CN107256795A - The method that performance Nd Fe B sintered magnet is prepared using two step grain boundary diffusion process - Google Patents

The method that performance Nd Fe B sintered magnet is prepared using two step grain boundary diffusion process Download PDF

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Publication number
CN107256795A
CN107256795A CN201710497739.1A CN201710497739A CN107256795A CN 107256795 A CN107256795 A CN 107256795A CN 201710497739 A CN201710497739 A CN 201710497739A CN 107256795 A CN107256795 A CN 107256795A
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diffusion
magnet
grain
performance
grain boundary
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CN201710497739.1A
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包小倩
卢克超
陈贵贤
高学绪
李纪恒
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
    • C23C10/30—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes using a layer of powder or paste on the surface
    • 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

Abstract

A kind of method that performance Nd Fe B sintered magnet is prepared using two step grain boundary diffusion process, belongs to field of rare-earth permanent magnetic.Concrete technology step is：Low-melting alloy diffusion source R1 R2 TM strips are coated with clean business Sintered NdFeB magnet surface, wherein, R1 is optionally, R2 is at least one of Dy, Tb in La, Ce, Pr, Nd, and TM is at least one of Cu, Al, Ti, Zn, Co, Ni, Fe；By 650 800 DEG C of 6 24h of heat treatment, make Tb/Dy along crystal boundary to magnet diffusion inside；850 950 DEG C are heat-treated 1 4h, and the Tb/Dy for being enriched in Grain-Boundary Phase spreads to Grain Surface, form richness Tb/Dy shell structurre；450 550 DEG C of 1.5 2.5h of annealing, further adjust border structure；Finally give performance Nd Fe B sintered magnet.It is an advantage of the invention that：Make full use of Tb/Dy to strengthen grain surface transition zone, improve coercivity；Shorten the high-temperature heat treatment time, save the energy；Avoid abnormal grain growth；Suitable for thicker magnet.

