Hydrogen adsorption vacuum heat treatment device, system and application method for LaFeSi-based materials

Abstract

To provide a hydrogen adsorption vacuum heat treatment device, a system, and an application method for LaFeSi system material.SOLUTION: A device is provided with a furnace body, a furnace pipe, an in-furnace pipe module, first cooling fluid pipings, second cooling fluid pipings, a cooling fluid supply device, and a vacuum extractor. The furnace pipe is provided with a furnace pipe body, a buffle plate valve, and a furnace pipe buffle plate. The in-furnace pipe module is provided with a sample chamber, a connecting rod, a heat insulation sheet, and a heat insulation plate.SELECTED DRAWING: Figure 1

Description

[Technical Field]

[0001] The present invention relates to a hydrogen adsorption vacuum heat treatment apparatus, system and application method for LaFeSi-based materials. [Background technology]

[0002] LaFeSi-based magnetic refrigeration materials are a new type of magnetic refrigeration material with a high magnetic entropy change temperature and low magnetic permeability, making them one of the current research hotspots. However, their Curie temperature is lower than room temperature. After hydrogenation, the Curie temperature of LaFeSi-based magnetic refrigeration materials can be raised above room temperature, while at the same time exhibiting a large isothermal magnetic entropy change.

[0003] Patent document CN208604168U discloses a vacuum heat treatment furnace equipped with a spiral water cooling system, including pipes, vacuum piping, a mounting box, a water storage tank, a condenser, a pumping pump, connecting piping, metal hoses, a metal spiral pipe, and support fixtures. The pipes are connected to the vacuum piping. The vacuum piping is fixed to the exterior of the mounting box by support fixtures, the water storage tank is fixed to the interior of the mounting box, and the condenser is fixed to the exterior of the mounting box. The water storage tank is connected to the first water outlet of the condenser and the water inlet of the pumping pump by connecting piping. The metal spiral pipe is installed on the outer wall of the vacuum piping, and one end of the metal spiral pipe is connected to the first water inlet of the condenser and the other end is connected to a metal hose, the other end of which is connected to the water outlet of the pumping pump. The pumping pump is fixed on top of the mounting box, and the water inlet of the pumping pump is connected to the connecting piping. This application only relates to a portion of the furnace body's external structure.

[0004] CN216514003U discloses a heat treatment apparatus for metal components, which includes a heat treatment furnace for placing metal components therein and performing heat treatment, an ammonia decomposer for decomposing an ammonia to produce hydrogen gas and nitrogen gas, a ventilation pipe connected between the ammonia decomposer and the heat treatment furnace for introducing a mixed gas of hydrogen gas and nitrogen gas into the heat treatment furnace to replace the air inside the heat treatment furnace (the ventilation pipe is equipped with a replacement valve that controls the opening and closing of the pipe), and an ignition nozzle attached to the heat treatment furnace, which passes through the heat treatment furnace to the outside and exhausts the gas inside the heat treatment furnace, stabilizing the mixed gas of hydrogen gas and nitrogen gas inside the heat treatment furnace, and then igniting the overflowing hydrogen gas. The apparatus is used for oxidation-reduction of the surface of a metal component. Summary of the Invention

[0005] In view of this, one object of the present invention is to provide a hydrogen adsorption vacuum heat treatment apparatus that can be used for hydrogen adsorption treatment of LaFeSi-based materials. Furthermore, the apparatus can make the flow of hydrogen gas more stable and uniform, improving the hydrogen adsorption effect. Furthermore, the apparatus can reduce the high-temperature impact on the elastic seal of the furnace tube, extending its service life and improving the vacuum effect. Another object of the present invention is to provide a hydrogen adsorption vacuum heat treatment system. Furthermore, another object of the present invention is to provide an application method for the hydrogen adsorption vacuum heat treatment system. The application method can improve the vacuum effect and the hydrogen adsorption effect of LaFeSi-based materials.

[0006] The present invention achieves the above object by adopting the following configuration.

[0007] The present invention provides a furnace including a furnace body, a furnace tube, a module in the furnace tube, a first cooling fluid pipe, a second cooling fluid pipe, a cooling fluid supply device, and a vacuum extraction device, The furnace body is used to heat a furnace tube; the furnace tube comprises a furnace tube body, a baffle plate valve, and a furnace tube baffle plate, both ends of the furnace tube body are open, and the furnace tube body comprises a first furnace tube body section, a second furnace tube body section, and a third furnace tube body section, which are connected in order to the furnace tube body, the second furnace tube body section being located inside the furnace body, and the first furnace tube body section and the third furnace tube body section being located outside the furnace body; the baffle plate valve is sealed at the open end of the first furnace tube body by an elastic seal, a first pipe joint and a second pipe joint are disposed on the baffle plate valve, the first pipe joint is used to connect with a hydrogen gas supply device, and the second pipe joint is used to connect with an inert gas supply device; the furnace tube baffle plate is sealed at the open end of the third furnace tube body portion by an elastic seal; the furnace tube internal module comprises a sample chamber, a connecting rod, a heat insulating sheet, and a heat insulating plate; the sample chamber comprises a sample chamber body and a chamber baffle plate, both ends of the sample chamber body are open ends, the chamber baffle plate is covered on the open end of the sample chamber body, at least a part of the chamber baffle plate is formed of foam metal, the sample chamber body comprises a first chamber body and a second chamber body, the first chamber body and the second chamber body are connected in an assembled manner, One end of the connecting rod is connected to one end of the sample chamber, and the connecting rod extends from the end connected to the sample chamber in a direction away from the sample chamber; the connecting rod passes through the insulating plate, and the insulating plate is disposed near one end of the connecting rod that is remote from the sample chamber; the connecting rod penetrates the heat insulating sheet, the heat insulating sheet is disposed between the sample chamber and the heat insulating plate, and an air vent is disposed in the heat insulating sheet; the first cooling fluid piping is configured to cool the first furnace tube body, and the first cooling fluid piping is connected to the cooling fluid supply device; the second cooling fluid piping is configured to cool the third furnace tube body, and the second cooling fluid piping is connected to the cooling fluid supply device; The hydrogen adsorption vacuum heat treatment apparatus for LaFeSi-based materials is provided, wherein the vacuum extraction device is connected to the furnace tube and is used to suck out gas in the furnace tube.

