CN109003802A - A kind of method that grain boundary decision prepares low-cost and high-performance bulk neodymium iron boron magnetic body - Google Patents
A kind of method that grain boundary decision prepares low-cost and high-performance bulk neodymium iron boron magnetic body Download PDFInfo
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- CN109003802A CN109003802A CN201810921550.5A CN201810921550A CN109003802A CN 109003802 A CN109003802 A CN 109003802A CN 201810921550 A CN201810921550 A CN 201810921550A CN 109003802 A CN109003802 A CN 109003802A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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Abstract
The invention belongs to technical field of magnetic materials, it is related to a kind of method that grain boundary decision prepares inexpensive bulk neodymium iron boron magnetic body, more particularly to selection dysprosium, terbium, iron, aluminium, copper, gallium alloy powder is as diffusion source, coated on 2~8mm orientation or non-oriented face, then according to finished product final size, it selects an appropriate number of magnet superposition to be put into diffusion bonding in sintering furnace to handle, obtain the high performance sintered magnet of bulk, according still further to customer demand using machine finishing at the finished product of other specifications, it is unrestricted to be orientated size, the rubidium iron boron magnet performance prepared by this law is high, it is at low cost.
Description
Technical field
The invention belongs to technical field of magnetic materials, it is related to a kind of grain boundary decision and prepares inexpensive bulk neodymium iron boron magnetic body
Method.
Background technique
By the way that in the alloy of Sintered NdFeB magnet, the pure metal or dysprosium terbium alloy that dysprosium (Dy) or terbium (Tb) is added can
To improve the coercivity of neodymium iron boron magnetic body, but neodymium will cause since dysprosium or terbium element primarily enter main phase grain using the method
The remanent magnetism of iron boron magnet is substantially reduced, and limits the preparation of more high energy product product, but the method can not be by magnet size
Limitation.
By penetrating into dysprosium, terbium element or dysprosium terbium alloy at neodymium iron boron main phase edge, hardening neodymium iron boron main phase can be effective
Improve the coercivity of neodymium iron boron magnetic body.According to this theory, have at present many technologies by by neodymium iron boron magnetic body be placed in containing dysprosium,
In the environment of the heavy rare earth elements such as terbium, and pass through High temperature diffusion and ageing treatment, so that dysprosium, terbium element grain boundary diffusion are to neodymium iron
Boron magnet phase boundray improves the magnetic anisotropy of neodymium iron boron, and then effectively improves the coercivity of neodymium iron boron magnetic body.
It is the chip shape for being in a certain way 1~5mm or so to orientation thickness that usual dysprosium (terbium), which expands infiltration technology,
Oxide, hydride or the fluoride of Dy/Tb is supplied on Sintered NdFeB magnet surface, then carry out suitable heat treatment with it is low
Warm tempering, to make that intrinsic coercivity in magnetic body is greatly improved while its remanent magnetism is not decreased obviously.Such dysprosium
(terbium) expands the magnet that infiltration method is suitable within 5mm, and the magnet big for orientation size is such as orientated size and is greater than 5mm, especially
The magnet of 10mm or more, no positive effect.
The application field and application amount of Nd-Fe-B permanent magnet material increase day by day, and annual market demand increases close to 20% amplitude
Long, Dy-Fe alloy, the price of terbium are higher and higher, and supply is very nervous.Therefore the performance of magnet, drop how are promoted from technique
The usage amount of low dysprosium, terbium becomes the research direction of numerous scholars.
The present invention is directed to spread source using new low melting point, low-cost and high-performance is prepared using new grain boundary diffusion process
Bulk Sintered NdFeB magnet.
Summary of the invention
The present invention is in view of the above problems, propose that a kind of new grain boundary diffusion process prepares low-cost and high-performance neodymium iron boron magnetic body
Method, i.e., selection dysprosium, terbium, iron, aluminium, copper, gallium alloy powder be used as diffusion source, be coated in 2~8mm be orientated or non-oriented face
On, then according to finished product final size, selects an appropriate number of magnet superposition to be put into diffusion bonding in sintering furnace and handle, obtain big
The high performance sintered magnet of block is orientated size not at the finished product of other specifications using machine finishing according still further to customer demand
It is restricted.
