CN104759628A - Method for preparing heat-resistance sintering NdFeB permanent magnet material - Google Patents
Method for preparing heat-resistance sintering NdFeB permanent magnet material Download PDFInfo
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- CN104759628A CN104759628A CN201510036814.5A CN201510036814A CN104759628A CN 104759628 A CN104759628 A CN 104759628A CN 201510036814 A CN201510036814 A CN 201510036814A CN 104759628 A CN104759628 A CN 104759628A
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Abstract
The invention discloses a method for preparing a heat-resistance sintering NdFeB permanent magnet material without heavy rare earth elements. The preparing method comprises the following detailed steps of (1) preparing an NdFeB alloy and an SmCo alloy sheet by adopting a vacuum rapid-hardening method; (2) respectively crushing said two alloys into powder; (3) fully mixing said powder according to a certain proportion; (4) after vacuum drying mixed powder, orientation compression molding under magnetic fields, and then performing cold isostatic pressing to molded blanks; (5) sintering green bodies and performing twice thermal treatment, preparing the heat-resistance sintering NdFeB permanent magnet material. The preparing method has the beneficial effects that tiny SmCo phase grains are doped among Nd2Fe14B phase grains of the materials through a fine-grained doped technology, and the NdFeB permanent magnet material with high residual magnetism, and high coercive force and temperature stability is prepared without adding Dy, Tb and other heavy metal based on high coercive force and good temperature stability in the SmCo phase grains.
Description
Technical field
The present invention relates to rare earth permanent-magnetic material correlative technology field, refer in particular to a kind of preparation method of high temperature resistant sintered NdFeB permanent magnets.
Background technology
Rare earth permanent-magnetic material is the class high performance permanent magnetic materials formed with transition metal TM (Fe, Co etc.) by rare-earth element R (Sm, Nd, Pr etc.).Up to the present this kind of material comprises first generation RCo
5system, second generation R
2co
17system and third generation NdFeB system rare earth permanent-magnetic material.Wherein, third generation NdFeB system rare earth permanent-magnetic material is the class permanent-magnet material that magnetic property is best up to now, its theoretical magnetic energy product up to 64MGOe, considerably beyond the SmCo of the first generation
5the SmCo rare earth permanent magnet of rare earth permanent magnet and the second generation.And the Fe element maximum due to content in NdFeB material is cheap, its price will far below SmCo5 rare earth permanent magnet and SmCo rare earth permanent magnet, is the maximum rare earth permanent-magnet material of Vehicles Collected from Market consumption.
Adopt the Sintered NdFeB ternary permanent-magnet material prepared of traditional handicraft, although have good magnetic property, coercivity is lower and temperature stability is poor, limits its further use at automotive field.In order to improve the coercivity of sintered ndfeb permanent magnet and improve its temperature stability, people have attempted various method, magnetic phase Nd as main in refinement
2fe
14the crystallite dimension of B compound, improve material crystal boundary pattern, add other alloying elements etc.Wherein most effective method adds the heavy rare earth elements such as Dy, Tb, makes it to replace main magnetic phase Nd
2fe
14rare earth element nd in B compound, makes its anisotropy field and coercivity be greatly improved.But, be that anti-ferromagnetism is coupled between heavy rare earth element with transition element Fe, the remanent magnetism of magnet after interpolation, can be caused to reduce.On the other hand, the heavy rare earth elements such as Dy, Tb reserves are on earth very low, and distribution dispersion, be difficult to exploitation, therefore price is very expensive, greatly improves the material cost of sintered ndfeb permanent magnet after interpolation.Making NdFeB magnet obtain high-coercive force and high-temperature stability under the condition of therefore how to add in burning, even not adding the heavy rare earth elements such as Dy, Tb, is the focus of current numerous researchers' research.
