CN104332300A - Method for sintering neodymium iron boron magnet - Google Patents
Method for sintering neodymium iron boron magnet Download PDFInfo
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- CN104332300A CN104332300A CN201410537940.4A CN201410537940A CN104332300A CN 104332300 A CN104332300 A CN 104332300A CN 201410537940 A CN201410537940 A CN 201410537940A CN 104332300 A CN104332300 A CN 104332300A
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Abstract
The invention relates to a method for sintering a neodymium iron boron magnet, belonging to the technical field of rare earth magnetic material. The method comprises the following steps: weighing raw materials according to a formula of the neodymium iron boron magnet, namely Pr6-8Nd22-24B1-1.2Nb0.2-0.5Co1-2Al0.5-0.8Fe63.5-69.3, and melting; pouring the materials to form a thrown sheet; carrying out hydrogen crushing on the thrown sheet and grinding by airflow to prepare powder with the average granularity of 3-5 microns; orientating the powder and pressing and molding; pressurizing at 180MPa-200MPa and carrying out isostatic pressing treatment; keeping the pressure for 16-22 seconds to form a blank; dehydrogenating the blank in a vacuum sintering furnace and carrying out high-temperature sintering under the conditions that the temperature is 1,050-1,060 DEG C and the vacuum degree is 2E-2Pa; then tempering; and finally, carrying out air cooling by adopting nitrogen gas to a room temperature, and discharging from a furnace to obtain the neodymium iron boron magnet. The preparation method is simple and feasible and the prepared neodymium iron boron magnet has better performance.
Description
Technical field
The present invention relates to a kind of method of Sintered NdFeB magnet, belong to Rare-Earth Magnetic field of material technology.
Technical background
NdFeB permanent-magnet alloy, because it has high remanent magnetism, high-coercive force and high energy product, is applied in computer hard disk drive, motor, human body NMR imaging instrument, audio device etc. are many.The preparation method of NdFeB permanent magnetic material mainly comprises sintering, thermal deformation and bonding.NdFeB is owing to making magnetic property generally on the low side adding of binding agent for bonding.Conventional sintering NdFeB then because of structural heterogenity, there is non-magnetic phase and high temperature sintering brings out the reasons such as coarse grains, cause that its temperature stability is poor, the magnetization and corrosion resistance on the low side.Compared with bonding, conventional sintering NdFeB; thermal deformation (Hot-Deformation; HD) NdFeB magnet because of sintering after thermal deformation field crystal grain along pressure direction (C axle) orientation, and more excellent magnetic property, corrosion resistance and fracture toughness can be shown.At present, researchers have carried out comparatively deep research for relation between thermal deformation technique, microstructure and magnetic property three, and notice that the crystal grain in conventional sintering and subsequent thermal deformation process is all easily grown up and causes magnetic property to worsen.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of method of Sintered NdFeB magnet is provided, make the neodymium iron boron magnetic body obtained have superior performance.
Object of the present invention is achieved through the following technical solutions, a kind of method of Sintered NdFeB magnet, and described method comprises the steps:
S1, formula (percentage by weight) Pr by neodymium iron boron magnetic body
6-8nd
22-24b
1-1.2nb
0.2-0.5co
1-2al
0.5-0.8fe
63.5-69.3take raw material and carry out melting, the alloy after melting is completely poured into rejection tablet;
S2, above-mentioned rejection tablet to be placed in hydrogen crushing furnace hydrogen broken that average grain diameter is the powder of 10 μm-20 μm, then use airflow milling make the powder that particle mean size is 3 μm-5 μm, by above-mentioned powder content higher than 99.99% inert gas protection under stir 1h-3h;
S3, entered in moulding press mould to add magnetic field by the powder be stirred carry out orientation at the protection down of nitrogen, compressing after orientation is green compact, green compact is put into isostatic pressing machine and pressurizes under 180-200MPa, and pressurize 16s-22s forms blank;
S4, the blank after isostatic pressed is first shelled oil under the protection of nitrogen, then is placed in vacuum sintering furnace and first carries out dehydrogenation, then at 1050-1060 DEG C, vacuum degree is 2E
-2high temperature sintering under handkerchief, then tempering, finally adopt air-cooled the coming out of the stove to normal temperature of nitrogen to obtain neodymium iron boron magnetic body.
