CN101476055A - Preparation of fully dense massive anisotropic nanocrystalline SmCo5 magnet - Google Patents
Preparation of fully dense massive anisotropic nanocrystalline SmCo5 magnet Download PDFInfo
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- CN101476055A CN101476055A CNA2009100770091A CN200910077009A CN101476055A CN 101476055 A CN101476055 A CN 101476055A CN A2009100770091 A CNA2009100770091 A CN A2009100770091A CN 200910077009 A CN200910077009 A CN 200910077009A CN 101476055 A CN101476055 A CN 101476055A
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Abstract
The invention pertaining to the field of preparing magnetic materials provides a method of preparing full-compact block body eolotropy nanocrystalline SmCo5 magnet for solving the problems that by the conventional sinter method of preparing SmCo5 permanent magnet alloy, the technique is complex, the mechanical performances and corrosion resistance capability of the produced alloy is not good, and the like.The method comprises steps of preparing key metal for smelting by using Sm and Co according to the mixture ratio of the components of SmCo5, performing the ball mill process to obtain amorphous alloy powder, performing quick hot pressing and heat distortion processes to the amorphous alloy powder sequentially, finally obtaining the ull-compact block body eolotropy nanocrystalline SmCo5 permanent magnet alloy. The method has advantages of simple technique, short production cycle and low cost, and the produced magnet has high degree of compactness, fine grains, a SmCo5 phase C axes crystal texture and high magnetic property.
Description
Technical field
The invention belongs to the magneticsubstance preparation field, be specifically related to the nanocrystalline SmCo of a kind of full compact block anisotropy
5The preparation method of magnet.
Background technology
SmCo
5Permanent magnet alloy is the first-generation RE permanent magnetic alloy of developing the sixties in last century, not only has excellent intrinsic magnetic properties, and has the good high-temperature characteristic, and promptly alloy still can keep higher magnetic property under hot environment.Therefore, this class permanent magnet material still has good practical values so far, to being used widely under the higher environment of temperature requirement.
At present, generally adopt traditional powder metallurgy process to prepare SmCo at industrial quilt
5Permanent magnet alloy comprises following process substantially: alloy melting → broken powder process → magnetic field orientating compacting → sintering → thermal treatment → machine-shaping.Adopt the SmCo of this method preparation
5Permanent magnet alloy has higher magnetic property, but has following deficiency: at first, the grain-size of prepared alloy is a micro-meter scale, so the mechanical property of alloy is relative with erosion resistance relatively poor, has limited the range of application of alloy to a certain extent; Secondly, problem such as there is complex procedures in prior powder metallurgy technology, the production cycle is long and homogeneity of product is relatively poor, thereby make the manufacturing cost of alloy high.Therefore, explore preparation high-performance SmCo
5The novel method of permanent magnet alloy is significant.
In order to make SmCo
5Permanent magnet alloy obtains high magnetic property, must adopt effective means to make alloy obtain magneticanisotropy.In above-mentioned prior powder metallurgy method, SmCo
5Permanent magnet alloy is to utilize the magnetic field orientating method of magnetocrystalline anisotropy to obtain magneticanisotropy.In fact, also be a kind of effective way that obtains magneticanisotropy with the alloy plastic deformation, and in another kind of RE permanent magnetic alloy Nd-Fe-B, obtained success.But also do not obtain fine and close magneticanisotropy SmCo at present by the alloy plastic deformation
5The precedent of magnet.
Summary of the invention
The objective of the invention is to solve the problems of the prior art, and provide a kind of full compact block anisotropy nanocrystalline SmCo
5The preparation method of magnet.
The present invention by with behind Sm and the Co master alloy melting, ball milling, fast hot pressing and thermal distortion are handled, and make fully compact massive SmCo
5Nanocrystalline permanent magnet alloy specifically may further comprise the steps:
1) with purity greater than 99.9% Sm and purity greater than 99.9% Co metal according to SmCo
5Composition proportion be under 99.999% the argon shield condition in purity, in shower furnace behind the master alloy melting, be ball milling 5 hours under 99.999% the argon shield condition with mother alloy in purity, obtain the amorphous alloy powder (see figure 1);
2) after amorphous alloy powder being packed in the carboloy mould, carry out quick hot-pressing processing and obtain the nanocrystalline SmCo of complete fine and close isotropy
5Magnet, hot pressing parameters is fast: under the pressure of 100-1000Mpa,, be warming up to 600-700 ℃ from room temperature with the temperature rise rate of 50-200 ℃/min, and insulation 0-10min;
3) to complete fine and close isotropy SmCo
5Magnet carries out the Rapid Thermal compressive strain to be handled, and obtains the nanocrystalline SmCo of complete fine and close anisotropy
5Magnet, Rapid Thermal compressive strain processing parameter is: under the pressure of 20-60Mpa, be warming up to 750-900 ℃ with the temperature rise rate of 50-150 ℃/min, and insulation 0-10min.
