CN107845464A - A kind of method for preparing high-coercive force Nd-Fe-B series permanent magnet - Google Patents
A kind of method for preparing high-coercive force Nd-Fe-B series permanent magnet Download PDFInfo
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- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000009792 diffusion process Methods 0.000 claims abstract description 40
- 238000000137 annealing Methods 0.000 claims abstract description 38
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 27
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 25
- 239000000956 alloy Substances 0.000 claims abstract description 25
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 14
- 238000007493 shaping process Methods 0.000 claims abstract description 14
- 239000013618 particulate matter Substances 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 14
- 238000005266 casting Methods 0.000 claims description 11
- 238000002844 melting Methods 0.000 claims description 11
- 230000008018 melting Effects 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 239000011261 inert gas Substances 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 6
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 5
- 229910052771 Terbium Inorganic materials 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 4
- 239000012928 buffer substance Substances 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 229910052733 gallium Inorganic materials 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 3
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical group O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 2
- 229910017086 Fe-M Inorganic materials 0.000 claims 4
- 230000005389 magnetism Effects 0.000 abstract description 11
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 29
- 230000005291 magnetic effect Effects 0.000 description 28
- 230000000052 comparative effect Effects 0.000 description 19
- 229910000521 B alloy Inorganic materials 0.000 description 14
- 238000005275 alloying Methods 0.000 description 11
- 239000008188 pellet Substances 0.000 description 11
- 239000012300 argon atmosphere Substances 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 238000000926 separation method Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 3
- -1 rare earth compound Chemical class 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910001092 metal group alloy Inorganic materials 0.000 description 2
- 230000005290 antiferromagnetic effect Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
Classifications
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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
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
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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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Abstract
The present invention provides a kind of method for preparing high-coercive force Nd-Fe-B series permanent magnet, and it comprises the following steps：（1）By Nd-Fe-B series alloy rapid-hardening flake with diffusion source rare earth alloys particulate matter according to weight ratio be 0.2：1~10：After 1 is well mixed, mixture is put into vacuum heat treatment furnace and is diffused heat treatment；（2）After unnecessary diffusion source is separated, homogenizing annealing processing is carried out to product；（3）Sintered NdFeB based permanent magnet is made through powder processed, shaping, sintering.The present invention implements diffusion heat treatments to neodymium iron boron rapid-hardening flake by rare earth alloys particulate matter and homogenizing annealing is heat-treated, and may be implemented under conditions of not reducing remanent magnetism, improves the coercivity of magnet, and technical process is simple, it is easy to accomplish industrialization.
Description
Technical field
The invention belongs to rare earth permanent magnet technical field, specially a kind of side for preparing high-coercive force Nd-Fe-B series permanent magnet
Method.
Background technology
Magnetic material be using one of high-tech functional material indispensable as the modernized society of the strong point, its application and
Development has gradually obtained the attention of people, particularly third generation rare earth permanent magnet-Nd-Fe-B permanent magnet material, with its excellent magnetic
Can, one it is found that i.e. obtain a wide range of applications, be mainly used in wind-power electricity generation, Aero-Space, health care, new-energy automobile
Etc. various fields.
With the further expansion of application field, higher requirement also is proposed to the performance of Nd-Fe-B permanent magnet material, it is special
It is not the coercivity of magnet.It is exactly that heavy rare earth element is added in magnet to improve neodymium iron boron magnetic body coercivity most efficient method
(such as Dy, Tb), but heavy rare earth element and iron dust, in antiferromagnetic coupling, the addition of heavy rare earth element can cause the drop of magnet remanent magnetism
It is low.Simultaneously as heavy rare earth element resource reserve is few, price is high, the addition of heavy rare earth element improves to a certain extent
The price of magnet, and then limit the expansion of its application field.How in the case where not reducing magnet remanent magnetism, rectifying for magnet is improved
Stupid power, and the content of heavy rare earth element is reduced simultaneously, having become Nd-Fe-B series permanent magnet development must solve the problems, such as.
