CN106373688B - A method of preparing rare earth permanent-magnetic material - Google Patents
A method of preparing rare earth permanent-magnetic material Download PDFInfo
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- CN106373688B CN106373688B CN201610792950.1A CN201610792950A CN106373688B CN 106373688 B CN106373688 B CN 106373688B CN 201610792950 A CN201610792950 A CN 201610792950A CN 106373688 B CN106373688 B CN 106373688B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
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Abstract
The invention discloses a kind of methods for preparing rare earth permanent-magnetic material.It includes the following steps: selection sintered NdFeB blank, waste and old neodymium iron boron magnetic body or the neodymium iron boron leftover pieces after over cleaning and drying, is broken into neodymium iron boron powder；Alignment magnetic field is applied to neodymium iron boron powder, neodymium iron boron green compact are made；Neodymium iron boron green compact are placed in the cavity of pressure sintering mold, pressure sintering mold is in a closed space, and under vacuum or inert gas shielding, heating pressurization carries out pressure sintering, then cooling to take out；Double tempering heat treatment will be carried out in magnet merging vacuum drying oven after pressure sintering, neodymium iron boron magnetic body is made.The beneficial effects of the present invention are: magnetic powder good fluidity, high production efficiency, the small cracking of deformation of products are few；Alignment magnetic field is low, and the batch steady production of the particular orientations magnets such as radiation ring may be implemented；Pressure sintering is carried out using pressure sintering mold, for magnet outer dimension close to the size of final finished, stock utilization is high, and at low cost, magnetic property is high.
Description
Technical field
The present invention relates to magnetic material correlative technology fields, refer in particular to a kind of method for preparing rare earth permanent-magnetic material.
Background technique
Since the neodymium iron boron magnetic body eighties in last century comes out, since its excellent magnetic property is rapidly in electronics, communication, friendship
The fields such as logical transport, automation, medical treatment and new energy are widely applied.Up to the present, Nd-Fe-B permanent magnet material is comprehensive
The most excellent permanent-magnet material of magnetic property is closed, " magnetic king " is known as, there is important meaning to device miniaturization, integrated and high efficiency
Justice.
By preparation method point, neodymium iron boron magnetic body is broadly divided into sintering, bonding, hot pressing/heat distortion magnet, wherein to be sintered neodymium
Iron boron dosage is maximum.The preparation process of Sintered NdFeB magnet mainly uses strip casting to obtain Nd Fe B alloys, then will
Alloy grinds to obtain 3-5 μm of single crystal grain, and monocrystalline magnetic powder particle is put into oriented moulding in magnetic field and obtains green compact, green compact are existed
1040-1100 DEG C of temperature is sintered to obtain sintered NdFeB blank, and blank finally obtains sintered NdFeB using machining and produces
Product.In production, other than small part larger product can be formed by monolithic and is made, other most of sintered NdFeBs
Product requires to be machined, and compound material utilization rate is about 66%, and the material benefit for some thin slices and special-shaped product
With rate less than 50%.The especially special-shaped thin walls product such as magnet ring or magnetic shoe, since magnetic powder poor fluidity causes green density uneven
Even, the deformation that shrinkage ratio difference during the sintering process causes product is even cracked, to influence the yield rate and material of product
Expect utilization rate.In addition, when the particular orientations product such as preparation radiation ring, due to being limited by core sataration, it is strong magnetic field can not to be obtained
The radiation orientation magnetic field for spending very high (1T or more), to limit the development of radiation magnetic loop.
The nanocrystalline fast quenching neodymium-iron-boron that it is about 200 μm that hot pressing/thermal deformation neodymium iron boron magnetic body preparation process, which is by granularity,
Powder obtains isotropic magnet in 500-600 DEG C of hot pressing densification, then obtains anisotropy using thermal deformation at 850-950 DEG C
Neodymium iron boron magnetic body.In general, hot pressing/heat distortion magnet intrinsic coercivity is more slightly higher than sintered NdFeB, this is because
The temperature that hot pressing/thermal deformation uses is lower than sintering temperature, and the time is short, so crystal grain is more tiny.And hot pressing/heat distortion magnet can
To realize dead size or connect near-net-shape, while the strain cracking of magnet can also be effectively inhibited, so material use
Rate is higher.Hot pressing/heat distortion magnet major defect is at high cost.First nanocrystalline rapidly quenched magnetic powder price used in hot pressing compared with
It is high；Thermal deformation technique production efficiency is very low simultaneously, so high production cost.
