Heavy rare earth metal powder recovery device and recovery method

By combining vacuum treatment, inert gas protection, and hydrogen reaction with vibration and knocking, a heavy rare earth metal powder recovery device and method has been developed, which solves the problems of oxidation and safety hazards of heavy rare earth metal powder, and achieves efficient recovery of heavy rare earth hydrogenated powder with low oxygen content, thereby improving resource utilization efficiency.

CN120210567BActive Publication Date: 2025-12-16EARTH PANDA ADVANCE MAGNETIC MATERIAL +1
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Patent Information

Application Number
CN202510430920.5
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-04-08
Publication Date
2025-12-16
Estimated Expiration
2045-04-08

AI Technical Summary

Technical Problem

In existing technologies, the oxygen content of heavy rare earth metal powder increases during the cleaning process, which leads to a decrease in magnetic properties and poses safety hazards. Furthermore, traditional recycling methods are inefficient.

Method used

A heavy rare earth metal powder recovery device is adopted. This device achieves efficient recovery of heavy rare earth metal powder by combining vacuum treatment, inert gas protection and hydrogen reaction with vibration and knocking, reducing oxygen content and forming heavy rare earth hydrogenated powder.

Benefits of technology

It achieves complete recovery of heavy rare earth metal powder, with low oxygen content and high safety, and can be reused in subsequent grain boundary infiltration, thus improving the utilization efficiency of heavy rare earth resources.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application discloses a heavy rare earth metal powder recovery device and a recovery method. The recovery device comprises a main tank body, wherein the main tank body comprises an upper part and a lower part; a supporting part is arranged in the upper part; a material frame for placing a metal mesh with heavy rare earth metal powder adhered thereon is arranged on the supporting part; a plurality of pipeline interfaces are arranged on the main tank body; the lower part comprises a large end and a small end; the large end is connected with the upper part; the large end and the small end are connected through a guide slope; a vibration part is arranged on the guide slope and used for vibrating and knocking the side wall of the main tank body; and a recovery tank body is arranged, wherein a feeding port of the recovery tank body is connected with a discharging port of the main tank body. The heavy rare earth metal powder recovery device can completely recover the heavy rare earth metal powder adhered on the metal mesh, the oxygen content of the recovered heavy rare earth hydrogenated powder is low, the heavy rare earth hydrogenated powder can be repeatedly used in subsequent grain boundary penetration, and the heavy rare earth resource can be efficiently utilized.
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Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of permanent magnet materials, and particularly relates to a heavy rare earth metal powder recovery device and a heavy rare earth metal powder recovery method based on the heavy rare earth metal powder recovery device. BACKGROUND

[0002] Sintered neodymium iron boron (NdFeB) is currently the strongest rare earth permanent magnet material in terms of magnetic performance. For high remanence and high coercivity magnets (such as 45UH, 48UH, 50UH, etc.), based on cost requirements, a heavy rare earth grain boundary diffusion penetration process is currently often used. Generally, in operation, a heavy rare earth (commonly dysprosium, terbium heavy rare earth) or heavy rare earth alloy is plated or coated on the surface of the base material magnet. The heavy rare earth element penetrates and diffuses into the internal grain boundaries of the magnet under vacuum and high temperature conditions, thereby increasing the coercivity of the magnet. To prevent adhesion between products during the high-temperature penetration process, a metal mesh (such as a molybdenum mesh, etc.) is usually used to place the products (such as Figure 1 and Figure 2 As shown), so that the products are isolated from each other. However, while the heavy rare earth diffuses into the internal part of the magnet at high temperature, a small part of it also adheres to the metal mesh belt. When the metal mesh is used continuously subsequently, the heavy rare earth metal on the mesh belt (which has been in contact with air multiple times, and the heavy rare earth magnet powder absorbs moisture and the oxygen content increases) will diffuse into the internal part of the magnet again, affecting the magnetic performance of the magnet and reducing the penetration effect. Therefore, the metal mesh must be cleaned before being used repeatedly.