Find through carrying out retrieval to prior art document, a kind of preparation method of ultra-high coercive force sintered Nd-Fe-B magnetic material is disclosed in Chinese patent CN 1862717A, but its Dy content is 3%-10%, Tb content is 0%-6%, heavy rare earth content is very high, from the angle of economy, very do not calculate; A kind of preparation method of low heavy rare earth high-coercive force Sintered NdFeB magnet is disclosed in Chinese patent CN103824668A, the method compensates mutually by adopting the rich neodymium of rare earth element powder to neodymium iron boron, reduce the use amount of heavy rare earth element, although the method can the consistent high-coercivity magnet of production performance, still need to add a small amount of heavy rare earth element; Disclose a kind of R-T-B-M based sintered magnet alloy and manufacture method thereof in FDAC metal Co., Ltd. patent CN102361998A, although the method reduces the use amount of heavy rare earth, but still inevitably employ a part of heavy rare earth element; Hitachi of Amada Co., Ltd. patent CN 103021613A discloses a kind of manufacture method of sintered magnet, it adopts and is gathered near the crystal boundary of NdFeB tying intracrystalline by FeCo or heavy rare earth element, realize the magnet preparing high magnetic characteristics, high-coercive force under the condition of low heavy rare earth, but the FeCo alloy in this patent as a class soft magnetism be gathered in mutually crystal boundary whether be conducive to coercivity improve there is theoretic query, and this patent still inevitably employs heavy rare earth element Dy and Tb.
Summary of the invention
There is above-mentioned deficiency to overcome in prior art in the present invention, provides a kind of preparation method not adding the high temperature resistant sintered NdFeB permanent magnets of heavy rare earth element.
To achieve these goals, the present invention is by the following technical solutions:
A preparation method for high temperature resistant sintered NdFeB permanent magnets, concrete preparation process is as follows:
(1) method of vacuum rapid hardening is adopted to prepare NdFeB alloy and SmCo alloy sheet;
(2) two kinds of alloys are broken into powder respectively;
(3) two kinds of powder are fully mixed according to a certain percentage;
(4) mixed-powder after vacuum drying again under magnetic field orientation compressing, then the blank after shaping is carried out isostatic cool pressing;
(5) base substrate to be sintered and 2 heat treatment, obtained high temperature resistant sintered NdFeB permanent magnets.
In the preparation process of sintered NdFeB magnet, the crystal boundary composition of sintered NdFeB magnet and distribution have great impact to the coercivity of magnet, and the rich-Nd phase of fcc structure can isolate adjacent Nd
2fe
14magnetic coupling interaction between B phase crystal grain, makes the coercivity of magnet be kept.But, the present inventor in the recent period through repeatedly testing discovery, if intercrystalline rich-Nd phase to be replaced with the Dy of high-coercive force
2fe
14b, Tb
2fe
14the Hard Magnetic phase crystal grain such as B, SmCo, not only can not because of itself and Nd
2fe
14magnetic coupling interaction between B phase crystal grain and reduce the coercivity of material, can promote the coercivity of magnet on the contrary.So inventor infers it is because Nd
2fe
14high-coercive force Hard Magnetic between B phase crystal grain can promote Nd mutually in reverse magnetization process
2fe
14the difficulty of B phase magnetic domain upset, thus improves the coercivity of material.Because the heavy metal materials such as Dy, Tb are very expensive, therefore the present inventor chooses the lower and coercivity of price and the temperature stability all well thin brilliant doping phase as NdFeB permanent-magnet material of SmCo.Compared with other is invented, the present invention's design has following special character: in traditional handicraft, and adopt Sm to substitute Nd, Co substitutes iron, is formed (Nd, Sm)
2(Fe, Co)
14b phase, though this method can improve coercivity and the temperature stability of magnet, but due to this alternative saturation magnetization that can reduce material, therefore the remanent magnetism of magnet can decrease.In the present invention, SmCo hard magnetic is independently present in Nd mutually
2fe
14between B phase crystal grain, both can utilize the high-coercive force of SmCo phase, the advantage of high-temperature stability, the remanent magnetism reducing magnet can be avoided again too to reduce.
As preferably, in step (1), described NdFeB alloy, according to percentage by weight, the content of the content of Nd to be the content of 20%-40%, Fe be 50%-75%, B is 0.5%-1.6%, Pr in addition containing 5%-10%, the Ga of the Nb of 0.4%-2%, 0.01%-0.6%.
As preferably, in step (1), described SmCo alloy, according to percentage by weight, the Zr of the Cu of the Fe of the Co of the Sm containing 20%-30%, 40%-60%, 15%-25%, 3%-6%, 0.5%-1%.
As preferably, in step (2), NdFeB alloy adopt hydrogen break+mode of airflow milling carries out fragmentation, after broken, the powder size of NdFeB alloy is 0.8 μm-5 μm.
As preferably, in step (2), SmCo alloy adopts the mode of vibration+mechanical ball milling to carry out fragmentation, and ball milling solvent is methyl alcohol, ethanol, acetone, benzinum or other organic solvent, ball radius is 0.5mm-3mm, and after broken, the powder size of SmCo alloy is 50nm-100nm.
