CN1242427C - Method for preparing high-performance biphase rare-earth permanent magnet material using hydrogenation heat treatment process - Google Patents
Method for preparing high-performance biphase rare-earth permanent magnet material using hydrogenation heat treatment process Download PDFInfo
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- CN1242427C CN1242427C CN 200310108666 CN200310108666A CN1242427C CN 1242427 C CN1242427 C CN 1242427C CN 200310108666 CN200310108666 CN 200310108666 CN 200310108666 A CN200310108666 A CN 200310108666A CN 1242427 C CN1242427 C CN 1242427C
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Abstract
The present invention discloses a method for preparing high-performance bi-phase rare-earth permanent magnet material using a hydrogenation heat treatment method. The present invention comprises: firstly, alloy is prepared in a vacuum melting method; secondly, prealloy powder is prepared by using a rapid quenching method or a mechanical alloying method; then, the prealloy powder is arranged in a hydryzing device, hydrogen is led into the hydryzing device after the hydryzing device is pumped with vacuum and hydrogen pick-up and hydrogen relief treatment is carried out within the temperature range of 600 to 1000 DEG C; finally, an alloy magnet is prepared by using a bonding, a cold pressing, a hot pressing or a warm deformation method. Magnetic powder and magnets obtained by using the present invention has better comprehensive permanent magnet performance compared with a traditional bi-phase permanent magnet rare-earth material, and the method for preparing high-performance bi-phase rare-earth permanent magnet material also has the advantages of simple production equipment and process and little process consumption.
Description
Technical field
The present invention relates to the method that a kind of heat of hydrogenation facture prepares dual-phase permaneng-magnet rare-earth material.
Background technology
Rare-earth bond magnet is a kind of magnetic material that is formed with organic or soft metal binding agent bonding by the magnetic rare earth alloy powder.Rare-earth bond magnet has the very high ratio of performance to price, can be formed directly in or be processed into the parts of shape complexity, has very high toughness, not cracky, cracking, advantages such as the magnetic property deviation is little, meet in recent years requirement, so its total sales volume is increased rapidly to the high performance and the low price of magnetic material.The rare-earth bond magnet magnetic property is subjected to the influence of Magnaglo performance and packing density, and wherein the body of powder magnetic property is considered to primary factor.At present, the comprehensive magnetic property of isotropism Nd-Fe-B rare earth permanent-magnet powder is generally: B
r=0.55-0.80T,
iH
c=720-1200kA/m, (BH)
Max=64-96kJ/m
3
The nano double phase rare earth permanent magnetic material is made of with soft magnetism mutually mutually nanocrystalline hard magnetic, hard magnetic has high HCJ mutually, soft magnetism has high saturation magnetization mutually, there is the magnetic exchange-coupling interaction in the two-phase interface place, make material have the high saturation and magnetic intensity and Hard Magnetic high-coercive force mutually of soft magnetism phase simultaneously, thereby have high energy product.The magnetic energy product theoretical value of nanometer two-phase permanent magnet can reach 1000kJ/m
3, than the theoretical magnetic energy product height of Sintered NdFeB magnet nearly 1 times.And the content of rare earth of nanometer two-phase permanent magnetic material is few, and low price has than the wide development application prospect.
At present typical nanometer two-phase permanent magnetic material has Nd
2Fe
14B/ α-Fe type and Nd
2Fe
14B/Fe
3Type B.Although soft magnetism phase α-Fe and Fe
3B is improved the remanent magnetization of nanometer two-phase permanent magnet, but coercive force also descends with the adding of soft magnetism phase, is generally less than 450kA/m, has influenced its application in many occasions, particularly when magnet is thin.And because the restriction of preparation means at present, the crystal structure of magnetic is difficult to reach the microstructure that requires in the theoretical model, i.e. two-phase crystallization is continuous, size about 10nm, no non magneticly exist mutually between the two-phase, and being coupled fully.Therefore, the general magnetic energy product of material is the highest can only reach 158kJ/m
-3, greatly differ from each other with theoretical value, can not satisfy the requirement of high-performance magnet.Above factor makes this material fail to be widely used.