[0008] According to the hydrogen adsorption vacuum heat treatment apparatus of the present invention, preferably, the furnace body comprises a first furnace body and a second furnace body, and the first furnace body and the second furnace body are configured to be able to move along the radial direction of the furnace tube, and the first furnace body and the second furnace body move in opposite directions.

[0009] According to the hydrogen adsorption vacuum heat treatment apparatus of the present invention, preferably, the hydrogen adsorption vacuum heat treatment apparatus further includes an electric machine, a running track, and a running support, The electric machine is configured to drive the traveling support to move; A slider that matches the running track is disposed on the running support; The running track and the slider are configured to limit the movement path of the running support; The traveling support includes a first traveling support and a second traveling support, the first traveling support is connected to the first furnace body, and the second traveling support is connected to the second furnace body.

[0010] In the hydrogen adsorption vacuum heat treatment apparatus according to the present invention, it is preferable that the thermal conductivity of the material forming the first furnace tube main body is greater than the thermal conductivity of the material forming the second furnace tube main body, and that the thermal conductivity of the material forming the third furnace tube main body is greater than the thermal conductivity of the material forming the second furnace tube main body.

[0011] In the hydrogen adsorption vacuum heat treatment apparatus according to the present invention, it is preferable that the baffle plate valve further includes a vacuum gauge and a pressure transmitter.

[0012] According to the hydrogen adsorption vacuum heat treatment apparatus of the present invention, preferably, the vacuum extraction device includes a main pipe, a first control valve, a second control valve, a first branch, a metal oil diffusion pump, a third control valve, a second branch, a third branch, a Roots vacuum pump, and a rotary vane vacuum pump; One end of the main pipe is connected to the baffle plate valve, the other end of the main pipe is connected to a second control valve, and a first control valve is disposed in the main pipe; One end of the first branch is connected to the first control valve, and the other end of the first branch is connected to the vent inlet end of the metal oil diffusion pump; One end of the second branch is connected to the vent outlet end of the metal oil diffusion pump, the other end of the second branch is connected to the second control valve, and a third control valve is disposed in the second branch; One end of the third branch is connected to a portion of the second branch located between the second control valve and the third control valve, and the other end of the third branch is connected to the vent inlet end of the Roots vacuum pump and the vent inlet end of the rotary vane vacuum pump, respectively.

[0013] In the hydrogen adsorption vacuum heat treatment apparatus according to the present invention, it is preferable that an electric resistance vacuum gauge and an ionization vacuum gauge are disposed in the main pipe between the baffle plate valve and the first control valve.

[0014] In the hydrogen adsorption vacuum heat treatment apparatus according to the present invention, preferably, the first control valve comprises an air-operated baffle plate valve and an electromagnetic valve, the second control valve comprises an air-operated baffle plate valve and an electromagnetic valve, and the third control valve comprises an air-operated baffle plate valve and an electromagnetic valve; The cooling fluid supply device includes a chiller and a water tank, the water tank configured to supply a water source to the chiller, the chiller configured to cool water, and the chiller connected to the first cooling fluid piping and the second cooling fluid piping, respectively.

[0015] On the other hand, the present invention provides a hydrogen adsorption vacuum heat treatment apparatus comprising the above-mentioned hydrogen adsorption vacuum heat treatment apparatus, a control table, a hydrogen gas supply device, and an inert gas supply device, the control platform is configured to control the hydrogen adsorption vacuum heat treatment device; A hydrogen adsorption vacuum heat treatment system for LaFeSi-based materials is provided, in which the hydrogen gas supply device is connected to the first piping joint, and the inert gas supply device is connected to the second piping joint.

[0016] The present invention also provides a method for producing a method for manufacturing a semiconductor device, comprising the steps of: (1) With the LaFeSi-based material placed in the sample chamber and the furnace tube module positioned inside the furnace tube, the baffle plate valve is closed, the rotary vane vacuum pump, the first control valve, and the second control valve are opened to evacuate the gas in the main pipe to a pressure of 20 Pa or less, and then the Roots vacuum pump is turned on to evacuate the gas in the main pipe to a pressure of 10 Pa or less. -2 evacuating the chamber to a pressure of less than 1 Pa; (2) After heating the metal oil diffusion pump for 15 to 60 minutes, open the baffle plate valve and the third control valve, close the second control valve, evacuate the gas in the furnace tube to a pressure of 0.1 Pa or less, and then turn off the metal oil diffusion pump, the Roots vacuum pump and the rotary vane vacuum pump; (3) With the first furnace body and the second furnace body closed, turn on the heating device of the furnace body to raise the furnace tube temperature to 250-360°C; (4) Close the first control valve and the baffle plate valve, turn on the hydrogen gas supply device, set the pressure in the furnace tube to 110~150kPa, maintain the temperature and pressure for 170~250 minutes, then turn off the heating device of the furnace body, keep the pressure constant, move the first furnace body and the second furnace body along the diameter of the furnace tube, keep the first furnace body and the second furnace body open, and then cool for 100~150 minutes; (5) The hydrogen gas supply device controls the amount of hydrogen gas introduced into the furnace tube, and after the pressure in the furnace tube is set to 80-120 kPa, the baffle plate valve, rotary vane vacuum pump, first control valve and second control valve are opened to evacuate the gas in the main pipe and furnace tube to a pressure of 0.001 Pa or less, and then the Roots vacuum pump is turned on to evacuate the gas in the main pipe and furnace tube; (6) Turn off the first control valve, the second control valve, the baffle plate valve, the rotary vane vacuum pump and the Roots vacuum pump, turn on the inert gas supply device, and make the pressure in the furnace tube 80-120 kPa. Then, open the baffle plate valve, the rotary vane vacuum pump, the first control valve and the second control valve to evacuate the gas in the main pipe to a pressure of 0.001 Pa or less, then turn on the Roots vacuum pump and evacuate the gas in the main pipe. (7) repeating step (6) to vent the hydrogen gas; The present invention also provides an application method for the hydrogen adsorption vacuum heat treatment system, including:

[0017] The hydrogen adsorption vacuum heat treatment device of the present invention can be applied to the hydrogen adsorption treatment of LaFeSi-based materials, which can make the hydrogen gas flow more stable and uniform, improve the hydrogen adsorption effect, reduce the high temperature impact on the elastic seal of the furnace tube, extend the service life, and improve the vacuum effect. [Brief explanation of the drawings]