As preferably, in step (3), SmCo alloy powder accounts for the 0.5%-15% of total powder quality, and hybrid mode is: wet-milling in ball mill, and ball milling solvent is methyl alcohol, ethanol, acetone, benzinum or other organic solvent.
As preferably, in step (4), mixed-powder after vacuum drying again under the magnetic field of 1.5-2T orientation compressing.
As preferably, in step (5), sintering temperature is 1000 DEG C-1150 DEG C, and sintering time is 1-6 hour.
As preferably, in step (5), first order heat treatment is 900 DEG C, and the time is 2-2.5h; Second level heat treatment is 500 DEG C, and the time is 2-3.5h.
The invention has the beneficial effects as follows: by the technology of thin brilliant doping, at the Nd of material
2fe
14between B phase crystal grain, mix tiny SmCo phase crystal grain, utilize the advantage that SmCo phase crystal grain coercivity is high, temperature stability is good, under the condition of not adding the heavy metals such as Dy, Tb, prepare the NdFeB permanent-magnet material with high remanent magnetism, high-coercive force, high-temperature stability.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention will be further described.
If no special instructions, of the present invention be the material adopted in embodiment is the common used material of this area, and the method adopted is the common method of this area.
Embodiment 1
During NdFeB reasonable offer, original material is Nd-Pr alloy (about 80% is Nd), electrolysis pure iron, ferroboron, pure Nb, pure Ga, carries out proportioning according to the composition Nd24Pr6Fe68.5B1Nb0.4Ga0.1 (percentage by weight) designed in advance, then adopts vacuum rapid hardening rejection tablet technique to obtain NdFeB alloy sheet; The mode adopting hydrogen decrepitation to add airflow milling carries out fragmentation to NdFeB alloy sheet, and obtained average grain diameter is the alloy powder of 2 μm.
During SmCo reasonable offer, proportioning is carried out according to the composition Sm26Co47Fe20Cu4.5Zr2.5 (percentage by weight) designed in advance, vacuum rapid hardening rejection tablet technique is adopted to obtain SmCo alloy sheet, then adopt the technique of vibration+mechanical ball milling (wet-milling) to carry out fragmentation, obtained average grain diameter is the SmCo alloy powder of 100nm.
Be the NdFeB alloy powder of 95% and SmCo alloy powder wet-milling in ball mill of 5% by mass ratio, ball milling solvent adopts acetone, and ball material mass ratio is 5: 1, and Ball-milling Time is 1 hour, then carries out drying process under vacuo.
By compressing for the powder orientation under the magnetic field of 1.5T mixed, then carries out isostatic cool pressing, obtain the square blank of 40mm × 50mm × 30mm.
Blank is put into vacuum sintering furnace, at 1100 DEG C, sinters 4h, 900 DEG C of next stage tempering 2 hours, second annealing 3.5 hours at 500 DEG C, obtained sintered magnet; From magnet, extract 5 Φ 10mm × 10mm cylindrical sample carry out magnetism testing.
The magnet performance prepared under this condition is: Br=14.7-14.9kGs, Hcj=16.1-16.5kOe, (BH) max=49.1-50.3MGOe.
Embodiment 2
Other operation of the present embodiment is with embodiment 1, and difference is: in mixed-powder, and the content of NdFeB alloy powder is the content of 90%, SmCo alloy powder is 10%.Detected by the magnet standard specimen prepared under this condition, its magnetic property is: Br=14.1-14.3kGs, Hcj=17.1-17.5kOe, (BH) max=48.5-48.7MGOe.
Embodiment 3
Other operation of the present embodiment is with embodiment 1, and difference is: in mixed-powder, and the content of NdFeB alloy powder is the content of 85%, SmCo alloy powder is 15%.Detected by the magnet standard specimen prepared under this condition, its magnetic property is: Br=13.7-13.9kGs, Hcj=17.6-18.1kOe, (BH) max=48.1-48.3MGOe.
Embodiment 4
Other operation of the present embodiment is with embodiment 1, and difference is: in mixed-powder, and the average grain diameter of SmCo alloy powder is 50nm.Detected by the magnet standard specimen prepared under this condition, its magnetic property is: Br=14.2-14.4kGs, Hcj=17.0-17.3kOe, (BH) max=48.6-48.9MGOe.