Summary of the invention
The purpose of this invention is to provide the method that a kind of heat of hydrogenation facture prepares dual-phase permaneng-magnet rare-earth material.
The step that a kind of heat of hydrogenation facture prepares the method for dual-phase permaneng-magnet rare-earth material is:
1) at first prepared composition is R
xTM
100-x-yM
yIngot casting, R is a rare earth element in the formula, wherein the content of Nd is no less than the 70at% of R total amount; TM is a magnesium-yttrium-transition metal, and wherein the content of Fe is not less than the 75at% of TM total amount; M is a metalloid, and wherein B content is not less than the 90at% of M total amount; X is 6.0～12.0at%, and y is 4.5～10.0at%, ingot casting melting in arc furnace, induction furnace or magnetic levitation melting stove, and melting is carried out under vacuum or protective atmosphere;
2) ingot casting is put into vacuum quick quenching furnace, in a vacuum or high-purity argon gas protection fusing back single roller rapid quenching down, during the ingot casting fast melt-quenching, the linear resonance surface velocity of molybdenum roller is 12m/s～45m/s;
3) under high-purity argon gas atmosphere, it is 30～150 microns particle that fast quenched alloy is broken into diameter;
4) the fast quenching powder is packed in the vacuum furnace, be evacuated to 10
-3～10
-5Pa, feeding purity is 99.999% hydrogen, is heated to 600 ℃-1000 ℃ and inhales hydrogen 5-50 minute, still rests on same temperature range then, being evacuated to hydrogen pressure is 10
-2-10
-4Pa is incubated 5-30 minute, is chilled to room temperature soon;
5) the gained powder by bond, cold pressing, hot pressing or warm deformation come moulding.
The step that another kind of heat of hydrogenation facture prepares the method for dual-phase permaneng-magnet rare-earth material is:
1) at first prepared composition is R
xTM
100-x-yM
yIngot casting, R is a rare earth element in the formula, wherein the content of Nd is no less than the 70at% of R total amount; TM is a magnesium-yttrium-transition metal, and wherein the content of Fe is not less than the 75at% of TM total amount; M is a metalloid, and wherein B content is not less than the 90at% of M total amount; X is 7.0～15.0at%, and y is 5.5～12.0at%, ingot casting melting in arc furnace, induction furnace or magnetic levitation melting stove, and melting is carried out under vacuum or protective atmosphere;
2) under high-purity argon gas protection, it is 50～110 microns particle that ingot casting is broken into diameter, sneaks into purity more than 99.5%, and particle diameter is less than 15 microns iron powder, and the volumn concentration of iron powder is 10%～40%;
3) under high-purity argon gas atmosphere, with mixed-powder high-energy ball milling 35～50 hours;
4) powder behind the high-energy ball milling is packed in the vacuum furnace, be evacuated to 10
-3～10
-5Pa, feeding purity is 99.999% hydrogen, is heated to 600 ℃-1000 ℃ and inhales hydrogen 5-50 minute, still rests on same temperature range then, being evacuated to hydrogen pressure is 10
-2-10
-4Pa is incubated 5-30 minute, is chilled to room temperature soon;
5) the gained powder by bond, cold pressing, hot pressing or warm deformation come moulding.
Advantage of the present invention is:
4) the present invention inhales nitrogen and dehydrogenation owing to adopted suction hydrogen when heat treatment, denitrification process, and the gained magnetic has more tiny, more regular nanometer microstructure than traditional two-phase permanent magnet, thereby has strengthened R
2TM
14M phase and TM exchange-coupling interaction mutually, material has the high saturation and magnetic intensity and the R of TM phase simultaneously
2TM
14The high-coercive force of M phase, thereby can obtain than traditional dual-phase permaneng-magnet rare-earth material better synthesis permanent magnetism.
5) magnetic powders method of the present invention: production equipment and technology are simpler, and processes expend is less.
6) gained magnetic of the present invention and bonded permanent magnet, required ree content is less, thereby with low cost.