Grain boundary decision technology is emerging technology developed in recent years, and can realize to a certain extent is not reducing magnetic
In the case of body remanent magnetism, the coercivity of magnet is improved, reduces the content of heavy rare earth element in magnet.However, that has invented is more
Kind grain boundary decision technology is diffused mainly for the magnet of densified sintering product, is influenceed by elements diffusion depth, and these technologies are only
It can apply to the magnet that minimum dimension direction is less than 10mm, it is impossible to meet the expansion of bulk magnet of the minimum dimension direction more than 10mm
Dissipate and require.
On the basis of magnet grain boundary decision, it is proposed that rapid-hardening flake diffusion technique (patent No. ZL200910098063.4),
Cladding diffusion is carried out by the way that neodymium iron boron rapid-hardening flake is put into heavy rare earth compound turbid liquid, the basis of magnetic energy product can not reduced
Upper raising magnet coercivity, but this method is difficult to ensure that heavy rare earth compound in the surface coated uniformity of rapid-hardening flake, and due to
The preparation difficulty of heavy rare earth compound turbid liquid is larger, and this method is difficult to industrialized production.
The content of the invention
It is an object of the invention to provide a kind of method for preparing high-coercive force Nd-Fe-B series permanent magnet, the Nd-Fe-B series of preparation
Permanent magnet has higher coercivity in the case where remanent magnetism and maximum magnetic energy product are same or like
A kind of method for preparing high-coercive force Nd-Fe-B series permanent magnet, it comprises the following steps：
(1) by Nd-Fe-B series alloy rapid-hardening flake and diffusion source rare earth-metal (AxD100-x) alloying pellet thing is according to weight ratio
For 0.2：1~10：After 1 is well mixed, mixture is put into vacuum heat treatment furnace and is diffused heat treatment；
(2) after unnecessary diffusion source is separated, homogenizing annealing processing is carried out to product；
(3) sintered NdFeB based permanent magnet is made through powder processed, shaping, sintering.
Further scheme, the Nd-Fe-B series alloy rapid-hardening flake are prepared using melting strip casting, and its is main
Composition is RE- (Fe-M)-B, and wherein RE is the one or more in Pr, Nd, Dy, Tb, Ho, Gd, Ce, M Cu, Al, Co, Nb,
One or more in Ga, Zr, Zn.
Further scheme, RE mass percent is 29%~33% in RE- (the Fe-M)-B, the quality of (Fe-M)
Percentage is that 0.5%~8%, the B that 60%~69%, M accounts for (Fe-M) is surplus.
Further scheme, the rare earth-metal alloy particle thing middle rare earth are at least one of Dy, Tb element, metal
For at least one of Fe, Co, Ni, Cu, Zn, Al, Ga element.
Further scheme, the average thickness of the Nd-Fe-B series alloy rapid-hardening flake is 100~500 μm, the rare earth-metal
The particle mean size of alloying pellet thing is 100 μm~3mm.
Further scheme, the vacuum heat treatment furnace carry agitating device, can constantly stirred during diffusion heat treatments
Mix, diffusion source rare earth-metal alloy particle thing is uniformly contacted with Nd-Fe-B series alloy rapid-hardening flake；Vacuum heat furnace interior is
Vacuum or inert gas atmosphere.
Further scheme, the vacuum of the vacuum heat treatment furnace are higher than 1.0 × 10-2Pa；The inert gas is pressure
For 5~120Kpa argon gas and/or helium.
Further scheme, the temperature of the diffusion heat treatments is 600~850 DEG C, the time is 4~20h；In diffusion heat treatments
When add and account for 0~10% buffer substance of total weight of the mixture.
Further scheme, the buffer substance are aluminum oxide, zirconium oxide or titanium oxide.
Further scheme, the temperature of the homogenizing annealing processing is 500~900 DEG C, and annealing time is 3~10h；It is described
The vacuum of vacuum is higher than 1.0 × 10-2Pa, and the inert gas is the argon gas and/or helium that pressure is 5~120Kpa.
The present invention, which utilizes, spreads source rare earth-metal (AxD100-x) alloying pellet thing expands Nd-Fe-B series alloy rapid-hardening flake
Sintered NdFeB based permanent magnet is made through homogenizing annealing, powder processed, shaping, sintering in radiating treatment, the rapid-hardening flake after diffusion.
