CN112017831B - Preparation method of high-toughness samarium-cobalt magnet - Google Patents
Preparation method of high-toughness samarium-cobalt magnet Download PDFInfo
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- CN112017831B CN112017831B CN202010842920.3A CN202010842920A CN112017831B CN 112017831 B CN112017831 B CN 112017831B CN 202010842920 A CN202010842920 A CN 202010842920A CN 112017831 B CN112017831 B CN 112017831B
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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
- H01F1/0555—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together
- H01F1/0557—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together sintered
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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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Abstract
The invention discloses a preparation method of a high-toughness samarium-cobalt magnet, which comprises the following steps: preparing powder, mixing powder, molding, sintering and aging treatment. On one hand, the added copper-based nanowires are distributed at the crystal boundary, so that the coercive force of the magnet can be improved; on the other hand, the carbon nano tube has good mechanical properties such as strength, elasticity, fatigue resistance, flexibility and the like, has a very high melting point, and does not change the form of the carbon nano tube in a grain boundary phase. Therefore, the strength and toughness of the grain boundary phase are optimized by adding the copper-based nanowires and the carbon nanotubes with high toughness, the purpose of improving the toughness of the samarium-cobalt magnet is achieved on the premise of damaging the magnetic performance of the samarium-cobalt magnet, the processing brittleness of the sintered samarium-cobalt magnet is reduced, and the mechanical stability of the samarium-cobalt magnet is improved.
Description
Technical Field
The invention relates to the field of rare earth permanent magnet materials, in particular to a preparation method of a high-toughness samarium-cobalt magnet.
Background
As a second-generation rare earth permanent magnet material, the 2. Compared with a neodymium-iron-boron magnet, the maximum working temperature of the 2. In addition, samarium cobalt magnets have a particularly strong corrosion resistance, and generally do not require surface protection treatment. However, the rare earth permanent magnet material has generally poor mechanical properties, particularly, samarium-cobalt magnets have large brittleness, poor ductility and low machining yield, and defects such as unfilled corners and cracks are easy to occur in the subsequent processes of turnover, inspection, magnetization and transportation of products. Severely restricts the further application of samarium cobalt magnets and hinders the conversion of China from the large rare earth resource country to the strong rare earth resource application country. Therefore, how to improve the mechanical properties of 2.
As an important magnetic functional material, people mainly focus on the magnetic properties, but the research on the mechanical properties is less. However, as instrumentation moves to miniaturization, weight reduction, miniaturization, and high precision, higher demands are placed on the mechanical properties of samarium-cobalt magnets both for reliability and stability. Chinese patent ZL201610272301.9 discloses a preparation method of a high-toughness samarium cobalt permanent magnet, the microstructure of a single-phase solid solution blank obtained by sintering is decomposed into a two-phase complex by controlling the aging process, unstable decomposition occurs inside each crystal grain, the two phases comprise 2. Chinese patent CN201910811537.9 discloses a preparation method of a high-toughness high-performance samarium cobalt magnet, which comprises the steps of coating pasty liquid obtained by mixing iron-based self-fluxing alloy powder and rare earth powder and performing high-energy ball milling on the surface of the samarium cobalt magnet, performing laser heating cladding treatment to obtain a laser cladding layer, and matching with subsequent high-intensity magnetic field auxiliary heat treatment to effectively promote the diffusion of rare earth atoms in the samarium cobalt magnet and improve the magnetic performance of the samarium cobalt magnet; meanwhile, the addition of the iron-based self-fluxing alloy improves the laser cladding property and toughness of the magnet. However, the mechanical property of the samarium cobalt magnet still has a large lifting space, and how to improve the mechanical property of the samarium cobalt magnet still needs to be solved urgently.