Description

The method that performance Nd Fe B sintered magnet is prepared using two step grain boundary diffusion process
Technical field
The present invention relates to a kind of method that performance Nd Fe B sintered magnet is prepared using two step grain boundary diffusion process, belong to Field of rare-earth permanent magnetic.
Background technology
Sintered Nd-Fe-B system alloy is because with higher remanent magnetism, coercivity and maximum magnetic energy product, high comprehensive performance, quilt Referred to as " magnetic king ".Since the advent of the world, is widely used in electronic information, medicine equipment, wind-power electricity generation and auto industry.Through The development of decades is crossed, the magnetic property of sintered Nd-Fe-B system permanent-magnet alloy is improved constantly, wherein remanent magnetism Br and maximum magnetic energy product (BH) max is already close to limiting value, but the actual coercivity of sintered Nd-Fe-B only has 30% of theoretical value or so, Er Qiekao Consider the use environment of Sintered NdFeB magnet, it usually needs magnet has higher room temperature coercivity.Therefore, coercivity is improved It is the key for improving Sintered NdFeB magnet combination property.
Research finds, when alloyed powder or compound of the surface with the heavy rare earth element such as Tb/Dy of Sintered NdFeB magnet, By diffusion heat treatments, heavy rare earth element grain boundary diffusion, and in Nd2Fe14B Grain Surfaces formation (Nd, Tb/Dy)2Fe14B shells Rotating fields, improve grain surface anisotropy field, while improving crystal boundary microscopic structure, so processing can make the coercivity of magnet bright Show and improve and remanent magnetism does not reduce or reduced very little, this technology is referred to as grain boundary decision technology.The advantage of grain boundary diffusion process exists Grain Surface is only enriched in heavy rare earth element, without largely entering transgranular, heavy rare earth element is reduced to a certain extent Consumption, while remanent magnetism will not be significantly reduced.General diffusion source used is Dy203、DyF3、TbF3Deng.In recent years, using low Melting alloy is used as diffusion source (such as Nd70Cu30,Pr68Cu32,Dy70Cu30,Dy73Ni9.5Al17.5,Pr35Dy35Cu30, Nd60Dy20Cu20,Nd62D20yAl18Deng) grain boundary diffusion process obtained widely studied.Usually, grain boundary diffusion process includes High temperature diffusion processing is carried out at 800-950 DEG C, it is therefore an objective to which the diffusion source containing heavy rare earth element enters Grain-Boundary Phase along crystal boundary；With 450-550 DEG C of lonneal is carried out afterwards, it is therefore an objective to adjust the microstructure and form of Grain-Boundary Phase.Current grain boundary decision technology is present Subject matter be magnet top layer heavy rare earth element concentration gradient it is higher, body diffusion is violent, forms thicker shell structurre, disappears Substantial amounts of heavy rare earth element is consumed, causes to waste；And thicker magnet is spread, it is necessary to which high temperature diffusion for a long time, causes crystal grain abnormal Grow up.
The content of the invention
The invention aims to suppress the violent body diffusion couple heavy rare earth element Tb/ of magnet surface during grain boundary decision Dy is consumed, efficient to utilize heavy rare earth element Tb/Dy, while improving the distribution of Grain-Boundary Phase and rich rare earth shell structurre, it is to avoid brilliant Grain abnormal growth, obtains the magnet with higher coercivity.
The present invention specific implementation step be：
(1) business neodymium iron boron magnetic body is processed into 3-10mm thickness along differently- oriented directivity, then cleans magnet surface, and ensure Its upper and lower surface is bright and clean, smooth；Diffusion source is attached to the neodymium iron boron magnetic body upper and lower surface of cleaning, diffusion source is spread for low melting point Source R1-R2-TM；Wherein, R1 is the one or two kinds of in La, Ce, Pr, Nd；R2 is the one or two kinds of in Dy, Tb；TM For in Cu, Al, Ti, Zn, Co, Ni, Fe optionally；
(2) disperser for laying diffusion source is placed in diffusion in vacuum stove, is evacuated to (3-5) × 10-3Pa, then Start to warm up；
(3) in 650-800 DEG C of low temperature diffusion 6-24h, it is therefore an objective to make heavy rare earth element Tb/Dy grain boundary diffusions and be distributed In Grain-Boundary Phase；
(4) in 850-950 DEG C of high-temperature heat treatment 1-4h, it is therefore an objective to promote to be present in the Tb/Dy elements in Grain-Boundary Phase in master Phase Grain Surface forms rich Tb/Dy shell structurres；
(5) make annealing treatment 1.5-2.5h at 450-550 DEG C and obtain high-coercive force Nd-Fe-B permanent magnet；
(6) further, diffusion source alloy thin band thickness is 10-100 μm, preferably 30-50 μm；
(7) further, by adjusting diffusion derived components, by the control of alloy diffusion source fusing point in the range of 450-700 DEG C.
The invention has the advantages that：Tb/Dy utilization rate is improved to greatest extent；Avoiding high temperature, diffusion causes crystal grain different for a long time Often grow up, possibility is provided for the thicker magnet of grain boundary decision.
Brief description of the drawings
Fig. 1 is N50 original structures respectively
Fig. 2 utilizes Pr50Tb20Cu15Al15After the processing 6h and (b) 900 DEG C × 1h+500 DEG C × 2h of 700 DEG C of diffusion source (a) Tissue
Fig. 3 utilizes Pr60Tb10Cu10Al10Co10650 DEG C of diffusion source (a) processing 6h and (b) 900 DEG C × 1h+500 DEG C × 2h Tissue afterwards
Embodiment
Embodiment 1：
The commercial magnets of N50 are selected, size is processed into for φ 8mm × 5mm sample and cleaning treatment is carried out to surface.Pass through Strip casting prepared composition is Pr50Tb20Cu15Al15The alloy thin band (30 μ m-thick) of (atomic percentage) is used as diffusion source；Directly It is covered in the magnet upper and lower surface handled by surface cleaning；The sample handled well is placed in stove, be evacuated to (3-5) × 10-3Pa carries out one-level heat treatment, i.e., be incubated 6h at 700 DEG C；Then two grades of heat treatments are carried out, i.e., are incubated 1h at 900 DEG C；It is most laggard The heat treatment of row three-level is in 500 DEG C of vacuum annealing processing 2h；Obtain high-coercive force sintered Nd-Fe-B magnetic material.By magnet coercivity The 22.5kOe brought up to from the 12.2kOe before grain boundary decision after diffusion, and remanent magnetism hardly declines.After original magnet and diffusion The magnetic property of magnet, such as following table：
Sample Remanent magnetism (T) Coercivity (kOe) Magnetic energy product (MGOe)
Original magnet 1.41 12.2 49
Magnet after diffusion 1.38 22.5 47.8
Embodiment 2：
The commercial magnets of N50 are selected, size is processed into for φ 8mm × 5mm sample and cleaning treatment is carried out to surface.Pass through Strip casting prepared composition is Pr60Tb10Cu10Al10Co10The alloy thin band (30 μ m-thick) of (atomic percentage) is used as diffusion source； Directly overlay the magnet upper and lower surface handled by surface cleaning；The sample handled well is placed in stove, is evacuated to (3-5) × 10-3Pa carries out one-level heat treatment, i.e., be incubated 6h at 650 DEG C；Then two grades of heat treatments are carried out, i.e., are incubated 1h at 900 DEG C；Most Three-level heat treatment is carried out afterwards in 500 DEG C of vacuum annealing processing 2h；Obtain high-coercive force sintered Nd-Fe-B magnetic material.Magnet coercive The 20.5kOe that power is brought up to after diffusion from the 12.5kOe before grain boundary decision, and remanent magnetism hardly declines.Original magnet and diffusion The magnetic property of magnet, such as following table afterwards：
Sample Remanent magnetism (T) Coercivity (kOe) Magnetic energy product (MGOe)
Original magnet 1.41 12.5 49.5
Magnet after diffusion 1.39 20.5 48.6

