CN101241789A - A lanthanon permanent magnetic powder and its making method - Google Patents
A lanthanon permanent magnetic powder and its making method Download PDFInfo
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Abstract
The present invention provides a rare-earth permanent-magnetic powder and the preparing method thereof. The basic representation of the rare-earth permanent-magnetic powder is as follows: (R<1-a>La<a>)uFe<100-u-x-y>MxBy, wherein R is Nd, Pr or NdPr or the mixed rare earth metal alloy which is mainly La, Ce and Nd. La is metal lanthanum element. Fe is metal iron element. M is metal Zr, Hf, Nb, V or the alloy. B is boron element. The rare-earth permanent-magnetic powder of the invention can be prepared with arc remelting fast quenching method or induction remelting fast quenching method. Under the condition that the Nd content is reduced greatly, the invention keeps higher synthetic magnetic character and has better temperature stability. After the 150 DEG C high temperature aging experiment, the irreversible flux loss is only 3to 5 The performance-price ratio of the rare-earth permanent-magnetic powder of the invention is higher and the invention has better market applying prospect.
Description
Technical field
The invention belongs to the magnetic material preparing technical field, be specifically related to a kind of lanthanon permanent magnetic powder and preparation method thereof.
Background technology
The NdFeB permanent magnetic material is a present magnetic property magnetic material preferably.The NdFeB permanent magnetic material is divided into sintered ndfeb permanent magnet material and two kinds of bonding NdFeB permanent magnetic materials.Bonding NdFeB permanent magnetic material can be made into various thin-walleds, abnormal shape and many pole magnet owing to have good moulding and multipole magnetized characteristic.Be mainly used in fields such as motor.
Bonding NdFeB permanent magnetic material is formed by NdFeB permanent magnetic powder bonding, and the NdFeB permanent magnetic powder adopts quick-quenching method to generate.NdFeB permanent magnetic powder microstructure is made of nanocrystal, and main crystalline phase is Nd
2Fe
14B phase or Nd
2Fe
14B/ α-Fe, Nd
2Fe
14B/Fe
3The B two-phase is compound.
At present, adopting quick-quenching method to produce the higher company of NdFeB permanent magnetic powder level in the world is american wheat lattice elder brother magnetic company, and the said firm mainly adopts quick-quenching method to produce the NdFeB permanent magnetic powder and has multinomial corresponding patented technology.The said firm's invention and created name discloses a kind of Nd for the patent documentation (patent No. is 00813322.0) of " Rare earth permanent-magnet material and its preparation method "
2Fe
14The B lanthanon permanent magnetic powder, wherein the atom percentage content of rare earth element such as Nd, Pr is 10%～40%, the atom percentage content of B is 0.5%～10%, and atom percentage contents such as Fe, Co are 50%～90%, and atomic percents such as other interpolation metallic Z r are 0.01%～1%.The rare earth metal Nd that adopts in this patented technology costs an arm and a leg, and the price of lanthanon permanent magnetic powder is increased, and range of application is restricted.The metallic Z r content of preparing burden simultaneously in the composition is low, adopts the coercive force of the lanthanon permanent magnetic powder that electric arc remelting fast quenching produces relatively poor.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of lanthanon permanent magnetic powder and preparation method thereof.
Lanthanon permanent magnetic powder of the present invention comprises following content:
A kind of lanthanon permanent magnetic powder, it forms expression formula is (R
1-aLa
a)
uFe
100-u-x-yM
xB
y, R is metal Nd, metal Pr, NdPr alloy or based on the misch metal alloy of La, Ce, Nd in the formula; La is the lanthanoid metal element; Fe is the metallic iron element; M is one or more among metallic Z r, Hf, Nb, the V; B is a boron element; Each constituent content is respectively 0.05≤a≤0.7,8≤u≤14,1≤x≤5,3≤y≤10 in the lanthanon permanent magnetic powder.
Lanthanon permanent magnetic powder also comprises 0.05%wt～4%wt metal Co.
Lanthanon permanent magnetic powder of the present invention can adopt electric arc remelting quick-quenching method or the preparation of inducting remolten quick-quenching method.