[0018] [Figure 1] 1 is a schematic diagram showing the layout of a hydrogen adsorption vacuum heat treatment apparatus according to the present invention; [Figure 2] FIG. 2 is a schematic diagram showing the first furnace body and the second furnace body in a closed state. [Figure 3] FIG. 1 is a schematic diagram showing the first furnace body and the second furnace body in an open state. [Figure 4] FIG. 2 is a schematic diagram of one baffle plate valve. [Figure 5] FIG. 2 is a schematic diagram of one furnace tube module. [Figure 6] FIG. 2 is a schematic diagram of one chamber baffle plate. [Figure 7] FIG. 2 is a schematic diagram of one heat insulating sheet. [Figure 8] FIG. 1 is a schematic diagram of one vacuum extraction device. [Explanation of symbols]

[0019] 1 - furnace body, 101 - first furnace body, 102 - second furnace body, 201 - furnace tube body, 202 - baffle plate valve, 2021 - first piping joint, 2022 - second piping joint, 2023 - vacuum gauge, 2024 - pressure transmitter, 203 - furnace tube baffle plate, 204 - pneumatic ball valve, 205 - elbow piping, 3011 - first chamber body, 3012 - second chamber body, 3013 - chamber baffle plate, 302 - insulation sheet, 3021 - vent, 303 - insulation plate, 304 - flange, 305 - connecting Rod, 4 - furnace tube support seat, 401 - support part, 402 - connecting part, 5 - furnace body support, 601 - chiller, 602 - water tank, 701 - main piping, 702 - first control valve, 703 - second control valve, 704 - first branch, 705 - metal oil diffusion pump, 706 - third control valve, 707 - second branch, 708 - third branch, 709 - Roots vacuum pump, 710 - rotary vane vacuum pump, 711 - electrical resistance vacuum gauge, 712 - ionization vacuum gauge, 713 - fourth control valve, 8 - lateral movement mechanism support, 901 - first traveling support, 902 - second traveling support. DETAILED DESCRIPTION OF THE INVENTION

[0020] The present invention will be further described below with reference to specific examples, but the scope of the present invention is not limited to these examples.

[0021] <Hydrogen adsorption vacuum heat treatment device> The hydrogen adsorption vacuum heat treatment apparatus of the present invention includes a furnace body, a furnace tube, a furnace tube internal module, a first cooling fluid piping, a second cooling fluid piping, a cooling fluid supply device, and a vacuum extraction device. In some embodiments, the apparatus further includes a furnace tube support seat, a furnace body support, and a furnace body lateral movement mechanism.

[0022] Furnace body and furnace body lateral movement mechanism The furnace body is used to heat the furnace tube. A heating device is disposed in the furnace body. The heating device may be a heating electric resistance. A thermocouple and a thermocouple insulation layer may be disposed in the furnace body. This makes it possible to detect the temperature of the furnace body.

[0023] The furnace body may include a first furnace body and a second furnace body. The first furnace body and the second furnace body are configured to be movable along the diameter of the furnace tube, and the first furnace body and the second furnace body move in opposite directions. In this way, the first furnace body and the second furnace body can be opened during cooling to increase the cooling rate of the furnace tube. The movement paths of the first furnace body and the second furnace body can be restricted by using movable rails and sliders.

[0024] In some embodiments, the furnace body lateral movement mechanism comprises an electric motor, a travel track, and a travel support. The electric motor is configured to drive the travel support for movement. It may be used in the form of a chain drive. The travel support is provided with a slider that matches the travel track. The travel track and the slider are configured to limit the movement path of the travel support. The travel track may be disposed within the lateral movement mechanism support. The lateral movement mechanism support is disposed through the furnace body support. The travel support comprises a first travel support and a second travel support. The first travel support is connected to the first furnace body. The second travel support is connected to the second furnace body.

[0025] furnace tube The furnace tube of the present invention comprises a furnace tube body, a baffle plate valve, and a furnace tube baffle plate.

[0026] Both ends of the furnace tube body are open. The furnace tube body comprises a first furnace tube body section, a second furnace tube body section, and a third furnace tube body section, which are connected in order. The second furnace tube body section is located inside the furnace body. The first furnace tube body section and the third furnace tube body section are located outside the furnace body. The furnace tube body has an integral structure.

[0027] The baffle plate valve is sealed at the open end of the first furnace tube body by an elastic seal. The elastic seal may be a rubber seal. The furnace tube baffle plate is sealed at the open end of the third furnace tube body by an elastic seal. The elastic seal may be a rubber seal. Although the elastic seal can improve the sealing performance of the furnace tube, it has poor heat resistance. Long-term exposure to high temperatures will affect the service life and sealing performance of the elastic seal. Therefore, it is necessary to cool the furnace tube body near the elastic seal.

[0028] In some embodiments, the thermal conductivity of the material forming the first furnace tube body is greater than the thermal conductivity of the material forming the second furnace tube body, and the thermal conductivity of the material forming the third furnace tube body is greater than the thermal conductivity of the material forming the second furnace tube body. In this manner, heat can be dissipated in time by the first furnace tube body and the third furnace tube body, reducing the temperature of the furnace tube body near the elastic seal. The first furnace tube body and the third furnace tube body may be formed from metallic aluminum. The second furnace tube body may be formed from stainless steel.

[0029] The baffle plate valve is provided with a first pipe fitting and a second pipe fitting. The first pipe fitting is used to connect to a hydrogen gas supply device. The second pipe fitting is used to connect to an inert gas supply device. In some embodiments, the baffle plate valve is further provided with a vacuum gauge and / or a pressure transmitter. The vacuum gauge is used to detect the pressure in the furnace tube body. The pressure transmitter is used to convert the pressure in the furnace tube body into an electrical signal.

[0030] In some embodiments, an air-operated ball valve is connected to the end of the baffle plate valve that is away from the furnace tube, thereby increasing the airtightness.

[0031] Furnace tube support seat and furnace body support The furnace tube support seat of the present invention is configured to support a furnace tube. The furnace tube support seat may include a support portion and a connecting portion.

[0032] The support has a hollow structure inside it that can accommodate cooling fluid piping, and the support is sleeved around the furnace tube body.