Disclosure of Invention
The invention aims to provide a preparation method of a high-toughness samarium-cobalt magnet, which can solve the problems of the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a high-toughness samarium-cobalt magnet comprises the following steps:
(1) Milling: preparing a 17-type samarium cobalt magnet, performing vacuum melting under the protection of helium, then performing coarse crushing under the protection of helium, then performing medium crushing under the protection of helium, and finally performing air flow milling powder under the protection of helium to prepare micron-sized samarium cobalt alloy powder;
(2) Mixing powder: fully mixing the micron-sized samarium cobalt alloy powder prepared in the step (1) with a tough material to prepare mixed powder;
(3) Molding: performing orientation molding on the mixed powder in the step (2) under the protection of helium, and then performing oil-cooled isostatic pressing to obtain a samarium-cobalt green compact;
(4) And (3) sintering: placing the samarium cobalt pressed blank in the step (3) into a vacuum sintering furnace, and sintering to obtain sintered samarium cobalt;
(5) Aging: and (5) placing the sintered samarium cobalt in the step (4) in an aging furnace for aging heat treatment, wherein high-purity helium is filled into the aging furnace in the cooling stage to prepare the sintered samarium cobalt magnet.
Preferably, in step (1), the composition of the 2: 25 to 27.5 weight percent of Sm, 48 to 51.2 weight percent of Co, 15 to 19 weight percent of Fe, 4.5 to 6 weight percent of Cu and 2 to 3 weight percent of Zr, placing the prepared 2.
Preferably, in the step (2), the tough material is composed of copper-based alloy nanowires and carbon nanotubes, the tough material has a diameter of 10-100 nm and a length of 1-20 μm, and the copper-based nanowires include at least one of Cu-Sm alloy nanowires, cu-Fe nanowires, cu-Co nanowires, or Cu-Zr nanowires.
Preferably, in the step (2), the micron-sized samarium cobalt alloy powder in the step (1), the copper-based alloy nanowire and the carbon nanotube are mixed according to the mass ratio of (98.0-99.4): (0.5-1.5): (0.1-0.5) and fully mixing to prepare mixed powder.
Preferably, in the step (3), the mixed powder is subjected to orientation molding in a magnetic field with a magnetic field strength of 1.5T or more, and the protective atmosphere is helium.
Preferably, in the step (4), the sintering temperature is 1180-1240 ℃, the sintering time is 2-8 hours, the solid melting temperature is 1150-1180 ℃, and the solid melting time is 2-6 hours.
Preferably, in the step (5), the aging temperature of the aging heat treatment is 820-860 ℃, and the aging time is 4-20 h.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the tough copper-based nanowires are added into the micron-sized samarium-cobalt alloy powder, so that the Cu content of the crystal boundary is increased, and the coercive force of the magnet is improved. The carbon nanotube has good mechanical properties such as strength, elasticity, fatigue resistance, flexibility and the like, the melting point of the carbon nanotube is 3652-3697 ℃, and the form of the carbon nanotube in a grain boundary phase cannot be changed. Therefore, the strength and toughness of the grain boundary phase are optimized by adding the copper-based nanowires and the carbon nanotubes with high toughness, the purpose of improving the toughness of the samarium-cobalt magnet is achieved on the premise of damaging the magnetic performance of the samarium-cobalt magnet, the processing brittleness of the sintered samarium-cobalt magnet is reduced, and the mechanical stability of the samarium-cobalt magnet is improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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.
Example 1
A preparation method of a high-toughness samarium-cobalt magnet comprises the following steps:
(1) Powder preparation:
first, the composition of a 2: 25wt% of Sm, 51.2wt% of Co, 15wt% of Fe, 6wt% of Cu and 2.8wt% of Zr. And placing the prepared 2. Then coarse crushing is carried out under the protection of helium, and then medium crushing is carried out under the protection of helium, wherein the average particle size of medium crushing powder is 0.1mm. Finally, the samarium cobalt alloy powder with the average grain size of 3.0 mu m is prepared by airflow milling under the protection of helium.