Electric arc remelting fast quenching preparation method comprises following content:
Alloy pig after the melting is broken into the fritter of 5mm～10mm, is alloy liquid with the electric arc remelting in copper crucible, and the running roller that the alloy hydrorrhea flow to high speed rotating is rapidly solidificated into strip, is ground into powder.
Inducting remolten fast quenching preparation method comprises following content:
Alloy cast ingot after the melting is at Al
2O
3Be alloy liquid through the induction heating remelting in the crucible, alloy liquid is rapidly solidificated into strip by the nozzle spray to the running roller of high speed rotating.Because inducting remolten rapid quenching technique temperature is even, stability of flow can obtain high-quality fast quenching thin strap, is ground into powder.
Because neodymium metal and metal praseodymium neodymium price height, the price of the bonding lanthanon permanent magnetic powder of fast quenching is also high, in order to make full use of the rare earth resources of China's abundant, reduce the bonding lanthanon permanent magnetic powder cost of fast quenching, the present invention adopts cheap metal La or based on the alternative wherein expensive metal Nd of the norium of La, Ce, Nd, has prepared the bonding lanthanon permanent magnetic powder of fast quenching of high performance-price ratio.
The present invention adopts the cheap metal La of high-load or substitutes higher metal Nd, Pr or the Nd Pr alloy of price based on the norium of La, Ce, Nd, to reduce production costs; Add Zr, Hf, V or its alloy of high level simultaneously, increase the stability of rapid quenching technique, improve the magnetic coercive force, make the magnetic property of magnetic can reach 8MGOe～13MGOe, HCJ can reach 7kOe～10kOe, and its irreversible flux loss is 3%～3.5%.Can add 0.05%～4% metal Co of total weight in the material, to improve the Curie temperature of permanent magnetic powder.
Lanthanon permanent magnetic powder of the present invention can adopt electric arc remelting quick-quenching method or the preparation of inducting remolten quick-quenching method, under the condition that Nd content declines to a great extent, kept higher comprehensive magnetic characteristic, also has temperature stability preferably, through 150 ℃ of high-temperature circulation tests, its irreversible flux loss only is 3%～3.5%.Lanthanon permanent magnetic powder cost performance of the present invention is higher, and better market application is arranged.
Description of drawings
Fig. 1 is the (Nd among the embodiment 1 of a kind of lanthanon permanent magnetic powder of the present invention and preparation method thereof
0.49La
0.51)
12.7Fe
76.4B
7.7Zr
3.2Electric arc fast quenching magnet performance curve synoptic diagram
Fig. 2 is the (Nd among the embodiment 2 of a kind of lanthanon permanent magnetic powder of the present invention and preparation method thereof
0.49La
0.51)
12.7Fe
76.4B
7.7Zr
3.2Induction fast quenching magnet performance curve synoptic diagram
Fig. 3 is the (Nd among the embodiment 3 of a kind of lanthanon permanent magnetic powder of the present invention and preparation method thereof
0.61La
0.39)
11.6Fe
77.6B
7.6Zr
3.2The magnet performance curve synoptic diagram
Fig. 4 is the (Nd among the embodiment 4 of a kind of lanthanon permanent magnetic powder of the present invention and preparation method thereof
0.73La
0.27)
10.1Fe
79.3B
7.5Zr
3.1The magnet performance curve synoptic diagram
Fig. 5 is the (Nd among the embodiment 5 of a kind of lanthanon permanent magnetic powder of the present invention and preparation method thereof
0.87La
0.13)
10.0Fe
79.4B
7.5Zr
3.1The magnet performance curve synoptic diagram
Fig. 6 is the (Nd among the embodiment 6 of a kind of lanthanon permanent magnetic powder of the present invention and preparation method thereof
0.87La
0.13)
9.93Fe
82.46B
6.59Zr
1.02The magnet performance curve synoptic diagram
Fig. 7 is the (Nd among the embodiment 7 of a kind of lanthanon permanent magnetic powder of the present invention and preparation method thereof
0.86La
0.14)
10.15Fe
78.61B
6.73Zr
4.51The magnet performance curve synoptic diagram
Fig. 8 is the (Nd among the embodiment 8 of a kind of lanthanon permanent magnetic powder of the present invention and preparation method thereof
0.7La
0.3)
10.5Fe
81.845B
6.63Zr
1.025The magnet performance curve synoptic diagram
Fig. 9 is the (Nd among the embodiment 9 of a kind of lanthanon permanent magnetic powder of the present invention and preparation method thereof
0.83La
0.17)
10.92Fe
82.87B
3.0Zr
3.21The magnet performance curve synoptic diagram
Figure 10 is the (Nd among the embodiment 10 of a kind of lanthanon permanent magnetic powder of the present invention and preparation method thereof
0.83La
0.17)
10.41Fe
77.93B
8.6Zr
3.06The magnet performance curve synoptic diagram
Figure 11 is the (Nd among the embodiment 11 of a kind of lanthanon permanent magnetic powder of the present invention and preparation method thereof
0.76La
0.24)
13.86Fe
76.16B
6.72Zr
3.26The magnet performance curve synoptic diagram
Figure 12 is the (Nd among the embodiment 12 of a kind of lanthanon permanent magnetic powder of the present invention and preparation method thereof
0.8La
0.2)
10.1Fe
76.37B
6.42Zr
3.11Co
4The magnet performance curve synoptic diagram
Embodiment
The invention will be further described below in conjunction with accompanying drawing.
