Apparatus for producing hydrogenated metal and method for producing hydrogenated metal powder

Abstract

The application belongs to the field of hydrogen metallurgy technology, and discloses a device for preparing hydrogenated metal and a method for preparing hydrogenated metal powder. The device is characterized by that a closed furnace pot is arranged in the furnace body, a heating device is arranged outside and / or below the closed furnace pot in the furnace body, a furnace neck is arranged at the top of the furnace body, the upper part of the closed furnace pot penetrates through the furnace neck and is fixed, a furnace cover is detachably fixed at the top of the furnace neck and is provided with a sealing ring between the furnace neck, the furnace cover is provided with an exhaust pipe which is communicated with a vacuum device, the exhaust pipe is connected with an air inlet pipe which is communicated with a gas supply device, the exhaust pipe and the air inlet pipe are provided with air valves, the exhaust pipe or the air inlet pipe is further provided with an air pressure gauge, a thermocouple extends into the closed furnace pot through the furnace cover, a charging device is arranged in the closed furnace pot, and the charging device is in a tower-like structure with multiple layers of charging discs arranged at intervals. The method comprises the steps of pretreatment, hydrogenation and ball milling and screening. The application has the characteristics of simple structure, easy operation, safety and reliability, uniform particle size, high purity and the like.

Description

Technical Field

[0001] This invention relates to the field of hydrogen metallurgy technology, specifically to an apparatus and method for preparing hydride metal powder that is simple in structure, easy to operate, safe and reliable, and produces powder with uniform particle size and high purity. Background Technology

[0002] Hydrogenation metallurgy is a smelting method that uses hydrogen to reduce various oxides or chlorides to produce hydride metals, and then crushes (and dehydrogenates) the brittle hydride metals to produce metal powder.

[0003] Metal hydrides are compounds composed of metallic elements and hydrogen, and are widely used as hydrogen storage materials, catalysts, and electrode materials. Due to the highly reactive chemical properties of metal hydrides, especially ultrafine and nanoscale metal hydrides which possess unique chemical properties, it is particularly important to find a simple, reliable, and high-purity method for preparing metal hydrides and their powders.

[0004] Currently, metal powders are mainly prepared using methods such as reduction, atomization, electrolysis, mechanical pulverization, and hydroxyl methods. Among these, mechanical pulverization is the simplest, but due to the high ductility and hardness of most metals, it is quite difficult. Therefore, it is generally necessary to modify the metal's properties to make it brittle before mechanical pulverization. The most common method is to use gas-phase hydride to make the metal brittle after absorbing hydrogen, and then mechanically pulverize the brittle hydride metal to directly prepare hydride metal powder. Alternatively, the hydride metal powder can be further dehydrogenated to obtain the final metal powder.

[0005] In existing technologies, obtaining high-purity hydride metals often requires multiple reactions and processes, thus consuming significant manpower and resources. However, traditional gas-phase hydrogenation methods typically involve spreading the metal material or powder to be hydrogenated evenly within the furnace. Excessive material thickness slows hydrogen diffusion and causes uneven metal heating, resulting in poor hydrogenation and limiting the amount of hydride metal to ensure optimal hydrogenation, thus reducing production capacity. To address this, existing technologies incorporate a stirring device within the hydrogenation furnace. This device stirs the metal to be hydrogenated during hydrogenation, improving temperature uniformity, accelerating hydrogen diffusion, and increasing the metal loading capacity, thereby significantly enhancing hydrogenation efficiency and effectiveness. However, since hydrogenation needs to be carried out at high temperatures, the drive unit of the stirring device generally needs to be located outside the furnace. The hydrogenation process requires pre-vacuuming and is carried out in a high-pressure hydrogen atmosphere, which means that the seal of the stirring device needs to be able to withstand both low vacuum and high-pressure hydrogen. This makes sealing the stirring shaft more difficult, resulting in higher maintenance costs for the sealing structure and reduced reliability during hydrogenation. Summary of the Invention

[0006] To address the shortcomings of existing technologies, this invention provides an apparatus for preparing metal hydrides that is simple in structure, easy to operate, safe and reliable, and has high purity. It also provides a method for preparing metal hydride powder that is easy to operate, produces powder with uniform particle size, and has high purity.

