CN110211797A - A method of promoting Sintered NdFeB magnet magnetic property - Google Patents
A method of promoting Sintered NdFeB magnet magnetic property Download PDFInfo
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- CN110211797A CN110211797A CN201910521802.XA CN201910521802A CN110211797A CN 110211797 A CN110211797 A CN 110211797A CN 201910521802 A CN201910521802 A CN 201910521802A CN 110211797 A CN110211797 A CN 110211797A
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- magnetic property
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- rare earth
- sintered ndfeb
- heavy rare
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
Abstract
The invention discloses a kind of methods for promoting Sintered NdFeB magnet magnetic property, this method utilizes the characteristic of low melting metal oxide, metal oxide is restored at high temperature using hydrogen, successively low melting metal is obtained according to reduction sequence, the discontinuous crystal boundary rare-earth phase in magnet surface layer is repaired in preferential diffusion, obtain continuous low melting point rare earth phase, again in this, as the quick diffusion admittance of heavy rare earth element, effectively promote diffusion depth of the heavy rare earth element in magnet, and reduce the dosage of heavy rare earth element, realize the coercitive promotion of magnet, the dosage of heavy rare earth element is significantly reduced simultaneously, this method simple process, it is easily achieved, it has broad application prospects.
Description
Technical field
The invention belongs to rare-earth permanent-magnet material technical field more particularly to a kind of promote Sintered NdFeB magnet magnetic property
Method.
Background technique
Nd-Fe-B permanent magnetic rely on excellent magnetic property, referred to as " magnetic king ", be widely used in aerospace, wind-power electricity generation,
The fields such as energy saving household electrical appliances, electronic apparatus and new-energy automobile.And as being constantly progressive for manufacturing technology is anticipated with people's environmental protection
The promotion of knowledge is attracted attention in energy conservation and environmental protection, new energy, the big field of new-energy automobile three by market, and dosage is with annual 10 ~ 20 %
Speed rapid growth, show good application prospect.
For magnet, coercivity is the important indicator for evaluating Nd-Fe-B permanent-magnet material magnetic property superiority and inferiority.And heavy rare earth
The important element that element Dy, Tb are promoted as coercivity, can effectively promote 2:14:1 phase magnetocrystalline anisotropy constant, but its valence
Lattice are high.Traditional surface deposition it is simple coercivity is promoted using the mode of rare earth oxide or fluoride, reduce magnetic
Body manufacturing cost, but heavy rare earth element fusing point is higher, and required diffusion activation energy is higher, and by table, the concentration range of decrease is larger inwards, therefore
Diffusion depth is shallower, performance boost limited extent.
Summary of the invention
It is an object of the invention to provide a kind of methods for promoting Sintered NdFeB magnet magnetic property, utilize low melting metal oxide
The characteristic easily restored realizes the reduction of low melting metal, and by stepped thermal treatment, repairs magnet surface layer and be damaged crystal boundary, formed
Uniformly continuous low melting point Nd-rich phase, and in this, as heavy rare earth diffusion admittance, promote elements diffusion depth and its rate, is promoted
Coercivity, and save manufacturing cost.
To achieve the above object, the present invention provides the following technical scheme that
A method of Sintered NdFeB magnet magnetic property is promoted, is included the following steps:
1. a kind of method for promoting Sintered NdFeB magnet magnetic property, which comprises the steps of:
1) oxide skin of magnet surface is purified, and dried；
2) it is lower than 2 × 10 in vacuum degree-3Under the conditions of Pa, magnet surface deposits the oxide of low melting metal oxide and heavy rare earth
Or fluoride；
3) magnet after mixed deposit is put into the horizontal sintering furnace of high vacuum, vacuumized, vacuum degree is lower than 1 × 10-3When Pa, lead to
Enter hydrogen, then raise temperature to 660-880 DEG C, keeps the temperature 3-5 h；
4) it is warming up to 850-950 DEG C, keeps the temperature 5-10 h.
Further, the method for the surface deposition is one or more of magnetron sputtering, electrophoretic deposition, spraying or coating
Combination.
Further, the heavy rare earth metal is one of Dy, Tb.
Further, the low melting metal oxide is MgO, ZnO, Al2O3、SnO2One of or a variety of combinations.
Further, low melting metal oxide is deposited using electrophoresis or coating method in step 2；Heavy rare-earth oxide or fluorine
Compound is using vapor deposition or magnetically controlled sputter method deposition.
