CN105990019A - Preparation method for low heavy rare earth sintered neodymium iron boron - Google Patents
Preparation method for low heavy rare earth sintered neodymium iron boron Download PDFInfo
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- CN105990019A CN105990019A CN201610403627.0A CN201610403627A CN105990019A CN 105990019 A CN105990019 A CN 105990019A CN 201610403627 A CN201610403627 A CN 201610403627A CN 105990019 A CN105990019 A CN 105990019A
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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
- H01F41/0266—Moulding; Pressing
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
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Abstract
The invention discloses a preparation method for low heavy rare earth sintered neodymium iron boron. The preparation method comprises the following steps of: selecting magnetic powder sintered with neodymium iron boron magnet, namely mainly comprising a main phase and an auxiliary phase, wherein the main phase is the prepared neodymium iron boron alloy and the auxiliary phase comprises a grain boundary phase with low melting point and a submicron phase with high melting point; preparing main phase alloy powder and preparing into the powder with the grain size of 2-5mu m; uniformly mixing the main phase alloy powder with the auxiliary phase alloy powder in different proportions; performing orientation forming in the magnetic field on the uniformly mixed powder and then sintering and tempering, thereby acquiring the low heavy rare earth sintered neodymium iron boron magnet. The preparation method provided by the invention has the beneficial effects that the method is simple in operation, the heavy rare earth used in the product is reduced or the heavy rare earth is not used, the coercive force of the magnet according to the traditional production method is achieved, the production cost is greatly lowered and the preparation method is suitable for batch production. Besides, the magnet prepared by taking same quantity of heavy rare earth has the magnet coercive force higher than that of the magnet prepared according to the traditional method.
Description
Technical field
The present invention relates to sintered Nd-Fe-B magnetic material field, refer in particular to a kind of low heavy rare earth sintering neodymium ferrum
The preparation method of boron.
Background technology
Sintered Nd-Fe-B permanent magnetic material, for other permanent magnet material, has at a relatively high intrinsic rectify
Stupid power and magnetic energy product, be therefore widely used in electronic circuit, metallic weapon, space flight and aviation, therapeutic machine
The fields such as tool, more typically have magneto, speaker, computer disc driver, nuclear magnetic resonance
Equipment instrument etc..Meanwhile, high performance Nd-Fe-B permanent magnet material obtains in modern industry and electronic technology
Extensively application, such that it is able to make instrument and equipment trend towards miniaturization, lightening and energy-saving.
But the magnetic stability of such magnet is poor, hinder its extension in high-new application.In order to
Improving the combination property of neodymium iron boron magnetic body, in currently used high-performance neodymium-iron-boron magnet, major part all needs
Will be by mixing appropriate heavy rare earth element metal dysprosium or terbium.Dy2Fe14B and Tb2Fe14The magnetocrystalline of B is each
Anisotropy can all be far above Nd2Fe14B, wherein the anisotropy field of dysprosium ferrum boron is about the twice of neodymium iron boron
Many, and terbium ferrum boron is about four times.Further, since Dy2Fe14B phase have higher anisotropy field and
Relatively low saturation magnetization, the interpolation of Dy element can increase substantially the coercivity of magnet.Dy element
Interpolation also improve the Curie temperature of magnet, reduce coercivity and residual magnetism temperature coefficient, reduce magnetic
Logical irreversible loss, improves the temperature stability of magnet, drastically increases the highest of material and use
Temperature.Meanwhile, along with the interpolation of Dy element, the heat resistance corrosion of magnet and electrochemically resistant corrosive power
There is significant raising.
But, heavy rare earth element abundance in the earth's crust is the lowest and proved reserves are very limited, from present
From the point of view of the exploitation situation of rare earth, heavy rare earth the most gradually trends towards exhausted state, and Chinese Government has also begun to
Consciousness ground controls the outlet amount of rare earth, causes heavy rare earth price drastically to promote, has significantly increased the weight of enterprise
Financial burden.Therefore, in order to save heavy rare earth resource, reducing the cost of raw material, each state all begins one's study
How to reduce the usage amount of heavy rare earth in high-performance Ne-Fe-B.How to add or to be not added with dysprosium, terbium less
Scholar and manufacturing enterprise in the industry increasingly it is subject to Deng the coercivity improving neodymium iron boron magnetic body on the basis of heavy rare earth
Attention.