[0007] The apparatus for preparing metal hydride according to the present invention is implemented as follows: it includes a furnace body, a heating device, a furnace cover, and a thermocouple. The furnace body is a cylindrical structure and has an open, sealed furnace tank inside. The heating device is arranged around and / or below the sealed furnace tank inside the furnace body. The furnace body is also provided with an upwardly extending furnace neck at the top. The upper part of the sealed furnace tank passes through the furnace neck and is fixedly connected to the furnace neck. The furnace cover is detachably fixedly installed at the top of the furnace neck. A sealing ring is provided between the furnace cover and the furnace neck. An exhaust pipe communicating with a vacuum device is provided through the furnace cover. The exhaust pipe is also connected in parallel with an inlet pipe communicating with a gas supply device. Gas valves are provided on the exhaust pipe and the inlet pipe respectively. A pressure gauge is also provided on the exhaust pipe or the inlet pipe. The thermocouple passes through the furnace cover and extends into the sealed furnace tank. A charging device is provided inside the sealed furnace tank. The charging device is a tower-shaped structure with multiple charging trays spaced apart.

[0008] Furthermore, a cooling water channel is arranged around the inside of the furnace neck and furnace cover. An inlet I and an outlet I connected to the internal cooling water channel are respectively provided on both sides of the furnace neck. An inlet II and an outlet II connected to the internal cooling water channel are respectively provided on both sides of the furnace cover. The outlet I is connected to the inlet II through a pipe. The inlet I and the outlet II are respectively connected to the water supply pipe and the water return pipe of the cooling water circulation system.

[0009] Furthermore, the furnace neck is circular and has multiple latches spaced circumferentially along its top outer edge. Each latch has a slot on the side facing the center of the furnace neck. The top of the furnace cover has multiple limiting ribs spaced circumferentially, with one end of each limiting rib extending out of the edge of the furnace cover and engaging with the slot of the latch.

[0010] Furthermore, a fixing rod is fixedly and vertically installed at the top center of the furnace cover, the limiting ribs are evenly distributed around the top of the furnace cover and their inner ends are fixedly connected to the fixing rod, and the outer edge of the top of the furnace neck is evenly distributed with ear clips corresponding to the fixing rod. Each limiting rib of the furnace cover can be tightly engaged and interlocked with the slots of each ear clip of the furnace neck.

[0011] Furthermore, the exhaust pipe is vertically installed on the furnace cover, and the intake pipe has an inverted L-shaped structure with the intake port facing the furnace cover and the exhaust port end is vertically connected to the exhaust pipe. The air passage between the intake port of the intake pipe and the opening of the exhaust pipe in the sealed furnace forms a right-angled trapezoid. The length of the base formed by the opening to the end of the exhaust pipe and the intake pipe in the right-angled trapezoid is equal to the length of the hypotenuse formed by the straight connection of the opening to the intake port of the intake pipe.

[0012] Furthermore, the sealing ring is a metal sealing ring, a graphite metal sealing ring, or a flexible graphite sealing ring.

[0013] Furthermore, the furnace body is a cylindrical structure with an open top, and a sealed cover plate is fixedly installed on the open top of the furnace body. The furnace neck is sealed and fixedly installed at the top of the cover plate, and the upper part of the sealed furnace tank penetrates the cover plate and the furnace neck and is fixedly connected to the furnace neck.

[0014] The method for preparing hydrogenated metal powder of the present invention is implemented as follows: it includes pretreatment, hydrogenation, and ball milling and sieving steps, specifically as follows: A. Pretreatment: Pickling removes surface grease and impurities from the metal material, followed by cleaning and drying to obtain dry metal material; B. Hydrogenation: Dry metal material is loaded into the loading tray of the aforementioned apparatus for preparing hydride metal, and hydrogenated under pressure at 600~800℃ and hydrogen pressure of 0.1~0.2MPa for 1~2 hours. After cooling, the hydride metal is obtained. C. Ball milling and sieving: Ball milling is carried out with the ball milling media and the hydride metal at a ball-to-material ratio of 2:1 to 4:1 for 0.5 to 2 hours, and the hydride metal powder is obtained by sieving. The ball milling media is 304 or 316 stainless steel.

[0015] Furthermore, in the hydrogenation step, the dried metal material is loaded into a charging tray, then heated to 350~400℃ and held at that temperature while being vacuumed to below 10Pa. Subsequently, the pressure is maintained and the metal material is heated to 600~800℃. Then, high-purity hydrogen gas is introduced to 0.1~0.2MPa and hydrogenation is carried out under pressure. After hydrogenation, the metal is discharged from the furnace while maintaining pressure and cooling.

