CN103123862A - Method for improving performance of thermal compression or thermal deformation radiation orientation neodymium iron boron permanent magnet ring and axial uniformity thereof - Google Patents

Method for improving performance of thermal compression or thermal deformation radiation orientation neodymium iron boron permanent magnet ring and axial uniformity thereof Download PDF

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CN103123862A
CN103123862A CN201110371635.9A CN201110371635A CN103123862A CN 103123862 A CN103123862 A CN 103123862A CN 201110371635 A CN201110371635 A CN 201110371635A CN 103123862 A CN103123862 A CN 103123862A
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magnet ring
magnetic
magnet
predeformation
thermal deformation
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CN103123862B (en
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唐旭
陈仁杰
尹文宗
林旻
李东
闫阿儒
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Ningbo Institute of Material Technology and Engineering of CAS
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Abstract

The invention relates to a method for improving the performance of thermal compression or thermal deformation radiation orientation neodymium iron boron permanent magnet ring and the axial uniformity of the thermal compression or thermal deformation radiation orientation neodymium iron boron permanent magnet ring. The method for improving the performance of the thermal compression or thermal deformation radiation orientation neodymium iron boron permanent magnet ring comprises the following steps: (1) conducting thermal compression on rapid quenching magnetic powder which has a nanocrystalline structure or high density digital recording (HDDR) magnetic powder in a vacuum inductive thermal compressor to form an isotropous magnetic body by utilization of a thermal compression technology; (2) conducting thermal deformation on the isotropous magnetic body through cutting or replacement of a series of molds with different internal diameters to obtain an anisotropy magnetic body with different predeformation amounts; and (3) preparing the above predeformation anisotropyv magnetic body through a back extrusion technology to form a radiation orientation permanent magnet ring; by means of the predeformation technology, blank of the prepared radiation orientation magnet ring is enabled to have a certain degree of orientation and texture. In the process of preparation of the radiation orientation ring, the radiation orientation is benefited to be formed, thus under the condition that coercive force is not significantly reduced, the performance and the uniformity of the radiation orientation magnet ring are improved, the ratio of briquetting of the magnet ring can be greatly improved in the process of preparation of the magnet ring, energy consumption is reduced, and cost is saved.

Description

Improve hot pressing/thermal deformation radially oriented Nd-Fe-B permanent magnetic ring performance and axial inhomogeneity method thereof
Technical field
The present invention relates to the rare earth permanent-magnetic material field, be specifically related to a kind of predeformation technique of utilizing and improve hot pressing/thermal deformation radially oriented Nd-Fe-B permanent magnetic ring performance and axial inhomogeneity method thereof.
Background technology
Radially oriented magnetic Nd-Fe-B ring has obtained application on motor, such as voice coil motor, and brushless electric machine etc.These magnets mainly obtain by dual mode at present, and a kind of is traditional powder metallurgic method, and another is exactly hot-extrudable method.
Due to single-phase RE permanent magnetic material good plastic deformation ability at high temperature, therefore prepare flawless, the nanocrystalline radially oriented ring of high radially oriented degree just becomes the important application direction of nanocrystalline rare-earth permanent magnetic material.The radially oriented ring of sintering permanent magnet has obtained application in motor, these sintered magnet major parts are all to be attached to above motor with magnetic shoe or laminated structure.Although the whole magnet ring of sintering can prepare and be applied, due to sintering magnet ring preparation technology's restriction itself, therefore be difficult to prepare high length-diameter ratio, the sintering magnet ring of thin-walled.The radial oriented anisotropy magnet ring of back of the body expressing technique preparation can be prepared the magnet ring of complete high length-diameter ratio owing to having less wall thickness, therefore can reduce the volume and weight of motor.Because the magnet ring for preparing is an integral body, therefore stable and uniform magnetic field not only can be provided, and can reduce the preparation time in the motor preparation process, be compared to the sintering magnet ring, have very significantly advantage.
