CN105405555B - A kind of sintered Nd-Fe-B permanent magnetic material of the holmium containing cerium - Google Patents
A kind of sintered Nd-Fe-B permanent magnetic material of the holmium containing cerium Download PDFInfo
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Abstract
The invention discloses a kind of sintered Nd-Fe-B permanent magnetic material of holmium containing cerium, which consists of the following compositions：((PrNd)1‑x‑yCexHoy)a(FeCoCuAlNb)100‑a‑bBb, wherein a=30~33, b=0.95~1.05, x=0.05~0.30, y≤0.20.The preparation method of the material includes the following steps：(1) dispensing melting, (2) hydrogen is broken, and (3) mix powder processed, (4) oriented moulding, and (5) sintering tempering, wherein holmium are added in the form of hydrogen is crushed holmium iron in mixing powder process.The present invention replaces praseodymium neodymium, the dysprosium of high price, solves the problems, such as to reduce the cost of sintered Nd-Fe-B permanent magnetic material because praseodymium neodymium and the dysprosium cost at high price brought are higher at present by cerium, the holmium of addition low price.
Description
Technical field
The present invention relates to sintered Nd-Fe-B permanent magnetic materials of a kind of holmium containing cerium and preparation method thereof.
Background technology
In recent years, due to the fast development of sintered NdFeB industry, commonly use rare earth material praseodymium neodymium (or neodymium), dysprosium iron (or
Dysprosium), the consumptions such as terbium increase, lead to its price Continued, the cost of sintered Nd-Fe-B permanent magnetic material promoted to improve.Praseodymium at present
The price of neodymium is 30~400,000 yuan/ton, and the price of dysprosium iron is 130~1,500,000 yuan/ton, the price of terbium is 240~2,600,000 yuan/
Ton.And the price of the more rich cerium of reserves is 3~40,000 yuan/ton, the price of holmium iron is 26~280,000 yuan/ton.It can be seen that cerium
Price be only 1/10th of praseodymium neodymium, and holmium is also cheap much relative to dysprosium, terbium.Therefore, if cerium part may be used
Praseodymium neodymium, holmium/holmium iron partial alternative dysprosium iron/dysprosium are substituted, then can substantially reduce the cost of sintered Nd-Fe-B permanent magnetic material.
Invention content
The technical problem to be solved by the present invention is to, using the cerium of low price, holmium iron substitute part high price praseodymium neodymium and
Dysprosium iron, and by process modification, sintered Nd-Fe-B permanent magnetic material is prepared, material cost is reduced, the market competitiveness is improved.
The present invention solve its technical problem the technical solution adopted is that：
A kind of sintered Nd-Fe-B permanent magnetic material of the holmium containing cerium, the ingredient of the sintered Nd-Fe-B permanent magnetic material are
((PrNd)1-x-yCexHoy)a(FeCoCuAlNb)100-a-bBb, wherein a=30~33, b=0.95~1.05, x=0.05~
0.30, y≤0.20；The sintered Nd-Fe-B permanent magnetic material is prepared by following steps：
(1) in addition to holmium, remaining raw material praseodymium neodymium, cerium, iron, cobalt, copper, aluminium, ferro-niobium and ferro-boron etc. are designed into dispensing by formula,
It puts into smelting furnace, when vacuum degree reaches 5Pa or less in smelting furnace, melting pours into and gets rid of strap；The holmium is in the form of holmium iron
It is added in subsequent step；
(2) by holmium iron and it is described get rid of strap be respectively charged into hydrogen be crushed stove in, be flushed with hydrogen after vacuumizing qi leel not Po Sui, get rid of strap
Through 560~580 DEG C of dehydrogenations, holmium iron obtains getting rid of in strap powder in powder and holmium iron through 520 DEG C~560 DEG C dehydrogenations；
(3) it is got rid of in strap in powder described, powder in the holmium iron is added in the ratio that step (1) calculates, then be added into
Powder processed is carried out in airflow milling equipment, the fine powder that Laser particle-size distribution is D50=4.0~4.8 μm is obtained, by the fine powder batch mixing 1
~2h obtains uniformly mixed fine powder；
(4) by the fine powder under magnetic field oriented moulding, nitrogen protection is led in forming process, makes its oxygen content≤0.1%,
Alignment magnetic field >=1.7T, obtain be orientated green compact, and by the green compact be vacuum-packed after, isostatic cool pressing；
(5) green compact is sintered 4~5h in vacuum sintering furnace through 1060 DEG C~1080 DEG C, after being cooled to≤100 DEG C
2~3h is tempered through 900 DEG C~920 DEG C level-ones obtain blank through 500 DEG C~530 DEG C second annealing 5h again.
