CN112071545A - Surface treatment method for improving coercivity of neodymium iron boron base material - Google Patents

Surface treatment method for improving coercivity of neodymium iron boron base material Download PDF

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Publication number
CN112071545A
CN112071545A CN202010904377.5A CN202010904377A CN112071545A CN 112071545 A CN112071545 A CN 112071545A CN 202010904377 A CN202010904377 A CN 202010904377A CN 112071545 A CN112071545 A CN 112071545A
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neodymium
iron boron
neodymium iron
coercivity
iron
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CN202010904377.5A
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Chinese (zh)
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张震
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Anhui Hanhai New Material Co ltd
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Anhui Hanhai New Material Co ltd
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Priority to CN202010904377.5A priority Critical patent/CN112071545A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets

Abstract

The invention belongs to the field of neodymium iron boron production, and particularly discloses a surface treatment method for improving coercivity of a neodymium iron boron substrate, which comprises the following specific steps: s1: carrying out oil removal, acid cleaning and activation treatment on the sintered neodymium-iron-boron magnet base material; s2: forming an aluminum base film on the surface of the processed neodymium iron boron magnet by using an ion sputtering instrument, and heating and evaporating the alloy under a vacuum condition by using vacuum evaporation equipment to form a vacuum aluminum plated layer on the surface of the neodymium iron boron magnet; s3: tb is to be0.27Dy0.73Fe2Placing the alloy powder in the solution and fully stirring to form a mixed solution; s4: coating the mixed solution on the surface of the neodymium iron boron magnet, and performing diffusion treatment on the neodymium iron boron magnet by using a thermal diffusion treatment device; s5: ultrasonic treatment and drying. The aluminum die formed by the invention has excellent corrosion resistance; utilize hot diffusion and infiltration treatment device to carry out diffusion and infiltration treatment to neodymium iron boron magnetism body for neodymium iron boron magnetism body that makesThe coercive force is obviously improved, and the utilization rate of the heavy rare earth is higher.

Description

Surface treatment method for improving coercivity of neodymium iron boron base material
Technical Field
The invention relates to the field of neodymium iron boron production, in particular to a surface treatment method for improving the coercive force of a neodymium iron boron base material.
Background
The Nd-Fe-B permanent magnet is the permanent magnet material with the best magnetic performance at present, is widely applied to the fields of electronic information, electromechanics, instruments, medical instruments and the like, and is the fastest developing one of the magnetic materials. In recent years, with the accelerated development of science and technology, the popularization speed and the application range of the sintered neodymium-iron-boron magnet in high-end fields such as new energy automobiles, variable frequency compressors, wind power generation and the like are rapidly expanded. The sintered Nd-Fe-B magnet is required to have higher comprehensive magnetic performance in the fields, and particularly, the sintered Nd-Fe-B magnet is required to have high remanence and high coercive force. Therefore, how to improve the coercive force of the high neodymium iron boron substrate becomes a problem which needs to be solved urgently.
Disclosure of Invention
The invention aims to provide a surface treatment method for improving the coercivity of a neodymium iron boron base material, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a surface treatment method for the coercivity of a high neodymium iron boron base material comprises the following specific steps:
s1: carrying out oil removal, acid cleaning and activation treatment on the sintered neodymium-iron-boron magnet base material;
s2: forming an aluminum base film on the surface of the processed neodymium iron boron magnet by using an ion sputtering instrument, and heating and evaporating the alloy under a vacuum condition by using vacuum evaporation equipment to form a vacuum aluminum plated layer on the surface of the neodymium iron boron magnet;
s3: tb is to be0.27Dy0.73Fe2Placing the alloy powder in the solution and fully stirring to form a mixed solution;
s4: coating the mixed solution on the surface of the neodymium iron boron magnet, and performing diffusion treatment on the neodymium iron boron magnet by using a thermal diffusion treatment device;
s5: and (3) putting the magnet subjected to the diffusion treatment into ultrasonic equipment for ultrasonic treatment, and then drying to finish the surface treatment of the neodymium iron boron substrate.