[0016] Furthermore, during the hydrogenation process, high-purity hydrogen is continuously introduced and pressurized until the preset hydrogenation time is reached, at which point the hydrogenation process ends and the temperature is lowered; or, during the hydrogenation process, high-purity hydrogen is introduced to the preset maximum pressure and then the gas valve is closed. Once the gas pressure inside the sealed furnace is lower than the preset minimum pressure, the gas valve is opened and high-purity hydrogen is introduced again to the preset maximum pressure, until the gas pressure inside the sealed furnace no longer decreases within 10-30 minutes or the preset hydrogenation time is reached, at which point the hydrogenation process ends and the temperature is lowered.

[0017] The beneficial effects of this invention are as follows: 1. The present invention provides a tower-shaped charging device with multiple charging trays inside a sealed furnace. The multiple charging trays can control the thickness of the material layer to ensure the hydrogen diffusion rate and temperature uniformity, and can also increase the amount of metal to be hydrogenated in the furnace, thereby effectively improving the purity of the hydrogenated metal and the hydrogenation efficiency. Furthermore, since the charging device has no moving structure and is built into the sealed furnace, there is no need to consider additional sealing structures, thereby reducing maintenance workload and improving hydrogenation reliability.

[0018] 2. This invention provides a sealed furnace tank within the furnace body, with the sealed furnace tank fixedly connected to the furnace neck, and the furnace neck sealed to the furnace cover via a sealing ring. This allows the sealed furnace tank to form a sealed space after the furnace cover is closed. Therefore, compared to an integral sealed furnace cavity structure, this simplifies the sealing process and provides a more reliable sealing effect, ensuring the reliability of the hydrogenation process.

[0019] 3. The present invention provides cooling water channels around the furnace neck and furnace cover, which can solve the problem of large temperature difference between the upper and lower parts of the sealed furnace tank due to heat accumulation, thus affecting the uniformity of hydrogenation. In addition, the cooling water channels can keep the sealing ring at a lower temperature to improve its service life.

[0020] 4. The furnace cover and furnace neck of the present invention are connected by multiple latches and limiting ribs to form a tightly fitted and interlocking connection structure. Not only is the detachable connection structure convenient for hoisting the charging device, but the connection between the multiple latches and limiting ribs is also reliable and can withstand both vacuum low pressure and high pressure hydrogen atmosphere at the same time, which can effectively improve hydrogenation safety.

[0021] 5. This invention utilizes the reversible properties of metals such as zirconium, titanium, and niobium with hydrogen to prepare metal powder. After absorbing hydrogen, corresponding hydride metals are formed and brittleness is generated simultaneously. By controlling the hydrogen pressure, furnace temperature, and hydrogenation time in the furnace during hydrogenation, as well as controlling the ball-to-material ratio during ball milling, regular hydride metal powder with an oxygen content of 0.15~0.18% and a particle size of 15~25μm can be obtained by sieving. Not only is the purity of the hydride metal powder high, but the particle size of the powder is also uniform.

[0022] In summary, the present invention has the characteristics of simple structure, easy operation, safety and reliability, uniform particle size and high purity of powder. Attached Figure Description

[0023] Figure 1 This is a schematic diagram of the apparatus for preparing metal hydrides according to the present invention; Figure 2 This is a flowchart of the method for preparing hydride metal powder according to the present invention; In the diagram: 1-furnace body, 2-heating device, 3-furnace cover, 4-sealed furnace tank, 5-furnace neck, 6-sealing ring, 7-air outlet pipe, 8-air inlet pipe, 9-air valve, 10-air pressure gauge, 11-charging device, 12-water inlet I, 13-water outlet I, 14-water inlet II, 15-water outlet II, 16-clamp, 17-limiting rib, 18-fixing rod, 19-opening, 20-cover plate. Detailed Implementation

[0024] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention.

