CN113690040A - Radiation-oriented nanocrystalline Co-based rare earth permanent magnet ring and preparation method thereof - Google Patents
Radiation-oriented nanocrystalline Co-based rare earth permanent magnet ring and preparation method thereof Download PDFInfo
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- CN113690040A CN113690040A CN202110732161.XA CN202110732161A CN113690040A CN 113690040 A CN113690040 A CN 113690040A CN 202110732161 A CN202110732161 A CN 202110732161A CN 113690040 A CN113690040 A CN 113690040A
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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
- H01F41/0266—Moulding; Pressing
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F7/00—Magnets
- H01F7/02—Permanent magnets [PM]
- H01F7/0205—Magnetic circuits with PM in general
- H01F7/021—Construction of PM
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Abstract
A radiation orientation nanocrystalline Co-based rare earth permanent magnet ring and a preparation method thereof belong to the technical field of functional materials. The alloy of the invention is RCo5‑xTMx(x is more than or equal to 0 and less than or equal to 0.3), R is one or more of rare earth elements such as Sm, Pr, La, Ce, Y and the like, TM is one or more of elements such as Ni, Fe, Mn, Cr, Al, Sn, Ga, Ti, Zn, Zr, Mo, Ag, Cu and the like, alloy ingot casting is prepared by vacuum melting → nanocrystalline/amorphous rapid quenching is prepared by melt rapid quenching → amorphous powder is prepared by high-energy ball milling → precursor is prepared by hot pressing → a permanent magnet ring with radial orientation is prepared by backward extrusion. The method can successfully prepare nanocrystalline Co-based rare earth permanent magnet rings with various sizes and wall thicknesses, and the prepared permanent magnet rings are high in magnetic performance and good in uniformity and can be widely applied to the field of permanent magnet high temperature.
Description
The technical field is as follows:
the invention relates to a radiation orientation nanocrystalline Co-based rare earth permanent magnet ring and a preparation method thereof, belonging to the technical field of functional magnetic materials.
Background art:
the radiation oriented rare earth permanent magnet ring is widely applied to electromechanical equipment such as motors, generators, servo motors, various direct current motors and the like. Although the Fe-based rare earth permanent magnet ring is applied to the electromechanical field and the preparation method is mature, the low Curie temperature of the Fe-based rare earth permanent magnet is not favorable for the application of the Fe-based rare earth permanent magnet in a high-temperature environment, and the Co-based rare earth permanent magnet has high coercive force, Curie temperature and high temperature stability and is suitable for the high-temperature field. In the high-temperature application fields of aerospace, military and the like, the working temperature of electromechanical equipment needs to be 180 ℃ or even higher, so that the Co-based rare earth permanent magnet ring needs to be developed urgently to meet the application requirement.
At present, the method for preparing the Co-based rare earth permanent magnet ring mainly comprises the following steps: bonding and sintering. The bonding method is to mix permanent magnetic powder and adhesive according to a certain proportion, then to solidify and mold to prepare the permanent magnetic ring, the process is simple, the cost is low, the processing property is good, the method can be used to prepare the permanent magnetic ring with complex shape, but the density is low, the isotropy is provided, the magnetic property is low, in addition, the use temperature is low under the influence of the adhesive, and the method can not be applied to the motor and the generator with larger power. The sintering method can be used for preparing anisotropic permanent magnet rings, and is characterized by utilizing the powder metallurgy technology to orient magnetic powder in a special magnetic field, and sintering, heat treatment and processing are carried out after the crystal grain orientation is consistent. Therefore, the preparation of the rare earth permanent magnet ring with high performance and no cracks is an urgent problem to be solved in the field of high-temperature permanent magnet. In the Fe-based rare earth permanent magnet, an anisotropic permanent magnet ring is prepared by a back extrusion method, and the nanocrystalline rare earth permanent magnet can obtain high performance while being highly compact by the back extrusion method through thermal deformation. However, compared with the preparation of the Fe-based rare earth permanent magnet ring, the preparation of the Co-based rare earth permanent magnet ring by a back extrusion method is difficult and heavy. Mainly because the interior of the Co-based rare earth permanent magnet does not have a rare earth-rich phase similar to NdFeB, and the rare earth-cobalt compound has lower crystal symmetry, less slip system and more difficult deformation.
The invention content is as follows:
the invention aims to overcome the problems and provides a radiation-oriented nanocrystalline Co-based rare earth permanent magnet ring and a preparation method thereof.