Comparative example 1
During NdFeB reasonable offer, original material is Nd-Pr alloy (about 80% is Nd), electrolysis pure iron, ferroboron, pure Nb, pure Ga, carries out proportioning according to the composition Nd24Pr6Fe68.5B1Nb0.4Ga0.1 (percentage by weight) designed in advance, then adopts vacuum rapid hardening rejection tablet technique to obtain NdFeB alloy sheet; The mode adopting hydrogen decrepitation to add airflow milling carries out fragmentation to NdFeB alloy sheet, and obtained average grain diameter is the alloy powder of 2 μm.
By compressing for NdFeB alloy powder orientation under the magnetic field of 1.5T, then carry out isostatic cool pressing, obtain the square blank of 40mm × 50mm × 30mm.
Blank is put into vacuum sintering furnace, at 1100 DEG C, sinters 4h, 900 DEG C of next stage tempering 2 hours, second annealing 3.5 hours at 500 DEG C, obtained sintered magnet; From magnet, extract 5 Φ 10mm × 10mm cylindrical sample carry out magnetism testing.
The magnet performance prepared under this condition is: Br=14.8-15.0kGs, Hcj=14.3-14.5kOe, (BH) max=49.2-50.5MGOe.
Other operation of this comparative example is with embodiment 1, but difference is: do not add SmCo alloy powder.This comparative example is compared with embodiment 1-4, and as can be seen from magnetism testing result, the remanent magnetism of magnet and magnetic energy product are substantially unchanged, but HCJ significantly declines.
Comparative example 2
By material N d-Pr alloy (about 80% is Nd), electrolysis pure iron, ferroboron, pure Nb, pure Ga, carry out proportioning according to the composition Nd24Pr6Fe68.5B1Nb0.4Ga0.1 (percentage by weight) designed in advance, obtain mixture A.
By raw material Sm, Co, Fe, Cu, Zr carry out proportioning according to the composition Sm26Co47Fe20Cu4.5Zr2.5 (percentage by weight) designed in advance, obtain mixture B.
By A, B two groups of materials by 9: 1 weight ratio put into smelting furnace melting, then adopt vacuum rapid hardening rejection tablet technique to obtain NdFeBSmCo alloy sheet; The mode adopting hydrogen decrepitation to add airflow milling carries out fragmentation to NdFeBSmCo alloy sheet, and obtained average grain diameter is the alloy powder of 2 μm.
By compressing for alloy powder orientation under the magnetic field of 1.5T, then carry out isostatic cool pressing, obtain the square blank of 40mm × 50mm × 30mm.
Blank is put into vacuum sintering furnace, at 1100 DEG C, sinters 4h, 900 DEG C of next stage tempering 2 hours, second annealing 3.5 hours at 500 DEG C, obtained sintered magnet; From magnet, extract 5 Φ 10mm × 10mm cylindrical sample carry out magnetism testing.
The magnet performance prepared under this condition is: Br=12.5-13.0kGs, Hcj=14.1-14.3kOe, (BH) max=44.2-44.5MGOe.
This comparative example is compared with embodiment 2, and the chemical composition of prepared magnet is substantially identical, but due to preparation technology's difference, causes magnetic property to there is very big difference, far below embodiment 2.
Claims (9)
1. a preparation method for high temperature resistant sintered NdFeB permanent magnets, is characterized in that, concrete preparation process is as follows:
(1) method of vacuum rapid hardening is adopted to prepare NdFeB alloy and SmCo alloy sheet;
(2) two kinds of alloys are broken into powder respectively;
(3) two kinds of powder are fully mixed according to a certain percentage;
(4) mixed-powder after vacuum drying again under magnetic field orientation compressing, then the blank after shaping is carried out isostatic cool pressing;
(5) base substrate to be sintered and 2 heat treatment, obtained high temperature resistant sintered NdFeB permanent magnets.
2. the preparation method of a kind of high temperature resistant sintered NdFeB permanent magnets according to claim 1, it is characterized in that, in step (1), described NdFeB alloy, according to percentage by weight, the content of Nd is 20%-40%, the content of Fe is the content of 50%-75%, B is 0.5%-1.6%, the Pr in addition containing 5%-10%, the Ga of the Nb of 0.4%-2%, 0.01%-0.6%.
3. the preparation method of a kind of high temperature resistant sintered NdFeB permanent magnets according to claim 1, it is characterized in that, in step (1), described SmCo alloy, according to percentage by weight, the Sm containing 20%-30%, the Co of 40%-60%, the Zr of the Cu of the Fe of 15%-25%, 3%-6%, 0.5%-1%.
