CN106128671B - High-performance Ne-Fe-B permanent-magnet material and preparation method thereof - Google Patents

High-performance Ne-Fe-B permanent-magnet material and preparation method thereof Download PDF

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CN106128671B
CN106128671B CN201610424512.XA CN201610424512A CN106128671B CN 106128671 B CN106128671 B CN 106128671B CN 201610424512 A CN201610424512 A CN 201610424512A CN 106128671 B CN106128671 B CN 106128671B
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permanent
magnet material
performance
preparation
temperature
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CN106128671A (en
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路河树
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NINGBO XIONGHAI RARE EARTH RAPID HARDENING TECHNOLOGY Co Ltd
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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
    • H01F1/0573—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 obtained by reduction or by hydrogen decrepitation or embrittlement
    • 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
    • H01F1/0576—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 pressed, e.g. hot working
    • 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
    • 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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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Hard Magnetic Materials (AREA)

Abstract

A kind of high-performance Ne-Fe-B permanent-magnet material, it is characterised in that：The permanent-magnet material is made of each component of following weight percent：PrNd 31 35%, Gd0.5 1%, Ga 0.05 0.15%, Zr 0.05 0.15%, B 0.8 1.6%, Co 0.2 0.5%, Al 0.1 0.4%, Cu 0.05 0.2%, Mo 0.05 0.3%, Ti 0.05 0.3%, LaCe 0.1 0.5%, surplus Fe.Rationally control PrNd contents and the content of Nd of the invention, while by adding the elements such as rare earth and Zr, the maximum magnetic energy product of magnet entirety is improved, so as to reduce the usage amount of magnet, more lightweight, Costco Wholesale is low.