Specifically, the present invention provides a kind of preparation methods of new neodymium iron boron magnetic body, comprising:
1) dysprosium, terbium, iron, aluminium, copper, gallium alloy powder slurry are uniformly coated to neodymium iron boron magnetic body piece surface；
2) superposition of coated magnet muti-piece is put into magazine, bonding bulk sintered magnet is obtained by sintering.
Preferably, step 1) dysprosium, terbium, iron, aluminium, copper, gallium alloy powder slurry are uniformly coated to neodymium iron boron magnetic body piece orientation
Or non-oriented face surface, orientation or non-oriented face preferably 2~8mm, more preferably 2~6mm.
Preferably, the coated magnet of step 2) can be superimposed along oriented surface or non-oriented face muti-piece.
Preferably, rapid 1) dysprosium, terbium, iron, aluminium, copper, gallium alloy ingot casting are selected from (Dy)80Fe3Al10Cu4Ga3Or (Tb)80Fe3Al10Cu4Ga3, 80:3:10:4:3 is weight ratio.
Preferably, step 1) dysprosium, terbium, iron, aluminium, copper, gallium alloy ingot casting are by commercially available terbium, iron, aluminium, copper, gallium according to weight
Proportions are made by vacuum melting furnace fusing.
Preferably, step 1) dysprosium, terbium, iron, aluminium, copper, gallium alloy powder coating weight account for neodymium-iron-boron body weight 0.3~
1%.
Preferably, step 1) dysprosium, terbium, iron, aluminium, copper, the alloy powder and solvent that gallium alloy powder slurry is 2~4 microns
The slurries being mixed according to the mass ratio of 1:1~1.5, wherein solvent is selected from ethyl alcohol, methanol or petroleum ether, preferably sewage second
Alcohol, sewage methanol or petroleum ether.
It is furthermore preferred that 2~4 microns of alloy powder inhales hydrogen using hydrogen broken furnace by dysprosium, terbium, iron, aluminium, copper, gallium alloy ingot casting
The powders A of 110~150 μm or so partial sizes is made in dehydrogenation, then 2~4 microns of alloy powder B is made on centrifugal ball mill.
It is further preferred that dysprosium, terbium, iron, aluminium, copper, gallium alloy ingot casting utilize hydrogen broken furnace, in 0.1~0.2Mpa hydrogen pressure
Lower saturation inhales hydrogen, and the powders A of 110~150 μm or so partial sizes is made in the dehydrogenation at 400~600 DEG C.
It is furthermore preferred that step 2) superposition quantity is calculated according to finished size, coated magnet muti-piece superposition is put into magazine
In, it is placed in vacuum sintering furnace and is sintered 3~10 hours for 700~1000 DEG C, be then quickly cooled to 70 DEG C hereinafter, being warming up to again
500~600 DEG C, second annealing keeps the temperature 3~5 hours, finally obtains bonding bulk sintered magnet.
Preferably, the bonding bulk sintered magnet of step 2) can according to customer demand using machine finishing at other
The finished product of specification.
Dysprosium that the present invention uses, terbium, iron, aluminium, copper, gallium alloy have lower than dysprosium, the hydride of terbium, oxide, fluoride
Many fusing points, the non-oriented face of powder coating and 2~8mm can be melt into liquid phase, diffuse to magnet at 700~1000 DEG C
Inside, diffusion velocity and depth are higher than hydride, oxide, fluoride, improve performance amplitude and also become apparent.In addition, its
Liquid phase plays bonding effect, the magnet being superimposed can be closely bonded together, achieve the effect that welding, ultimately form
The high performance magnet of bulk, it is identical that orientation size can directly add dysprosium terbium magnet with melting, is then added again according to customer demand
Work at different size finished product, orientation size is unrestricted, and the rubidium iron boron magnet performance prepared by this law is high, at low cost.
Specific embodiment
The present invention will be further described with reference to the examples below.Described embodiment and its result are merely to illustrate
The present invention, without the present invention described in detail in claims should will not be limited.
