In-situ atmosphere quenching tube furnace

Abstract

The utility model belongs to the technical field of quenching tube furnaces, and particularly relates to an in-situ atmosphere quenching tube furnace and a quenching method thereof. The in-situ atmosphere quenching tube furnace comprises a high-temperature furnace body, a furnace tube penetrates through the high-temperature furnace body, the front end of the furnace tube is connected with a T-shaped tee joint, a sample groove with a long handle is formed in the T-shaped tee joint in the horizontal direction, the T-shaped tee joint is an air inlet end in the vertical direction, a quenching pool connector is vertically formed in the rear portion of the furnace tube, and a quenching pool is arranged in the quenching pool connector. A quenching pool is connected below the quenching pool connector, the rear end of the furnace tube is an air outlet end, and the air outlet end is connected with a hose. Through a full-sealed operation chain and precise time sequence control, full-flow atmosphere protection from high-temperature treatment to ultra-fast cooling of the nano material is realized, grain boundary oxidation and element segregation are effectively inhibited, quenching treatment of materials extremely sensitive to oxygen, water and carbon dioxide is supported, and the service life of the nano material is prolonged. The problem of material decomposition caused by temporary air exposure of traditional open or semi-closed equipment is solved.

Description

Technical Field

[0001] This utility model belongs to the technical field of quenching tube furnaces, specifically relating to an in-situ atmosphere quenching tube furnace. Background Technology

[0002] Quenching technology, as a heat treatment process that rapidly cools and modulates the microstructure of materials, has been widely used in the field of traditional metal heat treatment. In recent years, with the increasing demand for nanomaterial preparation, quenching technology has been gradually introduced into the development of advanced materials such as nanocatalysts and functional ceramics. Studies have shown that the quenching process can achieve precise control of the surface and interface properties of nanomaterials by rapidly cooling and fixing the high-temperature metastable structure. For example, quenching promotes metal ion doping (ACS Appl. Nano Mater., 2020, 3, 10454-10461), constructs active sites rich in defects on the surface (Environ. Sci. Technol., 2023, 57, 5831-5840), and even prepares single-atom / sub-nanometer catalysts (J. Mater. Chem. A, 2021, 9, 3492), improving the electrocatalytic performance and stability of materials (patent CN110975877B). Compared with other nanotechnology preparation techniques, quenching process has advantages such as simple process, short time and low cost, showing potential for industrial production.

[0003] However, traditional quenching equipment has the following key drawbacks in the preparation of nanomaterials: 1) Oxidation contamination: During conventional quenching, the sample is heated and transferred at high temperatures in air, causing the material surface to easily react with the air, reducing the purity and activity of the material; 2) Limitations in handling sensitive materials: For reactive materials that are easily reacted with oxygen / moisture, existing open quenching equipment cannot avoid chemical denaturation of the material during the transfer stage. To address the above problems, Chinese patent CN103673611B proposes a rapid quenching tubular furnace with a protective atmosphere. By heating in an inert gas environment and rapidly immersing the sample in the quenching tank, the risk of oxidation during the high-temperature stage is reduced to some extent. However, the device still has obvious limitations: 1) When the sample is transferred from the heating zone to the quenching tank, it needs to pass through an open transition zone, which means that the material is still exposed to the air environment during the transfer process, which cannot meet the preparation requirements of highly active nanomaterials (such as lithium-ion battery anode materials and metal-organic framework compounds); 2) When the sample is pushed into the quenching tank together with the ceramic boat, the ceramic boat may react with the quenching medium and introduce impurities; 3) The quenching medium is placed in the open, and direct contact with the air may lead to oxidation and contamination of the medium. If an organic quenching medium is used, there is also a safety hazard of explosion. Utility Model Content

[0004] The purpose of this invention is to provide an in-situ atmosphere quenching tube furnace, which is mainly used for heating and quenching air-sensitive nanomaterials. The in-situ atmosphere quenching tube furnace designed in this invention includes a movable and tiltable sample tank in a sealed environment and a detachable quenching pool for holding the quenching medium. This ensures that heating, quenching, and the quenching medium are all carried out under in-situ atmosphere protection. During quenching, the sample is separated from the sample tank, ensuring that even air-sensitive nanomaterials can maintain their purity and performance, while maintaining the high efficiency and economy of the quenching process.

