CN103060657B - Method for preparing sintered neodymium iron boron permanent magnet material with high coercive force and high corrosion resistance - Google Patents
Method for preparing sintered neodymium iron boron permanent magnet material with high coercive force and high corrosion resistance Download PDFInfo
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Abstract
The invention discloses a method for preparing a sintered neodymium iron boron permanent magnet material with high coercive force and high corrosion resistance, and belongs to the technical field of a magnetic material. The method comprises the steps of adding dysprosium zinc nano powder of which the mean grain size is 1-10 microns to neodymium iron boron powder with the grain size of 3-5 microns and evenly mixing, wherein the adding amount is 0.3-3.0%, and then orienting, pressing and molding in 1.8T magnetic field; putting in a vacuum sintering furnace, then heating and sintering at 1000-1100 DEG C for 3-5 hours, and finally carrying out thermal treatment by two levels, wherein the primary thermal treatment temperature is 850-950 DEG C; the time is 1-3 hours; the secondary thermal treatment temperature is 460-600 DEG C, and the time is 1-3 hours, finally obtaining the sintered neodymium iron boron permanent magnet material with high coercive force and high corrosion resistance. The corrosion resistance of the magnetic body is greatly improved when the coercive force of the magnetic body is obviously improved, and the rare earth content is also reduced.
Description
Technical field
A method of preparing the neodymium-iron-B permanent magnetic material with high-coercive force and high anti-corrosion, belongs to technical field of magnetic materials.
Background technology
NdFeB permanent magnet material developed since the middle and later periods eighties 20th century, the novel material that belongs to national encourage growth, mainly comprise sintering and bonding rare earth permanent magnet material, become each industry of national economy, especially a kind of irreplaceable base mateiral of electronics and automotive industry, it is of a great variety, be widely used in the various fields such as electronics, automobile, computer, electric power, machinery, the energy, environmental protection, national defence, medicine equipment, be again the product of energy-conservation, material-saving and foreign exchange earning, driving the development of every profession and trade.
NdFeB is that rare earth permanent-magnetic material is after occurring, in short decades, obtain swift and violent development, people constantly optimize its chemical constitution, improve manufacturing process technology and equipment, its magnetic property is constantly improved, and Japan now can produce magnetic energy product in batches and reach 400kJ/m
3(50MMGOe) anisotropy sintered ndfeb permanent magnet body, the sintered ndfeb permanent magnet magnetic energy product of experimental study has reached 474kJ/m
3(59.5MMGOe), reached 93% of its theoretical value, from magnetic energy product angle, seen there is no too large room for promotion.
NdFeB based permanent magnetic material principal phase Nd
2fe
14b has very high anisotropy field, and its coercitive theoretical limit is up to 70kOe, but the coercive force of actual magnet is only 1/10th to 1/3rd of theoretical value.Why the coercive force of NdFeB permanent magnet is much smaller than theoretical anisotropy field, is to cause due to its concrete microstructure and defect.The loose synthetic effective demagnetizing field (N in magnetic field in inside that the self-demagnetizing field of the irregularly shaped decision of magnet Hard Magnetic phase crystal grain and intergranule interact and produce
effms) coercive force of magnet is reduced.Crystal grain boundary textural defect is another one influence factor.Textural defect certainly will cause the distortion of magnetic texure parameter, i.e. the crystal anisotropy constant K in grain surface textural defect district, exchange integral A and saturated pole intensity J
s(or saturation magnetization M
s) all can be different from the value of the inner respective amount of crystal grain.They are the nucleation centre of crystal grain reversal magnetization, are again the pinning positions that hinders intercrystalline domain wall displacement, and magnet coercive force is had a significant impact.
