube body. The pressing element is located at the other end of the sealing element and is used to close the connecting hole to seal the chamber. This can be achieved through a simple connection of the pressing element and the sealing element. This connection method does not require special conditions such as high temperature, thus simplifying the use of the solid-state sintered sealing tube and further improving experimental efficiency and saving experimental time.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] This invention relates to the field of laboratory instrument technology, and more specifically, to a solid-state sintered sealing tube. Background Technology

[0002] With rapid economic development, science and technology have been studied in depth, and basic scientific research is usually conducted in laboratories. A test tube is a commonly used instrument in laboratories, serving as a reaction vessel for small amounts of reagents, used at room temperature or under heat.

[0003] When existing test tubes are used in experiments involving inorganic synthetic materials, the internal space of the tube needs to be sealed beforehand. This sealing process typically involves sintering the tube opening to a deformable state at high temperatures, then pinching the opening together to seal the internal space, allowing for subsequent use at higher temperatures. This sealing method is quite cumbersome. Summary of the Invention

[0004] The purpose of this invention is to address the shortcomings of the prior art by providing a solid-state sintered sealing tube, thereby solving the cumbersome problem caused by the need for high-temperature sintering sealing of existing test tubes.

[0005] To achieve the above objectives, the technical solutions adopted in the embodiments of the present invention are as follows:

[0006] In one aspect of the present invention, a solid-state sintered sealing tube is provided, comprising: a tube body having a cavity and a metal sealer; one end of the tube body is provided with an opening communicating with the cavity; the metal sealer includes a sealing member and a pressing member; a connecting hole is provided on the sealing member, one end of the sealing member is fitted against the inner wall of the tube body through the opening, and the connecting hole communicates with the cavity of the tube body; the pressing member is provided at the other end of the sealing member and is used to close the connecting hole to seal the cavity.

[0007] Optionally, the sealing element is sealed to the inner wall of the pipe; the absolute value of the difference between the expansion coefficient of the sealing element and the expansion coefficient of the pipe is less than or equal to 10% of the preset expansion coefficient, wherein, when the expansion coefficient of the sealing element is greater than the expansion coefficient of the pipe, the preset expansion coefficient is equal to the expansion coefficient of the pipe; when the expansion coefficient of the sealing element is equal to the expansion coefficient of the pipe, the preset expansion coefficient is equal to the expansion coefficient of the sealing element or the expansion coefficient of the pipe; when the expansion coefficient of the sealing element is less than the expansion coefficient of the pipe, the preset expansion coefficient is equal to the expansion coefficient of the sealing element.

[0008] Optionally, the sealing component includes a flange and a connecting shaft disposed on one side of the flange; a through hole is provided on the connecting shaft, which communicates with the flange shaft hole to form a connecting hole; the other end of the connecting shaft is fitted against the inner wall of the pipe body, and the pressing component is disposed on the other side of the flange.

[0009] Optionally, the metal seal also includes a gasket located between the flange and the press-fit member; an annular boss that mates with the gasket is provided on the inner wall of the flange shaft hole near the press-fit member, the gasket is located on the inner wall of the flange shaft hole and one side of the gasket abuts against the annular boss, the gasket protrudes from the surface of the flange near the press-fit member, and the press-fit member abuts against the other side of the gasket and is connected to the flange.

[0010] Optionally, the washer can be made of copper.

[0011] Optionally, the metal seal may also include a connecting portion; the pressing element is detachably connected to the sealing element via the connecting portion.

[0012] Optionally, the connection part is a bolt.

[0013] Optionally, an internal thread is provided in the connecting hole on the sealing component, and an external thread is provided on the pressing component; the pressing component is threadedly connected to the sealing component through the mutually mating external and internal threads.

[0014] Optionally, the tube body is made of tungsten glass, and the sealing component is made of tungsten.

[0015] Optionally, the tube body is made of quartz glass, and the sealing component is made of molybdenum.