Embodiment
Embodiment 1
Adopting purity is that 99.9% Fe, Nd, Dy and 20wt%B-Fe alloy are as raw material, according to Nd
8.5Dy
1Fe
84.5B
6Proportioning, put into the magnetic levitation melting stove, be evacuated down to 10
-3Pa feeds 1.2 * 10 then
5The high-purity argon gas of Pa, melt back is 3 times under argon shield, to guarantee to obtain the uniform ingot casting of composition, for the composition that guarantees ingot casting meets design mix substantially, must pay close attention to the waste of rare earth element in fusion process.Then, alloy cast ingot is put into quick quenching furnace, the vacuum degree that is evacuated in the quick quenching furnace cavity is 10
-3Pa feeds 0.5 * 10 then
5The high-purity argon gas of Pa, ingot casting is behind arc-melting under the high-purity argon gas protection, and being ejected into linear resonance surface velocity is on the molybdenum roller of 35m/s, obtains fast quenched alloy.The fast quenched alloy of gained under the high-purity argon gas protection, is broken into the particle that diameter is the 80-100 micron in ball mill, then, in the vacuum furnace of packing into, is evacuated to 10
-5Pa, feeding purity is 99.999% hydrogen, is heated to 720 ℃, is incubated 25 minutes, being evacuated to hydrogen pressure then is 10
-3Pa is incubated 25 minutes, is chilled to room temperature soon.The gained Magnaglo is mixed with the epoxy resin of 2.5wt%, and compression moulding under the pressure of 300MPa then keeps pressed compact 1 hour down at 150 ℃, makes it to solidify, and obtains bonded permanent magnet.Use vibrating specimen magnetometer, the magnetic property result who measures magnetic is as follows: B
r=1.21T,
iH
c=786kA/m, (BH)
Max=203kJ/m
3The magnetic property result who measures bonded permanent magnet is as follows: B
r=1.03T,
iH
c=785kA/m, (BH)
Max=179kJ/m
3
Embodiment 2
Adopting purity is that 99.9% Fe, Nd, Pr, Zr and 20wt%B-Fe alloy are as raw material, according to Nd
3.6Pr
5.4Fe
84Zr
1B
6Proportioning, put into the magnetic levitation melting stove, be evacuated down to 10
-3Pa feeds 1.2 * 10 then
5The high-purity argon gas of Pa, melt back is 3 times under argon shield, to guarantee to obtain the uniform ingot casting of composition, for the composition that guarantees ingot casting meets design mix substantially, must pay close attention to the waste of rare earth element in fusion process.Then, alloy cast ingot is put into quick quenching furnace, the vacuum degree that is evacuated in the quick quenching furnace cavity is 10
-3Pa feeds 0.5 * 10 then
5The high-purity argon gas of Pa, ingot casting is behind arc-melting under the high-purity argon gas protection, and being ejected into linear resonance surface velocity is on the molybdenum roller of 35m/s, obtains fast quenched alloy.The fast quenched alloy of gained under the high-purity argon gas protection, is broken into the particle that diameter is the 80-100 micron in ball mill, then, in the vacuum furnace of packing into, is evacuated to 10
-5Pa, feeding purity is 99.999% hydrogen, is heated to 750 ℃, is incubated 20 minutes, being evacuated to hydrogen pressure then is 10
-3Pa is incubated 25 minutes, is chilled to room temperature soon.The gained Magnaglo is mixed with the epoxy resin of 2.5wt%, and compression moulding under the pressure of 300MPa then keeps pressed compact 1 hour down at 150 ℃, makes it to solidify, and obtains bonded permanent magnet.Use vibrating specimen magnetometer, the magnetic property result who measures magnetic is as follows: B
r=1.06T,
iH
c=710kA/m, (BH)
Max=195kJ/m
3The magnetic property result who measures bonded permanent magnet is as follows: B
r=0.92T,
iH
c=708kA/m, (BH)
Max=162kJ/m
3
Embodiment 3
Adopting purity is that 99.9% Fe, Nd, Co, Cr and 20wt%B-Fe alloy are as raw material, according to Nd
12.5Fe
69.5Co
10Cr
2B
6Proportioning, put into the magnetic levitation melting stove, be evacuated down to 10