Neodymium iron boron magnetic body by certain mass percent proportioning, by selecting the element such as niobium, aluminium with appropriate mass percentage, and is suitably added other elements by the present invention, crystal grain thinning, optimizing Grain-Boundary Phase, by improving sintering process, improving performance and the resistance to corrosion of product further.And add appropriate Pr, Nd, form appropriate Nd-Fe-B principal phase tissue, improve the microscopic structure of magnet, thus improve wear-corrosion resistance and the temperature stability of magnet more all sidedly.The raw material of having prepared burden first directly is carried out hydrogen broken, ensures the even refinement of heavy rare earth powder, and by airflow milling, it is made to 3-5 μm of fine powder further, this scope powder particles evenly, granularity concentration degree is better.And powder is thinner, more contribute to the lifting of magnet HCJ, if powder is too thick, then crystal boundary cannot be incorporated, but powder is thinner, more easily be oxidized, cause usefulness to reduce, therefore the particle of alloy is when 3-5 μm of scope, and its HCJ promotes obviously, the control of oxygen content is relatively easy, can play the cooperative effect in neodymium iron boron magnetic body between each element further.Then shaping compacting in highfield after powder being mixed by high pure nitrogen or argon shield mixer; then sinter at 1050-1060 DEG C; second annealing; the Nd-rich phase of the magnet crystal boundary after coming out of the stove is uniformly distributed, heavy rare earth is mainly distributed in Grain-Boundary Phase; and the increase of heavy rare earth content can improve the HCJ of product greatly in Grain-Boundary Phase; the Br of product reduces less simultaneously, reaches the requirement of high performance low temperature degree coefficient.
As preferably, melting described in step S1 is carry out in the vacuum rapid hardening furnace of 0.2-1.0Pa in vacuum degree, and smelting temperature is 1450-1550 DEG C.Under this smelting temperature, final neodymium iron boron magnetic body can be made to obtain reasonable performance and higher productive rate.
As preferably, when step S2 hydrogen is broken, desorption temperature is 550-570 DEG C, and dehydrogenation time is 3-5h.
As preferably, step S2 airflow milling is carried out under the nitrogen protection of anaerobic.
In step S2, utilize the hydrogen absorption characteristic of intermetallic compound, under raw material is placed in hydrogen environment, hydrogen enters raw material along rich neodymium phase thin layer, makes it expansion explosion and broken, along rich neodymium phase layer place cracking, thus makes raw material become meal.And with high pressure draught, the meal after stirring is blown afloat be less than the nitrogen protection of 200ppm in oxygen content under; by collision each other, dynamics is diminished; meal is made the powder that granularity is 3 μm-5 μm, increase the contact area of powder, thus improve the comprehensive utilization ratio of neodymium-iron-boron powder.Milling efficiency can be improved 2-3 doubly by broken being combined with airflow milling of hydrogen, reaches 150-200KG/H.
As preferably, the magnetic field of step S3 oriented moulding is 1.5-3.5T.By experimental results demonstrate, under 1.5-3.5T magnetic field, carry out the shaping degree of orientation that pressed compact has had that can ensure, can further improve magnetic property.
Further preferably, the pressure of step S3 isostatic pressed process is 180MPa, pressurize 20min.
As preferably, green density described in step S3 is 3.5-3.9g/cm
3, blank density is 4.1-4.3g/cm
3.Generally, more high-performance is higher for blank density.
As preferably, desorption temperature described in step S4 is 550-560 DEG C, and dehydrogenation time is 4-5h.
Further preferably, the temperature of high temperature sintering described in step S4 is 1050 DEG C.
As preferably, described in step S4, temper for carry out one-level tempering at 910-930 DEG C, and one-level tempering time is 2-3h, is then cooled to 480-510 DEG C and carries out second annealing 4-5h.
Further preferably, in described temper, one-level temperature is 920 DEG C, and second annealing temperature is 490 DEG C.
By by first for the blank after isostatic pressed dehydrogenation in step S4, at the sintering of 1050-1060 DEG C, and sintering vacuum degree must be less than 2E
-2handkerchief, and then carry out above-mentioned second annealing, the neodymium iron boron magnetic body of reasonable performance and higher productive rate can be obtained.If sintering temperature is too high and the too low performance that all can affect final neodymium iron boron, performance can not be met the requirements of.
Compared with prior art, tool of the present invention has the following advantages: the present invention by the material composition of rational proportion neodymium iron boron magnetic body, and obtains the neodymium iron boron magnetic body of better performances by the simple preparation method of shaping, sintering, tempering.