[0003] For these metal meshes, the current method often used is to use a mechanical method to polish and knock in the atmosphere or the box, so as to strip the heavy rare earth metal powder from the metal mesh. The heavy rare earth metal powder is heated and absorbs oxygen due to polishing or knocking, resulting in an increase in the oxygen content of the recovered heavy rare earth metal powder, which reduces the magnetic performance of the penetration magnet when the powder is reused as a silk screen powder. In addition, the heavy rare earth metal powder may be oxidized and combusted during the polishing process, causing safety accidents. SUMMARY

[0004] Therefore, the primary purpose of the present application is to provide a heavy rare earth metal powder recovery device that can completely recover heavy rare earth metal powder, is safe during the recovery process, has low oxygen content of the recovered heavy rare earth hydrogenated powder, and can be reused in subsequent grain boundary penetration, thereby achieving efficient use of heavy rare earth resources.

[0005] To achieve the above purpose, the present application adopts the following technical solutions:

[0006] One aspect of the present application provides a heavy rare earth metal powder recovery device, comprising:

[0007] A main tank body, the main tank body comprises an upper part and a lower part, the inside of the upper part is provided with a supporting part, a material frame is placed on the supporting part, the material frame is used for placing a metal mesh adhered with heavy rare earth metal powder; a plurality of pipeline interfaces are arranged on the main tank body, the pipeline interfaces are respectively connected with a vacuum pipeline, an inert gas pipeline, a hydrogen pipeline, a cooling water inlet pipeline and a cooling water outlet pipeline; the lower part comprises a large end and a small end, the large end is connected with the upper part, the large end and the small end are connected through a guide slope, a vibrating part is arranged on the guide slope, and the vibrating part is used for vibrating and knocking the side wall of the main tank body;

[0008] and a recovery tank body, the feeding port of the recovery tank body is connected with the discharging port of the main tank body.

[0009] Further scheme, the supporting part is a hollow platform, so that the heavy rare earth metal powder in the material frame can smoothly enter the recovery tank body. In the present application, the hollow platform refers to a platform provided with through holes, or a net structure. Preferably, the supporting part is a net platform.

[0010] Further scheme, preferably, the material frame is divided into a plurality of receiving parts. Specifically, the material frame is separated to form a plurality of receiving spaces, and the metal mesh adhered with heavy rare earth metal powder is separated and placed, so as to improve the sufficiency of the subsequent reaction. Preferably, each receiving part can accommodate a metal mesh adhered with heavy rare earth metal powder. In addition, in another specific embodiment of the present application, through holes are arranged on the outer side wall or the inner partition wall of the material frame, so as to further facilitate the entry of reaction gas into the material frame and improve the reactivity of the reaction gas and the heavy rare earth metal on the metal mesh.

[0011] Further scheme, the upper part is provided with a cover body and a fastener, the cover body is used for sealing the main tank body, and the fastener is used for locking the cover body and the main tank body. Specifically, the main tank body is sealed by the cover body, and the connection mode of the cover body and the main tank body is not particularly limited or required, and a conventional mode in the art can be used. In some preferred embodiments of the present application, the connection mode of the cover body and the main tank body is hinged. The fastener is a fastening rod, which is used for fastening the cover body and the main tank body. Preferably, a first sealing member, such as an elastic sealing ring, is arranged on the inner surface of the cover body and the upper end surface of the main tank body, so as to improve the sealing property between the cover body and the main tank body.

[0012] Further scheme, in the present application, the angle of the guide slope can be designed as required, and there is no particular limitation, as long as the hydrogenated heavy rare earth metal powder can smoothly enter the recovery tank body. In some specific embodiments of the present application, the guide slope forms an angle of 75° with the horizontal plane, so as to facilitate the hydrogenated heavy rare earth metal powder falling off from the metal mesh to fall into the recovery tank body.

[0013] In a further aspect, the vibrating part refers to any part that can knock the guide slope by vibration, so that the side hydrogenated heavy rare earth magnetic powder falls into the recovery tank. In some embodiments, the vibrating part is a pneumatic hammer. The number and angle of the vibrating part are not particularly limited, and can be adjusted according to the angle of the guide slope, for example, so that the side hydrogenated heavy rare earth magnetic powder can smoothly fall into the recovery tank. In some embodiments, the number of vibrating parts is three, and the vibrating parts are equally spaced from each other, and the vibrating parts are arranged at an angle of 120° with respect to the horizontal plane.

[0014] In a further aspect, the outlet of the main tank and the inlet of the recovery tank are respectively provided with first and second valves, so as to separate the main tank and the recovery tank from each other. For example, by closing the first valve of the main tank and the second valve of the recovery tank, the protective gas in the recovery tank can be kept inert, and the hydrogen gas in the main tank can be used as the main reaction gas to react with the heavy rare earth magnetic powder in the main tank.