-3Pa feeds 1.2 * 10 then
5The high-purity argon gas of Pa, melt back is 3 times under argon shield, to guarantee to obtain the uniform ingot casting of composition, for the composition that guarantees ingot casting meets design mix substantially, must pay close attention to the waste of rare earth element in fusion process.Under the high-purity argon gas protection, with the ingot casting fragmentation, the particle diameter that sieves is then prepared against high-energy ball milling (particle diameter is good with the 50-90 micron) less than 110 microns ingot casting powder with disintegrating machine.Ingot casting powder after will sieving under protective atmosphere and iron powder (purity is 99.9%, and particle diameter is less than 15 microns) mix, and wherein the volumn concentration of iron powder is 35%.Be under 99.999% the argon gas atmosphere in purity,, then, the product behind the high-energy ball milling packed in the vacuum furnace, be evacuated to 10 above-mentioned mixed powder high-energy ball milling 40 hours
-5Pa, feeding purity is 99.999% hydrogen, is heated to 780 ℃, is incubated 12 minutes, being evacuated to hydrogen pressure then is 10
-3Pa is incubated 20 minutes, and it is cold soon to come out of the stove.Then, the gained Magnaglo is mixed with the epoxy resin of 2.5wt%, compression moulding under 300MPa pressure then keeps pressed compact 1 hour down at 150 ℃, makes it to solidify, and obtains bonded permanent magnet.Use vibrating specimen magnetometer, the magnetic property result who measures magnetic is as follows: B
r=1.18T,
iH
c=755kA/m, (BH)
Max=212kJ/m
3The magnetic property result who measures bonded permanent magnet is as follows: B
r=1.01T,
iH
c=748kA/m, (BH)
Max=175kJ/m
3
Embodiment 4
Adopting purity is that 99.9% Fe, Nd, Nb, Cr and 20wt%B-Fe alloy are as raw material, according to Nd
12.5Fe
79.5CrNbB
6Proportioning, put into the magnetic levitation melting stove, be evacuated down to 10
-3Pa feeds 1.2 * 10 then
5The high-purity argon gas of Pa, melt back is 3 times under argon shield, to guarantee to obtain the uniform ingot casting of composition, for the composition that guarantees ingot casting meets design mix substantially, must pay close attention to the waste of rare earth element in fusion process.Under the high-purity argon gas protection, with the ingot casting fragmentation, the particle diameter that sieves is then prepared against high-energy ball milling (particle diameter is good with the 50-90 micron) less than 110 microns ingot casting powder with disintegrating machine.Ingot casting powder after will sieving under protective atmosphere and iron powder (purity is 99.9%, and particle diameter is less than 15 microns) mix, and wherein the volumn concentration of iron powder is 37%.Be under 99.999% the argon gas atmosphere in purity,, then, the product behind the high-energy ball milling packed in the vacuum furnace, be evacuated to 10 above-mentioned mixed powder high-energy ball milling 42 hours
-5Pa, feeding purity is 99.999% hydrogen, is heated to 700 ℃, is incubated 30 minutes, being evacuated to hydrogen pressure then is 10
-3Pa is incubated 25 minutes, and it is cold soon to come out of the stove.Then, the gained Magnaglo is mixed with the epoxy resin of 2.5wt%, compression moulding under 300MPa pressure then keeps pressed compact 1 hour down at 150 ℃, makes it to solidify, and obtains bonded permanent magnet.Use vibrating specimen magnetometer, the magnetic property result who measures magnetic is as follows: B
r=1.26T,
iH
c=760kA/m, (BH)
Max=221kJ/m
3The magnetic property result who measures bonded permanent magnet is as follows: B
r=1.15T,
iH
c=758kA/m, (BH)
Max=185kJ/m
3
Embodiment 5
Adopting purity is that 99.9% Fe, Nd, La, Tb, Ti, Co, Cu, Ga, Nb, Zr, Si and 20wt%B-Fe alloy are as raw material, according to Nd
9Ga
0.5Fe
84.5B
6, Nd
7Tb
1Fe
86Nb
0.5Zr
0.5B
5, Nd
9La
0.5Fe
78.5Ti
2B