The ingredient of the sintered Nd-Fe-B permanent magnetic material is preferably a=31~32, and b=0.95~1.01, x=0.10~
0.30, y≤0.07.
The ingredient of the sintered Nd-Fe-B permanent magnetic material can also be preferably a=30~32, b=0.98~1.05, x=
0.05~0.15, y=0.08~0.20.
The preparation method of the description of summary, the sintered Nd-Fe-B permanent magnetic material includes the following steps：(1) dispensing melting,
(2) hydrogen is broken, and (3) mix powder processed, and (4) oriented moulding, (5) sintering tempering, wherein holmium is mixing in the form of hydrogen is crushed holmium iron
Powder process processed is added.
Preferred embodiment, holmium iron described in the preparation method step (2) of the sintered Nd-Fe-B permanent magnetic material are de- through 560 DEG C
Hydrogen.
Preferred embodiment, through 200MPa isostatic cool pressings in the preparation method step (4) of the sintered Nd-Fe-B permanent magnetic material.
Preferred embodiment burns the green compact in vacuum in the preparation method step (5) of the sintered Nd-Fe-B permanent magnetic material
Through 1060 DEG C~1080 DEG C sintering 5h in freezing of a furnace, it is cooled to after 100 DEG C and is tempered 2~3h through 900~920 DEG C of level-ones again, through 500 DEG C
Second annealing 5h.
Compared with prior art, advantages of the present invention is as follows：
The present invention substitutes the praseodymium neodymium and dysprosium iron of part high price using cerium, the holmium iron of low price, and by process modification, will
The independent hydrogen of holmium iron is broken, and powder in holmium iron is added in airflow milling powder, and so, holmium does not enter in main phase grain substantially,
The remanent magnetism of main phase is not reduced, and holmium only plays magnetic hardening or so at edge, improves coercivity.Sintered NdFeB permanent magnet prepared by the present invention
Material, performance is higher, and material cost reduces, and is conducive to improve the market competitiveness.
Specific implementation mode
With reference to specific embodiment, present invention is further described in detail.
Embodiment 1
The materials such as praseodymium neodymium, cerium, holmium iron, iron, cobalt, copper, aluminium, ferro-niobium and ferro-boron are pressed into ingredient ((PrNd)0.69Ce0.3Ho0.01)32(FeCoCuAlNb)67.02B0.98Dispensing 300kg, wherein cerium are 28.8kg, and holmium iron (containing holmium 80%) is
1.2kg.By in raw material (298.8kg) the input smelting furnace in addition to holmium iron, wait for that vacuum degree reaches 5Pa or less in smelting furnace
When, add power melting, pours into and get rid of strap.Strap will be got rid of to be fitted into the broken stove of hydrogen, gas is flushed with hydrogen after vacuumizing and is crushed, through 580 DEG C
Dehydrogenation obtains getting rid of powder in strap.50kg holmium iron is fitted into hydrogen to be crushed in stove, it is broken to be flushed with hydrogen gas after vacuumizing, through 520 DEG C of dehydrogenations,
Obtain powder in holmium iron.It weighs powder and 298.8kg in 1.2kg holmium iron and gets rid of powder in strap and be added together in airflow milling equipment and made
Powder obtains the fine powder that Laser particle-size distribution is D50=4.8 μm and fine powder batch mixing 2h is obtained uniformly mixed fine powder.By fine powder
The oriented moulding under magnetic field leads to nitrogen protection in forming process, its oxygen content≤0.1%, alignment magnetic field >=1.7T is made to be taken
To green compact.And after green compact is vacuum-packed, through 200MPa isostatic cool pressings, green density is improved.Green compact is packed into vacuum sintering furnace
It is interior to be sintered 5h through 1070 DEG C, it is cooled to after 100 DEG C and obtains blank through 530 DEG C of second annealing 5h through 920 DEG C of level-ones tempering 3h again.