Further, soaking time is 4 hours in step 3), and temperature is 800 DEG C.
Further, soaking time is 8 hours in step 4), and temperature is 900 DEG C.
Further, in step 1) when the oxide or fluoride of deposition MgO and heavy rare earth element, Mg atom in sedimentary
Quantity and the ratio of heavy rare earth element atomic quantity are between 1:2 ~ 1:3；When being changed to ZnO；In sedimentary Zn atomic quantity with
The ratio of heavy rare earth element atomic quantity is between 1:2 ~ 1:4；It is changed to Al2O3When；Al atomic quantity and heavy rare earth in sedimentary
The ratio of Elements Atom quantity is between 1:2 ~ 1:4；It is changed to SnO2When；Sn atomic quantity and heavy rare earth element are former in sedimentary
The ratio of subnumber amount is between 1:3 ~ 1:5.
The solution of the present invention utilizes the characteristic of low melting metal oxide, and metal oxide is carried out at high temperature using hydrogen
Reduction successively obtains low melting metal according to reduction sequence, and the discontinuous crystal boundary rare-earth phase in magnet surface layer is repaired in preferential diffusion, obtains
Continuous low melting point rare earth phase, then in this, as the quick diffusion admittance of heavy rare earth element, effectively promote heavy rare earth element and exist
Diffusion depth in magnet, and the dosage of heavy rare earth element is reduced, the realization coercitive promotion of magnet, while heavy rare earth element
Dosage is significantly reduced, this method simple process, it is easy to accomplish, it has broad application prospects.
Specific embodiment
The present invention is made a more thorough explanation below with embodiment.The present invention can be presented as a variety of different forms,
It should not be construed as limited to the exemplary embodiments described herein.
Embodiment 1
(1) neodymium iron boron magnetic body sintered is sliced into the block of 10*20*6 mm.
(2) it is successively thrown respectively using 6 faces of the sand paper polishing magnet of 600 CW, 1000CW, 1500CW, 2000CW
Light processing is subsequently placed into progress ultrasonic oscillation cleaning in alcohol；The ultrasonic oil removing 3 in 50 DEG C of degreasing fluid by magnet again
Min is then washed, and washing time is 5-15 s.
(3) magnet is placed in the nitric acid solution of 3 % of concentration and shakes cleaning, the time is 10-20 s, is carried out twice after taking-up
Washing, each washing time are 5-15 s, the processing of subsequent ultrasonic vibration, it is to be observed completely fallen off to magnet superficial oxidation skin after take
Out, drying and processing is carried out, drying temperature is 40 DEG C, and drying time is 20 min.It can also make magnet surface layer using other modes
Oxide skin is completely fallen off.
(4) by MgO powder and Dy2O3Powder mixes, and the atomicity of Mg and the atomicity ratio of Dy are 1:2 in mixture；Make
Mixed membranous layer is formed in magnet surface deposited mixture with magnetron sputtering method.It can also be deposited with spray coating method and other methods.Wherein
Film layer average thickness is tested to be 20 μm；Wherein MgO can be replaced with other low melting metal oxides.Low melting metal oxide
Refer to by hydrogen reducing (or by CaH2Powder reduction) after can obtain quasi-metal oxides of contained pure metal；Such as:
MgO、ZnO、Al2O3、SnO2Or binary or ternary mixture composed by above-mentioned metal oxide: MgO+ZnO, MgO+Al2O3、
MgO+SnO2、ZnO+Al2O3、ZnO+SnO2、Al2O3+SnO2、MgO+ZnO+Al2O3、ZnO+Al2O3+SnO2Deng；Low melting metal oxygen
The ratio between atomicity and heavy rare-earth oxide in compound or the atomicity of heavy rare earth element in fluoride should be controlled in 1:2 to 1:
Between 5.Heavy rare earth metal can also be as Tb.
(5) it is lower than 1 × 10 in vacuum degree-3Under conditions of Pa, it is passed through after hydrogen in level-one reduction and 800 DEG C of diffusion temperature
4 h are kept the temperature, then again with 900 DEG C of second level diffusion temperature 8 h of heat preservation, finally carry out 500 DEG C of 2 h of tempering.At different levels heat treated
Cheng Zhong, level-one reduction and diffusion temperature can be 660-880 DEG C, and soaking time is 3-5 h；Second level diffusion temperature can be
850-950 DEG C, soaking time is 5-10 h.It it can also be covered on magnet surface with CaH2 powder replaces being passed through hydrogen and be gone back
Original reaction.