Preferably, in step S3, the solution is ethanol, span-60, ethyl orthosilicate, silane coupling agent KH560 according to the ratio of 100-: 1.1-1.2: mixed liquid obtained by mixing the components in a ratio of 6-7: 30-35.
Preferably, in step S3, Tb0.27Dy0.73Fe2The ratio of alloy powder to solution is 0.9-1.1: 1.
preferably, the thermal diffusion treatment device comprises a base, the periphery of the top of the base extends upwards to form a sleeve, a diffusion treatment cover is embedded in the sleeve in a matching manner, the sleeve is of a cylindrical structure with a closed top surface and an open bottom surface, a heating seat is installed at the top of the diffusion treatment cover, and an electric heating pipe installed on the heating seat is arranged in the diffusion treatment cover; the electric heating pipes are surrounded to form a cylindrical structure, a plurality of layers are arranged at intervals from inside to outside, and a diffusion interlayer cavity is formed between every two adjacent layers of electric heating pipes; the bottom of the sleeve is provided with a turntable, a tray is arranged on the turntable, positioning grooves with annular inward-sinking structures are arranged on the tray corresponding to the positions of the diffusion interlayer cavities, and neodymium iron boron base materials obtained in the step S5 and distributed in an annular mode are placed in the positioning grooves; and a vacuum pumping hole and a pressure gauge are respectively arranged on two sides of the diffusion treatment cover.
Preferably, a driving motor is installed in the base, and the output end of the driving motor is upwards and vertically connected with the center of the turntable.
Preferably, the tray is made of a magnetic material, and the tray is magnetically attracted to the neodymium iron boron base material.
Preferably, a layer of rubber sealing layer is pasted on the inner wall of the sleeve, ear plates are symmetrically arranged on two sides of the permeation treatment cover, mounting plates are symmetrically arranged on two sides of the base under the two ear plates, a hydraulic telescopic rod is respectively mounted on the two mounting plates, and the output ends of the two hydraulic telescopic rods are upwards and respectively fixedly connected with the corresponding ear plates.
Preferably, the bottom surface of the tray is provided with a plurality of positioning blocks with protruding structures, and the top surface of the turntable is correspondingly provided with positioning grooves in which the positioning blocks are embedded.
Preferably, the base is provided with an operation panel, and the operation panel is respectively connected with the control ends of the electric heating pipe, the driving motor and the hydraulic telescopic rod.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the aluminum base film is formed on the surface of the magnet through magnetron sputtering, and then the vacuum aluminum coating layer is formed through a vacuum evaporation mode, so that the formed aluminum mold has excellent corrosion resistance; the invention is realized by adding a certain amount of Tb0.27Dy0.73Fe2Dissolving alloy powder to prepare mixed solution, coating the mixed solution on the surface of the neodymium iron boron magnet, performing diffusion treatment on the neodymium iron boron magnet by using a thermal diffusion treatment device, and coating the mixed solution on Tb on the surface layer of the magnet0.27Dy0.73Fe2The alloy will diffuse into the magnetIn the layer area, heavy rare earth elements in the coating layer can diffuse into the magnet, the microstructure of the magnet is improved together, the boundary structure of a magnetic phase is optimized, and the purpose of improving the coercivity is achieved, so that the coercivity of the prepared neodymium iron boron magnet is obviously improved, and the utilization rate of the heavy rare earth is higher.
2. The invention provides a thermal diffusion and permeation treatment device, which is characterized in that a plurality of diffusion and permeation interlayer cavities are formed in a heating mode of surrounding a plurality of layers of electric heating pipes, the inner side and the outer side of a magnet can be simultaneously heated, the heat distribution is uniform, the diffusion and permeation treatment device is matched with a tray and used for placing and treating the magnet in batches, the surface of the magnet is uniformly heated under the auxiliary action of a turntable, and the diffusion and permeation treatment device is good in diffusion and permeation effect.
