CN107895621A - A kind of method for improving rare-earth Nd-Fe-B magnetic property - Google Patents
A kind of method for improving rare-earth Nd-Fe-B magnetic property Download PDFInfo
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- CN107895621A CN107895621A CN201711100452.7A CN201711100452A CN107895621A CN 107895621 A CN107895621 A CN 107895621A CN 201711100452 A CN201711100452 A CN 201711100452A CN 107895621 A CN107895621 A CN 107895621A
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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
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
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Abstract
The present invention relates to rare-earth Nd-Fe-B permanent magnetic material technical field, more particularly to a kind of method for improving rare-earth Nd-Fe-B magnetic property, comprise the following steps：Broken antioxidant low temperature batch mixing low-temperature passivation forming vacuum sintering temper.The advantages of method that the present invention improves rare-earth Nd-Fe-B magnetic property has that technique is simple, low energy consumption, and production is safer, while properties of product uniformity is good, reduces the dosage of heavy rare earth, reduces material cost.The magnetic property of rare-earth Nd-Fe-B can be effectively improved using this method.
Description
Technical field
The present invention relates to rare-earth Nd-Fe-B permanent magnetic material technical field, more particularly to a kind of cost is low, technique simply carries
The method of high rare-earth Nd-Fe-B magnetic property.
Background technology
Sintered NdFeB magnet is the permanent-magnet material that comprehensive magnetic can be most strong in the world today, is surmounted with it in traditional permanent magnetism
The excellent specific property and cost performance of material, are widely applied to the fields such as the energy, traffic, machinery, medical treatment, computer, household electrical appliances, in state
Played an important role in people's economy.In the technical indicator of magnetic material, magnetic energy product is mostly important.Magnetic energy product representation unit volume
Magnet produces the energy size of external magnetic field.Magnetic energy product is high, it is meant that can export bigger power on motor with less magnet.
Neodymium iron boron is a kind of important rare earth permanent-magnetic material, has high energy product, high-coercive force, the characteristic such as in light weight, cost is low, is so far
Cost performance highest magnet untill the present, obtain reputation " magnetic king ".The appearance of neodymium iron boron, make magnetic device to high efficiency, minimize, light-duty
Change direction to develop.
In the prior art, heavy rare earth element Dy, Tb, Ho are mainly used in order to obtain high performance sintered neodymium-iron-boron, and its
The compound addition of its nonmetalloid, but heavy rare earth element Dy, Tb, Ho cost is higher, and more severe, heavy rare earth element has been visited
Bright reserves are very limited.With present depletion rate, in the near future, people's predicament rare by heavy rare earth element is faced.
Therefore, exploitation does not have to or is that strategy is needed badly less with low high performance sintered neodymium-iron-boron technologies of preparing of heavy rare earth such as Dy, Tb, Ho.
But same composition design and the performance of production technology summer blank are far below the blank performance of winter production in actual production.
The content of the invention
The present invention improves the method cost height of rare-earth Nd-Fe-B magnetic property, resource to overcome by adding heavy rare earth element
The problem of limited, there is provided a kind of method that cost is low, technique simply improves rare-earth Nd-Fe-B magnetic property.
To achieve these goals, the present invention uses following technical scheme：
A kind of method for improving rare-earth Nd-Fe-B magnetic property, comprises the following steps：
(1) rare-earth Nd-Fe-B permanent magnetic material alloy is crushed, obtains the powder that particle diameter is 2~100 μm；
(2) on the basis of powder gross mass, 0.1~5 ‰ antioxidant is added in the powder, is entered at -10~10 DEG C
Row low temperature batch mixing, obtains mixed powder；
(3) mixed powder is subjected to low-temperature passivation at -10~10 DEG C；
(4) powder after step (3) is passivated is injected in mould under nitrogen protection, is carried out oriented moulding and is obtained green compact, described
Green compact obtain base substrate through isostatic pressing；
(5) base substrate is put into vacuum sintering furnace, temperature-gradient method, then fast aeration cools down, and completes sintering；
(6) base substrate after vacuum-sintering is subjected to temper, is quickly cooled to room temperature, high magnetic characteristics rare-earth Nd-Fe-B is made forever
Magnetic material alloys.