Claims (4)

1. a kind of method that performance Nd Fe B sintered magnet is prepared using two step grain boundary diffusion process, it is characterised in that specific Processing step is：
(1) business neodymium iron boron magnetic body is processed into 3-10mm thickness along differently- oriented directivity, then cleans magnet surface, and ensure thereon Lower surface is bright and clean, smooth；Source alloy thin band will be spread and be attached to clean neodymium iron boron magnetic body upper and lower surface, diffusion source is low melting point Diffusion source R1-R2-TM；Wherein, R1 is the one or two kinds of in La, Ce, Pr, Nd；R2 is one kind or two in Dy, Tb Kind；TM is optional in Cu, Al, Ti, Zn, Co, Ni, Fe；
(2) disperser for laying diffusion source is placed in diffusion in vacuum stove, is evacuated to (3-5) × 10-3Pa, then starts Heating；
(3) in 650-800 DEG C of low temperature diffusion 6-24h, it is therefore an objective to make heavy rare earth element Tb/Dy grain boundary diffusions and be distributed in crystalline substance Boundary's phase；
(4) in 850-950 DEG C of high-temperature heat treatment 1-4h, it is therefore an objective to which the Tb/Dy elements for promoting to be present in Grain-Boundary Phase are brilliant in principal phase Grain top layer forms rich Tb/Dy shell structurres；
(5) make annealing treatment 1.5-2.5h at 450-550 DEG C and obtain high-coercive force Nd-Fe-B permanent magnet.
2. a kind of two step grain boundary diffusion process of utilization prepare the side of performance Nd Fe B sintered magnet according to claim 1 Method, it is characterized in that：Described diffusion source alloy thin band thickness is 10-100 μm；
3. a kind of two step grain boundary diffusion process of utilization according to claim 1 or claim 2 prepare performance Nd Fe B sintered magnet Method, it is characterized in that：Described diffusion source alloy thin band thickness is 30-50 μm；
4. a kind of two step grain boundary diffusion process of utilization prepare the side of performance Nd Fe B sintered magnet according to claim 1 Method, it is characterized in that：By adjusting diffusion derived components, by the control of alloy diffusion source fusing point in the range of 450-700 DEG C.
CN201710497739.1A 2017-06-27 2017-06-27 The method that performance Nd Fe B sintered magnet is prepared using two step grain boundary diffusion process Pending CN107256795A (en)