[0016] The beneficial effects of this invention include:

[0017] This invention provides a solid-state sintered sealing tube comprising a tube body and a metal sealer. The tube body has a chamber structure and an opening at one end. Correspondingly, the metal sealer includes a sealing element and a pressing element. One end of the sealing element extends into the inner wall of the tube body through the opening, ensuring a tight seal between the sealing element and the tube body. To allow communication between the sealing element and the tube body's chamber, a connecting hole is provided on the sealing element. This connecting hole connects the tube body's chamber to the external space, allowing external reactants to be added to the tube body's chamber during use. A pressing element is also provided at the other end of the sealing element, which covers the connecting hole on the sealing element, thereby achieving a seal for the internal chamber of the tube body. By using metal for both the sealing and pressing components, the high melting point of the metal can be utilized to avoid the influence of low-melting-point seals on the experiment, thus preventing deformation and damage to the solid-state sintered sealed tube during subsequent heating requirements, as the solid-state sintered sealed tube may be subjected to heating. This also prevents deformation and damage to the solid-state sintered sealed tube when used at high temperatures. The connection between the pressing and sealing components is simple and does not require special conditions such as high temperatures. Therefore, it not only simplifies the use of the solid-state sintered sealed tube but also further improves experimental efficiency and saves experimental time. Attached Figure Description

[0018] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of the present invention and should not be regarded as a limitation on the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.

[0019] Figure 1 This is one of the structural schematic diagrams of a solid-state sintered sealing tube provided in an embodiment of the present invention;

[0020] Figure 2 This is a second schematic diagram of the structure of a solid-state sintered sealing tube provided in an embodiment of the present invention;

[0021] Figure 3 This is the third schematic diagram of a solid-phase sintered sealing tube provided in an embodiment of the present invention.

[0022] Icons: 100 - Pipe body; 210 - Press-fit component; 220 - Sealing component; 221 - Flange; 222 - Connecting shaft; 300 - Washer; 400 - Bolt. Detailed Implementation

[0023] 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 some embodiments of the present invention, and not all embodiments. The components of the embodiments of the present invention described and shown in the accompanying drawings can generally be arranged and designed in various different configurations.

[0024] Therefore, the following detailed description of the embodiments of the invention provided in the accompanying drawings is not intended to limit the scope of the claimed invention, but merely to illustrate selected embodiments of the invention. It should be noted that, without conflict, the various features in the embodiments of the invention can be combined with each other, and the combined embodiments are still within the protection scope of the invention.

[0025] It should be noted that similar labels and letters in the following figures indicate similar items. Therefore, once an item is defined in one figure, it does not need to be further defined and explained in subsequent figures.

[0026] In the description of this invention, it should be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, or the orientation or positional relationship commonly used when the product of this invention is in use. They are only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this invention. In addition, the terms "first," "second," "third," etc., are only used to distinguish descriptions and should not be construed as indicating or implying relative importance.

[0027] Furthermore, terms such as "horizontal" and "vertical" do not imply that components must be absolutely horizontal or suspended, but rather that they can be slightly tilted. For example, "horizontal" simply means that its direction is more horizontal than "vertical," and does not mean that the structure must be completely horizontal, but can be slightly tilted.

[0028] In the description of this invention, it should also be noted that, unless otherwise explicitly specified and limited, the terms "set," "install," "connect," and "link" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.

[0029] In one aspect of the embodiments of the present invention, reference is made to Figure 1 A solid-state sintered sealing tube is provided, comprising: a tube body 100 having a cavity and a metal sealer; one end of the tube body 100 is provided with an opening communicating with the cavity; the metal sealer includes a sealing member 220 and a pressing member 210; a connecting hole is provided on the sealing member 220, one end of the sealing member 220 is fitted against the inner wall of the tube body 100 through the opening, and the connecting hole communicates with the cavity of the tube body 100; the pressing member 210 is provided at the other end of the sealing member 220 and is used to close the connecting hole to seal the cavity.

