CN101178962B - Non-pressure preparation method of rare-earth-iron-boron sintered magnetic material - Google Patents
Non-pressure preparation method of rare-earth-iron-boron sintered magnetic material Download PDFInfo
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- CN101178962B CN101178962B CN200710071189A CN200710071189A CN101178962B CN 101178962 B CN101178962 B CN 101178962B CN 200710071189 A CN200710071189 A CN 200710071189A CN 200710071189 A CN200710071189 A CN 200710071189A CN 101178962 B CN101178962 B CN 101178962B
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Abstract
The invention relates to a non-pressure preparation method for sintered magnetic material of rare earth-Fe-B, which includes the following steps: adopting a common ingot method to prepare alloy ingots with a thickness of 10-20mm, filling magnetic powders with a granularity of 1-5 microns into dies in different shapes and with different specifications after the magnetic power is crushed coarsely and grinded by airflow, placing the magnetic powders and dies together in a vacuum sintering furnace after magnetic orientation for sintering, and at last obtaining the sintered permanent magnetic material of rare earth-Fe-B after tempering treatment. The sintered magnetic material of rare earth-Fe-B prepared by the method has the advantages of small processing volume, high utilization rate of material, less product cost, etc.
Description
Technical field
The present invention relates to a kind of preparation method of magnetic material, relate in particular to a kind of non-pressure preparation method of rare-earth-iron-boron sintered magnetic material.
Background technology
Rare earth permanent-magnetic material as the new material important component part, be widely used in industries such as the energy, traffic, machinery, medical treatment, IT, household electrical appliances, its product relates to a lot of fields of national economy, and its output and consumption also become one of important symbol of weighing a national overall national strength and national economic development level.Rare earth (mainly being neodymium)-iron-B permanent magnetic material is as third generation rare earth permanent-magnetic material, be known as with its high-performance " magnetic king ", and owing to account for abundant, the iron low price of the neodymium reserves of main content, so with first and second in generation rare earth permanent-magnetic material compare and have the very high ratio of performance to price, therefore all obtained growing continuously and fast in scientific research, production, application facet in recent years.The advantage of China's and human resources abundant particularly with the rare earth reserves, the development of sintered Nd-Fe-B permanent magnetic material increases rapidly, and output was from 50 tons of 50,000 tons of bringing up to 2006 in 1985, and the sintered NdFeB output of China has been sure to occupy the first in the world now.
NdFeB material is mainly used in voice coil motor (VCM), NMR imaging instrument (MRI), all kinds of motor and various audio-video equipment, microwave communication, magnetic machinery (magnetic drive pump, magnet valves), household electrical appliance of computer disc driver etc.
In the process that mind-set China shifts in world's manufacturing industry, new material industry, new material industry as the new high-tech industry basis gets most of the attention, as the rare earth permanent-magnetic material of new material industry important component part, especially the neodymium iron boron industry has also entered key developing period; The sintered NdFeB output of China in 2005 has accounted for 70% of whole world total value.And, just because of a large amount of supplies of China's sintered neodymium iron boron material, make and develop into being applied to every field by the expensive NdFeB material that only is used for the part high-tech industry originally, directly promoted the application and the development of sintered neodymium iron boron material.
Along with progress of science and technology, new method and new technology continues to bring out now.As the Nd Fe B alloys ingot casting is transformed into thin plate ingot casting about 20mm from the cylindric ingot casting of routine, sheet ingot casting to about the 2mm again, the improvement of technical process mainly is to reach the content that reduces and eliminate α-Fe in the alloy cast ingot by the cooling rate that improves ingot casting, makes Nd
2Fe
14Tiny even, the rich neodymium of B principal phase crystallization is evenly distributed between the main phase grain mutually.Adopt this sheet ingot casting can obtain higher magnetic energy product and coercive force.
Emerging in large numbers of present various new technologies all is improvement or the innovation of carrying out round each operation of this technology of powder metallurgical technique; but when moulding, all adopt mould (metal pattern or rubber die) compression moulding (perhaps first precompressed; wait static pressure then); the demoulding is then packed product placement into and to be carried out sintering in the sintering furnace in the product holder.Generally speaking, require green density high more good more, as be of a size of the product of 52 * 52 * 29 specifications, behind the static pressure such as process, the performance of final magnet is good, shrinks evenly.The product that sintering comes out mostly is cylinder or square, again the sintering blank is cut into all sizes such as disk, annulus, blockage or magnetic shoe through section or line according to customer demand.In the courses of processing such as section and line cutting, produce a large amount of stub bars and edge of a knife material powder, wasted a large amount of NdFeB materials, product size is more little, the edge of a knife is wasted big more more at most.Sometimes the utilance of material only 50%.