Description

High-performance Ne-Fe-B permanent-magnet material and preparation method thereof
Technical field
The present invention relates to permanent-magnet material technical fields, and in particular to a kind of high-performance (more than maximum magnetic energy product 390MGOe) Nd-Fe-B permanent magnet material and preparation method thereof.
Background technology
Ndfeb magnet is to the permanent magnet so far with most strong magnetic force.Neodymium iron boron is referred to as third generation rare earth forever Magnetic material, is the highest permanent-magnet material of current magnetic energy product, nineteen eighty-three, by SUMITOMO CHEMICAL particulate metal company and AM General automobile Company succeeds in developing at first.With the development of the industries such as computer, communication, the preparation and application of NdFeB permanent-magnet materials are flown Speed development.Its application can greatly reduce the volume and quality of complete machine, and the application such as on disk can make disc driver Micromation, and performance is more preferable.In audio device, neodymium iron boron is widely used in Microspeaker, earphone and superior automobile Loud speaker substantially increases fidelity and the signal-to-noise ratio of sound equipment.Direct current generator and Magnetic resonance imaging are additionally can be applied to, Not only quantity is big for application particularly on magnetic suspension train, but also can realize that rapid transit, safe and reliable and noise are small etc. Feature.
But at present, China market is mostly the low permanent-magnet material of the comparison of magnetic property used, in use due to property Can be undesirable, it will result in that usage amount is big, increase the deficiency of cost.
Invention content
The present invention is directed to the above-mentioned deficiency of the prior art, provides a kind of magnetic energy product height, the high high-performance Ne-Fe-B of toughness is forever Magnetic material.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：A kind of high-performance Ne-Fe-B permanent-magnet material, The permanent-magnet material is made of each component of following weight percent：PrNd 31-35%, Gd 0.5-1%, Ga 0.05- 0.15%, Zr 0.05-0.15%, B 0.8-1.6%, Co 0.2-0.5%, Al 0.1-0.4%, Cu 0.05-0.2%, Mo 0.05-0.3%, Ti 0.05-0.3%, LaCe 0.1-0.5%, surplus Fe.
Preferably, the high-performance Ne-Fe-B permanent-magnet material, the permanent-magnet material is each by following weight percent Component forms：PrNd 32-34%, Gd 0.6-0.8%, Ga 0.06-0.10%, Zr 0.06-0.1%, B 0.8-1.2%, Co 0.25-0.35%, Al 0.25-0.35%, Cu 0.06-0.10%, Mo 0.05-0.3%, Ti 0.05-0.3%, LaCe 0.1-0.5%, surplus Fe.
The above-mentioned PrNd of the present invention is PrNd alloys, and the occupancy volume of Nd therein is 1-5%.
The present invention also provides a kind of preparation method of above-mentioned Nd-Fe-B permanent magnet material, preparation process is：
(1) it matches raw material by the constituent of neodymium iron boron magnetic body and mass percent and carries out melting, after melting is complete It pours into a mould, be cooled to and get rid of strap；
(2) band obtained above that gets rid of is carried out that hydrogen is broken and airflow milling, powder is made；
(3) above-mentioned powder under inert gas shielding is put into moulding press mold plus magnetic field is orientated, after orientation Compression moulding；
(4) green compact obtained after above-mentioned molding are put into sintering furnace and be sintered at high temperature, be then tempered, obtained To neodymium iron boron magnetic body green body
The melting of step (1) of the present invention be vacuum melting, vacuum degree 0.05-0.2Pa；The thickness for getting rid of strap is 0.1- 0.3mm；
Step (2) hydrogen of the present invention carries out the dehydrogenation of 4-8h after crushing, it is micro- that diameter of particle then is ground to 3-5 with airflow milling Rice；Then antioxidant is added in into batch mixing in powder, it is vertical orientated in the pulsed magnetic field of 8T again after mixed to be pressed into briquet；
Being sintered in step (4) of the present invention：It is put into RVS-300 vacuum sintering furnaces and is sintered, sintering temperature 1060- 1120 DEG C, sintering time 40-100min；
Tempering in inventive step (4) is：1-3Pa will be evacuated in stove, then increases furnace temperature to 250-350 DEG C, protect Warm 1-2h；450-550 DEG C is then heated to, keeps the temperature 1-2h；Then furnace temperature is increased to 980-1100 DEG C, keeps the temperature 3-5h；Then with Furnace cooling is but.