Lanthanon permanent magnetic powder of the present invention adopts electric arc remelting fast quenching or two kinds of method preparations of inducting remolten fast quenching.
The preparation of embodiment 1 electric arc remelting quick-quenching method
The used metal batching of present embodiment composition is: (Nd
0.49La
0.51)
12.7Fe
76.4B
7.7Zr
3.2
Each element gross mass percentage of simple metal and mishmetal is in the batching: Nd:13.95wt% La:13.92wt% Fe:66.31wt% B:1.29wt% Zr:4.53wt%, and electric arc remelting quick-quenching method preparation process is as follows:
(1) alloy melting is with broken
Above-mentioned raw material are prepared back founding in vacuum induction melting furnace by the batching composition become alloy pig.Alloy pig jaw crusher after the melting is broken into＜alloying pellet of 10mm.
(2) fast quenching powder process
With the alloying pellet of the fragmentation vacuum arc quick quenching furnace of packing into, vacuumize.After vacuum is lower than 10Pa, fills Ar gas and arrive-0.04MPa～0.2MPa, start the electric arc fast quenching, the running roller linear velocity adopts 15m/s～32m/s; The fast quenching thin strap that makes is crushed to below the 200 μ m with ball mill.
(3) crystallization
The fast quenching permanent magnetism powder that obtains is carried out crystallization and thermal treatment with crystallization furnace, and temperature is 640 ℃～740 ℃, and the time is 5 minutes～40 minutes, can obtain the permanent magnetic powder finished product.
(4) sample preparation is measured
The metal permanent magnetic powder is added 2%～2.5% binding agent, with press be pressed into the high 10mm of diameter 10mm, density (ρ) is 6.0g/m
3Bonded permanent magnet, measure magnetic property with magnetic determining device.
After tested, the fast quenching magnet performance is:
B
r：570.38mT?H
cj：577.03kA/m?(BH)
max：52.559kJ/m
3?H
k：194.90kA/m
Test curve is seen Fig. 1
The preparation of embodiment 2 inducting remolten quick-quenching methods
The used metal batching of present embodiment composition is: (Nd
0.49La
0.51)
12.7Fe
76.4B
7.7Zr
3.2
Each element gross mass percentage of simple metal and mishmetal is in the batching: Nd:13.95wt% La:13.92wt% Fe:66.31wt% B:1.29wt% Zr:4.53wt%, adopt the inducting remolten rapid quenching technique to make and comprise the steps:
(1) alloy melting
Above-mentioned raw material are prepared back founding in vacuum induction melting furnace by the batching composition become alloy pig.
(2) fast quenching powder process
With the vacuum induction quick quenching furnace of packing into of the alloy pig after the founding, vacuumize, vacuum is below 10Pa, start intermediate frequency and high frequency melting bag, after treating the alloy pig melting, charge into Ar gas to-0.04MPa～0.2MPa, the molten metal after the melting flows to fast quenching on the high speed rotating running roller by nozzle, and the running roller linear velocity adopts 15m/s～32m/s; The fast quenching thin strap that obtains is crushed to below the 200 μ m with ball mill.