4. the preparation method of a kind of high temperature resistant sintered NdFeB permanent magnets according to claim 1, it is characterized in that, in step (2), NdFeB alloy adopt hydrogen break+mode of airflow milling carries out fragmentation, after broken, the powder size of NdFeB alloy is 0.8 μm-5 μm.
5. the preparation method of a kind of high temperature resistant sintered NdFeB permanent magnets according to claim 1, it is characterized in that, in step (2), SmCo alloy adopts the mode of vibration+mechanical ball milling to carry out fragmentation, ball milling solvent is methyl alcohol, ethanol, acetone, benzinum or other organic solvent, ball radius is 0.5mm-3mm, and after broken, the powder size of SmCo alloy is 50nm-100nm.
6. the preparation method of a kind of high temperature resistant sintered NdFeB permanent magnets according to claim 1, it is characterized in that, in step (3), SmCo alloy powder accounts for the 0.5%-15% of total powder quality, hybrid mode is: wet-milling in ball mill, and ball milling solvent is methyl alcohol, ethanol, acetone, benzinum or other organic solvent.
7. the preparation method of a kind of high temperature resistant sintered NdFeB permanent magnets according to claim 1, is characterized in that, in step (4), mixed-powder after vacuum drying again under the magnetic field of 1.5-2T orientation compressing.
8. the preparation method of a kind of high temperature resistant sintered NdFeB permanent magnets according to claim 1, is characterized in that, in step (5), sintering temperature is 1000 DEG C-1150 DEG C, and sintering time is 1-6 hour.
9. the preparation method of a kind of high temperature resistant sintered NdFeB permanent magnets according to claim 1 or 8, is characterized in that, in step (5), first order heat treatment is 900 DEG C, and the time is 2-2.5h; Second level heat treatment is 500 DEG C, and the time is 2-3.5h.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105448513A (en) * | 2015-12-29 | 2016-03-30 | 江苏大学 | Preparation method of multi-phase composite permanent magnet |
| CN105469918A (en) * | 2015-12-30 | 2016-04-06 | 江苏大学 | High-resistivity composite permanent magnet and preparation method thereof |
| CN106673148A (en) * | 2017-01-19 | 2017-05-17 | 张克豪 | Efficient magnetizer |
| CN107528399A (en) * | 2017-07-12 | 2017-12-29 | 中国北方车辆研究所 | A kind of asymmetric air gap permanent magnet motor of new gradual change |
| CN107845470A (en) * | 2017-12-10 | 2018-03-27 | 武汉朋谊科技有限公司 | A kind of printer permanent magnet |
| CN107845469A (en) * | 2017-12-10 | 2018-03-27 | 武汉朋谊科技有限公司 | A kind of preparation technology of printer permanent magnet |
| CN113205936A (en) * | 2021-04-23 | 2021-08-03 | 安徽吉华新材料有限公司 | NdFeB/YCo5 type high-performance magnet and preparation process thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105448513A (en) * | 2015-12-29 | 2016-03-30 | 江苏大学 | Preparation method of multi-phase composite permanent magnet |
| CN105469918A (en) * | 2015-12-30 | 2016-04-06 | 江苏大学 | High-resistivity composite permanent magnet and preparation method thereof |
| CN106673148A (en) * | 2017-01-19 | 2017-05-17 | 张克豪 | Efficient magnetizer |
| CN106673148B (en) * | 2017-01-19 | 2019-03-29 | 万明蓉 | A kind of high efficient magnetizing device |
| CN107528399A (en) * | 2017-07-12 | 2017-12-29 | 中国北方车辆研究所 | A kind of asymmetric air gap permanent magnet motor of new gradual change |
| CN107845470A (en) * | 2017-12-10 | 2018-03-27 | 武汉朋谊科技有限公司 | A kind of printer permanent magnet |
| CN107845469A (en) * | 2017-12-10 | 2018-03-27 | 武汉朋谊科技有限公司 | A kind of preparation technology of printer permanent magnet |
| CN113205936A (en) * | 2021-04-23 | 2021-08-03 | 安徽吉华新材料有限公司 | NdFeB/YCo5 type high-performance magnet and preparation process thereof |
| CN113205936B (en) * | 2021-04-23 | 2022-10-14 | 安徽吉华新材料有限公司 | NdFeB/YCo5 type high-performance magnet and preparation process thereof |
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