In hot-extrudable process, magnet ring has produced strong radially texture, and the c-axis direction of flake crystalline is along the radial direction of magnet ring, perpendicular to pressure direction.Anisotropy than the sintering magnet ring is compared, and very significantly advantage is arranged.Yet due to back of the body expressing technique itself, the magnet ring for preparing has very strong inhomogeneities.Often kept the character of isotropism blank at the top of magnet ring, had high-coercive force, the character of low remanent magnetism.Along with the position moves down, gradually strong of texture, the final microstructure with good degree of orientation that forms in the bottom.
No matter utilize the magnetic of HDDR method or quick quenching technique preparation to prepare radially oriented nanocrystalline permanent-magnetic clamp, in the performance of acquisition, magnet ring top and bottom have very large performance difference.But there is work to show, utilizes nanocrystalline magnetic to prepare flawless radially oriented ring and have feasibility.The inhomogeneities of magnet ring not only shows the inconsistent of up and down, also shows inside and outside inhomogeneous of ring.The people such as W.Grtinberger study discovery, by the mode of polishing, from the outer surface fritter that downcuts of attenuate magnet ring gradually, and the magnetic property of test different-thickness, find that remanent magnetization brought up to 1.3T from 1.24T.Therefore in order to solve the problem of magnet ring inhomogeneities, researchers have carried out very large effort.The people such as H.T.Kim utilize CAPA (current applied pressure-assisted process) technique, and expectation changes the inhomogeneities of magnet ring by changing heating means.In this research work, the magnetic property at magnet ring top has still kept the isotropism of hot-pressed magnets, along with the position moves down, has engendered strong texture, but because the position near the bottom is in high temperature for a long time, abnormal grain growth.The staff such as D.Hinz utilize the isotropism magnet ring, and the mode that adopts the heat back of the body to extrude prepares the radially oriented magnet ring of having prepared thin-walled, and having obtained very excellent magnetic property is the Nanocrystalline core of 30mm with the height that has good uniformity.
We know, in heat distortion magnet, the formation of texture is but to be easy to very much.Therefore, adding the middle process of a predeformation, the blank that makes the back of the body extrude in extrusion at hot pressing and the back of the body is no longer the hot pressing blank of isotropic but anisotropic thermal deformation blank.Reach thus the purpose that improves magnet ring uniformity and magnet ring performance.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of raising hot pressing/thermal deformation radially oriented Nd-Fe-B permanent magnetic ring magnetic property and inhomogeneity method, by add the middle process of a predeformation in hot pressing and back of the body extrusion, when improving the magnet ring performance, improve the uniformity of magnet ring from the top to the bottom.
The present invention solves the problems of the technologies described above the technical scheme that adopts: a kind of raising hot pressing/thermal deformation radially oriented Nd-Fe-B permanent magnetic ring magnetic property and inhomogeneity method is characterized in that comprising the following steps:
1) hot pressing: nanocrystalline magnetic is put into hot pressing die, hot pressing die is put into the vacuum induction hot press carry out hot pressing, in hot pressing, vacuum degree is higher than 9 * 10 -2Pa, hot pressing temperature is at 500-850 ℃, room temperature to the highest temperature intensification time be 5-10 minute, be incubated 1-3 minute, then cooled to room temperature in 20-30 minute, the demoulding obtains isotropic magnet;
2) predeformation: isotropic magnet that will make is cut into suitable diameter by line, put into the thermal deformation mould thermal deformation of different inner diameters, control heat distortion temperature at 500-850 ℃, room temperature to the highest temperature intensification time be 5-10 minute, be incubated 0.5-5 minute, then open hydraulic system, slowly exert pressure, magnet at the uniform velocity is out of shape, and the deformation time is controlled at 30-90 second, is incubated 10-30 second after predeformation is completed.Then cooled to room temperature in 20-30 minute, the demoulding obtains the anisotropic nanocrystalline magnet of different distortion amount;
3) back of the body is extruded: at last above-mentioned anisotropic nanocrystalline magnet through predeformation is prepared into radially oriented permanent-magnetic clamp by back of the body expressing technique.
As preferably, described nanocrystalline magnetic is a kind of in rapidly quenched magnetic powder or HDDR magnetic.
As improvement, described step 1) in hot pressing, vacuum degree is higher than 9 * 10 -2Pa.
