CN108987017A - A kind of no heavy rare earth sintered NdFeB - Google Patents

A kind of no heavy rare earth sintered NdFeB Download PDF

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Publication number
CN108987017A
CN108987017A CN201810815001.XA CN201810815001A CN108987017A CN 108987017 A CN108987017 A CN 108987017A CN 201810815001 A CN201810815001 A CN 201810815001A CN 108987017 A CN108987017 A CN 108987017A
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phase alloy
rare earth
heavy rare
main
alloy
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洪群峰
韩相华
孙永阳
郝忠彬
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Zhejiang Dongyang Dmegc Rare Earth Co ltd
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Zhejiang Dongyang Dmegc Rare Earth 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
    • 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

Abstract

The present invention relates to permanent-magnet material fields, disclose a kind of no heavy rare earth sintered NdFeB, and raw material includes main-phase alloy and auxiliary phase alloy；Each element mass component is Pr in the main-phase alloyaNdbTMcFe100‑a‑b‑c‑dBd, wherein TM Nb, Al, Cu, Co, Ni, Ga, one or more of Zr；27≤a, b≤32,0≤c≤10,0.7≤d≤1.1, remaining is Fe and inevitable impurity；Each element mass component is Nd in the auxiliary phase alloymFenAlloy, m+n=1；The quality of auxiliary phase alloy is the 0.5-4wt% of main-phase alloy.The attainable magnetic property of 1 ~ 3wt% dysprosium institute is added using the neodymium iron boron magnetic body that the present invention can make neodymium iron boron magnetic body performance reach Conventional processing methods preparation in the case where not using heavy rare earth.