Sintered NdFeB magnetic property another one shortcoming is corrosion-resistant, thereby greatly limited it, further applies.The poor feature of sintered NdFeB magnet solidity to corrosion is first with himself crystalline structure with distribute and have close contacting mutually.The same with most metals and alloy, sintered NdFeB alloy is comprised of polycrystal, and its polycrystalline tissue is by principal phase Nd
2fe
14b phase, rich Nd phase and rich B phase Nd
1+ εfe
4b
4three phase composites.With regard to distribution, rich Nd is distributed in principal phase Nd in network-like mode
2fe
14the grain boundary of B or triangle crystal boundary position, form so-called Grain-Boundary Phase, in addition a small amount of rich B with the formal distribution of particle in the crystal boundary position of principal phase.The magnetic of NdFeB magnet is mainly by Hard Magnetic phase Nd
2fe
14b determines; The existence of rich Nd phase can promote the sintering of magneticsubstance, makes magnet densification, while distributing along crystal boundary, can play magnetic coupling buffer action, is conducive to coercitive raising, but can reduces saturation magnetization and remanent magnetism.Another causes the poor reason of sintered NdFeB magnet solidity to corrosion relevant to the chemical characteristic of phase in alloy.Particularly, rich Nd mutually in a large amount of simple substance Nd elements that exist are one of metallic elements that chemically reactive is the highest, poor chemical stability, is easily oxidized.Generally speaking, when magnet is under room temperature and dry environment (<15%RH), its oxidation corrosion process is very slow, and chemical stability is better.But when alloy is in dry high temperature (>250 ℃) or electrochemical environment, will there is obvious corrosion process.Wherein, in the environment of dry high temperature, in alloy, rich Nd meets and first changes Nd into
2o
3, also can progressively there is principal phase Nd subsequently
2fe
14the oxygenolysis of B becomes α-Fe and Nd
2o
3, further oxidation generates Fe
2o
3; And in electrochemical environment, between the three-phase being in contact with one another in alloy structure, exist obvious potential difference.The electrochemical potential of three-phase respectively is rich Nd phase, rich B phase and principal phase Nd from low to high
2fe
14b, so the erosion rate of three-phase is different.The difference of three alternate electrochemical properties has caused galvanic effect, for alloy forms galvanic cell, provides possibility.Rich Nd phase and rich B meet with respect to principal phase Nd
2fe
14b forms anode, preferentially corrodes.This two-phase will be born very large corrosion electric current density as anode metal, rich Nd phase especially wherein, and due to network-like distribution in tissue, corrosion speed is very fast.Its corrosion can cause principal phase Nd
2fe
14b intergranule bonding interface disappears, and occurs crystal grain obscission, finally causes the general corrosion of alloy.As can be seen here, no matter, in which kind of corrosive environment, the corrosion process of sintered Nd Fe B alloy all belongs to selective corrosion with regard to its essence.The prime mover that this process occurs is that in alloy, rich Nd had both had strong chemically reactive mutually, again with principal phase Nd
2fe
14between B, there is obvious potential difference.Meanwhile, because the rich Nd in alloy is network-like being distributed on main phase grain border mutually, make the etch state of NdFeB magnet there is typical intergranular corrosion feature, greatly accelerated the corrosion speed of alloy.Visible, the chemical property of rich Nd phase and distribution thereof are the key factors that determines NdFeB magnet erosion resistance.
Accordingly, the present invention adopts the particle doped preparation of dysprosium Zinc alloy powder to have the sintered NdFeB permanent magnets of high-coercive force and high anti-corrosion concurrently.Compare with the doping of Single Phase Metal powder particle, the present invention utilizes two kinds of elementary composition powdered alloy doping magnets, has fully utilized the characteristic of two kinds of elements, makes the magnetic property of magnet and corrosion resistance nature better.Compare with two alloyages, the present invention has simplified the preparation section of magnet, simultaneously improving magnet microstructure, improve magnet magnetic property, corrosion resistance nature and reducing aspect content of rare earth also makes moderate progress.
Summary of the invention
The present invention is directed to above-mentioned two problems, proposing to adopt the particle doped method of dysprosium Zinc alloy powder to prepare the Sintered NdFeB magnet of high-coercive force and high corrosion resistance, is to improve sintered NdFeB permanent magnets coercive force and corrosion proof method by adding dysprosium Zinc alloy powder particle.