Summary of the invention
The present invention is directed to existing moulding process and cause the serious problem of following process waste of material, a kind of sintered NdFeB non-pressure preparation method is provided, the Sintered NdFeB magnet that makes by this method only need subsequent handling such as just can electroplate through surfacing processing, has significantly reduced the waste of material.
Above-mentioned technical problem of the present invention is mainly solved by following technical proposals: a kind of non-pressure preparation method of rare-earth-iron-boron sintered magnetic material, and this method may further comprise the steps:
(1) preparation Magnaglo: the composition according to the rare-earth-iron-boron sintered magnetic material that designs carries out preparation raw material, is 1～5 micron Magnaglo then with raw material acquisition granularity after melting, grinding;
(2) dress mould, vibration: the above-mentioned Magnaglo that makes is encased in the mould, by mechanical oscillation Magnaglo is evenly distributed in mould then;
(3) magnetic field orientating, sintering: the magnetic after the above-mentioned vibration is put into D.C. magnetic field or impulse magnetic field orientation; Put into after the orientation and carry out sintering and temper in the sintering furnace, promptly obtain required rare-earth-iron-boron sintered magnetic material after the temper.
The present invention fully according to the characteristics of rare-earth-iron-boron magnetic material, adopts and does not have the production technology of pressure, significantly reduces the waste of material, and the rare-earth-iron-boron magnetic material product cost of making is low, and the market competitiveness is strong.
In the non-pressure preparation method of above-mentioned rare-earth-iron-boron sintered magnetic material, the mould described in the step (2) becomes disk or watt type; Wherein die cavity adopts not magnetic conduction or the low material of magnetic permeability to make, and die head adopts magnetic conduction or the high material of magnetic permeability to make up and down.Die head adopts magnetic conduction or the high material of magnetic permeability to make so that the orientation of magnetic wherein obtains the high magnet of the degree of orientation up and down; The degree of orientation is high more, and the performance of magnet is good more.
In the non-pressure preparation method of above-mentioned rare-earth-iron-boron sintered magnetic material, the density of vibration back magnetic is 0.5～3.5 * 10 in the step (2)
3Kilograms per cubic meter.If the too big needed cost of density of vibration back magnetic is higher.
In the non-pressure preparation method of above-mentioned rare-earth-iron-boron sintered magnetic material, the D.C. magnetic field described in the step (3) or the intensity 〉=15kOe of impulse magnetic field.Alignment magnetic field is too little, is unfavorable for the orientation of magnetic, and the magnetic property of the rare-earth-iron-boron sintered magnetic material of making is just low.
As preferably, in the step (3) the above-mentioned mould that magnetic is housed is placed on sintering in the vacuum air-quenching furnace, adopt vacuum or high purity argon protection sintering, sintering temperature is 900 ℃～1100 ℃, sintering time is 1～4 hour; Then the magnet that sinters is carried out one-level or two-stage temper, temper all adopts the gas quenching but or air cooling or furnace cooling; Wherein first order temper temperature is 600～950 ℃, and the time is 1～3 hour, and when adopting the two-stage temper, second level temper temperature is 350～600 ℃, and the time is 2～6 hours.
In sum, the present invention has the following advantages:
What the non-pressure preparation method of rare-earth-iron-boron sintered magnetic material of the present invention adopted is no compression technology technology, the Sintered NdFeB magnet that makes only need just can carry out subsequent handling (as electroplating, magnetize etc.) through surfacing processing, reduced the waste of material, improve rate of finished products, reduced product cost.
Description of drawings
Fig. 1 is the structural representation of magnetic shoe mould of the present invention;
Fig. 2 is along the A A sectional structure schematic diagram among Fig. 1;
Fig. 3 is the structural representation of disk of the present invention or cylindrical magnetic mould;
Fig. 4 is along the B B sectional structure schematic diagram among Fig. 3;
Among the figure, 1, the die cavity of magnetic shoe mould; 2, the last die head of magnetic shoe mould; 3, the lower die head of magnetic shoe mould; 4, the die cavity of disk or cylindrical magnet mould; 5, the last die head of disk or cylindrical magnet mould; 6, the lower die head of disk or cylindrical magnet mould.
Embodiment
Below by embodiment, and in conjunction with the accompanying drawings, technical scheme of the present invention is described in further detail; But the present invention is not limited to these embodiment.