Summary of the invention
The present invention is to there is above-mentioned deficiency in prior art to overcome, it is provided that a kind of reduction production cost
With the preparation method improving the coercitive low heavy rare earth sintered NdFeB of magnet.
To achieve these goals, the present invention is by the following technical solutions:
The preparation method of a kind of low heavy rare earth sintered NdFeB, comprises the steps:
(1) choosing the magnetic powder of Sintered NdFeB magnet: mainly by principal phase and auxiliary phase composition, principal phase is preparation
The Nd Fe B alloys of gained, auxiliary phase includes low melting point Grain-Boundary Phase and high-melting-point submicron phase；
(2) main-phase alloy powder is prepared: use rapid hardening furnace rejection tablet, hydrogen break process and air-flow pulverized powder broken,
Make the powder that particle mean size is 2～5 μm；
(3) powder process: by main-phase alloy powder from auxiliary phase alloy powder according to different ratio mix homogeneously；
(4) powder after mix homogeneously in magnetic field oriented moulding and be sintered, temper, prepare
Low heavy rare earth Sintered NdFeB magnet.
The present invention improves magnet coercivity by adding auxiliary phase in the powder process stage, and the auxiliary phase of interpolation can optimize
The grain boundary structure of magnet, refinement main phase grain after sintering, thus have and significantly improve the coercitive effect of magnet
Really.In the present invention, the auxiliary phase of interpolation primarily serves following two effect: one, inhibiting grain growth；
Its two, repair plane defect.In the first acts on, the high-melting-point submicron of addition plays notable effect mutually
Really, fusing point is higher than the sintering temperature of neodymium iron boron simultaneously, and the high-melting-point submicron of interpolation is dispersed in neodymium mutually
In iron boron magnet, the effect stoping main phase grain to be grown up can be played；In the second effect, due to add
High-melting-point submicron is met and is caused high-melting-point submicron mutually internal portion crystal boundary boundary defect occur, so adding again
Adding low melting point Grain-Boundary Phase to make up plane defect, make crystal boundary Nd-rich phase more continuous, crystal boundary becomes apparent from,
Spin-exchange-coupled is risen buffer action, and it can play the effect of inhibiting grain growth equally simultaneously.The method is grasped
Make simple, and the heavy rare earth used in production can be reduced, or do not use heavy rare earth, reach tradition raw
Magnet coercivity during product method, makes production cost be greatly reduced, is suitable for mass production；It addition,
Same amount of heavy rare earth is used to obtain magnet coercivity more higher than magnet prepared by traditional method.
As preferably, in step (1), the composition of main-phase alloy is REaTMbFe100-a-b-cBc, wherein
RE is La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Dy, Tb, Ho, Er, Tm, Yb,
One or more in Lu, Y element, TM is Nb, Al, Cu, Co, Ni, Ga, Zr, Ti,
One or more in Cr, V, Mo, Sn, W, wherein: 20≤a≤35,0≤b≤10,0.9≤c
≤1.2。
As preferably, in step (1), the composition of auxiliary phase alloy includes low melting point crystal-boundary phase alloy powder
And high-melting-point submicron phase alloy powder, wherein: the composition of low melting point crystal-boundary phase alloy powder include Pr,
One or more in Nd, Tb, Dy, Ho, Er, Gd, its particle diameter is 0.5～5 μm；High-melting-point is sub-
Micron phase alloy powder composition include Nb, Ti, W, V, Mo, Cr, Zr, Gd, Ni, Tb,
One or more in Dy, Ho, Co, its particle diameter is less than 800nm.
As preferably, in step (3), in auxiliary phase alloy powder, low melting point crystal-boundary phase alloy powder adds
It is 1～4%wt that dosage accounts for the percentage by weight of Sintered NdFeB magnet, high-melting-point sub-micro in auxiliary phase alloy powder
It is 0.1～1%wt that the addition of rice phase alloy powder accounts for the percentage by weight of Sintered NdFeB magnet.