Agglutinate neodymium-iron-boron magnet is also to be prepared using nanocrystalline rapidly quenched magnetic powder, will by adding a certain proportion of bonding agent
The magnet that magnetic powder is bonded to.The stock utilization of Agglutinate neodymium-iron-boron magnet is very high, close to 100%, and special-shaped production may be implemented
The preparation of product.The disadvantage of Agglutinate neodymium-iron-boron is that magnetic property is low, and Agglutinate neodymium-iron-boron magnet magnetic energy product is mostly in 60-90kJm-3。
In conclusion the advantages of Sintered NdFeB magnet is that magnetic powder is cheap, simple production process is high-efficient, at low cost；It lacks
Point is that stock utilization is low, easily-deformable cracking.The advantages of hot pressing/heat distortion magnet is that magnet crystal grain is tiny, and stock utilization is high；
The disadvantage is that magnetic powder (the dedicated quenched powder of hot pressing/thermal deformation) price is high, thermal deformation low efficiency is at high cost.Agglutinate neodymium-iron-boron magnet
Advantage is stock utilization height, and the production of special-shaped magnet may be implemented；Major defect is that magnetic property is low, Agglutinate neodymium-iron-boron magnet magnetic
Energy product is mostly in 60-90kJm-3。
Summary of the invention
The present invention is that in order to overcome the above deficiencies in the prior art, providing one kind can be improved stock utilization
And realize the method for preparing rare earth permanent-magnetic material of sustainable development.
To achieve the goals above, the invention adopts the following technical scheme:
A method of rare earth permanent-magnetic material is prepared, is included the following steps:
(1) magnetic powder prepares: choosing sintered NdFeB blank, waste and old neodymium iron boron magnetic body or the neodymium after over cleaning and drying
Iron boron leftover pieces are broken into 10 μm or more of neodymium iron boron powder；
(2) oriented moulding: apply the alignment magnetic field of 0.2-1.5T to neodymium iron boron powder, neodymium iron boron green compact are made；
(3) pressure sintering: neodymium iron boron green compact being placed in the cavity of pressure sintering mold, and pressure sintering mold is in one
Closed space is warming up to 450~900 DEG C under vacuum or inert gas shielding, and pressurize 1~200MPa, pressure maintaining 10 seconds~10
Minute carries out pressure sintering, then cooling to take out；
(4) it is heat-treated: double tempering heat treatment will be carried out in the magnet merging vacuum drying oven after pressure sintering, using 850~
950 DEG C keep the temperature 1~8 hour, then keep the temperature 0.5~6 hour using 350~650 DEG C, and neodymium iron boron magnetic body is made.
In the present invention, sintered NdFeB blank, waste and old neodymium iron boron magnetic body or the neodymium iron after over cleaning and drying are chosen
Boron leftover pieces carry out powder processed, and stock utilization can be improved, while can also realize that waste and old neodymium iron boron magnetic body efficient circulation utilizes,
To realize the sustainable development of Rare-earth Permanent Magnet Industry.Obtained neodymium iron boron powder diameter is apparently higher than traditional sintering neodymium iron
Boron magnetic powder, so magnetic powder good fluidity；Required alignment magnetic field is low, and the batch of the particular orientations magnets such as radiation ring may be implemented
Steady production；Pressure sintering is carried out by pressure sintering mold, so that size of the magnet outer dimension close to final finished, material
Utilization rate is high.
Preferably, in step (1), choose sintered NdFeB blank, waste and old neodymium iron boron magnetic body or through over cleaning and
The neodymium iron boron powder that neodymium iron boron leftover pieces after drying are broken into 10 μm or more is polycrystal powder.Using polycrystalline bulky grain magnetic powder system
Standby magnet, so that magnetic powder good fluidity, high production efficiency, the small cracking of deformation of products are few.
Preferably, the average particle size range that neodymium iron boron powder is made is controlled at 50-300 μm in step (1).It is in
Neodymium iron boron powder flowbility in the particle size range is more preferable, and production efficiency is higher, and the smaller cracking of deformation of products is less.
Preferably, after obtained neodymium iron boron powder, rich rare earth alloy powder is added, rich rare earth closes in step (1)
The constituent at bronze end are as follows: one of Rare Earth Elements of Praseodymium, neodymium, dysprosium, terbium are a variety of, other non-rare earths be aluminium, copper,
One of gallium, iron are a variety of, and the sum of mass percent of Rare Earth Elements of Praseodymium, neodymium, dysprosium, terbium is greater than 50%；Rich rare earth alloy
The adding proportion of powder is the 0-30% of Nd Fe B alloys powder, and the rich rare earth alloy powder average particle size range control exists
0.3-10μm.The temperature that pressure sintering can be reduced in this way helps that crystal grain is inhibited to grow up and extends the use of pressure sintering mold
Service life improves production efficiency；Adding rich rare earth alloy powder by crystal boundary simultaneously improves grain boundary structure, improves magnet consistency,
So as to improve the HAST weightlessness and yield rate of magnet.