The present invention has following beneficial effect:
1) the prepared SmCo of the present invention
5Magnet has tangible SmCo
5Phase C axialite body texture (see figure 2) and corresponding remarkable magneticanisotropy (Fig. 5); Magnet density reaches more than 98% of congruent materials theory density (seeing Table 1); The average grain size of magnet is nano level (seeing Fig. 3 and Fig. 4); Has good magnetic performance (seeing Table 1).
2) preparation technology of the present invention is simple, and is with short production cycle, and cost is low.
Description of drawings
The XRD figure spectrum (2 θ are angle of diffraction) of the non-crystalline state powder that Fig. 1, the present invention are prepared.
The fully compact massive anisotropic nanocrystalline SmCo of Fig. 2, embodiment 1 preparation
5The crystalline structure XRD figure spectrum that is parallel to deformation direction of magnet.
The fully compact massive anisotropic nanocrystalline SmCo of Fig. 3, embodiment 1 preparation
5The crystal grain micro-organization chart that is parallel to deformation direction (transmission electron microscope photo) of magnet.
The fully compact massive anisotropic nanocrystalline SmCo of Fig. 4, embodiment 1 preparation
5The crystal grain micro-organization chart perpendicular to deformation direction of magnet (transmission electron microscope photo).
The fully compact massive anisotropic nanocrystalline SmCo of Fig. 5, embodiment 1 preparation
5The magnetzation curve that is parallel and perpendicular to deformation direction of magnet and magnetic hysteresis loop (H is a magneticstrength, and M is the specific magnetising moment).
The invention will be further described below in conjunction with the drawings and specific embodiments.
Embodiment
Embodiment 1
1) with purity greater than 99.9% Sm and purity greater than 99.9% Co metal according to SmCo
5Composition proportion adopt the melting of vacuum shower furnace after, carried out fragmentation and ball milling 5 hours, the acquisition amorphous alloy powder;
2) amorphous alloy powder is packed into carry out quick hot pressing in the carboloy grinding tool: under the pressure of 100Mpa,, be warming up to 700 ℃ from room temperature with the temperature rise rate of 50 ℃/min, and insulation 0min, obtain the nanocrystalline SmCo of complete fine and close isotropy
5Magnet;
3) with the nanocrystalline SmCo of complete fine and close isotropy
5Magnet carries out the Rapid Thermal compressive strain to be handled: under the pressure of 20Mpa, be warming up to 900 ℃ with the temperature rise rate of 50 ℃/min, and insulation 0min, deformation ratio 90% obtains the nanocrystalline SmCo of complete fine and close anisotropy
5Magnet (magnetic property and density see Table).
Embodiment 2
1) with purity greater than 99.9% Sm and purity greater than 99.9% Co metal according to SmCo
5Composition proportion adopt the melting of vacuum shower furnace after, carried out fragmentation and ball milling 5 hours, the acquisition amorphous alloy powder;
2) amorphous alloy powder is packed into carry out quick hot pressing in the carboloy grinding tool: under the pressure of 1000Mpa,, be warming up to 600 ℃ from room temperature with the temperature rise rate of 200 ℃/min, and insulation 10min, obtain the nanocrystalline SmCo of complete fine and close isotropy
5Magnet;
3) with the nanocrystalline SmCo of complete fine and close isotropy
5Magnet carries out the Rapid Thermal compressive strain to be handled: under the pressure of 60Mpa, be warming up to 750 ℃ with the temperature rise rate of 150 ℃/min, and insulation 10min, deformation ratio 70% obtains the nanocrystalline SmCo of complete fine and close anisotropy
5Magnet (magnetic property and density see Table).
Embodiment 3
1) with purity greater than 99.9% Sm and purity greater than 99.9% Co metal according to SmCo
5Composition proportion adopt the melting of vacuum shower furnace after, carried out fragmentation and ball milling 5 hours, the acquisition amorphous alloy powder;
2) amorphous alloy powder is packed into carry out quick hot pressing in the carboloy grinding tool: under the pressure of 500Mpa,, be warming up to 650 ℃ from room temperature with the temperature rise rate of 100 ℃/min, and insulation 5min, obtain the nanocrystalline SmCo of complete fine and close isotropy
5Magnet;
3) with the nanocrystalline SmCo of complete fine and close isotropy
5Magnet carries out the Rapid Thermal compressive strain to be handled: under the pressure of 30Mpa, be warming up to 850 ℃ with the temperature rise rate of 100 ℃/min, and insulation 5min, deformation ratio 80% obtains the nanocrystalline SmCo of complete fine and close anisotropy
5Magnet (magnetic property and density see Table).
