CN109192493A - A kind of preparation method of high performance sintered neodymium-iron-boron permanent-magnet material - Google Patents
A kind of preparation method of high performance sintered neodymium-iron-boron permanent-magnet material Download PDFInfo
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- CN109192493A CN109192493A CN201811100185.8A CN201811100185A CN109192493A CN 109192493 A CN109192493 A CN 109192493A CN 201811100185 A CN201811100185 A CN 201811100185A CN 109192493 A CN109192493 A CN 109192493A
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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
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- Hard Magnetic Materials (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
Abstract
A kind of preparation method of high performance sintered neodymium-iron-boron permanent-magnet material, belongs to field of rare-earth permanent magnetic.Quaternary and the above rare earth alloy film of quaternary are deposited on pretreatment neodymium iron boron magnetic body surface by magnetron sputtering method, as diffusion source, by homogenization, grain boundary decision and low-temperature tempering heat treatment, improve the border structure of magnet, to increase substantially the coercivity of magnet, while guaranteeing that remanent magnetism is basically unchanged.The quaternary and the above rare earth alloy thin film composition of quaternary are LRE100‑x‑y‑zHRExMyAlz(1≤x≤40,1≤y≤20,1≤z≤20), wherein LRE is one of light rare earth elements such as Y, La, Ce, Pr, Nd or more, HRE is one of heavy rare earth elements such as Tb, Dy, Ho or more, one of alloying elements such as M Cu, Fe, Co, Ga, Zr, Zn, Mn, Mg or more.It is prepared by the present invention uniformly, the rare earth alloy film that fine and close, binding force is strong as diffusion source, quantity is continuously controllable, and the magnetic property consistency of magnet is preferable after DIFFUSION TREATMENT；Rare-earth usage can be reduced, industrialized production is suitable for.
Description
Technical field
The invention belongs to field of rare-earth permanent magnetic, in particular to a kind of preparation of high performance sintered neodymium-iron-boron permanent-magnet material
Method.
Background technique
Sintered NdFeB (Nd-Fe-B) permanent magnet is excellent because of its remanent magnetism, coercivity and maximum magnetic energy product with higher etc.
Magnetic property and have the title of " magnetic king ".It is right with generation information technology, the continuous development of high-end equipment, new energy technology
The requirement of Nd-Fe-B permanent magnet is higher and higher.
Dy, Tb heavy rare earth element are added by DIRECT ALLOYING method, it is different high magnetocrystalline can be formed in neodymium-iron-boron body
(Nd, the Dy/Tb) of property field2Fe14B hardens magnetic phase, so that the coercivity and temperature stability of magnet are directly effectively promoted, but by
In (Nd, Dy/Tb)2Fe14Dy, Tb atom are coupled with Fe atom anti-ferromagnetism in B phase, will cause the fast of magnet remanence and magnetic energy product
Speed reduces.Furthermore Dy, Tb element abundance in rare earth resources are low and expensive, DIRECT ALLOYING will lead to neodymium iron boron magnetic body at
This is significantly increased.From the angle of Elemental redistribution and regulating microstructure, developing heavy rare earth Reduction Technology becomes sintering
The important directions of Nd-Fe-B permanent magnet material research and development.And in terms of heavy rare earth element is distributed regulation, improved by grain boundary decision technology
The heterogeneous microstructure and component distributing of Nd-Fe-B magnet can improve the comprehensive performance of magnet well, while can be effectively
Control manufacturing cost.
Using grain boundary decision treatment process, enter Dy, Tb element inside magnet by grain boundary decision by magnet surface,
And it is present in grain boundary area, realize the magnetic hardening of main phase grain surface region.The high intrinsic coercivity sintering so prepared
Neodymium iron boron magnetic body, not only its remanent magnetism fall is small, but also significantly reduces Dy, Tb element consumption.
Source attachment technique is commonly spread in grain boundary decision technology to be had very much, such as magnetron sputtering, thermal spraying, dual alloy powder
Method, hot-dip, thermal deformation etc..Compared to other preparation methods, the film diffusion source of magnetron sputtering method preparation, with basal body binding force
By force, film layer dense uniform.It is more conducive to the diffusion in diffusion source.Moreover, magnetron sputtering is heavy compared to hot-dip and hot spray process
Long-pending constant rate, thicknesses of layers can be controlled accurately, and the quantitative addition of rare earth element may be implemented, improve the utilization of rare earth
Rate.