Drawings
FIG. 1 is a schematic view of the thermal diffusion treatment apparatus according to the present invention;
FIG. 2 is a schematic distribution diagram of an electric heating tube and a neodymium-iron-boron substrate according to the present invention;
FIG. 3 is a schematic view of a specific structure of the tray of the present invention;
fig. 4 is a schematic view of an assembly structure of the tray and the turntable of the present invention.
In the figure: 1. a base; 2. a sleeve; 3. a diffusion treatment cover; 4. a heating base; 5. an electric heating tube; 6. a diffusion interlayer cavity; 7. a turntable; 8. a drive motor; 9. a tray; 10. positioning a groove; 11. positioning blocks; 12. a rubber sealing layer; 13. a vacuum pumping port; 14. a pressure gauge; 15. an ear plate; 16. mounting a plate; 17. a hydraulic telescopic rod.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "vertical", "upper", "lower", "horizontal", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of describing the present invention and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
In the description of the present invention, it should also be noted that, unless otherwise explicitly specified or limited, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Example 1: the invention provides a technical scheme that: a surface treatment method for the coercivity of a high neodymium iron boron base material comprises the following specific steps:
s1: carrying out oil removal, acid cleaning and activation treatment on the sintered neodymium-iron-boron magnet base material;
s2: forming an aluminum base film on the surface of the processed neodymium iron boron magnet by using an ion sputtering instrument, and heating and evaporating the alloy under a vacuum condition by using vacuum evaporation equipment to form a vacuum aluminum plated layer on the surface of the neodymium iron boron magnet;
s3: tb is to be0.27Dy0.73Fe2Placing the alloy powder in the solution and fully stirring to form a mixed solution;
s4: coating the mixed solution on the surface of the neodymium iron boron magnet, and performing diffusion treatment on the neodymium iron boron magnet by using a thermal diffusion treatment device;
s5: and (3) putting the magnet subjected to the diffusion treatment into ultrasonic equipment for ultrasonic treatment, and then drying to finish the surface treatment of the neodymium iron boron substrate.
In the present embodiment, in step S3, the solution is ethanol, span-60, ethyl orthosilicate, silane coupling agent KH560 according to the formula of 100-: 1.1-1.2: mixed liquid obtained by mixing the components in a ratio of 6-7: 30-35.
In the present embodiment, in step S3, Tb0.27Dy0.73Fe2The ratio of alloy powder to solution is 0.9-1.1: 1.
firstly, forming an aluminum base film on the surface of a magnet through magnetron sputtering, and then forming a vacuum aluminum plated layer through a vacuum evaporation mode, wherein the formed aluminum die has excellent corrosion resistance; the invention is realized by adding a certain amount of Tb0.27Dy0.73Fe2Dissolving alloy powder to prepare mixed solution, coating the mixed solution on the surface of the neodymium iron boron magnet, performing diffusion treatment on the neodymium iron boron magnet by using a thermal diffusion treatment device, and coating the mixed solution on Tb on the surface layer of the magnet0.27Dy0.73Fe2The alloy can diffuse and enter the surface layer area of the magnet, the heavy rare earth element in the coating layer can diffuse and enter the magnet, the microstructure of the magnet is improved and the boundary structure of the magnetic phase is optimized together, the purpose of improving the coercivity is achieved, the coercivity of the manufactured neodymium iron boron magnet is obviously improved, and the utilization rate of the heavy rare earth is higher.
Example 2: referring to fig. 1-4, the thermal diffusion treatment device includes a base 1, a sleeve 2 is formed by extending upward from the top periphery of the base, a diffusion treatment cover 3 is inserted into the sleeve 2, the sleeve is of a cylindrical structure with a closed top surface and an open bottom surface, a heating base 4 is installed on the top of the diffusion treatment cover 3, and an electric heating tube 5 installed on the heating base 4 is arranged inside the diffusion treatment cover 3; the electric heating pipes 5 are surrounded to form a cylindrical structure, a plurality of layers are arranged at intervals from inside to outside, and a diffusion interlayer cavity 6 is formed between every two adjacent layers of electric heating pipes 5; the bottom of the sleeve 2 is provided with a turntable 7, a tray 9 is arranged on the turntable, positioning grooves 10 with annular inward-concave structures are arranged on the positions, corresponding to the diffusion interlayer cavities 6, of the tray 9, and neodymium iron boron base materials obtained through treatment in the step S5 and distributed in an annular mode are placed in the positioning grooves 10; and a vacuum pumping hole 13 and a pressure gauge 14 are respectively arranged on two sides of the diffusion treatment cover 3.