Embodiment
Be below specific embodiments of the invention, technical scheme of the present invention is further described, but the present invention is not limited to these embodiments.
Embodiment 1
By formula (mass percent) Pr of neodymium iron boron magnetic body
7nd
23b
1.1nb
0.3co
1.5al
0.6fe
66.5take raw material, the raw material taken is loaded vacuum rapid hardening furnace, when vacuum spun furnace is evacuated down to 0.5Pa, start melting of heating, when material is rubescent in stove, be filled with argon gas, and be warming up to 1500 DEG C and carry out melting, until raw material melt completely, after refining 10min, pour into rejection tablet, come out of the stove lower than when 80 DEG C until rejection tablet;
By above-mentioned obtained rejection tablet in hydrogen crushing furnace, hydrogen is passed in hydrogen crushing furnace, inhale completely after hydrogen until rejection tablet and be warming up to 560 DEG C of dehydrogenase 34 h, hydrogen is broken obtains the powder that average grain diameter is 20 μm, then the powder after hydrogen is broken is put into airflow milling and is finely ground into the powder that particle mean size is 4 μm under the nitrogen protection of micro-oxygen, and content higher than 99.99% inert gas protection under stir 2h;
The described powder stirred is put into moulding press mould under the nitrogen protection of micro-oxygen, and orientation is carried out in the magnetic field adding 2.5T, and after orientation, compressing density is 3.8g/cm
3green compact, green compact demagnetization and Vacuum Package, the green compact of Vacuum Package are put into isostatic pressing machine pressurize 20s under 190MPa and carry out isostatic pressed process, formation density is 4.3g/cm
3blank;
Blank after isostatic pressed is first shelled oil under the protection of nitrogen, then is placed in vacuum sintering furnace first dehydrogenase 34 .5h at 555 DEG C, then be warming up to 1055 DEG C and carry out high temperature sintering, high temperature sintering vacuum degree is 2E
-2sinter under handkerchief, then at 920 DEG C, carry out one-level tempering, one-level tempering time is 2.5h, is cooled to 490 DEG C and carries out second annealing 4.5h tempering, finally adopts air-cooled the coming out of the stove to normal temperature of high pure nitrogen to obtain neodymium iron boron magnetic body.
Embodiment 2
By formula (mass percent) Pr of neodymium iron boron magnetic body
7nd
22b
1.2nb
0.4co
1.8al
0.7fe
66.9take raw material, the raw material taken is loaded vacuum rapid hardening furnace, when vacuum spun furnace is evacuated down to 0.2Pa, start melting of heating, when material is rubescent in stove, be filled with argon gas, and be warming up to 1550 DEG C and carry out melting, until raw material melt completely, after refining 8min, pour into rejection tablet, come out of the stove lower than when 80 DEG C until rejection tablet;
By above-mentioned obtained rejection tablet in hydrogen crushing furnace, hydrogen is passed in hydrogen crushing furnace, inhale completely after hydrogen until rejection tablet and be warming up to 550 DEG C of dehydrogenase 35 h, hydrogen is broken obtains the powder that average grain diameter is 30 μm, then the powder after hydrogen is broken is put into airflow milling and is finely ground into the powder that particle mean size is 3 μm under the nitrogen protection of micro-oxygen, and content higher than 99.99% inert gas protection under stir 2.5h;
The described powder stirred is put into moulding press mould under the nitrogen protection of micro-oxygen, and orientation is carried out in the magnetic field adding 1.7T, and after orientation, compressing density is 3.9g/cm
3green compact, green compact demagnetization and Vacuum Package, the green compact of Vacuum Package are put into isostatic pressing machine pressurize 22s under 180MPa and carry out isostatic pressed process, formation density is 4.2g/cm
3blank;
Blank after isostatic pressed is first shelled oil under the protection of nitrogen, then is placed in vacuum sintering furnace first dehydrogenase 34 h at 550 DEG C, then be warming up to 1050 DEG C and carry out high temperature sintering, high temperature sintering vacuum degree is 2E
-2sinter under handkerchief, then at 930 DEG C, carry out one-level tempering, one-level tempering time is 2h, is cooled to 510 DEG C and carries out second annealing 4h tempering, finally adopts air-cooled the coming out of the stove to normal temperature of high pure nitrogen to obtain neodymium iron boron magnetic body.
