CN104952580B - A kind of corrosion-resistant Sintered NdFeB magnet and preparation method thereof - Google Patents
A kind of corrosion-resistant Sintered NdFeB magnet and preparation method thereof Download PDFInfo
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- CN104952580B CN104952580B CN201510284717.8A CN201510284717A CN104952580B CN 104952580 B CN104952580 B CN 104952580B CN 201510284717 A CN201510284717 A CN 201510284717A CN 104952580 B CN104952580 B CN 104952580B
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Abstract
The invention belongs to field of magnetic material, and in particular to a kind of corrosion-resistant Sintered NdFeB magnet and preparation method thereof.The corrosion-resistant Sintered NdFeB magnet of the present invention, by following mass percent into being grouped into：Pr 10 ~ 15%, Nd 18 ~ 21%, Ho 3 ~ 5%, F 0.5 ~ 0.8%, Ni 0.5 ~ 2.0%, Mn 0.1 ~ 0.2%, Cu 0.1 ~ 0.35%, Al 0.1 ~ 0.5%, B 0.6 ~ 1.2%, balance of Fe, and prepared using segmentation microwave sintering process, it is effectively improved the uniformity of chemical composition, microstructure and magnetic performance, corrosion resistance is significantly improved, and magnetic product range of application is greatly increased.
Description
Technical field
The invention belongs to field of magnetic material, and in particular to a kind of corrosion-resistant Sintered NdFeB magnet and preparation method thereof.
Background technology
With the development of science and technology, magnetic material is widely used in industrial production and resident living.Magnetic material
Material can realize magnetic energy and electric transformation of energy, and then realize the automation and intellectuality of electric equipment, it may be said that magnetic material with
Informationization, automation, electromechanical integration, national defence, the every aspect of national economy are closely related.But obtained extensively in magnetic material
Using while, requirement higher it is also proposed to its performance.
From after rare earth permanent-magnetic material appearance, the performance of permanent-magnet material has qualitative leap, and samarium-cobalt magnet is superior with its
Coercivity and heat endurance are well used in high temperature magnet, but its raw material reserves in nature are less, cause valency
Lattice are expensive, limit its application in civil area；The raw material resources deposit of neodymium iron boron magnetic body is sufficient, and with its magnetic energy product higher
Come out top in high performance magnet, be described as " magnetic king ", thus cost performance is higher, is widely used, but its heat endurance is poor,
Corrosion-resistant, also have impact on its application to a certain extent.
Sintered NdFeB magnet is that rich neodymium is mutually as brilliant by the Multiphase Powder alloy of principal phase, boron-rich phase and rich neodymium phase composition
Boundary mutually surrounds principal phase (being concentrated mainly on triangle grain boundaries), and boron-rich phase is existed in crystal boundary, and the difference of each phase chemical composition
The different chemical potential that resulted in is different, and corrosion current is easily formed under wet heat condition, causes intercrystalline corrosion.In addition, rich neodymium
The oxide etch and suction hydrogen efflorescence of phase are also the main reason of magnet corrosion：In general, magnet is placed in normal temperature, dry ring
When in border, due to the presence for there are a large amount of simple substance Nd (poor chemical stability) in rich-Nd phase in sintering process, easily there is oxidation anti-
Nd should be produced2O3, cause oxide etch；And under higher temperature, damp condition, the Nd of rich neodymium phase is easily oxidized generation Nd
(OH)3, while producing H2, and then occur to inhale hydrogen efflorescence, corrode more serious.
The content of the invention
Regarding to the issue above, the invention provides a kind of corrosion-resistant Sintered NdFeB magnet and preparation method thereof, effectively
The uniformity of chemical composition, microstructure and magnetic performance is improve, corrosion resistance is significantly improved, products application scope is big
It is big to increase.
The present invention is achieved through the following technical solutions：
A kind of corrosion-resistant Sintered NdFeB magnet is designed, by following mass percent into being grouped into：Pr 10~15%,
Nd 18~21%, Ho 3~5%, F 0.5~0.8%, Ni 0.5~2.0%, Mn 0.1~0.2%, Cu 0.1~
0.35%th, Al 0.1~0.5%, B 0.6~1.2%, balance of Fe.
Preferably, by following mass percent into being grouped into：Pr 12%, Nd 20%, Ho 4%, F 0.6%, Ni
1.8%th, Mn 0.15%, Cu 0.12%, Al 0.1%, B 0.95%, balance of Fe.
A kind of preparation method of above-mentioned corrosion-resistant Sintered NdFeB magnet is designed, is comprised the following steps：
(1) get the raw materials ready ingot casting：Raw material is equipped with according to the ratio, is added in smelting furnace, vacuumized, and in 0.05MPa argon gas
Melting is carried out under protection, after iron dissolves in aluminium alloy entirely, 2~5 minutes is stood, ingot of casting；
(2) the broken powder processed of hydrogen：Gained ingot casting is carried out into hydrogen to crush, to 180~240 μm of alloy powder, then is carried out at dehydrogenation
Reason；Then, gained alloy powder is placed in airflow milling, is ground to 1~2 μm；
(3) magnetic shaping is taken：After ground metal dust is sufficiently mixed, it is placed in vertical orientated in magnetic field, and is pressed into
Type；
(4) microwave sintering：Moulded blank is carried out into microwave multi-steps sintering, ar gas environment protection sinters 1.5 in 6KW first
Hour, then sintered 2 hours in 4KW, then sintered 2 hours in 4KW, with stove natural cooling, obtain final product.
