CN1905088A - Method for preparing high coercive force sintering rare-earth-iron-p permanent magnetic material - Google Patents

Method for preparing high coercive force sintering rare-earth-iron-p permanent magnetic material Download PDF

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CN1905088A
CN1905088A CN 200610089124 CN200610089124A CN1905088A CN 1905088 A CN1905088 A CN 1905088A CN 200610089124 CN200610089124 CN 200610089124 CN 200610089124 A CN200610089124 A CN 200610089124A CN 1905088 A CN1905088 A CN 1905088A
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powder
terbium
dysprosium
ndfeb
heat treatment
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CN100394518C (en
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岳明
张久兴
张东涛
曹爱利
刘卫强
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Beijing University of Technology
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Abstract

The invention relates to the method used to make rare earth-iron-boron permanent magnetic material with high coercive force which belongs to magnetic material field. The excellent magnetism of the NdFeB permanent magnetism will be obviously reduced while the working environment temperature rises. The invention includes the following steps: using rapid hardening slice technology to make NdFeB rapid hardening slice; smashing to powder with 3-5 micron; making terbium and dysprosium powder with 10-50nm; mixing them with 1-3% weight ratio; orientating at 2.5T magnetic field; processing secondary heat treatment after 2-4 hours sintering at 1050-1120 centigrade degree; the first order heat treatment is at 900-1000 degree centigrade for 1-3h; the secondary is at 550-700 degree centigrade for 1-3h. The invention has better coercive force and lower terbium and dysprosium content compared with the traditional NdFeB permanent magnetic material.