[0005] The implementation process of this utility model is as follows:

[0006] An in-situ atmosphere quenching tube furnace includes a high-temperature furnace body, through which a furnace tube longer than the furnace body passes. A T-shaped tee is connected to the front end of the furnace tube. A sample groove with a long handle is arranged horizontally inside the T-shaped tee. The vertical direction of the T-shaped tee is the gas inlet end. A quenching pool interface is arranged vertically at the rear end of the furnace tube. A quenching pool is connected below the quenching pool interface. The rear end of the furnace tube is the gas outlet end, which is connected to a flexible hose for connecting a vacuum pump or for exporting gas.

[0007] Furthermore, the air inlet end is provided with a high-precision pressure gauge and an air inlet valve from bottom to top; the air outlet end is provided with an air outlet valve.

[0008] Furthermore, both the interface surfaces of the quenching pool and the quenching pool are frosted, and the quenching pool and the quenching pool are sealed together by a locking device; the length of the sample slot opening at the front end of the sample slot with the long handle is less than the diameter of the quenching pool interface.

[0009] Furthermore, the locking device is a clamp or a spring clamp type sealing clip.

[0010] Furthermore, the upper sidewall of the quenching pool is provided with a quenching medium injection port, and a top-mounted high-temperature resistant rubber gasket cover with a spiral structure is installed on the quenching medium injection port.

[0011] Furthermore, the T-shaped tee has a sealing cap at its horizontal front end, the long handle of the sample slot with the long handle passes through the central hole of the sealing cap and can rotate freely, and O-rings are provided on the inner side of the contact point between the long handle of the sample slot with the long handle and the sealing cap; the length of the sample slot with the long handle is greater than or equal to the length of the furnace tube; and the long handle of the sample slot with the long handle has a positioning scale line corresponding to the uniform temperature zone in the middle of the furnace tube.

[0012] Furthermore, the air inlet is connected to a high-purity gas source.

[0013] Furthermore, a lifting platform for auxiliary support of the quenching pool is provided below the quenching pool.

[0014] Furthermore, the rear end of the T-shaped tee is connected to the front end of the furnace tube via a first sealing flange; the gas outlet is connected to the rear end of the furnace tube via a second sealing flange to achieve a seal.

[0015] The quenching method of the above-mentioned in-situ atmosphere quenching tube furnace includes the following steps:

[0016] (1) Sample loading and sealing assembly

[0017] (1.1) Spread the sample to be processed evenly in the sample trough with a long handle;

[0018] (1.2) Install the furnace tube horizontally inside the in-situ atmosphere quenching tube furnace, and pass the long end of the sample groove with the long handle through the center hole of the first sealing flange, T-type tee, O-ring and sealing cover in sequence. Fix the sealing cover to the front end of the T-type tee in the horizontal direction by tightening the thread, and connect and fix the rear end of the T-type tee to the front end of the furnace tube through the first sealing flange.

[0019] (1.3) Push the sample cell with the long handle and observe the positioning scale line on the long handle of the sample cell until the sample cell containing the sample is in the uniform temperature zone in the middle of the furnace tube. Connect and fix the gas outlet end to the rear end of the furnace tube through the second sealing flange. Finally, connect and lock the interface of the quenching pool to the interface of the quenching pool with the locking device. Tighten the headspace high temperature resistant rubber gasket cover on the quenching medium injection port. The gas inlet end is connected to a high purity gas source. The gas outlet end is connected to a hose for connecting a vacuum pump or exporting gas. Close the gas inlet valve and the gas outlet valve to complete the construction of the fully enclosed system.

[0020] (2) Gas atmosphere control

[0021] (2.1) Connect the outlet end to the vacuum pump through a hose. After starting the vacuum pump, slowly open the outlet valve to the half-open state, evacuate the system and monitor the pressure in the system with a high-precision pressure gauge until it is ≤10Pa. Close the outlet valve and maintain it for 3 minutes to confirm that the pressure does not rise. Verify that the airtightness meets the standard. Disconnect the vacuum pump and repeat the evacuation three times to ensure that the residual gas in the cavity is completely removed.

[0022] (2.2) Open the inlet valve to introduce high-purity target gas, control the flow meter to stabilize the high-precision pressure gauge in the range of +50~100Pa micro-positive pressure, and then fine-tune the outlet valve to fully open so that the sample is in the target gas environment.