A method of preparing high-coercive force and sintered NdFeB permanent magnetic material with high corrosion resistance, is characterized in that, comprises the following steps:
(1) adopt rapid hardening thin slice technique to prepare neodymium iron boron base rapid hardening thin slice, by the quick-fried method of hydrogen, by alloy sheet fragmentation and by airflow milling, pulverize preparation 3-5 micron neodymium iron boron based raw material powder afterwards;
(2) by dysprosium zinc alloy DyZn or the DyZn of median size 1-10 micron
5powder adds in the neodymium iron boron based powders preparing in step (1), and adding proportion is the 0.3-3.0% of neodymium iron boron based powders weight, and two kinds of powder are mixed;
(3) step (2) is orientated and compression moulding through even mixed powder in the magnetic field of 1.8T, obtains pressed compact;
(4) pressed compact is inserted in vacuum sintering furnace, the temperature that then raises, at 1000-1100 ℃ of sintering 2-4 hour, is finally carried out secondary thermal treatment, and wherein one-level thermal treatment temp is 850 ℃-950 ℃, time 1-3 hour; 460 ℃-600 ℃ of secondary thermal treatment temps, time 1-3 hour; The final sintered Nd-Fe-B magnetic material that obtains.
Compare with the doping of Single Phase Metal powder particle, the present invention utilizes two kinds of elementary composition powdered alloy doping magnets, has fully utilized the characteristic of two kinds of elements, makes the magnetic property of magnet and corrosion resistance nature better.Compare with two alloyages, the present invention has simplified the preparation section of magnet, simultaneously improving magnet microstructure, improve magnet magnetic property, corrosion resistance nature and reducing aspect content of rare earth also makes moderate progress.
The present invention mixes certain dysprosium Zinc alloy powder particle with neodymium iron boron micron particle, make dysprosium Zinc alloy powder uniform particles be scattered in principal phase Nd
2fe
14b grain surface.Add dysprosium Zinc alloy powder and be enriched in rich Nd phase and main phase grain boundary through oversintering and heat treatment process.Low melting point element forms liquid under sintering temperature, improve the wettability of rich Nd phase and principal phase, rich Nd is distributed along crystal boundary mutually more uniformly, crystal boundary is more clear, smooth, strengthen the forming core field on reversal magnetization farmland on intercrystalline degaussing exchange-coupling interaction and crystal boundary, thereby improved the coercive force of magnet.Meanwhile, this method can be introduced one deck dysprosium on the frictional belt of principal phase NdFeB crystal grain, forms DyFeB compound, thereby can improve the coercive force of magnet.First, can reduce like this ratio of DyFeB in sintered NdFeB permanent magnets, thereby reduce the negative impact to magnet remanent magnetism and magnetic energy product, can also realize the object that improves coercive force and improve temperature profile simultaneously.Secondly, the addition of dysprosium can significantly reduce thus, thereby is conducive to reduce the manufacturing cost of material.On the other hand the replacement of these dysprosium zinc intermetallic compounds that add part on crystal boundary rich neodymium Grain-Boundary Phase because this compounds has metastable chemical property, its existence can be played and improve the poor weakness of rich Nd Grain-Boundary Phase solidity to corrosion.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described, but the present invention is not limited to following examples.
Embodiment 1
Utilizing rapid hardening technology is Nd by composition
13.5fe
balal
0.4b
6the alloy of (atomic percentage conc) is prepared as thin slice, adopts subsequently hydrogen fragmentation-gas flow crushing process powder to be made to the powder of 3 microns of median sizes.Afterwards by dysprosium Zinc alloy powder (DyZn weight percent 0.3%, 1 micron of median size
5) add in above-mentioned initial powder, utilize mixer that two kinds of powder are mixed uniformly.To in the magnetic field of 1.8T, be orientated and compression moulding through even mixed powder.Then pressed compact is inserted in high vacuum sintering furnace, be warming up to 1060 ℃ of sintering 3 hours.Carry out afterwards secondary thermal treatment, wherein one-level thermal treatment temp is 950 ℃, time 2 h; 580 ℃ of secondary thermal treatment temps, 1 hour time.Obtain sintered magnet.
