CN112382499B - Preparation method of neodymium iron boron and nano Fe powder high-performance composite permanent magnet material - Google Patents
Preparation method of neodymium iron boron and nano Fe powder high-performance composite permanent magnet material Download PDFInfo
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- CN112382499B CN112382499B CN202011322850.5A CN202011322850A CN112382499B CN 112382499 B CN112382499 B CN 112382499B CN 202011322850 A CN202011322850 A CN 202011322850A CN 112382499 B CN112382499 B CN 112382499B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus 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
- H01F41/02—Apparatus 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
- H01F41/0253—Apparatus 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets 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
- H01F1/04—Magnets 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
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
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Abstract
The invention discloses a preparation method of a high-performance composite permanent magnetic material of neodymium iron boron and nano Fe powder, which comprises the following steps: mixing nanoscale iron powder with an organic solvent to form a diffusion source mixed solution; perforating the surface of the neodymium iron boron magnet by using femtosecond to nano laser pulse to form a coalball-shaped magnet; immersing the coal ball-shaped magnet into the diffusion source mixed solution, taking out the magnet, presintering the magnet at low temperature under the protection of nitrogen, and obtaining the magnet with the diffusion source coating inside and on the surface of the magnet; and finally, carrying out heat treatment on the magnet under the protection of argon and a strong magnetic field to obtain the high-performance neodymium iron boron magnet. On the basis of not destroying the orientation of the neodymium iron boron hard magnetic phase, the invention ensures that the soft magnetic phase can be uniformly distributed in the hard magnetic phase matrix through diffusion, realizes the effective addition of the soft magnetic phase, improves the magnetic performance of the neodymium iron boron permanent magnet, and has simple process, easy operation and suitability for batch production.
Description
Technical Field
The invention relates to the technical field of magnetic materials, in particular to a preparation method of a high-performance composite permanent magnetic material of neodymium iron boron and nano Fe powder.
Background
Although many advances have been made experimentally since the concept of nano-bi-phase composite permanent magnetic materials was proposed, the progress in the preparation of anisotropic bulk materials is slow. The bottom-up approach is a potential route to the preparation of anisotropic nanocomposite magnets. The anisotropic nano two-phase composite permanent magnetic material is mainly prepared by preparing anisotropic nano hard magnetic particles and forming a certain coating structure with the soft magnetic particles, obtaining an anisotropic green compact by using a magnetic field orientation forming technology, and obtaining the block-state anisotropic nano two-phase composite permanent magnetic material by subsequent processes such as hot pressing or sintering. Nd (neodymium)2Fe14B is difficult to be prepared controllably by a chemical method due to the complex crystal structure and the active chemical property of the rare earth element. Therefore, the problem of preparing high-performance nano permanent magnetic particles is solved firstly.
Despite the important progress in understanding the soft and hard magnetic phase exchange coupling mechanism and in the preparation of nanocomposite magnets in recent years, experimental results are far from the ultrahigh magnetic energy product of nanocomposite magnets given by theoretical models. The most important difficulty is how to prepare a microstructure required by a theoretical model, namely, the hard magnetic phase is fully oriented, and the soft magnetic phase is uniformly dispersed in a hard magnetic phase matrix, namely, an anisotropic nano composite magnet.
Currently, there are many methods of adding soft magnetic phase, such as high energy ball milling, CVD, sonochemical methods, electrochemical coating, etc., which to some extent introduce oxide layers, impurities and damage the hard magnetic phase. Therefore, there is a need to develop a simple and pollution-free method for effectively coating the soft magnetic phase on the hard magnetic particles, so as to realize breakthrough of magnetic performance.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of a neodymium iron boron and Fe high-performance composite permanent magnetic material.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a preparation method of a high-performance composite permanent magnetic material of neodymium iron boron and nano Fe powder comprises the following steps:
(1) preparation of diffusion source: fully mixing nanoscale iron powder and a certain amount of Cu or Al low-melting-point metal powder to form a mixture, and mixing the mixture with an organic solvent to form a diffusion source mixed solution;
(2) and (3) neodymium iron boron laser perforation: perforating the surface of the neodymium iron boron magnet by using femtosecond to nanosecond laser pulses to form a coalball-shaped magnet;
(3) coating the surface and the inside of the neodymium iron boron: immersing the coal ball-shaped magnet into the diffusion source mixed solution, taking out the magnet, and presintering the magnet at low temperature under the protection of nitrogen to obtain a magnet with diffusion source coatings inside and on the surface;
(4) heat treatment under a magnetic field: and (4) carrying out heat treatment on the magnet obtained in the step (3) under the protection of argon and a strong magnetic field to obtain the neodymium iron boron magnet with high coercivity.
Specifically, the particle diameter of the iron powder and the metal in the step (1) is less than 15 nm, the low-melting-point metal is Cu or Al, the content of the low-melting-point metal in the mixture is 5-20 wt%, and the organic solvent is acetone or ethanol solution.
Specifically, the femtosecond to nanosecond laser pulse in the step (2) has the laser wavelength of 800-1560 nm, the pulse duration of 1 ps-10 ns, the pulse intensity of 100 uJ-100 mJ, the spot size of 5-100 μm and the distance between holes of 10 μm-10 mm.
Specifically, the low-temperature pre-sintering time in the step (3) is 1-10 hours, and the temperature is 80-150 ℃.
Specifically, the strong magnetic field in the step (4) is 7-12T, the heat treatment temperature is 200-600 ℃, and the heat treatment time is 24-36 h.
