CN109192489A - A kind of preparation method of high-performance heavy rare earth neodymium iron boron magnetic body - Google Patents
A kind of preparation method of high-performance heavy rare earth neodymium iron boron magnetic body Download PDFInfo
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- CN109192489A CN109192489A CN201811021452.2A CN201811021452A CN109192489A CN 109192489 A CN109192489 A CN 109192489A CN 201811021452 A CN201811021452 A CN 201811021452A CN 109192489 A CN109192489 A CN 109192489A
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- iron boron
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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
- 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
Abstract
The present invention relates to technical field of magnetic materials, more particularly to a kind of preparation method of high-performance heavy rare earth neodymium iron boron magnetic body, the following steps are included: (1), which places RTM alloy powder and neodymium iron boron blank in vacuum rotating furnace, carries out pre- infiltration processing, the neodymium iron boron semi-finished product that surface adhesion has RTM alloyed powder last layer are obtained；(2) neodymium iron boron semi-finished product are subjected to High temperature diffusion and heat treatment to get high-performance heavy rare earth neodymium iron boron magnetic body.By realizing significantly improving for neodymium iron boron magnetic body intrinsic coercivity in neodymium iron boron magnetic body grain boundary decision heavy rare earth, heavy rare earth element quantity consumed significantly reduces the present invention, while substantially reducing the reduction amplitude of the original remanent magnetism of neodymium iron boron magnetic body and maximum magnetic energy product.
Description
Technical field
The present invention relates to technical field of magnetic materials more particularly to a kind of preparation sides of high-performance heavy rare earth neodymium iron boron magnetic body
Method.
Background technique
Sintered NdFeB magnet is a kind of important basic functional material, and application field is quite extensive.With wind-force
The high-technology fields such as generating equipment, electric car, hybrid vehicle, frequency conversion electrical installation, industrial energy saving motor it is quick
Development, for high magnetic characteristics, operation at high temperature, high operational stability Sintered NdFeB magnet demand it is growing.
It is the primary condition that Sintered NdFeB magnet has operation at high temperature, high operational stability with high intrinsic coercivity.
It is to significantly improve intrinsic coercivity in magnetic body currently, adding the heavy rare earth elements such as Dy, Tb by preparing link in alloy
Technical way.But to will cause magnet remanence fall big for the technological means, while the heavy rare earth elements such as Dy, Tb
Quantity consumed is big, and cost of goods manufactured rises.
Using pairing gold process, oxide, the fluorine of a certain number of Dy, Tb heavy rare earth elements is added in powder preparation link
Compound, hydride powder or its alloy powder, also can effectively improve the intrinsic coercivity of magnet, if but technical process control
System is not suitable for, and the heavy rare earth elements such as Dy, Tb are difficult to realize grain boundary Assembled distribution, result in magnet remanence to a certain extent
Be decreased obviously, and increase the consumption of heavy rare earth element.
Summary of the invention
The present invention provides a kind of high-performance heavy rare earth neodymium-iron-boron to overcome above-mentioned problems of the prior art
The preparation method of body, by realizing significantly mentioning for neodymium iron boron magnetic body intrinsic coercivity in neodymium iron boron magnetic body grain boundary decision heavy rare earth
Height as long as reaching heavy rare earth traditional handicraft 1/4 in the case where traditional handicraft equal performance, while substantially reducing neodymium iron boron magnetic body
The reduction amplitude of original remanent magnetism and maximum magnetic energy product, comprehensive performance are higher than what traditional handicraft can be done.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of preparation method of high-performance heavy rare earth neodymium iron boron magnetic body, comprising the following steps:
(1) RTM alloy powder and neodymium iron boron blank are placed in vacuum rotating furnace and carries out pre- infiltration processing, obtaining surface adhesion has
The neodymium iron boron semi-finished product of RTM alloyed powder last layer；
(2) neodymium iron boron semi-finished product are subjected to High temperature diffusion and heat treatment to get high-performance heavy rare earth neodymium iron boron magnetic body.
