CN104952580A - Corrosion-resistant sintered NdFeB magnet and manufacturing method thereof - Google Patents
Corrosion-resistant sintered NdFeB magnet and manufacturing method thereof Download PDFInfo
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- CN104952580A CN104952580A CN201510284717.8A CN201510284717A CN104952580A CN 104952580 A CN104952580 A CN 104952580A CN 201510284717 A CN201510284717 A CN 201510284717A CN 104952580 A CN104952580 A CN 104952580A
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Abstract
The invention belongs to the field of magnetic materials, and particularly relates to a corrosion-resistant sintered NdFeB magnet and a manufacturing method thereof. The corrosion-resistant sintered NdFeB magnet is composed of, by weight, 10-15% of Pr, 18-21% of Nd, 3-5% of Ho, 0.5-0.8% of F, 0.5-2.0% of Ni, 0.1-0.2% of Mn, 0.1-0.35% of Cu, 0.1-0.5% of Al, 0.6-1.2% of B and the balance Fe. A staged microwave sintering technology is adopted for manufacturing the magnet, the chemical components, the microstructure and the magnetic property of the magnet are effectively improved, corrosion resistance is remarkably improved, and the application range of magnetic products is greatly increased.
Description
Technical field
The invention belongs to field of magnetic material, be specifically related to a kind of corrosion-resistant Sintered NdFeB magnet and preparation method thereof.
Background technology
Along with the development of science and technology, magnetic material is widely used in industrial production and resident living.Magnetic material can realize magnetic energy and electric transformation of energy, and then realizes automation and the intellectuality of electric equipment, can say, magnetic material is closely related with the every aspect of informationization, automation, electromechanical integration, national defence, national economy.But while magnetic material is used widely, higher requirement be it is also proposed to its performance.
After rare earth permanent-magnetic material occurs, the performance of permanent magnetic material has had qualitative leap, and samarium cobalt magnet is well used in high temperature magnet with its superior coercive force and thermal stability, but its raw material is less at occurring in nature reserves, cause expensive, limit its application at civil area; The raw material resources deposit of neodymium iron boron magnetic body is sufficient, and comes out top in high performance magnet with its higher magnetic energy product, is described as " magnetic king ", thus cost performance is higher, is widely used, but its thermal stability is poor, corrosion-resistant, also have impact on its application to a certain extent.
Sintered NdFeB magnet is by the Multiphase Powder alloy of principal phase, boron-rich phase and rich neodymium phase composition, rich neodymium surrounds principal phase (mainly concentrating on triangle grain boundaries) as Grain-Boundary Phase, boron-rich phase is also present in crystal boundary, and the difference of each phase chemistry composition just to cause chemical potential different, under wet heat condition, easily form corrosion current, cause intercrystalline corrosion.In addition, the oxide etch of rich neodymium phase and the efflorescence of suction hydrogen are also the main reasons of magnet corrosion: generally speaking, when magnet is placed in normal temperature, dry environment, owing to there being the existence of a large amount of simple substance Nd (poor chemical stability) in rich-Nd phase in sintering process, very easily there is oxidation reaction and produce Nd
2o
3, cause oxide etch; And under higher temperature, damp condition, the easy oxidized generation Nd (OH) of Nd of rich neodymium phase
3, produce H simultaneously
2, and then occur to inhale hydrogen efflorescence, corrode more serious.
Summary of the invention
For the problems referred to above, the invention provides a kind of corrosion-resistant Sintered NdFeB magnet and preparation method thereof, effectively improve the uniformity of chemical composition, microstructure and magnetic performance, corrosion resistance is significantly improved, and products application scope increases greatly.
The present invention is achieved through the following technical solutions:
Design a kind of corrosion-resistant Sintered NdFeB magnet, be grouped into by the one-tenth of following mass percent: 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%, surplus is Fe.
Preferably, be grouped into by the one-tenth of following mass percent: Pr 12%, Nd 20%, Ho 4%, F 0.6%, Ni 1.8%, Mn 0.15%, Cu 0.12%, Al 0.1%, B 0.95%, surplus is Fe.
