CN101393791A - Anisotropic magnetic powder and manufacturing method thereof - Google Patents
Anisotropic magnetic powder and manufacturing method thereof Download PDFInfo
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- CN101393791A CN101393791A CN 200710161419 CN200710161419A CN101393791A CN 101393791 A CN101393791 A CN 101393791A CN 200710161419 CN200710161419 CN 200710161419 CN 200710161419 A CN200710161419 A CN 200710161419A CN 101393791 A CN101393791 A CN 101393791A
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Abstract
The invention provides a high-performance bonded rare earth permanent magnet powder and a preparation method thereof. Raw material compositions and the preparation method of the rare earth permanent magnet powder are as follows: an alloyed casting strip, the composition ratio of which is R1-xNdx8 to 20MyFebalB4 to 12(atm%), is prepared to be high-performance bonded anisotropic magnet powder through a heat treatment (or untreated process), a hydrogenation and dehydrogenation process and fragmentation. The preparation method comprises the following steps: a rare-iron-boron alloyed casting strip is prepared through a strip casting process, the thickness of the rare-iron-boron alloyed casting strip is 0.1 mm to 1.0 mm; and finally the bonding rare earth permanent magnet powder with high coercive force and high oxidation resistance are prepared through the processes of hydrogenation and dehydrogenation. Compared with the magnet powder taking the traditional cast ingot as the raw material, the bonded magnet powder has higher magnetism property and higher oxidation resistance property.
Description
Technical field
The present invention relates to the manufacture method of rare earth-iron-boron alloy and anisotropic bond magnetic.
Background technology
Bonding NdFeB magnet has excellent magnetism energy, mechanical performance, good machinability, has a good application prospect and development prospect, is widely used in automobile, computer peripheral equipment, electronics, office automation and other electronic devices.80% the NdFeB magnet of wherein boning is used for HDD, and CD2ROM in the spindle motor and stepping motor of DVD2ROM, also has very big potentiality in the demand such as automobile and market, small instruments and tools field.But, require further to improve the magnetic property of bonding rare earth magnet, and the most effectual way of raising magnetic property is to prepare anisotropic bonded permanent magnet for further miniaturization, saving power consumption and the reduction cost etc. that adapt to components and parts and system.In order to prepare anisotropic bonded magnet, people have carried out unremitting effort.At present, carry out research that anisotropic magnet powder prepares the aspect and mainly contain the earliest that MIT is equipped with the NdFeB magnetic with the HDDR legal system, like to know that the system steel is equipped with the NdFeB magnetic with the d-HDDR legal system, Japanese Datong District special steel company and MQ company adopt the hot upset forging method to prepare the NdFeB magnetic.In theory, HDDR (being hydrogenation (Hydrogenation), disproportionation (Disproportionation), dehydrogenation (Desorption), compound (Recombination)) method helps producing in batches, cost hangs down and has the popularization future, take all factors into consideration from large-scale production, cost, magnetic property equal angles, have only the hydrogenation dehydriding to realize that industrialization is the most feasible, that therefore announces anisotropic bond NdFeB industrialization in the world also has only this process route.
Existing patent about rear earth-iron-boron based alloy magnetic anisotropy magnetic mainly contains units such as liking to know system steel, Mitsubishi and Sumitomo.Patent CN94104992.2, CN97114074.X, CN97121194.9, CN99123355.7, CN01140696.8, CN200480001073.7 and CN200510070024.5 have mainly told about with the hydrogenation dehydrogenating technology and have prepared anisotropy rare earth-iron-boron magnetic.But the foundry alloy of above patent all adopts traditional metal mold technology, has following shortcoming:
1) contains a large amount of α-Fe phase, Nd in the alloy cast ingot
2Fe
14B principal phase content is low;
2) rich neodymium phase distributed pole is inhomogeneous in the alloy;
3) alloy graining speed is low, is difficult to reduce the content of rare earth in the alloy;
4) conventional heat treatment is difficult to overcome the above problems fully.
Studies show that no matter how thin alloy cast ingot is for metal mold technology, when total amount of rare earth is lower than 33.0% percetage by weight, just contains a large amount of α-Fe phase in the alloy cast ingot, has a strong impact on the magnetic property of rare earth-iron-boron magnet.
Patent CN02805171.8 adopts and utilizes the method that forms the solidified superalloy layer to prepare foundry alloy, but still has α-Fe phase, is difficult to obtain high performance bonded permanent magnet.
The present invention mainly is the invention of finishing at the problems referred to above, its objective is to obtain high-performance anisotropic bond magnetic, and the realization that reduces cost is produced in batches.