Present invention application grain boundary decision heavy rare earth technique expands the heavy rare earth elements such as Dy, Tb by crystal boundary by magnet surface
It dissipates and enters inside magnet, and be present in grain boundary area, realize the magnetic hardening of main phase grain surface region.Using this technique
The high-performance rare-earth neodymium iron boron magnetic body of preparation has significant intrinsic coercivity, not only the lower range of decrease of its remanent magnetism and maximum magnetic energy product
Degree is reduced, as long as reaching heavy rare earth traditional handicraft 1/4 in the case where traditional handicraft equal performance.
Preferably, R is selected from one of heavy rare earth element or a variety of in the RTM alloy powder in step (1)；Institute
Stating T is Fe and/or Co；The M is selected from one of Al, Si, Cu, Nb, Zr and Ga or a variety of.
Preferably, in step (1), on the basis of RTM alloy powder gross mass, the accounting of R in the RTM alloy powder
For 60~100wt%, the accounting of T is 0~35wt%, and the accounting of M is 0~5wt%.
Preferably, in step (1), on the basis of RTM alloy powder gross mass, the accounting of R in the RTM alloy powder
For 60~99.8wt%, the accounting of T is 0.1~35wt%, and the accounting of M is 0.1~5wt%.
Wherein, R is used to improve the intrinsic coercivity of magnet after infiltration as heavy rare earth element, and T and M are mainly refining alloy
Crystal grain improves alloy permeability.If pressing traditional handicraft, the additional amount of heavy rare earth needs 5~6%, and heavy rare earth adds in the present invention
Dosage reduces by 400%, but performance is but significantly increased.
Preferably, on the basis of neodymium iron boron blank gross mass, the RTM alloy-layer is in neodymium iron boron blank in step (1)
The adhesive capacity on surface is 0.5~3wt%.
Preferably, pre- temperature of permeating is 650~750 DEG C, and pre- time of penetration is 3~8h in step (1).
Preferably, High temperature diffusion temperature is 800~1000 DEG C in step (2), the High temperature diffusion time is 10~20h.
Preferably, in step (2), the heat treatment is that lonneal is handled, the temperature of the lonneal is 450~
600 DEG C, the time is 2~8h.
Preferably, the average particle size of the RTM alloy powder is 1~30 μm in step (1).
Preferably, the RTM alloy powder is made using neodymium iron boron powder metallurgical technique in step (1)；The neodymium iron
Boron powder metallurgical technology is to first pass through strip casting RTM alloy is made, and is then broken RTM alloy by hydrogen, jet milling process system
Obtain RTM alloy powder.
A kind of high-performance heavy rare earth neodymium iron boron magnetic body as made from the above method.
Therefore, the invention has the following beneficial effects: by realizing neodymium iron boron in neodymium iron boron magnetic body grain boundary decision heavy rare earth
Intrinsic coercivity in magnetic body significantly improves, and heavy rare earth element quantity consumed significantly reduces, and reaches the feelings of traditional handicraft equal performance
If heavy rare earth traditional handicraft 1/4 under condition, while substantially reducing the drop of neodymium iron boron magnetic body original remanent magnetism and maximum magnetic energy product
Low amplitude.
Specific embodiment
Below by specific embodiment, the technical solutions of the present invention will be further described.
In the present invention, if not refering in particular to, all devices and raw material is commercially available or the industry is common are following
Method in embodiment is unless otherwise instructed conventional method in that art.
Embodiment 1
(1) it is prepared by formula as below and RTM alloy is made through strip casting, then broken, jet milling process prepares average grain by hydrogen
The RTM alloy powder that about 2.0 μm of degree；R is selected from Tb, and T is selected from Fe, and M is selected from Al；The mass percent of Tb, Fe, Al point in powder
It Wei 80%, 15% and 5%；
(2) powder smelting, processed, molding, sintering step prepare N50H magnet blank, and being processed as 50 × 30 × 2mm, (2mm is
Differently- oriented directivity) size；
(3) RTM alloy powder is placed in vacuum rotating furnace together with 50 × 30 × 2mm N50H magnet blank and is evacuated to 10-2Pa is carried out after permeating 4h in advance hereinafter, being heated to 700 DEG C, and the RTM alloyed powder last layer that surface adhesion weight is about 1% obtains N50H
Magnet semi-finished product separate it with remaining RTM alloy powder；
(4) the N50H magnet semi-finished product after pre- infiltration are put into sintering furnace, are evacuated to 10-2Pa is hereinafter, be heated to 900 DEG C
Carry out High temperature diffusion handle 16h, then 500 DEG C at a temperature of, carry out lonneal two stage treatment 4h after, after being spread
High-performance heavy rare earth N50H neodymium iron boron magnetic body.