[0023] (3) Process heating treatment

[0024] According to the quenching requirements of the sample, the target heating temperature, heating rate and holding time are set by the temperature controller of the tube furnace, and then the power supply of the tube furnace is turned on to heat.

[0025] (4) Quenching operation

[0026] (4.1) Three minutes before the end of heating, use a syringe to inject the predetermined quenching medium into the quenching medium injection port of the quenching tank, and the injection volume should completely cover the expected landing area of ​​the sample.

[0027] (4.2) When heating is finished, quickly push the handle of the sample tank with the long handle to move it from the heating zone to directly above the quenching tank, and then rotate the handle 180° so that the sample falls vertically into the quenching medium of the quenching tank under the action of gravity.

[0028] (5) Sample recovery and post-processing

[0029] Close the air inlet valve, loosen the locking device, remove the quenching tank, and perform subsequent processing on the sample as needed.

[0030] The positive effects of this utility model are:

[0031] (1) The in-situ atmosphere quenching tube furnace of this utility model isolates air throughout the entire process to achieve the preparation of ultra-high purity materials. Through the complete sealing integration of the heating zone, transfer channel and quenching pool, the sample is always in an inert gas (such as Ar, N2) or reducing gas (such as H2 / Ar mixture) protective atmosphere during the heating, transfer and quenching process, eliminating the risk of material oxidation and contamination.

[0032] (2) The in-situ atmosphere quenching tube furnace described in this utility model breaks through the limitations of sensitive material processing and expands the application scope: it supports the quenching treatment of materials that are extremely sensitive to oxygen, water and carbon dioxide, and solves the problem of material decomposition caused by short-term air exposure in traditional open or semi-closed equipment.

[0033] (3) This utility model achieves full-process atmosphere protection for nanomaterials from high-temperature treatment to ultra-fast cooling through a fully sealed operation chain and precise timing control, effectively suppressing grain boundary oxidation and element segregation. Attached Figure Description

[0034] Figure 1 This is a schematic diagram of the structure of the in-situ atmosphere quenching tube furnace described in this utility model;

[0035] Figure 2 A schematic diagram of a sample well with a long handle passing through a T-shaped tee;

[0036] Figure 3 This is a schematic diagram of the furnace tube structure;

[0037] Figure 4 This is a schematic diagram of the quenching tank.

[0038] Figure 5 A sample image of the quenching tank interface;

[0039] Figure 6 This is a picture of the actual headspace high-temperature resistant rubber gasket cover;

[0040] Figure 7 This is a prototype image of the quenching tank;

[0041] Figure 8 This is a picture of a spring clamp type sealing clip.

[0042] Figure 9 Images of various types of clamps;

[0043] The components include: 1. Furnace body; 2. Furnace tube; 3. T-type tee; 4. Sample tank with long handle; 5. Quenching pool interface; 6. Quenching pool; 7. Gas outlet; 8. Hose; 9. High-precision pressure gauge; 10. Inlet valve; 11. Outlet valve; 12. Locking device; 13. Quenching medium injection port; 14. Headspace high-temperature resistant rubber gasket cover; 15. Sealing cover; 16. High-purity gas source; 17. Lifting platform; 18. First sealing flange; 19. Second sealing flange. Detailed Implementation

[0044] The present invention will be further described below with reference to the embodiments.

[0045] The in-situ atmosphere quenching tube furnace of this invention, through a fully enclosed design, ensures that the sample is always under the protection of the target gas during the heating, transfer and quenching process. It solves the problems of material oxidation and compositional segregation caused by atmosphere interruption and open quenching medium in traditional quenching processes. It is especially suitable for the quenching preparation of nano-metals and compounds that are sensitive to oxygen and water vapor.