10, Nd
9Fe
75.5Co
8Nb
1Cu
0.5B
6, (Nd
0.4Pr
0.6)
8Fe
85.5Si
1Zr
0.5B
5Proportioning, put into the magnetic levitation melting stove respectively, be evacuated down to 10
-3Pa feeds 1.2 * 10 then
5The high-purity argon gas of Pa, melt back is 3 times under argon shield, to guarantee to obtain the uniform ingot casting of composition, for the composition that guarantees ingot casting meets design mix substantially, must pay close attention to the waste of rare earth element in fusion process.Then, alloy cast ingot is put into quick quenching furnace, the vacuum degree that is evacuated in the quick quenching furnace cavity is 10
-3Pa feeds 0.5 * 10 then
5The high-purity argon gas of Pa, ingot casting is behind arc-melting under the high-purity argon gas protection, and being ejected into linear resonance surface velocity is on the molybdenum roller of 35m/s, obtains fast quenched alloy.The fast quenched alloy of gained under the high-purity argon gas protection, is broken into the particle that diameter is the 80-100 micron in ball mill, then, in the vacuum furnace of packing into, is evacuated to 10
-5Pa, feeding purity is 99.999% hydrogen, is heated to 750 ℃, is incubated 20 minutes, being evacuated to hydrogen pressure then is 10
-3Pa is incubated 20 minutes, is chilled to room temperature soon.The gained Magnaglo is mixed with the epoxy resin of 2.5wt%, and compression moulding under the pressure of 300MPa then keeps pressed compact 1 hour down at 150 ℃, makes it to solidify, and obtains bonded permanent magnet.Use vibrating specimen magnetometer, the magnetic property result who measures magnetic is as follows:
| Composition | Br(T) | iHc(kA/m) | (BH) max (kJ/m 3) |
| Nd 9Ga 0.5Fe 84.5B 6 | 1.10 | 695 | 158 |
| Nd 7Tb 1Fe 86Nb 0.5Zr 0.5B 5 | 1.05 | 780 | 163 |
| Nd 9La 0.5Fe 78.5Ti 2B 10 | 1.09 | 732 | 168 |
| Nd 9Fe 75.5Co 8Nb 1Cu 0.5B 6 | 1.16 | 681 | 152 |
| (Nd 0.4Pr 0.6) 8Fe 85.5Si 1Zr 0.5B 5 | 1.11 | 743 | 171 |
The magnetic property result who measures bonded permanent magnet is as follows:
| Composition | Br(T) | iHc(kA/m) | (BH) max(kJ/m 3) |
| Nd 9Ga 0.5Fe 84.5B 6 | 0.95 | 692 | 131 |
| Nd 7Tb 1Fe 86Nb 0.5Zr 0.5B 5 | 0.88 | 779 | 136 |
| Nd 9La 0.5Fe 78.5Ti 2B 10 | 0.94 | 731 | 138 |
| Nd 9Fe 75.5Co 8Nb 1Cu 0.5B 6 | 1.03 | 678 | 127 |
| (Nd 0.4Pr 0.6) 8Fe 85.5Si 1Zr 0.5B 5 | 0.95 | 740 | 143 |
Claims (2)
1. a heat of hydrogenation facture prepares the method for dual-phase permaneng-magnet rare-earth material, it is characterized in that its step is:
1) at first prepared composition is R
xTM
100-x-yM
yIngot casting, R is a rare earth element in the formula, wherein the content of Nd is no less than the 70at% of R total amount; TM is a magnesium-yttrium-transition metal, and wherein the content of Fe is not less than the 75at% of TM total amount; M is a metalloid, and wherein B content is not less than the 90at% of M total amount; X is 6.0～12.0at, and y is 4.5～10.0at, ingot casting melting in arc furnace, induction furnace or magnetic levitation melting stove, and melting is carried out under vacuum or protective atmosphere;
2) ingot casting is put into vacuum quick quenching furnace, in a vacuum or high-purity argon gas protection fusing back single roller rapid quenching down, during the ingot casting fast melt-quenching, the linear resonance surface velocity of molybdenum roller is 12m/s～45m/s;
3) under high-purity argon gas atmosphere, it is 30～150 microns particle that fast quenched alloy is broken into diameter;
4) the fast quenching powder is packed in the vacuum furnace, be evacuated to 10
-3～10
-5Pa, feeding purity is 99.999% hydrogen, is heated to 600 ℃-1000 ℃ and inhales hydrogen 5-50 minute, still rests on same temperature range then, being evacuated to hydrogen pressure is 10
-2-10
-4Pa is incubated 5-30 minute, is chilled to room temperature soon;
5) the gained powder by bond, cold pressing, hot pressing or warm deformation come moulding.