After detecting its performance, material property reaches N38.The formulation cost is that (praseodymium neodymium presses 300 yuan/kg, containing holmium 80% to 83.1 yuan/kg
Holmium iron is calculated by 1300 yuan/kg, cerium by 40 yuan/kg by 260 yuan/kg, the dysprosium iron containing dysprosium 80%, is tax included price, similarly hereinafter).
Embodiment 2
The materials such as praseodymium neodymium, cerium, holmium iron, iron, cobalt, copper, aluminium, ferro-niobium and ferro-boron are pressed into ingredient ((PrNd)0.72Ce0.22Ho0.06)32(FeCoCuAlNb)67.05B0.95Dispensing 300kg, wherein cerium 21.12kg, holmium iron (containing holmium 80%) are
7.2kg.By in raw material (292.8kg) the input smelting furnace in addition to holmium iron, wait for that vacuum degree reaches 5Pa or less in smelting furnace
When, add power melting, pours into and get rid of strap.Strap will be got rid of to be fitted into the broken stove of hydrogen, gas is flushed with hydrogen after vacuumizing and is crushed, through 580 DEG C
Dehydrogenation obtains getting rid of powder in strap.50kg holmium iron is fitted into hydrogen to be crushed in stove, it is broken to be flushed with hydrogen gas after vacuumizing, through 560 DEG C of dehydrogenations,
Obtain powder in holmium iron.It weighs powder and 292.8kg in 7.2kg holmium iron and gets rid of powder in strap and be added together in airflow milling equipment and made
Powder obtains the fine powder that Laser particle-size distribution is D50=4.2 μm and fine powder batch mixing 2h is obtained uniformly mixed fine powder.By fine powder
The oriented moulding under magnetic field leads to nitrogen protection in forming process, its oxygen content≤0.1%, alignment magnetic field >=1.7T is made to be taken
To green compact.And after green compact is vacuum-packed, through 200MPa isostatic cool pressings, green density is improved.Green compact is packed into vacuum sintering furnace
It is interior to be sintered 5h through 1080 DEG C, it is cooled to after 100 DEG C and obtains blank through 500 DEG C of second annealing 5h through 900 DEG C of level-ones tempering 2h again.
After detecting its performance, material property reaches N35M.The formulation cost is 84.2 yuan/kg.
Embodiment 3
The materials such as praseodymium neodymium, cerium, holmium iron, iron, cobalt, copper, aluminium, ferro-niobium and ferro-boron are pressed into ingredient ((PrNd)0.76Ce0.05Ho0.2)30(FeCoCuAlNb)68.95B1.05Dispensing 300kg, wherein cerium are 4.5kg, and holmium iron (containing holmium 80%) is
22.5kg.By in raw material (277.5kg) the input smelting furnace in addition to holmium iron, wait for that vacuum degree reaches 5Pa or less in smelting furnace
When, add power melting, pours into and get rid of strap.Strap will be got rid of to be fitted into the broken stove of hydrogen, gas is flushed with hydrogen after vacuumizing and is crushed, through 580 DEG C
Dehydrogenation obtains getting rid of powder in strap.50kg holmium iron is fitted into hydrogen to be crushed in stove, it is broken to be flushed with hydrogen gas after vacuumizing, through 520 DEG C of dehydrogenations,
Obtain powder in holmium iron.It weighs powder and 298.8kg in 22.5kg holmium iron and gets rid of powder in strap and be added together in airflow milling equipment and made
Powder obtains the fine powder that Laser particle-size distribution is D50=4.5 μm and fine powder batch mixing 2h is obtained uniformly mixed fine powder.By fine powder
The oriented moulding under magnetic field leads to nitrogen protection in forming process, its oxygen content≤0.1%, alignment magnetic field >=1.7T is made to be taken
To green compact.And after green compact is vacuum-packed, through 200MPa isostatic cool pressings, green density is improved.Green compact is packed into vacuum sintering furnace
It is interior to be sintered 5h through 1050 DEG C, it is cooled to after 100 DEG C and obtains blank through 500 DEG C of second annealing 5h through 910 DEG C of level-ones tempering 3h again.