(2) Mixing powder:
mixing the prepared samarium cobalt alloy powder with the Cu-Sm alloy nanowire and the carbon nanotube according to the mass ratio of 98.0:1.5:0.5, wherein the Cu-Sm alloy nanowire and the carbon nanotube had a diameter of 10nm and a length of 1 μm, to prepare a mixed powder.
(3) Molding:
and (3) placing the mixed powder in a magnetic field with the magnetic field intensity of 1.5T for orientation forming under the protection atmosphere of helium, and then performing oil-cooled isostatic pressing to obtain the samarium cobalt green compact.
(4) And (3) sintering:
and placing the samarium cobalt compact in a vacuum sintering furnace for sintering heat treatment, wherein the sintering temperature is 1180 ℃, the sintering time is 2 hours, the solid melting temperature is 1150 ℃, and the solid melting time is 2 hours, so as to obtain the sintered samarium cobalt.
(5) Aging:
and placing the sintered samarium cobalt in a vacuum aging furnace for aging heat treatment, wherein the aging temperature is 820 ℃, the aging time is 4h, then cooling, and filling high-purity helium gas in the cooling stage to obtain the sintered samarium cobalt magnet.
Example 2
A preparation method of a high-toughness samarium-cobalt magnet comprises the following steps:
(1) Milling:
first, the composition of a 2: 26wt% of Sm, 48wt% of Co, 19wt% of Fe, 5wt% of Cu and 2wt% of Zr. The prepared 2. Then coarse crushing is carried out under the protection of helium, and then medium crushing is carried out under the protection of helium, wherein the average particle size of medium crushing powder is 0.3mm. Finally, the samarium cobalt alloy powder with the average grain size of 3.4 mu m is prepared by airflow milling under the protection of helium.
(2) Mixing powder:
mixing the prepared samarium cobalt alloy powder with the Cu-Fe alloy nanowire and the carbon nanotube according to the mass ratio of 99.0:0.8:0.2, fully mixing, wherein the diameter of the Cu-Fe alloy nano wire and the carbon nano tube is 30nm, and the length of the Cu-Fe alloy nano wire and the carbon nano tube is 7 mu m, and preparing mixed powder.
(3) Molding:
and (3) placing the mixed powder in a magnetic field with the magnetic field intensity of 1.8T for orientation forming under the protection atmosphere of helium, and then performing oil-cooled isostatic pressing to obtain the samarium-cobalt green compact.
(4) And (3) sintering:
and (3) placing the samarium cobalt compact in a vacuum sintering furnace for sintering heat treatment, wherein the sintering temperature is 1200 ℃, the sintering time is 4 hours, the solid melting temperature is 1160 ℃, and the solid melting time is 4 hours, so as to obtain the sintered samarium cobalt.
(5) Aging:
and placing the sintered samarium cobalt into a vacuum aging furnace for aging heat treatment, wherein the aging temperature is 830 ℃, the aging time is 8h, then cooling, and filling high-purity helium gas in the cooling stage to obtain the sintered samarium cobalt magnet.
Example 3
A preparation method of a high-toughness samarium-cobalt magnet comprises the following steps:
(1) Powder preparation:
first, the composition of a 2: 27.5wt% of Sm, 49wt% of Co, 16wt% of Fe, 4.5wt% of Cu and 3wt% of Zr. The prepared 2. Then coarse crushing is carried out under the protection of helium, and then medium crushing is carried out under the protection of helium, wherein the average particle size of medium crushing powder is 0.5mm. Finally, the samarium cobalt alloy powder with the average grain size of 3.8 mu m is prepared by airflow milling under the protection of helium.
(2) Mixing powder:
mixing the prepared samarium cobalt alloy powder with the Cu-Co alloy nanowire and the carbon nanotube according to the mass ratio of 99.4:0.5:0.1, fully mixing, wherein the diameter of the Cu-Co alloy nano wire and the carbon nano tube is 70nm, and the length of the Cu-Co alloy nano wire and the carbon nano tube is 15 mu m, and preparing mixed powder.
