CN1171313A - Process for preparing permanent magnet powder - Google Patents

Process for preparing permanent magnet powder Download PDF

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Publication number
CN1171313A
CN1171313A CN 97104337 CN97104337A CN1171313A CN 1171313 A CN1171313 A CN 1171313A CN 97104337 CN97104337 CN 97104337 CN 97104337 A CN97104337 A CN 97104337A CN 1171313 A CN1171313 A CN 1171313A
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hydrogen
powder
temperature
described method
ndfeb
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CN 97104337
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CN1059368C (en
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李岫梅
潘伟
王平
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Central Iron and Steel Research Institute
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Central Iron and Steel Research Institute
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Abstract

A process for preparing permanant-megnet rare-earth powder, especially the bounded magnetic powder of NdFeB, includes such technological steps as atomized pulverization to obtain spherical particles, screening to 30-400 microns of granularity, sucking hydrogen at ordinary temp to 950 deg. C, and dehydrogenation at 700-800 deg. C and staged tempering, and features simple process, wide application range, good effect of HDDR treatment and high magnetism of product.

Description

A kind of preparation method of permanent magnet powder
The invention belongs to the preparation field of rare earth permanent magnet powder.Be particularly suitable for the preparation method of NdFeB bonding magnetic.
In the prior art, the production method that is used as bonded permanent magnet NdFeB alloy powder has the NdFeB alloy pig through fragmentation, and ball milling becomes the powder of certain size, and then manufactures bonded permanent magnet.Because the magnetic property of this bonded permanent magnet is lower, can not satisfy present instructions for use.In recent years, along with improving constantly of production technology, the method for preparing the NdFeB alloy magnetic powder also had breakthrough.For example disclose a kind of method that adopts gas atomization to produce thicker spherical NdFeB alloyed powder among the United States Patent (USP) NO.51227970, this method comprises that the spherical NdFeB alloyed powder with 200 μ m～300 μ m particle diameters is inhaled hydrogen one under 660～850 ℃ temperature separate the hydrogen processing.But the NdFeB alloy powder character that this patent place of matchmakers produces is still isotropism, and therefore the magnet remanent magnetism and the maximum magnetic energy product of being produced is all lower.U.S. Rhone-Poulenc Specialty Chemicals Co is arranged again at Chinese patents " the spherical powder and the manufacture method thereof of magnetic anisotropy " (publication number CN1100228A), this patent introduction be to adopt inert gas atomizer, or other method is produced average grain diameter and is lower than 200 μ m, and the optimum grain-diameter scope is at the spherical powder of the NdFeB of 10 μ m～70 μ m, again this powder is carried out about 1 hour hydrogen disproportionation in the temperature of 500 ℃～1000 ℃ of scopes, best disproportionation temperature is 900 ℃～950 ℃ disproportionations 1 hour.Desorption temperature 500 ℃～1000 ℃ dehydrogenation 1-3 hour, best dehydrogenating technology is to carry out dehydrogenation in 1 hour in the vacuum of 900 ℃～950 ℃ of scopes.Be to improve the intrinsic coercive force of powder, can be again the powder of dehydrogenation be heated to 500 ℃～700 ℃.This method is to produce the magnetic anisotropy powder of NdFeB, and its best magnetic property is about Br=7.8 (KG), Hci=15.7 (KOe), BHmax=15.5 (MGOe).The main weak point of the magnetic that adopts this method to produce is that the on the low side and powder of magnetic property requires tight powder process condition harshness etc.
The purpose of the inventive method is that a kind of preparation technology of proposition is reasonable, the method for the production NdFeB permanent-magnet powder that the wide magnetic product performance of the scope of application is good