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Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107845464A (en) * 2017-11-23 2018-03-27 安徽大地熊新材料股份有限公司 A kind of method for preparing high-coercive force Nd-Fe-B series permanent magnet
CN108010705A (en) * 2017-11-29 2018-05-08 宁德市星宇科技有限公司 A kind of preparation method of neodymium iron boron magnetic body
CN108335898A (en) * 2018-02-05 2018-07-27 宁波松科磁材有限公司 A kind of sintered NdFeB sheet magnet steel temperature stability of improving oozes dysprosium technique
CN108417380A (en) * 2018-05-21 2018-08-17 钢铁研究总院 A kind of low cost diffusion source alloy and grain boundary decision magnet and preparation method thereof
CN108987018A (en) * 2018-08-01 2018-12-11 宁波科升磁业有限公司 A method of preparing high-coercive force and high-corrosion resistance Sintered NdFeB magnet
CN110136909A (en) * 2019-05-22 2019-08-16 包头稀土研究院 The grain boundary decision method of sintered Nd-Fe-B permanent magnet
CN111403167A (en) * 2020-04-26 2020-07-10 江苏科技大学 Grain boundary diffusion method for sintered neodymium-iron-boron magnet heavy rare earth element
CN111430142A (en) * 2019-01-10 2020-07-17 中国科学院宁波材料技术与工程研究所 Method for preparing neodymium iron boron magnet by grain boundary diffusion
CN112017834A (en) * 2020-08-20 2020-12-01 合肥工业大学 High-performance sintered neodymium-iron-boron magnet and preparation method thereof
CN112489914A (en) * 2020-11-03 2021-03-12 北京科技大学 Method for preparing high-coercivity neodymium-iron-boron magnet through composite diffusion
CN112802677A (en) * 2020-08-27 2021-05-14 北京工业大学 Method for simultaneously improving coercivity and mechanical property of small-size sintered neodymium-iron-boron magnet
CN113270241A (en) * 2020-09-16 2021-08-17 江西理工大学 Neodymium-iron-boron magnet and preparation method thereof
CN113314327A (en) * 2021-06-02 2021-08-27 中国科学院力学研究所 Method for grain boundary diffusion of multi-element heavy rare earth of sintered neodymium-iron-boron magnet
CN114334416A (en) * 2021-12-21 2022-04-12 北京工业大学 Method for preparing high-performance neodymium iron boron magnet by solid-liquid phase separation diffusion process
CN114883104A (en) * 2022-05-06 2022-08-09 中国科学院宁波材料技术与工程研究所 Processing method for grain boundary diffusion of neodymium iron boron magnet
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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CN104851545A (en) * 2015-05-21 2015-08-19 唐海峰 Production method of permanent magnet material with grain boundary diffusion layer
CN105170976A (en) * 2015-10-23 2015-12-23 北京科技大学 Method for preparing high-coercivity neodymium iron boron by means of low-temperature sintering after blank compacting permeation
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Cited By (27)