The invention relates to a radiation orientation nanocrystalline Co-based rare earth permanent magnet ring and a preparation method thereof, comprising the following steps:
(1) weighing each element according to the atomic ratio, and preparing into an alloy ingot in a vacuum induction intermediate frequency furnace; (2) preparing nanocrystalline/amorphous powder from the ingot by melt rapid quenching and/or high-energy ball milling in an inert gas atmosphere; (3) carrying out hot-pressing sintering on the nanocrystalline/amorphous powder under a vacuum environment to obtain a precursor; (4) and carrying out backward extrusion on the precursor in a vacuum environment to obtain the radially oriented permanent magnet ring.
The alloy in the step (1) of the invention is RCo5-xTMx(x is more than or equal to 0 and less than or equal to 0.3), R is one or more of rare earth elements such as Sm, Pr, La, Ce, Y and the like, and TM is one or more of elements such as Ni, Fe, Mn, Cr, Al, Sn, Ga, Ti, Zn, Zr, Mo, Ag, Cu and the like.
The alloy of step (1) of the present invention is according to the RCo5-xTMxAnd (4) preparing materials, wherein the actual R preparation amount is 1.05-1.15 times of the theoretical R consumption. The additional addition of rare earth components is a key factor in the success of the back-extrusion deformation described in the present invention.
The step (2) of the invention obtains the nanocrystalline/amorphous powder with uniform components by using one or two methods of melt rapid quenching and high-energy ball milling. The grain diameter of the nanocrystalline/amorphous powder is less than or equal to 150 microns.
In the step (3) of the invention, the hot-pressing sintering temperature is 500-700 ℃ and the pressure is 400-1000MPa in the hot-pressing sintering process.
In the step (4) of the invention, in the process of back extrusion, the extrusion temperature is 600-800 ℃, the pressure is 50-500MPa, the pressure head 5 moves downwards, and the lantern ring 6 moves upwards, so as to prepare the radial oriented permanent magnet ring.
The equipment adopted in the step (3): the center of the outer die is provided with an extrusion through hole which is communicated up and down, the diameter of the extrusion through hole is consistent with the diameter of the upper pressure head and the lower pressure head, magnetic powder to be hot-pressed is filled between the upper pressure head and the lower pressure head during hot pressing, the upper pressure head is pressed downwards, and a product obtained after pressing is a cylindrical precursor which is consistent with the diameters of the upper pressure head and the lower pressure head.
The equipment adopted in the step (4): an extrusion through hole which is communicated up and down is arranged in the center of the outer die, an upper opening of the extrusion outer die is coaxially matched with the upper pressure head and the lantern ring, and the lantern ring is sleeved on the periphery of the upper pressure head and can slide up and down along the axial direction; in the vertical axial direction, the sum of the size of the upper pressure head and the size of the lantern ring is equal to the diameter of the outer die; during extrusion, the upper pressure head during hot pressing can be directly replaced to perform backward extrusion, the upper pressure head is pressed downwards, under the action of temperature and pressure, a part of precursor is molded upwards along the lantern ring to obtain the annular magnet, and the thickness of the annular magnet in the vertical axial direction after pressing is equal to the thickness of the lantern ring. And finally, the precursor becomes thin, and the height of the annular magnet becomes large.
The die for hot pressing and back extrusion comprises a hot pressing upper pressure head 1, an outer die 2, a lower pressure head 4, an extrusion upper pressure head 5 and a lantern ring 6; the outer die 2 and the lantern ring 6 are hollow cylinders, the inner diameter of the outer die 2 is equal to the outer diameter of the permanent magnet ring, and the wall thickness of the lantern ring is equal to the wall thickness of the permanent magnet ring.
The back extrusion can be directly carried out after the upper pressure head is replaced when the hot pressing is finished.
In the process of die filling, the inner part of an outer die, the outer parts of an upper pressure head and a lower pressure head and the contact surface with a sample are sprayed with lubricant so as to facilitate die releasing.
The invention has the beneficial effects that:
(1) the radiation orientation nanocrystalline Co-based rare earth permanent magnet ring is successfully prepared by a back extrusion method, and the prepared permanent magnet ring has high performance and good consistency.
(2) The precursor obtained by hot pressing can be directly extruded in a back direction only by replacing the upper pressure head, so that stress concentration in the demolding process is avoided, the yield is improved, the process time is reduced, and the production efficiency is improved.
Description of the drawings:
FIG. 1 (a) is a view showing a structure of a mold at the start of hot pressing, and (b) is a view showing a structure of a mold at the end of hot pressing.
FIG. 2 shows a view of a die structure at the start of extrusion, and FIG. 2 shows a view of a die structure at the end of extrusion.
FIG. 3 is a topographic map of a radiation-oriented Co-based rare earth permanent magnet ring.
Reference numerals
1 hot-pressing upper pressure head 2 outer die 3 magnetic powder 4 lower pressure head 5 extruding upper pressure head 6 lantern ring 7 extruding precursor
The specific implementation mode is as follows:
the invention will be further described with reference to the drawings and the embodiments without limiting the scope of the invention thereto.