According to purpose of the present invention, the method for preparing NdFeB permanent magnetism powder that we proposed is that NdFeB alloy mother liquor is jetted on the atomising device of being furnished with the annular flow nozzle, make the molten steel atomizing form fine spherical grains particle and quench solidification, then with this NdFeB powder vacuum dehydrogenation again after the stage is inhaled the hydrogen disproportionation, for improving the magnetic property of product, can carry out tempering heat treatment again.Therefore the atomization powder process of being adopted in the methods of the invention is meant by designer's requirement and carries out the alloyage composition, makes steel under argon shield, when molten steel reaches atomization temperature, molten steel is injected the bottom have the tundish that leaks eye; And the atomizing of in leaking the atomising device of being furnished with ring-type nozzle (full-shape) near the eyes admittedly, jetting, the atomization temperature that it is characterized in that the NdFeB molten steel should be in 1440 ℃～1510 ℃ scopes, the winding-up molten steel angle of annular nozzle is in 40 °～60 ° scopes, and the stream pressure of annular nozzle winding-up molten steel should be at 8-20Kg/cm 2The best atomization temperature of its molten steel is 1480 ℃ in said method, and the best winding-up angle (full-shape) of annular nozzle winding-up molten steel is 45 °, and best winding-up stream pressure is 15Kg/cm 2NdFeB powder after atomizing should carry out sub-sieve, the axle crystallite such as belong to or non crystalline structure should screen out less than the powder of 30 μ m, its reason is the NdFeB powder that the HDDR processing method that is unfavorable for the later stage adopts HDDR to handle in the methods of the invention, should select the powder granularity is the screening powder of 30 μ m～400 μ m, wherein should account for the 10%-20% of NdFeB powder total amount, the processing method of this powder be should be the stage inhale hydrogen disproportionation and dehydrogenation at 200 μ m～powder of 400 μ m.It is that the NdFeB powder is placed in the container that HDDR in the methods of the invention handles, and is evacuated to 1 * 10 -8Charge into 2-5 atmospheric hydrogen behind the torr again, temperature ranges is 20 ℃-200 ℃, to temperature back insulation 1 hour, continue to be warming up to 800 ℃-950 ℃ when inhaling for the first time again after hydrogen finishes, Hydrogen Vapor Pressure increases to 5-10 atmospheric pressure, is incubated after 10 minutes, again Hydrogen Vapor Pressure is reduced to 2-4 and go into air pressure, continue insulation again and carried out the disproportionation processing in 2-4 hour, after inhaling for the second time the hydrogen end, should cool to 700 ℃-850 ℃, and be evacuated to 1 * 1 -4Torr should be cooled to room temperature rapidly after being incubated 1 hour, this process is a certain embodiments, and in certain embodiments, the disproportionated reaction product reverts to former alloy composition again, but the superfine new grainiess of the inner formation of alloy powder particle.In said method of the present invention, the best holding temperature of inhaling hydrogen for the first time is 100 ℃, it is 4 atmospheric pressure that the best is filled hydrogen pressure, and the best holding temperature of inhaling for the second time hydrogen is 850 ℃, the best fill hydrogen pressure be 8 go into air pressure and be incubated 10 minutes after hydrogen be depressurized to 4 atmospheric pressure and be incubated 2 hours again.Best desorption temperature is 780 ℃
In said method of the present invention, adopt the atomized particle of 30 μ m～400 μ m to be commonly uniform radial columnar crystal structure, because the crystal of this structure extremely is beneficial to the orientation development of C axle, after adopting the inventive method above-mentioned NdFeB powder to be carried out the HDDR processing, cause Nd 2Fe 14The C axle directional profile of B crystal grain makes Nd inherent in the alloy powder particle 2Fe 14B crystal grain promptly shows tangible magnetic anisotropy towards the direction growth that helps the C axle, and this behavior causes under the effect of outside magnetic field, and magnet has very strong anisotropic magnetic performance.In the methods of the invention, for improving the magnetic property of NdFeB magnetic, can adopt the stage tempering heat treatment, the method for its tempering heat treatment is that the NdFeB powder after HDDR is handled is placed in the container, and is evacuated to 1 * 10 -4Torr charges into argon gas protection then, and temperature ranges is that 600 ℃ of insulations were chilled to the chamber after 1 hour, or 600 ℃ of insulations were reduced to 500 ℃ of insulations in 1 hour again and are chilled to room temperature after 1 hour.