Positive beneficial effect of the invention：
The present invention, by numerous studies, adds appropriate Pr and replaces part Nd on the basis of ternary neodymium iron boron magnetic body, improves
Principal phase coercivity；Appropriate Cu, Al are added instead of part Fe；The appropriate Ni of addition improves the resistance to corrosion of magnet；Addition is certain
The Mn of amount can effectively suppress magnet crystal grain in sintering process and grow up.A certain amount of F is added, remaining in sintering process is can absorb
A small amount of O, the Ho-O-F for being confined to magnet triangle grain boundaries is collectively forming with Ho, its on a small quantity exist can be carried in sintering process
Grain uniformity high, effectively suppresses the different growth of main phase grain, so as to ensure that the remanent magnetism and coercivity of magnet；In this base
On plinth, the slightly formation of volume Ho-O-F can combine considerable amount of oxygen again, greatly reduce oxide etch and inhale the phenomenon of hydrogen efflorescence,
Improve the corrosion resistance of magnet.In addition, the present invention is combined optimizing components with segmentation microwave sintering process, it is effectively improved
The uniformity of chemical composition, microstructure and magnetic performance, and make the thickness of rich neodymium border phase minimum, that is, intercrystalline corrosion hair
Raw space is minimum, also significantly inhibits the progress of intercrystalline corrosion, improves product quality.
Brief description of the drawings
Fig. 1 is the fracture secondary electron image of the gained neodymium iron boron magnetic body of the embodiment of the present invention 1.
Fig. 2 is the fracture secondary electron image of the gained neodymium iron boron magnetic body of the embodiment of the present invention 2.
Fig. 3 is the fracture secondary electron image of the gained neodymium iron boron magnetic body of the embodiment of the present invention 3.
Fig. 4 is the fracture secondary electron image of the gained neodymium iron boron magnetic body of the embodiment of the present invention 4.
Fig. 5 is the fracture secondary electron image of the gained neodymium iron boron magnetic body of the embodiment of the present invention 5.
Specific embodiment
Technical scheme, but protection scope of the present invention not limited to this are illustrated with specific embodiment below：
Embodiment 1
A kind of corrosion-resistant Sintered NdFeB magnet, by following mass percent into being grouped into：Pr 12%, Nd 20%,
Ho 4%, F 0.6%, Ni 1.8%, Mn 0.15%, Cu 0.12%, Al 0.1%, B 0.95%, balance of Fe.Preparation side
Method is as follows：
(1) get the raw materials ready ingot casting：Raw material is equipped with according to the ratio, is added in smelting furnace, vacuumized, and in 0.05MPa argon gas
Melting is carried out under protection, after iron dissolves in aluminium alloy entirely, 3 minutes is stood, ingot of casting；When there are incidental impurities in raw material,
Or when the impurity of trace is introduced in preparation process, completion of the invention is not influenceed；F is with the metal fluoride needed for matching
Form addition；
(2) the broken powder processed of hydrogen：Gained ingot casting is carried out into hydrogen to crush, to 180~240 μm of alloy powder, then is carried out at dehydrogenation
Reason；Then, gained alloy powder is placed in airflow milling, is ground to 1~2 μm；
(3) it is molded：After ground metal dust is sufficiently mixed, it is placed in vertical orientated in magnetic field and compressing；
(4) microwave sintering：Moulded blank is carried out into microwave multi-steps sintering, ar gas environment protection sinters 1.5 in 6KW first
Hour, then sintered 2 hours in 4KW, then sintered 2 hours in 4KW, with stove natural cooling, obtain final product.
Embodiment 2
A kind of corrosion-resistant Sintered NdFeB magnet, by following mass percent into being grouped into：Pr 10%, Nd 21%,
Ho 5%, F 0.5%, Ni 2.0%, Mn 0.1%, Cu 0.35%, Al0.1%, B 1.2%, balance of Fe.Preparation method
It is same as Example 1.
Embodiment 3
A kind of corrosion-resistant Sintered NdFeB magnet is designed, by following mass percent into being grouped into：Pr 15%, Nd
18%th, Ho 3%, F 0.8%, Ni 0.5%, Mn 0.2%, Cu 0.1%, Al 0.5%, B 0.6%, balance of Fe.Prepare
Method is same as Example 1.
Embodiment 4
A kind of corrosion-resistant Sintered NdFeB magnet is designed, by following mass percent into being grouped into：Pr 10%, Nd
18%th, Ho 3%, F 0.5%, Ni 0.5%, Mn 0.1%, Cu 0.1%, Al 0.1%, B 0.6%, balance of Fe.Prepare
Method is same as Example 1.