Example 1
(1) The alloy of example 1 is SmCo5The actual Sm amount is 1.1 times of the theoretical Sm consumption, and alloy cast ingots are prepared by vacuum melting;
(2) preparing the alloy ingot into a nanocrystalline/amorphous rapid quenching belt through melt rapid quenching;
(3) grinding the quick quenching belt into powder with the particle size less than or equal to 150 microns;
(4) in the hot pressing process, the hot pressing temperature is 650 ℃ and the pressure is 500 MPa;
(5) in the back extrusion process, the extrusion temperature is 700 ℃, the pressure is 500MPa, the pressure head 5 moves downwards, the lantern ring 6 moves upwards, and the radial orientation permanent magnet ring with the wall thickness of 3mm is prepared.
Example 2
(1) The alloy of example 2 is (Sm)0.6Pr0.4)Co5Actually prepared rare earth amount is 1.1 times of theoretical rare earth consumption, and alloy cast ingots are prepared by vacuum melting;
(2) preparing the alloy ingot into nanocrystalline/amorphous powder by melt rapid quenching auxiliary high-energy ball milling;
(3) the grain size of the powder is less than or equal to 150 microns;
(4) in the hot pressing process, the hot pressing temperature is 650 ℃ and the pressure is 500 MPa;
(5) in the back extrusion process, the extrusion temperature is 750 ℃, the pressure is 100MPa, the pressure head 5 moves downwards, the lantern ring 6 moves upwards, and the radial orientation permanent magnet ring with the wall thickness of 4mm is prepared.
Example 3
(1) The alloy of example 1 is SmCo4.82Zr0.18Actually prepared Sm amount is 1.1 times of theoretical Sm consumption, and alloy cast ingots are prepared by vacuum melting;
(2) preparing the alloy ingot into a nanocrystalline/amorphous rapid quenching belt through melt rapid quenching;
(3) grinding the quick quenching belt into powder with the particle size less than or equal to 150 microns;
(4) in the hot pressing process, the hot pressing temperature is 650 ℃ and the pressure is 500 MPa;
(5) in the back extrusion process, the extrusion temperature is 800 ℃, the pressure is 50MPa, the pressure head 5 moves downwards, the lantern ring 6 moves upwards, and the radial orientation permanent magnet ring with the wall thickness of 5mm is prepared.
And (3) magnetic property testing:
the magnetic performance data of 3 samples of the back-extruded permanent magnet ring obtained in example 1, taken along the circumference of the magnet ring, are shown in table 1 below.
TABLE 1
| Remanence (kG) | Coercive force (kOe) | Maximum magnetic energy product (MGOe) | |
| Position 1 | 7.82 | 35.17 | 13.17 |
| |
7.89 | 35.28 | 13.39 |
| |
7.93 | 34.6 | 13.64 |
As can be seen from table 1, the magnetic rings have uniform magnetic properties (remanence difference < 2%, coercivity difference < 2%, magnetic energy product difference < 4%) around the circumference, indicating that the back-pressed permanent magnetic rings prepared in example 1 have good uniformity.
The magnetic properties of the back-pressed permanent magnet rings prepared in examples 1 to 3 were measured and the data are shown in Table 2.
TABLE 2
| Remanence (kG) | Coercive force (kOe) | Maximum magnetic energy product (MGOe) | |
| Example 1 | 7.93 | 34.6 | 13.64 |
| Example 2 | 8.01 | 25.4 | 10.55 |
| Example 3 | 7.73 | 27.8 | 9.97 |
Claims (9)
1. A radiation orientation nanocrystalline Co-based rare earth permanent magnet ring and a preparation method thereof are characterized by comprising the following steps:
(1) weighing each element according to the atomic ratio, and preparing into an alloy ingot in a vacuum induction intermediate frequency furnace; (2) preparing nanocrystalline/amorphous powder from the ingot by melt rapid quenching and/or high-energy ball milling in an inert gas atmosphere; (3) carrying out hot-pressing sintering on the nanocrystalline/amorphous powder in a vacuum environment to obtain a precursor; (4) and carrying out backward extrusion on the precursor in a vacuum environment to obtain the radially oriented permanent magnet ring.
2. The radiation-oriented nanocrystalline Co-based rare earth permanent magnet ring and the preparation method thereof according to claim 1, wherein the alloy in the step (1) is RCo5-xTMx(x is more than or equal to 0 and less than or equal to 0.3), R is one or more of rare earth elements such as Sm, Pr, La, Ce, Y and the like, and TM is one or more of elements such as Ni, Fe, Mn, Cr, Al, Sn, Ga, Ti, Zn, Zr, Mo, Ag, Cu and the like.