Preferably, pressure sintering mold is in a closed space, in vacuum or inert gas in step (3)
Under protection, 650~850 DEG C are warming up to, pressurize 3~100MPa, and 10 seconds~10 minutes progress pressure sinterings of pressure maintaining, then cooling takes
Out.
Preferably, in step (4), double tempering heat treatment: keeping the temperature 2~6 hours using 880 DEG C, then using 450~
620 DEG C keep the temperature 2~4 hours.
The beneficial effects of the present invention are:
1, magnetic powder good fluidity, high production efficiency, the small cracking of deformation of products are few；
2, alignment magnetic field is low, and the batch steady production of the particular orientations magnets such as radiation ring may be implemented；
3, pressure sintering, size of the magnet outer dimension close to final finished, material benefit are carried out using pressure sintering mold
With rate height, at low cost, magnetic property is high.
Specific embodiment
The present invention will be further described With reference to embodiment.
Embodiment 1:
It 1, is Nd by ingredient26.25Pr8.75Fe64B1The sintered NdFeB blank Mechanical Crushing of (mass percentage) is at average
The particle that partial size is 200 μm；
2, apply the magnetic field of 1T, green compact size R8.1 × R3.6 × 10, green compact weight 29.97g；
3, green compact are placed in the cavity of pressure sintering mold, pressure sintering mold is in a closed space, first takes out
Sky is to 8 × 10-3Pa, then applying argon gas is to 8 × 104Pa then heats to 850 DEG C, and the thickness direction along sintered NdFeB green compact adds
200MPa is pressed, it is cooling after pressure maintaining 6 minutes to take out；
4, by after pressure sintering magnet merging vacuum drying oven in be heat-treated, be respectively adopted 900 DEG C heat preservation 4 hours and
500 DEG C of heat preservations, 4 hours technique is heat-treated hot pressing blank, and the magnet that specification is R8.1 × R3.6 × 5.3, material benefit is made
With rate 100%, no arrisdefect cracking, yield rate 100%.
Embodiment 2:
It is Nd by ingredient26.25Pr8.75Fe64B1The sintered NdFeB blank Mechanical Crushing of (mass percentage) is at average grain
The particle that diameter is 50 μm.5%Nd is added in polycrystalline neodymium iron boron particles70Cu30(mass percentage) richness rare earth alloy powder,
Wherein the average grain diameter of neodymium copper alloy powder is 3 μm.Temperature when pressure sintering is 700 DEG C, other techniques and 1 phase of embodiment
Together.
Embodiment 3:
The leftover pieces of sintered NdFeB are broken into 300 μm of polycrystalline particle after over cleaning and drying, then add 5%
Nd70Cu30(mass percentage) richness rare earth alloy powder, the average grain diameter of neodymium copper alloy powder are 3 μm.It is radiated using 0.5T
The annular green compact of 30 × φ of φ 24 × 20 are made in magnetic field orientating.Temperature when pressure sintering is 650 degrees Celsius, other techniques and reality
It is identical to apply example 1.
Comparative example 1:
Magnetic powder oriented moulding, green compact specification 43.56 × 39.6 × 29.82, by conventional sintering work are criticized together using with embodiment 1
Skill is in 1068 DEG C of sintering densifications, technique heat treatment same as Example 1.
It is sintered blank specification 33 × 30 × 2, wire cutting adds at the black-film and the inside and outside arc mill of progress of R8.1 × R3.6 × 5.5
Work, finally obtains the magnet of R8.1 × R3.6 × 5.3, stock utilization 76%, and 0.3 yuan of expense of machining/only, process
In have arrisdefect, yield rate 98%.
Embodiment 1, the preparation process of embodiment 2 and comparative example 1 and product characteristic comparison are shown in Table 1.Embodiment 1 basically reaches
Dead size molding, can be in order to avoid processing, stock utilization be close to 100%, but the production of embodiment 1 for the not high product of tolerance
Product HAST weightlessness is bigger.Embodiment 2, which adds rich rare earth alloy powder by crystal boundary, improves grain boundary structure, improve magnet consistency from
And improve the HAST weightlessness and yield rate of magnet.Comparative example 1 is prepared using conventional method, and product, which needs to grind by wire cutting, to be added
The processes such as work greatly reduce stock utilization, while increasing processing cost.
1 embodiment 1 of table, the preparation process and product characteristic of embodiment 2 and comparative example 1
| Densification temperature | Stock utilization | HAST is weightless | Machining expense | Yield rate | |
| Embodiment 1 | 850℃ | ~100% | 2mg/cm2 | 0 | 99% |
| Embodiment 2 | 700℃ | ~100% | 0.5mg/cm2 | 0 | ~100% |
| Comparative example 1 | 1068℃ | 76% | 1mg/cm2 | 0.3 yuan/only | 97% |
2 are shown in Table using neodymium iron boron magnetic body items magnetic property index prepared by different process.High-performance may be implemented in embodiment 3
The preparation of thin-walled magnet ring product.Compared with similar thin-walled magnet ring in the market, embodiment 3 has obvious price advantage.And implement
Magnetic powder particle is larger in example 3, good fluidity, and the alignment magnetic field needed is low, is conducive to produce in batches.