[0015] In a further aspect, the end surface of the outlet of the main tank and the inlet of the recovery tank is respectively provided with a second sealing member, so as to increase the sealing performance of the main tank after vacuumizing. The second sealing member is the same as or similar to the first sealing member, and in some examples, both are elastic sealing rings.

[0016] Another aspect of the present application provides a method for recovering heavy rare earth metal powder, which is based on the heavy rare earth metal powder recovery device described above and comprises the following steps:

[0017] Placing the metal mesh with heavy rare earth metal powder adhered thereon in the frame, and placing the frame in the main tank, and locking and sealing the main tank; connecting the main tank and the recovery tank, and vacuumizing the main tank and the recovery tank, and stopping when the vacuum degree of the main tank is less than 0.1 Pa;

[0018] Filling inert gas into the main tank and the recovery tank, so that the pressure of the inert gas is not more than 50 KPa;

[0019] Separating the main tank and the recovery tank into independent spaces, filling hydrogen gas into the main tank, so that the pressure of the mixed gas of hydrogen gas and inert gas in the main tank is not more than 0.098 MPa, and opening the cooling water to cool the main tank, and the hydrogen gas reacts with the heavy rare earth metal powder on the metal mesh to form heavy rare earth metal hydride powder, which falls to the bottom of the main tank;

[0020] When the pressure of the mixed gas of hydrogen gas and inert gas in the main tank remains 0.095 MPa and does not decrease any more, the reaction is completed, the main tank and the recovery tank are connected, and the vibrating part is opened to vibrate and knock the side wall of the main tank, so that the heavy rare earth hydride powder on the side wall and the bottom of the main tank falls into the recovery tank.

[0021] The beneficial effects of this application are:

[0022] This application provides a heavy rare earth metal powder recovery device and method. The device enables the heavy rare earth metal powder to undergo a hydrogen absorption reaction within the main tank, forming more heavy rare earth metal powder. Simultaneously, the structural design at the bottom of the main tank allows for the recovery of heavy rare earth hydride powder on the metal mesh. Furthermore, the main tank is equipped with multiple pipe interfaces, allowing for the introduction of inert gas to control the reaction rate between heavy rare earth and hydrogen. The inert gas also serves as a protective gas within the recovery tank, protecting the recovered heavy rare earth hydride powder.

[0023] The heavy rare earth metal powder recovery device and method of this application not only achieve more thorough recovery, but also facilitate and ensure safety. Furthermore, the recovered heavy rare earth hydrogenated powder has a low oxygen content and can be reused through grain boundary infiltration, effectively improving the utilization of heavy rare earth resources. Attached Figure Description

[0024] Figure 1 This is a photograph of the actual magnet placement in the current heavy rare earth grain boundary diffusion infiltration process.

[0025] Figure 2 for Figure 1 A schematic diagram of the magnet placement in the medium-heavy rare earth grain boundary diffusion infiltration process.

[0026] Figure 3 This is a three-dimensional structural diagram of a heavy rare earth metal powder recovery device according to a preferred embodiment of this application.

[0027] Figure 4 for Figure 3 Schematic diagram of the internal structure of a medium-heavy rare earth metal powder recovery device.

[0028] Figure 5 for Figure 3 A schematic diagram of the cross-sectional structure of the main tank 1 and the recovery tank 2.

[0029] Figure 6 for Figure 3 A schematic diagram of the structure of the material frame 14.

[0030] Figure 7 for Figure 3 A schematic diagram of the structure of the recycling tank 2.

[0031] In the figure: 1-main tank body, 11-upper part, 12-lower part, 121-large end, 122-small end, 123-guiding slope, 13-supporting part, 14-material frame, 141-through hole, 15-vibrating part, 16-cover body, 161-fastener; 2-recovery tank body; 31-vacuum pipeline, 32-inert gas pipeline, 33-hydrogen pipeline, 34-cooling water inlet pipeline, 35-cooling water outlet pipeline; 41-first valve, 42-second valve; 51-first sealing member, 52-second sealing member. DETAILED DESCRIPTION

[0032] The embodiments of the present application will be described below in detail, the technical solutions in the embodiments described below are exemplary, and only possible technical implementations of the present application, and not all possible implementations. Those skilled in the art can combine the embodiments of the present application without creative labor to obtain other embodiments, and these embodiments are also within the protection scope of the present application.