Summary of the invention
The main object of the present invention is to form even compact, the adjustable complex alloy thin film of thickness in magnet surface, to magnetic
Body border structure carries out multiple improvement, solves the problems, such as low-melting alloy grain boundary decision technical industryization using upper diffusion source.
A kind of preparation method of high performance sintered neodymium-iron-boron permanent-magnet material, it is characterised in that located in advance by magnetron sputtering method
Neodymium iron boron magnetic body surface deposition quaternary and the above rare earth alloy film of quaternary are managed, as diffusion source, is expanded by homogenization, crystal boundary
Scattered and low-temperature tempering heat treatment, improves the border structure of magnet, to increase substantially the coercivity of magnet, while guaranteeing remanent magnetism
It is basically unchanged；The quaternary and the above rare earth alloy thin film composition of quaternary are LRE100-x-y-zHRExMyAlz(1≤x≤40,1≤y
≤ 20,1≤z≤20) (atomic fraction), wherein LRE is one of light rare earth elements such as Y, La, Ce, Pr, Nd or more, HRE
For one of heavy rare earth elements such as Tb, Dy, Ho or more, in the alloying elements such as M Cu, Fe, Co, Ga, Zr, Zn, Mn, Mg
It is a kind of or more.
Further, specific process step of the present invention are as follows:
1) surface preparation is carried out to neodymium iron boron magnetic body；
2) in magnetron sputtering apparatus, magnet and target are further activated；
3) surface magnetic control sputtering is carried out to magnet after processing described in step 2), deposits quaternary and the above rare earth alloy of quaternary is thin
Film；
4) Homogenization Treatments carried out to rare earth alloy film described in step 3), then carry out grain boundary decision and lonneal
Heat treatment.
Further, magnet surface roughness Ra≤0.1 μm is pre-processed in step 1), clean surface, without greasy dirt.
Further, it is activated in step 2), is evacuated to 1 × 10 first-3~2 × 10-4Pa is then passed to high-purity
Argon gas adjusts working vacuum to 1.5 × 10-2~1.0Pa range, target power output 100W, bias 100V, 5~10min of working time are right
Magnet is activated；Then, it is then turned on DC power supply, bombards target material surface 15min, the oxide skin(coating) of removal target surface covering
And pollutant, Hong target process block substrate using baffle.
Further, use high-purity argon gas as working gas in step 3), air pressure is 0.1~10Pa, throughput 20
~50sccm, sputtering power are 80~200W, and sputtering time is 0.5~5h.
Further, Homogenization Treatments described in step 4) are: being first evacuated to 2 × 10-3Pa then passes to high-purity argon gas
Protection；Homogenization Treatments carry out in 0.8-0.9 times of melting range of alloy, keep the temperature 2-10h；Grain boundary decision is in 650~950 DEG C of models
Interior progress is enclosed, 0.5~10h is kept the temperature；Lonneal carries out in 400~600 DEG C, keeps the temperature 0.5~4h.
Further, the fusing point of the rare earth alloy film is within the scope of 450-600 DEG C.
Further, deposition of rare-earth alloy firm thickness control is in 0.1-10 μ m.
The homogenization heat treatment, it is therefore an objective to make rare earth alloy thin film composition uniformity；
The grain boundary decision heat treatment, it is therefore an objective to rare earth alloy film be melted and penetrated into inside magnet；
The low-temperature tempering heat treatment, it is therefore an objective to which the magnet institutional framework after DIFFUSION TREATMENT is further adjusted.