The present invention relates to a kind of method for improving rare-earth Nd-Fe-B magnetic property, especially dropped with the neodymium iron boron of middle high-coercive force
The method that self raising flour material mixture temperature and storage temperature improve magnetic property.Its principle is：The powder that airflow milling makes is in low temperature
Batch mixing is carried out under environment, and is stored at low ambient temperatures, reduces the activity of powder, reaches the oxygen content in magnet after reduction sinters
Improve the purpose of magnetic property.Temperature is lower, and the protective effect for powder is better, temperature control effect between -10~10 DEG C
Most preferably, when powder activity is reduced to a certain extent, without adding antioxidant.Present invention process is simply to reducing heavy rare earth dosage drop
Low cost has remarkable effect.
Preferably, in step (1), using the broken crushing process being combined with airflow milling of hydrogen to rare-earth Nd-Fe-B permanent magnetism material
Material alloy is crushed.
Preferably, in step (2), mixing time is controlled in 60~100min.
Preferably, in step (3), passivation time is controlled in 8~12h.
Preferably, in step (4), the magnetic field intensity of oriented moulding is 1.2~2T, and pressure is 5~15MPa.
Preferably, in step (4), the Stress control of isostatic pressing is in 18~21Mpa.
Preferably, in step (5), before vacuum-sintering, by vacuum sintering furnace 60~100min of forvacuum, stove is set
Interior vacuum is 1 × E-2~1 × E-1Pa。
Preferably, in step (5), the temperature-gradient method is：
A. 400~450 DEG C are warming up to by 10/ DEG C of programming rate, are incubated 40~80min；
B. 850~900 DEG C are warming up to by 3 DEG C/min of programming rate, are incubated 180~240min；
C. 1000~1040 DEG C are warming up to by 3.5 DEG C/min of programming rate, are incubated 30~60min；
D. 1060~1080 DEG C are warming up to by 3.5 DEG C/min of programming rate, are incubated 240~300min.
Preferably, in step (6), the temper is double tempering, and 120~150min is incubated at 890~900 DEG C
First paragraph temper is carried out, then second of temper is carried out by 450~560 DEG C of 180~240min of insulation.
Therefore, the present invention has the advantages that：Technique is simple, low energy consumption, and production is safer, while properties of product
Uniformity is good, reduces the dosage of heavy rare earth, reduces material cost.Rare-earth Nd-Fe-B can be effectively improved using this method
Magnetic property.
Embodiment
Below by specific embodiment, technical scheme is described in further detail.
In the present invention, if not refering in particular to, all devices and raw material are commercially available or the industry is conventional, following
Method in embodiment, it is this area conventional method unless otherwise instructed.
Embodiment 1
It is (Nd, Pr) by composition29.5Dy2Co2Cu0.15Al1Nb0.3FeIt is remainingB0.95(wt%) Nd-Fe-B permanent magnet material alloy, by upper
Composition is stated to carry out dispensing and Nd-Fe-B permanent magnet material alloy is made with rapid hardening thin slice technique；
(1) above-mentioned rare-earth Nd-Fe-B permanent magnetic material alloy is crushed using hydrogen is broken with the crushing process that airflow milling is combined,
Obtain the powder that particle diameter is 2 μm；
(2) on the basis of powder gross mass, 5 ‰ antioxidant is added in the powder, low temperature batch mixing is carried out at 10 DEG C,
Mixing time is controlled in 60min, obtains mixed powder；
(3) mixed powder is subjected to low-temperature passivation at 10 DEG C, passivation time is controlled in 8h；
(4) powder after step (3) is passivated is injected in mould under nitrogen protection, sets magnetic field intensity as 1.2T, pressure is
5MPa carries out oriented moulding and obtains 50 × 39 × 32 (mm) green compact, and green compact obtain base substrate through 18Mpa isostatic pressings；
(5) base substrate is put into vacuum sintering furnace, by vacuum sintering furnace forvacuum 60min, sets in stove vacuum as 5
×E-2Pa, temperature-gradient method：
A. 400 DEG C are warming up to by 10/ DEG C of programming rate, are incubated 80min；
B. 850 DEG C are warming up to by 3 DEG C/min of programming rate, are incubated 240min；
C. 1000 DEG C are warming up to by 3.5 DEG C/min of programming rate, are incubated 60min；
D. 1060 DEG C are warming up to by 3.5 DEG C/min of programming rate, are incubated 300min；Then fast aeration cools down, and completes sintering；
(6) base substrate after vacuum-sintering is subjected to double tempering processing, being incubated 150min at 890 DEG C is carried out at first paragraph tempering
Reason, then second of temper is carried out by 450 DEG C of insulation 240min, room temperature is quickly cooled to, high magnetic characteristics rare earth neodymium is made
Iron B permanent magnetic material alloy A.
