CN103060657A - 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 kind of method for preparing neodymium-iron with high-coercive force and high anti-corrosion-B permanent magnetic material belongs to technical field of magnetic materials.
Background technology
The 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, obtain swift and violent development in short decades, people constantly optimize its chemical constitution, improve manufacturing process technology and equipment, its magnetic property constantly is improved, and Japan now can produce magnetic energy product in batches and reach 400kJ/m
3Anisotropy sintered ndfeb permanent magnet body (50MMGOe), the sintered ndfeb permanent magnet magnetic energy product of experimental study has reached 474kJ/m
3(59.5MMGOe), reached 93% of its theoretical value, seen there is not too large room for promotion from the magnetic energy product angle.
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 only is 1/10th to 1/3rd of theoretical value.Why the coercive force of NdFeB permanent magnet is because its concrete microstructure and defective cause much smaller than theoretical anisotropy field.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.The crystal grain boundary textural defect is the 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 the intercrystalline domain wall displacement, and the magnet coercive force is had a significant impact.
Sintered NdFeB magnetic property another one shortcoming is corrosion-resistant, thereby has greatly limited its further application.The poor characteristics of sintered NdFeB magnet solidity to corrosion are at first with himself crystalline structure with distribute mutually close contacting arranged.The same with most metals and alloy, sintered NdFeB alloy is comprised of polycrystal, and its polycrystalline tissue is by principal phase Nd
2Fe
14The B phase, rich Nd phase and rich B be Nd mutually
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 the magnet densification, when distributing along crystal boundary, can play the 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 then relevant with the chemical characteristic of phase in the alloy.Particularly, rich Nd mutually in a large amount of simple substance Nd elements that exist are one of the highest metallic elements of chemically reactive, oxidation more easily occurs in poor chemical stability.Generally speaking, when magnet be in room temperature and dry environment (＜15%RH) under, its oxidation corrosion process is very slow, chemical stability is better.But be in 250 ℃ of dry high temperature (〉 when alloy) or electrochemical environment in, obvious corrosion process will occur.Wherein in the environment of dry high temperature, rich Nd meets and at first changes Nd in the alloy
2O
3, also principal phase Nd can progressively occur subsequently
2Fe
14The oxygenolysis of B becomes α-Fe and Nd
2O
3, further oxidation generates Fe
2O
3And in electrochemical environment, exist obvious potential difference between the three-phase that is in contact with one another in the alloy structure.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, provides possibility for alloy forms galvanic cell.Rich Nd phase and rich B meet with respect to principal phase Nd
2Fe
14B forms anode, preferential corrosion.This two-phase will be born very large corrosion electric current density as anode metal, rich Nd phase especially wherein, because network-like distribution in tissue, corrosion speed is very fast.Its corrosion can cause principal phase Nd
2Fe
14B intergranule bonding interface disappears, and the crystal grain obscission occurs, finally causes the general corrosion of alloy.This shows that 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 rich Nd had both had strong chemically reactive mutually in the alloy, again with principal phase Nd
2Fe
14Obvious potential difference is arranged between the B.Meanwhile, because the rich Nd in the alloy is network-like being distributed on the main phase grain border mutually, so that the etch state of NdFeB magnet has typical intergranular corrosion feature, greatly accelerated the corrosion speed of alloy.As seen, 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 improve the magnet microstructure, improve the magnet magnetic property, corrosion resistance nature and reducing also makes moderate progress aspect the content of rare earth.
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 kind of method for preparing high-coercive force and sintered NdFeB permanent magnetic material with high corrosion resistance is characterized in that, may further comprise the steps:
(1) adopts rapid hardening thin slice technique to prepare neodymium iron boron base rapid hardening thin slice, pulverize preparation 3-5 micron neodymium iron boron based raw material powder with the quick-fried method of hydrogen with the alloy sheet fragmentation and by airflow milling afterwards;
(2) with dysprosium zinc alloy DyZn or the DyZn of median size 1-10 micron
5Powder adds in the neodymium iron boron based powders for preparing in the 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 in the magnetic field of 1.8T and compression moulding through even mixed powder, obtains pressed compact;
(4) pressed compact is inserted in the vacuum sintering furnace, the temperature that then raises was carried out secondary thermal treatment at last at 1000-1100 ℃ of sintering 2-4 hour, and wherein the 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 improve the magnet microstructure, improve the magnet magnetic property, corrosion resistance nature and reducing also makes moderate progress aspect the content of rare earth.