Embodiment 1
1) commercially available dysprosium, iron, aluminium, copper, gallium are proportionally matched, are melted by vacuum melting furnace, alloy cast ingot is made,
Alloying component is (Dy)80Fe3Al10Cu4Ga3(weight ratio)；
2) by (Dy)80Fe3Al10Cu4Ga3Alloy cast ingot utilizes hydrogen broken furnace, depresses saturation in 0.1MPa hydrogen and inhales hydrogen,
The powders A of 110~150 μm or so partial sizes is made in dehydrogenation at 500 DEG C；
3) by (Dy) of step 2)80Fe3Al10Cu4Ga3Powder is made 3 microns of average grain diameter on centrifugal ball mill
(Dy)80Fe3Al10Cu4Ga3Powder B；
4) B powder and dehydrated alcohol are mixed and made into slurries according to 1:1 weight ratio, be uniformly coated to clean up it is commercially available
N50 neodymium iron boron matrix, specification are the non-oriented face of 6mm*50.8mm*51.2mm having a size of on the non-oriented face of 6mm, and coated weight accounts for
The 0.6% of magnet weight；
5) the coated magnet of step 4) is put into magazine according to the superposition of 7, the direction 6mm, is placed in vacuum sintering furnace
900 DEG C are sintered 4 hours, are then quickly cooled to 70 DEG C hereinafter, being warming up to 500 DEG C again, second annealing keeps the temperature 3~5 hours, most
The bulk sintered magnet of bonding 42mm*50.8mm*51.2mm orientation size 51.2mm is obtained eventually；
6) by the bulk sintered magnet of 42mm*50.8mm*51.2mm using machine finishing at 4 41.5mm*50mm*
The finished product of the customer demand of 12mm size.
The performance of magnet is shown in Table 1 after the performance and DIFFUSION TREATMENT of matrix before the processing of its grain boundary decision.
Embodiment 2
1) commercially available dysprosium, iron, aluminium, copper, gallium are proportionally matched, are melted by vacuum melting furnace, alloy cast ingot is made,
Alloying component is (Dy)80Fe3Al10Cu4Ga3(weight ratio)；
2) by (Dy)80Fe3Al10Cu4Ga3Alloy cast ingot utilizes hydrogen broken furnace, depresses saturation in 0.1MPa hydrogen and inhales hydrogen,
The powders A of 110~150 μm or so partial sizes is made in dehydrogenation at 500 DEG C；
3) by (Dy) of step 2)80Fe3Al10Cu4Ga3Powder is made 3 microns of average grain diameter on centrifugal ball mill
(Dy)80Fe3Al10Cu4Ga3Powder B；
4) B powder and dehydrated alcohol are mixed and made into slurries according to 1:1 weight ratio, be uniformly coated to clean up it is commercially available
N50 neodymium iron boron matrix, specification are the non-oriented face of 3mm*50.8mm*51.2mm having a size of on the non-oriented face of 3mm, and coated weight accounts for
The 0.8% of magnet weight；
5) the coated magnet of step 4) is put into magazine according to the superposition of 14, the direction 3mm, is placed in vacuum sintering furnace
900 DEG C are sintered 4 hours, are then quickly cooled to 70 DEG C hereinafter, being warming up to 500 DEG C again, and second annealing keeps the temperature 3~5 hours,
Finally obtain the bulk sintered magnet of bonding 42mm*50.8mm*51.2mm orientation size 51.2mm；
6) by the bulk sintered magnet of 42mm*50.8mm*51.2mm using machine finishing at 4 41.5mm*50mm*
The finished product of the customer demand of 12mm or other specifications.
The performance of magnet is shown in Table 1 after its DIFFUSION TREATMENT.
Embodiment 3
1) commercially available terbium, iron, aluminium, copper, gallium are proportionally matched, are melted by vacuum melting furnace, alloy cast ingot is made,
Alloying component is (Tb)80Fe3Al10Cu4Ga3(weight ratio)；
2) by (Tb)80Fe3Al10Cu4Ga3Alloy cast ingot utilizes hydrogen broken furnace, depresses saturation in 0.1MPa hydrogen and inhales hydrogen,
The powders A of 110~150 μm or so partial sizes is made in dehydrogenation at 500 DEG C；
3) by (Tb) of step 2)80Fe3Al10Cu4Ga3Powder is made 3 microns of average grain diameter on centrifugal ball mill
(Tb)80Fe3Al10Cu4Ga3Powder B；
4) B powder and dehydrated alcohol are mixed and made into slurries according to 1:1 weight ratio, be uniformly coated to clean up it is commercially available
N50 neodymium iron boron matrix, specification are the non-oriented face of 6mm*50.8mm*51.2mm having a size of on the non-oriented face of 6mm, and coated weight accounts for
The 0.6% of magnet weight.