After detecting its performance, material property reaches N42M.The formulation cost is 94.5 yuan/kg.
Comparative example 1
The materials such as praseodymium neodymium, gadolinium iron, iron, cobalt, copper, aluminium, ferro-niobium and ferro-boron are pressed into ingredient ((PrNd)0.84Gd0.16)32
(FeCoCuAlNb)66.99B1.01Dispensing 300kg.Raw material are put into smelting furnace, wait for that vacuum degree reaches 5Pa or less in smelting furnace
When, add power melting, pours into and get rid of strap.Strap will be got rid of to be fitted into the broken stove of hydrogen, gas is flushed with hydrogen after vacuumizing and is crushed, through 580 DEG C
Dehydrogenation obtains getting rid of powder in strap.It will get rid of in strap and carry out powder processed in powder addition airflow milling equipment, obtaining Laser particle-size distribution is
Fine powder batch mixing 2h is obtained uniformly mixed fine powder by D50=4.5 μm of fine powder.Oriented moulding, molding under magnetic field by fine powder
Lead to nitrogen protection in the process, its oxygen content≤0.1%, alignment magnetic field >=1.7T is made to obtain being orientated green compact.And by green compact vacuum packet
After dress, through 200MPa isostatic cool pressings, green density is improved.Green compact is packed into vacuum sintering furnace through 1070 DEG C of sintering 5h, cooling
3h is tempered through 920 DEG C of level-ones obtain blank through 530 DEG C of second annealing 5h again after to 100 DEG C.After detecting its performance, material property
Reach N38.The formula reduces cost, formulation cost 91.6 using gadolinium iron substitution part praseodymium neodymium (gadolinium iron is calculated by 80 yuan/kg)
Member/kg.In contrast, same trade mark performance, formulation cost reduces by 8.5 yuan/kg to embodiment 1, reduces by 9.3%.
Comparative example 2
The materials such as praseodymium neodymium, gadolinium iron, holmium iron, iron, cobalt, copper, aluminium, ferro-niobium and ferro-boron are pressed into ingredient ((PrNd)0.825Gd0.145Ho0.03)31(FeCoCuAlNb)68B1Dispensing 300kg.Raw material are put into smelting furnace, wait for vacuum in smelting furnace
When degree reaches 5Pa or less, adds power melting, pour into and get rid of strap.Strap will be got rid of to be fitted into the broken stove of hydrogen, gas is flushed with hydrogen after vacuumizing
It is broken, through 580 DEG C of dehydrogenations, obtain getting rid of powder in strap.It will get rid of in strap and carry out powder processed in powder addition airflow milling equipment, and obtain laser
Size distribution is that fine powder batch mixing 2h is obtained uniformly mixed fine powder by D50=4.3 μm of fine powder.Fine powder is orientated under magnetic field
It is molded, nitrogen protection is led in forming process, its oxygen content≤0.1%, alignment magnetic field >=1.7T is made to obtain being orientated green compact.And it will
After green compact vacuum packaging, through 200MPa isostatic cool pressings, green density is improved.Green compact is packed into vacuum sintering furnace and is burnt through 1065 DEG C
4.5h is tied, is cooled to after 100 DEG C and obtains blank through 500 DEG C of second annealing 5h through 910 DEG C of level-ones tempering 3h again.Detect its performance
Afterwards, material property reaches N35M.The formula reduces cost using gadolinium iron retrieval section praseodymium neodymium (gadolinium iron is calculated by 80 yuan/kg), adds
Holmium iron is added to improve coercivity, formulation cost is 90 yuan/kg.Embodiment 2 in contrast, same trade mark property formulae cost reduction
5.8 yuan/kg, reduce by 6.4%.