To the above method preparation high-performance heavy rare earth N50H neodymium iron boron magnetic body and N50H magnet blank magnetic performance into
Row test, the results are shown in Table 1:
The magnetic performance result of the N50H neodymium iron boron magnetic body of 1. crystal phase of table diffusion front and back
| Sample | Br/KGs | HcJ/KOe | (BH)m/MGsOe |
| N50H magnet blank | 14.21 | 16.85 | 49.52 |
| High-performance heavy rare earth N50H neodymium iron boron magnetic body | 14.15 | 26.34 | 49.33 |
It can be obtained by table 1, high-performance heavy rare earth N50H neodymium iron boron magnetic body ratio manufactured in the present embodiment spreads N50H magnet without crystal phase
Blank improves 56% in magnet coercivity aspect of performance, and remanent magnetism and maximum magnetic energy product aspect of performance are held essentially constant, together
When current traditional handicraft be difficult to accomplish the performance of the trade mark.
Embodiment 2
(1) it is prepared by formula as below and RTM alloy is made through strip casting, then broken, jet milling process prepares average grain by hydrogen
The RTM alloy powder that about 2.5 μm of degree；R is selected from Dy, and T is selected from Co, and M is selected from Cu；The mass percent of Dy, Co, Cu point in powder
It Wei 75%, 20% and 5%；
(2) N40SH magnet blank is made in powder smelting, processed, molding, sintering step, and is processed as 60 × 20 × 3mm (3mm is to take
To direction) size；
(3) RTM alloy powder is placed in vacuum rotating furnace together with 60 × 20 × 3mm N40SH magnet blank and is evacuated to
10-2Pa is carried out after permeating 3.5h in advance hereinafter, being heated to 680 DEG C, and making its surface adhesion weight is about 1.5%RTM alloyed powder last layer,
N40SH magnet semi-finished product are obtained, it is separated with remaining RTM alloy powder；
(4) the N40SH magnet semi-finished product after pre- infiltration are put into sintering furnace, are evacuated to 10-2Pa is hereinafter, be heated to 890 DEG C
Carry out High temperature diffusion handle 15h, then 500 DEG C at a temperature of, carry out lonneal two stage treatment 5h after, after being spread
High-performance heavy rare earth N40SH neodymium iron boron magnetic body.
The magnetic performance of high-performance heavy rare earth N40SH neodymium iron boron magnetic body and N40SH magnet blank to above method preparation
It is tested, the results are shown in Table 2:
The magnetic performance result of the N40SH neodymium iron boron magnetic body of 2 crystal phase of table diffusion front and back
| Sample | Br/KGs | HcJ/KOe | (BH)m/MGsOe |
| N40SH magnet blank | 12.85 | 20.86 | 39.66 |
| High-performance heavy rare earth N40SH neodymium iron boron magnetic body | 12.79 | 26.42 | 39.51 |
It can be obtained by table 2, high-performance heavy rare earth N40SH neodymium iron boron magnetic body ratio manufactured in the present embodiment spreads N40SH magnetic without crystal phase
Chaeta base improves 26% in magnet coercivity aspect of performance, and remanent magnetism and maximum magnetic energy product aspect of performance are held essentially constant,
If pressing traditional handicraft, the additional amount of heavy rare earth needs 5~6%, the additive amount reduction by 400% of heavy rare earth in the present invention, but property
It can be but significantly increased.