The technique, which is realized, spreads low temperature+high temperature grading: (660-880 DEG C) is with hydrogen to eutectic first at a lower temperature
Metal oxide carries out restoring obtained low melting metal, then carries out low melting metal or alloy during incubation to magnet from the inside to the outside
It is diffused, it is preferential to repair impaired crystal boundary, improve the continuity and lubricity of crystal boundary, obtains the crystal boundary for being conducive to the diffusion of element
Channel；Then (850-950 DEG C) excitation surface layer heavy rare earth element passes through the good continuous eutectic crystal boundary of reparation at relatively high temperatures
It carries out solid-liquid mixing to diffuse into inside magnet, improves diffusion depth and efficiency.
Sample made from above-mentioned technique is subjected to magnetic property detection with NIM-500C high temperature permanent magnets measuring system, using eutectic
The magnet performance situation of change of alloy reparation diffusion front and back is as shown in table 1.
Table 1 repairs magnet diffusion front and back performance change situation using the reduction of low melting metal oxide
Comparative example 1
Comparative example 1 is substantially the same manner as Example 1, the difference is that, low melting metal oxide is not deposited using step (4) are middle,
But carry out diffusion after Dy directly dilute to heavy deposition and obtain magnet, eutectic gold in institute's expendable weight rare earth β-diketone complex element quality and embodiment 1
It is identical as heavy rare earth element quality sum to belong to oxide, magnet magnetic property such as table 2 is restored and spread without low melting metal oxide
It is shown.
Table 2 restores without low melting metal oxide and repairs magnet magnetic property
Comparative example 2
Comparative example 2 is substantially the same manner as Example 1,.The difference is that: it is not diffused into using low temperature+high temperature grading in step 5)
Row heat treatment, but High temperature diffusion processing (900 DEG C × 8 h) directly is carried out to magnet, at low temperature+high temperature grading diffusion
It is as shown in table 3 to manage magnet magnetic property.
Table 3 spreads magnet magnetic property without low temperature+high temperature grading
Comparative example 3
Comparative example 3 is substantially the same manner as Example 1, the difference is that: when surface metal oxide and heavy rare earth element deposition film
Layer is with a thickness of 70 μm；Test of many times is compared, when metal oxide is greater than 30 μm with heavy rare earth element depositional coating thickness,
Only surface part low melting metal oxide is reduced but cannot be introduced into inside magnet and repaired, and heavy rare earth element is hindered to enter
It is limited that magnet causes coercivity to be promoted, and different deposit thicknesses of layers magnet magnetic properties are as shown in table 4.
Magnet magnetic property is repaired in the reduction of 4 different content low melting metal oxide of table
Comparative example 4
Experiment twice and 1 step of embodiment in comparative example 4 is essentially identical, the difference is that: the atomicity of Mg in mixture
Atomicity ratio with Dy is respectively 1:1 or 1:7.Work as total deposit shared by low melting metal oxide too through test of many times discovery
Small, low melting metal oxide content is limited, and liquid metal concentration gradient is lower after reduction, cannot carry out crystal boundary well into magnet
It repairs, causes subsequent heavy rare earth element diffusion depth limited, magnetic property is promoted limited；When low melting metal oxide atomic quantity and
When rare earth atoms ratio of number is greater than 1:2, heavy rare earth Dy constituent content is less, and low melting metal oxide rate of reduction has
Limit easily causes diffusion admittance blocking in crystal boundary repair process, subsequent heavy rare earth element is hindered to spread, and magnetic property promotion has
Limit, magnet magnetic property when table 3 is the atomicity of Mg and the atomicity of Dy is 1:1 or 1:7.
Magnet magnetic property is repaired in the reduction of 5 different content low melting metal oxide of table
It can be seen that by the magnetic property result of embodiment 1 and comparative example 4 in the case where low melting metal oxide is more, magnetic
Performance decreases, this is because low melting metal reduction is inadequate in deposition process, not only bad for the reparation of crystal boundary, while
The diffusion for hindering subsequent heavy rare earth element, causes magnetic property to decline.