[0030] For example, such as Figure 1As shown, the solid-state sintered sealing tube includes a tube body 100 and a metal sealer. The tube body 100 has a chamber structure. To allow reactants to enter and be contained within the chamber of the tube body 100, an opening can be made at one end of the tube body 100. Correspondingly, the metal sealer includes a sealing element 220 and a pressing element 210. One end of the sealing element 220 should fit into the inner wall of the tube body 100 through the opening. This fits snugly between the sealing element 220 and the opening of the tube body 100, ensuring a tight seal at the connection between the sealing element 220 and the tube body 100. To enable the sealing element 220 to communicate with the chamber of the tube body 100, a connection hole should be provided on the sealing element 220. This connection hole connects the chamber of the tube body 100 with the external space, allowing external reactants to be added to the chamber of the tube body 100 during use. A pressing element 210 is also provided at the other end of the sealing element 220. The pressing element 210 covers the connection hole on the sealing element 220, thereby achieving the requirement of sealing the internal chamber of the tube body 100. By using both the sealing element 220 and the pressing element 210 as metal materials, after the solid-state sintered sealed tube body 100, the high melting point of the metal can be utilized to avoid the influence of low-melting-point seals on the experiment during subsequent heating requirements. Simultaneously, it also prevents deformation and damage to the solid-state sintered sealed tube when used at high temperatures.

[0031] In practical use, the solid-state sintered sealed tube can be sterilized, including sterilizing the tube body 100, sealing component 220, and pressing component 210 separately, so that the solid-state sintered sealed tube meets the experimental requirements. Then, the reactants are placed into the cavity of the tube body 100 through the connecting hole. The pressing component 210 is detachably mounted on the sealing component 220, allowing it to completely cover the connecting hole. Simultaneously, to ensure effective sealing of the cavity, a clamping force is applied to the sealing component 220 while the pressing component 210 is closing, thus maintaining good sealing performance. After sealing the cavity of the tube body 100, it is placed in a high-temperature environment for the experiment. As illustrated, in the preparation of the anti-perovskite material Na3OBr, the original reactants NaBr and NaCl are thoroughly ground evenly in a mortar; the mixed original reactants are directly loaded into the cavity inside the tube 100; or the original reactants are initially pressed into a relatively dense sheet and loaded into the cavity inside the tube 100; a gasket of appropriate size (oxygen-free copper material) is placed inside the connection hole of the sealing component 220, the metal pressing component 210 is fastened, and the bolts 400 are tightened to ensure that the oxygen-free copper gasket fully seals the connection under the compression of the pressing component 210; the solid-state sintering sealing tube containing the reactants is placed in a muffle furnace for a high-temperature solid-state sintering reaction at 350°C for 3 hours; after the reaction is completed, the solid-state sintering sealing tube is cooled, the fastening bolts 400 are loosened, and the required sample Na3OBr is taken out. After the experiment is completed, the solid-state sintered sealing tube can be cleaned by cleaning components such as the tube body 100, sealing component 220, and pressing component 210. Since the structure of the entire solid-state sintered sealing tube is not damaged, it can be reused in subsequent related experiments, effectively reducing the cost of the experiment. At the same time, sealing the chamber can be achieved through a simple connection between the pressing component 210 and the sealing component 220. This connection method does not require special conditions such as high temperature, thus simplifying the use of the solid-state sintered sealing tube and further improving the efficiency of the experiment and saving experimental time.

[0032] It should be noted that, firstly, the material of the tube 100 in this application can be glass or quartz glass, and the material of the sealing component 220 and the pressing component 210 can be molybdenum, tungsten, steel, Kovar alloy, etc. This example does not impose specific limitations on them, as long as they can meet the experimental usage conditions and can be fitted and sealed with the metal sealing component 220.

[0033] Second, the material of the pressing component 210 in this application can be the same as or different from that of the sealing component 220, as long as the pressing component 210 can maintain a seal on the connection hole at all times under experimental or room temperature after closing the connection hole.

[0034] Third, when the sealing component 220 and the inner wall of the tube body 100 are fitted together in this application, the fitting method can be a perfect match or an interference fit. This application does not make specific limitations on it, as long as the two can meet the sealing requirements of the fitting point throughout the entire experimental process.

[0035] Fourth, in this embodiment, the pressing member 210 can be connected to the sealing member 220 in a detachable manner, or it can be hinged and fastened.