The present invention utilizes magnetron sputtering technique deposition of rare-earth alloy firm on neodymium iron boron magnetic body, the binding force with matrix
By force, even compact promotes grain boundary decision process；Magnetron sputtering technique can accurately control the thickness of film, as diffusion source,
The quantity that diffusion source can accurately be controlled avoids excessive rare earth element from being enriched in magnet surface, and it is coercitive simultaneously to strengthen magnet
Utilization rate that is smaller, and improving rare earth element is damaged to remanent magnetism.Due to diffusion source be quaternary and the above rare earth alloy film of quaternary,
The compound addition of multiple element can significantly improve the wetability of Grain-Boundary Phase, reduce grain boundary defects, and the magnetic isolation for strengthening Grain-Boundary Phase is made
With to improve magnet coercivity.In particular, the result shows that, adding a small amount of alloy element Al can be significantly according to correlative study
Ground promotes the grain boundary decision process of heavy rare earth element, thin and continuous magnetic hardening layer is formed in Grain Surface, to significantly mention
The coercivity of high magnet and on remanent magnetism influence it is smaller.In addition, reducing magnetic due to the eutectic dot characteristics of designed rare earth alloy film
The time of sputter coating is controlled, temperature needed for reducing grain boundary decision reduces growing up for main phase grain.
Specific embodiment
1 4mm thickness N50 magnet surface of embodiment sputters Pr60Tb10Cu15A1l5(at.%) it is heat-treated after alloy firm.
Commercial magnet N50 is selected, magnet size isCylindrical body, target material composition Pr60Tb10Cu15A1l5
(at.%).Magnet is surface-treated, it is clean surface, oil-free by pretreated magnet surface roughness Ra≤0.1 μm
It is dirty；Magnetron sputtering apparatus cavity is evacuated to 1 × 10-3Pa is passed through high-purity argon gas, adjusts working vacuum to 6 × 10-2Pa, target
Power is 100W, bias 100V, working time 5min, is activated to magnet to be processed；Then, it is then turned on direct current
Source, bombards target material surface 15min, the oxide skin(coating) and pollutant of removal target surface covering, and Hong target process blocks substrate using baffle；
By direct current magnetron sputtering process in magnet surface deposition of rare-earth alloy firm, and by adjusting technological parameter for rare earth alloy film
Control is at 5 μm or so, splash-proofing sputtering process parameter are as follows: operating air pressure 0.5Pa, sputtering power 100W, voltage 300V, gas flow
40sccm, sputtering time 120min；By sputter coating treated magnet (sample #2) and without the sky of sputter process
White sample (sample #1) is placed in vacuum heat treatment furnace simultaneously, is first evacuated to 2 × 10-3Pa then passes to high-purity argon gas guarantor
Shield；420 DEG C of homogenization heat treatments are carried out again, keep the temperature 6h；950 DEG C of High temperature diffusions keep the temperature 4h；500 DEG C of temperings keep the temperature 2h；
#1 diffusion samples are made；#1 and #2 properties of sample is measured, and is summarized in table 1.
The magnetic property of table 1#1 and #2 magnet
| Number | Hci(kOe) | Br(T) | (BH)max(MGOe) |
| #1 blank magnet | 12.2 | 1.435 | 48.8 |
| #2 spreads magnet | 23.2 | 1.389 | 47.9 |
2 4mm thickness 52M magnet surface of embodiment sputters Pr60Tb10Fe15All5(at.%) it is heat-treated after alloy firm.
Commercial magnet 52M is selected, magnet size isCylindrical body, target material composition Pr60Tb10Fe15All5
(at.%).Magnet is surface-treated, it is clean surface, oil-free by pretreated magnet surface roughness Ra≤0.1 μm
It is dirty；Magnetron sputtering apparatus cavity is evacuated to 1 × 10-3Pa is passed through high-purity argon gas, adjusts working vacuum to 6 × 10-2Pa, it splashes
Penetrate power be 100W, bias 100V, working time 5min, magnet to be processed is activated；Then, it is then turned on direct current
Power supply, bombards target material surface 15min, the oxide skin(coating) and pollutant of removal target surface covering, and Hong target process blocks base using baffle
Piece；The alloy firm of target component is deposited in magnet surface by direct current magnetron sputtering process, and will be closed by adjusting technological parameter
Gold thin film control is at 10 μm or so, splash-proofing sputtering process parameter are as follows: operating air pressure 0.5Pa, target power output 100W, voltage 300V, gas
Flow 40sccm, sputtering time 150min；By sputter coating treated magnet (sample #4) and without sputter process
Blank sample (sample #3) simultaneously be placed in vacuum heat treatment furnace, be first evacuated to 2 × 10-3Pa then passes to high-purity argon
Gas shielded；460 DEG C of homogenization heat treatments are carried out again, keep the temperature 6h；950 DEG C of High temperature diffusions keep the temperature 4h；500 DEG C of temperings, heat preservation
2h；#4 diffusion samples are made；#3 and #4 properties of sample is measured, and is summarized in table 2.