Summary of the invention
Goal of the invention:, obtain the technology of the anisotropy rare-earth-iron boron bonding magnetic of high magnetic characteristics, and the realization that reduces cost is produced in batches by tissue and the hydrogenation dehydrogenation operation of improving foundry alloy.
The invention provides a kind of anisotropy rare-earth-iron boron bonding magnetic and preparation method thereof.The degree of orientation DOA of this anisotropy rare-earth-iron boron bonding magnetic is greater than 0.6, and wherein degree of orientation DOA (degree of alignment) represents the size of the magnetic anisotropy degree of material.The size of DOA is expressed from the next:
DOA＝(Br
∥-Br
⊥)/Br
∥
In the formula: Br
∥-magnet is parallel to the remanent magnetism of magnetic field orientating direction
Br
⊥-magnet is perpendicular to the remanent magnetism of magnetic field orientating direction
Described alloy raw material composition is (R
1-xNd
x)
8～20M
yFe
BalB
4～12The composition of alloy casting piece (atm%) is: R for do not comprise Nd and comprise Sc and the 16 middle rare earth elements of Y in a kind of, x=0～1; M is one or more among Zr, Hf, Mn, Ti, Si, V, Co, Ni, Cr, Mo, Al, Nb, Ga, In, Cu, the Zn, y=0.01～3, and surplus is Fe and unavoidable impurities element.
The preparation method of described anisotropy rare-earth-iron boron bonding magnetic comprises the steps:
The step of preparation terres rares-ferroboron casting sheet alloy casting piece heat treatment or do not handle, is carried out the step that the hydrogenation dehydrogenation is processed into anisotropic magnet powder.
The step that preparation terres rares-iron boron closes alloy casting piece comprises: alloy raw material is added thermosetting rear earth-iron-boron based alloy liquation with Medium frequency induction melting, high-frequency induction melting, electric arc melting, resistance wire heating melting a kind of method wherein, make the rear earth-iron-boron based alloy liquation get rid of into the rear earth-iron-boron based alloy casting sheet that thickness is 0.1～1.0mm by the water-cooled metal wheel (as copper wheel or molybdenum wheel) of rotation, at least 80% alloy casting piece thickness distribution is at [μ-0.1mm, μ+0.1mm] scope in, σ
2≤ 0.011mm
2, wherein μ is the average thickness of alloy casting piece, σ
2Be the variance of alloy casting piece thickness, the degree of scatter of expression alloy casting piece thickness.Cooling rate during wherein from alloy melting point～800 ℃ is 10
2～10
4℃/s, the cooling rate in the time of 800 ℃～600 ℃ is 10
2℃/below the s, alloy flow quantity size is 10
2G/s～10
4Adjustable and can stablize control in the g/s scope, the width of water cooled rolls that alloy liquid is cast to rotation is adjustable and can stablize control in 50mm～600mm scope, alloy liquid cast temperature is adjustable and can stablize control in 1300 ℃～1600 ℃ scopes, and the water cooled rolls rotating speed is adjustable and can stablize control in 0.2m/s～5.0m/s scope.
Organizing of the alloy casting piece that described alloy raw material is made is as follows: α-Fe is lower than 5% mutually, and rich rare earth is evenly distributed mutually and is inner as seen at principal phase crystal boundary and crystal grain, principal phase Nd
2Fe
14B is the column crystal of proper alignment, accounts for more than 80%, and its width is 0.2～40.0 μ m, and length is 1.0～800.0 μ m.
The alloy pretreatment process comprises: with RNdMFeB is that alloy casting piece (vacuum or inert gas shielding) in anti-oxidant atmosphere carries out 850～1180 ℃, the heat treatment of 3～48h.Purpose mainly is for coarsened grain, a small amount of α-the Fe and the part original grain boundary that may exist have been eliminated simultaneously, owing to do not have a large amount of α-Fe in the alloy, therefore can adopt the raising heat treatment temperature and the mode in shortening heat processing time that the original grain of foundry alloy is grown up, simultaneously, because alloy casting piece becomes flakey, volume is little, therefore needn't need to carry out coarse crushing before hydrogenation treatment as traditional ingot casting, therefore more traditional ingot ways has improved production efficiency, has reduced production cost.
Multistep hydrogenation process process comprises: will carry out fully inhaling in 1 step or the multistep process hydrogen 10～500min under heat treatment or the not heat treated RNdMFeB alloy casting piece condition in hydrogen dividing potential drop P1=60～300kPa and temperature T 1=20～600 ℃, and it is quick-fried broken that hydrogen takes place, to reduce the follow-up broken time, reduce magnetic oxygen content and production cost.In temperature-rise period subsequently, hydrogen dividing potential drop P=10～80kPa, but guarantee to suppress unexpected disproportionation, to improve the material anisotropy by hydrogen dividing potential drop≤60kPa during in temperature T 〉=650 ℃; The hydrogen dividing potential drop P2=5～150kPa of the high temperature hydrogenation stage in 1-5 step, guarantee simultaneously pressure be controlled at the best stabilized value ± 0.5kPa between, temperature T 2=750～900 ℃; The hydrogen dividing potential drop P3≤5kPa of the dehydrogenation stage in 1-5 step, temperature T 3=750～900 ℃, with T2 can be unequal.