Design a kind of preparation method of above-mentioned corrosion-resistant Sintered NdFeB magnet, comprise the following steps:
(1) to get the raw materials ready ingot casting: with raw material according to described ratio, add in smelting furnace, vacuumize, and carry out melting under 0.05MPa argon shield, after iron dissolves in aluminium alloy entirely, leave standstill 2 ~ 5 minutes, be cast into ingot;
(2) the broken powder process of hydrogen: gained ingot casting is carried out hydrogen fragmentation, to the alloy powder of 180 ~ 240 μm, then carries out Dehydroepiandrosterone derivative; Then, gained alloy powder is placed in airflow milling, carries out being ground to 1 ~ 2 μm;
(3) magnetic is got shaping: after fully being mixed by ground metal dust, be placed in magnetic field vertical orientated, and compressing;
(4) microwave sintering: moulded blank is carried out microwave multi-steps sintering, ar gas environment is protected, and first sinters 1.5 hours at 6KW, then sinters 2 hours at 4KW, then sinter 2 hours at 4KW, naturally cool, to obtain final product with stove.
Positive beneficial effect of the present invention:
The present invention, on the basis of ternary neodymium iron boron magnetic body, through large quantity research, adds appropriate Pr and replaces part Nd, improve principal phase coercive force; Add the addition of C u, Al and replace part Fe; Add the resistance to corrosion that appropriate Ni improves magnet; Add a certain amount of Mn and effectively can suppress magnet the growing up of crystal grain in sintering process.Add a certain amount of F, a small amount of O remaining in Absorbable rod sintering process, the Ho-O-F being confined to magnet triangle grain boundaries is jointly formed with Ho, it exists on a small quantity can improve grain uniformity in sintering process, the different growth of effective suppression main phase grain, thus the remanent magnetism and the coercive force that ensure that magnet; On this basis, slightly the formation of volume Ho-O-F in conjunction with the oxygen of a great deal of, can greatly reduce the phenomenon of oxide etch and the efflorescence of suction hydrogen, improves the corrosion resistance of magnet again.In addition, optimizing components is combined with segmentation microwave sintering process by the present invention, effectively improve the uniformity of chemical composition, microstructure and magnetic performance, and make the thickness of rich neodymium border phase minimum, the space that namely intercrystalline corrosion occurs is minimum, also inhibit the progress of intercrystalline corrosion significantly, improve product quality.
Accompanying drawing explanation
Fig. 1 is the fracture secondary electron image of the embodiment of the present invention 1 gained neodymium iron boron magnetic body.
Fig. 2 is the fracture secondary electron image of the embodiment of the present invention 2 gained neodymium iron boron magnetic body.
Fig. 3 is the fracture secondary electron image of the embodiment of the present invention 3 gained neodymium iron boron magnetic body.
Fig. 4 is the fracture secondary electron image of the embodiment of the present invention 4 gained neodymium iron boron magnetic body.
Fig. 5 is the fracture secondary electron image of the embodiment of the present invention 5 gained neodymium iron boron magnetic body.
Embodiment
With specific embodiment, technical scheme of the present invention is described below, but protection scope of the present invention is not limited thereto:
Embodiment 1
A kind of corrosion-resistant Sintered NdFeB magnet, be grouped into by the one-tenth of following mass percent: Pr 12%, Nd 20%, Ho 4%, F 0.6%, Ni 1.8%, Mn 0.15%, Cu 0.12%, Al 0.1%, B 0.95%, surplus is Fe.Preparation method is as follows:
(1) to get the raw materials ready ingot casting: with raw material according to described ratio, add in smelting furnace, vacuumize, and carry out melting under 0.05MPa argon shield, after iron dissolves in aluminium alloy entirely, leave standstill 3 minutes, be cast into ingot; When there is incidental impurities in raw material, or when introducing the impurity of trace in preparation process, do not affect of the present invention completing; F adds with the form of metal fluoride required in proportioning;
(2) the broken powder process of hydrogen: gained ingot casting is carried out hydrogen fragmentation, to the alloy powder of 180 ~ 240 μm, then carries out Dehydroepiandrosterone derivative; Then, gained alloy powder is placed in airflow milling, carries out being ground to 1 ~ 2 μm;
(3) shaping: after fully being mixed by ground metal dust, to be placed in magnetic field vertical orientated, and compressing;
(4) microwave sintering: moulded blank is carried out microwave multi-steps sintering, ar gas environment is protected, and first sinters 1.5 hours at 6KW, then sinters 2 hours at 4KW, then sinter 2 hours at 4KW, naturally cool, to obtain final product with stove.