Nd-Fe-B series permanent magnet prepared by the present invention compares Nd-Fe-B series permanent magnet prepared by non-crystal boundary diffusion technique, surplus
In the case that magnetic and maximum magnetic energy product are same or like, there is higher coercivity.
Nd-Fe-B series permanent magnet prepared by the present invention compares magnet grain boundary decision technology, and the present invention is directed to Nd-Fe-B series rapid hardening
Piece is diffused heat treatment, and any specification can be made after homogenizing annealing, powder processed, shaping, sintering in the rapid-hardening flake after diffusion
Sintered Nd-Fe-B permanent magnet.
The present invention compares the rapid-hardening flake diffusion technique mentioned in patented technology ZL200910098063.4, and the present invention uses dilute
Soil-metal alloy particle thing is diffusion source, and technical process is simple, it is easy to accomplish industrialization；Meanwhile rare earth-metal alloy particle
After thing separates with rapid-hardening flake, it can reuse, diffusion cost significantly reduces.
Embodiment
With reference to instantiation, the present invention is further described.
Embodiment 1：
Using Nd Fe B alloys rapid-hardening flake made of melting strip casting, its composition is (PrNd)29.7Dy1.0B1.02Co0.9Cu0.1Al0.1Tb0.6Ga0.2Fe66.38；Prepare the Dy as diffusion source80Cu20Alloying pellet thing, it is average
Granularity 3mm；Then diffusion source is pressed 1 with Nd Fe B alloys rapid-hardening flake:1 weight after being well mixed than being put into vacuum heat treatment furnace
In, 16h is heat-treated under the conditions of 750 DEG C, using 100kPa argon atmosphere.Rapid-hardening flake and alloy after separation diffusion
Grain thing, rapid-hardening flake is subjected to homogenizing annealing processing under vacuum conditions, 900 DEG C, time 2h of annealing temperature, vacuum 3.2 ×
10-3Pa.Rapid-hardening flake after annealing obtains sintered magnet through powder processed, shaping and sintering.
Comparative example 1：
Using Nd Fe B alloys rapid-hardening flake made of melting strip casting, its composition is (PrNd)29.7Dy1.0B1.02Co0.9Cu0.1Al0.1Tb0.6Ga0.2Fe66.38；Then put it into vacuum heat treatment furnace, under the conditions of 750 DEG C
16h is heat-treated, using 100kPa argon atmosphere, then carries out homogenizing annealing processing, annealing temperature under vacuum conditions
900 DEG C, time 2h, vacuum 3.2 × 10-3Pa.Rapid-hardening flake after annealing obtains sintered magnet through powder processed, shaping and sintering.
The magnetic property of two kinds of magnets is as shown in table 1.
| Sample ID | Remanent magnetism (kGs) | Coercivity (kOe) | Maximum magnetic energy product (MGOe) |
| Embodiment 1 | 13.38 | 22.11 | 43.39 |
| Comparative example 1 | 13.46 | 18.1 | 43.37 |
The above results show that the present invention uses rare earth-metal alloy particle thing to implement to spread to rapid-hardening flake for diffusion source, warp
Magnet coercivity improves about 4kOe relative to comparative example 1 after sintering；And two kinds of magnets preparing of embodiment 1 and comparative example 1 is surplus
Magnetic and maximum magnetic energy product are suitable, but the comprehensive magnetic of the magnet of the preparation of embodiment 1 can be improved.
Embodiment 2：
Nd Fe B alloys rapid-hardening flake is made using melting strip casting, its composition is (PrNd)31.3Dy1.0B1.0Al0.6Cu0.18Co1.0Ga0.1Zr0.02Fe64.8, prepare the Dy as diffusion source60Fe40Alloying pellet thing, average grain
2mm is spent, itself and Nd Fe B alloys rapid-hardening flake are pressed 2:1 weight after being well mixed than being put into vacuum heat treatment furnace, at 700 DEG C
Under the conditions of be heat-treated 20h, vacuum 3.6 × 10-3Pa.Rapid-hardening flake and alloying pellet thing after separation diffusion, by rapid-hardening flake true
Homogenizing annealing processing, 500 DEG C, time 3h of annealing temperature, vacuum 3.8 × 10 are carried out under Altitude-3Pa.Rapid hardening after annealing
Piece obtains sintered magnet through powder processed, shaping and sintering.