3. The radiation-oriented nanocrystalline Co-based rare earth permanent magnet ring and the preparation method thereof according to claims 1 and 2, wherein according to RCo5-xTMxAnd (4) preparing materials, wherein the actual R preparation amount is 1.05-1.15 times of the theoretical R consumption. The additional addition of rare earth components is a key factor in the success of the back-extrusion deformation described in the present invention.
4. The radiation-oriented nanocrystalline Co-based rare earth permanent magnet ring and the preparation method thereof according to claim 1, wherein the nanocrystalline/amorphous powder with uniform components is obtained in the step (2) by using one or two methods of melt rapid quenching and high-energy ball milling; the grain diameter of the nanocrystalline/amorphous powder is less than or equal to 150 microns.
5. The radiation orientation nanocrystalline Co-based rare earth permanent magnet ring and the preparation method thereof as claimed in claim 1, wherein the hot-pressing sintering temperature in the step (3) is 500-700 ℃ and the pressure is 400-1000MPa in the hot-pressing sintering process.
6. The radiation orientation nanocrystalline Co-based rare earth permanent magnet ring and the preparation method thereof as claimed in claim 1, wherein in the step (4) in the process of back extrusion, the extrusion temperature is 600-800 ℃, the pressure is 50-500MPa, the pressure head 5 moves downwards, and the lantern ring 6 moves upwards to prepare the radial orientation permanent magnet ring.
7. The radiation-oriented nanocrystalline Co-based rare earth permanent magnet ring and the preparation method thereof according to claim 1, characterized in that the equipment adopted in the step (3): the center of the outer die is provided with an extrusion through hole which is communicated up and down, the diameter of the extrusion through hole is consistent with the diameters of the upper pressure head and the lower pressure head, magnetic powder to be hot-pressed is filled between the upper pressure head and the lower pressure head during hot pressing, the hot pressure head is pressed downwards, and a product obtained after pressing is a cylindrical precursor with the diameters consistent with the diameters of the upper pressure head and the lower pressure head;
the equipment adopted in the step (4): an extrusion through hole which is communicated up and down is arranged in the center of the outer die, an upper opening of the extrusion outer die is coaxially matched with the upper pressure head and the lantern ring, and the lantern ring is sleeved on the periphery of the upper pressure head and can slide up and down along the axial direction; in the vertical axial direction, the sum of the size of the upper pressure head and the size of the lantern ring is equal to the diameter of the outer die; during extrusion, the upper pressure head during hot pressing can be directly replaced to perform backward extrusion, the upper pressure head is pressed downwards, under the action of temperature and pressure, a part of precursor is molded upwards along the lantern ring to obtain the annular magnet, and the thickness of the annular magnet in the vertical axial direction after pressing is equal to the thickness of the lantern ring. And finally, the precursor becomes thin, and the height of the annular magnet becomes large.
8. The radially oriented nanocrystalline Co-based rare earth permanent magnet ring and the preparation method thereof according to claim 1, wherein during the die filling process, lubricants are sprayed on the inner part of the outer die, the outer parts of the upper and lower pressing heads and the contact surface with the sample so as to release the die.
9. The radiation-oriented nanocrystalline Co-based rare earth permanent magnet ring prepared according to the method of any one of claims 1 to 8.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101476055A (en) * | 2009-01-16 | 2009-07-08 | 北京工业大学 | Preparation of fully dense massive anisotropic nanocrystalline SmCo5 magnet |
| CN106887293A (en) * | 2017-03-10 | 2017-06-23 | 钢铁研究总院 | A kind of high performance radial is orientated rare earth permanent magnet pipe and its thermoforming method |
| CN111009408A (en) * | 2019-12-31 | 2020-04-14 | 安泰科技股份有限公司 | Method for preparing rare earth permanent magnetic ring by adopting hot pressing-thermal deformation process and special die |
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- 2021-06-29 CN CN202110732161.XA patent/CN113690040A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101476055A (en) * | 2009-01-16 | 2009-07-08 | 北京工业大学 | Preparation of fully dense massive anisotropic nanocrystalline SmCo5 magnet |
| CN106887293A (en) * | 2017-03-10 | 2017-06-23 | 钢铁研究总院 | A kind of high performance radial is orientated rare earth permanent magnet pipe and its thermoforming method |
| CN111009408A (en) * | 2019-12-31 | 2020-04-14 | 安泰科技股份有限公司 | Method for preparing rare earth permanent magnetic ring by adopting hot pressing-thermal deformation process and special die |
Non-Patent Citations (1)
| Title |
|---|
| XIAOCHANG XU ET AL.: ""Sm2Co7 nanophase inducing low-temperature hot deformation to fabricate high performance SmCo5 magnet"", 《SCRIPTA MATERIALIA》, pages 1 - 5 * |
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