Adopt method that the present invention prepares the NdFeB permanent magnet powder compared with prior art, have powder and prepare advantages of simple, product magnetic property height, the high NdFeB powder scope of application after atomizing is wide and through characteristics such as the HDDR treatment effect are good.
Embodiment
According to two kinds of NdFeB alloying components that the designer proposed, we have smelted two stove alloy pigs, and its concrete chemical analysis sees Table 1, and we have enumerated the concrete composition of NdFeB material in table 1.In order to contrast conveniently, we are divided into this two stoves material is 2 groups, and according to the different process parameters range of the inventive method these 2 groups of materials has been carried out contrast test, and sequence number 1,2,3 is first composition part in each table, 4,5,6 is second composition part, and 7 is the composition of contrast material.Table 2 is the contrast of atomization process and powder.Table 3 is the contrast of the different technical parameters handled through HDDR in the inventive method.Table 4 should be evacuated to 1 * 10 for the contrast of dehydrogenation processing and temper different technical parameters when dehydrogenation -8Torr should be evacuated to 1 * 10 earlier when temper -4Torr charges into argon shield and intensification again.The LDJ9600 vibrating specimen magnetometer is adopted in the measurement of magnetic property in the embodiment of the invention.Table 5 is the contrast of magnetic property.
Table 1 composition at%
Numbering ????Nd ??Fe ????B ????Co ????Ga ????Nb ??Dy
????1 ????12.8 ??70.7 ????6 ????10 ????- ????- ??0.5
????2 ????12.8 ??70.7 ????6 ????10 ????- ??0.5 ???-
????3 ????12.8 ??70.7 ????6 ????10 ????0.5 ????- ???-
????4 ????12 ??75.5 ????6 ????5 ????1.5 ????- ???-
????5 ????12 ??75.5 ????6 ????5 ????- ??1.5 ???-
????6 ????12 ??75.5 ????6 ????5 ????- ????- ??1.5
????7 * ????11.7 ??80 ????6 ????- ????- ??0.5 ??1.3
Table 2 atomization process and powder contrast
Numbering Atomization temperature (℃) Winding-up angle (degree) Jetting pressure Kg/cm2 Particle mean size d (μ m) ＞200μm
??1 ????1440 ????50 ????12 ????72 ??12％
??2 ????1440 ????50 ????12 ????70 ??12％
??3 ????1480 ????45 ????15 ????65 ??15％
??4 ????1480 ????45 ????15 ????67 ??15％
??5 ????1480 ????40 ????8 ????69 ??19％
??6 ????1500 ????40 ????8 ????75 ??19％
??7 * ????- ?????- ?????- ????10-70 ???-
Table 3 HDDR handles
Numbering Inhale for the first time hydrogen Inhale for the second time hydrogen
Temperature (℃) Hydrogen Vapor Pressure) (atm) Insulation (h) Temperature (℃) Hydrogen Vapor Pressure (atm) Insulation (h)
?1 ????150 ????2 ????1 ????900 ????5→4 ????10’+2
?2 ????150 ????2 ????1 ????850 ????5→4 ????10’+2
?3 ????100 ????4 ????1 ????850 ????8→4 ????10’+2
?4 ????100 ????4 ????1 ????850 ????8→4 ????10’+2
?5 ????20 ????5 ????1 ????800 ????8→4 ????10’+2
?6 ????20 ????5 ????1 ????800 ????10→5 ????10’+2
?7 * ???900-950 ????- ????1 ????- ????- ????-
Table 4 takes off H and temper
Numbering Take off the H temperature (℃) Time (h) Temperature (℃) Time (h)
????1 ????700 ????1 ????600 ????1
????2 ????750 ????1 ????600 ????1
????3 ????780 ????1 ????600+500 ????1+1
????4 ????780 ????1 ????600+520 ????1+1
????5 ????800 ????1 ????600 ????1
????6 ????800 ????1 ????600+500 ????1+1
????7 * ??900～950 ????1.5 ????550 ????1.5
Table 5 permanent magnetism performance
Numbering ????Br ???(T) ?????iHc ????(KA/m) ???(BH)max ???(KJ/m 3)
??1 ??0.82 ????1289.8 ????117.0
??2 ??0.91 ????1170.4 ????140.9
??3 ??0.94 ????1186.3 ????152.9
??4 ??0.92 ????1126.1 ????146.5
??5 ??0.79 ????1337.6 ????118.6
??6 ??0.78 ????1194.3 ????115.4
??7 * ??0.78 ????1250 ????123.4