With the pulverizing process of the thick alloy after the above-mentioned hydrogenation be: the mill in protective atmosphere or anti-oxidant medium, ball milling etc., alloy is made the magnetic that granularity is 50～250 μ m.This magnetic is mainly used in the preparation of anisotropic bonded magnet.
Description of drawings
Fig. 1 hydrogenation dehydrogenating technology figure
Embodiment
Press the ingredient composition shown in the table 1.Its preparation method is: under inert gas shielding, form rare-earth alloy molten solution with the Medium frequency induction melting, be cast on the water-cooled copper roller of rotation by the mode of casting groove with planar flows then, obtain alloy casting piece with the rotating speed of water cooled rolls shown in the table 3, casting sheet thickness and σ
2See Table 3, the alloy casting piece that obtains is heat-treated (or not handling) according to the temperature and time shown in the table 3 in vacuum or inert gas atmosphere.After heat treatment the alloy casting piece of (or not handling) is put into hydrogenation apparatus and is carried out the hydrogenation dehydrogenation with the process conditions shown in the table 3 and handle, and the magnetic particle capability that obtains sees Table 2.
Table 1
| Composition | Nd | Pr | Fe | B | Ga | Al | Zr | Nb |
| Proportioning (atm%) | 12.5 | 0.3 | Surplus | 6.4 | 0.3 | 0.1 | 0.2 | 0.1 |
Table 2
| No. | DOA | (BH)max kJ/m 3 | iHc(MA/m) | The permanent magnetic ratio that reduces |
| 1 | 0.80 | 248 | 0.84 | -3.50 |
| 2 | 0.89 | 356 | 0.97 | -2.44 |
| 3 | 0.85 | 316 | 0.96 | -2.95 |
| 4 | 0.81 | 346 | 1.03 | -2.80 |
| 5 | 0.80 | 286 | 0.88 | -3.61 |
| 6 | 0.82 | 359 | 0.95 | -3.40 |
| 7 | 0.85 | 362 | 0.93 | -2.45 |
| 8 | 0.88 | 348 | 0.89 | -2.64 |
| 9 | 0.82 | 335 | 0.89 | -2.89 |
| 10 | 0.86 | 381 | 0.94 | -2.50 |
| 11 | 0.89 | 394 | 0.96 | -2.35 |
| 12 | 0.83 | 356 | 1.02 | -2.63 |
Claims (9)
1 one kinds of anisotropic bond magnetics is characterized in that degree of orientation DOA is greater than 0.6.
2 anisotropic bond magnetics according to claim 1 is characterized in that, are that the employing alloy casting piece is a foundry alloy, are prepared from through over hydrogenation dehydrogenation operation again, and degree of orientation DOA is greater than 0.8.
3 anisotropic bond magnetics according to claim 2 is characterized in that the thickness μ of described foundry alloy is 0.1～1.0mm, and 80% thickness distribution is in the scope of [μ-0.1mm, μ+0.1mm], σ
2≤ 0.02mm
2, wherein μ is the average thickness of alloy casting piece, σ
2Be the variance of alloy casting piece thickness, the degree of scatter of expression alloy casting piece thickness.
4 anisotropic bond magnetics according to claim 1 and 2 is characterized in that composition is: (R
1-xNd
x)
8～20M
yFe
BalB
4～12(atm%), R is one or more in the 16 kinds of rare earth elements that comprise Sc and Y except that Nd, 0＜x＜1; M is one or more among Zr, Hf, Mn, Ti, Si, V, Co, Ni, Cr, Mo, Al, Nb, Ga, In, Cu, the Zn, y=0～3.
5 one kinds of methods that prepare claim 1 or 2 described anisotropic bond magnetics is characterized in that may further comprise the steps:
A. the alloy liquid of fusion is cast to that cooling forms the uniform alloy casting piece of thickness on the water cooled rolls of rotation;
B. with this alloy casting piece through 850 ℃～1180 ℃, the heat treatment of 3～48h or do not handle;
C. the alloy casting piece that obtains through above-mentioned steps obtains thick alloy through over hydrogenation dehydrogenation operation;
D. the above-mentioned thick alloy of Mechanical Crushing, obtaining granularity is the anisotropic bond magnetic of 50 μ m～250 μ m.