[0033] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the present application belongs. The terms used in the specification of the present application are only for the purpose of describing the specific embodiments, and are not intended to limit the present application.

[0034] Example 1

[0035] In this embodiment, a heavy rare earth metal powder recovery device is first provided, which has a structure as shown in the figure. The heavy rare earth metal powder recovery device comprises a main tank body 1 and a recovery tank body 2, and the discharge port of the main tank body 1 is connected to the feed port of the recovery tank body 2, so that the treated heavy rare earth metal powder in the main tank body 1 can be recovered into the recovery tank body 2. Figure 1 The main tank body 1 comprises an upper part 11 and a lower part 12, which are in abutment and in communication. The upper part 11 provides a space for accommodating a metal mesh (such as a molybdenum mesh) with heavy rare earth metal powder adhered thereto, so that the metal mesh is reacted or treated therein. Specifically, the upper part 11 is provided with a supporting part 13, and a material frame 14 is placed on the supporting part 13, and the material frame 14 is used to place the metal mesh. In the embodiments of the present application, the supporting part 13 is a hollow platform or a mesh structure, so that the heavy rare earth hydrogenated powder peeled off from the metal mesh can smoothly enter the recovery tank body 2.

[0036] The main tank body 1 comprises an upper part 11 and a lower part 12, which are in abutment and in communication. The upper part 11 provides a space for accommodating a metal mesh (such as a molybdenum mesh) with heavy rare earth metal powder adhered thereto, so that the metal mesh is reacted or treated therein. Specifically, the upper part 11 is provided with a supporting part 13, and a material frame 14 is placed on the supporting part 13, and the material frame 14 is used to place the metal mesh. In the embodiments of the present application, the supporting part 13 is a hollow platform or a mesh structure, so that the heavy rare earth hydrogenated powder peeled off from the metal mesh can smoothly enter the recovery tank body 2.

[0037] In the embodiment of the present application, the material frame 14 is divided into several independent spaces, so that the metal mesh can be placed separately, which is convenient for the reaction. In addition, the side wall of the material frame 14 is provided with a plurality of through holes 141, so as to facilitate the reaction gas to fully contact with the heavy rare earth metal powder. The bottom of the material frame 14 is hollow or mesh-shaped, specifically, it can support the metal mesh, and at the same time, the heavy rare earth metal powder on the metal mesh can fall into the recovery tank body 2.

[0038] The lower part 12 includes a large end 121 and a small end 122, the large end 121 is connected with the upper part 11, and the large end 121 and the small end 122 are connected through a guide slope 123, so that the lower part 12 is funnel-shaped, which is convenient for guiding the heavy rare earth hydrogenated powder from the upper part 11 to the recovery tank body 2. It can be understood that the inclination angle of the guide slope 123 is not particularly limited, and can be adjusted according to the needs. In the embodiment, the guide slope 123 is 75° with the horizontal plane, so as to facilitate the hydrogenated heavy rare earth hydrogenated powder to fall into the recovery tank body 2. Further, a plurality of vibration parts 15 are arranged on the inner surface of the guide slope 123, and the specific number can be selected according to the needs. In the embodiment, three vibration parts 15 are arranged, and the interval between each vibration part 15 is equal. The vibration part 15 is used to vibrate the side wall of the main tank body 1, so that the hydrogenated heavy rare earth powder falling on the guide slope 123 is shaken to fall into the recovery tank body 2. Specifically, the angle of the vibration part 15 can be set according to the needs. In the embodiment, the vibration part 15 is 120° with the horizontal plane, so as to facilitate the hydrogenated heavy rare earth powder on the side wall to shake and fall into the recovery tank body 2. It can be understood that the vibration part 15 can be any common part in the art. In the embodiment, the vibration part 15 is a gas vibration hammer, but is not limited thereto.