[0033] One end of the connecting part is connected to the bottom of the support part, and the other end is connected to the furnace body support, which is placed on the ground.

[0034] In some embodiments, two furnace tube support seats are provided, one of which has a support portion sleeved around the outer periphery of the first furnace tube body, preferably near the baffle plate valve, and the other of which has a support portion sleeved around the outer periphery of the third furnace tube body, preferably near the furnace tube baffle plate.

[0035] Furnace tube module The furnace tube module of the present invention comprises a sample chamber, a connecting rod, an insulating sheet, and an insulating plate. In some embodiments, it further comprises a flange.

[0036] The sample chamber comprises a sample chamber body and a chamber baffle plate. Both ends of the sample chamber body are open. The open ends of the sample chamber body are covered with the chamber baffle plate. At least a portion of the chamber baffle plate is formed from metal foam. This allows hydrogen gas to flow uniformly and smoothly into the sample chamber, contributing to improving the hydrogen adsorption effect.

[0037] The sample chamber body includes a first chamber body and a second chamber body. The first chamber body and the second chamber body are connected to each other in an assembled manner. In some embodiments, the first chamber body and the second chamber body are connected to each other using a locking connection method. This allows a plate-shaped or large-sized LaFeSi-based material to be easily placed in the sample chamber.

[0038] In use, a sample chamber is located within the second furnace tube body.

[0039] One end of the connecting rod is connected to one end of the sample chamber and extends away from the sample chamber. In some embodiments, the connecting rod is connected to the sample chamber by a flange. The flange is connected to the chamber baffle plate. The portion of the chamber baffle plate formed by the metal foam is not covered. The connecting rod is connected to the flange.

[0040] The connecting rod is passed through an insulating plate, and the insulating plate is located near one end of the connecting rod remote from the sample chamber.

[0041] The connecting rod passes through the heat insulating sheet, which is placed between the sample chamber and the heat insulating plate. Multiple heat insulating sheets may be installed. The heat insulating sheet has ventilation holes. This provides insulation, reduces the effect of high temperatures on the elastic seal, and does not affect the flow of gas.

[0042] Cooling fluid piping and cooling fluid supply device A first cooling fluid line is configured to cool the first furnace tube body, and in some embodiments, at least a portion of the first cooling fluid line is disposed within a cavity of a support sleeved around the first furnace tube body, and the first cooling fluid line is connected to a cooling fluid supply.

[0043] A second cooling fluid line is configured to cool the third furnace tube body, and in some embodiments, at least a portion of the second cooling fluid line is disposed within a cavity of the support sleeved around the periphery of the third furnace tube body, and the second cooling fluid line is connected to a cooling fluid supply.

[0044] The cooling fluid supply device may include a chiller and a water tank, the water tank configured to supply a source of water to the chiller, the chiller configured to chill the water, and the chillers connected to the first cooling fluid line and the second cooling fluid line, respectively.

[0045] vacuum extraction equipment The vacuum extractor of the present invention is connected to the furnace tube. The vacuum extractor is used to extract gas from the furnace tube and create a vacuum. The vacuum extractor can be connected to the baffle plate valve. In some embodiments, an air-operated ball valve is further disposed between the vacuum extractor and the baffle plate valve.

[0046] The axial vacuum system may include a main line, a first control valve, a second control valve, a first branch, a metal oil diffusion pump, a third control valve, a second branch, a third branch, a Roots vacuum pump, and a rotary vane vacuum pump.

[0047] One end of the main pipe is connected to the baffle plate valve, and the other end of the main pipe is connected to the second control valve, which includes an air-operated baffle plate valve and a solenoid valve.

[0048] A first control valve is disposed in the main pipe, and includes an air-operated baffle plate valve and a solenoid valve.

[0049] One end of the first branch is connected to the first control valve, and the other end of the first branch is connected to the vent inlet end of the metal oil diffusion pump.

[0050] One end of the second branch is connected to the vent outlet end of the metal oil diffusion pump, and the other end of the second branch is connected to the second control valve.

[0051] A third control valve is disposed in the second branch, the third control valve including an air-operated baffle plate valve and a solenoid valve.

[0052] One end of the third branch is connected to a portion of the second branch located between the second control valve and the third control valve, and the other ends of the third branch are connected to the vent inlet end of the Roots vacuum pump and the vent inlet end of the rotary vane vacuum pump, respectively.

[0053] In some embodiments, the vacuum extraction device may further comprise an electrical resistance gauge and / or an ionization gauge.

[0054] An electrical resistance vacuum gauge and / or an ionization vacuum gauge may be disposed in the main pipe between the baffle plate valve and the first control valve, and the electrical resistance vacuum gauge and / or the ionization vacuum gauge is used to measure the vacuum level in the main pipe.

[0055] In some embodiments, the vacuum extraction device may further include a fourth control valve. The fourth control valve may be disposed in the main line between the first control valve and the second control valve. The fourth control valve may be a solenoid valve.

[0056] <Hydrogen adsorption vacuum heat treatment system> The hydrogen adsorption vacuum heat treatment system of the present invention comprises a hydrogen adsorption vacuum heat treatment device, a control table, a hydrogen gas supply device, and an inert gas supply device. The details of the hydrogen adsorption vacuum heat treatment device are as described above, and therefore will not be described in detail here.

[0057] A control platform is set up to control the hydrogen adsorption vacuum heat treatment device.

[0058] A hydrogen gas supply device is connected to the first pipe joint. The hydrogen gas supply device may be a hydrogen gas bottle.

[0059] An inert gas supply is connected to the second pipe joint, and the inert gas supply may be an argon gas bottle.

[0060] <Application of the hydrogen adsorption vacuum heat treatment system> The application method of the hydrogen adsorption vacuum heat treatment system of the present invention includes the following steps: (1) main piping vacuum extraction step, (2) furnace tube vacuum extraction step, (3) heating step, (4) hydrogen gas supply and cooling step, (5) hydrogen gas exhaust step, and (6) inert gas supply and vacuum extraction step, which will be described in detail below.

[0061] Steps for Main Pipe Vacuum Extraction The LaFeSi-based material is placed in the sample chamber. With the furnace tube module positioned inside the furnace tube, the baffle plate valve is closed, the rotary vane vacuum pump, the first control valve, and the second control valve are opened, and the gas in the main pipe is evacuated to a pressure of 20 Pa or less, preferably 10 Pa or less. Next, the Roots vacuum pump is turned on, and the main pipe is evacuated to a pressure of 10 -2 Pa or less.