Compared with the prior art, the invention has the following implementation effects:
according to the preparation method of the neodymium iron boron and nano Fe powder high-performance composite permanent magnetic material, on the basis of not destroying the orientation of the neodymium iron boron hard magnetic phase, the soft magnetic phase can be uniformly distributed in the hard magnetic phase matrix through diffusion, so that the effective addition of the soft magnetic phase is realized, and the magnetic remanence and the maximum magnetic energy product of the neodymium iron boron permanent magnet are improved under the condition of not reducing the coercive force.
Drawings
Fig. 1 shows that the magnetic properties of the composite ndfeb magnet obtained by laser perforation assisted diffusion (examples 1 and 2) and the magnetic properties of the composite ndfeb magnet obtained by the conventional surface coating diffusion process (comparative examples 1 and 2).
Detailed Description
The present invention will be further described with reference to the following specific embodiments and comparative examples.
Example 1: a preparation method of a high-performance composite permanent magnetic material of neodymium iron boron and nano Fe powder comprises the following steps:
step (1) preparation of a diffusion source:
fully mixing nanoscale iron powder and a certain amount of Cu metal powder to form a mixture, wherein the content of Cu in the mixture is 5 wt%, and mixing the mixture with an organic solvent to form a diffusion source mixed solution;
and (2) carrying out neodymium iron boron laser perforation:
using femtosecond to nanosecond laser pulse, wherein the laser wavelength is 800nm, the pulse duration is 300fs, the pulse intensity is 150uJ, the spot size is 5 mu m, holes are punched on the surface of the neodymium iron boron magnet with the size of 10mm multiplied by 10mm, the distance between the holes is 10 mu m, and a coalball-shaped magnet is formed;
step (3), coating the surface and the inside of the neodymium iron boron:
immersing the coalball-shaped magnet into the diffusion source mixed solution, taking out the coalball-shaped magnet, and presintering the coalball-shaped magnet at the low temperature of 80 ℃ for 2 hours under the protection of nitrogen to obtain a magnet with diffusion source coatings in the interior and on the surface of the magnet;
step (4) heat treatment under a magnetic field:
and (4) carrying out heat treatment on the magnet obtained in the step (3) for 36h under the protection of argon and a strong magnetic field (7T), wherein the temperature is 300 ℃, and the magnetic property of the neodymium iron boron permanent magnet with high performance is shown in figure 1.
Comparative example 1:
the preparation procedure is the same as in example 1, except that there is no step (2), i.e., a conventional surface diffusion coating process is employed.
Example 2:
step (1) preparation of a diffusion source:
fully mixing nanoscale iron powder and a certain amount of Al metal powder to form a mixture, wherein the content of Al in the mixture is 15 wt%, and mixing the mixture with an organic solvent to form a diffusion source mixed solution;
and (2) carrying out neodymium iron boron laser perforation:
using femtosecond to nanosecond laser pulse, wherein the laser wavelength is 800nm, the pulse duration is 1ns, the pulse intensity is 100uJ, the spot size is 10 mu m, holes are punched on the surface of the neodymium iron boron magnet with the size of 20mm multiplied by 20mm, and the distance between the holes is 15 mu m, so as to form a coalball-shaped magnet;
step (3), coating the surface and the inside of the neodymium iron boron:
immersing the coal ball-shaped magnet into the diffusion source mixed solution, taking out, and presintering at the low temperature of 100 ℃ for 4 hours under the protection of nitrogen to obtain a magnet with diffusion source coatings inside and on the surface;
and (4) heat treatment under a magnetic field:
and (4) carrying out heat treatment on the magnet obtained in the step (3) for 24 hours under the protection of argon and a strong magnetic field (9T), wherein the temperature is 400 ℃, and thus obtaining the high-performance neodymium iron boron permanent magnet.
Comparative example 2:
the preparation procedure is the same as in example 2, except that there is no step (2), i.e., a conventional surface diffusion coating process is used.
Claims (5)
1. A preparation method of a high-performance composite permanent magnetic material of neodymium iron boron and nano Fe powder is characterized by comprising the following steps:
(1) preparation of diffusion source: fully mixing nanoscale iron powder and a certain amount of Cu or Al low-melting-point metal powder to form a mixture, and mixing the mixture with an organic solvent to form a diffusion source mixed solution;
(2) and (3) neodymium iron boron laser perforation: perforating the surface of the neodymium iron boron magnet by using femtosecond to nanosecond laser pulses to form a coalball-shaped magnet;
(3) coating the surface and the inside of the neodymium iron boron: immersing the coal ball-shaped magnet into the diffusion source mixed solution, taking out the magnet, and presintering the magnet at low temperature under the protection of nitrogen to obtain a magnet with diffusion source coatings inside and on the surface;
(4) heat treatment under a magnetic field: and (4) carrying out heat treatment on the magnet obtained in the step (3) under the protection of argon and a strong magnetic field to obtain the neodymium iron boron composite magnet with high performance.
2. The method according to claim 1, wherein the particle diameter of the iron powder and the metal in step (1) is less than 15 nm, the low-melting metal is one of Cu or Al, the content of the low-melting metal in the mixture is 5-20 wt%, and the organic solvent is acetone or ethanol solution.
3. The method according to claim 1, wherein the femtosecond to nanosecond laser pulse of step (2) has a laser wavelength of 800nm to 1560nm, a pulse duration of 200fs to 10ns, a pulse intensity of 100uJ to 100mJ, a spot size of 5 to 100 μm, and a hole pitch of 10 μm to 10 mm.
4. The method according to claim 1, characterized in that the low-temperature pre-sintering time in the step (3) is 1-10 h, and the temperature is 80-150 ℃.
5. The method according to claim 1, wherein the high magnetic field in step (3) is 7-12T, the heat treatment temperature is 200-600 ℃, and the heat treatment time is 24-36 h.
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| WO2012159096A2 (en) * | 2011-05-18 | 2012-11-22 | The Regents Of The University Of California | Nanostructured high-strength permanent magnets |
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