Comparative example 2：
Using Nd Fe B alloys rapid-hardening flake made of melting strip casting, its composition is (PrNd)31.3Dy1.0B1.0Al0.6Cu0.18Co1.0Ga0.1Zr0.02Fe64.8；Then put it into vacuum heat treatment furnace, under the conditions of 700 DEG C
It is heat-treated 20h, vacuum 3.6 × 10-3Pa, then homogenizing annealing processing is carried out under vacuum conditions, 500 DEG C of annealing temperature, when
Between 3h, vacuum 3.8 × 10-3Pa.Rapid-hardening flake after annealing obtains sintered magnet through powder processed, shaping and sintering.
The magnetic property of two kinds of magnets is as shown in table 2.
| Sample ID | Remanent magnetism (kGs) | Coercivity (kOe) | Maximum magnetic energy product (MGOe) |
| Embodiment 2 | 13.49 | 22.16 | 44.86 |
| Comparative example 2 | 13.53 | 17.83 | 44.53 |
The above results show that the present invention uses rare earth-metal alloy particle thing to implement to spread to rapid-hardening flake for diffusion source, warp
Magnet coercivity improves about 4kOe relative to comparative example 2 after sintering；And two kinds of magnets preparing of embodiment 2 and comparative example 2 is surplus
Magnetic and maximum magnetic energy product are suitable, but the comprehensive magnetic of the magnet of the preparation of embodiment 2 can be improved.
Embodiment 3：
Nd Fe B alloys rapid-hardening flake is made using melting strip casting, its composition is
Nd29.7Tb0.3Co0.5Cu0.1Zr0.1Ga0.1Fe68.22B0.98, prepare the Tb as diffusion source70Fe20Co10Alloying pellet thing, it is average
500 μm of granularity, itself and Nd Fe B alloys rapid-hardening flake are pressed 1.5:1 weight ratio is put into vacuum heat treatment furnace after being well mixed,
4h is heat-treated under the conditions of 850 DEG C, using 80kPa argon atmosphere.Rapid-hardening flake and alloying pellet thing after separation diffusion,
Rapid-hardening flake is subjected to homogenizing annealing processing, 700 DEG C, time 5h of annealing temperature, using 50kPa argon atmosphere.Annealing
Rapid-hardening flake afterwards obtains sintered magnet through powder processed, shaping and sintering.
Comparative example 3：
Using Nd Fe B alloys rapid-hardening flake made of melting strip casting, its composition is
Nd29.7Tb0.3Co0.5Cu0.1Zr0.1Ga0.1Fe68.22B0.98；Then put it into vacuum heat treatment furnace, it is hot under the conditions of 850 DEG C
4h is handled, using 80kPa argon atmosphere, then carries out homogenizing annealing processing, 700 DEG C, time 5h of annealing temperature, is used
50kPa argon atmosphere.Rapid-hardening flake after annealing obtains sintered magnet through powder processed, shaping and sintering.
The magnetic property of two kinds of magnets is as shown in table 3.
| Sample ID | Remanent magnetism (kGs) | Coercivity (kOe) | Maximum magnetic energy product (MGOe) |
| Embodiment 3 | 14.33 | 16.9 | 50.63 |
| Comparative example 3 | 14.46 | 11.47 | 50.34 |
The above results show that the present invention uses rare earth-metal alloy particle thing to implement to spread to rapid-hardening flake for diffusion source, warp
Magnet coercivity improves about 5.4kOe relative to comparative example 3 after sintering；And embodiment 3 and two kinds of magnets of the preparation of comparative example 3
Remanent magnetism and maximum magnetic energy product are suitable, but the comprehensive magnetic of the magnet of the preparation of embodiment 3 can be improved.