Description

A kind of method for preparing the high coercive force sintering rare-earth-iron-p permanent magnetic material
Technical field
A kind of preparation has the method for the rare earth-iron-B permanent magnetic material of high-coercive force, belongs to technical field of magnetic materials.
Background technology
The sintered ndfeb permanent magnet typical case of the rare earth-iron-B permanent magnetic material (representative) is the best permanent magnetic material of present magnetic property, is widely used in numerous areas such as automobile, motor, instrument and medicine equipment, is with fastest developing speed a kind of in the magnetic material.But significant disadvantages of this class magnet ubiquity is promptly compared with permanent magnetic materials such as SmCo, aluminium nickel cobalts, has relatively poor temperature stability.In other words, the excellent magnetic of sintered ndfeb permanent magnet can significantly reduce along with the rising of operating ambient temperature (comprising multiple parameters such as remanent magnetism, coercive force and magnetic energy product).This shortcoming makes the sintered ndfeb permanent magnet material can't be applied in the field that working temperature is had relatively high expectations, and as starter motor of automobile or the like, thereby has limited the scope of application of this class material to a great extent.
In order to address this problem, people have carried out extensive studies work.A kind of effective solution is to add the metallic cobalt element of certain content in material, improves the Curie temperature of material, thereby improves its temperature characterisitic.But this method has difficulties in actual applications, and its reason is that the metallic element cobalt is a kind of strategic element, and price is very expensive.And a large amount of cheap as the NdFeB permanent magnetism of civil use material, if add more cobalt element, its manufacturing cost can significantly improve.This is the application of limiting material greatly undoubtedly.By comparison, a kind of effective and practical method is to add the heavy rare earth element terbium or the dysprosium of trace in the sintered ndfeb permanent magnet material at present.The interpolation of trace terbium and dysprosium can effectively improve the coercive force of material, and coercitive raising has remarkable effect for the temperature stability of improving magnet.Simultaneously,, only account for about the 2-4% of magnet gross mass because the addition of terbium and dysprosium is very little, little to the manufacturing cost influence of magnet.Therefore, thisly in the industrial production of current sintered ndfeb permanent magnet material, obtained adopting widely by improving the technology that the magnet coercive force improves its temperature stability.
Regrettably, the practical technique of above-mentioned this interpolation terbium and dysprosium also exists some problems.At first, when single terbium and dysprosium join in the sintered ndfeb permanent magnet material, can form the TeFeB or the DyFeB compound that are similar to NdFeB, though this compounds helps improving the coercive force of magnet, but can cause the remarkable decline of material remanent magnetism simultaneously, thereby cause the magnet magnetic energy product to descend.In other words, improve the magnet coercive force so that temperature stability is to be cost with the magnetic property that reduces magnet, this obviously is disadvantageous.Secondly, although the addition of terbium and dysprosium is little, the price of these heavy rare earth elements but is higher than light rare earth element such as Nd far away.Therefore,, then help reducing manufacturing cost more, thereby further enlarge the range of application of material if can further reduce the addition of terbium and dysprosium.And the difficulty that faces is, adopts present manufacturing technology, and the addition of terbium and dysprosium can't reduce, otherwise just can't play the effect that improves coercive force and improve temperature stability.
At present the addition manner that adopts is to add in foundry alloy, so terbium and dysprosium are evenly to be present in the magnet substantially.And,, form TeFeB or DyFeB compound if can on the boundary layer of principal phase NdFeB crystal grain, introduce one deck terbium and dysprosium according to the coercive force theory of sintered ndfeb permanent magnet material, just can obtain good effect.At first, can reduce TeFeB or the DyFeB ratio in the sintered ndfeb permanent magnet material like this, thereby reduce negative effect, simultaneously the purpose that can also realize improving coercive force and improve temperature characterisitic magnet remanent magnetism and magnetic energy product.Secondly, the addition of terbium and dysprosium can significantly reduce thus, thereby helps reducing the manufacturing cost of material.
At present, some relevant reports have been arranged.Prior art is carried out the coating of terbium and dysprosium respectively to magnet surface, utilize the method for diffusion to make terbium and dysprosium then respectively on the border of principal phase NdFeB crystal grain and form one deck TeFeB or the DyFeB compound, thereby realized raising material coercive force, improved its temperature stability, avoided declining to a great extent of magnet remanent magnetism and magnetic energy product simultaneously.This is particularly in the automobile field of magnets, significant for the expansion of Sintered NdFeB range of application.On the other hand, participating in the addition that these technology can effectively reduce terbium and dysprosium in the sintered magnet, is very favourable from the angle of manufacturing cost.But there is a restriction simultaneously in these patented technologies, and promptly the high-coercive force magnet by the diffusion method preparation has considerable restraint on overall dimension, and the thickness of magnet can not be above 5 millimeters.In other words, utilize these technology can only prepare the small size magnet.And the technology of relevant unconfined this class magnet of preparation size is not appeared in the newspapers at present.