Improve again described step 2) the predeformation deformation quantity between 20%-80%, in the predeformation process, be evacuated down in advance 4 * 10 -2Pa-8 * 10 -2Pa, after pour Ar to 1-1.2 * 10 2Pa is as the anti-oxidation of protection gas and as heat-conduction medium.
Further improve, described step 3) process that back of the body expressing technique prepares radially oriented permanent-magnetic clamp is: with step 2) the anisotropic nanocrystalline magnet that makes puts into magnet ring and prepares mould, control temperature at 700-850 ℃, room temperature to the highest temperature intensification time be 5-10 minute, be incubated and open hydraulic system after 0.5-5 minute, slowly exert pressure, magnet is at the uniform velocity carried on the back to be extruded, the preparation magnet ring time is 1-3 minute, be incubated 10-30 second after preparation is completed, then cooled to room temperature in 20-30 minute.Pressure 100-500Mpa, preferred 100-200Mpa.
In the process of preparation magnet ring at last, described step 3), be evacuated down in advance 4 * 10 -2Pa-8 * 10 -2Pa, after pour Ar to 1 * 10 2Pa-1.2 * 10 2Pa is as the anti-oxidation of protection gas.
Compared with prior art, the invention has the advantages that: by thermal deformation technique in advance, making the blank of preparation radially oriented magnetic ring is anisotropic thermal deformation blank, has to a certain degree the degree of orientation and texture.In the process of the radially oriented ring of preparation, be conducive to radially oriented formation, thereby significantly do not reducing in coercitive situation, improve performance and the uniformity of radially oriented magnetic ring.By method of the present invention, can improve greatly the ratio of briquetting of magnet ring in preparation magnet ring process, reduce the wastage, save cost, the application for preparing radially oriented Nd-Fe-B permanent magnetic ring for hot pressing/thermal deformation is laid a solid foundation.
Description of drawings
Fig. 1 is the magnet ring magnetic property of diverse location from top to bottom of predeformation 57%.
Embodiment
Embodiment is described in further detail the present invention below in conjunction with accompanying drawing.
Embodiment 1
Adopt business to put into MQU-F rapidly quenched magnetic powder 17g the hot pressing die that internal diameter is 13mm.
Hot pressing die is put into the vacuum induction hot press, and be evacuated down to 6 * 10 -2Below Pa.
Treat that vacuum degree reaches 6 * 10 -2During Pa, open heating system, open simultaneously hydraulic system, the pressure that acts on mould is adjusted to 200MPa, and at the uniform velocity be warmed up to 670 ℃ from room temperature, the heating-up time was 5 minutes, 670 ℃ of heat-insulation pressure keepings 1 minute.
After heat-insulation pressure keeping is completed, close rapidly heating system and hydraulic system, pressure is transferred to minimum, and cool to room temperature in 30 minutes, the demoulding after mould is taken out.
The above-mentioned hot-pressed magnets of preparing is put into the mould that internal diameter is 19.5mm and mould is put into the vacuum induction hot press, be evacuated down to 6 * 10 -2Below Pa.
When vacuum degree reaches 6 * 10 -2After Pa is following, pour Ar to 1 * 10 2Pa is as protective gas and heat-conduction medium.
Open heating system, at the uniform velocity be warmed up to 800 ℃ from room temperature, the heating-up time is 6 minutes, after temperature reaches 800 ℃, is incubated 1 minute.
After insulation is completed, open hydraulic system, slowly exert pressure, magnet at the uniform velocity is out of shape, and the deformation time is controlled at 60 seconds, after thermal deformation is completed, slowly pressure is adjusted to 5MPa,, and kept 20 seconds at 168MPa with the pressure that guarantees to put on mould, obtain predeformation amount and be 57% anisotropic magnet.
Close rapidly hydraulic system and heating system after thermal deformation is completed, and pressure be transferred to minimum, reduced the temperature to room temperature in 30 minutes after the demoulding.
The magnet ring of magnet after the demoulding being put into internal diameter 19mm prepares mould, and the contact position in mould evenly applies release agent MoS 2
Mould is put into the vacuum induction hot press, and be evacuated down to 6 * 10 -2Pa pours argon gas to 1 * 10 2Pa is as protective gas.