The present invention mixes certain dysprosium Zinc alloy powder particle with the neodymium iron boron micron particle, so that dysprosium Zinc alloy powder uniform particles is scattered in principal phase Nd
2Fe
14The B grain surface.Add the 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, make that rich Nd is more uniform mutually to distribute along crystal boundary, crystal boundary is more clear, smooth, strengthen the forming core field on reversal magnetization farmland on intercrystalline degaussing exchange-coupling interaction and the crystal boundary, thereby improved the coercive force of magnet.Simultaneously, this method can be introduced one deck dysprosium in the frictional belt of principal phase NdFeB crystal grain, forms the DyFeB compound, thereby can improve the coercive force of magnet.At 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, the purpose that can also realize improving 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
The present invention is further described below in conjunction with specific embodiment, but the present invention is not limited to following examples.
Embodiment 1
Utilize the rapid hardening technology that composition is Nd
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 the powder of 3 microns of median sizes.Afterwards with dysprosium Zinc alloy powder (DyZn weight percent 0.3%, 1 micron of median size
5) add in the 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 the high vacuum sintering furnace, be warming up to 1060 ℃ of sintering 3 hours.Carry out afterwards secondary thermal treatment, wherein the one-level thermal treatment temp is 950 ℃, time 2 h; 580 ℃ of secondary thermal treatment temps, 1 hour time.Namely 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 mix
13.5Fe
BalAl
0.4B
6Sintered magnet is tested as a comparison.
Utilize the BH loop instrument to test the magnetic property of two kinds of magnets, the erosion resistance of utilizing simultaneously autoclave (121 ℃, 0.2MPa, 500h) to test magnet.Every magnetic property and the corrosion resistance nature index of prepared magnet are listed in the table 1.
Table 1 embodiment 1 and Comparative Examples 1 magnet magnetic property and corrosion resistance nature contrast
Above presentation of results is for the identical sintered NdFeB magnet of composition, adopt magnet that the present invention adds the preparation of dysprosium Zinc alloy powder particle to significantly improve than the coercive force of the magnet that do not mix, the remanent magnetism of two kinds of magnets and magnetic energy product are suitable in addition, and the erosion resistance of magnet is obviously improved simultaneously.
Embodiment 2
Utilize the rapid hardening technology that composition is Nd
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 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 the 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 the high vacuum sintering furnace, be warming up to 1000 ℃ of sintering 4 hours.Carry out afterwards secondary thermal treatment, wherein the one-level thermal treatment temp is 900 ℃, 3 hours time; 460 ℃ of secondary thermal treatment temps, time 2 h.Namely obtain sintered magnet.
Comparative Examples 2
Adopt the technique identical with embodiment 2 to prepare the Nd of the dysprosium Zinc alloy powder particle that do not mix
12.5Fe
BalAl
0.5Nb
0.2B
6Sintered magnet is tested as a comparison.
Utilize the BH loop instrument to test the magnetic property of two kinds of magnets, the erosion resistance of utilizing simultaneously autoclave (121 ℃, 0.2MPa, 500h) to test magnet.Every magnetic property and the corrosion resistance nature index of prepared magnet are listed in the table 2.
Table 2 embodiment 2 and Comparative Examples 2 magnet magnetic properties and corrosion resistance nature contrast
Above presentation of results is for the identical sintered NdFeB magnet of composition, adopt magnet that the present invention adds the preparation of dysprosium Zinc alloy powder particle to significantly improve than the coercive force of the magnet that do not mix, the remanent magnetism of two kinds of magnets and magnetic energy product are suitable in addition, and the erosion resistance of magnet is obviously improved simultaneously.
Embodiment 3
Utilize the rapid hardening technology that composition is Nd
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 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 the 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 the high vacuum sintering furnace, be warming up to 1100 ℃ of sintering 2 hours.Carry out afterwards secondary thermal treatment, wherein the one-level thermal treatment temp is 900 ℃, 1 hour time; 600 ℃ of secondary thermal treatment temps, time 2 h.Namely obtain sintered magnet.
Comparative Examples 3
Adopt the technique identical with embodiment 3 to prepare the Nd of the dysprosium Zinc alloy powder particle that do not mix
12.5Fe
BalNb
0.1Co
0.3Al
0.2B
6Sintered magnet is tested as a comparison.
Utilize the BH loop instrument to test the magnetic property of two kinds of magnets, the erosion resistance of utilizing simultaneously autoclave (121 ℃, 0.2MPa, 500h) to test magnet.Every magnetic property and the corrosion resistance nature index of prepared magnet are listed in the table 3.
Table 3 embodiment 3 and Comparative Examples 3 magnet magnetic properties and corrosion resistance nature contrast
Above presentation of results is for the identical sintered NdFeB magnet of composition, adopt magnet that the present invention adds the preparation of dysprosium Zinc alloy powder particle to significantly improve than the coercive force of the magnet that do not mix, the remanent magnetism of two kinds of magnets and magnetic energy product are suitable in addition, and the erosion resistance of magnet is obviously improved simultaneously.