(3) Molding:
and (3) placing the mixed powder in a magnetic field with the magnetic field intensity of more than 2.0T for orientation forming under the protection atmosphere of helium, and then performing oil-cooled isostatic pressing to obtain the samarium-cobalt green compact.
(4) And (3) sintering:
and (3) placing the samarium cobalt compact into a vacuum sintering furnace for sintering heat treatment, wherein the sintering temperature is 1220 ℃, the sintering time is 6h, the solid solution temperature is 1170 ℃, and the solid solution time is 5h, so as to obtain the sintered samarium cobalt.
(5) Aging:
and placing the sintered samarium cobalt in a vacuum aging furnace for aging heat treatment, wherein the aging temperature is 850 ℃, the aging time is 15h, then cooling, and filling high-purity helium gas in the cooling stage to obtain the sintered samarium cobalt magnet.
Example 4
A preparation method of a high-toughness samarium-cobalt magnet comprises the following steps:
(1) Milling:
first, the composition of a 2: 26.3wt% of Sm, 48.2wt% of Co, 18wt% of Fe, 5wt% of Cu and 2.5wt% of Zr. And (3) placing the prepared 2. Then coarse crushing is carried out under the protection of helium, and then medium crushing is carried out under the protection of helium, wherein the average particle size of medium crushing powder is 0.7mm. Finally, the samarium cobalt alloy powder with the average grain size of 4.2 mu m is prepared by airflow milling under the protection of helium.
(2) Mixing powder:
mixing the prepared samarium cobalt alloy powder, the Cu-Zr alloy nanowire and the carbon nanotube according to the mass ratio of 98.7:1.0:0.3, fully mixing, wherein the diameter of the Cu-Zr alloy nano wire and the carbon nano tube is 100nm, and the length of the Cu-Zr alloy nano wire and the carbon nano tube is 20 mu m, and preparing mixed powder.
(3) Molding:
and (3) placing the mixed powder in a magnetic field with the magnetic field intensity of more than 2.2T for orientation forming under the protection atmosphere of helium, and then performing oil-cooled isostatic pressing to obtain the samarium-cobalt green compact.
(4) And (3) sintering:
and placing the samarium cobalt compact in a vacuum sintering furnace for sintering heat treatment, wherein the sintering temperature is 1240 ℃, the sintering time is 8 hours, the solid melting temperature is 1180 ℃, and the solid melting time is 6 hours, so as to obtain the sintered samarium cobalt.
(5) Aging:
and placing the sintered samarium cobalt in a vacuum aging furnace for aging heat treatment, wherein the aging temperature is 860 ℃, the aging time is 20 hours, then cooling, and filling high-purity helium gas in the cooling stage to obtain the sintered samarium cobalt magnet.
Comparative example 1
A method of making a samarium cobalt magnet, comprising the steps of:
(1) Powder preparation:
first, the composition of a 2: 25wt% of Sm, 51.2wt% of Co, 15wt% of Fe, 6wt% of Cu and 2.8wt% of Zr. The prepared 2. Then coarse crushing is carried out under the protection of helium, and then medium crushing is carried out under the protection of helium, wherein the average particle size of medium crushing powder is 0.1mm. Finally, the samarium cobalt alloy powder with the average grain size of 3.0 mu m is prepared by airflow milling under the protection of helium.
(2) Molding:
and (3) placing the mixed powder in a magnetic field with the magnetic field intensity of more than 2.2T for orientation forming under the protection atmosphere of helium, and then performing oil-cooled isostatic pressing to obtain the samarium-cobalt green compact.
(3) And (3) sintering:
and placing the samarium cobalt compact in a vacuum sintering furnace for sintering heat treatment, wherein the sintering temperature is 1200 ℃, the sintering time is 4 hours, the solid melting temperature is 1180 ℃, and the solid melting time is 3 hours, so as to obtain the sintered samarium cobalt.