(3) crystallization
The fast quenching that obtains is carried out crystallization and thermal treatment with magnetic with crystallization furnace, and temperature is 640 ℃～740 ℃, and the time is 5 minutes～40 minutes, can obtain the finished product permanent magnetic powder.
(4) sample preparation is measured
The metal permanent magnetic powder is added 2%～2.5% binding agent, with press be pressed into the high 10mm of diameter 10mm, density (ρ) is 6.0g/m
3Bonded permanent magnet, measure magnetic property with magnetic determining device.
After tested, the fast quenching magnet performance is:
B
r：640.38mT?H
cj：666.16kA/m?(BH)
max：67.633kJ/m
3?H
k：220.02kA/m
Test curve is seen Fig. 2
The preparation of embodiment 3 electric arc remelting quick-quenching methods
The used metal batching of present embodiment composition is: (Nd
0.61La
0.39)
11.6Fe
77.6B
7.6Zr
3.2
Each element gross mass percentage of simple metal and mishmetal is in the batching: Nd:16.05wt% La:9.89wt% Fe:68.18wt% B:1.29wt% Zr:4.59wt%, implementation process such as embodiment 1.
After tested, the fast quenching magnet performance is:
B
r：597.10mT?H
cj：707.17kA/m?(BH)
max：57.761kJ/m
3?H
k：206.79kA/m
Test curve is seen Fig. 3
The preparation of embodiment 4 electric arc remelting quick-quenching methods
The used metal batching of present embodiment composition is: (Nd
0.73La
0.27)
10.1Fe
79.3B
7.5Zr
3.1
Each element gross mass percentage of simple metal and mishmetal is in the batching: Nd:17.06wt% La:6.07wt% Fe:71.03wt% B:1.30wt% Zr:4.54wt%, implementation process such as embodiment 1.
After tested, the fast quenching magnet performance is:
B
r：595.82mT?Hc
j：688.21kA/m?(BH)
max：58.053kJ/m
3?H
k：218.09kA/m
Test curve is seen Fig. 4
The preparation of embodiment 5 electric arc remelting quick-quenching methods
The used metal batching of present embodiment composition is: (Nd
0.87La
0.13)
10.0Fe
79.4B
7.5Zr
3.1
Each element gross mass percentage of simple metal and mishmetal is in the batching: Nd:20.13wt% La:2.9wt% Fe:71.14wt% B:1.3wt% Zr:4.53wt%, implementation process such as embodiment 1.
After tested, the fast quenching magnet performance is:
B
r：640.76mT?H
cj：754.90kA/m?(BH)
max：67.564kJ/m
3?H
k：241.88kA/m
Test curve is seen Fig. 5
The preparation of embodiment 6 inducting remolten quick-quenching methods
The used metal batching of present embodiment composition is: (Nd
0.87La
0.13)
9.93Fe
82.46B
6.59Zr
1.02
Each element gross mass percentage of simple metal and mishmetal is in the batching: Nd:20.11wt% La:2.9wt% Fe:74.34wt% B:1.15wt% Zr:1.5wt%, implementation process such as embodiment 2.
After tested, the fast quenching magnet performance is:
B
r：663.38mT?H
cj：835.82kA/m?(BH)
max：73.670kJ/m
3?H
k：279.06kA/m
Test curve is seen Fig. 6
The preparation of embodiment 7 electric arc remelting quick-quenching methods
The used metal batching of present embodiment composition is: (Nd
0.86La
0.14)
10.15Fe
78.61B
6.73Zr
4.51
Each element gross mass percentage of simple metal and mishmetal is in the batching: Nd:19.89wt% La:3.11wt% Fe:69.35wt% B:1.15wt% Zr:6.5wt%, implementation process such as embodiment 1.