5) the coated magnet of step 4) is put into magazine according to the superposition of 7, the direction 6mm, is placed in vacuum sintering furnace
900 DEG C are sintered 4 hours, are then quickly cooled to 70 DEG C hereinafter, being warming up to 500 DEG C again, and second annealing keeps the temperature 3~5 hours,
Finally obtain the bulk sintered magnet of bonding 42mm*50.8mm*51.2mm orientation size 51.2mm；
6) by the bulk sintered magnet of 42mm*50.8mm*51.2mm using machine finishing at 4 41.5mm*50mm*
The finished product of the customer demand of 12mm size.
The performance of magnet is shown in Table 1 after the processing of its grain boundary decision.
Embodiment 4
1) commercially available terbium, iron, aluminium, copper, gallium are proportionally matched, are melted by vacuum melting furnace, alloy cast ingot is made,
Alloying component is (Tb)80Fe3Al10Cu4Ga3(weight ratio)；
2) by (Tb)80Fe3Al10Cu4Ga3Alloy cast ingot utilizes hydrogen broken furnace, depresses saturation in 0.1MPa hydrogen and inhales hydrogen,
The powders A of 110~150 μm or so partial sizes is made in dehydrogenation at 500 DEG C；
3) with (Tb) of step 2)80Fe3Al10Cu4Ga3Powder is made 3 microns of average grain diameter on centrifugal ball mill
(Tb)80Fe3Al10Cu4Ga3Powder B；
4) B powder and dehydrated alcohol are mixed and made into slurries according to 1:1 weight ratio, be uniformly coated to clean up it is commercially available
N50 neodymium iron boron matrix, specification are the non-oriented face of 3mm*50.8mm*51.2mm having a size of on the non-oriented face of 3mm, and coated weight accounts for
The 0.8% of magnet weight；
5) the coated magnet of step 4) is put into magazine according to the superposition of 14, the direction 3mm, is placed in vacuum sintering furnace
900 DEG C are sintered 4 hours, are then quickly cooled to 70 DEG C hereinafter, being warming up to 500 DEG C again, and second annealing keeps the temperature 3~5 hours,
Finally obtain the bulk sintered magnet of the orientation size 51.2mm of bonding 42mm*50.8mm*51.2mm；
6) by the bulk sintered magnet of 42mm*50.8mm*51.2mm using machine finishing at 4 pieces of 41.5mm*50mm*
The finished product of the customer demand of 12mm or other specifications.
The performance of magnet is shown in Table 1 after the processing of its grain boundary decision.
The different magnet performance parameters of table 1
The magnet of the different embodiments of table 2 and its quite commercially available magnet dysprosium terbium content
| Magnet | The trade mark | Dysprosium content | Terbium content |
| N50 rubidium iron boryl body | N50 | 0 | 0 |
| Magnet after the processing of embodiment 1 | 50H | 0.48% | 0 |
| Magnet after the processing of embodiment 2 | 50SH | 0.64% | 0 |
| Magnet after the processing of embodiment 3 | 50HT | 0 | 0.48% |
| Magnet after the processing of embodiment 4 | 50SHT | 0 | 0.64% |
| Commercially available magnet (suitable with example 1) | 50H | 0 | 1.0% |
| Commercially available magnet (suitable with example 2) | 50SH | 0 | 1.8% |
By the magnet and its quite commercially available magnet dysprosium terbium content of the different magnet performance parameters of upper table 1 and the different embodiments of table 2
It is found that by the method for the invention, preparing the bulk magnet of orientation length 51.2mm, coercivity is substantially increased, and dysprosium terbium content is big
Width reduces, namely high, at low cost by rubidium iron boron magnet performance prepared by this law.
In short, technique according to the invention, using dysprosium, terbium, iron, aluminium, copper, gallium alloy powder as diffusion source, fusing point
Low, 900 DEG C of whens, are diffused into inside magnet with liquid form along the non-oriented face of 3~6mm, and diffusion depth and speed are better than
It is bigger to promote coercivity amplitude for dysprosium, the fluoride of terbium, hydride, oxide；In addition, alloy powder at 900 DEG C at liquid,
Be conducive to be bonded integrally between magnet, prepare the magnet of bulk；Compared with existing grain boundary decision technology, the prior art limits magnetic
The size of body usually permeates dysprosium, terbium being orientated within size 5mm oriented surface, and the present invention to orientation size there is no limit.