[0036] Optionally, the sealing element 220 is sealed to the inner wall of the pipe body 100, and the absolute value of the difference between the expansion coefficient of the sealing element 220 and the expansion coefficient of the pipe body 100 is less than or equal to 10% of the preset expansion coefficient. Specifically, when the expansion coefficient of the sealing element 220 is greater than the expansion coefficient of the pipe body 100, the preset expansion coefficient is equal to the expansion coefficient of the pipe body 100; when the expansion coefficient of the sealing element 220 is equal to the expansion coefficient of the pipe body 100, the preset expansion coefficient is equal to the expansion coefficient of the sealing element 220 or the expansion coefficient of the pipe body 100; when the expansion coefficient of the sealing element 220 is less than the expansion coefficient of the pipe body 100, the preset expansion coefficient is equal to the expansion coefficient of the sealing element 220.

[0037] For example, such as Figure 1 As shown, the sealing component 220 can be fitted to the inner wall of the tube 100 through a sealing process to seal the joint (meeting the requirements of the entire experiment). It has advantages such as excellent sealing performance, high reliability, long service life, and good mechanical stability. In addition, in the use of solid-state sintered sealed tubes, when the experiment needs to be carried out at a high temperature, both the entire tube 100 and the metal seal will experience a certain degree of temperature rise. According to the properties of the materials, both the tube 100 and the metal sealing component 220 will expand to a certain extent as the temperature rises. Therefore, in order to maintain a high degree of airtightness throughout the entire heating and cooling process, the expansion rates of the two components need to be similar, that is, the expansion coefficient of the sealing component 220 and the expansion coefficient of the tube 100 should have similar trends in the temperature range throughout the entire experiment. To prevent leakage between the sealing element 220 and the tube 100 due to excessive difference in their expansion coefficients during temperature changes (heating and cooling), the absolute value of the difference between the expansion coefficients of the sealing element 220 and the tube 100 should be less than or equal to 10% of the preset expansion coefficient. Specifically, when the expansion coefficient of the sealing element 220 is greater than that of the tube 100, the preset expansion coefficient is equal to the expansion coefficient of the tube 100; when the expansion coefficient of the sealing element 220 is equal to that of the tube 100, the preset expansion coefficient is equal to either the expansion coefficient of the sealing element 220 or the expansion coefficient of the tube 100; and when the expansion coefficient of the sealing element 220 is less than that of the tube 100, the preset expansion coefficient is equal to the expansion coefficient of the sealing element 220.

[0038] The sealing process mainly utilizes the mutual wetting and bonding of the oxide films on glass and metal to achieve a mating seal. The following is an illustrative example of one such process:

[0039] First, the metal sealing component 220 must be cleaned before sealing with the glass to remove grease and dirt from the metal surface. The general cleaning process follows these steps: mechanical cleaning followed by degreasing, then chemical or electrochemical cleaning, and finally drying. Mechanical cleaning uses mechanical friction to partially remove various compounds (such as oxide layers) and adhering dirt from the material surface. Common methods include scrubbing with sandpaper and fine tungsten wire, and sometimes soap. Degreasing commonly uses alkaline solutions and organic solvents. Alkaline degreasing involves heating a 20% sodium hydroxide or potassium hydroxide solution to 70-80°C to saponify the grease. Grease can also be dissolved in many organic solvents to achieve degreasing. Commonly used organic solvents include acetone, ether, and trichloroethylene, with trichloroethylene having the strongest degreasing power. Chemical cleaning utilizes the dissolution of chemical contaminants on the surface of the parts in a chemical liquid to achieve a highly clean surface. Electrochemical cleaning is also known as electrolytic cleaning or reverse electroplating. This method involves immersing the parts in a specially prepared solution and applying an electric current, causing the metal and metal compounds on the surface of the parts to detach and become immersed in the solution, thus achieving a highly cleaned surface. After cleaning, the metal surface may retain residual alkali or acid ions. It must be rinsed thoroughly with distilled or deionized water and dried. Then, it should be wrapped in clean paper and stored in a desiccator for later use.