To Billy 1
Adopt the technique identical with embodiment 1 to prepare the Nd of the dysprosium Zinc alloy powder particle that do not adulterate
13.5fe
balal
0.4b
6sintered magnet is tested as a comparison.
Utilize BH loop instrument to test the magnetic property of two kinds of magnets, the erosion resistance of simultaneously utilizing autoclave (121 ℃, 0.2MPa, 500h) to test magnet.Every magnetic property and the corrosion resistance nature index of prepared magnet are listed in table 1.
Table 1 embodiment 1 and comparative example 1 magnet magnetic property and corrosion resistance nature contrast
These results suggest that for the identical sintered NdFeB magnet of composition, adopting the present invention to add magnet prepared by dysprosium Zinc alloy powder particle significantly improves than the coercive force of the magnet that do not adulterate, in addition the remanent magnetism of two kinds of magnets and magnetic energy product are suitable, and the erosion resistance of magnet is obviously improved simultaneously.
Embodiment 2
Utilizing rapid hardening technology is Nd by composition
12.5fe
balal
0.5nb
0.2b
6the alloy of (atomic percentage conc) is prepared as thin slice, adopts subsequently hydrogen fragmentation-gas flow crushing process powder to be made to the powder of 5 microns of median sizes.Afterwards dysprosium zinc alloy (DyZn) powder weight percent 1.0%, 3 microns of median sizes is added in above-mentioned initial powder, utilize mixer that two kinds of powder are mixed uniformly.To in the magnetic field of 1.8T, be orientated and compression moulding through even mixed powder.Then pressed compact is inserted in high vacuum sintering furnace, be warming up to 1000 ℃ of sintering 4 hours.Carry out afterwards secondary thermal treatment, wherein one-level thermal treatment temp is 900 ℃, 3 hours time; 460 ℃ of secondary thermal treatment temps, time 2 h.Obtain sintered magnet.
Comparative example 2
Adopt the technique identical with embodiment 2 to prepare the Nd of the dysprosium Zinc alloy powder particle that do not adulterate
12.5fe
balal
0.5nb
0.2b
6sintered magnet is tested as a comparison.
Utilize BH loop instrument to test the magnetic property of two kinds of magnets, the erosion resistance of simultaneously utilizing autoclave (121 ℃, 0.2MPa, 500h) to test magnet.Every magnetic property and the corrosion resistance nature index of prepared magnet are listed in table 2.
Table 2 embodiment 2 and comparative example 2 magnet magnetic properties and corrosion resistance nature contrast
These results suggest that for the identical sintered NdFeB magnet of composition, adopting the present invention to add magnet prepared by dysprosium Zinc alloy powder particle significantly improves than the coercive force of the magnet that do not adulterate, in addition the remanent magnetism of two kinds of magnets and magnetic energy product are suitable, and the erosion resistance of magnet is obviously improved simultaneously.
Embodiment 3
Utilizing rapid hardening technology is Nd by composition
12.5fe
balnb
0.1co
0.3al
0.2b
6the alloy of (atomic percentage conc) is prepared as thin slice, adopts subsequently hydrogen fragmentation-gas flow crushing process powder to be made to the powder of 4 microns of median sizes.Afterwards dysprosium zinc alloy (DyZn) powder weight percent 3.0%, 10 microns of median sizes is added in above-mentioned initial powder, utilize mixer that two kinds of powder are mixed uniformly.To in the magnetic field of 1.8T, be orientated and compression moulding through even mixed powder.Then pressed compact is inserted in high vacuum sintering furnace, be warming up to 1100 ℃ of sintering 2 hours.Carry out afterwards secondary thermal treatment, wherein one-level thermal treatment temp is 900 ℃, 1 hour time; 600 ℃ of secondary thermal treatment temps, time 2 h.Obtain sintered magnet.