[0062] In some embodiments, it is further necessary to close the pneumatic ball valve and open the fourth control valve.

[0063] Furnace tube vacuum extraction step After heating the metal oil diffusion pump for 15 to 60 minutes, preferably 30 to 50 minutes, the baffle plate valve and the third control valve are opened, the second control valve is closed, and the gas in the furnace tube is evacuated to a pressure of 0.1 Pa or less, preferably 10 -2 Pa or less, and then the metal oil diffusion pump, the Roots vacuum pump, and the rotary vane vacuum pump are turned off.

[0064] The gas pumped out by the metal oil diffusion pump is transported to the Roots vacuum pump and the rotary vane vacuum pump through the second branch and the third branch, and is discharged from the system by the Roots vacuum pump and the rotary vane vacuum pump.

[0065] In some embodiments, it is further necessary to open the pneumatic ball valve and close the fourth control valve.

[0066] Heating step With the first furnace body and the second furnace body closed, the heating device of the furnace body is turned on, and the temperature of the furnace tube is raised to 250 - 360 °C, preferably 300 - 330 °C.

[0067] Hydrogen gas supply and cooling steps Close the first control valve and the baffle plate valve, turn on the hydrogen gas supply device, set the pressure in the furnace tube to 110-150 kPa, preferably 120-140 kPa, and maintain the temperature and pressure for 170-250 minutes, preferably 200-220 minutes. Then, turn off the heating device of the furnace body and maintain the pressure constant. Move the first furnace body and the second furnace body along the diameter of the furnace tube, leaving the first furnace body and the second furnace body open. Cool for 100-150 minutes, preferably 110-130 minutes.

[0068] In some embodiments, when the first control valve and the baffle plate valve are closed, it is also necessary to close the air operated ball valve.

[0069] Hydrogen gas discharge step The hydrogen gas supply device controls the amount of hydrogen gas in the furnace tube, and after the pressure in the furnace tube reaches 80 to 120 kPa, preferably 90 to 110 kPa, open the baffle plate valve, rotary vane vacuum pump, first control valve, and second control valve to evacuate the gas in the main pipe and furnace tube to a pressure of 0.001 Pa or less. Then, turn on the Roots vacuum pump and evacuate the gas in the main pipe and furnace tube.

[0070] In some embodiments, when the baffle plate valve, rotary vane vacuum pump, first control valve, and second control valve are opened, it is necessary to also open the air operated ball valve and the fourth control valve.

[0071] Inert gas supply and vacuum extraction steps Turn off the first control valve, second control valve, baffle plate valve, rotary vane vacuum pump and Roots vacuum pump, turn on the inert gas supply device and set the pressure in the furnace tube to 80-120 kPa, preferably 90-110 kPa, then open the baffle plate valve, rotary vane vacuum pump, first control valve and second control valve to evacuate the gas in the main pipe to a pressure of 0.001 Pa or less, then turn on the Roots vacuum pump and evacuate the gas in the main pipe.

[0072] In some embodiments, when the first control valve, the second control valve, the baffle plate valve, the rotary vane vacuum pump, and the Roots vacuum pump are turned off, it is also necessary to close the fourth control valve and the air-operated ball valve.

[0073] In some embodiments, when the baffle plate valve, rotary vane vacuum pump, first control valve, and second control valve are closed, it is necessary to also open the fourth control valve and the air-operated ball valve.

[0074] The inert gas supply and vacuum extraction steps can be repeated a sufficient number of times until the hydrogen gas is exhausted. The system is then shut down and the LaFeSi-based material in the sample chamber is removed.

[0075] Example 1 As shown in Fig. 1 and Fig. 5, the hydrogen adsorption vacuum heat treatment apparatus for LaFeSi-based materials of the present invention comprises a furnace body 1, a furnace tube, a furnace tube inner module, a furnace tube support seat 4, a furnace body support 5, a cooling fluid supply device, and a vacuum extraction device.

[0076] The furnace body 1 is used to heat the furnace tube. A heating device is disposed within the furnace body 1. The heating device may be an electric heating resistor. The temperature of the furnace tube can be raised to 80 to 520°C depending on the amount of heat generated by the heating device. A thermocouple and a thermocouple insulation layer may be disposed within the furnace body 1. This makes it possible to detect the temperature of the furnace body 1.

[0077] The furnace tube comprises a furnace tube body 201, a baffle plate valve 202, and a furnace tube baffle plate 203. The furnace tube body 201 comprises a first furnace tube body section, a second furnace tube body section, and a third furnace tube body section, which are connected in sequence. The furnace tube body 201 has a tubular structure open at both ends. The baffle plate valve 202 is sealed at the open end of the first furnace tube body section by an elastic seal (e.g., a rubber seal). The furnace tube baffle plate 203 is sealed at the open end of the third furnace tube body section by an elastic seal (e.g., a rubber seal). The second furnace tube body section is located inside the furnace body 1, and the first furnace tube body section and the third furnace tube body section are located outside the furnace body. The thermal conductivity of the material forming the first furnace tube body section is greater than that of the material forming the second furnace tube body section. The thermal conductivity of the material forming the third furnace tube body section is greater than that of the material forming the second furnace tube body section. This increases the heat dissipation efficiency of the furnace tubes outside the furnace body 1, lowers the temperature at both ends of the furnace tube body 201, and reduces the impact of high temperatures on the elastic seal. One end of the baffle plate valve 202 away from the furnace tube body 201 is connected to a pneumatic ball valve 204, which increases the airtightness.

[0078] 4, the baffle plate valve 202 is provided with a first pipe joint 2021, a second pipe joint 2022, a vacuum gauge 2023, and a pressure transmitter 2024. The first pipe joint 2021 is used to connect to a hydrogen gas supply device. The second pipe joint 2022 is used to connect to an inert gas supply device (e.g., an argon gas bottle). The vacuum gauge 2023 is used to detect the pressure inside the furnace tube body 201. The pressure transmitter 2024 is used to convert the pressure inside the furnace tube body 201 into an electrical signal.