[0046] The sample trough 4 of the in-situ atmosphere quenching tube furnace of this invention uses a long-handled metal spoon (stainless steel, molybdenum alloy, etc.) or a quartz spoon, depending on the properties of the quenched sample. Quartz troughs are preferred for metallic materials or easily oxidized samples, while long-handled metal troughs can be used for conventional alloys or non-reactive materials. The sample trough 4 has a recessed sample-carrying structure to prevent sample spillage and can move horizontally and rotate 180° within the furnace tube 2. The furnace tube 2 is made of high-temperature resistant quartz tube, with a temperature resistance ≥1200℃ and a diameter of 50-100mm. It has a branch for the quenching pool interface 5, used to connect to the quenching pool 6. A locking device 12 connects and locks the quenching pool interface 5 to the interface of the quenching pool 6 to ensure the stability and safety of the gas atmosphere during quenching. The heating system is used to heat the sample to the required temperature. This utility model uses a tubular furnace equipped with a temperature controller with an accuracy of ±1℃ and a power switch for precise temperature control. The furnace contains heating elements, such as K-type thermocouples; these components remain unchanged and will not be detailed further in this utility model. The quenching section uses a quenching pool 6 with a quenching medium injection port 13. The quenching pool 6 is a quartz cup container, and its diameter is the same as the diameter of the quartz tube branch quenching pool interface 5. The high-temperature resistant quartz tube in the quenching pool 6 and interface 5 can be sealed together. The quenching medium injection port 13 is equipped with a sealed headspace high-temperature resistant rubber gasket 14, allowing the injection of quenching media such as water, organic solvents, and salt solutions using a syringe. The second sealing flange 19 is a standard flange with an exhaust valve 11, the end of which can be connected to a plastic hose 8 for connecting a vacuum pump or exporting gas. The high-purity target gas mentioned in this utility model includes Ar, N2, or a H2 / Ar mixture.

[0047] This invention successfully constructs a fully enclosed nanomaterial quenching platform. It adopts a sealed linkage structure between the branched quartz tube and the quenching pool 6, breaking through the limitations of traditional open quenching. It realizes oxygen-free operation of the entire process from high-temperature treatment to rapid cooling of materials, and is particularly suitable for the preparation of novel nanomaterials that are sensitive to surface states. It provides reliable equipment support for the development of high-performance nanomaterials.

[0048] Example 1

[0049] An in-situ atmosphere quenching tube furnace, see Figures 1-9 The furnace includes a high-temperature furnace body 1, through which a furnace tube 2, longer than the furnace body 1, passes. A T-shaped tee 3 is connected to the front end of the furnace tube 2. A sample groove 4 with a long handle is arranged horizontally inside the T-shaped tee 3. The T-shaped tee 3 is a gas inlet in the vertical direction. A quenching pool interface 5 is vertically arranged at the rear of the furnace tube 2. A quenching pool 6 is connected below the quenching pool interface 5. The rear end of the furnace tube 2 is a gas outlet 7. The gas outlet 7 is connected to a flexible hose 8 for connecting a vacuum pump or for exporting gas.

[0050] The air inlet end is equipped with a high-precision pressure gauge 9 and an air inlet valve 10, arranged sequentially from bottom to top; the air outlet end 7 is equipped with an air outlet valve 11. The interface surfaces of the quenching pool interface 5 and the quenching pool 6 are both frosted surfaces, which can be sealed by applying a small amount of Vaseline. The quenching pool interface 5 and the quenching pool 6 are sealed together by a locking device 12, achieving a leak-free connection between the furnace tube 2 and the quenching pool 6. The length of the sample slot opening at the front end of the sample slot 4 with the long handle is less than the diameter of the quenching pool interface 5. The locking device 12 is a clamp or spring clamp type sealing clip. A quenching medium injection port 13 is provided on the upper side wall of the quenching pool 6, and a spiral-connected headspace high-temperature resistant rubber gasket cover 14 is installed on the quenching medium injection port 13. The T-shaped tee 3 has a sealing cap 15 at its horizontal front end. The long handle of the sample groove 4 passes through the central hole of the sealing cap 15 and can rotate freely. O-rings are provided on the inner side of the contact point between the long handle of the sample groove 4 and the sealing cap 15. The length of the sample groove 4 is greater than or equal to the length of the furnace tube 2. The long handle of the sample groove 4 has positioning scale lines corresponding to the uniform temperature zone in the middle of the furnace tube 2. The gas inlet is connected to a high-purity gas source 16. The rear end of the T-shaped tee 3 is connected to the front end of the furnace tube 2 through a first sealing flange 18. The gas outlet 7 is connected to the rear end of the furnace tube 2 through a second sealing flange 19 and is sealed. A lifting platform 17 for auxiliary support of the quenching tank 6 is provided below the quenching tank 6.