Comparative example 3
Adopt the technique identical with embodiment 3 to prepare the Nd of the dysprosium Zinc alloy powder particle that do not adulterate
12.5fe
balnb
0.1co
0.3al
0.2b
6sintered magnet is tested as a comparison.
Utilize BH loop instrument to test the magnetic property of two kinds of magnets, the erosion resistance of simultaneously utilizing autoclave (121 ℃, 0.2MPa, 500h) to test magnet.Every magnetic property and the corrosion resistance nature index of prepared magnet are listed in table 3.
Table 3 embodiment 3 and comparative example 3 magnet magnetic properties and corrosion resistance nature contrast
These results suggest that for the identical sintered NdFeB magnet of composition, adopting the present invention to add magnet prepared by dysprosium Zinc alloy powder particle significantly improves than the coercive force of the magnet that do not adulterate, in addition the remanent magnetism of two kinds of magnets and magnetic energy product are suitable, and the erosion resistance of magnet is obviously improved simultaneously.
Embodiment 4
Utilizing rapid hardening technology is Nd by composition
12.5fe
balal
1.2b
6the alloy of (quality percentage composition) is prepared as thin slice, adopts subsequently hydrogen fragmentation-gas flow crushing process powder to be made to the powder of 3 microns of median sizes.Afterwards by dysprosium zinc alloy (DyZn weight percent 2.0%, 6 microns of median sizes
5) powder adds in above-mentioned initial powder, utilizes mixer that two kinds of powder are mixed uniformly.To in the magnetic field of 1.8T, be orientated and compression moulding through even mixed powder.Then pressed compact is inserted in high vacuum sintering furnace, be warming up to 1050 ℃ of sintering 2 hours, carry out afterwards secondary thermal treatment, wherein one-level thermal treatment temp is 860 ℃, time 2 h; 500 ℃ of secondary thermal treatment temps, time 2 h.Obtain sintered magnet.Prepared magnet
Comparative example 4
Adopt the technique identical with embodiment 4 to prepare the Nd of the dysprosium Zinc alloy powder particle that do not adulterate
12.5fe
balal
1.2b
6sintered magnet is tested as a comparison.
Utilize BH loop instrument to test the magnetic property of two kinds of magnets, the erosion resistance of simultaneously utilizing autoclave (121 ℃, 0.2MPa, 500h) to test magnet.Every magnetic property and the corrosion resistance nature index of prepared magnet are listed in table 4.
Table 4 embodiment 4 and comparative example 4 magnet magnetic properties and corrosion resistance nature contrast
These results suggest that for the identical sintered NdFeB magnet of composition, adopting the present invention to add magnet prepared by dysprosium Zinc alloy powder particle significantly improves than the coercive force of the magnet that do not adulterate, in addition the remanent magnetism of two kinds of magnets and magnetic energy product are suitable, and the erosion resistance of magnet is obviously improved simultaneously.
Embodiment 5
Utilizing rapid hardening technology is Nd by composition
12.5fe
balnb
0.1co
0.3al
0.2b
6the alloy of (atomic percentage conc) is prepared as thin slice, adopts subsequently hydrogen fragmentation-gas flow crushing process powder to be made to the powder of 3 microns of median sizes.Afterwards by dysprosium zinc alloy (DyZn weight percent 1.5%, 5 microns of median sizes
5) powder adds in above-mentioned initial powder, utilizes mixer that two kinds of powder are mixed uniformly.To in the magnetic field of 1.8T, be orientated and compression moulding through even mixed powder.Then pressed compact is inserted in high vacuum sintering furnace, be warming up to 1030 ℃ of sintering 2 hours.Carry out afterwards secondary thermal treatment, wherein one-level thermal treatment temp is 850 ℃, 1 hour time; 540 ℃ of secondary thermal treatment temps, time 2 h.Obtain sintered magnet.