Comparative example 3
The materials such as praseodymium neodymium, dysprosium iron, iron, cobalt, copper, aluminium, ferro-niobium and ferro-boron are pressed into ingredient ((PrNd)0.994Dy0.006)30.8
(FeCoCuAlNb)68.2B1Dispensing 300kg.Raw material are put into smelting furnace, when vacuum degree reaches 5Pa or less in smelting furnace,
Add power melting, pours into and get rid of strap.Strap will be got rid of to be fitted into the broken stove of hydrogen, gas is flushed with hydrogen after vacuumizing and is crushed, it is de- through 580 DEG C
Hydrogen obtains getting rid of powder in strap.It will get rid of in strap and carry out powder processed in powder addition airflow milling equipment, it is D50 to obtain Laser particle-size distribution
Fine powder batch mixing 2h is obtained uniformly mixed fine powder by=4.4 μm of fine powder.By fine powder under magnetic field oriented moulding, forming process
In lead to nitrogen protection, make its oxygen content≤0.1%, alignment magnetic field >=1.7T obtains being orientated green compact.And green compact is vacuum-packed
Afterwards, through 200MPa isostatic cool pressings, green density is improved.Green compact is packed into vacuum sintering furnace through 1060 DEG C of sintering 4.5h, cooling
3h is tempered through 910 DEG C of level-ones obtain blank through 500 DEG C of second annealing 5h again after to 100 DEG C.After detecting its performance, material property
Reach N42M.The formulation cost is 101 yuan/kg.Embodiment 3 in contrast, same 6.5 yuan of trade mark property formulae cost reduction/
Kg, drop 6.4%.
The present invention substitutes the praseodymium neodymium and dysprosium iron of part high price using cerium, the holmium iron of low price, and passes through process modification, system
Standby sintered Nd-Fe-B permanent magnetic material, reduces material cost, improves the market competitiveness.
Those skilled in the art can be carry out various modifications to the embodiment of the present invention and modification, if these modifications and change
For type within the scope of the claims in the present invention and its equivalent technologies, then these modifications and variations are also in protection scope of the present invention
Within.
The prior art that the content not being described in detail in specification is known to the skilled person.
Claims (4)
1. a kind of sintered Nd-Fe-B permanent magnetic material of holmium containing cerium, which is characterized in that the ingredient of the sintered Nd-Fe-B permanent magnetic material
For：((PrNd)1-x-yCexHoy)a(FeCoCuAlNb)100-a-bBb, wherein a=31~32, b=0.95~1.01, x=0.10~
0.30, y≤0.07 or a=30~32, b=0.98~1.05, x=0.05~0.15, y=0.08~0.20；The sintering
Nd-Fe-B permanent magnet material is prepared by following steps：
(1) in addition to holmium, by remaining raw material praseodymium neodymium, cerium, iron, cobalt, copper, aluminium, ferro-niobium and ferro-boron by formula design dispensing, input is molten
In furnace, when vacuum degree reaches 5Pa or less in smelting furnace, melting pours into and gets rid of strap；The holmium is in the form of holmium iron follow-up
It is added in step；
(2) by holmium iron and it is described get rid of strap and be respectively charged into hydrogen be crushed in stove, it is not broken to be flushed with hydrogen qi leel after vacuumizing, and gets rid of strap and passes through
560~580 DEG C of dehydrogenations, holmium iron obtain getting rid of in strap powder in powder and holmium iron through 520 DEG C~560 DEG C dehydrogenations；
(3) it is got rid of in strap in powder described, powder in the holmium iron is added in the ratio that step (1) calculates, then be added into air-flow
Powder processed is carried out in mill equipment, obtains the fine powder that Laser particle-size distribution is D50=4.0~4.8 μm, by 1~2h of the fine powder batch mixing,
Obtain uniformly mixed fine powder；
(4) by the fine powder under magnetic field oriented moulding, nitrogen protection is led in forming process, makes its oxygen content≤0.1%, is orientated
Magnetic field >=1.7T, obtain be orientated green compact, and by the green compact be vacuum-packed after, isostatic cool pressing；
(5) green compact is sintered 4~5h through 1060 DEG C~1080 DEG C in vacuum sintering furnace, is passed through again after being cooled to≤100 DEG C