After tested, the fast quenching magnet performance is:
B
r：646.34mT?H
cj：701.55kA/m?(BH)
max：69.252kJ/m
3?H
k：254.78kA/m
Test curve is seen Fig. 7
The preparation of embodiment 8 inducting remolten quick-quenching methods
The used metal batching of present embodiment composition is: (Nd
0.7La
0.3)
10.5Fe
81.845B
6.63Zr
1.025
Each element gross mass percentage of simple metal and mishmetal is in the batching: Nd:17.06wt% La:7.04wt% Fe:73.25wt% B:1.15wt% Zr:1.5wt%, implementation process such as embodiment 2.
After tested, the fast quenching magnet performance is:
B
r：643.51mT?H
cj：675.78kA/m?(BH)
max：66.894kJ/m
3?H
k：219.50kA/m
Test curve is seen Fig. 8
The preparation of embodiment 9 electric arc remelting quick-quenching methods
The used metal batching of present embodiment composition is: (Nd
0.83La
0.17)
10.92Fe
82.87B
3.0Zr
3.21
Each element gross mass percentage of simple metal and mishmetal is in the batching: Nd:20wt% La:4wt% Fe:71wt% B:0.5wt% Zr:4.5wt%, implementation process such as embodiment 1.
After tested, the fast quenching magnet performance is:
B
r：623.36mT?H
cj：697.34kA/m?(BH)
max：62.482kJ/m
3?H
k：208.08kA/m
Test curve is seen Fig. 9
The preparation of embodiment 10 electric arc remelting quick-quenching methods
The used metal batching of present embodiment composition is: (Nd
0.83La
0.17)
10.41Fe
77.93B
8.6Zr
3.06
Each element gross mass percentage of simple metal and mishmetal is in the batching: Nd:20wt% La:4wt% Fe:70wt% B:1.5wt% Zr:4.5wt%, implementation process such as embodiment 1.
After tested, the fast quenching magnet performance is:
B
r：651.50mT?H
cj：740.90kA/m?(BH)
max：70.709kJ/m
3?H
k：265.79kA/m
Test curve is seen Figure 10
The preparation of embodiment 11 electric arc remelting quick-quenching methods
The used metal batching of present embodiment composition is: (Nd
0.76La
0.24)
13.86Fe
76.16B
6.72Zr
3.26
Each element gross mass percentage of simple metal and mishmetal is in the batching: Nd:23wt% La:7wt% Fe:64.4wt% B:1.1wt% Zr:4.5wt%, implementation process such as embodiment 1.
After tested, the fast quenching magnet performance is:
B
r：644.96mT?H
cj：669.69kA/m?(BH)
max：67.712kJ/m
3?H
k：228.54kA/m，
Test curve is seen Figure 11
The preparation of embodiment 12 electric arc remelting quick-quenching methods
The used metal batching of present embodiment composition is: (Nd
0.8La
0.2)
10.1Fe
76.37B
6.42Zr
3.11Co
4
Each element gross mass percentage of simple metal and mishmetal is in the batching: Nd:18.5wt% La:4.5wt% Fe:67.7wt%B:1.1wt% Zr:4.5wt% Co:3.7wt%, implementation process such as embodiment 1.
After tested, the fast quenching magnet performance is:
B
r：645.46mT?H
cj：735.23kA/m?(BH)
max：68.373kJ/m
3?H
k：239.28kA/m
Test curve is seen Figure 12
It is the feedstock production lanthanon permanent magnetic powder that above embodiment of the present invention all adopts the commercially available norium based on La, Ce, Nd.The contained composition of norium is: La:1-35wt%, and Ce:1-40wt%,, Pr:1-10wt%, Nd:5-50wt%, other compositions are: 1%～10%.
Lanthanon permanent magnetic powder of the present invention also can adopt other quick setting method preparation.
Claims (4)
1. lanthanon permanent magnetic powder is characterized in that: it is formed expression formula and is (R
1-aLa
a)
uFe
100-u-x-yM
xB
y, R is metal Nd, metal Pr, NdPr alloy or based on the misch metal alloy of La, Ce, Nd in the formula; La is the lanthanoid metal element; Fe is the metallic iron element; M is one or more among metallic Z r, Hf, Nb, the V; B is a boron element; Each constituent content is respectively 0.05≤a≤0.7,8≤u≤14,1≤x≤5,3≤y≤10 in the lanthanon permanent magnetic powder.
2. lanthanon permanent magnetic powder according to claim 1 is characterized in that: described lanthanon permanent magnetic powder also comprises 0.05%wt～4%wt metal Co.