Open heating system, at the uniform velocity be warmed up to 800 ℃ from room temperature, the heating-up time is 6 minutes, after temperature reaches 800 ℃, is incubated 1 minute.
After insulation is completed, opening hydraulic system, slowly exert pressure, magnet is at the uniform velocity carried on the back extruded, is 2 minutes from beginning to apply pressure to last magnet ring molding time, and pressure is adjusted to 5MPa the most at last,, and keeps 20 seconds at 168MPa with the pressure that guarantees to put on mould.
The back of the body is extruded and is closed rapidly hydraulic system and heating system after completing, and pressure is transferred to minimum, reduced the temperature to room temperature in 30 minutes after the demoulding, the magnet ring height that obtains is 13mm.Radially cut from top to bottom little square column from magnet ring, utilize vibrating specimen magnetometer that little square column is measured.
The Performance Ratio of the radially oriented magnetic Nd-Fe-B ring of table 1 employing different process preparation
Figure BDA0000110596350000051
Embodiment 2
Adopt business to put into MQU-F rapidly quenched magnetic powder 27g the hot pressing die that internal diameter is 19mm.
Hot pressing die is put into the vacuum induction hot press, and be evacuated down to 6 * 10 -2Below Pa.
Treat that vacuum degree reaches 6 * 10 -2During Pa, open heating system, open simultaneously hydraulic system, the pressure that acts on mould is adjusted to 200MPa, and at the uniform velocity be warmed up to 670 ℃ from room temperature, the heating-up time was 5 minutes, 670 ℃ of heat-insulation pressure keepings 1 minute.
After heat-insulation pressure keeping is completed, close rapidly heating system and hydraulic system, pressure is transferred to minimum, and cool to room temperature in 30 minutes, the demoulding after mould is taken out.
The above-mentioned hot-pressed magnets line of preparing is cut into the hot-pressed magnets of 15.5mm, puts into the mould that internal diameter is 19.5mm and mould is put into the vacuum induction hot press, be evacuated down to 6 * 10 -2Below Pa.
When vacuum degree reaches 6 * 10 -2After Pa is following, pour Ar to 1 * 10 2Pa is as protective gas and heat-conduction medium.
Open heating system, at the uniform velocity be warmed up to 800 ℃ from room temperature, the heating-up time is 6 minutes, after temperature reaches 800 ℃, is incubated 1 minute.
After insulation is completed, open hydraulic system, slowly exert pressure, magnet at the uniform velocity is out of shape, and the deformation time is controlled at 60 seconds, after thermal deformation is completed, slowly pressure is adjusted to 5MPa,, and kept 20 seconds at 168MPa with the pressure that guarantees to put on mould, can obtain thus deflection and be 40% anisotropic magnet.
Close rapidly hydraulic system and heating system after thermal deformation is completed, and pressure be transferred to minimum, reduced the temperature to room temperature in 30 minutes after the demoulding.
The magnet ring of magnet after the demoulding being put into internal diameter 19mm prepares mould, and the contact position in mould evenly applies release agent MoS 2
Mould is put into the vacuum induction hot press, and be evacuated down to 6 * 10 -2Pa.
Open heating system, at the uniform velocity be warmed up to 800 ℃ from room temperature, the heating-up time is 6 minutes, after temperature reaches 800 ℃, is incubated 1 minute.
After insulation is completed, opening hydraulic system, slowly exert pressure, magnet is at the uniform velocity carried on the back extruded, is 2 minutes from beginning to apply pressure to last magnet ring molding time, and pressure is adjusted to 5MPa the most at last,, and keeps 20 seconds at 168MPa with the pressure that guarantees to put on mould.
The back of the body is extruded and is closed rapidly hydraulic system and heating system after completing, and pressure is transferred to minimum, reduced the temperature to room temperature in 30 minutes after the demoulding, the magnet ring height 13mm that obtains.Radially cut from top to bottom little square column from magnet ring, utilize vibrating specimen magnetometer that little square column is measured.