[0025] like Figure 1 As shown, the apparatus for preparing metal hydride according to the present invention includes a furnace body 1, a heating device 2, a furnace cover 3, and a thermocouple. The furnace body 1 has a cylindrical structure and an open-top sealed furnace tank 4 is provided inside. The heating device 2 is arranged around the outside and / or below the sealed furnace tank 4 inside the furnace body 1. The furnace body 1 is also provided with an upwardly extending furnace neck 5 at its top. The upper part of the sealed furnace tank 4 passes through the furnace neck 5 and is fixedly connected to the furnace neck 5. The furnace cover 3 is detachably fixedly installed at the top of the furnace neck 5. A sealing ring 6 is provided between the furnace cover 3 and the furnace neck 5. An exhaust pipe 7 connected to a vacuum device is provided through the furnace cover 3. An inlet pipe 8 connected to a gas supply device is also connected in parallel to the exhaust pipe 7. Gas valves 9 are respectively provided on the exhaust pipe 7 and the inlet pipe 8. A pressure gauge 10 is also provided on the exhaust pipe 7 or the inlet pipe 8. The thermocouple passes through the furnace cover 3 and extends into the sealed furnace tank 4. A charging device 11 is provided inside the sealed furnace tank 4. The charging device 11 is a tower-shaped structure with multiple charging trays spaced apart.

[0026] Cooling water channels are arranged around the furnace neck 5 and the furnace cover 3. Water inlet I12 and water outlet I13, which are connected to the internal cooling water channels, are respectively arranged on both sides of the furnace neck 5. Water inlet II14 and water outlet II15, which are connected to the internal cooling water channels, are respectively arranged on both sides of the furnace cover 3. Water outlet I13 is connected to water inlet II14 through a pipe. Water inlet I12 and water outlet II15 are respectively connected to the water supply pipe and water return pipe of the cooling water circulation system.

[0027] The furnace neck 5 is circular and has multiple latches 16 spaced apart around its top outer edge. Each latch 16 has a slot on the side facing the center of the furnace neck 5. The top of the furnace cover 3 has multiple limiting ribs 17 spaced apart around its top edge. One end of each limiting rib 17 extends out of the edge of the furnace cover 3 and can engage with the slot of the latch 16.

[0028] A fixing rod 18 is fixedly and vertically installed at the top center of the furnace cover 3. The limiting ribs 17 are evenly distributed around the top of the furnace cover 3 and their inner ends are fixedly connected to the fixing rod 18. The outer edge of the top of the furnace neck 5 is evenly distributed with lugs 16 corresponding to the fixing rod 18. Each limiting rib 17 of the furnace cover 3 can be tightly fitted and interlocked with the groove of each lug 16 of the furnace neck 5.

[0029] The top of the furnace cover 3 is provided with three limiting ribs 17 spaced 120° apart in the circumferential direction, and the top outer edge of the furnace neck 5 is provided with three latches 16 spaced 120° apart in the circumferential direction. Each limiting rib 17 and the latch 16 are tightly fitted and interlocked, so that the furnace cover 3 and the furnace neck 5 form a stable connection. The limiting ribs 17 are evenly stressed and not easily deformed, so the connection is highly safe.

[0030] The exhaust pipe 7 is vertically mounted on the furnace cover 3. The intake pipe 8 has an inverted L-shaped structure with its intake facing the furnace cover 3 and its exhaust end perpendicularly connected to the exhaust pipe 7. The air passage between the intake of the intake pipe 8 and the opening 19 of the exhaust pipe 7 within the sealed furnace 4 forms a right-angled trapezoid. The base formed by the connection between the opening 19 and the end of the exhaust pipe 7 connected to the intake pipe 8, and the hypotenuse formed by the straight line connecting the opening 19 and the intake of the intake pipe 8, are of equal length. The right-angled trapezoidal structure of the intake pipe passage can slow down the air intake.

[0031] The sealing ring 6 is a metal sealing ring, a graphite metal sealing ring, or a flexible graphite sealing ring.

[0032] The furnace body 1 is a cylindrical structure with an open top. A sealed cover plate 20 is fixedly installed on the open top of the furnace body 1. The furnace neck 5 is sealed and fixedly installed at the top of the cover plate 20. The upper part of the sealed furnace tank 4 passes through the cover plate 20 and the furnace neck 5 and is fixedly connected to the furnace neck 5.

[0033] The inner wall of the sealed furnace 4 is surrounded by a refractory layer formed of refractory material.

[0034] The loading device 11 is provided with 4 to 8 layers of loading trays at intervals. The center of the loading device 11 is provided with a support rod and multiple support platforms are provided along the axial direction of the support rod. The center of the loading tray is provided with a relief groove that extends to one side and has a width greater than the diameter or minimum width of the support rod. The loading tray can slide into the support rod through the relief groove and sit on the support platform.