Embodiment 4
Utilize the rapid hardening technology that composition is Nd
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 the powder of 3 microns of median sizes.Afterwards with dysprosium zinc alloy (DyZn weight percent 2.0%, 6 microns of median sizes
5) powder adds in the 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 the high vacuum sintering furnace, be warming up to 1050 ℃ of sintering 2 hours, carry out afterwards secondary thermal treatment, wherein the one-level thermal treatment temp is 860 ℃, time 2 h; 500 ℃ of secondary thermal treatment temps, time 2 h.Namely obtain sintered magnet.Prepared magnet
Comparative Examples 4
Adopt the technique identical with embodiment 4 to prepare the Nd of the dysprosium Zinc alloy powder particle that do not mix
12.5Fe
BalAl
1.2B
6Sintered magnet is tested as a comparison.
Utilize the BH loop instrument to test the magnetic property of two kinds of magnets, the erosion resistance of utilizing simultaneously autoclave (121 ℃, 0.2MPa, 500h) to test magnet.Every magnetic property and the corrosion resistance nature index of prepared magnet are listed in the table 4.
Table 4 embodiment 4 and Comparative Examples 4 magnet magnetic properties and corrosion resistance nature contrast
Above presentation of results is for the identical sintered NdFeB magnet of composition, adopt magnet that the present invention adds the preparation of dysprosium Zinc alloy powder particle to significantly improve than the coercive force of the magnet that do not mix, the remanent magnetism of two kinds of magnets and magnetic energy product are suitable in addition, and the erosion resistance of magnet is obviously improved simultaneously.
Embodiment 5
Utilize the rapid hardening technology that composition is Nd
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 the powder of 3 microns of median sizes.Afterwards with dysprosium zinc alloy (DyZn weight percent 1.5%, 5 microns of median sizes
5) powder adds in the 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 the high vacuum sintering furnace, be warming up to 1030 ℃ of sintering 2 hours.Carry out afterwards secondary thermal treatment, wherein the one-level thermal treatment temp is 850 ℃, 1 hour time; 540 ℃ of secondary thermal treatment temps, time 2 h.Namely obtain sintered magnet.
Comparative Examples 5
Adopt the technique identical with embodiment 5 to prepare the Nd of the dysprosium Zinc alloy powder particle that do not mix
12.5Fe
BalNb
0.1Co
0.3Al
0.2B
6Sintered magnet is tested as a comparison.
Utilize the BH loop instrument to test the magnetic property of two kinds of magnets, the erosion resistance of utilizing simultaneously autoclave (121 ℃, 0.2MPa, 500h) to test magnet.Every magnetic property and the corrosion resistance nature index of prepared magnet are listed in the table 5.
Table 5 embodiment five and Comparative Examples five magnet magnetic properties and corrosion resistance nature contrast
Above presentation of results is for the identical sintered NdFeB magnet of composition, adopt magnet that the present invention adds the preparation of dysprosium Zinc alloy powder particle to significantly improve than the coercive force of the magnet that do not mix, the remanent magnetism of two kinds of magnets and magnetic energy product are suitable in addition, and the erosion resistance of magnet is obviously improved simultaneously.
Claims (2)
1. a method for preparing high-coercive force and sintered NdFeB permanent magnetic material with high corrosion resistance is characterized in that, may further comprise the steps:
(1) adopts rapid hardening thin slice technique to prepare neodymium iron boron base rapid hardening thin slice, pulverize preparation 3-5 micron neodymium iron boron based raw material powder with the quick-fried method of hydrogen with the alloy sheet fragmentation and by airflow milling afterwards;
(2) with dysprosium zinc alloy DyZn or the DyZn of median size 1-10 micron
5Powder adds in the neodymium iron boron based powders for preparing in the 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 in the magnetic field of 1.8T and compression moulding through even mixed powder, obtains pressed compact;
(4) pressed compact is inserted in the vacuum sintering furnace, the temperature that then raises was carried out secondary thermal treatment at last at 1000-1100 ℃ of sintering 2-4 hour, and wherein the 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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Cited By (5)
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| CN103506624A (en) * | 2012-06-20 | 2014-01-15 | 中磁科技股份有限公司 | Method for sintering neodymium iron boron magnets |
| 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 |
| CN108417379A (en) * | 2018-03-30 | 2018-08-17 | 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 |
| CN111243846A (en) * | 2020-01-19 | 2020-06-05 | 北京工业大学 | Method capable of simultaneously improving oxidation corrosion resistance of NdFeB powder and magnet |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103506624A (en) * | 2012-06-20 | 2014-01-15 | 中磁科技股份有限公司 | Method for sintering neodymium iron boron magnets |
| 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 |
| CN108417379A (en) * | 2018-03-30 | 2018-08-17 | 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 |
| CN111243846A (en) * | 2020-01-19 | 2020-06-05 | 北京工业大学 | Method capable of simultaneously improving oxidation corrosion resistance of NdFeB powder and 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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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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