900 DEG C~920 DEG C level-ones are tempered 2~3h and obtain blank through 500 DEG C~530 DEG C second annealing 5h.
2. the sintered Nd-Fe-B permanent magnetic material of the holmium containing cerium described in claim 1, which is characterized in that the sintered NdFeB permanent magnet material
Holmium iron is through 560 DEG C of dehydrogenations described in the preparation method step (2) of material.
3. the sintered Nd-Fe-B permanent magnetic material of the holmium containing cerium described in claim 1, which is characterized in that the sintered NdFeB permanent magnet material
Through 200MPa isostatic cool pressings in the preparation method step (4) of material.
4. the sintered Nd-Fe-B permanent magnetic material of the holmium containing cerium described in claim 1, which is characterized in that the sintered NdFeB permanent magnet material
The green compact is sintered 5h through 1060 DEG C~1080 DEG C in vacuum sintering furnace in the preparation method step (5) of material, is cooled to 100
It is tempered 2~3h through 900~920 DEG C of level-ones again after DEG C, through 500 DEG C of second annealing 5h.
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| CN105903950A (en) * | 2016-05-23 | 2016-08-31 | 苏州思创源博电子科技有限公司 | Preparation method of nanometer neodymium iron boron magnetic material |
| CN106409455A (en) * | 2016-06-29 | 2017-02-15 | 无锡新大力电机有限公司 | Sintered neodymium-iron-boron permanent magnet material containing samarium and terbium |
| CN108806910B (en) * | 2017-05-05 | 2019-12-06 | 中国科学院宁波材料技术与工程研究所 | Method for improving coercive force of neodymium iron boron magnetic material |
| CN107887091A (en) * | 2017-11-15 | 2018-04-06 | 宁德市星宇科技有限公司 | A kind of neodymium iron boron magnetic body containing dysprosium and its method for preparation |
| CN108831646A (en) * | 2018-05-22 | 2018-11-16 | 中铝山东依诺威强磁材料有限公司 | The broken technique for directly adding aluminium powder and ferrocerium mixture production sintered NdFeB of hydrogen |
| CN113223801A (en) * | 2021-05-21 | 2021-08-06 | 慈溪市兴发磁业科技有限公司 | High-boron neodymium-iron-boron permanent magnet and preparation method thereof |
| CN113436826B (en) * | 2021-07-05 | 2023-06-02 | 宁波市易赞磁业有限公司 | High-abundance rare earth sintered permanent magnet and preparation method thereof |
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| JPH0421744A (en) * | 1990-05-16 | 1992-01-24 | Daido Steel Co Ltd | Rare earth magnetic alloy excellent in hot workability |
| CN103123839A (en) * | 2013-01-30 | 2013-05-29 | 浙江大学 | Rare earth permanent magnet produced by applying abundant rare earth cerium (Ce) and preparation method thereof |
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| JPH0421744A (en) * | 1990-05-16 | 1992-01-24 | Daido Steel Co Ltd | Rare earth magnetic alloy excellent in hot workability |
| CN103123839A (en) * | 2013-01-30 | 2013-05-29 | 浙江大学 | Rare earth permanent magnet produced by applying abundant rare earth cerium (Ce) and preparation method thereof |
| CN104505206A (en) * | 2014-12-04 | 2015-04-08 | 浙江大学 | Preparation method of high-coercivity sintered Nd-Fe-B and product |
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