[0079] As shown in FIG. 1 , the furnace tube support seat 4 comprises a support portion 401 and a connecting portion 402. The support portion 401 has a hollow structure inside. The support portion 401 is sleeve-shaped around the outer periphery of the furnace tube body 201. One end of the connecting portion 402 is connected to the bottom of the support portion 401. The other end is connected to the furnace body support 5. The furnace body support 5 is placed on the ground. Two furnace tube support seats 4 may be provided. The support portion 401 of one of the furnace tube support seats 4 is sleeve-shaped around the outer periphery of the first furnace tube body portion, and the support portion 401 of the other furnace tube support seat 4 is sleeve-shaped around the outer periphery of the third furnace tube body portion.

[0080] As shown in FIGS. 2 and 3, the furnace body 1 comprises a first furnace body 101 and a second furnace body 102. The first furnace body 101 and the second furnace body 102 can move along the radial direction of the furnace tube. FIG. 2 is a schematic diagram of the first furnace body 101 and the second furnace body 102 in a closed state. FIG. 3 is a schematic diagram of the first furnace body 101 and the second furnace body 102 in an open state. The movement paths of the first furnace body 101 and the second furnace body 102 can be restricted using a movable rail and slider. In some embodiments, the hydrogen adsorption vacuum heat treatment apparatus further comprises an electric motor (not shown), a lateral movement mechanism support 8, and a traveling support. The traveling support comprises a first traveling support 901 and a second traveling support 902. The first traveling support 901 is connected to the first furnace body 101. The second traveling support 902 is connected to the second furnace body 102. The lateral movement mechanism support 8 is disposed to penetrate through the furnace body support 5. A movable rail is arranged on the lateral movement mechanism support 8. The movable rail matches with a slider arranged at the lower end of the traveling support to limit the movement path of the first furnace body 101 and the second furnace body 102. An electric motor drives the traveling support to move it. A chain drive system may also be used.

[0081] As shown in FIG. 5, the furnace tube module includes a sample chamber, a flange 304, a connecting rod 305, a heat insulating sheet 302, and a heat insulating plate 303. The sample chamber includes a sample chamber body and a chamber baffle plate 3013. In use, the sample chamber is located inside the second furnace tube body. Both ends of the sample chamber body are open. The chamber baffle plate 3013 covers the open end of the sample chamber body. As shown in FIG. 6, at least a portion of the chamber baffle plate 3013 is formed of metal foam. This allows for more uniform hydrogen distribution and improved hydrogen absorption. The sample chamber body includes a first chamber body 3011 and a second chamber body 3012. The first chamber body 3011 and the second chamber body 3012 are connected to each other using a locking connection. This allows for easy placement of plate-shaped or large-sized LaFeSi-based materials in the sample chamber.

[0082] When the sample chamber is in use, one end of the third furnace tube closest to the main body is connected to a flange 304. The flange 304 is connected to a chamber baffle plate 3013, and the metal foam portion of the chamber baffle plate 3013 is not covered. A connecting rod 305 is connected to the flange 304. The connecting rod 305 extends from the end connected to the flange 304 in a direction away from the sample chamber. The connecting rod 305 penetrates an insulating plate 303, which is disposed near the end of the connecting rod 305 that faces away from the sample chamber. The connecting rod 305 penetrates an insulating sheet 302, which is disposed between the sample chamber and the insulating plate 303. Multiple insulating sheets 302 may be installed. As shown in FIG. 7, the insulating sheet 302 has ventilation holes 3021. This provides insulation, reduces the effect of high temperatures on the elastic seal, and does not affect gas flow.

[0083] As shown in FIG. 1 , the cooling fluid supply device includes a chiller 601 and a water tank 602. The hydrogen adsorption vacuum heat treatment device further includes a first cooling fluid pipe (not shown) and a second cooling fluid pipe (not shown). At least a portion of the first cooling fluid pipe is disposed within the cavity of the support part 401, which forms a sleeve around the outer periphery of the first furnace tube main body. At least a portion of the second cooling fluid pipe is disposed within the cavity of the support part 401, which forms a sleeve around the outer periphery of the third furnace tube main body. The water tank 602 provides a water source to the chiller 601. The chiller 601 is used to cool the water. The chiller 601 is connected to the first cooling fluid pipe and the second cooling fluid pipe, respectively.

[0084] As shown in Figures 1 and 8, the vacuum extraction device includes a main pipe 701, a first control valve 702, a second control valve 703, a first branch 704, a metal oil diffusion pump 705, a third control valve 706, a second branch 707, a third branch 708, a Roots vacuum pump 709, a rotary vane vacuum pump 710, an electrical resistance vacuum gauge 711, an ionization vacuum gauge 712, and a fourth control valve 713.

[0085] One end of the main pipe 701 is connected to the elbow pipe 205, and the other end of the elbow pipe 205 is connected to the air-operated ball valve 204. The other end of the main pipe 701 is connected to the second control valve 703. A first control valve 702 is disposed in the main pipe 701. The first control valve 702 includes a solenoid valve and an air-operated baffle plate valve. The second control valve 703 includes a solenoid valve and an air-operated baffle plate valve.

[0086] One end of the first branch 704 is connected to the first control valve 702. The other end of the first branch 704 is connected to the vent inlet end of the metal oil diffusion pump 705.

[0087] One end of the second branch 707 is connected to the vent outlet end of the metal oil diffusion pump 705. The other end of the second branch 707 is connected to the second control valve 703. A third control valve 706 is disposed in the second branch 707. The third control valve 706 includes a solenoid valve and an air-operated baffle plate valve.

[0088] One end of the third branch 708 is connected to a portion of the second branch 707 located between the third control valve 706 and the second control valve 703. The other ends of the third branch 708 are connected to a Roots vacuum pump 709 and a rotary vane vacuum pump 710, respectively.

[0089] An electrical resistance vacuum gauge 711 and an ionization vacuum gauge 712 are disposed in the main pipe 701 between the elbow pipe 205 and the first control valve 702. The electrical resistance vacuum gauge 711 and the ionization vacuum gauge 712 are used to measure the vacuum level in the measurement main pipe 701.

[0090] A fourth control valve 713 is disposed in the main pipe 701 between the first control valve 702 and the second control valve 703. The fourth control valve 713 may be a solenoid valve.