As depicted in figs. 1 and 2: the mould that the present invention prepares rare-earth-iron-boron sintered magnetic shoe includes the die cavity (1) of magnetic shoe mould, and described die cavity adopts not magnetic conduction or the low material of magnetic permeability to make, and magnetic is equipped with in inside; The die cavity top is provided with the last die head (2) of magnetic shoe mould, and the bottom is provided with the lower die head (3) of magnetic shoe mould; Described magnetic shoe mould last die head (2) and the lower die head (3) of magnetic shoe mould make by magnetic conduction or the high material of magnetic permeability; So that in D.C. magnetic field or pulsed magnetic field, be orientated;
As shown in Figure 3 and Figure 4: the mould that the present invention prepares rare-earth-iron-boron sintered cylinder or disk magnet includes the die cavity (4) of disk or cylindrical magnet mould, and described die cavity adopts not magnetic conduction or the low material of magnetic permeability to make, and magnetic is equipped with in inside; The die cavity top is provided with the last die head (5) of disk or cylindrical magnet mould, and the bottom is provided with the lower die head (6) of disk or cylindrical magnet mould; The last die head (5) of described disk or cylindrical magnet mould and lower die head (6) are made by magnetic conduction or the high material of magnetic permeability; So that in D.C. magnetic field or pulsed magnetic field, be orientated;
Press design mix Nd
23.3Pr
5Dy
2Tb
0.2Fe
66.5Co
1Al
0.5Nb
0.5B
1(mass fraction, %) preparation raw material, and it is smelted into alloy pig, and broken then alloy pig, through the airflow milling grind into powder, the particle mean size of magnetic is 4.1 microns.Above-mentioned powder is packed in as depicted in figs. 1 and 2 the mould, in the magnetic field of 19kOe, be orientated, sintering in vacuum air-quenching furnace then, 1070 ℃ of sintering temperatures, sintering time is 3 hours, and first order temper temperature is 900 ℃, and the time is 2.5 hours, second level temper temperature is 500 ℃, and the time is 2 hours; Obtain magnetic shoe after the applying argon gas cooling, it is as shown in table 1 to test its magnetic property:
The magnetic property of table 1: embodiment 1
| Magnetic property | Br (kGs) | Hcb (kOe) | Hcj (kOe) | Hk (kOe) | (BH)m (MGOe) |
| |
13.18 | 12.78 | 17.20 | 16.64 | 42.1 |
Press design mix Nd
22Pr
3Dy
5Tb
2Fe
61.82Co
3Nb
1Al
0.5Cu
0.5Ga
0.1B
1.08(mass fraction, %) preparation raw material, and it is smelted into alloy pig, broken then alloy pig, through the airflow milling grind into powder, the particle mean size of magnetic is 4 microns, above-mentioned powder is packed in as shown in Figure 3 and Figure 4 the mould, in the magnetic field of 19.5kOe, be orientated sintering in vacuum air-quenching furnace, 1065 ℃ of sintering temperatures, sintering time is 3 hours, and first order temper temperature is 900 ℃, and the time is 3 hours, second level temper temperature is 500 ℃, and the time is 2 hours.Obtain cylindrical magnet after the applying argon gas cooling, it is as shown in table 2 to test its magnetic property;
The magnetic property of table 2: embodiment 2
| Magnetic property | Br (kGs) | Hcb (kOe) | Hcj (kOe) | (BH)m (MGOe) |
| |
11.34 | 11.18 | 33.2 | 32.4 |
Shown in table 1 and table 2, it is better that the present invention makes the magnetic property of rare-earth iron-boron sintering magnetic shoe and cylindrical magnet, but need not compression moulding, make magnetic shoe and magnet and only need just can carry out subsequent handling (as electroplating, magnetize etc.) through surfacing processing, reduced the waste of material, improve rate of finished products, reduced product cost.
Specific embodiment described herein only is that the present invention's spirit is illustrated.The technical staff of the technical field of the invention can make various modifications or replenishes or adopt similar mode to substitute described specific embodiment, but can't depart from spirit of the present invention or surmount the defined scope of appended claims.
Although the present invention has been made detailed explanation and has quoted some instantiations as proof, to those skilled in the art, only otherwise leave that the spirit and scope of the present invention can be done various variations or correction is obvious.
Claims (3)
1. the non-pressure preparation method of a rare-earth-iron-boron sintered magnetic material, this method may further comprise the steps:
(1) preparation Magnaglo: the composition according to the rare-earth-iron-boron sintered magnetic material that designs carries out preparation raw material, is 1～5 micron Magnaglo then with raw material acquisition granularity after melting, grinding;
(2) dress mould, vibration: the above-mentioned Magnaglo that makes is encased in the mould, by mechanical oscillation Magnaglo is evenly distributed in mould then; The density of vibration back magnetic is 0.5～3.5 * 10
3Kilograms per cubic meter;
(3) magnetic field orientating, sintering: the magnetic after the above-mentioned vibration is put into D.C. magnetic field or impulse magnetic field orientation with mould; Intensity 〉=the 15kOe of D.C. magnetic field or impulse magnetic field; Put into after the orientation and carry out sintering and temper in the sintering furnace, promptly obtain required rare-earth-iron-boron sintered magnetic material after the temper.