Claims (10)
1. a kind of preparation method of new neodymium iron boron magnetic body, comprising:
1) dysprosium, terbium, iron, aluminium, copper, gallium alloy powder slurry are uniformly coated to neodymium iron boron magnetic body piece surface；
2) superposition of coated magnet muti-piece is put into magazine, bonding bulk sintered magnet is obtained by sintering.
2. preparation method according to claim 1, wherein step 1) dysprosium, terbium, iron, aluminium, copper, gallium alloy powder slurry are equal
It is even to be coated to neodymium iron boron magnetic body piece orientation or non-oriented face surface, orientation or non-oriented face preferably 2~8mm, more preferable 2~6mm；
The coated magnet of step 2) can be preferably superimposed along oriented surface or non-oriented face muti-piece.
3. preparation method according to claim 1, wherein step 1) dysprosium, terbium, iron, aluminium, copper, gallium alloy ingot casting are selected from
(Dy)80Fe3Al10Cu4Ga3Or (Tb)80Fe3Al10Cu4Ga3, 80:3:10:4:3 is weight ratio.
4. preparation method according to claim 1, wherein step 1) dysprosium, terbium, iron, aluminium, copper, gallium alloy ingot casting is will be commercially available
Terbium, iron, aluminium, copper, gallium are matched according to weight ratio, are made by vacuum melting furnace fusing.
5. preparation method according to claim 1, wherein step 1) dysprosium, terbium, iron, aluminium, copper, gallium alloy powder coating weight
Amount accounts for the 0.3~1% of neodymium-iron-boron body weight.
6. preparation method according to claim 1, wherein step 1) dysprosium, terbium, iron, aluminium, copper, gallium alloy powder slurry are 2
The slurries that~4 microns of alloy powder and solvent is mixed according to the mass ratio of 1:1~1.5, wherein solvent is selected from ethyl alcohol, first
Alcohol or petroleum ether.
7. preparation method according to claim 6, wherein 2~4 microns of alloy powder is by dysprosium, terbium, iron, aluminium, copper, gallium
Alloy cast ingot inhales hydrogen dehydrogenation using hydrogen broken furnace, the powders A of 110~150 μm or so partial sizes is made, then make on centrifugal ball mill
At 2~4 microns of alloy powder B.
8. preparation method according to claim 7, wherein dysprosium, terbium, iron, aluminium, copper, gallium alloy ingot casting utilize hydrogen broken furnace,
0.1~0.2Mpa hydrogen pressure saturation inhales hydrogen, and the powders A of 110~150 μm or so partial sizes is made in the dehydrogenation at 400~600 DEG C.
9. preparation method according to claim 1, wherein step 2) superposition quantity is calculated according to finished size, is coated
The superposition of magnet muti-piece be put into magazine, be placed in vacuum sintering furnace 700~1000 DEG C and be sintered 3~10 hours, then fast quickly cooling
But to 70 DEG C hereinafter, being warming up to 500~600 DEG C again, second annealing keeps the temperature 3~5 hours, finally obtains bonding bulk and burns
Tie magnet.
10. preparation method according to claim 1, wherein the bonding bulk sintered magnet of step 2) can be according to client
Demand is using machine finishing at the finished product of other specifications.
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| CN110335752A (en) * | 2019-07-25 | 2019-10-15 | 宁波合盛磁业有限公司 | A kind of Sintered NdFeB magnet infiltration dysprosium technique |
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| CN112908601A (en) * | 2020-01-21 | 2021-06-04 | 福建省长汀金龙稀土有限公司 | R-Fe-B sintered magnet and grain boundary diffusion treatment method thereof |
| CN112908672A (en) * | 2020-01-21 | 2021-06-04 | 福建省长汀金龙稀土有限公司 | Grain boundary diffusion treatment method for R-Fe-B rare earth sintered magnet |
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| WO2021147908A1 (en) * | 2020-01-21 | 2021-07-29 | 厦门钨业股份有限公司 | R-fe-b sintered magnet and grain boundary diffusion treatment method therefor |
| CN112908672B (en) * | 2020-01-21 | 2024-02-09 | 福建省金龙稀土股份有限公司 | Grain boundary diffusion treatment method for R-Fe-B rare earth sintered magnet |
| CN112908601B (en) * | 2020-01-21 | 2024-03-19 | 福建省金龙稀土股份有限公司 | R-Fe-B sintered magnet and grain boundary diffusion treatment method thereof |
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