[0039] Further, the main tank body 1 is provided with a plurality of pipeline interfaces for connecting the main tank body 1 with external pipelines or equipment to supply reaction gas and the like into the main tank body 1. In the embodiment, preferably, the pipeline interfaces are provided on the side wall of the main tank body 1. Specifically, the main tank body 1 is connected with a vacuum pipeline 31, an inert gas pipeline 32, a hydrogen pipeline 33, and the main tank body 1 is further connected with a cooling water inlet pipeline 34 and a cooling water outlet pipeline 35, wherein the vacuum pipeline 31 is used for vacuumizing the main tank body 1 to ensure the vacuum environment inside the main tank body 1. The inert gas pipeline 32 is used for introducing protective gas into the main tank body 1, which aims to avoid the heavy rare earth hydride powder in the main tank body 1 from being oxidized. The introduced inert gas is a protective gas well known in the art, such as noble gas, and in the embodiment, the introduced protective gas is argon. The hydrogen pipeline 33 is used for introducing hydrogen into the main tank body 1, which can react with the heavy rare earth metal powder on the metal mesh as reaction gas to generate heavy rare earth hydride powder. Since the hydrogen absorption reaction of the heavy rare earth metal powder with hydrogen releases heat, in the embodiment, the cooling water inlet pipeline 34 and the cooling water outlet pipeline 35 are arranged to cool the main tank body 1 to improve the safety of the whole recovery process.

[0040] Further, the upper portion 11 of the main tank body 1 is provided with a cover body 16 for sealing the main tank body 1. The connection mode of the cover body 16 and the main tank body 1 is not particularly required and can be a common mode in the art. In the embodiment, preferably, the cover body 16 is hinged to the main tank body 1, and the upper portion 11 of the main tank body 1 is provided with a fastener 161 located on the side of the main tank body 1 away from the hinged end of the cover body 16. After the cover body 16 seals the main tank body 1, the cover body 16 and the main tank body 1 are fastened and locked by the fastener 161. Further, the upper end surface of the upper portion 11 and the inner surface of the cover body 16 are both provided with a first sealing member 51 to increase the sealing property of the main tank body 1.

[0041] The recovery tank body 2 and the main tank body 1 can be directly connected, but preferably, in the embodiment, the discharge port of the main tank body 1 and the feed port of the recovery tank body 2 are respectively provided with a first valve 41 and a second valve 42, so as to facilitate the isolation of the main tank body 1 and the recovery tank body 2. Specifically, after the recovery tank body 2 is filled with inert gas, the first valve 41 and the second valve 42 can be closed to isolate the main tank body 1, the main tank body 1 is then filled with reaction gas hydrogen for reaction, and the recovered heavy rare earth hydride powder in the recovery tank body 2 can be protected. Further, the end surfaces of the discharge port of the main tank body 1 and the feed port of the recovery tank body 2 are respectively provided with a second sealing member 52 to increase the sealing property of the main tank body 1 and the recovery tank body 2, and to better connect the main tank body 1 and the recovery tank body 2, and to improve the sealing property of the main tank body 1 after vacuumizing.

[0042] The first seal 51 and the second seal 52 are both sealing elements that are conventional in the art, and can be, for example, elastic sealing rings.

[0043] Example 2

[0044] A heavy rare earth metal recovery method is provided in this example, and is based on the heavy rare earth metal recovery device described above. The specific steps are as follows:

[0045] The main tank 1 is connected to an external vacuum pump through the vacuum pipeline 31, and the vacuum pump is used to vacuumize the main tank 1 and the recovery tank 2. After the vacuum degree of the main tank 1 is lower than 0.1 Pa, the vacuumization is stopped.

[0046] Argon is filled into the main tank 1 and the recovery tank 2 through the inert gas pipeline 32 at 50 kPa. The argon controls the reaction speed of the hydrogen and the heavy rare earth metal powder, and at the same time, the argon acts as a protective gas to protect the heavy rare earth hydride powder in the main tank 1 and the recovery tank 2 from being oxidized.

[0047] The first valve 41 at the discharge port of the main tank 1 and the second valve 42 at the inlet of the recovery tank 2 are closed, and the hydrogen pipeline 33 is opened to fill hydrogen into the main tank 1. The pressure of the hydrogen and the argon in the main tank 1 is controlled to be no more than 0.098 MPa. The hydrogen acts as a reaction gas to react with the heavy rare earth metal powder on the metal mesh in the material frame 14 to form heavy rare earth hydride powder. Since the hydrogen absorption reaction of the heavy rare earth releases heat, the main tank 1 is cooled at the same time through the cooling water inlet pipeline 34 and the cooling water outlet pipeline 35.