Embodiment 3
By formula (mass percent) Pr of neodymium iron boron magnetic body
6nd
24b
1nb
0.5co
2al
0.5fe
66take raw material, the raw material taken is loaded vacuum rapid hardening furnace, when vacuum spun furnace is evacuated down to 1.0PaPa, start melting of heating, when material is rubescent in stove, be filled with argon gas, and be warming up to 1450 DEG C and carry out melting, until raw material melt completely, after refining 15min, pour into rejection tablet, come out of the stove lower than when 80 DEG C until rejection tablet;
By above-mentioned obtained rejection tablet in hydrogen crushing furnace, hydrogen is passed in hydrogen crushing furnace, inhale completely after hydrogen until rejection tablet and be warming up to 570 DEG C of dehydrogenase 13 h, hydrogen is broken obtains the powder that average grain diameter is 15 μm, then the powder after hydrogen is broken is put into airflow milling and is finely ground into the powder that particle mean size is 3.5 μm under the nitrogen protection of anaerobic, and content higher than 99.99% inert gas protection under stir 1.5h;
The described powder stirred is put into moulding press mould under the nitrogen protection of micro-oxygen, and orientation is carried out in the magnetic field adding 1.8T, and after orientation, compressing density is 3.5g/cm
3green compact, green compact demagnetization and Vacuum Package, the green compact of Vacuum Package are put into isostatic pressing machine pressurize 16s under 200MPa and carry out isostatic pressed process, formation density is 4.2g/cm
3blank;
Blank after isostatic pressed is first shelled oil under the protection of nitrogen, then is placed in vacuum sintering furnace first dehydrogenase 34 h at 560 DEG C, then be warming up to 1060 DEG C and carry out high temperature sintering, high temperature sintering vacuum degree is 2E
-2sinter under handkerchief, then at 910 DEG C, carry out one-level tempering, one-level tempering time is 3h, is cooled to 480 DEG C and carries out second annealing 5h tempering, finally adopts air-cooled the coming out of the stove to normal temperature of high pure nitrogen to obtain neodymium iron boron magnetic body.
Embodiment 4
By formula (mass percent) Pr of neodymium iron boron magnetic body
8nd
23b
1nb
0.2co
1al
0.8fe
66take raw material, the raw material taken is loaded vacuum rapid hardening furnace, when vacuum spun furnace is evacuated down to 0.8Pa, start melting of heating, when material is rubescent in stove, be filled with argon gas, and be warming up to 1480 DEG C and carry out melting, until raw material melt completely, after refining 12min, pour into rejection tablet, come out of the stove lower than when 80 DEG C until rejection tablet;
By above-mentioned obtained rejection tablet in hydrogen crushing furnace, hydrogen is passed in hydrogen crushing furnace, inhale completely after hydrogen until rejection tablet and be warming up to 555 DEG C of dehydrogenase 13 .5h, hydrogen is broken obtains the powder that average grain diameter is 25 μm, then the powder after hydrogen is broken is put into airflow milling and is finely ground into the powder that particle mean size is 3 μm under the nitrogen protection of anaerobic, and content higher than 99.99% inert gas protection under stir 1.5h;
The described powder stirred is put into moulding press mould under the nitrogen protection of micro-oxygen, and orientation is carried out in the magnetic field adding 2.0T, and after orientation, compressing density is 3.9g/cm
3green compact, green compact demagnetization and Vacuum Package, the green compact of Vacuum Package are put into isostatic pressing machine pressurize 18s under 180MPa and carry out isostatic pressed process, formation density is 4.1g/cm
3blank;
Blank after isostatic pressed is first shelled oil under the protection of nitrogen, then is placed in vacuum sintering furnace first dehydrogenase 35 h at 550 DEG C, then be warming up to 1050 DEG C and carry out high temperature sintering, high temperature sintering vacuum degree is 2E
-2sinter under handkerchief, then at 930 DEG C, carry out one-level tempering, one-level tempering time is 2.5h, is cooled to 505 DEG C and carries out second annealing 5h tempering, finally adopts air-cooled the coming out of the stove to normal temperature of high pure nitrogen to obtain neodymium iron boron magnetic body.