Summary of the invention
At above-mentioned present Research, the present invention adopts the nano-powder particles adding technique preparation of rare earth element terbium and dysprosium to have the sintered ndfeb permanent magnet material of high-coercive force and excellent magnetic energy concurrently.Test result shows, compares with the sintered ndfeb permanent magnet material that the conventional art of identical nominal composition prepares, and adopts the magnet of the technology of the present invention preparation not only to have higher coercive force.In addition, compare with having quite coercitive sintered ndfeb permanent magnet material, the terbium of the required interpolation of magnet of employing the technology of the present invention preparation and the ratio (being the quality percentage composition) of dysprosium significantly reduce.
The purpose of this invention is to provide a kind of by adding the coercitive method of nano-powder particles raising sintered ndfeb permanent magnet material of rare earth element terbium and dysprosium.
A kind of method for preparing the high coercive force sintering rare-earth-iron-p permanent magnetic material provided by the invention is characterized in that, may further comprise the steps:
(1) adopts rapid hardening thin slice prepared NdFeB rapid hardening thin slice, pulverize preparation 3-5 micron NdFeB material powder with the quick-fried method of hydrogen with the alloy sheet fragmentation and by airflow milling afterwards;
(2) adopt physical gas phase deposition technology to prepare and collect the 10-50 nanometer powder of terbium and dysprosium;
(3) prepared terbium and dysprosium nano metal powder are added in the NdFeB powder for preparing in the step (1), adding proportion is the 1-3% of NdFeB powder weight, and two kinds of powder are even;
(4) will in the magnetic field of 2.5T, be orientated and compression moulding through even mixed powder;
(5) pressed compact is inserted in the vacuum sintering furnace, at 1050-1120 ℃ of sintering 2-4 hour, carry out secondary heat treatment afterwards, wherein the one-level heat treatment temperature is 900 ℃-1000 ℃, time 1-3hr; 550 ℃-700 ℃ of secondary heat treatment temperatures, time 1-3hr; Obtain sintered magnet.
NdFeB permanent magnetic material provided by the present invention is characterised in that: prepares the Sintered NdFeB magnet with the conventional art of identical component (containing terbium or dysprosium) and compares, have suitable remanent magnetism and the coercive force that significantly improves, and high slightly magnetic energy product; And have close coercitive conventional art and prepare the Sintered NdFeB magnet and compare, then the quality percentage composition of terbium metal or dysprosium is obviously on the low side.Technology of preparing of the present invention is adopted in the The above results explanation, can effectively improve terbium and dysprosium element interpolation efficient in the Sintered NdFeB magnet.Simultaneously, because the technology of the present invention is to add nanometer terbium and dysprosium particle before the material compacting sintering, therefore can prepare the unrestricted magnet of overall dimension.
Embodiment
Embodiment 1
Utilize the rapid hardening technology that composition is Nd 30.0Fe 67.5Co 1.4B 1.1The alloy of (quality percentage composition) is prepared as thin slice, adopts hydrogen fragmentation-gas flow crushing process powder to be made the powder of 3 microns of average grain diameters subsequently.(in detail referring to Chinese patent: 93115008.6, patent name: rare earth-iron-B permanent magnetic material and this preparation methods, the day for announcing: on January 10th, 1996, publication number: CN 1114779A, following examples are common a kind of this technology that is not limited to of prior art together).
(nanometer powder prepares the patent that detailed process can be applied in earlier stage referring to this seminar: 200510089080.3 Granted publication day: 2006.3.8 with terbium nanometer powders percentage by weight 1%, average grain diameter 10 nanometers afterwards, publication number: CN 1743103 patent names: rare earth nanometer particle and nano crystal material preparation method and equipment following examples thereof are common a kind of this technology that is not limited to of prior art together)
Add in the above-mentioned initial powder, utilize batch mixer that two kinds of powder are mixed uniformly.To in the magnetic field of 2.5T, be orientated and compression moulding through even mixed powder.Then pressed compact is inserted in the high vacuum sintering furnace, 1050 ℃ of sintering 4 hours, carry out secondary heat treatment afterwards, wherein the one-level heat treatment temperature is 950 ℃, time 2hr; 600 ℃ of secondary heat treatment temperatures, time 1hr.Promptly obtain sintered magnet.The every magnetic property index and the density of prepared magnet are listed in the table 1.
Comparative Examples 1
Utilize the rapid hardening technology that composition is Nd 29.7Tb 1.0Fe 66.8Co 1.4B 1.1The alloy of (quality percentage composition) is prepared as thin slice, adopts hydrogen fragmentation-gas flow crushing process powder to be made the powder of 3 microns of average grain diameters subsequently.Powder is orientated in the magnetic field of 2.5T and compression moulding.Then pressed compact is inserted in the high vacuum sintering furnace, 1050 ℃ of sintering 4 hours, carry out secondary heat treatment afterwards, wherein the one-level heat treatment temperature is 950 ℃, time 2hr; 600 ℃ of secondary heat treatment temperatures, time 1hr.Promptly obtain sintered magnet.The every magnetic property index and the density of prepared magnet are listed in the table 1.