[0040] Untreated metal parts will develop numerous air bubbles at their sealing joints, affecting airtightness and sealing strength, and even causing leaks or cracks. Therefore, after cleaning, metal parts require heat treatment, which involves placing the metal in hydrogen (wet hydrogen) or a vacuum and heating it at high temperatures. This causes the gases inside the metal to rapidly diffuse to the lower-pressure exterior, or allows hydrogen to diffuse into the metal, replacing other gases. This process is called hydrogen burning. For example, Kovar alloys, even after cleaning, cannot be sealed to glass without hydrogen burning. The purpose is to remove impurities and gases, especially compounds like oxygen and carbon, from the Kovar material. After hydrogen burning, the sealing surface of Kovar with glass is smooth and transparent, with a strong bond and good airtightness. During hydrogen burning, the hydrogen gas in the metal is easily removed during vacuum degassing, and the oxide layer on the metal surface can also be removed, reducing it.

[0041] After cleaning and hydrogen burning, metal parts require oxidation treatment at the sealing joints to improve the wettability of the metal and glass and ensure the bonding quality of the sealing interface. However, during flame oxidation, the degree of oxidation must be strictly controlled. The metal should not be burned until it becomes shiny, as excessive temperature will lead to over-oxidation. Conversely, insufficient oxidation will result in a thin oxide film, causing leakage after sealing.

[0042] The bonding method during sealing can be a matching seal, which means selecting glass and metal with similar coefficients of thermal expansion (within the range of room temperature to glass softening temperature). During the gradual cooling process after high-temperature sealing, the shrinkage of glass and metal is kept consistent, thereby reducing the internal stress caused by the difference in shrinkage between glass and metal.

[0043] Alternatively, compression sealing can be used, where the coefficient of thermal expansion of the metal is greater than that of the glass. When the seal cools, the metal contracts more than the glass, thus generating compressive stress on the glass (utilizing the property that the compressive strength of glass is much greater than its tensile strength) to achieve a seal.

[0044] Optionally, the sealing component 220 includes a flange 221 and a connecting shaft 222 disposed on one side of the flange 221; a through hole is provided on the connecting shaft 222, which communicates with the shaft hole of the flange 221 to form a connecting hole; the other end of the connecting shaft 222 is fitted against the inner wall of the pipe body 100, and the pressing component 210 is disposed on the other side of the flange 221.

[0045] For example, the sealing element 220 can be in the form of a flange 221, such as... Figure 2As shown, the sealing component 220 includes a flange 221 and a connecting shaft 222. The connecting shaft 222 is disposed on one side of the flange 221. A through hole can also be provided along the axial direction of the connecting shaft 222. The end of the connecting shaft 222 away from the flange 221 extends into the cavity of the tube 100 through an opening on the tube 100, fitting snugly against the inner wall of the tube 100. This allows the opening at one end of the through hole to communicate with the cavity inside the tube 100, while the opening at the other end of the through hole communicates with the shaft hole of the flange 221. Together, they form the connecting hole on the sealing component 220, thereby connecting the cavity of the tube 100 with the external space, facilitating subsequent operations such as adding reactants. To achieve a seal in the cavity, a pressing component 210 is also disposed on the side of the flange 221 opposite to or away from the connecting shaft 222. By detachably mounting the pressing component 210 on the flange 221, the shaft hole of the flange 221 is closed. The connection between the press-fit component 210 and the flange 221 can be a threaded connection as in subsequent embodiments, or it can be a bolt connection 400. This embodiment does not specifically limit it. It should be noted that the connection between the flange 221 and the connecting shaft 222 can be integrally formed, or they can be formed separately and then welded. The flange 221 mentioned above can be a solid flange 221, a threaded flange 221, and many other forms. When the sealing component 220 consists of a flange 221 and a connecting shaft 222, the corresponding connection is as follows: Figure 2 As shown, the press-fit part 210 can be a blind flange (flange 221 cover).

[0046] Optionally, the metal seal also includes a gasket 300 located between the flange 221 and the press-fit member 210; an annular boss that mates with the gasket 300 is provided on the inner wall of the shaft hole of the flange 221 near the press-fit member 210, the gasket 300 is located on the inner wall of the shaft hole of the flange 221 and one side of the gasket 300 abuts against the annular boss, the gasket 300 protrudes from the surface of the flange 221 near the press-fit member 210, and the press-fit member 210 abuts against the other side of the gasket 300 and is connected to the flange 221.