Embodiment 3
(1) it is prepared by formula as below and RTM alloy is made through strip casting, then broken, jet milling process prepares average grain by hydrogen
The RTM alloy powder that about 2.8 μm of degree；R is selected from Nd, and T is selected from Co, and M is selected from Al；The mass percent of Nd, Co, Al point in powder
It Wei 70%, 20% and 10%；
(2) N52 magnet blank is made in powder smelting, processed, molding, sintering step, and is processed as 55 × 25 × 2.5mm (2.5mm is
Differently- oriented directivity) size；
(3) RTM alloy powder is placed in vacuum rotating furnace together with 55 × 25 × 2.5mm N52 magnet blank and is evacuated to
10-2Pa is carried out after permeating 4.5h in advance hereinafter, being heated to 720 DEG C, and making its surface adhesion weight is about 1.8%RTM alloyed powder last layer,
N52 magnet semi-finished product are obtained, it is separated with remaining RTM alloy powder；
(4) the N52 magnet semi-finished product permeated in advance are put into sintering furnace, are evacuated to 10-2Pa is hereinafter, be heated to 890 DEG C of progress
Infiltration processing 18h, then 510 DEG C at a temperature of, carry out lonneal two stage treatment 4h after, the high-performance weight after being spread
Rare earth N52 neodymium iron boron magnetic body.
The magnetic performance of high-performance heavy rare earth N52 neodymium iron boron magnetic body and N52 magnet blank to above method preparation carries out
Test, the results are shown in Table 3:
The magnetic performance result of the N52 neodymium iron boron magnetic body of 3. crystal phase of table diffusion front and back
| Sample | Br/KGs | HcJ/KOe | (BH)m/MGsOe |
| N52 magnet blank | 14.63 | 12.28 | 50.3 |
| High-performance heavy rare earth N52 neodymium iron boron magnetic body | 14.57 | 17.51 | 50.68 |
It can be obtained by table 3, high-performance heavy rare earth N52 neodymium iron boron magnetic body ratio manufactured in the present embodiment spreads N52 magnet hair without crystal phase
Base improves 42% in magnet coercivity aspect of performance, and remanent magnetism and maximum magnetic energy product aspect of performance are held essentially constant, simultaneously
Traditional handicraft is difficult to accomplish the performance.
Embodiment 4
(1) it is prepared by formula as below and RTM alloy is made through strip casting, then broken, jet milling process prepares average grain by hydrogen
The RTM alloy powder that about 1.5 μm of degree；R is selected from Dy and Tb,；The mass percent of Dy and Tb is respectively 75% He in powder
25%；
(2) N48H magnet blank is made in powder smelting, processed, molding, sintering step, and is processed as 50 × 10 × 4mm (4mm is to take
To direction) size；
(3) RTM alloy powder is placed in vacuum rotating furnace together with 50 × 10 × 4mm N48H magnet blank and is evacuated to 10-2Pa is carried out after permeating 8h in advance hereinafter, being heated to 650 DEG C, and making its surface adhesion weight is about 0.8%RTM alloyed powder last layer, is obtained
N48H magnet semi-finished product separate it with remaining RTM alloy powder；
(4) the N48H magnet semi-finished product after pre- infiltration are put into sintering furnace, are evacuated to 10-2Pa is hereinafter, be heated to 900 DEG C
Carry out High temperature diffusion handle 10h, then 450 DEG C at a temperature of, carry out lonneal two stage treatment 8h after, after being spread
High-performance heavy rare earth N48H neodymium iron boron magnetic body.
To the above method preparation high-performance heavy rare earth N48H neodymium iron boron magnetic body and N48H magnet blank magnetic performance into
Row test, the results are shown in Table 4:
The magnetic performance result of the N48H neodymium iron boron magnetic body of 4. crystal phase of table diffusion front and back
| Sample | Br/KGs | HcJ/KOe | (BH)m/MGsOe |
| N48H magnet blank | 13.77 | 17.31 | 46.3 |
| High-performance heavy rare earth N48H neodymium iron boron magnetic body | 13.71 | 24.85 | 45.93 |
It can be obtained by table 4, high-performance heavy rare earth N48H neodymium iron boron magnetic body ratio manufactured in the present embodiment spreads N48H magnet without crystal phase
Blank improves 43% in magnet coercivity aspect of performance, and remanent magnetism and maximum magnetic energy product aspect of performance are held essentially constant.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the present invention in any form, and is not surpassing
There are also other variations and modifications under the premise of technical solution documented by claim out.
