CN1059368C - Process for preparing permanent magnet powder - Google Patents
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- CN1059368C CN1059368C CN97104337A CN97104337A CN1059368C CN 1059368 C CN1059368 C CN 1059368C CN 97104337 A CN97104337 A CN 97104337A CN 97104337 A CN97104337 A CN 97104337A CN 1059368 C CN1059368 C CN 1059368C
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Abstract
The present invention belongs to the field of the manufacture of rare-earth permanent magnetic powder, which is especially suitable for a method for the manufacture NdFeB bounded magnetic powder. The method comprises the following steps: producing powder by atomization, sieving powder particles, sucking hydrogen, dehydrogenating and tempering for treatment. The method of the present invention is capable of producing spherical powder particles, particle sizes for the sieved powder particles range from 30 micrometers to 400 micrometers, temperature for sucking hydrogen ranges from room temperature to 850 DEG C, temperature for dehydrogenating ranges from 700 DEG C to 800 DEG C, and period tempering is carried out in tempering treatment. Compared with the prior art, the method has the advantages of simple and reasonable preparation of powder particles, wide application range, favourable effect after the treatment of HDDR, high magnetic performance of products, etc.
Description
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=0.78T, iHc=1250KA/m, (BH)
Max=124KJ/m
3The 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 sternly 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 solution that we proposed is the requirement preparation NaFeB alloy composition by the designer; under argon shield, make steel; when molten steel reaches with atomization temperature; molten steel is injected the bottom have the tundish that leaks eye, and be atomized into the powder grain leaking to enclose near the eyes to jet in the atomising device of being furnished with annular flow nozzle (full-shape), then with this NaFeB 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.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, should carry out sub-sieve through the NdFeB powder of atomizing reprocessing, and to select granularity be 30 μ m～400 μ m, then powder is placed in the container, be evacuated to 1 * 10
-3Charge into 2-5 atmospheric hydrogen behind the torr, temperature ranges is 20 ℃～200 ℃, to temperature back insulation 1 hour, after inhaling hydrogen for the first time, 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 handle, cool to 700 ℃～850 ℃ and be evacuated to 1 * 10 after hydrogen finishes when inhaling for the second time
-4Torr is incubated and is chilled to room temperature after 1 hour, and temper is the stage to be inhaled powder after hydrogen disproportionation and vacuum dehydrogenation are handled place in the container and be evacuated to 1 * 10
-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.
According to foregoing, other features in the methods of the invention also have 1480 ℃ of the best atomization temperatures of NaFeB molten steel.The best winding-up angle (full-shape) of annular nozzle winding-up molten steel is 45 °.The best winding-up of atomizing stream pressure is 15Kg/cm
2Other feature in the methods of the invention is that the best holding temperature of inhaling for the first time hydrogen is 100 ℃ in addition, and it is 4 atmospheric pressure that the best is filled hydrogen pressure.The best holding temperature of inhaling hydrogen for the second time is 850 ℃, and it is 8 atmospheric pressure that the best is filled hydrogen pressure, and hydrogen is depressurized to 4 atmospheric pressure after being incubated 10 minutes, is 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 that above-mentioned NdFeB powder is handled, causes 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 handling 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 NdFeB powder scope of application after atomizing is wide and inhale characteristics such as hydrogen disproportionation and dehydrogenation treatment effect are good through the stage.
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 inhaling the different technical parameters of hydrogen disproportionation and dehydrogenation processing in the inventive method through the stage.Table 4 should be evacuated to 1 * 10 for the contrast of dehydrogenation processing and temper different technical parameters when dehydrogenation
-3Torr 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 particle capability.
Table 1 composition percentage by weight %
| 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/cm 2 | 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 stage inhales the hydrogen disproportionation and dehydrogenation is handled
| 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 mealiness energy
| 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, should carry out sub-sieve through the NdFeB powder of atomizing reprocessing, and to select granularity be 30 μ m～400 μ m, then powder is placed in the container, be evacuated to 1 * 10
-3Charge 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 to be evacuated to 1 * 10 in the powder placement container that will inhale after hydrogen disproportionation and dehydrogenation are handled
-4Applying argon gas protection behind the torr, temper temperature are that 600 ℃ of insulations were 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97104337A CN1059368C (en) | 1997-05-23 | 1997-05-23 | Process for preparing permanent magnet powder |
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|---|---|---|---|
| CN97104337A CN1059368C (en) | 1997-05-23 | 1997-05-23 | Process for preparing permanent magnet powder |
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| CN1171313A CN1171313A (en) | 1998-01-28 |
| CN1059368C true CN1059368C (en) | 2000-12-13 |
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| CN97104337A Expired - Fee Related CN1059368C (en) | 1997-05-23 | 1997-05-23 | Process for preparing permanent magnet powder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104637667A (en) * | 2015-01-16 | 2015-05-20 | 浙江和也健康科技有限公司 | Oxidation-resisting flexible NdFeB pasting magnetic stripe and preparation method thereof |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101477866A (en) * | 2008-09-19 | 2009-07-08 | 广州金南磁塑有限公司 | Anisotropic flexible adhesion Nd-Fe-B magnets and manufacturing method thereof |
| 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 |
| EP2503567B1 (en) | 2010-03-31 | 2014-07-02 | Nitto Denko Corporation | Manufacturing method for permanent magnet |
| CN104609845B (en) * | 2014-12-15 | 2017-06-27 | 横店集团东磁股份有限公司 | It is a kind of to be molded with the preparation method for bonding magnetic |
| CN104625079B (en) * | 2015-01-28 | 2017-05-10 | 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 |
| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1075669A (en) * | 1993-03-01 | 1993-09-01 | 冶金工业部钢铁研究总院 | The preparation method of rare earth permanent-magnet powder |
| CN1100228A (en) * | 1993-05-28 | 1995-03-15 | 罗纳-布朗克特殊化学公司 | Magnetically anisotropic spherical powder |
-
1997
- 1997-05-23 CN CN97104337A patent/CN1059368C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1075669A (en) * | 1993-03-01 | 1993-09-01 | 冶金工业部钢铁研究总院 | The preparation method of rare earth permanent-magnet powder |
| CN1100228A (en) * | 1993-05-28 | 1995-03-15 | 罗纳-布朗克特殊化学公司 | Magnetically anisotropic spherical powder |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104637667A (en) * | 2015-01-16 | 2015-05-20 | 浙江和也健康科技有限公司 | Oxidation-resisting flexible NdFeB pasting magnetic stripe and preparation method thereof |
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| CN1171313A (en) | 1998-01-28 |
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