[0048] The heavy rare earth hydride powder falls off the metal mesh. Since the bottom of the material frame 14 is mesh-shaped, the heavy rare earth hydride powder formed can fall to the bottom of the main tank 1. When the pressure of the mixed gas of argon and hydrogen in the main tank 1 remains at 0.095 MPa and no longer decreases (the hydrogen absorption reaction of the heavy rare earth forms heavy rare earth hydride, consumes hydrogen, and the pressure of the mixed gas in the main tank 1 decreases), the reaction is ended. The first valve 41 at the discharge port of the main tank 1 and the second valve 42 at the inlet of the recovery tank 2 are opened, and at the same time, the vibration part 15 is opened to vibrate and knock the side wall of the main tank 1, so that the heavy rare earth hydride powder on the side wall and the bottom of the main tank 1 enters the recovery tank 2.

[0049] In the entire recovery process, the heavy rare earth metal powder in the metal mesh reacts with the hydrogen to form heavy rare earth hydride powder under low oxygen conditions (high vacuum degree of the main tank 1), so that the heavy rare earth metal powder is completely recovered. At the same time, the oxygen content of the recovered heavy rare earth hydride powder is low, and the heavy rare earth hydride powder can be reused in the subsequent infiltration process, realizing efficient utilization of heavy rare earth resources.

[0050] Comparative Example

[0051] In the comparative example, the heavy rare earth metal powder is recovered by using the traditional process, i.e. the Tb powder on the metal mesh is stripped by grinding and knocking, and then the recovered Tb powder is treated by hydrogen crushing. The hydrogen crushing process parameters are consistent with the tank hydrogen absorption process in Example 2, and the terbium hydride TbH powder is obtained.

[0052] Example 3

[0053] In this example, the molybdenum mesh (with heavy rare earth Tb powder adhered) recovered in multiple batches in the grain boundary diffusion process is recovered according to the recovery method of Example 2, and the powder recovered by the method in the comparative example is used as a control.

[0054] The oxygen content of the recovered TbH powder is tested by using an EMGA-830 oxygen-nitrogen-hydrogen tester and the inert gas melting-infrared absorption method (IGA) which is well known in the art.

[0055] According to the test, the oxygen content of the TbH powder recovered according to the recovery method of the present application is 600ppm-800ppm, while the oxygen content of the TbH powder recovered by the traditional method in the comparative example is basically 1500ppm-2200ppm. It shows that the heavy rare earth metal powder recovered by the recovery device and the recovery method of the present application has the characteristics of low oxygen.

[0056] Further, in this example, the recovered TbH powder is subjected to grain boundary diffusion according to the following infiltration process, and the TbH powder in the comparative example is used as a control test.

[0057] The grain boundary diffusion process steps are as follows:

[0058] S1, select a 54M blank magnet; cut into 20mm×20mm×4mm (M) magnets, and the magnets are subjected to oil removal + pickling + ultrasonic cleaning;

[0059] S2, air-jet mill the recovered TbH powder to obtain a powder with an average particle size of 2um-3um;

[0060] S3, at room temperature, silk screen the TbH powder on the surface of the magnet, and the powder weight gain is 0.4%-0.5%;

[0061] S4, place the permanent magnet obtained in step S3 in a heat treatment furnace, heat to 900℃ under a vacuum degree higher than 9×10 –3 Pa for 12 hours, and perform infiltration diffusion treatment; after the infiltration diffusion time is over, fill argon Ar to open the air cooling machine to cool below 90℃;

[0062] S5, place the permanent magnet obtained in step S4 in a heat treatment furnace, heat to 900℃ under a vacuum of 4×10 –1The sintered Nd-Fe-B magnet obtained after the 54M substrate magnet, the recycling method in Embodiment 2 of the present application, and the sintered Nd-Fe-B magnet obtained after the traditional method grain boundary diffusion in the comparative example were respectively subjected to normal temperature (25℃) magnetic property test (test standard, refer to Permanent Magnet (Hard Magnet) Pulse Measurement Method Guide GB / T 29628-2013), and the test results are shown in Table 1.

[0063] The sintered Nd-Fe-B magnet obtained after the 54M substrate magnet, the recycling method in Embodiment 2 of the present application, and the sintered Nd-Fe-B magnet obtained after the traditional method grain boundary diffusion in the comparative example were respectively subjected to normal temperature (25℃) magnetic property test (test standard, refer to Permanent Magnet (Hard Magnet) Pulse Measurement Method Guide GB / T 29628-2013), and the test results are shown in Table 1.