Comparative example 5
Adopt the technique identical with embodiment 5 to prepare the Nd of the dysprosium Zinc alloy powder particle that do not adulterate
12.5fe
balnb
0.1co
0.3al
0.2b
6sintered magnet is tested as a comparison.
Utilize BH loop instrument to test the magnetic property of two kinds of magnets, the erosion resistance of simultaneously utilizing autoclave (121 ℃, 0.2MPa, 500h) to test magnet.Every magnetic property and the corrosion resistance nature index of prepared magnet are listed in table 5.
Table 5 embodiment five and comparative example five magnet magnetic properties and corrosion resistance nature contrast
These results suggest that for the identical sintered NdFeB magnet of composition, adopting the present invention to add magnet prepared by dysprosium Zinc alloy powder particle significantly improves than the coercive force of the magnet that do not adulterate, in addition the remanent magnetism of two kinds of magnets and magnetic energy product are suitable, and the erosion resistance of magnet is obviously improved simultaneously.
Claims (2)
1. a method of preparing high-coercive force and sintered NdFeB permanent magnetic material with high corrosion resistance, is characterized in that, comprises the following steps:
(1) adopt rapid hardening thin slice technique to prepare neodymium iron boron base rapid hardening thin slice, by the quick-fried method of hydrogen, by alloy sheet fragmentation and by airflow milling, pulverize preparation 3-5 micron neodymium iron boron based raw material powder afterwards;
(2) by dysprosium zinc alloy DyZn or the DyZn of median size 1-10 micron
5powder adds in the neodymium iron boron based powders preparing in step (1), and adding proportion is the 0.3-3.0% of neodymium iron boron based powders weight, and two kinds of powder are mixed;
(3) step (2) is orientated and compression moulding through even mixed powder in the magnetic field of 1.8T, obtains pressed compact;
(4) pressed compact is inserted in vacuum sintering furnace, the temperature that then raises, at 1000-1100 ℃ of sintering 2-4 hour, is finally carried out secondary thermal treatment, and wherein one-level thermal treatment temp is 850 ℃-950 ℃, time 1-3 hour; 460 ℃-600 ℃ of secondary thermal treatment temps, time 1-3 hour; The final sintered Nd-Fe-B magnetic material that obtains.
2. according to the method for claim 1 prepared a kind of high-coercive force and sintered NdFeB permanent magnetic material with high corrosion resistance.
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| CN103506624B (en) * | 2012-06-20 | 2015-12-02 | 中磁科技股份有限公司 | The sintering method of neodymium iron boron magnetic body |
| WO2016086397A1 (en) * | 2014-12-04 | 2016-06-09 | 浙江大学 | Method for improving coercive force of sintered neodymium iron boron magnet by adding dysprosium hydrogen compound and product |
| CN108417379B (en) * | 2018-03-30 | 2019-07-30 | 严高林 | A kind of neodymium iron boron magnetic body and preparation method thereof of the nickel alloy of dysprosium containing low melting point |
| CN108987018A (en) * | 2018-08-01 | 2018-12-11 | 宁波科升磁业有限公司 | A method of preparing high-coercive force and high-corrosion resistance Sintered NdFeB magnet |
| CN111243846B (en) * | 2020-01-19 | 2021-12-24 | 北京工业大学 | Method capable of simultaneously improving oxidation corrosion resistance of NdFeB powder and magnet |
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| CN101026034A (en) * | 2006-02-22 | 2007-08-29 | 南京理工大学 | Method for preparing corrosion resistance rare earth permanent-magnetic material |
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Application publication date: 20130424 Assignee: Jiangsu koppes Magnetic Industry Co Ltd Assignor: Beijing University of Technology Contract record no.: 2015990000150 Denomination of invention: Method for preparing sintered neodymium iron boron permanent magnet material with high coercive force and high corrosion resistance Granted publication date: 20141126 License type: Exclusive License Record date: 20150331 |
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