2. a heat of hydrogenation facture prepares the method for dual-phase permaneng-magnet rare-earth material, it is characterized in that its step is:
1) at first prepared composition is R
xTM
100-x-yM
yIngot casting, R is a rare earth element in the formula, wherein the content of Nd is no less than the 70at% of R total amount; TM is a magnesium-yttrium-transition metal, and wherein the content of Fe is not less than the 75at% of TM total amount; M is a metalloid, and wherein B content is not less than the 90at% of M total amount; X is 7.0～15.0at, and y is 5.5～12.0at, ingot casting melting in arc furnace, induction furnace or magnetic levitation melting stove, and melting is carried out under vacuum or protective atmosphere;
2) under high-purity argon gas protection, it is 50～110 microns particle that ingot casting is broken into diameter, sneaks into purity more than 99.5%, and particle diameter is less than 15 microns iron powder, and the volumn concentration of iron powder is 10%～40%;
3) under high-purity argon gas atmosphere, with mixed-powder high-energy ball milling 35～50 hours;
4) powder behind the high-energy ball milling is packed in the vacuum furnace, be evacuated to 10
-3～10
-5Pa, feeding purity is 99.999% hydrogen, is heated to 600 ℃-1000 ℃ and inhales hydrogen 5-50 minute, still rests on same temperature range then, being evacuated to hydrogen pressure is 10
-2-10
-4Pa is incubated 5-30 minute, is chilled to room temperature soon;
5) the gained powder by bond, cold pressing, hot pressing or warm deformation come moulding.
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|---|---|---|---|
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|---|---|---|---|
| CN 200310108666 CN1242427C (en) | 2003-11-12 | 2003-11-12 | Method for preparing high-performance biphase rare-earth permanent magnet material using hydrogenation heat treatment process |
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Cited By (1)
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|---|---|---|---|---|
| CN102360702A (en) * | 2011-09-20 | 2012-02-22 | 浙江大学 | Simple and convenient functional magnetic material block and preparation method thereof |
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| JP5063918B2 (en) * | 2006-04-07 | 2012-10-31 | 昭和電工株式会社 | Alloy production equipment |
| CN102543341B (en) * | 2012-01-10 | 2014-11-05 | 福州大学 | Method for preparing anisotropic nanocrystalline rare-earth permanent magnet block material |
| CN102784920A (en) * | 2012-07-19 | 2012-11-21 | 河北工程大学 | Method for preparing rare earth permanent-magnet alloy nanosheet-shaped powder |
| CN105328196B (en) * | 2015-11-02 | 2017-03-22 | 中国核动力研究设计院 | U-Mo alloy powder manufacturing process for controlling nitrogen content |
| CN112342347B (en) * | 2020-10-21 | 2023-12-19 | 江苏大磁纳米材料有限公司 | Hydrogenation heat treatment process for amorphous nano alloy |
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| CN102360702A (en) * | 2011-09-20 | 2012-02-22 | 浙江大学 | Simple and convenient functional magnetic material block and preparation method thereof |
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