The Performance Ratio of the radially oriented magnetic Nd-Fe-B ring of table 2 employing different process preparation
Figure BDA0000110596350000061
Embodiment 1 and the embodiment 2 middle magnetic rings radially oriented permanent-magnetic clamp that recycling back of the body expressing technique is made after process predeformation PROCESS FOR TREATMENT axially has obvious uniformity improvement from the middle part of magnet ring.By the method, can improve greatly the ratio of briquetting of magnet ring in preparation magnet ring process, reduce the wastage, save cost, the application for preparing radially oriented Nd-Fe-B permanent magnetic ring for hot pressing/thermal deformation is laid a solid foundation.
Specific embodiment described herein is only the present invention to be done illustrate.Those skilled in the art can make various modifications or adopt similar mode to substitute described concrete case study on implementation, but can not depart from the defined scope of appended claims of the present invention.

Claims (6)

1. one kind is improved hot pressing/thermal deformation radially oriented Nd-Fe-B permanent magnetic ring magnetic property and inhomogeneity method, it is characterized in that comprising the following steps:
1) hot pressing: nanocrystalline magnetic is put into hot pressing die, hot pressing die is put into the vacuum induction hot press carry out hot pressing, hot pressing temperature is at 500-850 ℃, heating-up time was at 5~10 minutes, pressure 100-500MPa, compacting temperature retention time 1-3 minute obtains isotropic magnet;
2) predeformation: isotropic magnet that will make, put into the thermal deformation mould thermal deformation of different inner diameters, control heat distortion temperature at 500-850 ℃, heating-up time is 5~10 minutes, pressure 100-500MPa, compacting temperature retention time 1-3 minute, the anisotropic nanocrystalline magnet of acquisition different distortion amount;
3) hot-extrudable: as at last above-mentioned anisotropic nanocrystalline magnet through predeformation to be prepared into radially oriented permanent-magnetic clamp by hot-extrudable technique.
2. method according to claim 1 is characterized in that described nanocrystalline magnetic is a kind of in rapidly quenched magnetic powder or HDDR magnetic.
3. method according to claim 1, is characterized in that described step 1) hot pressing in, vacuum degree is higher than 9 * 10 -2Pa.
4. method according to claim 1, is characterized in that described step 2) the predeformation deformation quantity between 20%-80%, in the predeformation process, be evacuated down to 4 * 10 -2Pa-8 * 10 -2Below Pa, or pour Ar after vacuumizing to 1-1.2 * 10 2Pa, predeformation is 0.5-2 minute from being pressurized to the compacting deadline.
5. method according to claim 1, it is characterized in that described step 3) the hot-extrudable technique process for preparing radially oriented permanent-magnetic clamp be: with step 2) the anisotropic nanocrystalline magnet that makes puts into magnet ring and prepares mould, control temperature at 700-850 ℃, room temperature to the highest temperature intensification time be 5-10 minute, be incubated and open hydraulic system after 0.5-5 minute, slowly exert pressure, magnet is at the uniform velocity carried on the back to be extruded, the preparation magnet ring time is 2-3 minute, be incubated 10-30 second after preparation is completed, then cooled to room temperature in 20-30 minute.
6. method according to claim 5, is characterized in that described step 3) the process of preparation magnet ring in, be evacuated down to 4 * 10 -2Pa-8 * 10 -2Below Pa, or pour Ar after vacuumizing to 1-1.2 * 10 2Pa.