[0035] The support rod is a round rod or a square rod, and the width of the clearance groove is greater than the diameter of the round support rod or greater than the minimum width of the square support rod.

[0036] like Figure 2 As shown, the method for preparing hydrogenated metal powder of the present invention includes pretreatment, hydrogenation, and ball milling and sieving steps, the specific contents of which are as follows: A. Pretreatment: Pickling removes surface grease and impurities from the metal material, followed by cleaning and drying to obtain dry metal material; B. Hydrogenation: Dry metal material is loaded into the loading tray of the loading device 11 of the apparatus for preparing hydride metal according to any one of claims 1 to 7, and hydrogenated under pressure at 600~800°C and hydrogen pressure of 0.1~0.2MPa for 1~2 hours, and then cooled and removed from the furnace to obtain hydride metal. C. Ball milling and sieving: Ball milling is carried out with the ball milling media and the hydride metal at a ball-to-material ratio of 2:1 to 4:1 for 0.5 to 2 hours, and the hydride metal powder is obtained by sieving. The ball milling media is 304 or 316 stainless steel.

[0037] In the pretreatment step, the cleaned metal material is placed in an insulated box and dried at 110~130℃ for 2~3 hours.

[0038] In the hydrogenation step, the dried metal material is loaded into a charging tray, then heated to 350~400℃ and held at that temperature while being vacuumed to below 10Pa. Subsequently, the pressure is maintained and the metal material is heated to 600~800℃. Then, high-purity hydrogen gas is introduced to 0.1~0.2MPa and hydrogenation is carried out under pressure. After hydrogenation, the metal is discharged from the furnace while maintaining pressure and cooling.

[0039] During the hydrogenation process, high-purity hydrogen is continuously introduced and the pressure is maintained until the preset hydrogenation time is reached, at which point the hydrogenation ends and the temperature is lowered; or, during the hydrogenation process, high-purity hydrogen is introduced to the preset maximum pressure and then the gas valve 9 is closed. After the gas pressure inside the sealed furnace 4 is lower than the preset minimum pressure, the gas valve 9 is opened and high-purity hydrogen is introduced again to the preset maximum pressure until the gas pressure inside the sealed furnace 4 no longer decreases within 10-30 minutes or the preset hydrogenation time is reached, at which point the hydrogenation ends and the temperature is lowered.

[0040] In the ball milling and sieving step, the hydride metal and the ball milling media are wet-milled in an organic solvent, wherein the organic solvent is ethanol and the amount used is sufficient to submerge the milling balls and the hydride metal.

[0041] Example 1 like Figure 1 and 2 As shown, the apparatus for preparing hydride metals according to the present invention is used to perform hydride metallurgy on zirconium scraps, followed by wet milling and sieving to prepare ultrafine hydride zirconium powder. The specific process is as follows: S100: Zirconium chips of 1~5mm are acid-washed to remove surface grease and impurities, and then placed in an insulated oven at 120℃ for 2.5h to obtain dried zirconium chips.

[0042] S200: Dry zirconium chips are loaded layer by layer into the charging tray of the charging device 11 of the apparatus for preparing hydride metal of the present invention. The zirconium chips are then heated to 350°C and held at that temperature. At the same time, a vacuum is drawn to below 10 Pa. The pressure is then maintained and the zirconium chips are heated to 600~700°C. Then, high-purity hydrogen gas is introduced into the sealed furnace 4 through the gas inlet pipe 8 to 0.1 MPa and hydrogenated under pressure for 1 hour. After hydrogenation, the furnace is kept under pressure and cooled down. Finally, the hydride zirconium chips are obtained by removing them from the furnace.

[0043] S300: 316 stainless steel ball milling media and zirconium hydride chips are wet-milled in ethanol at a ball-to-material ratio of 2:1 for 0.5 hours, and then sieved to obtain ultrafine zirconium hydride powder with a particle size D50 of 25μm, wherein the oxygen content of the ultrafine zirconium hydride powder is about 0.18%.

[0044] Example 2 like Figure 1 and 2 As shown, the apparatus for preparing hydride metals according to the present invention is used to perform hydride metallurgy on titanium scraps, followed by wet milling and sieving to prepare ultrafine hydride titanium powder. The specific process is as follows: S100: Titanium shavings of 1~3mm are acid-washed to remove surface grease and impurities, and then placed in an insulated oven at 110℃ for 3 hours to obtain dried titanium shavings.