[0064] Table 1: Normal temperature magnetic property test results of sintered Nd-Fe-B magnet

[0065]

[0066] It can be seen from the test results in Table 1 that the intrinsic coercivity Hcj of the magnet after the TbH powder collected by the recycling method of the present application is significantly improved, and has little effect on other magnetic properties (such as maximum magnetic energy product, squareness, etc.) of the magnet. Although the intrinsic coercivity Hcj of the TbH powder collected by the traditional method in the comparative example is also improved, the effect is not as good as the heavy rare earth metal powder collected by the recycling method of the present application, and has a greater impact on other magnetic properties of the magnet.

[0067] It should be noted that the present application is not limited to the above-mentioned embodiments. The above-mentioned embodiments are only examples, and embodiments having the same technical idea and playing the same role and effect within the scope of the technical solution of the present application are all included in the technical scope of the present application. In addition, within the scope of the main idea of the present application, various modifications of the embodiments that can be thought of by those skilled in the art, and other ways constructed by combining part of the constituent elements in the embodiments are also included in the scope of the present application.

Claims

1. A heavy rare earth metal powder recovery device, characterized in that, The application relates to a main tank body and a recovery tank body. The main tank body comprises an upper part and a lower part, the inside of the upper part is provided with a supporting part, a material frame is arranged on the supporting part, the material frame is used for placing a metal screen adhered with heavy rare earth metal powder, a plurality of pipeline interfaces are arranged on the main tank body, the pipeline interfaces are respectively connected with vacuum pipelines, inert gas pipelines, hydrogen pipelines, cooling water inlet pipelines and cooling water outlet pipelines, the lower part comprises a large end and a small end, the large end is connected with the upper part, the large end and the small end are connected through a guide slope, a vibration part is arranged on the guide slope and used for vibrating and knocking the side wall of the main tank body. The recovery tank body is connected with the outlet of the main tank body. The supporting part is a net-shaped platform. The material frame is divided into a plurality of receiving parts, each receiving part can receive a metal screen adhered with heavy rare earth metal powder, and through holes are arranged on the outer side wall and the inner partition wall of the material frame. The upper part is provided with a cover and a fastener, the cover is used for sealing the main tank body, and the fastener is used for locking the cover and the main tank body; the inner surface of the cover and the upper end surface of the main tank body are provided with first sealing elements.

2. The heavy rare earth metal powder recovery apparatus of claim 1, wherein The guide slope is 75 degrees with the horizontal plane.

3. The heavy rare earth metal powder recovery apparatus of claim 1, wherein The vibration part is a gas vibration hammer.

4. The heavy rare earth metal powder recovery apparatus of claim 1, wherein The vibration part is 120 degrees with the horizontal plane.

5. The heavy rare earth metal powder recovery apparatus of claim 1, wherein First valves and second valves are arranged on the outlet of the main tank body and the inlet of the recovery tank body respectively.

6. The heavy rare earth metal powder recovery apparatus of claim 1, wherein Second sealing elements are arranged on the end surfaces of the outlet of the main tank body and the inlet of the recovery tank body.

7. A method for recovering heavy rare earth metal powder, which is performed using the heavy rare earth metal powder recovery apparatus according to any one of claims 1 to 6, characterized by, The application further discloses a method for preparing heavy rare earth metal powder. The metal screen adhered with heavy rare earth metal powder is placed in the material frame, the material frame is arranged in the main tank body, and the main tank body is locked and sealed; the main tank body and the recovery tank body are communicated, the main tank body and the recovery tank body are vacuumized, and the vacuum degree of the main tank body is less than 0.1 Pa after the vacuumization is stopped; Inert gas is filled into the main tank body and the recovery tank body, and the pressure of the inert gas is not more than 50 KPa; The main tank body and the recovery tank body are separated into independent spaces, hydrogen is filled into the main tank body, the pressure of the mixed gas of hydrogen and inert gas in the main tank body is not more than 0.098 MPa, the main tank body is cooled by cooling water, the heavy rare earth metal powder on the metal screen reacts with hydrogen to form heavy rare earth metal hydride powder, and the heavy rare earth metal hydride powder falls to the bottom of the main tank body; When the pressure of the mixed gas of hydrogen and inert gas in the main tank body is kept at 0.095 MPa and does not decrease any more, the reaction is ended, the main tank body and the recovery tank body are communicated, the vibration part is started to vibrate and knock the side wall of the main tank body, and the heavy rare earth metal hydride powder on the side wall and the bottom of the main tank body enters the recovery tank body.

Citation Information

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