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CN103426623A (en) * 2013-08-05 2013-12-04 四川大学 Method for preparing anisotropy nano-crystalline neodymium-iron-boron magnet
CN104051104A (en) * 2014-06-06 2014-09-17 中国科学院宁波材料技术与工程研究所 NdFeB permanent magnet and preparation method thereof
CN104134529A (en) * 2014-07-21 2014-11-05 华南理工大学 Anisotropic nanocrystal neodymium iron boron magnet, and preparation method and application of magnet
CN104599802A (en) * 2014-12-03 2015-05-06 中国科学院宁波材料技术与工程研究所 Rare earth permanent magnetic material and preparation method thereof
CN106964778A (en) * 2016-01-14 2017-07-21 罗伯特·博世有限公司 The method and apparatus for producing heat distortion magnet
CN107546025A (en) * 2017-07-10 2018-01-05 北京工业大学 A kind of preparation method of shearing force thermal deformation mould and neodymium iron boron magnetic body
CN107578871A (en) * 2017-09-26 2018-01-12 浙江东阳东磁稀土有限公司 A kind of preparation method of the radially oriented magnetic shoe of high-performance
CN108428541A (en) * 2017-02-14 2018-08-21 中国科学院宁波材料技术与工程研究所 A kind of preparation method of Ultra-fine Grained high-performance anisotropy Nd-Fe-B permanent magnet
CN108615596A (en) * 2016-12-12 2018-10-02 中国科学院宁波材料技术与工程研究所 A kind of abnormity permanent magnet and preparation method thereof, the equipment for preparing special-shaped permanent magnet
CN108666127A (en) * 2018-06-04 2018-10-16 安徽天宇磁业股份有限公司 Based on energy-saving and environment-friendly permanent magnet processing technology
CN109166720A (en) * 2018-08-22 2019-01-08 浙江东阳东磁稀土有限公司 A kind of method of continous way production hot extrusion radiation ring
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
CN113620701A (en) * 2021-09-29 2021-11-09 海安南京大学高新技术研究院 Preparation method of superfine-crystal high-temperature-resistant high-frequency manganese-zinc ferrite
CN114974866A (en) * 2022-05-09 2022-08-30 大连理工大学 Integrated forming die for hot-pressing-hot-deformation rare earth permanent magnet ring and preparation method thereof

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CN103426623B (en) * 2013-08-05 2015-12-02 四川大学 A kind of preparation method of anisotropy nano-crystalline neodymium-iron-boronmagnet magnet
CN103426623A (en) * 2013-08-05 2013-12-04 四川大学 Method for preparing anisotropy nano-crystalline neodymium-iron-boron magnet
CN104051104A (en) * 2014-06-06 2014-09-17 中国科学院宁波材料技术与工程研究所 NdFeB permanent magnet and preparation method thereof
CN104051104B (en) * 2014-06-06 2017-06-23 中国科学院宁波材料技术与工程研究所 Nd-Fe-B permanent magnetic magnet and preparation method thereof
CN104134529A (en) * 2014-07-21 2014-11-05 华南理工大学 Anisotropic nanocrystal neodymium iron boron magnet, and preparation method and application of magnet
CN104134529B (en) * 2014-07-21 2016-08-17 华南理工大学 A kind of anisotropy nano-crystalline neodymium-iron-boronmagnet magnet and preparation method and application
CN104599802A (en) * 2014-12-03 2015-05-06 中国科学院宁波材料技术与工程研究所 Rare earth permanent magnetic material and preparation method thereof
CN106964778A (en) * 2016-01-14 2017-07-21 罗伯特·博世有限公司 The method and apparatus for producing heat distortion magnet
CN108615596A (en) * 2016-12-12 2018-10-02 中国科学院宁波材料技术与工程研究所 A kind of abnormity permanent magnet and preparation method thereof, the equipment for preparing special-shaped permanent magnet
CN108428541A (en) * 2017-02-14 2018-08-21 中国科学院宁波材料技术与工程研究所 A kind of preparation method of Ultra-fine Grained high-performance anisotropy Nd-Fe-B permanent magnet
CN107546025A (en) * 2017-07-10 2018-01-05 北京工业大学 A kind of preparation method of shearing force thermal deformation mould and neodymium iron boron magnetic body
CN107578871A (en) * 2017-09-26 2018-01-12 浙江东阳东磁稀土有限公司 A kind of preparation method of the radially oriented magnetic shoe of high-performance
CN108666127A (en) * 2018-06-04 2018-10-16 安徽天宇磁业股份有限公司 Based on energy-saving and environment-friendly permanent magnet processing technology
CN109166720A (en) * 2018-08-22 2019-01-08 浙江东阳东磁稀土有限公司 A kind of method of continous way production hot extrusion radiation ring
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
CN113620701A (en) * 2021-09-29 2021-11-09 海安南京大学高新技术研究院 Preparation method of superfine-crystal high-temperature-resistant high-frequency manganese-zinc ferrite
CN114974866A (en) * 2022-05-09 2022-08-30 大连理工大学 Integrated forming die for hot-pressing-hot-deformation rare earth permanent magnet ring and preparation method thereof

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