The magnetic property of table 2#3 and #4 magnet
| Number | Hci(kOe) | Br(T) | (BH)max(MGOe) |
| #3 blank magnet | 14.6 | 1.435 | 50.2 |
| #4 spreads magnet | 23.2 | 1.390 | 48.9 |
3 4mm thickness 48SH magnet surface of embodiment sputters Pr50Tb20Cu10Fel5Al5(at.%) heat is carried out after alloy firm
Processing.
Commercial magnet 48SH is selected, magnet size isCylindrical body, target material composition Pr60Tb10Cu10Fel5Al5
(at.%).Magnet is surface-treated, it is clean surface, oil-free by pretreated magnet surface roughness Ra≤0.1 μm
It is dirty；Magnetron sputtering apparatus cavity is evacuated to 1 × 10-3Pa is passed through high-purity argon gas, adjusts working vacuum to 6 × 10-2Pa, target
Power is 100W, bias 100V, working time 5min, is activated to magnet to be processed；Then, it is then turned on direct current
Source, bombards target material surface 15min, the oxide skin(coating) and pollutant of removal target surface covering, and Hong target process blocks substrate using baffle；
The rare earth alloy film of target component is deposited in magnet surface by direct current magnetron sputtering process, and will be dilute by adjusting technological parameter
The control of native alloy firm is at 20 μm or so, splash-proofing sputtering process parameter are as follows: operating air pressure 0.5Pa, sputtering power 100W, voltage are
300V, gas flow 40sccm, sputtering time 180min；By sputter coating treated magnet (sample #6) and without
The blank sample (sample #5) of sputter process is placed in vacuum heat treatment furnace simultaneously, is first evacuated to 2 × 10-3Then Pa leads to
Enter high-purity argon gas protection；450 DEG C of homogenization heat treatments are carried out again, keep the temperature 6h；950 DEG C of High temperature diffusions keep the temperature 4h；500 DEG C of tempering
Processing keeps the temperature 2h；#6 diffusion samples are made；#5 and #6 properties of sample is measured, and is summarized in table 3.
The magnetic property of table 3#5 and #6 magnet
| Number | Hci(kOe) | Br(T) | (BH)max(MGOe) |
| #5 blank magnet | 21.2 | 1.396 | 48.6 |
| #6 spreads magnet | 30.8 | 1.378 | 48.9 |
Claims (8)
1. a kind of preparation method of high performance sintered neodymium-iron-boron permanent-magnet material, it is characterised in that pre-processed by magnetron sputtering method
Neodymium iron boron magnetic body surface deposits quaternary and the above rare earth alloy film of quaternary, as diffusion source, by homogenization, grain boundary decision
And low-temperature tempering heat treatment, improve the border structure of magnet, to increase substantially the coercivity of magnet, while guaranteeing remanent magnetism base
This is constant；The quaternary and the above rare earth alloy thin film composition of quaternary are LRE100-x-y-zHRExMyAlz(1≤x≤40,1≤y≤
20,1≤z≤20) (atomic fraction), wherein LRE is one of Y, La, Ce, Pr, Nd light rare earth elements or more, and HRE is
One of Tb, Dy, Ho heavy rare earth element or more, one of M Cu, Fe, Co, Ga, Zr, Zn, Mn, Mg alloying element and
More than.
2. the preparation method of high performance sintered neodymium-iron-boron permanent-magnet material according to claim 1, it is characterised in that concrete technology
Step are as follows:
1) surface preparation is carried out to neodymium iron boron magnetic body；
2) in magnetron sputtering apparatus, magnet and target are further activated；
3) surface magnetic control sputtering is carried out to magnet after processing described in step 2), deposits quaternary and the above rare earth alloy film of quaternary；
4) Homogenization Treatments carried out to rare earth alloy film described in step 3), then carried out at grain boundary decision and lonneal heat
Reason.