The fully compact massive anisotropic nanocrystalline SmCo for preparing among table 1, the embodiment 1-3
5The magnetic property of magnet and density
Claims (1)
1, a kind of fully compact massive anisotropic nanocrystalline SmCo
5The preparation method of magnet is characterized in that, may further comprise the steps:
1) with purity greater than 99.9% Sm and purity greater than 99.9% Co metal according to SmCo
5Composition proportion be under 99.999% the argon shield condition in purity, in shower furnace behind the master alloy melting, be ball milling 5 hours under 99.999% the argon shield condition with mother alloy in purity, obtain amorphous alloy powder;
2) after amorphous alloy powder being packed in the carboloy mould, carry out quick hot-pressing processing and obtain the nanocrystalline SmCo of complete fine and close isotropy
5Magnet, hot pressing parameters is fast: under the pressure of 100-1000Mpa,, be warming up to 600-700 ℃ from room temperature with the temperature rise rate of 50-200 ℃/min, and insulation 0-10min;
3) to complete fine and close isotropy SmCo
5Magnet carries out the Rapid Thermal compressive strain to be handled, and obtains the nanocrystalline SmCo of complete fine and close anisotropy
5Magnet, Rapid Thermal compressive strain processing parameter is: under the pressure of 20-60Mpa, be warming up to 750-900 ℃ with the temperature rise rate of 50-150 ℃/min, and insulation 0-10min.
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CN102140598A (en) * | 2011-03-07 | 2011-08-03 | 北京工业大学 | Preparation method of super high coercivity and low-Co type Sm-Co nanocrystalline alloy |
CN105632673A (en) * | 2014-11-20 | 2016-06-01 | 有研稀土新材料股份有限公司 | Preparation method for permanent magnet material and permanent magnet material |
CN106710764A (en) * | 2017-03-27 | 2017-05-24 | 河北工业大学 | SmCo5-based permanent magnet thin strip magnet and preparation method thereof |
CN106935350A (en) * | 2017-03-13 | 2017-07-07 | 中南大学 | A kind of anisotropy SmCo5Type rare earth permanent-magnetic material and preparation method |
CN108305736A (en) * | 2018-02-01 | 2018-07-20 | 北京工业大学 | A kind of fully compact massive anisotropic nanocrystalline Sm2Co7Magnet and preparation method thereof |
CN108364740A (en) * | 2018-04-10 | 2018-08-03 | 中国科学院物理研究所 | A kind of nanocrystalline mischmetal permanent magnet and its preparation method and application |
CN108899150A (en) * | 2018-09-10 | 2018-11-27 | 重庆科技学院 | A kind of Nd-Fe-B/Sm-Co compoiste adhering magnet and preparation method thereof |
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CN113690040A (en) * | 2021-06-29 | 2021-11-23 | 北京工业大学 | Radiation-oriented nanocrystalline Co-based rare earth permanent magnet ring and preparation method thereof |
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JP2003133117A (en) * | 2001-10-23 | 2003-05-09 | Nec Tokin Corp | METHOD FOR MANUFACTURING 2-17 BASED Sm-Co RARE-EARTH PERMANENT MAGNET |
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CN102140598A (en) * | 2011-03-07 | 2011-08-03 | 北京工业大学 | Preparation method of super high coercivity and low-Co type Sm-Co nanocrystalline alloy |
CN105632673B (en) * | 2014-11-20 | 2017-11-10 | 有研稀土新材料股份有限公司 | The preparation method and permanent-magnet material of permanent-magnet material |
CN105632673A (en) * | 2014-11-20 | 2016-06-01 | 有研稀土新材料股份有限公司 | Preparation method for permanent magnet material and permanent magnet material |
CN106935350A (en) * | 2017-03-13 | 2017-07-07 | 中南大学 | A kind of anisotropy SmCo5Type rare earth permanent-magnetic material and preparation method |
CN106710764B (en) * | 2017-03-27 | 2018-06-22 | 河北工业大学 | A kind of SmCo5Base permanent magnetism thin strip magnet and preparation method thereof |
CN106710764A (en) * | 2017-03-27 | 2017-05-24 | 河北工业大学 | SmCo5-based permanent magnet thin strip magnet and preparation method thereof |
WO2019047295A1 (en) * | 2017-09-07 | 2019-03-14 | 北京工业大学 | Method for preparing samarium-cobalt compound nanoparticle having adjustable composition and particle size |
CN108305736A (en) * | 2018-02-01 | 2018-07-20 | 北京工业大学 | A kind of fully compact massive anisotropic nanocrystalline Sm2Co7Magnet and preparation method thereof |
CN108364740A (en) * | 2018-04-10 | 2018-08-03 | 中国科学院物理研究所 | A kind of nanocrystalline mischmetal permanent magnet and its preparation method and application |
CN108899150A (en) * | 2018-09-10 | 2018-11-27 | 重庆科技学院 | A kind of Nd-Fe-B/Sm-Co compoiste adhering magnet and preparation method thereof |
CN108899150B (en) * | 2018-09-10 | 2020-10-16 | 重庆科技学院 | Nd-Fe-B/Sm-Co composite bonded magnet and preparation method thereof |
CN113690040A (en) * | 2021-06-29 | 2021-11-23 | 北京工业大学 | Radiation-oriented nanocrystalline Co-based rare earth permanent magnet ring and preparation method thereof |
CN113658791A (en) * | 2021-07-23 | 2021-11-16 | 北京工业大学 | Method for preparing nanocrystalline Co-based rare earth permanent magnet with high coercive force and high magnetic anisotropy |
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