Embodiment 4：
Nd Fe B alloys rapid-hardening flake is made using melting strip casting, its composition is (PrNd)31.5Fe66.48B1.02Co0.5Cu0.1Al0.2Ga0.2；Prepare the Tb as diffusion source60Dy20Fe16Zn2Cu2Alloying pellet thing, average grain
800 μm of degree, itself and Nd Fe B alloys rapid-hardening flake are pressed 3:It is put into vacuum heat treatment furnace, adds after 1 mass ratio is well mixed
Zirconia ball is heat-treated 10h, vacuum 3.3 × 10 as cushion (the 5% of mixture gross mass) under the conditions of 750 DEG C- 3Pa.Rapid-hardening flake and alloying pellet thing after separation diffusion, rapid-hardening flake is subjected to homogenizing annealing processing, 800 DEG C of annealing temperature,
Time 3h, using 110kPa argon atmosphere.Rapid-hardening flake after annealing obtains sintering magnetic through powder processed, shaping and sintering
Body.
Comparative example 4：
Using Nd Fe B alloys rapid-hardening flake made of melting strip casting, its composition is (PrNd)31.5Fe66.48B1.02Co0.5Cu0.1Al0.2Ga0.2；Then put it into vacuum heat treatment furnace, be heat-treated under the conditions of 750 DEG C
10h, vacuum 3.3 × 10-3Pa, then handled through homogenizing annealing, 800 DEG C, time 3h of annealing temperature, using 110kPa argon gas
Protective atmosphere.Rapid-hardening flake after annealing obtains sintered magnet through powder processed, shaping and sintering.
The magnetic property of two kinds of magnets is as shown in table 4.
Embodiment 5：
The Nd Fe B alloys rapid-hardening flake of composition same as Example 4 is made using melting strip casting, and (composition is
(PrNd)31.5Fe66.48B1.02Co0.5Cu0.1Al0.2Ga0.2), the Tb separated using embodiment 460Dy20Fe16Zn2Cu2Alloy
Particulate matter is diffused as diffusion source, and itself and Nd Fe B alloys rapid-hardening flake are pressed into 3:It is put into after 1 mass ratio is well mixed true
In empty heat-treatment furnace, titanium oxide ball is added as cushion (account for mixture gross mass 10%), is heat-treated under the conditions of 750 DEG C
10h, vacuum 3.3 × 10-3Pa.Rapid-hardening flake and alloying pellet thing after separation diffusion, rapid-hardening flake is carried out at homogenizing annealing
Reason, 800 DEG C, time 3h of annealing temperature, using 110kPa argon atmosphere.Rapid-hardening flake after annealing through powder processed, shaping and
Sintering, that is, obtain sintered magnet (identical with the technique of embodiment 4).
Comparative example 4 and comparative example 4, its magnetic property are as shown in table 4.
| Sample ID | Remanent magnetism (kGs) | Coercivity (kOe) | Maximum magnetic energy product (MGOe) |
| Embodiment 5 | 13.47 | 20.81 | 44.18 |
| Embodiment 4 | 13.49 | 20.76 | 44.08 |
| Comparative example 4 | 13.52 | 14.2 | 44.12 |
As a result show, the present invention uses rare earth-metal alloy particle thing to implement to spread to rapid-hardening flake for diffusion source, sintered
Magnet coercivity improves about 6.5kOe relative to comparative example 4 afterwards；And embodiment 4 and the remanent magnetism of two kinds of magnets of the preparation of comparative example 4
It is suitable with maximum magnetic energy product, but the comprehensive magnetic of the magnet of the preparation of embodiment 4 can be improved.In addition, rare earth in the present invention-
Metal alloy particle thing is as the repeatable utilization in diffusion source, by implementing to spread to rapid-hardening flake, sintered rear magnet coercivity phase
About 6.5kOe is also improved for comparative example 4；And embodiment 5 is suitable with the comprehensive magnetic energy of two kinds of magnets prepared by embodiment 4.
The above described is only a preferred embodiment of the present invention, not make any form to technical scheme
On limitation.Without departing from the spirit and scope of the present invention, the changes and improvements carried out to the present invention still fall within requirement
The scope of the present invention of protection.