As preferably, in step (4), sintering temperature is 1040 DEG C～1100 DEG C, and vacuum is
(10-1～10-5) Pa, sintering time is 2-8 hour, carries out two-stage nitration temper after sintering.
As preferably, in step (4), temper technique is as follows: the temperature of first paragraph is
850～950 DEG C, tempering time is 1～3 hour；The temperature of second segment is 480～550 DEG C, during tempering
Between be 3～6 hours.
The invention has the beneficial effects as follows: the method is simple to operate, and it is dilute to reduce the weight used in production
Soil, or do not use heavy rare earth, reach magnet coercivity during conventional production methods, make production cost big
Width reduces, and is suitable for mass production；It addition, use same amount of heavy rare earth to obtain ratio traditional method system
Standby magnet higher magnet coercivity.
Detailed description of the invention
The present invention will be further described for knot detailed description of the invention below.
Comparative example:
Prepared composition is (Pr0.25Nd0.75)27Fe65.93Nb0.4Co1.5Dy3.5Cu0.2Al0.3Ga0.2B0.97Magnet,
Employing strip casting prepares, and hydrogen is broken subsequently, airflow milling powder, and powder mean particle sizes is 3.2 μm.At magnetic
In Chang after oriented moulding, put into vacuum sintering furnace (vacuum 5*10-2Pa) respectively at 1080 DEG C of * 4.5H in
Sintering, 2H+520 DEG C of * 4H temper of 910 DEG C of *.
After sintered tempering, magnet performance result is: Br=12.2Gs, Hcj=24.1kOe,
(BH)max=36.1MOeGs.
Embodiment one:
Take particle diameter and be about the Ti powder of 300 nanometers and particle diameter is about the Pr powder of 3 microns, with
(Pr0.25Nd0.75)27Fe65.93Nb0.4Co1.5Dy3.5Cu0.2Al0.3Ga0.2B0.97Powder mixing after airflow milling, mixes
Enter ratio and be respectively 0.2%wt and 2%wt, in magnetic field orientating, after being sufficiently mixed, be pressed into blank.Through burning
After knot annealing, performance is: Br=12.1Gs, Hcj=26.8kOe, (BH)max=35.7MOeGs.
Embodiment two:
Take particle diameter and be about the w powder of 200 nanometers and particle diameter is about the Nd powder of 2 microns, mix
(Pr0.25Nd0.75)27Fe65.93Nb0.4Co1.5Dy3.5Cu0.2Al0.3Ga0.2B0.97In powder after airflow milling, mix
Amount is respectively 0.15%wt and 3%wt, is pressed into blank after being sufficiently mixed in magnetic field orientating.Sintered move back
After fire, performance is: Br=12.15Gs, Hcj=26.9kOe, (BH)max=35.8MOeGs.
Embodiment three:
Take particle diameter and be about the Mo powder of 500 nanometers and particle diameter is about the PrNd powder of 1 micron, mix
(Pr0.25Nd0.75)27Fe65.93Nb0.4Co1.5Dy3.5Cu0.2Al0.3Ga0.2B0.97In powder after airflow milling, mix
Amount is respectively 0.1% and 1%wt, is pressed into blank after being sufficiently mixed in magnetic field orientating.Sintered annealing
Rear performance is: Br=12.1Gs, Hcj=27kOe, (BH)max=35.6MOeGs.
Embodiment four:
Take particle diameter and be about the Ti powder of 800 nanometers and particle diameter is about the PrNd powder of 2 microns, mix
(Pr0.25Nd0.75)27Fe65.93Nb0.4Co1.5Dy3.5Cu0.2Al0.3Ga0.2B0.97In powder after airflow milling, mix
Amount is respectively 1% and 4%wt, is pressed into blank after being sufficiently mixed in magnetic field orientating.After sintered annealing
Performance is: Br=12.02Gs, Hcj=27.3kOe, (BH)max=35.4MOeGs.