3. the preparation method of lanthanon permanent magnetic powder according to claim 1 is characterized in that comprising following content:
Rare earth alloy ingot after the melting is broken into the fritter of 5mm～10mm, is alloy liquid with the electric arc remelting in copper crucible, and the running roller that the alloy hydrorrhea is flow to high speed rotating is rapidly solidificated into strip, is ground into powder.
4. the preparation method of lanthanon permanent magnetic powder according to claim 1 is characterized in that comprising following content:
Rare earth alloy ingot casting after the melting is at Al
2O
3Be alloy liquid through the induction heating remelting in the crucible, alloy liquid is rapidly solidificated into strip by the nozzle spray to the running roller of high speed rotating, be ground into powder.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102856029A (en) * | 2012-04-20 | 2013-01-02 | 漯河市三鑫稀土永磁材料有限责任公司 | High (BH)max quick quenching magnetic powder and preparation method thereof |
| CN102969112A (en) * | 2012-12-05 | 2013-03-13 | 麦格昆磁（天津）有限公司 | Rare-earth permanent magnetic powder, preparation method of rare-earth permanent magnetic powder and magnet and magnetic device prepared from rare-earth permanent magnetic powder |
| CN105810380A (en) * | 2016-03-11 | 2016-07-27 | 江西江钨稀有金属新材料有限公司 | High-temperature resistant and high-magnetism rear earth permanent magnetic material and preparation method thereof |
| CN106024244A (en) * | 2016-07-21 | 2016-10-12 | 江西理工大学 | High-heat-stability nanocrystal rare-earth permanent-magnet material and preparation method thereof |
| CN108015268A (en) * | 2016-10-28 | 2018-05-11 | 龙岩紫荆创新研究院 | The bonded permanent magnet that a kind of R-B-Ti-Fe alloy powders and preparation method thereof are prepared with the alloy powder |
| CN108133797A (en) * | 2017-12-18 | 2018-06-08 | 北京工业大学 | A kind of inhibition CeFe2The preparation method of the mischmetal iron boron magnet of phase |
| CN111390187A (en) * | 2020-03-12 | 2020-07-10 | 江苏巨鑫磁业有限公司 | Preparation method of permanent magnet powder by applying double-sided wet-warm oxidation treatment |
-
2007
- 2007-11-07 CN CNA2007100504569A patent/CN101241789A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102856029A (en) * | 2012-04-20 | 2013-01-02 | 漯河市三鑫稀土永磁材料有限责任公司 | High (BH)max quick quenching magnetic powder and preparation method thereof |
| CN102969112A (en) * | 2012-12-05 | 2013-03-13 | 麦格昆磁（天津）有限公司 | Rare-earth permanent magnetic powder, preparation method of rare-earth permanent magnetic powder and magnet and magnetic device prepared from rare-earth permanent magnetic powder |
| CN102969112B (en) * | 2012-12-05 | 2016-04-27 | 麦格昆磁（天津）有限公司 | Rare earth permanent magnet powder and preparation method thereof and magnet prepared therefrom and magnetic device |
| CN105810380A (en) * | 2016-03-11 | 2016-07-27 | 江西江钨稀有金属新材料有限公司 | High-temperature resistant and high-magnetism rear earth permanent magnetic material and preparation method thereof |
| CN106024244A (en) * | 2016-07-21 | 2016-10-12 | 江西理工大学 | High-heat-stability nanocrystal rare-earth permanent-magnet material and preparation method thereof |
| CN108015268A (en) * | 2016-10-28 | 2018-05-11 | 龙岩紫荆创新研究院 | The bonded permanent magnet that a kind of R-B-Ti-Fe alloy powders and preparation method thereof are prepared with the alloy powder |
| CN108133797A (en) * | 2017-12-18 | 2018-06-08 | 北京工业大学 | A kind of inhibition CeFe2The preparation method of the mischmetal iron boron magnet of phase |
| CN111390187A (en) * | 2020-03-12 | 2020-07-10 | 江苏巨鑫磁业有限公司 | Preparation method of permanent magnet powder by applying double-sided wet-warm oxidation treatment |
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