[0045] S200: Dry titanium shavings are layered into the loading tray of the loading device 11 of the apparatus for preparing hydride metals according to the present invention. The titanium shavings are then heated to 380°C and held at that temperature while a vacuum is drawn to below 10 Pa. The pressure is then maintained and the titanium shavings are heated to 700-800°C. High-purity hydrogen gas is then introduced into the sealed furnace 4 through the gas inlet pipe 8 to a pressure of 0.15 MPa and hydrogenated under pressure for 2 hours. After hydrogenation, the furnace is kept under pressure and cooled down. Finally, the hydrogenated titanium shavings are obtained by removing them from the furnace. During the hydrogenation process, after the high-purity hydrogen gas is introduced to 0.15 MPa, the gas valve 9 is closed. When the gas pressure in the sealed furnace 4 is lower than 0.1 MPa, the gas valve 9 on the gas inlet pipe 8 is opened and high-purity hydrogen gas is introduced again to 0.15 MPa. This process is repeated until the gas pressure in the sealed furnace 4 no longer decreases after 20 minutes or the hydrogenation time reaches 2 hours, at which point the hydrogenation is terminated.

[0046] S300: 304 stainless steel ball milling media and titanium hydride chips are wet-milled in ethanol at a ball-to-material ratio of 4:1 for 2 hours, and then sieved to obtain ultrafine titanium hydride powder with a particle size D50 of 20μm, wherein the oxygen content of the ultrafine titanium hydride powder is about 0.15%.

[0047] Example 3 like Figure 1 and 2 As shown, the apparatus for preparing hydride metals according to the present invention is used to perform hydride metallurgy on niobium scraps, followed by wet milling and sieving to prepare ultrafine hydride niobium powder. The specific process is as follows: S100: Niobium shavings of 1~3mm are acid-washed to remove surface grease and impurities, and then placed in an incubator at 130℃ for 2 hours to obtain dried niobium shavings.

[0048] S200: Dry niobium shavings are layered into the charging tray of the charging device 11 of the apparatus for preparing hydride metals according to the present invention. The niobium shavings are then heated to 400°C and held at that temperature while a vacuum is drawn to below 10 Pa. The pressure is then maintained and the niobium shavings are heated to 650-750°C. High-purity hydrogen gas is then introduced into the sealed furnace 4 through the gas inlet pipe 8 to 0.2 MPa and hydrogenated under pressure for 1.5 hours. After hydrogenation, the furnace is kept under pressure and cooled down. Finally, the hydrogenated niobium shavings are obtained by removing them from the furnace. During the hydrogenation process, after the high-purity hydrogen gas is introduced to 0.2 MPa, the gas valve 9 is closed. When the gas pressure in the sealed furnace 4 is lower than 0.15 MPa, the gas valve 9 on the gas inlet pipe 8 is opened and high-purity hydrogen gas is introduced again to 0.2 MPa. This process is repeated until the gas pressure in the sealed furnace 4 no longer decreases after 15 minutes or the hydrogenation time reaches 1.5 hours, at which point the hydrogenation is terminated.

[0049] S300: 304 stainless steel ball milling media and niobium hydrogenation chips are wet-milled in ethanol at a ball-to-material ratio of 3:1 for 1.5 hours, and then sieved to obtain ultrafine niobium hydrogenation powder with a particle size D50 of 15μm, wherein the oxygen content of the ultrafine niobium hydrogenation powder is about 0.16%.

[0050] The above description is merely a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.