Claims (6)
1. a preparation method for low heavy rare earth sintered NdFeB, is characterized in that, comprise the steps:
(1) magnetic powder of Sintered NdFeB magnet is chosen: main by principal phase and auxiliary phase composition, principal phase is for preparing gained
Nd Fe B alloys, auxiliary phase includes low melting point Grain-Boundary Phase and high-melting-point submicron phase；
(2) main-phase alloy powder is prepared: use rapid hardening furnace rejection tablet, hydrogen break process and air-flow pulverized powder broken, system
The powder becoming particle mean size to be 2～5 μm；
(3) powder process: by main-phase alloy powder from auxiliary phase alloy powder according to different ratio mix homogeneously；
(4) powder after mix homogeneously in magnetic field oriented moulding and be sintered, temper, prepare low heavy
Rare earth Sintered NdFeB magnet.
The preparation method of a kind of low heavy rare earth sintered NdFeB the most according to claim 1, is characterized in that,
In step (1), the composition of main-phase alloy is REaTMbFe100-a-b-cBc, wherein RE be La, Ce,
In Pr, Nd, Pm, Sm, Eu, Gd, Dy, Tb, Ho, Er, Tm, Yb, Lu, Y element
One or more, TM is Nb, Al, Cu, Co, Ni, Ga, Zr, Ti, Cr, V, Mo, Sn,
One or more in W, wherein: 20≤a≤35,0≤b≤10,0.9≤c≤1.2.
The preparation method of a kind of low heavy rare earth sintered NdFeB the most according to claim 1, is characterized in that,
In step (1), the composition of auxiliary phase alloy includes low melting point crystal-boundary phase alloy powder and high-melting-point submicron
Phase alloy powder, wherein: the composition of low melting point crystal-boundary phase alloy powder include Pr, Nd, Tb, Dy,
One or more in Ho, Er, Gd, its particle diameter is 0.5～5 μm；High-melting-point submicron is harmonious bronze
The composition at end includes Nb, Ti, W, V, Mo, Cr, Zr, Gd, Ni, Tb, Dy, Ho, Co
In one or more, its particle diameter be less than 800nm.
The preparation method of a kind of low heavy rare earth sintered NdFeB the most according to claim 1, is characterized in that,
In step (3), in auxiliary phase alloy powder, the addition of low melting point crystal-boundary phase alloy powder accounts for sintered NdFeB
The percentage by weight of magnet is 1～4%wt, and in auxiliary phase alloy powder, high-melting-point submicron phase alloy powder adds
It is 0.1～1%wt that dosage accounts for the percentage by weight of Sintered NdFeB magnet.
The preparation method of a kind of low heavy rare earth sintered NdFeB the most according to claim 1, is characterized in that,
In step (4), sintering temperature is 1040 DEG C～1100 DEG C, and vacuum is (10-1～10-5) Pa, sintering
Time is 2-8 hour, carries out two-stage nitration temper after sintering.