In this embodiment, a driving motor 8 is installed in the base 1, and its output end is connected vertically to the center of the turntable 7.
In this embodiment, the tray 9 is made of a magnetic material, which is magnetically attracted to the ndfeb substrate.
In this embodiment, a layer of rubber sealing layer 12 is adhered to the inner wall of the sleeve 2, two side symmetry of the permeation treatment cover 3 is provided with the ear plates 15, two sides of the base 1 are symmetrically provided with mounting plates 16 under the two ear plates 15, two hydraulic telescopic rods 17 are respectively mounted on the two mounting plates 16, and output ends of the two hydraulic telescopic rods 17 are upwards and respectively fixedly connected with the corresponding ear plates 15.
In this embodiment, the bottom surface of the tray 9 is provided with a plurality of positioning blocks 11 with protruding structures, and the top surface of the turntable 7 is correspondingly provided with positioning grooves in which the positioning blocks 11 are embedded.
In this embodiment, the base 1 is provided with a control panel, and the control panel is connected to the electric heating pipe 5, the driving motor 8 and the control end of the hydraulic telescopic rod 17.
The working principle is as follows: and during diffusion treatment, each electrical device is connected with an external power supply.
In the initial state, the diffusion treatment cover 3 is lifted above the sleeve 2, and the turntable 7 is in an exposed state; firstly, a tray 9 is arranged on a turntable 7, a positioning block 11 at the bottom of the tray is embedded into a positioning groove of the tray 7, and then the processed neodymium-iron-boron magnet is vertically placed along an annular positioning groove 10 of the tray 9 to form a plurality of rings which are distributed inside and outside; starting a hydraulic telescopic rod 17, moving the diffusion treatment cover 3 downwards to be embedded into the sleeve 2 to form a sealing structure, and covering the electric heating pipes 5 on each layer outside the annular neodymium iron boron magnets to form an enclosing structure; the inside of the diffusion treatment cover 3 is vacuumized by a vacuum pump through a vacuum pumping hole 13, and the vacuum degree inside the diffusion treatment cover is observed through a pressure gauge 14; after a vacuum state is formed in the diffusion treatment cover 3, the power supply of the electric heating pipe 5 is turned on for heating, and meanwhile, the driving motor 8 is started to drive the tray 9 to rotate so as to uniformly heat the surface of the magnet.
After the heat treatment is finished, the hydraulic telescopic rod 17 is started, the diffusion treatment cover 3 is lifted to the initial position, and the tray 9 is taken down, so that the neodymium iron boron magnet is conveniently subjected to batch treatment.
It is worth noting that: the whole device realizes control to the control button on the control panel, and because the equipment matched with the control button is common equipment, the device belongs to the prior mature technology, and the electrical connection relation and the specific circuit structure are not repeated.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (9)

1. A surface treatment method for improving the coercivity of a neodymium iron boron base material is characterized by comprising the following specific steps:
s1: carrying out oil removal, acid cleaning and activation treatment on the sintered neodymium-iron-boron magnet base material;
s2: forming an aluminum base film on the surface of the processed neodymium iron boron magnet by using an ion sputtering instrument, and heating and evaporating the alloy under a vacuum condition by using vacuum evaporation equipment to form a vacuum aluminum plated layer on the surface of the neodymium iron boron magnet;
s3: tb is to be0.27Dy0.73Fe2Placing the alloy powder in the solution and fully stirring to form a mixed solution;
s4: coating the mixed solution on the surface of the neodymium iron boron magnet, and performing diffusion treatment on the neodymium iron boron magnet by using a thermal diffusion treatment device;
s5: and (3) putting the magnet subjected to the diffusion treatment into ultrasonic equipment for ultrasonic treatment, and then drying to finish the surface treatment of the neodymium iron boron substrate.