[0047] For example, such as Figure 2As shown, to further enhance the stability of the connection between flange 221 and press-fit component 210, and to ensure that press-fit component 210 can always effectively close the shaft hole of flange 221 throughout the experiment, thereby improving the sealing performance of the internal cavity of pipe body 100, a gasket 300 can be provided between flange 221 and press-fit component 210. Simultaneously, to improve the stability of gasket 300 during installation, an annular boss can be provided on the inner wall of the shaft hole of flange 221. By placing the annular gasket 300 on the inner wall of the shaft hole of flange 221, and ensuring that one side of gasket 300 abuts against one side wall of the annular boss on the inner wall of the shaft hole, the annular boss limits the depth of gasket 300 extending into the shaft hole of flange 221. Furthermore, the inner wall of the shaft hole of flange 221 can also be used to limit the gasket 300 radially along the shaft hole, thereby improving installation efficiency. Additionally, as... Figure 3 As shown, when the gasket 300 is installed on the inner wall of the shaft hole of the flange 221 and abuts against the annular protrusion, the gasket 300 can also protrude from the surface of the flange 221 near the pressing member 210. Therefore, when the pressing member 210 is fitted onto the flange 221, it does not directly contact the flange 221, but rather contacts the portion of the gasket 300 protruding from the surface of the flange 221. As the flange 221 and the pressing member 210 are installed in place, the gasket 300 is gradually compressed, thereby effectively sealing the shaft hole of the flange 221. Furthermore, it can prevent deformation and damage caused by excessive contact between the flange 221 and the pressing member 210.

[0048] Optionally, the material of washer 300 is copper.

[0049] For example, when the gasket 300 is made of copper, its lower strength can be used to seal the cavity of the pipe body 100 during the connection of the flange 221 and the press-fit part 210.

[0050] Optionally, the metal seal also includes a connecting portion; the pressing member 210 is detachably connected to the sealing member 220 via the connecting portion.

[0051] Example, combination Figure 1 and Figure 2 As shown, the metal seal may also include a connecting part, through which the pressing part 210 is detachably connected to the sealing part 220, allowing the solid-state sintered sealing tube of this application to be reused multiple times. This effectively avoids the waste caused by the existing high-temperature sintered quartz tube seals, which can only be used once.

[0052] Optionally, the connection part is a 400 bolt.

[0053] For example, such as Figure 2 As shown, the connecting part can be a bolt 400, and there can be two or more bolts 400, for example... Figure 2 The diagram illustrates the connection method when there are six bolts 400. To achieve a uniform seal on the connection hole, the bolts 400 should be evenly distributed along the overlapping portion of the projections of the press-fit member 210 and the sealing member 220.

[0054] Optionally, an internal thread is provided in the connecting hole on the sealing member 220, and an external thread is provided on the pressing member 210; the pressing member 210 is threadedly connected to the sealing member 220 through the mutually mating external and internal threads.

[0055] For example, the sealing element 220 can also be connected to the pressing element 210 by means of a threaded connection. In order to improve the sealing performance, double threads can also be used for the connection.

[0056] Optionally, the tube body 100 is made of tungsten glass and the sealing component 220 is made of tungsten.

[0057] For example, to ensure that the tube body 100 and the seal 220 maintain similar coefficients of thermal expansion throughout the experimental temperature range, the tube body 100 can be made of molybdenum group glass, while the seal 220 can be made of molybdenum. In other embodiments of this application, the tube body 100 can also be made of tungsten group glass, with the seal 220 correspondingly made of tungsten. The tube body 100 can be made of platinum group glass or molybdenum group glass, and the seal 220 can be made of iron-nickel alloy (Dumex, where nickel accounts for 42.5% to 43.5%) or Kovar alloy.