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Publication number Priority date Publication date Assignee Title
CN107845464A (en) * 2017-11-23 2018-03-27 安徽大地熊新材料股份有限公司 A kind of method for preparing high-coercive force Nd-Fe-B series permanent magnet
CN108010705A (en) * 2017-11-29 2018-05-08 宁德市星宇科技有限公司 A kind of preparation method of neodymium iron boron magnetic body
CN111710519A (en) * 2017-11-29 2020-09-25 宁德市星宇科技有限公司 Method for preparing neodymium-iron-boron magnet through grain boundary diffusion
CN108335898A (en) * 2018-02-05 2018-07-27 宁波松科磁材有限公司 A kind of sintered NdFeB sheet magnet steel temperature stability of improving oozes dysprosium technique
WO2019223431A1 (en) * 2018-05-21 2019-11-28 钢铁研究总院 Low-cost diffusion source alloy, and grain boundary diffusion magnet and preparation method therefor
CN108417380A (en) * 2018-05-21 2018-08-17 钢铁研究总院 A kind of low cost diffusion source alloy and grain boundary decision magnet and preparation method thereof
CN108987018A (en) * 2018-08-01 2018-12-11 宁波科升磁业有限公司 A method of preparing high-coercive force and high-corrosion resistance Sintered NdFeB magnet
CN111430142A (en) * 2019-01-10 2020-07-17 中国科学院宁波材料技术与工程研究所 Method for preparing neodymium iron boron magnet by grain boundary diffusion
CN111430142B (en) * 2019-01-10 2021-12-07 中国科学院宁波材料技术与工程研究所 Method for preparing neodymium iron boron magnet by grain boundary diffusion
CN110136909A (en) * 2019-05-22 2019-08-16 包头稀土研究院 The grain boundary decision method of sintered Nd-Fe-B permanent magnet
CN110136909B (en) * 2019-05-22 2020-10-30 包头稀土研究院 Grain boundary diffusion method of sintered neodymium-iron-boron permanent magnet
CN111403167A (en) * 2020-04-26 2020-07-10 江苏科技大学 Grain boundary diffusion method for sintered neodymium-iron-boron magnet heavy rare earth element
CN111403167B (en) * 2020-04-26 2022-09-23 江苏科技大学 Sintered neodymium-iron-boron magnet heavy rare earth element crystal boundary diffusion method
CN112017834A (en) * 2020-08-20 2020-12-01 合肥工业大学 High-performance sintered neodymium-iron-boron magnet and preparation method thereof
CN112017834B (en) * 2020-08-20 2023-03-17 合肥工业大学 High-performance sintered neodymium-iron-boron magnet and preparation method thereof
CN112802677A (en) * 2020-08-27 2021-05-14 北京工业大学 Method for simultaneously improving coercivity and mechanical property of small-size sintered neodymium-iron-boron magnet
CN112802677B (en) * 2020-08-27 2023-09-01 北京工业大学 Method for simultaneously improving coercive force and mechanical property of small-size sintered NdFeB magnet
CN113270241A (en) * 2020-09-16 2021-08-17 江西理工大学 Neodymium-iron-boron magnet and preparation method thereof
CN113270241B (en) * 2020-09-16 2023-06-02 江西理工大学 Neodymium-iron-boron magnet and preparation method thereof
CN112489914A (en) * 2020-11-03 2021-03-12 北京科技大学 Method for preparing high-coercivity neodymium-iron-boron magnet through composite diffusion
CN113314327A (en) * 2021-06-02 2021-08-27 中国科学院力学研究所 Method for grain boundary diffusion of multi-element heavy rare earth of sintered neodymium-iron-boron magnet
CN114334416A (en) * 2021-12-21 2022-04-12 北京工业大学 Method for preparing high-performance neodymium iron boron magnet by solid-liquid phase separation diffusion process
WO2023116234A1 (en) * 2021-12-21 2023-06-29 北京工业大学 Method for preparing high-performance neodymium-iron-boron magnet through solid-liquid phase separation diffusion process
CN114334416B (en) * 2021-12-21 2024-03-19 北京工业大学 Method for preparing high-performance neodymium-iron-boron magnet by solid-liquid phase separation diffusion process
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
CN114883104A (en) * 2022-05-06 2022-08-09 中国科学院宁波材料技术与工程研究所 Processing method for grain boundary diffusion of neodymium iron boron magnet
CN114875290B (en) * 2022-05-06 2023-10-31 中国科学院宁波材料技术与工程研究所 Crystal boundary diffusion multiphase structure alloy and preparation method thereof, and method for preparing high-performance neodymium-iron-boron magnet

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