After pressing neodymium iron boron magnetic body surface grinding obtained in above-described embodiment 1-4, carry out Performance Detection according to GB/T3217 permanent magnetism (Hard Magnetic) magnetism of material test method, the magnetic property recorded is as follows:
In sum, the performance of neodymium iron boron magnetic body of the present invention is ideal, and the present invention by reasonable compatibility neodymium iron boron magnetic body raw material, and by specific preparation method, improves the performance of neodymium iron boron magnetic body, reduces production cost simultaneously.
Specific embodiment described herein is only to the explanation for example of the present invention's spirit.Those skilled in the art can make various amendment or supplement or adopt similar mode to substitute to described specific embodiment, but can't depart from spirit of the present invention or surmount the scope that appended claims defines.
Claims (10)
1. a method for Sintered NdFeB magnet, is characterized in that, described method comprises the steps:
S1, formula (percentage by weight) Pr by neodymium iron boron magnetic body
6-8nd
22-24b
1-1.2nb
0.2-0.5co
1-2al
0.5-0.8fe
63.5-69.3take raw material and carry out melting, the alloy after melting is completely poured into rejection tablet;
S2, above-mentioned rejection tablet to be placed in hydrogen crushing furnace hydrogen broken that average grain diameter is the powder of 10 μm-20 μm, then use airflow milling make the powder that particle mean size is 3 μm-5 μm, by above-mentioned powder content higher than 99.99% inert gas protection under stir 1h-3h;
S3, entered in moulding press mould to add magnetic field by the powder be stirred carry out orientation at the protection down of nitrogen, compressing after orientation is green compact, green compact is put into isostatic pressing machine and pressurizes under 180-200MPa, and pressurize 16s-22s forms blank;
S4, the blank after isostatic pressed is first shelled oil under the protection of nitrogen, then is placed in vacuum sintering furnace and first carries out dehydrogenation, then at 1050-1060 DEG C, vacuum degree is 2E
-2high temperature sintering under handkerchief, then tempering, finally adopt air-cooled the coming out of the stove to normal temperature of nitrogen to obtain neodymium iron boron magnetic body.
2. the method for Sintered NdFeB magnet according to claim 1, it is characterized in that, melting described in step S1 is carry out in the vacuum rapid hardening furnace of 0.2-1.0Pa in vacuum degree, and smelting temperature is 1450-1550 DEG C.
3. the method for Sintered NdFeB magnet according to claim 1, it is characterized in that, when step S2 hydrogen is broken, desorption temperature is 550-570 DEG C, and dehydrogenation time is 3-5h.
4. the method for Sintered NdFeB magnet according to claim 1, it is characterized in that, the magnetic field of step S3 oriented moulding is 1.5-3.5T.
5. the method for Sintered NdFeB magnet according to claim 1, it is characterized in that, the pressure of step S3 isostatic pressed process is 180MPa, pressurize 20s.
6. the method for Sintered NdFeB magnet according to claim 1, it is characterized in that, green density described in step S3 is 3.5-3.9g/cm
3, blank density is 4.1-4.3g/cm
3.
7. the method for Sintered NdFeB magnet according to claim 1, it is characterized in that, desorption temperature described in step S4 is 550-560 DEG C, and dehydrogenation time is 4-5h.
8. the method for Sintered NdFeB magnet according to claim 1, it is characterized in that, the temperature of high temperature sintering described in step S4 is 1050 DEG C.
9. the method for Sintered NdFeB magnet according to claim 1, it is characterized in that, described in step S4, temper for carry out one-level tempering at 910-930 DEG C, and one-level tempering time is 2-3h, is then cooled to 480-510 DEG C and carries out second annealing 4-5h.
10. the method for Sintered NdFeB magnet according to claim 9, it is characterized in that, in described temper, one-level temperature is 920 DEG C, and second annealing temperature is 490 DEG C.
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| CN104907560A (en) * | 2015-06-18 | 2015-09-16 | 包头金山磁材有限公司 | Sintering method capable of reducing cracks of neodymium iron boron products |
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| CN108766753A (en) * | 2018-05-11 | 2018-11-06 | 包头稀土研究院 | The preparation method of high energy product high-coercive force Sintered NdFeB magnet |
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| CN104907560A (en) * | 2015-06-18 | 2015-09-16 | 包头金山磁材有限公司 | Sintering method capable of reducing cracks of neodymium iron boron products |
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| CN110098027A (en) * | 2018-01-28 | 2019-08-06 | 蒋盼盼 | A kind of preparation method of the neodymium iron boron magnetic body without heavy rare earth |
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