3. the preparation method of high performance sintered neodymium-iron-boron permanent-magnet material according to claim 2, which is characterized in that step 1)
Middle pretreatment magnet surface roughness Ra≤0.1 μm, clean surface, without greasy dirt.
4. a kind of preparation method of high performance sintered neodymium-iron-boron permanent-magnet material according to claim 2, it is characterised in that step
Rapid 2) middle activation processing, is evacuated to 1 × 10 first-3~2 × 10-4Pa, then pass to high-purity argon gas adjust working vacuum to
1.5×10-2~1.0Pa range, target power output 100W, bias 100V, 5~10min of working time, are activated magnet；
Then, it is then turned on DC power supply, bombards target material surface 15min, the oxide skin(coating) and pollutant of removal target surface covering, Hong target process
Substrate is blocked using baffle.
5. the preparation method of high performance sintered neodymium-iron-boron permanent-magnet material according to claim 2, which is characterized in that step 3)
Middle to be used as working gas using high-purity argon gas, air pressure is 0.1~10Pa, and throughput is 20~50sccm, sputtering power for 80~
200W, sputtering time are 0.5~5h.
6. a kind of preparation method of high performance sintered neodymium-iron-boron permanent-magnet material according to claim 2, which is characterized in that step
It is rapid 4) described in Homogenization Treatments be: be first evacuated to 2 × 10-3Pa then passes to high-purity argon gas protection；Homogenization Treatments are closing
It is carried out in golden 0.8-0.9 times of melting range, keeps the temperature 2-10h；Grain boundary decision carries out within the scope of 650~950 DEG C, and heat preservation 0.5~
10h；Lonneal carries out in 400~600 DEG C, keeps the temperature 0.5~4h.
7. a kind of preparation method of high performance sintered neodymium-iron-boron permanent-magnet material according to claim 1, which is characterized in that institute
The fusing point of rare earth alloy film is stated within the scope of 450-600 DEG C.
8. a kind of preparation method of high performance sintered neodymium-iron-boron permanent-magnet material according to claim 1, which is characterized in that heavy
Product rare earth alloy plastics thickness control is in 0.1-10 μ m.
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Cited By (10)
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| CN111180191A (en) * | 2020-01-15 | 2020-05-19 | 太原科技大学 | Method for preparing high-performance sintered neodymium-iron-boron magnet |
| CN111304624A (en) * | 2020-03-10 | 2020-06-19 | 沈阳中北通磁科技股份有限公司 | Rare earth permanent magnet device added with lanthanum and cerium and manufacturing method thereof |
| CN112466645A (en) * | 2020-11-23 | 2021-03-09 | 北京麦戈龙科技有限公司 | Method for preparing rare earth permanent magnet |
| CN112820529A (en) * | 2020-12-31 | 2021-05-18 | 宁波松科磁材有限公司 | Preparation method of high-performance sintered neodymium iron boron |
| CN113096947A (en) * | 2020-07-06 | 2021-07-09 | 烟台首钢磁性材料股份有限公司 | Preparation method and microstructure of high-performance neodymium iron boron sintered magnet |
| CN113593798A (en) * | 2020-04-30 | 2021-11-02 | 有研稀土新材料股份有限公司 | R-T-B series sintered magnet and preparation method thereof |
| CN114664507A (en) * | 2022-04-14 | 2022-06-24 | 浙江大学 | High-performance rare earth permanent magnetic material with composite hard magnetic shell structure and preparation method thereof |
| CN114678182A (en) * | 2022-04-14 | 2022-06-28 | 浙江大学 | Low-cost high-performance multi-main-phase rare earth permanent magnet material and preparation method thereof |
| CN114875290A (en) * | 2022-05-06 | 2022-08-09 | 中国科学院宁波材料技术与工程研究所 | Grain boundary diffusion multiphase structure alloy, preparation method thereof and method for preparing high-performance neodymium iron boron magnet |
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| CN111180191A (en) * | 2020-01-15 | 2020-05-19 | 太原科技大学 | Method for preparing high-performance sintered neodymium-iron-boron magnet |
| CN111304624A (en) * | 2020-03-10 | 2020-06-19 | 沈阳中北通磁科技股份有限公司 | Rare earth permanent magnet device added with lanthanum and cerium and manufacturing method thereof |
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Application publication date: 20190111 |