The composition that it is pointed out that Comparative Examples 1 alloy is to design with proportioning according to the total composition after two kinds of powder among the embodiment 1, obtains to have the comparing result of two kinds of Sintered NdFeB magnets of identical component thus.
Table 1. adds the sintered magnet magnetic property and the density contrast of 1% terbium element in different ways
The terbium addition manner Remanent magnetism (kGs) Coercive force (kOe) Magnetic energy product (MGOe) Density (g/cm 3)
Nano particle 14.4 16.7 51 7.53
Traditional approach 14.3 13.6 50 7.51
Above presentation of results is for the identical Sintered NdFeB magnet of composition, and the magnet that adopts the present invention to add the terbium preparation has better coercive force than the magnet that adopts traditional approach to add terbium, and remanent magnetism and magnetic energy product are also good slightly in addition.
Embodiment 2
Utilize the rapid hardening technology that composition is Nd 30.0Fe 67.5Co 1.4B 1.1The alloy of (quality percentage composition) is prepared as thin slice, adopts hydrogen fragmentation-gas flow crushing process powder to be made the powder of 4 microns of average grain diameters subsequently.Afterwards dysprosium nanometer powders percentage by weight 3%, average grain diameter 30 nanometers are added in the above-mentioned initial powder, utilize batch mixer that two kinds of powder are mixed uniformly.To in the magnetic field of 2.5T, be orientated and compression moulding through even mixed powder.Then pressed compact is inserted in the high vacuum sintering furnace, 1080 ℃ of sintering 3 hours, carry out secondary heat treatment afterwards, wherein the one-level heat treatment temperature is 900 ℃, time 3hr; 700 ℃ of secondary heat treatment temperatures, time 1hr.Promptly obtain sintered magnet.The every magnetic property index and the density of prepared magnet are listed in the table 2.
Comparative Examples 2
Utilize the rapid hardening technology that composition is Nd 27.5Dy 6.5Fe 63.5Co 1.4B 1.1The alloy of (quality percentage composition) is prepared as thin slice, adopts hydrogen fragmentation-gas flow crushing process powder to be made the powder of 4 microns of average grain diameters subsequently.Powder is orientated in the magnetic field of 2.5T and compression moulding.Then pressed compact is inserted in the high vacuum sintering furnace, 1080 ℃ of sintering 3 hours, carry out secondary heat treatment afterwards, wherein the one-level heat treatment temperature is 900 ℃, time 3hr; 700 ℃ of secondary heat treatment temperatures, time 1hr.Promptly obtain sintered magnet.。The every magnetic property index and the density of prepared magnet are listed in the table 2.
Table 2. 3% dysprosium nano particle adds and 6.5% dysprosium tradition is added sintered magnet magnetic property and density
Terbium addition manner and amount Remanent magnetism (kGs) Coercive force (kOe) Magnetic energy product (MGOe) Density (g/cm 3)
Nano particle 3% 13.0 20.3 40 7.58
Traditional approach 6.5 % 12.8 19.9 38 7.61
Above presentation of results adopts the inventive method and conventional method to prepare the close Sintered NdFeB magnet of coercive force, and there is very big-difference in the interpolation content of required dysprosium.Compare with conventional method, adopt nano particle adding method of the present invention obtaining the remarkable addition that reduces metal dysprosium of close coercitive while.In addition, owing to adopt the inventive method can reduce the addition of dysprosium, therefore the remanent magnetism of magnet and magnetic energy product also are higher than the magnet of conventional method preparation.
Embodiment 3
Utilize the rapid hardening technology that composition is Nd 30.0Fe 67.5Co 1.4B 1.1The alloy of (quality percentage composition) is prepared as thin slice, adopts hydrogen fragmentation-gas flow crushing process powder to be made the powder of 3 microns of average grain diameters subsequently.Afterwards dysprosium nanometer powders percentage by weight 1%, average grain diameter 20 nanometers are added in the above-mentioned initial powder, utilize batch mixer that two kinds of powder are mixed uniformly.To in the magnetic field of 2.5T, be orientated and compression moulding through even mixed powder.Then pressed compact is inserted in the high vacuum sintering furnace, 1100 ℃ of sintering 2 hours, carry out secondary heat treatment afterwards, wherein the one-level heat treatment temperature is 1000 ℃, time 1hr; 550 ℃ of secondary heat treatment temperatures, time 3hr.Promptly obtain sintered magnet.The every magnetic property index and the density of prepared magnet are listed in the table 3.
Table 3. 1% dysprosium nano particle adds sintered magnet magnetic property and density
The terbium addition manner Remanent magnetism (kGs) Coercive force (kOe) Magnetic energy product (MGOe) Density (g/cm 3)
Nano particle 14.3 13.6 50 7.54
Embodiment 4
Utilize the rapid hardening technology that composition is Nd 30.0Fe 67.5Co 1.4B 1.1The alloy of (quality percentage composition) is prepared as thin slice, adopts hydrogen fragmentation-gas flow crushing process powder to be made the powder of 5 microns of average grain diameters subsequently.Afterwards dysprosium nanometer powders percentage by weight 3%, average grain diameter 50 nanometers are added in the above-mentioned initial powder, utilize batch mixer that two kinds of powder are mixed uniformly.To in the magnetic field of 2.5T, be orientated and compression moulding through even mixed powder.Then pressed compact is inserted in the high vacuum sintering furnace, 1120 ℃ of sintering 2 hours, carry out secondary heat treatment afterwards, wherein the one-level heat treatment temperature is 900 ℃, time 2hr; 650 ℃ of secondary heat treatment temperatures, time 2hr.Promptly obtain sintered magnet.The every magnetic property index and the density of prepared magnet are listed in the table 4.
Table 4. 2% dysprosium nano particle adds sintered magnet magnetic property and density
The terbium addition manner Remanent magnetism (kGs) Coercive force (kOe) Magnetic energy product (MGOe) Density (g/cm 3)
Nano particle 13.1 17.2 42 7.55