Embodiment 2
A kind of corrosion-resistant Sintered NdFeB magnet, be grouped into by the one-tenth of following mass percent: Pr 10%, Nd 21%, Ho 5%, F 0.5%, Ni 2.0%, Mn 0.1%, Cu 0.35%, Al0.1%, B 1.2%, surplus is Fe.Preparation method is identical with embodiment 1.
Embodiment 3
Design a kind of corrosion-resistant Sintered NdFeB magnet, be grouped into by the one-tenth of following mass percent: Pr 15%, Nd 18%, Ho 3%, F 0.8%, Ni 0.5%, Mn 0.2%, Cu 0.1%, Al 0.5%, B 0.6%, surplus is Fe.Preparation method is identical with embodiment 1.
Embodiment 4
Design a kind of corrosion-resistant Sintered NdFeB magnet, be grouped into by the one-tenth of following mass percent: Pr 10%, Nd 18%, Ho 3%, F 0.5%, Ni 0.5%, Mn 0.1%, Cu 0.1%, Al 0.1%, B 0.6%, surplus is Fe.Preparation method is identical with embodiment 1.
Embodiment 5
Design a kind of corrosion-resistant Sintered NdFeB magnet, be grouped into by the one-tenth of following mass percent: Pr 15%, Nd 21%, Ho 5%, F 0.8%, Ni 2.0%, Mn 0.2%, Cu 0.35%, Al 0.5%, B 1.2%, surplus is Fe.Preparation method is identical with embodiment 1.
The fracture of the present invention to embodiment 1 ~ 5 gained Sintered NdFeB magnet carries out secondary electron image detection, and see Fig. 1 ~ 5, result shows: magnet crystal grain of the present invention is evenly distributed, growth crystallization without exception, non-oxidation aggregate, regular shape, densification, rich neodymium border is mutually narrow, especially embodiment 1, crystal grain distributes very evenly, and reaches 5 ~ 10 μm, and surface configuration is extremely regular, fine and close, rich neodymium border is very narrow mutually, and namely intercrystalline corrosion space is minimum.And high pressure Acceleration study (PCT) is carried out to embodiment 1 ~ 5 gained Sintered NdFeB magnet, to test the corrosion rate of each magnet, record 125 DEG C, result under 100%RH, 0.25MPa condition is as table 1, these data show, the each magnet of gained under high-temperature and high-pressure conditions all without obvious corrosion phenomenon, corrosion resistance is good, especially embodiment 1, generation is not corroded completely in 24 hours, corrosion in 200h hour is also negligible, and this has widened the range of application of neodymium iron boron magnetic body greatly.High pressure Acceleration study is a kind of conventional evaluation and test neodymium iron boron magnetic body corrosion proof method [Filip O, El-Aziz A M, Hermann R, et al.materials letters.2001,51:213 in hot humid environment; Willman C J, Narasimhan K S V L.J Appl Phys., 1987,61 (8): 3766], in experimentation, removed by the corrosion product of magnet surface, the weightlessness measuring magnet unit are can characterize the corrosion rate of magnet.
The PCT of table 1 neodymium iron boron magnetic body of the present invention tests corrosion weight loss result (mg/cm
2)
The present invention has also carried out magnetic performance detection to embodiment 1 ~ 5 gained Sintered NdFeB magnet, in table 2, result shows: neodymium iron boron magnetic body of the present invention, while raising decay resistance, also ensure that the magnetic that itself is good, make to reach good combination property, significantly widen its range of application.