(5) Aging:
and placing the sintered samarium cobalt into a vacuum aging furnace for aging heat treatment, wherein the aging temperature is 830 ℃, the aging time is 16h, then cooling, and filling high-purity helium gas in the cooling stage to obtain the sintered samarium cobalt magnet.
The magnetic properties and mechanical properties of the sintered samarium cobalt magnets of examples 1 to 4 and comparative example 1 were respectively tested at room temperature using a permanent magnet material measurement system according to the methods specified in GB/T3217-2013 and GB/T31967.2-2015, and the specific results are shown in table 1 below.
TABLE 1 test results of magnetic and mechanical properties of samarium cobalt magnets
As can be seen from the magnetic performance and mechanical performance test data given in Table 1, after the tough copper-based nanowires and carbon nanotubes are added into the micron-sized samarium-cobalt alloy powder, the coercive force of the magnet is obviously improved under the condition of ensuring that the product of residual magnetism and magnetic energy is not reduced. And the bending strength and the fracture toughness of the samarium cobalt magnet are also obviously improved, and the mechanical stability of the magnet is improved.
The foregoing is merely exemplary and illustrative of the present invention and various modifications, additions and substitutions may be made by those skilled in the art to the specific embodiments described without departing from the scope of the present invention as defined in the accompanying claims.
Claims (6)
1. A preparation method of a high-toughness samarium-cobalt magnet is characterized by comprising the following steps of:
(1) Powder preparation: preparing a 2: 25 to 27.5 weight percent of Sm, 48 to 51.2 weight percent of Co, 15 to 19 weight percent of Fe, 4.5 to 6 weight percent of Cu and 2 to 3 weight percent of Zr;
(2) Mixing powder: fully mixing the micron samarium cobalt alloy powder prepared in the step (1) with a tough material to prepare mixed powder, wherein the tough material consists of a copper-based alloy nanowire and a carbon nanotube, the diameter of the tough material is 10-100 nm, the length of the tough material is 1-20 mu m, and the copper-based alloy nanowire comprises at least one of a Cu-Sm alloy nanowire, a Cu-Fe nanowire, a Cu-Co nanowire or a Cu-Zr nanowire;
(3) Molding: performing orientation molding on the mixed powder in the step (2) under the protection of helium, and then performing oil-cooled isostatic pressing to obtain a samarium-cobalt green compact;
(4) And (3) sintering: placing the samarium cobalt compact in the step (3) into a vacuum sintering furnace, and sintering to obtain sintered samarium cobalt;
(5) Aging: and (5) placing the sintered samarium cobalt in the step (4) in an aging furnace for aging heat treatment, wherein high-purity helium is filled into the aging furnace in the cooling stage to prepare the sintered samarium cobalt magnet.
2. The method of making a high-toughness samarium cobalt magnet of claim 1, characterized in that: in the step (1), the prepared 2.
3. The method of making a high-toughness samarium cobalt magnet of claim 1, characterized in that: in the step (2), the micron-sized samarium cobalt alloy powder in the step (1), the copper-based alloy nanowire and the carbon nanotube are mixed according to the mass ratio of (98.0-99.4): (0.5-1.5): (0.1-0.5) and fully mixing to prepare mixed powder.
4. The method of making a high-toughness samarium cobalt magnet of claim 1, characterized in that: in the step (3), the mixed powder is placed in a magnetic field with the magnetic field intensity of more than 1.5T for orientation forming, and the protective atmosphere is helium.
5. The method of making a high tenacity samarium cobalt magnet in accordance with claim 1, wherein: in the step (4), the sintering temperature is 1180-1240 ℃, the sintering time is 2-8 hours, the solid melting temperature is 1150-1180 ℃, and the solid melting time is 2-6 hours.
6. The method of making a high-toughness samarium cobalt magnet of claim 1, characterized in that: in the step (5), the aging temperature of the aging heat treatment is 820-860 ℃, and the aging time is 4-20 h.
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