Claims (1)

1, a kind of method for preparing high-coercive force sintering rare-earth-iron-B permanent magnetic material is characterized in that, may further comprise the steps:
1) adopts rapid hardening thin slice prepared NdFeB rapid hardening thin slice, pulverize preparation 3-5 micron NdFeB material powder with the quick-fried method of hydrogen with the alloy sheet fragmentation and by airflow milling afterwards;
2) adopt physical gas phase deposition technology to prepare and collect the 10-50 nanometer powder of terbium and dysprosium;
3) prepared terbium and dysprosium nano metal powder are added in the NdFeB powder for preparing in the step 1), adding proportion is the 1-3% of NdFeB powder weight, and two kinds of powder are even;
4) will in the magnetic field of 2.5T, be orientated and compression moulding through even mixed powder;
5) pressed compact is inserted in the vacuum sintering furnace, at 1050-1120 ℃ of sintering 2-4 hour, carry out secondary heat treatment afterwards, wherein the one-level heat treatment temperature is 900 ℃-1000 ℃, time 1-3hr; 550 ℃-700 ℃ of secondary heat treatment temperatures, time 1-3hr; Obtain sintered magnet.
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CN101847487A (en) * 2010-06-30 2010-09-29 烟台正海磁性材料股份有限公司 Gradient coercive-force neodymium-ferrum-boron magnet and production method thereof
CN101521069B (en) * 2008-11-28 2011-11-16 北京工业大学 Method for preparing heavy rare earth hydride nano-particle doped sintered NdFeB permanent magnet
CN102294479A (en) * 2011-08-30 2011-12-28 宁波韵升股份有限公司 Method for preparing sintered neodymium iron boron device
CN101572146B (en) * 2008-05-04 2012-01-25 比亚迪股份有限公司 Nd-Fe-B permanent magnetic material and preparing method thereof
CN101447268B (en) * 2007-11-26 2012-08-22 比亚迪股份有限公司 Neodymium iron boron permanent magnetic material and preparation method thereof
CN102655050A (en) * 2012-05-04 2012-09-05 江苏大学 Method for preparing high-performance high-temperature-resisting nanometer composite permanent magnet
CN103646777A (en) * 2013-12-11 2014-03-19 江苏大学 Method for preparing crystal boundary nano-composite intensified neodymium iron boron magnet
WO2014059772A1 (en) * 2012-10-17 2014-04-24 中磁科技股份有限公司 High corrosion-resistant re-(fe, tm)-b magnet and preparing method thereof
CN103956244A (en) * 2014-05-14 2014-07-30 辽宁五寰科技发展有限公司 Preparation method for high-coercivity sintered neodymium-iron-boron
CN104091666A (en) * 2014-08-04 2014-10-08 梁家新 Method for preparing neodymium-iron-boron permanent magnet material through nanometer modification
CN109065314A (en) * 2018-09-07 2018-12-21 京磁材料科技股份有限公司 The preparation method of high-coercivity magnet

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RU2113742C1 (en) * 1993-07-06 1998-06-20 Сумитомо Спешиал Металз Ко., Лтд. Permanent-magnet materials and their manufacturing processes
JP2005281795A (en) * 2004-03-30 2005-10-13 Tdk Corp R-T-B BASED SINTERED MAGNET ALLOY CONTAINING Dy AND Tb AND ITS PRODUCTION METHOD
CN1743103A (en) * 2005-08-05 2006-03-08 北京工业大学 Rear-earth nano granule and nano crystal material preparing method and apparatus

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101447268B (en) * 2007-11-26 2012-08-22 比亚迪股份有限公司 Neodymium iron boron permanent magnetic material and preparation method thereof
CN101572146B (en) * 2008-05-04 2012-01-25 比亚迪股份有限公司 Nd-Fe-B permanent magnetic material and preparing method thereof
CN101521069B (en) * 2008-11-28 2011-11-16 北京工业大学 Method for preparing heavy rare earth hydride nano-particle doped sintered NdFeB permanent magnet
CN101847487A (en) * 2010-06-30 2010-09-29 烟台正海磁性材料股份有限公司 Gradient coercive-force neodymium-ferrum-boron magnet and production method thereof
CN102294479A (en) * 2011-08-30 2011-12-28 宁波韵升股份有限公司 Method for preparing sintered neodymium iron boron device
CN102294479B (en) * 2011-08-30 2013-11-13 宁波韵升股份有限公司 Method for preparing sintered neodymium iron boron device
CN102655050A (en) * 2012-05-04 2012-09-05 江苏大学 Method for preparing high-performance high-temperature-resisting nanometer composite permanent magnet
WO2014059772A1 (en) * 2012-10-17 2014-04-24 中磁科技股份有限公司 High corrosion-resistant re-(fe, tm)-b magnet and preparing method thereof
CN103646777A (en) * 2013-12-11 2014-03-19 江苏大学 Method for preparing crystal boundary nano-composite intensified neodymium iron boron magnet
CN103956244A (en) * 2014-05-14 2014-07-30 辽宁五寰科技发展有限公司 Preparation method for high-coercivity sintered neodymium-iron-boron
CN104091666A (en) * 2014-08-04 2014-10-08 梁家新 Method for preparing neodymium-iron-boron permanent magnet material through nanometer modification
CN109065314A (en) * 2018-09-07 2018-12-21 京磁材料科技股份有限公司 The preparation method of high-coercivity magnet

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