Claims

1. An apparatus for preparing metal hydride, comprising a furnace body (1), a heating device (2), a furnace cover (3), and a thermocouple, characterized in that: The furnace body (1) is a cylindrical structure with an open top, and a sealed cover plate (20) is fixedly installed on the open top. The top of the cover plate (20) is provided with an upwardly extending furnace neck (5), and the furnace neck (5) is sealed and fixedly connected to the cover plate (20). A sealed furnace tank (4) is provided inside the furnace body (1), and the heating device (2) is arranged around the outside and / or below the sealed furnace tank (4). The upper part of the sealed furnace tank (4) passes through the cover plate (20) and the furnace neck (5) in sequence and is fixedly connected to the furnace neck (5). The furnace cover (3) is detachably fixed at the top of the furnace neck (5). A sealing ring (6) is provided between the furnace cover (3) and the furnace neck (5). An exhaust pipe (7) connected to a vacuum device is provided through the furnace cover (3). An inlet pipe (8) connected to a gas supply device is also connected in parallel to the exhaust pipe (7). A gas valve (9) is provided on the exhaust pipe (7) and the inlet pipe (8). A pressure gauge (10) is also provided on the exhaust pipe (7) or the inlet pipe (8). The thermocouple passes through the furnace cover (3) and extends into the sealed furnace tank (4). A charging device (11) is provided inside the sealed furnace tank (4). The charging device (11) is a tower-shaped structure with multiple charging trays spaced apart. Cooling water channels are arranged around the furnace neck (5) and furnace cover (3). Water inlet I (12) and water outlet I (13) connected to the internal cooling water channels are respectively arranged on both sides of the furnace neck (5). Water inlet II (14) and water outlet II (15) connected to the internal cooling water channels are respectively arranged on both sides of the furnace cover (3). Water outlet I (13) is connected to water inlet II (14) through a pipe. Water inlet I (12) and water outlet II (15) are respectively connected to the water supply pipe and water return pipe of the cooling water circulation system. The furnace neck (5) is circular and has multiple lugs (16) evenly distributed around its top edge. The lugs (16) facing the center of the furnace neck (5) have slots. The top of the furnace cover (3) has multiple limiting ribs (17) spaced apart. The top center of the furnace cover (3) has a fixed rod (18) fixed vertically. The limiting ribs (17) are evenly distributed around the top of the furnace cover (3), with their inner ends fixedly connected to the fixed rod (18) and their outer ends extending out of the edge of the furnace cover (3). The limiting ribs (17) and the slots of the lugs (16) can be tightly engaged and interlocked. The exhaust pipe (7) is vertically installed on the furnace cover (3). The intake pipe (8) has an inverted L-shaped structure with the intake port facing the furnace cover (3) and the exhaust port end is vertically connected to the exhaust pipe (7). The air passage between the intake port of the intake pipe (8) and the opening (19) of the exhaust pipe (7) in the sealed furnace (4) forms a right trapezoid. The base formed by the opening (19) to the end of the exhaust pipe (7) connected to the intake pipe (8) in the right trapezoid and the hypotenuse formed by the straight connection between the opening (19) and the intake port of the intake pipe (8) are of equal length. The sealing ring (6) is a metal sealing ring, a graphite metal sealing ring, or a flexible graphite sealing ring.

2. A method for preparing hydride metal powder, characterized in that, The process includes pretreatment, hydrogenation, and ball milling and sieving steps, including the following steps: A. Pretreatment: Pickling removes surface grease and impurities from the metal material, followed by cleaning and drying to obtain dry metal material; B. Hydrogenation: Dry metal material is loaded into the charging tray of the metal hydrogenation preparation apparatus described in claim 1, and hydrogenated under pressure at 600~800℃ and hydrogen pressure of 0.1~0.2MPa for 1~2 hours, and then cooled and removed from the furnace to obtain the metal hydrogenation. C. Ball milling and sieving: Ball milling is carried out with the ball milling media and the hydride metal at a ball-to-material ratio of 2:1 to 4:1 for 0.5 to 2 hours, and the hydride metal powder is obtained by sieving. The ball milling media is 304 or 316 stainless steel.

3. The method for preparing hydride metal powder according to claim 2, characterized in that, In the hydrogenation step, the dried metal material is loaded into a charging tray, then heated to 350~400℃ and held at that temperature while being vacuumed to below 10Pa. Subsequently, the pressure is maintained and the metal material is heated to 600~800℃. Then, high-purity hydrogen gas is introduced to 0.1~0.2MPa and hydrogenation is carried out under pressure. After hydrogenation, the metal is discharged from the furnace while maintaining pressure and cooling.

4. The method for preparing hydride metal powder according to claim 3, characterized in that, During the hydrogenation process, high-purity hydrogen is continuously introduced and the pressure is maintained until the preset hydrogenation time is reached, at which point the hydrogenation ends and the temperature is lowered; or during the hydrogenation process, high-purity hydrogen is introduced to the preset maximum pressure and then the gas valve (9) is closed. After the gas pressure in the sealed furnace (4) is lower than the preset minimum pressure, the gas valve (9) is opened again and high-purity hydrogen is introduced to the preset maximum pressure until the gas pressure in the sealed furnace (4) no longer decreases within 10 to 30 minutes or the preset hydrogenation time is reached, at which point the hydrogenation ends and the temperature is lowered.

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