The preparation method of 7 bonding magnetics according to claim 3 is characterized in that, the heat treatment step among the step b comprises: be incubated 3～48h in the vacuum heat treatment furnace under vacuum or inert gas shielding, temperature is 900～1180 ℃.
8 bonding magnetic powders methods according to claim 3 is characterized in that the hydrogen treatment process among the step c comprises: 1-5 step low temperature hydrogenation, 1-5 step high temperature hydrogenation, 1-5 step dehydrogenation operation.
Hydrogenation dehydrogenation operation among the step c of 9 preparation bonding magnetics according to claim 8 is characterized in that, comprises the hydrogen dividing potential drop P1=60～300kPa of the low temperature hydrogenation stage in 1-5 step, temperature T 1=20 ℃～600 ℃, fully inhales hydrogen; The hydrogen dividing potential drop P2=5～150kPa of the high temperature hydrogenation stage in 1-5 step, guarantee simultaneously the hydrogen dividing potential drop be controlled at the best stabilized value ± 0.5kPa between, temperature T 2=750～900 ℃, each stage temperature retention time is respectively 0.5～5h; The hydrogen dividing potential drop P3≤5kPa of the dehydrogenation stage in 1-5 step, temperature T 3=750～900 ℃, with T2 can be unequal.
10 1 kinds of rare earth magnets is characterized in that being made by the described bonding magnetic of claim 1～4.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101850425A (en) * | 2009-03-30 | 2010-10-06 | Tdk株式会社 | Rare earth alloy powder and manufacture method thereof, anisotropic bond magnet compound and anisotropic bond magnet |
| CN102568736A (en) * | 2010-12-21 | 2012-07-11 | 上海爱普生磁性器件有限公司 | Rigid anisotropy bonded neodymium iron boron permanent magnet |
| CN102768890A (en) * | 2012-08-10 | 2012-11-07 | 北矿磁材科技股份有限公司 | Preparation method of rare earth anisotropism magnetic powder, magnetic powder and magnetic body |
| CN102107277B (en) * | 2009-12-29 | 2013-01-16 | 北京有色金属研究总院 | Process and equipment for preparing anisotropic rare-earth permanent-magnet powder and product prepared thereby |
| CN103559971A (en) * | 2013-10-22 | 2014-02-05 | 江西江钨稀有金属新材料有限公司 | Nanometer rare earth permanent magnetic material with high-temperature stability and preparation method thereof |
| CN104716753A (en) * | 2014-11-25 | 2015-06-17 | 宁波金鸡强磁股份有限公司 | Magnet with low pole-arc coefficient and manufacturing method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0633581B1 (en) * | 1993-07-06 | 1998-04-22 | Sumitomo Special Metals Company Limited | R-Fe-B permanent magnet materials and process of producing the same |
| US6444052B1 (en) * | 1999-10-13 | 2002-09-03 | Aichi Steel Corporation | Production method of anisotropic rare earth magnet powder |
-
2007
- 2007-09-21 CN CN200710161419A patent/CN101393791B/en active Active
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101850425A (en) * | 2009-03-30 | 2010-10-06 | Tdk株式会社 | Rare earth alloy powder and manufacture method thereof, anisotropic bond magnet compound and anisotropic bond magnet |
| CN101850425B (en) * | 2009-03-30 | 2012-12-05 | Tdk株式会社 | Rare earth alloy powders and manufacturing method thereof, compound for anisotropic bonded magnet and anisotropic bonded magnet |
| CN102107277B (en) * | 2009-12-29 | 2013-01-16 | 北京有色金属研究总院 | Process and equipment for preparing anisotropic rare-earth permanent-magnet powder and product prepared thereby |
| CN102568736A (en) * | 2010-12-21 | 2012-07-11 | 上海爱普生磁性器件有限公司 | Rigid anisotropy bonded neodymium iron boron permanent magnet |
| CN102768890A (en) * | 2012-08-10 | 2012-11-07 | 北矿磁材科技股份有限公司 | Preparation method of rare earth anisotropism magnetic powder, magnetic powder and magnetic body |
| CN102768890B (en) * | 2012-08-10 | 2015-06-10 | 北矿磁材科技股份有限公司 | Preparation method of rare earth anisotropism magnetic powder, magnetic powder and magnetic body |
| CN103559971A (en) * | 2013-10-22 | 2014-02-05 | 江西江钨稀有金属新材料有限公司 | Nanometer rare earth permanent magnetic material with high-temperature stability and preparation method thereof |
| CN104716753A (en) * | 2014-11-25 | 2015-06-17 | 宁波金鸡强磁股份有限公司 | Magnet with low pole-arc coefficient and manufacturing method thereof |
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