2. the non-pressure preparation method of a kind of rare-earth-iron-boron sintered magnetic material according to claim 1, it is characterized in that: the mould described in the step (2) becomes disk or watt type; Wherein die cavity adopts non-magnet_conductible material to make, and die head adopts the material of magnetic conduction to make up and down.
3. the non-pressure preparation method of a kind of rare-earth-iron-boron sintered magnetic material according to claim 1, it is characterized in that, the mould that magnetic will be housed in the step (3) is placed on sintering in the vacuum air-quenching furnace, adopt vacuum or high purity argon protection sintering, sintering temperature is 900 ℃～1100 ℃, and sintering time is 1～4 hour; Then the magnet that sinters is carried out one-level or two-stage temper, temper all adopts the gas quenching but or air cooling or furnace cooling; Wherein first order temper temperature is 600～950 ℃, and the time is 1～3 hour, and when adopting the two-stage temper, second level temper temperature is 350～600 ℃, and the time is 2～6 hours.
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| CN200710071189A CN101178962B (en) | 2007-09-18 | 2007-09-18 | Non-pressure preparation method of rare-earth-iron-boron sintered magnetic material |
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|---|---|---|---|
| CN200710071189A CN101178962B (en) | 2007-09-18 | 2007-09-18 | Non-pressure preparation method of rare-earth-iron-boron sintered magnetic material |
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| CN101178962B true CN101178962B (en) | 2010-05-26 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120176212A1 (en) * | 2009-08-28 | 2012-07-12 | Intermetallics Co., Ltd. | METHOD AND SYSTEM FOR PRODUCING SINTERED NdFeB MAGNET, AND SINTERED NdFeB MAGNET PRODUCED BY THE PRODUCTION METHOD |
| KR101707362B1 (en) * | 2013-02-05 | 2017-02-15 | 인터메탈릭스 가부시키가이샤 | Sintered magnet production method |
| CN103286313A (en) * | 2013-06-26 | 2013-09-11 | 苏州唐氏机械制造有限公司 | Mold for sintering powder |
| CN104668558A (en) * | 2015-03-10 | 2015-06-03 | 济南大学 | Pressing die for round powder metallurgy material green body |
| CN106409456B (en) * | 2016-08-26 | 2018-09-07 | 宁波同创强磁材料有限公司 | A kind of rare earth permanent magnet preparation process improving magnetic property |
| CN106158210A (en) * | 2016-08-30 | 2016-11-23 | 赣州鑫磊稀土新材料股份有限公司 | The method of sintered NdFeB is prepared in a kind of pressureless compacting |
| JP7196468B2 (en) * | 2018-08-29 | 2022-12-27 | 大同特殊鋼株式会社 | RTB system sintered magnet |
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| US4431604A (en) * | 1980-01-24 | 1984-02-14 | Nippon Gakki Seizo Kabushiki Kaisha | Process for producing hard magnetic material |
| CN1258919A (en) * | 1998-12-28 | 2000-07-05 | 北京市石景山区京磁技术公司 | Forming method of sintered anisotropic magnet |
| CN1306286A (en) * | 1999-08-17 | 2001-08-01 | 三荣化成株式会社 | Method of sintering permanent magneto |
| CN1570155A (en) * | 2004-04-29 | 2005-01-26 | 山西汇镪磁性材料制作有限公司 | Sintered Nd Iron boron permanent magnet tempering process |
| CN1937112A (en) * | 2006-09-21 | 2007-03-28 | 上海交通大学 | Method for increasing neodymium-iron-boron permanent magnetic performance and corrosion-resisting performance |
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2007
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4431604A (en) * | 1980-01-24 | 1984-02-14 | Nippon Gakki Seizo Kabushiki Kaisha | Process for producing hard magnetic material |
| CN1258919A (en) * | 1998-12-28 | 2000-07-05 | 北京市石景山区京磁技术公司 | Forming method of sintered anisotropic magnet |
| CN1306286A (en) * | 1999-08-17 | 2001-08-01 | 三荣化成株式会社 | Method of sintering permanent magneto |
| CN1570155A (en) * | 2004-04-29 | 2005-01-26 | 山西汇镪磁性材料制作有限公司 | Sintered Nd Iron boron permanent magnet tempering process |
| CN1937112A (en) * | 2006-09-21 | 2007-03-28 | 上海交通大学 | Method for increasing neodymium-iron-boron permanent magnetic performance and corrosion-resisting performance |
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