The preparation method of a kind of low heavy rare earth sintered NdFeB the most according to claim 5, is characterized in that,
In step (4), temper technique is as follows: the temperature of first paragraph is 850～950 DEG C, during tempering
Between be 1～3 hour；The temperature of second segment is 480～550 DEG C, and tempering time is 3～6 hours.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106881459A (en) * | 2016-12-21 | 2017-06-23 | 包头稀土研究院 | The method that NdFeB magnetic powder is prepared using heavy rare earth |
| CN107316727A (en) * | 2017-07-06 | 2017-11-03 | 京磁材料科技股份有限公司 | A kind of sintered NdFeB preparation method |
| CN107464644A (en) * | 2017-09-06 | 2017-12-12 | 京磁材料科技股份有限公司 | The preparation method of performance Nd Fe B sintered magnet |
| CN108806911A (en) * | 2018-04-26 | 2018-11-13 | 安徽省瀚海新材料股份有限公司 | A kind of neodymium iron boron magnetic body and preparation method thereof |
| CN110033914A (en) * | 2019-05-22 | 2019-07-19 | 包头稀土研究院 | Improve the coercitive method of Sintered NdFeB magnet |
| CN110060833A (en) * | 2019-05-21 | 2019-07-26 | 宁波永久磁业有限公司 | A kind of high remanent magnetism, high-coercive force R-T-B permanent-magnet material and preparation method thereof |
| CN110534280A (en) * | 2019-09-23 | 2019-12-03 | 广西科技大学 | A kind of preparation method of the performance Nd Fe B sintered magnet based on crystal boundary addition |
| CN111952032A (en) * | 2020-08-15 | 2020-11-17 | 赣州嘉通新材料有限公司 | Preparation method of low-boron low-weight rare earth high-coercivity sintered neodymium-iron-boron permanent magnet |
| CN112002510A (en) * | 2020-08-25 | 2020-11-27 | 安徽万磁电子有限公司 | High-coercivity permanent magnet based on holmium-rich rare earth permanent magnet liquid phase alloy and preparation method thereof |
| CN112509775A (en) * | 2020-12-15 | 2021-03-16 | 烟台首钢磁性材料股份有限公司 | Neodymium-iron-boron magnet with low-amount heavy rare earth addition and preparation method thereof |
| CN112908665A (en) * | 2020-02-17 | 2021-06-04 | 廊坊京磁精密材料有限公司 | Infiltration method for improving coercivity of sintered neodymium-iron-boron |
| CN116313353A (en) * | 2023-05-23 | 2023-06-23 | 包头天石稀土新材料有限责任公司 | Neodymium-iron-boron magnet and preparation method thereof |
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| CN106881459A (en) * | 2016-12-21 | 2017-06-23 | 包头稀土研究院 | The method that NdFeB magnetic powder is prepared using heavy rare earth |
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| CN107464644A (en) * | 2017-09-06 | 2017-12-12 | 京磁材料科技股份有限公司 | The preparation method of performance Nd Fe B sintered magnet |
| CN108806911A (en) * | 2018-04-26 | 2018-11-13 | 安徽省瀚海新材料股份有限公司 | A kind of neodymium iron boron magnetic body and preparation method thereof |
| CN110060833A (en) * | 2019-05-21 | 2019-07-26 | 宁波永久磁业有限公司 | A kind of high remanent magnetism, high-coercive force R-T-B permanent-magnet material and preparation method thereof |
| CN110033914A (en) * | 2019-05-22 | 2019-07-19 | 包头稀土研究院 | Improve the coercitive method of Sintered NdFeB magnet |
| CN110534280A (en) * | 2019-09-23 | 2019-12-03 | 广西科技大学 | A kind of preparation method of the performance Nd Fe B sintered magnet based on crystal boundary addition |
| CN112908665A (en) * | 2020-02-17 | 2021-06-04 | 廊坊京磁精密材料有限公司 | Infiltration method for improving coercivity of sintered neodymium-iron-boron |
| CN112908665B (en) * | 2020-02-17 | 2022-12-27 | 廊坊京磁精密材料有限公司 | Infiltration method for improving coercivity of sintered neodymium-iron-boron |
| CN111952032A (en) * | 2020-08-15 | 2020-11-17 | 赣州嘉通新材料有限公司 | Preparation method of low-boron low-weight rare earth high-coercivity sintered neodymium-iron-boron permanent magnet |
| CN112002510A (en) * | 2020-08-25 | 2020-11-27 | 安徽万磁电子有限公司 | High-coercivity permanent magnet based on holmium-rich rare earth permanent magnet liquid phase alloy and preparation method thereof |
| CN112509775A (en) * | 2020-12-15 | 2021-03-16 | 烟台首钢磁性材料股份有限公司 | Neodymium-iron-boron magnet with low-amount heavy rare earth addition and preparation method thereof |
| CN116313353A (en) * | 2023-05-23 | 2023-06-23 | 包头天石稀土新材料有限责任公司 | Neodymium-iron-boron magnet and preparation method thereof |
| CN116313353B (en) * | 2023-05-23 | 2023-08-29 | 包头天石稀土新材料有限责任公司 | Neodymium-iron-boron magnet and preparation method thereof |
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