Claims (10)
1. a kind of preparation method of high-performance heavy rare earth neodymium iron boron magnetic body, which comprises the following steps:
(1) RTM alloy powder and neodymium iron boron blank are placed in vacuum rotating furnace and carries out pre- infiltration processing, obtaining surface adhesion has
The neodymium iron boron semi-finished product of RTM alloyed powder last layer；
(2) neodymium iron boron semi-finished product are subjected to High temperature diffusion and heat treatment to get high-performance heavy rare earth neodymium iron boron magnetic body.
2. a kind of preparation method of high-performance heavy rare earth neodymium iron boron magnetic body according to claim 1, which is characterized in that step
(1) in, R is selected from one of heavy rare earth element or a variety of in the RTM alloy powder；The T is Fe and/or Co；The M choosing
From one of Al, Si, Cu, Nb, Zr and Ga or a variety of.
3. a kind of preparation method of high-performance heavy rare earth neodymium iron boron magnetic body according to claim 1, which is characterized in that step
(1) in, on the basis of RTM alloy powder gross mass, the accounting of R is 60~100wt%, the accounting of T in the RTM alloy powder
For 0~35wt%, the accounting of M is 0~5wt%.
4. a kind of preparation method of high-performance heavy rare earth neodymium iron boron magnetic body according to claim 1, which is characterized in that step
(1) in, on the basis of neodymium iron boron blank gross mass, the RTM alloy-layer neodymium iron boron blank surface adhesive capacity be 0.5~
3wt%.
5. a kind of preparation method of high-performance heavy rare earth neodymium iron boron magnetic body according to claim 1, which is characterized in that step
(1) in, pre- temperature of permeating is 650~750 DEG C, and pre- time of penetration is 3~8h.
6. a kind of preparation method of high-performance heavy rare earth neodymium iron boron magnetic body according to claim 1, which is characterized in that step
(2) in, High temperature diffusion temperature is 800~1000 DEG C, and the High temperature diffusion time is 10~20h.
7. a kind of preparation method of high-performance heavy rare earth neodymium iron boron magnetic body according to claim 1, which is characterized in that step
(2) in, the heat treatment is that lonneal is handled, and the temperature of the lonneal is 450~600 DEG C, and the time is 2~8h.
8. a kind of preparation side of high-performance heavy rare earth neodymium iron boron magnetic body described according to claim 1 or 2 or 3 or 4 or 5 or 6 or 7
Method, which is characterized in that in step (1), the average particle size of the RTM alloy powder is 1~30 μm.
9. a kind of preparation method of high-performance heavy rare earth neodymium iron boron magnetic body according to claim 8, which is characterized in that step
(1) in, the RTM alloy powder is made using neodymium iron boron powder metallurgical technique；The neodymium iron boron powder metallurgical technique is first to lead to
It crosses strip casting and RTM alloy is made, then RTM alloy powder is made in broken, jet milling process by hydrogen by RTM alloy.
10. high-performance heavy rare earth neodymium iron boron magnetic body made from a kind of method as claimed in claim 9.
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| CN110164644A (en) * | 2019-06-04 | 2019-08-23 | 浙江英洛华磁业有限公司 | A kind of preparation method of high-performance neodymium-iron-boron magnet |
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| CN111383833A (en) * | 2019-11-11 | 2020-07-07 | 浙江东阳东磁稀土有限公司 | Grain boundary diffusion method for rare earth neodymium iron boron magnet |
| CN112017835A (en) * | 2020-08-20 | 2020-12-01 | 合肥工业大学 | Low-heavy rare earth high-coercivity sintered neodymium-iron-boron magnet and preparation method thereof |
| CN114999805A (en) * | 2022-06-13 | 2022-09-02 | 安徽吉华新材料有限公司 | Preparation method of high-performance regenerative permanent magnet material |
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| CN114999805A (en) * | 2022-06-13 | 2022-09-02 | 安徽吉华新材料有限公司 | Preparation method of high-performance regenerative permanent magnet material |
| CN114999805B (en) * | 2022-06-13 | 2023-12-26 | 安徽吉华新材料有限公司 | Preparation method of high-performance regenerated permanent magnet material |
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Application publication date: 20190111 |