Comparative example
The obtained rare-earth Nd-Fe-B permanent magnetic material alloy B of the step of comparative example is according to embodiment 1, its difference with embodiment 1
Part is：The mixture temperature of step (2) and the passivation of step (3) are 25 DEG C, remaining technological parameter and 1 complete phase of embodiment
Together.
Respectively to rare earth made from high magnetic characteristics rare-earth Nd-Fe-B permanent magnetic material alloy A made from embodiment 1 and comparative example
Nd-Fe-B permanent magnet material alloy B takes Φ 10 × 10 (mm) standard specimen to obtain magnetic property and carries out contrast test.As a result it is as shown in table 1.
The test result of table 1.
| Project | Br/KGs | HcJ/KOe | (BH)m/MGsOe |
| Embodiment 1 (A) | 12.18 | 23.8 | 35.36 |
| Comparative example (B) | 12.19 | 22.7 | 35.27 |
As can be seen from Table 1, using high magnetic characteristics rare-earth Nd-Fe-B permanent magnetism material made from the embodiment 1 of lower temperature preparation technology
Expect alloy A magnetic performance relative to the magnetic of rare-earth Nd-Fe-B permanent magnetic material alloy B made from the comparative example under room temperature condition
Performance significantly improves.
Embodiment 2
It is (Nd, Pr) by composition30Dy0.8Co1Cu0.2Al0.1Nb0.2FeIt is remainingB0.96(wt%) Nd-Fe-B permanent magnet material alloy, by upper
Composition is stated to carry out dispensing and Nd-Fe-B permanent magnet material alloy is made with rapid hardening thin slice technique；
(1) above-mentioned rare-earth Nd-Fe-B permanent magnetic material alloy is crushed using hydrogen is broken with the crushing process that airflow milling is combined,
Obtain the powder that particle diameter is 100 μm；
(2) above-mentioned powder is subjected to low temperature batch mixing at -10 DEG C, mixing time is controlled in 100min, obtains mixed powder；
(3) mixed powder is subjected to low-temperature passivation at -10 DEG C, passivation time is controlled in 12h；
(4) powder after step (3) is passivated is injected in mould under nitrogen protection, sets magnetic field intensity as 2T, pressure is
15MPa carries out oriented moulding and obtains 50 × 39 × 32 (mm) green compact, and green compact obtain base substrate through 21Mpa isostatic pressings；
(5) base substrate is put into vacuum sintering furnace, by vacuum sintering furnace forvacuum 100min, set in stove vacuum as
1×E-1Pa, temperature-gradient method：
A. 450 DEG C are warming up to by 10/ DEG C of programming rate, are incubated 40min；
B. 900 DEG C are warming up to by 3 DEG C/min of programming rate, are incubated 180min；
C. 1040 DEG C are warming up to by 3.5 DEG C/min of programming rate, are incubated 60min；
D. 1080 DEG C are warming up to by 3.5 DEG C/min of programming rate, are incubated 300min；Then fast aeration cools down, and completes sintering；
(6) base substrate after vacuum-sintering is subjected to double tempering processing, being incubated 120min at 900 DEG C is carried out at first paragraph tempering
Reason, then second of temper is carried out by 560 DEG C of insulation 180min, room temperature is quickly cooled to, high magnetic characteristics rare earth neodymium is made
Iron B permanent magnetic material alloy C.
Comparative example
The obtained rare-earth Nd-Fe-B permanent magnetic material alloy D of the step of comparative example is according to embodiment 2, its difference with embodiment 2
Part is：The mixture temperature of step (2) and the passivation of step (3) are 25 DEG C, remaining technological parameter and 2 complete phase of embodiment
Together.