[0091] Example 2 The hydrogen adsorption vacuum heat treatment system for LaFeSi-based materials of this embodiment includes the hydrogen adsorption vacuum heat treatment apparatus of Example 1, a control table, a hydrogen gas supply device, and an inert gas supply device.

[0092] A control platform is used to control the hydrogen adsorption vacuum heat treatment device.

[0093] A hydrogen gas supply device is connected to the first pipe joint 2021. The hydrogen gas supply device may be a hydrogen gas bottle.

[0094] An inert gas supply is connected to the second pipe joint 2022. The inert gas supply may be an argon gas bottle.

[0095] Example 3 The hydrogen adsorption vacuum heat treatment system of Example 2 was employed to perform a hydrogen adsorption treatment on a LaFeSi-based material, which included the following steps.

[0096] The first chamber body 3011 and the second chamber body 3012 were opened, and a plate-shaped LaFeSi-based material was placed in the sample chamber. The furnace tube baffle plate 203 was opened and placed inside the furnace tube inner module furnace tube body 201, so that the sample chamber was located inside the second furnace tube body. The furnace tube baffle plate 203 was sealed to the opening at the end of the furnace tube body 201.

[0097] The baffle plate valve 202 and the air-operated ball valve 204 were closed, and the rotary vane vacuum pump 710, the first control valve 702, the second control valve 703, and the fourth control valve 713 were opened to evacuate the gas in the main pipe 701 to a pressure of 10 Pa or less. Next, the Roots vacuum pump 709 was turned on, and the gas in the main pipe 701 was evacuated.

[0098] After heating the metal oil diffusion pump 705 for 40 minutes, the baffle plate valve 202, the air-operated ball valve 204, and the third control valve 706 were opened, the second control valve 703 and the fourth control valve 713 were closed, and the gas in the furnace tube was evacuated for 10 minutes. -2 The system was evacuated to a pressure of less than 100 Pa, and then the metal oil diffusion pump 705, the Roots vacuum pump 709, and the rotary vane vacuum pump 710 were turned off. The gas extracted by the metal oil diffusion pump 705 was transported to the Roots vacuum pump 709 and the rotary vane vacuum pump 710 through the second branch 707 and the third branch 708, and was discharged from the system by the Roots vacuum pump 709 and the rotary vane vacuum pump 710.

[0099] With the first furnace body 101 and the second furnace body 102 closed, the heating device in the furnace body 1 was turned on to raise the temperature inside the furnace tube to 320°C.

[0100] The first control valve 702, the baffle plate valve 202 and the air-operated ball valve 204 were closed, the hydrogen gas supply device was turned on, the pressure inside the furnace tube was set to 130 kPa, and the temperature and pressure were maintained for 210 minutes. After that, the heating device inside the furnace body 1 was turned off, the pressure was kept constant, the first furnace body 101 and the second furnace body 102 were moved along the diameter of the furnace tube, and then the first furnace body 101 and the second furnace body 102 were left in an open state, and then cooled for 120 minutes.

[0101] The hydrogen gas supply device controlled the amount of hydrogen gas supplied into the furnace tube, and after the pressure inside the furnace tube reached 100 kPa, the baffle plate valve 202, the air-operated ball valve 204, the rotary vane vacuum pump 710, the first control valve 702, the second control valve 703, and the fourth control valve 713 were opened to evacuate the gas inside the main pipe 701 and the furnace tube, and then the Roots vacuum pump 709 was opened to evacuate the gas inside the main pipe 701 and the furnace tube.

[0102] The first control valve 702, the second control valve 703, the fourth control valve 713, the baffle plate valve 202, the pneumatic ball valve 204, the rotary vane vacuum pump 710, and the Roots vacuum pump 709 were closed, the inert gas supply device (argon gas bottle) was opened, and the pressure in the furnace tube was adjusted to 100 kPa. Next, the baffle plate valve 202, the pneumatic ball valve 204, the rotary vane vacuum pump 710, the first control valve 702, the second control valve 703, and the fourth control valve 713 were opened to evacuate the gas in the main pipe 701 and the furnace tube. Next, the Roots vacuum pump 709 was opened to evacuate the gas in the main pipe 701 and the furnace tube. The argon gas supply and vacuum extraction steps were repeated to evacuate the hydrogen gas in the apparatus.

[0103] The system was closed and the LaFeSi-based material was removed from the sample chamber.

[0104] The present invention is not limited to the above-described embodiments, and any modifications, improvements, substitutions, etc. that may occur to those skilled in the art are intended to be included within the scope of the present invention, provided that they do not deviate from the spirit of the present invention.

Claims

1. The hydrogen adsorption vacuum heat treatment apparatus comprises a furnace body, a furnace tube, a module in the furnace tube, a first cooling fluid pipe, a second cooling fluid pipe, a cooling fluid supply device, and a vacuum extraction device; The furnace body is used to heat a furnace tube; the furnace tube comprises a furnace tube body, a baffle plate valve, and a furnace tube baffle plate, both ends of the furnace tube body are open, and the furnace tube body comprises a first furnace tube body section, a second furnace tube body section, and a third furnace tube body section, which are connected in order to the furnace tube body, the second furnace tube body section being located inside the furnace body, and the first furnace tube body section and the third furnace tube body section being located outside the furnace body; the baffle plate valve is sealed at the open end of the first furnace tube body by an elastic seal, a first pipe joint and a second pipe joint are disposed on the baffle plate valve, the first pipe joint is used to connect with a hydrogen gas supply device, and the second pipe joint is used to connect with an inert gas supply device; the furnace tube baffle plate is sealed at the open end of the third furnace tube body portion by an elastic seal; the furnace tube internal module comprises a sample chamber, a connecting rod, a heat insulating sheet, and a heat insulating plate; the sample chamber comprises a sample chamber body and a chamber baffle plate, both ends of the sample chamber body are open ends, the chamber baffle plate is covered on the open end of the sample chamber body, at least a part of the chamber baffle plate is formed of foam metal, the sample chamber body comprises a first chamber body and a second chamber body, the first chamber body and the second chamber body are connected in an assembled manner, One end of the connecting rod is connected to one end of the sample chamber, and the connecting rod extends from the end connected to the sample chamber in a direction away from the sample chamber; the connecting rod passes through the insulating plate, and the insulating plate is disposed near one end of the connecting rod that is remote from the sample chamber; the connecting rod penetrates the heat insulating sheet, the heat insulating sheet is disposed between the sample chamber and the heat insulating plate, and an air vent is disposed in the heat insulating sheet; the first cooling fluid piping is configured to cool the first furnace tube body, and the first cooling fluid piping is connected to the cooling fluid supply device; the second cooling fluid piping is configured to cool the third furnace tube body, and the second cooling fluid piping is connected to the cooling fluid supply device; a vacuum extraction device connected to the furnace tube, the vacuum extraction device being used to suck out gas from the furnace tube;

2. 2. The hydrogen adsorption vacuum heat treatment apparatus according to claim 1, wherein the furnace body comprises a first furnace body and a second furnace body, the first furnace body and the second furnace body are configured to be movable along the radial direction of the furnace tube, and the first furnace body and the second furnace body move in opposite directions.