Embodiment 5
A kind of corrosion-resistant Sintered NdFeB magnet is designed, by following mass percent into being grouped into：Pr 15%, Nd
21%th, Ho 5%, F 0.8%, Ni 2.0%, Mn 0.2%, Cu 0.35%, Al 0.5%, B 1.2%, balance of Fe.System
Preparation Method is same as Example 1.
The present invention carries out secondary electron image detection to the fracture of the gained Sintered NdFeB magnet of embodiment 1~5, see Fig. 1~
5, as a result show：Magnet crystal grain distribution of the present invention is uniform, growth crystallization without exception, non-oxidation aggregate, regular shape, densification,
Rich neodymium border is mutually narrow, especially embodiment 1, and crystal grain distribution is highly uniform, reaches 5~10 μm, surface configuration extremely rule, cause
Close, rich neodymium border is mutually very narrow, that is, intercrystalline corrosion space is minimum.And to the gained Sintered NdFeB magnet of embodiment 1~5
Enter horizontal high voltage Acceleration study (PCT), to test the corrosion rate of each magnet, measure in 125 DEG C, 100%RH, 0.25MPa condition
Under result such as table 1, the as shown by data, each magnet of gained is without obvious corrosion phenomenon under high-temperature and high-pressure conditions, and corrosion resistance is good
Good, especially embodiment 1, did not corrode generation completely in 24 hours, and the corrosion in 200h hours can also ignore,
This has widened the range of application of neodymium iron boron magnetic body significantly.High pressure Acceleration study is a kind of conventional evaluation and test neodymium iron boron magnetic body in high temperature
Corrosion proof method [Filip O, El-Aziz A M, Hermann R, et al.materials in wet environment
letters.2001,51:213；Willman C J,Narasimhan K S V L.J Appl Phys.,1987,61(8):
3766], in experimentation, the corrosion product of magnet surface is removed, the weightless of measurement magnet unit area can characterize magnetic
The corrosion rate of body.
The PCT experiment corrosion weight loss results (mg/cm of the neodymium iron boron magnetic body of the present invention of table 12)
The present invention has also carried out magnetic performance detection to the gained Sintered NdFeB magnet of embodiment 1~5, is shown in Table 2, as a result table
It is bright：Neodymium iron boron magnetic body of the present invention also ensure that good magnetic itself while decay resistance is improved, and make to reach well
Combination property, significantly widens its range of application.
The Magnetic Test result of the neodymium iron boron magnetic body of the present invention of table 2
The invention is not limited in above-mentioned specific embodiment, those skilled in the art can also accordingly make various changes,
But it is any all to cover within the scope of the claims with equivalent or similar change of the invention.
Claims (2)
1. a kind of corrosion-resistant Sintered NdFeB magnet, it is characterised in that by following mass percent into being grouped into：Pr 12%、
Nd 20%, Ho 4%, F 0.6%, Ni 1.8%, Mn 0.15%, Cu 0.12%, Al 0.1%, B 0.95%, balance of Fe.
2. the preparation method of corrosion-resistant Sintered NdFeB magnet described in a kind of claim 1, it is characterised in that including following step
Suddenly：
（1）Get the raw materials ready ingot casting：Raw material is equipped with according to the mass percent, is added in smelting furnace, vacuumized, and in 0.05MPa argons
Melting is carried out under gas shielded, after iron charge dissolves in aluminium alloy entirely, 2 ~ 5 minutes is stood, ingot of casting；
（2）The broken powder processed of hydrogen：Gained ingot casting is carried out into hydrogen to crush, to 180 ~ 240 μm of alloy powder, then Dehydroepiandrosterone derivative is carried out；So
Afterwards, gained alloy powder is placed in airflow milling, is ground to 1 ~ 2 μm；
（3）Take magnetic shaping：After ground alloy powder is sufficiently mixed, it is placed in vertical orientated in magnetic field and compressing；
（4）Microwave sintering：Moulded blank is carried out into microwave multi-steps sintering, ar gas environment protection is sintered 1.5 hours in 6KW first,
Sintered 2 hours in 4KW again, then after 4KW is sintered 2 hours, with stove natural cooling, obtained final product.
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| CN108063045B (en) * | 2016-11-08 | 2020-04-21 | 中国科学院宁波材料技术与工程研究所 | Heavy-rare-earth-free neodymium-iron-boron permanent magnet material and preparation method thereof |
| CN108172357B (en) * | 2017-12-21 | 2020-10-16 | 宁波金轮磁材技术有限公司 | Microwave sintered NdFeB magnet and preparation method thereof |
| CN108630369A (en) * | 2018-06-19 | 2018-10-09 | 江苏江淮磁业有限公司 | A kind of neodymium cerium Fe-Mn magnetism material preparation method based on cerium |
| 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 |
| CN115083714A (en) * | 2022-07-06 | 2022-09-20 | 烟台正海磁性材料股份有限公司 | High-coercivity Nd-Fe-B sintered magnet and preparation method and application thereof |
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| JP4700578B2 (en) * | 2006-08-30 | 2011-06-15 | 株式会社日立製作所 | Method for producing high resistance rare earth permanent magnet |
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