Respectively to rare earth made from high magnetic characteristics rare-earth Nd-Fe-B permanent magnetic material alloy C made from embodiment 2 and comparative example
Nd-Fe-B permanent magnet material alloy D takes Φ 10 × 10 (mm) standard specimen to obtain magnetic property and carries out contrast test.As a result it is as shown in table 2.
The test result of table 2.
| Project | Br/KGs | HcJ/KOe | (BH)m/MGsOe |
| Embodiment 2 (C) | 13.85 | 18.16 | 47.51 |
| Comparative example (D) | 13.88 | 17.31 | 47.69 |
As can be seen from Table 2, using high magnetic characteristics rare-earth Nd-Fe-B permanent magnetism material made from the embodiment 2 of lower temperature preparation technology
Expect alloy C magnetic performance relative to the magnetic of rare-earth Nd-Fe-B permanent magnetic material alloy D made from the comparative example under room temperature condition
Performance significantly improves.
Embodiment 3
It is (Nd, Pr) by composition26.5Dy4.5Co1.5Cu0.2Al0.6Nb0.3FeIt is remainingB0.96(wt%) Nd-Fe-B permanent magnet material alloy,
Dispensing is carried out by mentioned component and Nd-Fe-B permanent magnet material alloy is made with rapid hardening thin slice technique；
(1) above-mentioned rare-earth Nd-Fe-B permanent magnetic material alloy is crushed using hydrogen is broken with the crushing process that airflow milling is combined,
Obtain the powder that particle diameter is 50 μm；
(2) on the basis of powder gross mass, 2.5 ‰ antioxidant is added in the powder, low temperature is carried out at 0 DEG C and is mixed
Material, mixing time are controlled in 80min, obtain mixed powder；
(3) mixed powder is subjected to low-temperature passivation at 0 DEG C, passivation time is controlled in 10h；
(4) powder after step (3) is passivated is injected in mould under nitrogen protection, sets magnetic field intensity as 1.8T, pressure is
10MPa carries out oriented moulding and obtains 50 × 39 × 32 (mm) green compact, and green compact obtain base substrate through 20Mpa isostatic pressings；
(5) base substrate is put into vacuum sintering furnace, by vacuum sintering furnace forvacuum 80min, sets in stove vacuum as 1
×E-2Pa, temperature-gradient method：
A. 425 DEG C are warming up to by 10/ DEG C of programming rate, are incubated 60min；
B. 870 DEG C are warming up to by 3 DEG C/min of programming rate, are incubated 200min；
C. 1020 DEG C are warming up to by 3.5 DEG C/min of programming rate, are incubated 50min；
D. 1070 DEG C are warming up to by 3.5 DEG C/min of programming rate, are incubated 280min；Then fast aeration cools down, and completes sintering；
(6) base substrate after vacuum-sintering is subjected to double tempering processing, being incubated 140min at 895 DEG C is carried out at first paragraph tempering
Reason, then second of temper is carried out by 500 DEG C of insulation 200min, room temperature is quickly cooled to, high magnetic characteristics rare earth neodymium is made
Iron B permanent magnetic material alloy E.
Comparative example
The obtained rare-earth Nd-Fe-B permanent magnetic material alloy F of the step of comparative example is according to embodiment 3, its difference with embodiment 2
Part is：The mixture temperature of step (2) and the passivation of step (3) are 25 DEG C, remaining technological parameter and 2 complete phase of embodiment
Together.
Respectively to rare earth made from high magnetic characteristics rare-earth Nd-Fe-B permanent magnetic material alloy E made from embodiment 3 and comparative example
Nd-Fe-B permanent magnet material alloy F takes Φ 10 × 10 (mm) standard specimen to obtain magnetic property and carries out contrast test.As a result it is as shown in table 3.
The test result of table 3.
| Project | Br/KGs | HcJ/KOe | (BH)m/MGsOe |
| Embodiment 3 (E) | 12.57 | 26.89 | 38.36 |
| Comparative example (F) | 12.59 | 25.73 | 38.42 |
As can be seen from Table 3, using high magnetic characteristics rare-earth Nd-Fe-B permanent magnetism material made from the embodiment 1 of lower temperature preparation technology
Expect alloy E magnetic performance relative to the magnetic of rare-earth Nd-Fe-B permanent magnetic material alloy F made from the comparative example under room temperature condition
Performance significantly improves.