[0051] Example 2

[0052] An in-situ atmosphere quenching tube furnace includes a high-temperature furnace body 1, through which a furnace tube 2, longer than the furnace body 1, is passed. A T-shaped tee 3 is connected to the front end of the furnace tube 2. A sample groove 4 with a long handle is arranged horizontally inside the T-shaped tee 3. The T-shaped tee 3 is a gas inlet in the vertical direction. A quenching pool interface 5 is vertically arranged at the rear of the furnace tube 2. A quenching pool 6 is connected below the quenching pool interface 5. The rear end of the furnace tube 2 is a gas outlet 7. The gas outlet 7 is connected to a flexible hose 8 for connecting a vacuum pump or for exporting gas.

[0053] Example 3

[0054] An in-situ atmosphere quenching tube furnace includes a high-temperature furnace body 1, through which a furnace tube 2, longer than the furnace body 1, is passed. A T-shaped tee 3 is connected to the front end of the furnace tube 2. A sample groove 4 with a long handle is arranged horizontally inside the T-shaped tee 3. The T-shaped tee 3 is a gas inlet in the vertical direction. A quenching pool interface 5 is vertically arranged at the rear of the furnace tube 2. A quenching pool 6 is connected below the quenching pool interface 5. The rear end of the furnace tube 2 is a gas outlet 7. The gas outlet 7 is connected to a flexible hose 8 for connecting a vacuum pump or for exporting gas.

[0055] The upper sidewall of the quenching pool 6 is provided with a quenching medium injection port 13, and a top-hollow high-temperature resistant rubber gasket cover 14 with a spiral structure is installed on the quenching medium injection port 13.

[0056] Example 4

[0057] An in-situ atmosphere quenching tube furnace includes a high-temperature furnace body 1, through which a furnace tube 2, longer than the furnace body 1, is passed. A T-shaped tee 3 is connected to the front end of the furnace tube 2. A sample groove 4 with a long handle is arranged horizontally inside the T-shaped tee 3. The T-shaped tee 3 is a gas inlet in the vertical direction. A quenching pool interface 5 is vertically arranged at the rear of the furnace tube 2. A quenching pool 6 is connected below the quenching pool interface 5. The rear end of the furnace tube 2 is a gas outlet 7. The gas outlet 7 is connected to a flexible hose 8 for connecting a vacuum pump or for exporting gas.

[0058] The air inlet end is equipped with a high-precision pressure gauge 9 and an air inlet valve 10, arranged sequentially from bottom to top; the air outlet end 7 is equipped with an air outlet valve 11. The interface surfaces of the quenching pool interface 5 and the quenching pool 6 are both frosted surfaces, and the quenching pool interface 5 and the quenching pool 6 are sealed together by a locking device 12; the length of the sample slot opening at the front end of the sample slot 4 with the long handle is less than the diameter of the quenching pool interface 5. The locking device 12 is a clamp or spring clamp type sealing clip. A quenching medium injection port 13 is provided on the upper side wall of the quenching pool 6, and a spiral-connected headspace high-temperature resistant rubber gasket cover 14 is installed on the quenching medium injection port 13.

[0059] Example 5

[0060] An in-situ atmosphere quenching tube furnace includes a high-temperature furnace body 1, through which a furnace tube 2, longer than the furnace body 1, is passed. A T-shaped tee 3 is connected to the front end of the furnace tube 2. A sample groove 4 with a long handle is arranged horizontally inside the T-shaped tee 3. The T-shaped tee 3 is a gas inlet in the vertical direction. A quenching pool interface 5 is vertically arranged at the rear of the furnace tube 2. A quenching pool 6 is connected below the quenching pool interface 5. The rear end of the furnace tube 2 is a gas outlet 7. The gas outlet 7 is connected to a flexible hose 8 for connecting a vacuum pump or for exporting gas.