Claims (10)
- A kind of 1. method for preparing high-coercive force Nd-Fe-B series permanent magnet, it is characterised in that：Comprise the following steps：（1）By Nd-Fe-B series alloy rapid-hardening flake with diffusion source rare earth-metal alloy particle thing according to weight ratio be 0.2：1~10：1 After well mixed, mixture is put into vacuum heat treatment furnace and is diffused heat treatment；（2）After unnecessary diffusion source is separated, homogenizing annealing processing is carried out to product；（3）Sintered NdFeB based permanent magnet is made through powder processed, shaping, sintering.
- A kind of 2. method for preparing high-coercive force Nd-Fe-B series permanent magnet according to claim 1, it is characterised in that：It is described Nd-Fe-B series alloy rapid-hardening flake is prepared using melting strip casting, and its main component is RE- (Fe-M)-B, wherein RE For the one or more in Pr, Nd, Dy, Tb, Ho, Gd, Ce, the one or more in M Cu, Al, Co, Nb, Ga, Zr, Zn.
- A kind of 3. method for preparing high-coercive force Nd-Fe-B series permanent magnet according to claim 2, it is characterised in that：It is described RE mass percent is 29% ~ 33% in RE- (Fe-M)-B, and the mass percent of (Fe-M) accounts for (Fe-M) for 60% ~ 69%, M 0.5% ~ 8%, B are surplus.
- A kind of 4. method for preparing high-coercive force Nd-Fe-B series permanent magnet according to claim 1, it is characterised in that：It is described Rare earth-metal alloy particle thing middle rare earth is at least one of Dy, Tb element, in metal Fe, Co, Ni, Cu, Zn, Al, Ga At least one element.
- A kind of 5. method for preparing high-coercive force Nd-Fe-B series permanent magnet according to claim 1, it is characterised in that：It is described The average thickness of Nd-Fe-B series alloy rapid-hardening flake is 100 ~ 500 μm, and the particle mean size of the rare earth-metal alloy particle thing is 100μm ~3mm。
- A kind of 6. method for preparing high-coercive force Nd-Fe-B series permanent magnet according to claim 1, it is characterised in that：It is described Vacuum heat treatment furnace carries agitating device, can be stirred continuously during diffusion heat treatments, makes diffusion source rare earth-metal alloy Particulate matter uniformly contacts with Nd-Fe-B series alloy rapid-hardening flake；Vacuum heat furnace interior is vacuum or inert gas atmosphere.
- A kind of 7. method for preparing high-coercive force Nd-Fe-B series permanent magnet according to claim 6, it is characterised in that：It is described The vacuum of vacuum heat treatment furnace is higher than 1.0 × 10-2Pa；The inert gas is the argon gas and/or helium that pressure is 5 ~ 120Kpa Gas.
- A kind of 8. method for preparing high-coercive force Nd-Fe-B series permanent magnet according to claim 1, it is characterised in that：It is described The temperature of diffusion heat treatments is 600 ~ 850 DEG C, time 4-20h；In diffusion heat treatments add account for total weight of the mixture 0 ~ 10% buffer substance.
- A kind of 9. method for preparing high-coercive force Nd-Fe-B series permanent magnet according to claim 8, it is characterised in that：It is described Buffer substance is aluminum oxide, zirconium oxide or titanium oxide.
- A kind of 10. method for preparing high-coercive force Nd-Fe-B series permanent magnet according to claim 1, it is characterised in that：Institute The temperature for stating homogenizing annealing processing is 500 ~ 900 DEG C, and annealing time is 3 ~ 10h；The atmosphere of the homogenizing annealing is vacuum Or inert gas；The vacuum of the vacuum is higher than 1.0 × 10-2Pa, and the inert gas is the argon gas that pressure is 5 ~ 120Kpa And/or helium.
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| CN114974869A (en) * | 2022-06-01 | 2022-08-30 | 北京工业大学 | Method for efficiently regenerating high-performance neodymium iron boron magnet by using waste sintered neodymium iron boron blocks |
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