Present invention process is simple, low energy consumption, and production is safer, while properties of product uniformity is good, reduces heavy rare earth
Dosage, reduce material cost.The magnetic property of rare-earth Nd-Fe-B can be effectively improved using this method.
Presently preferred embodiments of the present invention is the foregoing is only, any formal limitation not is made to the present invention, not surpassed
There are other variants and remodeling on the premise of going out the technical scheme described in claim.
Claims (9)
- A kind of 1. method for improving rare-earth Nd-Fe-B magnetic property, it is characterised in that comprise the following steps：(1) rare-earth Nd-Fe-B permanent magnetic material alloy is crushed, obtains the powder that particle diameter is 2~100 μm；(2) on the basis of powder gross mass, 0~5 ‰ antioxidant is added in the powder, is carried out at -10~10 DEG C Low temperature batch mixing, obtains mixed powder；(3) mixed powder is subjected to low-temperature passivation at -10~10 DEG C；(4) powder after step (3) is passivated is injected in mould under nitrogen protection, is carried out oriented moulding and is obtained green compact, described Green compact obtain base substrate through isostatic pressing；(5) base substrate is put into vacuum sintering furnace, temperature-gradient method, then fast aeration cools down, and completes sintering；(6) base substrate after vacuum-sintering is subjected to temper, is quickly cooled to room temperature, high magnetic characteristics rare-earth Nd-Fe-B is made forever Magnetic material alloys.
- A kind of 2. method for improving rare-earth Nd-Fe-B magnetic property according to claim 1, it is characterised in that in step (1), Rare-earth Nd-Fe-B permanent magnetic material alloy is crushed with the crushing process that airflow milling is combined using hydrogen is broken.
- A kind of 3. method for improving rare-earth Nd-Fe-B magnetic property according to claim 1, it is characterised in that in step (2), Mixing time is controlled in 60~100min.
- A kind of 4. method for improving rare-earth Nd-Fe-B magnetic property according to claim 1, it is characterised in that in step (3), Passivation time is controlled in 8~12h.
- A kind of 5. method for improving rare-earth Nd-Fe-B magnetic property according to claim 1, it is characterised in that in step (4), The magnetic field intensity of oriented moulding is 1.2~2T, and pressure is 5~15MPa.
- A kind of 6. method for improving rare-earth Nd-Fe-B magnetic property according to claim 1 or 5, it is characterised in that step (4) In, the Stress control of isostatic pressing is in 18~21Mpa.
- A kind of 7. method for improving rare-earth Nd-Fe-B magnetic property according to claim 1, it is characterised in that in step (5), Before vacuum-sintering, by vacuum sintering furnace 60~100min of forvacuum, vacuum is set in stove as 1 × E-2~1 × E-1Pa。
- A kind of 8. method of raising rare-earth Nd-Fe-B magnetic property according to claim 1 or 7, it is characterised in that step (5) In, the temperature-gradient method is：A. 400~450 DEG C are warming up to by 10/ DEG C of programming rate, are incubated 40~80min；B. 850~900 DEG C are warming up to by 3 DEG C/min of programming rate, are incubated 180~240min；C. 1000~1040 DEG C are warming up to by 3.5 DEG C/min of programming rate, are incubated 30~60min；D. 1060~1080 DEG C are warming up to by 3.5 DEG C/min of programming rate, are incubated 240~300min.
- A kind of 9. method for improving rare-earth Nd-Fe-B magnetic property according to claim 1, it is characterised in that in step (6), The temper is double tempering, and being incubated 120~150min at 890~900 DEG C carries out first paragraph temper, then passes through 450~560 DEG C of 180~240min of insulation carry out second of temper.
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Denomination of invention: A method for improving the magnetic properties of rare earth Nd-Fe-B Effective date of registration: 20211227 Granted publication date: 20200811 Pledgee: Dongyang Branch of China Construction Bank Co.,Ltd. Pledgor: ZHEJIANG DONGYANG DMEGC RARE EARTH MAGNET Co.,Ltd. Registration number: Y2021330002688 |
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Date of cancellation: 20230628 Granted publication date: 20200811 Pledgee: Dongyang Branch of China Construction Bank Co.,Ltd. Pledgor: ZHEJIANG DONGYANG DMEGC RARE EARTH MAGNET Co.,Ltd. Registration number: Y2021330002688 |