Advantages of the present invention and beneficial aspects：
1. the formula of the present invention, PrNd：31-35%, Gd0.5-1%, Ga 0.05-0.15%, Zr 0.05-0.15%, B 0.8-1.6%, Co 0.2-0.5%, Al 0.1-0.4%, Cu 0.05-0.2%, Mo 0.05-0.3%, Ti 0.05- 0.3%, LaCe 0.1-0.5%, surplus Fe；The addition of Co, Cu, Al, Ti, Mo therein can obtain thinner crystal grain Tissue improves plasticity, the toughness of magnet；By adding high-melting-point element and low melting point element, low melting point element is first in intergranular Physical and chemical properties variation occurs in course of dissolution, improves the dissolubility of high-melting-point element in the liquid phase for dissolving, liquid phase, It is allowed to be uniformly distributed in intergranular region, and high-melting-point element can hinder growing up for crystal grain, crystal grain thinning, so as to make the tough of magnet Property is improved.After adding the elements such as Al, Nb, Ti in magnet, due to crystal grain refinement, obtain with higher impact toughness Sintered NdFeB magnet.In addition, the present invention rationally control PrNd contents and the content of Nd, while by adding rare earth and Zr etc. Element improves the maximum magnetic energy product of magnet entirety, and so as to reduce the usage amount of magnet, more lightweight, Costco Wholesale is low.
2. in the formula of the present invention, by control of the occupancy volume of Nd in PrNd alloys for 1-5%, Nb elements can refine Crystal grain, Nb elements solubility very little in hard magnetic phase, it is easy to form precipitation particle, crystal grain be inhibited to grow up, so as to improve magnet Impact flexibility.
3. the method for the present invention is simply easily operated, the particularly wherein control of tempering stage and temperature can effectively improve The magnetic property of product.
Specific embodiment
The present invention is described in more detail With reference to embodiment, but is not limited only to following embodiment.
Embodiment 1
The permanent-magnet material is made of each component of following weight percent：PrNd：32%, Gd1%, Ga 0.1%, Zr 0.1%, B 1%, Co0.3%, Al 0.3%, Cu 0.08%, Mo0.15%, Ti 0.1%, LaCe 0.3%, surplus Fe.
The above-mentioned PrNd of the present invention is PrNd alloys, and the occupancy volume of Nd therein is 2%.
The present invention also provides a kind of preparation method of above-mentioned Nd-Fe-B permanent magnet material, preparation process is：
(1) it matches raw material by the constituent of neodymium iron boron magnetic body and mass percent and carries out melting, after melting is complete It pours into a mould, be cooled to and get rid of strap；
(2) band obtained above that gets rid of is carried out that hydrogen is broken and airflow milling, powder is made；
(3) above-mentioned powder under inert gas shielding is put into moulding press mold plus magnetic field is orientated, after orientation Compression moulding；
(4) green compact obtained after above-mentioned molding are put into sintering furnace and be sintered at high temperature, be then tempered, obtained To neodymium iron boron magnetic body green body
The melting of step (1) of the present invention be vacuum melting, vacuum degree 0.2Pa；The thickness for getting rid of strap is 0.3mm；
Step (2) hydrogen of the present invention carries out the dehydrogenation of 4-8h after crushing, diameter of particle then is ground to 5 microns with airflow milling； Then antioxidant is added in into batch mixing in powder, it is vertical orientated in the pulsed magnetic field of 8T again after mixed to be pressed into briquet；
Being sintered in step (4) of the present invention：It is put into RVS-300 vacuum sintering furnaces and is sintered, sintering temperature 1110- 1120 DEG C, sintering time 80min；
Tempering in inventive step (4) is：1.5Pa will be evacuated in stove, then increases furnace temperature to 250-350 DEG C, protect Warm 1.5h；450-550 DEG C is then heated to, keeps the temperature 1.5h；Then furnace temperature is increased to 980-1100 DEG C, keeps the temperature 4h；Then with stove Cooling.
Embodiment 2
The permanent-magnet material is made of each component of following weight percent：PrNd：32.5%, Gd 0.70%, Ga 0.09%, Zr 0.08%, B 1.0%, Co 0.30%, Al 0.30%, Cu0.08%, Mo0.20%, Ti 0.20%, LaCe0.3%, surplus Fe.
Method is the same as embodiment 1.
Sample prepared by the present invention, performance detection
1 embodiment sample performance of table
From above-mentioned detection data it is found that the advantages of the present invention has magnetic strong and stablizes, while toughness is high.