Compared with the prior art, the beneficial effects of the present invention are:
(1) low melting metal oxide (or and CaH in a hydrogen atmosphere is utilized2Powder mixing) characteristic that easily restores, by with again
Rare earth oxide or fluoride mixing coating, preferential reduction and the reparation discontinuous crystal boundary rare-earth phase in magnet surface layer, obtain continuous
Low melting point rare earth phase, then in this, as the quick diffusion admittance of heavy rare earth element, effectively promote heavy rare earth element in magnet
In diffusion depth, promote the promotion of magnetic property.
(2) crystal boundary is repaired using the flowing of low melting point, promotes diffusion depth of the heavy rare earth in magnet, moreover it is possible to be effectively reduced
The use content of heavy rare earth element reduces magnet manufacturing cost.
(3) present invention process is simple, and equipment requirement is relatively low, can complete in original grain boundary decision Equipment Foundations, tool
There is the prospect that large-scale promotion uses.
Above-mentioned example is only intended to illustrate the present invention, and in addition to this, also there are many different embodiments, and these are implemented
Mode be all those skilled in the art after comprehension inventive concept it is also envisioned that therefore, will not enumerate herein.
Claims (8)
1. a kind of method for promoting Sintered NdFeB magnet magnetic property, which comprises the steps of:
1) oxide skin of magnet surface is purified, and dried；
2) it is lower than 2 × 10 in vacuum degree-3Under the conditions of Pa, magnet surface deposits low melting metal oxide and heavy rare-earth oxide or fluorine
Compound；
3) magnet after mixed deposit is put into the horizontal sintering furnace of high vacuum, vacuumized, vacuum degree is lower than 1 × 10-3When Pa, it is added
Reducing agent then raises temperature to 660-880 DEG C, keeps the temperature 3-5 h；
4) it is warming up to 850-950 DEG C, keeps the temperature 5-10 h.
2. promoting the method for Sintered NdFeB magnet magnetic property as described in claim 1, which is characterized in that the surface deposition
Method be one or more of magnetron sputtering, electrophoretic deposition, spraying or coating combination.
3. promoting the method for Sintered NdFeB magnet magnetic property as described in claim 1, which is characterized in that the heavy rare earth gold
Belong to is one of Dy, Tb.
4. promoting the method for Sintered NdFeB magnet magnetic property as described in claim 1, which is characterized in that the low melting metal
Oxide is MgO, ZnO, Al2O3、SnO2One of or a variety of combinations.
5. promoting the method for Sintered NdFeB magnet magnetic property as described in claim 1, which is characterized in that eutectic in step 2
Metal oxide is deposited using electrophoresis or coating method；Heavy rare-earth oxide or fluoride are heavy using vapor deposition or magnetically controlled sputter method
Product.
6. promoting the method for Sintered NdFeB magnet magnetic property as described in claim 1, which is characterized in that kept the temperature in step 3)
Time is 4 hours, and temperature is 800 DEG C.
7. promoting the method for Sintered NdFeB magnet magnetic property as described in claim 1, which is characterized in that kept the temperature in step 4)
Time is 8 hours, and temperature is 900 DEG C.
8. promoting the method for Sintered NdFeB magnet magnetic property as described in claim 1, which is characterized in that be added in step 3)
The mode of reducing agent is to be passed through hydrogen or cover CaH2 powder in magnet surface.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110473704A (en) * | 2019-09-12 | 2019-11-19 | 安吉县宏铭磁性器材有限公司 | A kind of preparation method of slim plate type rare earth permanent-magnetic material |
| CN111403167A (en) * | 2020-04-26 | 2020-07-10 | 江苏科技大学 | Grain boundary diffusion method for sintered neodymium-iron-boron magnet heavy rare earth element |
| CN112489914A (en) * | 2020-11-03 | 2021-03-12 | 北京科技大学 | Method for preparing high-coercivity neodymium-iron-boron magnet through composite diffusion |
| WO2023274034A1 (en) * | 2021-06-28 | 2023-01-05 | 烟台正海磁性材料股份有限公司 | R-fe-b sintered magnet, and preparation method therefor and use thereof |
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| WO2023274034A1 (en) * | 2021-06-28 | 2023-01-05 | 烟台正海磁性材料股份有限公司 | R-fe-b sintered magnet, and preparation method therefor and use thereof |
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Application publication date: 20190906 |