[0058] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A method for producing a reusable solid-phase sintering-seal tube for a solid-phase sintering reaction, characterized by, The solid-phase sintering sealing tube comprises a tube body with a cavity and a metal sealer; one end of the tube body is provided with an opening communicating with the cavity; the metal sealer comprises a sealing piece and a pressing piece; a connecting hole is arranged on the sealing piece, one end of the sealing piece is arranged in abutment with the inner wall of the tube body through the opening, the connecting hole communicates with the cavity of the tube body; the pressing piece is arranged at the other end of the sealing piece and is used for closing the connecting hole to seal the cavity; The sealing piece is a metal sealing piece, and the method comprises: Before the metal sealing piece is sealed with the tube body, the metal sealing piece and the tube body are subjected to cleaning treatment; After the cleaning treatment, the metal sealing piece is subjected to hydrogen burning treatment: high-temperature heating in a hydrogen atmosphere or a vacuum environment, so that the gas inside the metal sealing piece diffuses to the outside or hydrogen diffuses into the metal sealing piece to replace the gas inside the metal sealing piece; The sealing part of the metal sealing piece after the hydrogen burning treatment is subjected to oxidation treatment; The metal sealing piece after the oxidation treatment is matched and sealed with the tube body: the sealing piece is sealed and arranged with the inner wall of the tube body; the absolute value of the difference between the expansion coefficient of the sealing piece and the expansion coefficient of the tube body is less than or equal to 10% of the preset expansion coefficient, wherein when the expansion coefficient of the sealing piece is greater than the expansion coefficient of the tube body, the preset expansion coefficient is equal to the expansion coefficient of the tube body; when the expansion coefficient of the sealing piece is equal to the expansion coefficient of the tube body, the preset expansion coefficient is equal to the expansion coefficient of the sealing piece or the expansion coefficient of the tube body; when the expansion coefficient of the sealing piece is less than the expansion coefficient of the tube body, the preset expansion coefficient is equal to the expansion coefficient of the sealing piece; The material of the pressing piece is consistent with the material of the sealing piece.

2. The method for preparing a reusable solid-state sintered sealing tube as described in claim 1, characterized in that, The sealing piece comprises a flange and a connecting shaft arranged on one side of the flange; a through hole is arranged on the connecting shaft, the through hole communicates with the shaft hole of the flange to form the connecting hole; the other end of the connecting shaft is arranged in abutment with the inner wall of the tube body, and the pressing piece is arranged on the other side of the flange.

3. The method for preparing a reusable solid-state sintered sealing tube as described in claim 2, characterized in that, The metal sealer further comprises a gasket between the flange and the pressing piece; an annular boss matched with the gasket is arranged on the inner wall of the shaft hole of the flange close to the pressing piece, the gasket is located on the inner wall of the shaft hole of the flange, one side of the gasket abuts against the annular boss, the gasket protrudes from the surface of the flange close to the pressing piece, and the other side of the gasket abuts against the pressing piece and is connected with the flange.

4. The method for preparing a reusable solid-state sintered sealing tube as described in claim 3, characterized in that, The material of the gasket is copper.

5. The method for preparing a reusable solid-state sintered sealing tube as described in claim 1, characterized in that, The metal sealer further comprises a connecting part; the pressing piece is detachably connected with the sealing piece through the connecting part.

6. The method of claim 5, wherein the reusable solid-phase sintered seal tube is prepared by the steps of: The connecting part is a bolt.

7. The method for preparing a reusable solid-state sintered sealing tube as described in claim 1, characterized in that, An internal thread is further arranged in the connecting hole on the sealing piece, and an external thread is further arranged on the pressing piece; the pressing piece is threadedly connected with the sealing piece through the matched external thread and internal thread.

8. The method for preparing a reusable solid-state sintered sealing tube as described in claim 1, characterized in that, The material of the tube body is tungsten glass, and the material of the sealing piece is tungsten.

9. The method for preparing a reusable solid-state sintered sealing tube as described in claim 1, characterized in that, The material of the tube body is quartz glass, and the material of the sealing piece is molybdenum.

Citation Information

Patent Citations

  • Low temperature refrigerating machine-based visual experiment observation apparatus of controlled liquefaction and solidification process of fluid

    CN106568794A

  • Glass-metal hermetic seal connecting piece

    CN201363938Y

  • Sealing pipe

    CN212407552U