Claims (10)

1, a kind of method for preparing the NdFeB alloy powder particle, this method is with NdFeB alloy mother liquor, on the atomising device that the annular airflow nozzle is arranged, jet into powder, again with this powder vacuum dehydrogenation again after the stage is inhaled the hydrogen disproportionation, carry out tempering heat treatment at last again, the atomization temperature that it is characterized in that the inventive method atomizing NdFeB molten steel should be at 1440 ℃～1510 ℃, and the winding-up molten steel angle (full-shape) of annular nozzle is 40 °～60 °, and the stream pressure of annular nozzle winding-up molten steel is 8～20Kg/cm 2, the NdFeB powder granularity of handling through HDDR should be 30 μ m～400 μ m, and powder is placed in the container, is evacuated to 1 * 10 -aCharge into 2-5 atmospheric hydrogen behind the torr, temperature ranges is 20 ℃～200 ℃, to temperature back insulation 1 hour, be warming up to 800 ℃～950 ℃ Hydrogen Vapor Pressures again and increase to 5～10 atmospheric pressure, be incubated and again Hydrogen Vapor Pressure reduced to 2-4 atmospheric pressure after 10 minutes, and insulation carried out disproportionation in 2-4 hour and handles, and inhaled to cool to 700 ℃～850 ℃ and be evacuated to 1 * 10 after hydrogen finishes -4Torr is incubated and is chilled to room temperature after 1 hour, and temper is the powder after the HDDR processing to be placed in the container be evacuated to 1 * 100 -4Applying argon gas protection behind the torr, temper temperature are that 600 ℃ of insulations were chilled to room temperature after 1 hour, or 600 ℃ of insulations were reduced to 500 ℃ of insulations in 1 hour again and are chilled to room temperature after 1 hour.
2,, it is characterized in that the best atomization temperature of molten steel is 1480 ℃ according to the described method of claim 1.
3,, it is characterized in that the best winding-up folder (full-shape) of annular nozzle winding-up molten steel is 45 ° according to the described method of claim 1.
4,, it is characterized in that best winding-up stream pressure is 15Kg/cm according to the described method of claim 1 2
5,, it is characterized in that in the NdFeB powder, having 200 μ m～powder of 400 μ m should account for the 10%-20% of powder total amount according to the described method of claim 1.
6, according to the described method of claim 1, it is characterized in that inhaling for the first time the best holding temperature of hydrogen is 100 ℃.
7, according to the described method of claim 1, it is characterized in that inhaling for the first time hydrogen the best, to fill hydrogen pressure be 4 atmospheric pressure.
8, according to the described method of claim 1, the optimum temperature that it is characterized in that inhaling for the second time hydrogen is 850 ℃.
9, according to the described method of claim 1, the best that it is characterized in that inhaling for the second time hydrogen fill hydrogen pressure and temperature retention time be the best to fill hydrogen pressure be 8 atmospheric pressure, be incubated after 10 minutes hydrogen and reduce to 4 atmospheric pressure and be incubated 2 hours again.
10,, it is characterized in that best desorption temperature is 780 ℃ according to the described method of claim 1.
CN97104337A 1997-05-23 1997-05-23 Process for preparing permanent magnet powder Expired - Fee Related CN1059368C (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010031264A1 (en) * 2008-09-19 2010-03-25 广州金南磁塑有限公司 Anisotropic flexible bonded ndfeb magnet and manufacturing method of the same
CN101850425A (en) * 2009-03-30 2010-10-06 Tdk株式会社 Rare earth alloy powder and manufacture method thereof, anisotropic bond magnet compound and anisotropic bond magnet
CN101767200B (en) * 2010-01-05 2012-05-09 北京科技大学 Minute spherical Nd-Fe-B powder preparation method
CN102576602A (en) * 2010-03-31 2012-07-11 日东电工株式会社 Permanent magnet and method for manufacturing permanent magnet
CN104609845A (en) * 2014-12-15 2015-05-13 横店集团东磁股份有限公司 Preparation method of injection molding bonded magnetic powder
CN104625079A (en) * 2015-01-28 2015-05-20 北矿磁材科技股份有限公司 Preparing method of rare earth iron-boron-based anisotropy magnetic powder and prepared magnetic powder
CN108133796A (en) * 2017-12-11 2018-06-08 北京科技大学 A kind of preparation method of sintered magnet NdFeB magnetic powder

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CN104637667B (en) * 2015-01-16 2018-02-09 浙江和也健康科技有限公司 A kind of anti-oxidation flexible stickup NdFeB magnetic stripes and preparation method thereof

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1027577C (en) * 1993-03-01 1995-02-08 冶金工业部钢铁研究总院 Preparation method of rare-earthpermanent-magnet powder
US5474623A (en) * 1993-05-28 1995-12-12 Rhone-Poulenc Inc. Magnetically anisotropic spherical powder and method of making same

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010031264A1 (en) * 2008-09-19 2010-03-25 广州金南磁塑有限公司 Anisotropic flexible bonded ndfeb magnet and manufacturing method of the same
CN101850425A (en) * 2009-03-30 2010-10-06 Tdk株式会社 Rare earth alloy powder and manufacture method thereof, anisotropic bond magnet compound and anisotropic bond magnet
CN101850425B (en) * 2009-03-30 2012-12-05 Tdk株式会社 Rare earth alloy powders and manufacturing method thereof, compound for anisotropic bonded magnet and anisotropic bonded magnet
CN101767200B (en) * 2010-01-05 2012-05-09 北京科技大学 Minute spherical Nd-Fe-B powder preparation method
CN102576602A (en) * 2010-03-31 2012-07-11 日东电工株式会社 Permanent magnet and method for manufacturing permanent magnet
US9048014B2 (en) 2010-03-31 2015-06-02 Nitto Denko Corporation Permanent magnet and manufacturing method thereof
CN104609845A (en) * 2014-12-15 2015-05-13 横店集团东磁股份有限公司 Preparation method of injection molding bonded magnetic powder
CN104625079A (en) * 2015-01-28 2015-05-20 北矿磁材科技股份有限公司 Preparing method of rare earth iron-boron-based anisotropy magnetic powder and prepared magnetic powder
CN108133796A (en) * 2017-12-11 2018-06-08 北京科技大学 A kind of preparation method of sintered magnet NdFeB magnetic powder
CN108133796B (en) * 2017-12-11 2019-10-22 北京科技大学 A kind of preparation method of sintered magnet NdFeB magnetic powder

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