The neodymium iron boron magnetic body items magnetic property index of 2 different process of table preparation
The comparison of embodiment 1, embodiment 2, embodiment 3 and comparative example 1 is it is found that and traditional handicraft from above-mentioned Tables 1 and 2
Comparison, the present invention using polycrystalline bulky grain magnetic powder prepare magnet especially particular orientation magnet when, have stock utilization high, at
This low, advantage such as magnetic property height.
Claims (4)
1. a kind of method for preparing rare earth permanent-magnetic material, characterized in that include the following steps:
(1) magnetic powder prepares: choosing sintered NdFeB blank, waste and old neodymium iron boron magnetic body or the neodymium iron boron after over cleaning and drying
Leftover pieces are broken into 10 μm or more of neodymium iron boron powder；The average particle size range of the neodymium iron boron powder is controlled at 50-300 μm；
After obtained neodymium iron boron powder, rich rare earth alloy powder, the rich rare earth alloy powder average particle size range control is added
At 0.3-10 μm；
(2) oriented moulding: apply the alignment magnetic field of 0.2-0.5T to neodymium iron boron powder, neodymium iron boron green compact are made；
(3) pressure sintering: neodymium iron boron green compact being placed in the cavity of pressure sintering mold, and pressure sintering mold is closed in one
Space be warming up to 650~850 DEG C under vacuum or inert gas shielding, pressurize 3~100MPa, pressure maintaining 10 seconds~10 minutes
Pressure sintering is carried out, it is then cooling to take out；
(4) it is heat-treated: double tempering heat treatment will be carried out in the magnet merging vacuum drying oven after pressure sintering, using 850~950 DEG C
Heat preservation 1~8 hour, then 0.5~6 hour is kept the temperature using 350~650 DEG C, neodymium iron boron magnetic body is made.
2. a kind of method for preparing rare earth permanent-magnetic material according to claim 1, characterized in that in step (1), choose
Sintered NdFeB blank, waste and old neodymium iron boron magnetic body or the neodymium iron boron leftover pieces after over cleaning and drying are broken into 10 μm or more
Neodymium iron boron powder be polycrystal powder.
3. a kind of method for preparing rare earth permanent-magnetic material according to claim 1 or 2, characterized in that in step (1),
After obtained neodymium iron boron powder, rich rare earth alloy powder, the constituent of rich rare earth alloy powder are as follows: rare earth element is added
One of praseodymium, neodymium, dysprosium, terbium are a variety of, other non-rare earths are one of aluminium, copper, gallium, iron or a variety of, and rare earth is first
The sum of mass percent of plain praseodymium, neodymium, dysprosium, terbium is greater than 50%；The adding proportion of rich rare earth alloy powder is neodymium iron boron alloy powder
The 0-30% at end.
4. a kind of method for preparing rare earth permanent-magnetic material according to claim 1, characterized in that secondary in step (4)
Tempering heat treatment: 2~6 hours are kept the temperature using 880 DEG C, then keeps the temperature 2~4 hours using 450~620 DEG C.
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| CN201610792950.1A CN106373688B (en) | 2016-08-31 | 2016-08-31 | A method of preparing rare earth permanent-magnetic material |
| PCT/CN2016/106318 WO2018040299A1 (en) | 2016-08-31 | 2016-11-18 | Method for preparing rare-earth permanent magnetic materials |
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| CN201610792950.1A CN106373688B (en) | 2016-08-31 | 2016-08-31 | A method of preparing rare earth permanent-magnetic material |
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| CN113198614B (en) * | 2019-09-18 | 2023-09-19 | 安徽万磁电子有限公司 | Automatic sieving mechanism of neodymium iron boron magnetic powder |
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| CN103866127A (en) * | 2014-02-27 | 2014-06-18 | 中铝广西有色金源稀土股份有限公司 | Method for preparing neodymium iron boron through regenerating waste material containing neodymium, iron and boron |
| CN104576019A (en) * | 2014-11-26 | 2015-04-29 | 宁波格荣利磁业有限公司 | Method for preparing NdFeB (neodymium-iron-boron) magnet by waste materials |
| CN104801718A (en) * | 2015-05-07 | 2015-07-29 | 安徽万磁电子有限公司 | Recycling process of sintering neodymium iron boron discard black wafer |
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| CN106373688A (en) | 2017-02-01 |
| WO2018040299A1 (en) | 2018-03-08 |
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