2. The surface treatment method for improving the coercivity of the neodymium-iron-boron substrate according to claim 1, is characterized in that: in step S3, the solution is ethanol, span-60, tetraethoxysilane and silane coupling agent KH560 according to the formula of 100-: 1.1-1.2: mixed liquid obtained by mixing the components in a ratio of 6-7: 30-35.
3. The surface treatment method for improving the coercivity of the neodymium-iron-boron substrate according to claim 1, is characterized in that: in step S3, Tb0.27Dy0.73Fe2Alloy (I)The ratio of the powder to the solution is 0.9-1.1: 1.
4. the surface treatment method for improving the coercivity of the neodymium-iron-boron substrate according to claim 1, is characterized in that: the thermal diffusion treatment device comprises a base (1), wherein the periphery of the top of the base extends upwards to form a sleeve (2), a diffusion treatment cover (3) is embedded in the sleeve (2) in a matching manner and is of a cylindrical structure with a closed top surface and an open bottom surface, a heating seat (4) is installed at the top of the diffusion treatment cover (3), and an electric heating pipe (5) installed on the heating seat (4) is arranged in the diffusion treatment cover (3); the electric heating pipes (5) are surrounded to form a cylindrical structure, a plurality of layers are arranged at intervals from inside to outside, and a diffusion interlayer cavity (6) is formed between two adjacent layers of electric heating pipes (5); a turntable (7) is arranged at the bottom of the sleeve (2), a tray (9) is arranged on the turntable, positioning grooves (10) with annular inward-concave structures are arranged on the tray (9) corresponding to the positions of the diffusion interlayer cavities (6), and neodymium iron boron base materials obtained in the step S5 and distributed annularly are placed in the positioning grooves (10); and a vacuum pumping hole (13) and a pressure gauge (14) are respectively arranged at two sides of the diffusion treatment cover (3).
5. The surface treatment method for improving the coercivity of the neodymium-iron-boron substrate according to claim 4, is characterized in that: a driving motor (8) is installed in the base (1), and the output end of the driving motor is upwards vertically connected with the center of the rotary table (7).
6. The surface treatment method for improving the coercivity of the neodymium-iron-boron substrate according to claim 4, is characterized in that: the tray (9) is made of a magnetic material and is attracted with the neodymium iron boron base material in a magnetic mode.
7. The surface treatment method for improving the coercivity of the neodymium-iron-boron substrate according to claim 4, is characterized in that: one deck rubber seal layer (12) is pasted to sleeve (2) inner wall, expands to ooze and handle cover (3) bilateral symmetry and be provided with otic placode (15), and base (1) both sides are provided with mounting panel (16) in the symmetry under two otic placodes (15), installs a hydraulic telescoping rod (17) on two mounting panels (16) respectively, the output of two hydraulic telescoping rod (17) upwards respectively with otic placode (15) rigid coupling that correspond.
8. The surface treatment method for improving the coercivity of the neodymium-iron-boron substrate according to claim 4, is characterized in that: the bottom surface of the tray (9) is provided with a plurality of positioning blocks (11) with protruding structures, and the top surface of the turntable (7) is correspondingly provided with positioning grooves in which the positioning blocks (11) are embedded.
9. The surface treatment method for improving the coercivity of the neodymium-iron-boron substrate according to claim 4, is characterized in that: the base (1) is provided with an operation panel which is respectively connected with the control ends of the electric heating pipe (5), the driving motor (8) and the hydraulic telescopic rod (17).
CN202010904377.5A 2020-09-01 2020-09-01 Surface treatment method for improving coercivity of neodymium iron boron base material Pending CN112071545A (en)

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