The Magnetic Test result of table 2 neodymium iron boron magnetic body of the present invention
The present invention is not limited to above-mentioned embodiment, and those skilled in the art also can make multiple change accordingly, but to be anyly equal to the present invention or similar change all should be encompassed in the scope of the claims in the present invention.
Claims (3)
1. a corrosion-resistant Sintered NdFeB magnet, it is characterized in that, be grouped into by the one-tenth of following mass percent: 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%, surplus is Fe.
2. corrosion-resistant Sintered NdFeB magnet according to claim 1, it is characterized in that, be grouped into by the one-tenth of following mass percent: Pr 12%, Nd 20%, Ho 4%, F 0.6%, Ni 1.8%, Mn 0.15%, Cu 0.12%, Al 0.1%, B 0.95%, surplus is Fe.
3. a preparation method for corrosion-resistant Sintered NdFeB magnet described in claim 1 or 2, is characterized in that, comprise the following steps:
(1) to get the raw materials ready ingot casting: with raw material according to described ratio, add in smelting furnace, vacuumize, and carry out melting under 0.05MPa argon shield, after iron charge dissolves in aluminium alloy entirely, leave standstill 2 ~ 5 minutes, be cast into ingot;
(2) the broken powder process of hydrogen: gained ingot casting is carried out hydrogen fragmentation, to the alloy powder of 180 ~ 240 μm, then carries out Dehydroepiandrosterone derivative; Then, gained alloy powder is placed in airflow milling, carries out being ground to 1 ~ 2 μm;
(3) magnetic is got shaping: after fully being mixed by ground metal dust, be placed in magnetic field vertical orientated, and compressing;
(4) microwave sintering: moulded blank is carried out microwave multi-steps sintering, ar gas environment is protected, and first sinters 1.5 hours at 6KW, then sinters 2 hours at 4KW, then after 4KW sinters 2 hours, naturally cool, to obtain final product with stove.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108063045A (en) * | 2016-11-08 | 2018-05-22 | 中国科学院宁波材料技术与工程研究所 | A kind of no heavy rare earth Nd-Fe-B permanent magnet material and preparation method thereof |
| CN108172357A (en) * | 2017-12-21 | 2018-06-15 | 宁波金轮磁材技术有限公司 | A kind of microwave sintering NdFeB magnets 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 |
| 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 |
| WO2024007808A1 (en) * | 2022-07-06 | 2024-01-11 | 烟台正海磁性材料股份有限公司 | High-coercivity nd-fe-b series sintered magnet and preparation method and application thereof |
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| CN1934283A (en) * | 2004-06-22 | 2007-03-21 | 信越化学工业株式会社 | R-Fe-B-based rare earth permanent magnet material |
| JP2008060241A (en) * | 2006-08-30 | 2008-03-13 | Hitachi Ltd | High resistance rare-earth permanent magnet |
| CN101404195A (en) * | 2006-11-17 | 2009-04-08 | 信越化学工业株式会社 | Method for preparing rare earth permanent magnet |
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| CN1934283A (en) * | 2004-06-22 | 2007-03-21 | 信越化学工业株式会社 | R-Fe-B-based rare earth permanent magnet material |
| JP2008060241A (en) * | 2006-08-30 | 2008-03-13 | Hitachi Ltd | High resistance rare-earth permanent magnet |
| CN101404195A (en) * | 2006-11-17 | 2009-04-08 | 信越化学工业株式会社 | Method for preparing rare earth permanent magnet |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108063045A (en) * | 2016-11-08 | 2018-05-22 | 中国科学院宁波材料技术与工程研究所 | A kind of no heavy rare earth Nd-Fe-B permanent magnet material and preparation method thereof |
| 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 |
| CN108172357A (en) * | 2017-12-21 | 2018-06-15 | 宁波金轮磁材技术有限公司 | A kind of microwave sintering NdFeB magnets 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 |
| 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 |
| WO2024007808A1 (en) * | 2022-07-06 | 2024-01-11 | 烟台正海磁性材料股份有限公司 | High-coercivity nd-fe-b series sintered magnet and preparation method and application thereof |
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