[0061] The air inlet end is equipped with a high-precision pressure gauge 9 and an air inlet valve 10, arranged sequentially from bottom to top; the air outlet end 7 is equipped with an air outlet valve 11. The interface surfaces of the quenching pool interface 5 and the quenching pool 6 are both frosted surfaces, and the quenching pool interface 5 and the quenching pool 6 are sealed together by a locking device 12; the length of the sample slot opening at the front end of the sample slot 4 with the long handle is less than the diameter of the quenching pool interface 5. The locking device 12 is a clamp or spring clamp type sealing clip. A quenching medium injection port 13 is provided on the upper side wall of the quenching pool 6, and a spiral-connected headspace high-temperature resistant rubber gasket cover 14 is installed on the quenching medium injection port 13. The T-shaped tee 3 has a sealing cap 15 at its horizontal front end. The long handle of the sample groove 4 passes through the central hole of the sealing cap 15 and can rotate freely. O-rings are provided on the inner side of the contact point between the long handle of the sample groove 4 and the sealing cap 15. The length of the sample groove 4 is greater than or equal to the length of the furnace tube 2. The long handle of the sample groove 4 has positioning scale lines corresponding to the uniform temperature zone in the middle of the furnace tube 2. The gas inlet is connected to a high-purity gas source 16. The rear end of the T-shaped tee 3 is connected to the front end of the furnace tube 2 through a first sealing flange 18. The gas outlet 7 is connected to the rear end of the furnace tube 2 through a second sealing flange 19 and is sealed.

[0062] Example 6

[0063] A quenching method for an in-situ atmosphere quenching tube furnace includes the following steps:

[0064] (1) Sample loading and sealing assembly

[0065] (1.1) Spread the sample to be processed evenly in the sample trough 4 with a long handle to avoid accumulation;

[0066] (1.2) Install the furnace tube 2 horizontally inside the furnace body 1 of the in-situ atmosphere quenching tube furnace. Pass the long handle end of the sample groove 4 with the long handle through the center hole of the first sealing flange 18, T-type tee 3, O-ring seal and sealing cover 15 in sequence. Fix the sealing cover 15 to the front end of the T-type tee 3 in the horizontal direction by tightening the thread. Connect and fix the rear end of the T-type tee 3 to the front end of the furnace tube 2 through the first sealing flange 18.

[0067] (1.3) Push the sample tank 4 with a long handle and observe the positioning scale line on the long handle of the sample tank 4 until the sample tank 4 containing the sample is in the uniform temperature zone in the middle of the furnace tube 2. Connect and fix the gas outlet 7 to the rear end of the furnace tube 2 through the second sealing flange 19. Finally, connect and lock the interface 5 of the quenching pool to the interface of the quenching pool 6 with the locking device 12. Tighten the headspace high temperature resistant rubber gasket cover 14 on the quenching medium injection port 13. Place the lifting platform 17 below the quenching pool 6 to assist in supporting the quenching pool 6. The gas inlet is connected to the high purity gas source 16. The gas outlet 7 is connected to the hose 8 used to connect the vacuum pump or the gas outlet. Close the gas inlet valve 10 and the gas outlet valve 11 to complete the construction of the fully enclosed system.

[0068] (2) Gas atmosphere control

[0069] (2.1) Connect the outlet 7 to the vacuum pump through the hose 8. After starting the vacuum pump, slowly open the outlet valve 11 to the half-open state, evacuate the system and monitor the pressure in the system through the high-precision pressure gauge 9 until it is ≤10Pa. Close the outlet valve 11 and maintain it for 3 minutes to confirm that the pressure does not rise. Verify that the airtightness meets the standard. Disconnect the vacuum pump and repeat the evacuation three times to ensure that the residual gas in the cavity is completely removed.

[0070] (2.2) Open the inlet valve 10 and introduce high-purity target gas inert gas (such as Ar, N2) or reducing gas (such as H2 / Ar mixture). Control the flow meter to stabilize the high-precision pressure gauge 9 in the range of +50 to 100 Pa micro-positive pressure. Then fine-tune the outlet valve 11 to fully open so that the sample is in the target gas environment.

[0071] (3) Process heating treatment

[0072] According to the quenching requirements of the sample, the heating and holding programs are set through the temperature controller of the tube furnace: input the target temperature (e.g., 800~1200℃), heating rate (e.g., 10℃ / min) and holding time (e.g., 30min), and then start the power supply of the tube furnace to heat.

[0073] (4) Quenching operation

[0074] (4.1) Three minutes before the end of heating, use a syringe to inject the predetermined quenching medium (such as water, liquid nitrogen, silicone oil, etc.) into the quenching medium injection port 13 of the quenching tank 6, and the injection volume completely covers the expected landing area of ​​the sample.

[0075] (4.2) When heating is finished, quickly push the handle of the sample tank 4 with the long handle to move it from the heating zone to directly above the quenching tank 6, and then rotate the handle 180° so that the sample falls vertically into the quenching medium of the quenching tank 6 under the action of gravity.