3. The hydrogen adsorption vacuum heat treatment device further includes an electric machine, a running track, and a running support; The electric machine is configured to drive the traveling support to move, A slider that matches the running track is disposed on the running support; The running track and the slider are configured to limit the movement path of the running support; 3. The hydrogen adsorption vacuum heat treatment apparatus according to claim 2, wherein the running support comprises a first running support and a second running support, the first running support is connected to the first furnace body, and the second running support is connected to the second furnace body.

4. 2. The hydrogen adsorption vacuum heat treatment apparatus according to claim 1, wherein the thermal conductivity of the material forming the first furnace tube body is greater than the thermal conductivity of the material forming the second furnace tube body, and the thermal conductivity of the material forming the third furnace tube body is greater than the thermal conductivity of the material forming the second furnace tube body.

5. 2. The hydrogen adsorption vacuum heat treatment apparatus according to claim 1, wherein the baffle plate valve is further provided with a vacuum gauge and a pressure transmitter.

6. The vacuum extraction device comprises a main pipe, a first control valve, a second control valve, a first branch, a metal oil diffusion pump, a third control valve, a second branch, a third branch, a roots vacuum pump, and a rotary vane vacuum pump; One end of the main pipe is connected to the baffle plate valve, the other end of the main pipe is connected to a second control valve, and a first control valve is disposed in the main pipe; One end of the first branch is connected to the first control valve, and the other end of the first branch is connected to the vent inlet end of the metal oil diffusion pump; One end of the second branch is connected to the vent outlet end of the metal oil diffusion pump, the other end of the second branch is connected to the second control valve, and a third control valve is disposed in the second branch; one end of the third branch is connected to a portion of the second branch located between the second control valve and the third control valve, and the other end of the third branch is connected to the vent inlet end of the Roots vacuum pump and the vent inlet end of the rotary vane vacuum pump, respectively; 3. The hydrogen adsorption vacuum heat treatment apparatus according to claim 2.

7. 7. The hydrogen adsorption vacuum heat treatment apparatus according to claim 6, wherein an electric resistance vacuum gauge and an ionization vacuum gauge are disposed in the main pipe between the baffle plate valve and the first control valve.

8. the first control valve comprises an air-operated baffle plate valve and a solenoid valve, the second control valve comprises an air-operated baffle plate valve and a solenoid valve, and the third control valve comprises an air-operated baffle plate valve and a solenoid valve; 8. The hydrogen adsorption vacuum heat treatment apparatus according to claim 7, wherein the cooling fluid supply device comprises a chiller and a water tank, the water tank is configured to supply a water source to the chiller, the chiller is configured to cool water, and the chillers are connected to the first cooling fluid piping and the second cooling fluid piping, respectively.

9. A hydrogen adsorption vacuum heat treatment system includes the hydrogen adsorption vacuum heat treatment apparatus according to any one of claims 6 to 8, a control table, a hydrogen gas supply device, and an inert gas supply device, the control platform is configured to control the hydrogen adsorption vacuum heat treatment device; a hydrogen adsorption vacuum heat treatment system for a LaFeSi-based material, characterized in that the hydrogen gas supply device is connected to the first piping joint, and the inert gas supply device is connected to the second piping joint.

10. The steps below, (1) With the LaFeSi-based material placed in the sample chamber and the furnace tube module positioned inside the furnace tube, close the baffle plate valve, open the rotary vane vacuum pump, the first control valve, and the second control valve, evacuate the gas in the main pipe to a pressure of 20 Pa or less, then turn on the Roots vacuum pump to evacuate the gas in the main pipe to a pressure of 10 Pa or less. -2 Vacuuming to a pressure of less than 1 Pa; (2) After heating the metal oil diffusion pump for 15 to 60 minutes, open the baffle plate valve and the third control valve, close the second control valve, evacuate the gas in the furnace tube to a pressure of 0.1 Pa or less, and then turn off the metal oil diffusion pump, the Roots vacuum pump and the rotary vane vacuum pump; (3) With the first furnace body and the second furnace body closed, turn on the heating device of the furnace body to raise the furnace tube temperature to 250-360°C; (4) Close the first control valve and the baffle plate valve, turn on the hydrogen gas supply device, set the pressure in the furnace tube to 110-150 kPa, maintain the temperature and pressure for 170-250 minutes, then turn off the heating device of the furnace body, keep the pressure constant, move the first furnace body and the second furnace body along the diameter of the furnace tube, keep the first furnace body and the second furnace body open, and then cool for 100-150 minutes; (5) The hydrogen gas supply device controls the amount of hydrogen gas introduced into the furnace tube, and after the pressure in the furnace tube is 80-120 kPa, the baffle plate valve, rotary vane vacuum pump, first control valve and second control valve are opened to evacuate the gas in the main pipe and furnace tube to a pressure of 0.001 Pa or less, and then the Roots vacuum pump is turned on to evacuate the gas in the main pipe and furnace tube; (6) Turn off the first control valve, second control valve, baffle plate valve, rotary vane vacuum pump and Roots vacuum pump, turn on the inert gas supply device, and make the pressure in the furnace tube 80-120kPa. Then open the baffle plate valve, rotary vane vacuum pump, first control valve and second control valve to evacuate the gas in the main pipe to a pressure of 0.001Pa or less. Then turn on the Roots vacuum pump and evacuate the gas in the main pipe. (7) repeating step (6) to vent the hydrogen gas; 10. The method for applying the hydrogen adsorption vacuum heat treatment system according to claim 9, comprising:

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