Claims (7)

1. a kind of high-performance Ne-Fe-B permanent-magnet material, it is characterised in that：The permanent-magnet material is by each group of following weight percent It is grouped as：PrNd 31-35%, Gd0.5-1%, Ga 0.05-0.15%, Zr 0.05-0.15%, B 0.8-1.6%, Co 0.2- 0.5%, Al 0.1-0.4%, Cu 0.05-0.2%, Mo 0.05-0.3%, Ti 0.05-0.3%, LaCe 0.1-0.5%, surplus For Fe；The PrNd is PrNd alloys, and the occupancy volume of Nd therein is 1-5%.
2. high-performance Ne-Fe-B permanent-magnet material according to claim 1, it is characterised in that：The high-performance Ne-Fe-B is forever Magnetic material, the permanent-magnet material are made of each component of following weight percent：PrNd 32-34%, Gd 0.6-0.8%, Ga 0.06-0.10%, Zr 0.06-0.1%, B 0.8-1.2%, Co 0.25-0.35%, Al 0.25-0.35%, Cu 0.06- 0.10%, Mo 0.05-0.3%, Ti 0.05-0.3%, LaCe 0.1-0.5%, surplus Fe.
3. the preparation method of high-performance Ne-Fe-B permanent-magnet material according to claim 2, it is characterised in that：Preparation process For：
（1）Match raw material by the constituent and mass percent of neodymium iron boron magnetic body and carry out melting, melting completely afterwards cast, It is cooled to and gets rid of strap；
（2）The band obtained above that gets rid of is carried out that hydrogen is broken and airflow milling, powder is made；
（3）Above-mentioned powder is put under inert gas shielding in moulding press mold plus magnetic field is orientated, is suppressed after orientation Molding；
（4）The green compact obtained after above-mentioned molding are put into sintering furnace and are sintered at high temperature, is then tempered, obtains neodymium Iron boron magnet green body.
4. the preparation method of high-performance Ne-Fe-B permanent-magnet material according to claim 3, it is characterised in that：Step（1）'s Melting is vacuum melting, vacuum degree 0.05-0.2Pa；The thickness for getting rid of strap is 0.1-0.3mm.
5. the preparation method of high-performance Ne-Fe-B permanent-magnet material according to claim 3, it is characterised in that：Step（2）Hydrogen The dehydrogenation of 4-8h is carried out after broken, diameter of particle is then ground to 3-5 microns with airflow milling.
6. the preparation method of high-performance Ne-Fe-B permanent-magnet material according to claim 3, it is characterised in that：Step（4）In Be sintered to：It is put into RVS-300 vacuum sintering furnaces and is sintered, sintering temperature is 1060-1120 DEG C, sintering time 40-100min.
7. the preparation method of high-performance Ne-Fe-B permanent-magnet material according to claim 3, it is characterised in that：Step（4）In Tempering be：1-3Pa will be evacuated in stove, then increases furnace temperature to 250-350 DEG C, keep the temperature 1-2h；Then heat to 450- 550 DEG C, keep the temperature 1-2h；Then furnace temperature is increased to 980-1100 DEG C, keeps the temperature 3-5h；Then furnace cooling.
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Publication number Priority date Publication date Assignee Title
CN106158204B (en) * 2016-06-16 2018-10-02 宁波雄海稀土速凝技术有限公司 A kind of Nd-Fe-B permanent magnet material and preparation method thereof
CN106920617B (en) * 2017-03-21 2019-04-16 四川大学 High-performance Ne-Fe-B rare earth permanent-magnetic material and preparation method thereof
CN110148506A (en) * 2019-04-03 2019-08-20 宁波同创强磁材料有限公司 Widen the method for rare-earth permanent magnet sintering temperature window and the preparation method of rare-earth permanent magnet
CN110739113A (en) * 2019-10-09 2020-01-31 宁波科田磁业有限公司 high-performance sintered Nd-Fe-B material and preparation method thereof

Citations (4)

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JPH0422104A (en) * 1990-05-17 1992-01-27 Seiko Epson Corp Method of manufacturing permanent magnet
CN101552062A (en) * 2008-12-09 2009-10-07 宁波同创强磁材料有限公司 Medium-to-high grade neodymium-iron-boron magnet with composite addition of gadolinium and holmium
CN105280319A (en) * 2014-07-14 2016-01-27 中国科学院物理研究所 Rare earth iron boron material prepared from industrial pure mixed rare earth, and preparation method and application of rare earth iron boron material
CN106158204A (en) * 2016-06-16 2016-11-23 宁波雄海稀土速凝技术有限公司 A kind of Nd-Fe-B permanent magnet material and preparation method thereof

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Publication number Priority date Publication date Assignee Title
JPH0422104A (en) * 1990-05-17 1992-01-27 Seiko Epson Corp Method of manufacturing permanent magnet
CN101552062A (en) * 2008-12-09 2009-10-07 宁波同创强磁材料有限公司 Medium-to-high grade neodymium-iron-boron magnet with composite addition of gadolinium and holmium
CN105280319A (en) * 2014-07-14 2016-01-27 中国科学院物理研究所 Rare earth iron boron material prepared from industrial pure mixed rare earth, and preparation method and application of rare earth iron boron material
CN106158204A (en) * 2016-06-16 2016-11-23 宁波雄海稀土速凝技术有限公司 A kind of Nd-Fe-B permanent magnet material and preparation method thereof

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