[0076] (5) Sample recovery and post-processing

[0077] Close the air inlet valve 10, loosen the locking device 12, remove the quenching tank 6, and perform subsequent processing on the sample as needed.

[0078] The in-situ atmosphere quenching tube furnace of this invention employs a fully enclosed design to ensure that the sample remains in the target gas environment (such as inert gas) throughout the heating and quenching process, preventing contact with outside air and completely solving the oxidation or contamination problems caused by insufficient sealing in traditional equipment. It also features a movable and tiltable sample tank within the enclosed environment, enabling separation of the sample from the tank during quenching. In this invention, the quenching medium is placed in a sealed quenching pool and added via a syringe, achieving sterile / oxygen-free addition of the quenching medium.

[0079] Other embodiments of this application will readily conceive of by those skilled in the art upon consideration of the specification and practice of the disclosure herein. This application is intended to cover any variations, uses, or adaptations of this application that follow the general principles of this application and include common knowledge or customary techniques in the art not disclosed herein. The specification and embodiments are to be considered exemplary only, and this application is not limited to the precise structures described above and shown in the accompanying drawings, and various modifications and changes can be made without departing from its scope.

Claims

1. An in-situ atmosphere quenching tube furnace, comprising a high-temperature furnace body (1), wherein a furnace tube (2) with a length greater than that of the furnace body (1) passes through the high-temperature furnace body (1), characterized in that: The front end of the furnace tube (2) is connected to a T-shaped tee (3). A sample groove (4) with a long handle is provided in the horizontal direction of the T-shaped tee (3). The vertical direction of the T-shaped tee (3) is the air inlet end. The rear part of the furnace tube (2) is vertically provided with a quenching pool interface (5). A quenching pool (6) is connected below the quenching pool interface (5). The rear end of the furnace tube (2) is the air outlet end (7). The air outlet end (7) is connected to a hose (8) for connecting a vacuum pump or exporting gas.

2. The in-situ atmosphere quenching tube furnace according to claim 1, characterized in that: The air inlet end is provided with a high-precision air pressure gauge (9) and an air inlet valve (10) from bottom to top; the air outlet end (7) is provided with an air outlet valve (11).

3. The in-situ atmosphere quenching tube furnace according to claim 1, characterized in that: The interface surfaces of the quenching pool interface (5) and the quenching pool (6) are both frosted surfaces. The quenching pool interface (5) and the quenching pool (6) are sealed together by a locking device (12). The length of the sample slot at the front end of the sample slot (4) with a long handle is less than the diameter of the quenching pool interface (5).

4. The in-situ atmosphere quenching tube furnace according to claim 3, characterized in that: The locking device (12) is a clamp or spring clamp type sealing clip.

5. The in-situ atmosphere quenching tube furnace according to claim 1, characterized in that: The upper side wall of the quenching pool (6) is provided with a quenching medium injection port (13), and a top-hollow high-temperature resistant rubber gasket cover (14) with a spiral structure is installed on the quenching medium injection port (13).

6. The in-situ atmosphere quenching tube furnace according to claim 1, characterized in that: The T-shaped tee (3) is provided with a sealing cap (15) at the front end in the horizontal direction. The long handle of the sample groove (4) with a long handle passes through the central hole of the sealing cap (15) and can rotate freely. The inner side of the contact point between the long handle of the sample groove (4) with the sealing cap (15) is provided with an O-ring. The length of the sample groove (4) with a long handle is ≥ the length of the furnace tube (2). The long handle of the sample groove (4) with a long handle is provided with a positioning scale line corresponding to the uniform temperature zone in the middle of the furnace tube (2).

7. The in-situ atmosphere quenching tube furnace according to claim 1, characterized in that: The air inlet is connected to a high-purity gas source (16).

8. The in-situ atmosphere quenching tube furnace according to claim 1, characterized in that: A lifting platform (17) for auxiliary support of the quenching pool (6) is provided below the quenching pool (6).

9. The in-situ atmosphere quenching tube furnace according to claim 1, characterized in that: The rear end of the T-shaped tee (3) is connected to the front end of the furnace tube (2) through the first sealing flange (18); the gas outlet (7) is connected to the rear end of the furnace tube (2) through the second sealing flange (19) and sealed.

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