Description

A kind of no heavy rare earth sintered NdFeB
Technical field
The present invention relates to permanent-magnet material field more particularly to a kind of no heavy rare earth sintered NdFeBs.
Background technique
Sintered Nd-Fe-B permanent magnetic material has quite high intrinsic coercivity and magnetic for other permanent-magnet materials Energy product is therefore widely used in the fields such as electronic circuit, metallic weapon, space flight and aviation, medical machinery, and more typical has permanent magnetism Motor, loudspeaker, computer disc driver, MR imaging apparatus instrument etc..Meanwhile high performance Nd-Fe-B permanent magnet material It is used widely in modern industry and electronic technology, so that instrument and equipment be made to be intended to miniaturization, lightening and energy-saving.
Rare earth permanent magnet develops towards the high-performance direction of high-residual magnetism high-coercive force always, in order to improve the comprehensive of neodymium iron boron magnetic body Close performance, in high-performance neodymium-iron-boron magnet used at present, largely require by mix suitable heavy rare earth metal dysprosium or Person's terbium.Dy2Fe14B and Tb2Fe14The magnetocrystalline anisotropy energy of B is all much higher than Nd2Fe14B, wherein the anisotropy field of dysprosium iron boron is big About more than twice of neodymium iron boron, and terbium iron boron is four times or so.But abundance of the heavy rare earth element in the earth's crust is very low and has visited Bright reserves are very limited, and from the point of view of the exploitation situation of current rare earth, heavy rare earth is gradually intended to exhausted state, Chinese Government Also start the outlet amount for controlling rare earth consciously, heavy rare earth price is caused sharply to be promoted, aggravate the economy of enterprise significantly Burden.Therefore, in order to save heavy rare earth resource, the cost of raw material is reduced, how the heavy rare earth such as dysprosium, terbium to be not added less plus either On the basis of improve attention of the coercivity increasingly by scholar in the industry and manufacturing enterprise of neodymium iron boron magnetic body.
The preparation cost of sintered NdFeB can be saved by not adding heavy rare earth element not only, rare earth element can also be promoted to provide The reasonable utilization in source, the development healthy and stable to rare-earth trade have important practical significance.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides a kind of no heavy rare earth sintered NdFeBs, and the present invention can be not Make in the case where using heavy rare earth neodymium iron boron magnetic body performance reach Conventional processing methods preparation neodymium iron boron magnetic body addition 1~ The attainable magnetic property of 3wt% dysprosium institute.
The specific technical proposal of the invention is: a kind of no heavy rare earth sintered NdFeB, raw material include main-phase alloy and auxiliary phase Alloy.
Each element mass component is Pr in the main-phase alloyaNdbTMcFe100-a-b-c-dBd, wherein TM Nb, Al, Cu, One or more of Co, Ni, Ga, Zr；27≤a, b≤32,0≤c≤10,0.7≤d≤1.1, remaining is for Fe and unavoidably Impurity.
Each element mass component is Nd in the auxiliary phase alloymFenAlloy, m+n=1.
The quality of auxiliary phase alloy is the 0.5-4wt% of main-phase alloy.
Sintered NdFeB product in currently available technology, if not adding the heavy rare earth such as dysprosium, terbium, performance is generally poor. And the present inventor after furtheing investigate to magnetic material formula, is adjusting element in the case where not adding heavy rare earth In the case that content does not have evident regularity guiding, found out one it is small range of at present for optimal formula, make Prepared neodymium iron boron magnetic body performance of the invention can reach the neodymium iron boron magnetic body addition 1 of Conventional processing methods preparation~ The attainable magnetic property of 3wt% dysprosium institute.
In formula of the invention, although seem with similar product element species in the prior art difference be not it is very big, Be in field of magnetic material, common element be exactly it is so several, be difficult have breakthrough in the selection of new raw material at present, and The difference of magnetic material performance mostlys come from the combination of different elements and the adjustment of dosage.For a certain kind of magnetic material For performance, preferable performance can be obtained perhaps by the test of simple limited times, but to obtain a kind of synthesis The product haveing excellent performance, but there is no imagine so simple.For example, increasing a certain element in allocation process and perhaps can Coercivity is enough improved, but may but will affect remanent magnetism performance simultaneously.For at present, since element species are numerous, people are also A set of more apparent rule can not be summed up from a large number of experiments of this complexity.This is also current magnetic material major in the world The reason of material producer can not develop a high performance no heavy rare earth neodymium iron boron magnetic body product.
Specifically, Nd is added in magnet crystal boundary of the inventionmFenAuxiliary phase alloy primarily serves two kinds of effects: first, NdmFenFor amorphous phase, fusing point repairs plane defect compared with low energy, keeps crystal boundary continuous；Second, NdmFenThe smaller energy of average particle size Inhibit the abnormal growth of crystal grain.Continuously without the Grain-Boundary Phase of reunion be guarantee neodymium iron boron magnetic body have high-coercive force it is important because Element.
It should be noted that NdmFenMust be in the form of auxiliary phase alloy add, and cannot directly in main-phase alloy phase The content of Nd and Fe element should be increased, if directly added in main phase, and above-mentioned technical effect can not be played, specifically be detailed in reality Apply part case.
Preferably, the preparation method of the no heavy rare earth sintered NdFeB the following steps are included:
1) it the preparation of main-phase alloy: successively broken is made by rapid hardening furnace rejection tablet, hydrogen crushing treatment and air-flow milling；
2) it the preparation of auxiliary phase alloy: is successively made through fast quenching, high-energy ball milling；
3) mixing: main-phase alloy and auxiliary phase alloy are mixed in proportion；
4) it is orientated: the oriented moulding under magnetic field；
5) it suppresses: being pressed into blank；
4) sintering tempering.
Preferably, the average particle size of the main-phase alloy is greater than the average particle size of auxiliary phase alloy.
Preferably, the average particle size of the main-phase alloy is 2-5 μm.
Preferably, the average particle size of the auxiliary phase alloy is 0.5-1.5 μm.
Preferably, step 3) specifically comprises the processes of: Nd and Fe are placed in heating and melting in quartz ampoule according to the ratio and closed Melt, 1300~1450 DEG C of smelting temperature, argon atmospher pressure is 20kPa~30kPa；It pushes alloy molten solution by Ar gas through earthenware Crucible small hole at bottom part is ejected into high-speed rotating water cooling molybdenum roller surface, forms rapid tempering belt；Rapid tempering belt is placed in high energy ball mill again It is prepared into particle, obtains auxiliary phase alloy.
Preferably, sintering temperature is 1040~1100 DEG C, vacuum degree 10 in step 4)-1~10-5Pa, sintering time For 2-8h.
Preferably, in step 4), tempering is divided into two sections, 850~950 DEG C of the tempering temperature of first segment, the time 1~ 3h；Second segment tempering temperature is 480~550 DEG C, 3~6h of time.
In addition to needing in strict control magnet other than the ratio of each element, the preparation process control of magnet is also very crucial, excellent Magnet performance can further be promoted by changing preparation process.
It is compared with the prior art, the beneficial effects of the present invention are:
1, auxiliary phase alloy Nd is added in magnet of the present inventionmFen, primarily serve two kinds of effects: first, NdmFenFor amorphous phase, Fusing point repairs plane defect compared with low energy, keeps crystal boundary continuous；Second, NdmFenAverage particle size it is smaller can inhibit crystal grain exception it is long Greatly.It is continuously to guarantee that neodymium iron boron magnetic body has an important factor for high-coercive force without the Grain-Boundary Phase of reunion.
2, the present invention is for a set of preparation process of neodymium iron boron magnetic body product design of the invention, especially to sintering and returns Fire process conducts in-depth research, so that magnet performance is further promoted.
3, neodymium iron boron magnetic body performance can be made to reach traditional handicraft in the case where not using heavy rare earth using the method for the present invention The attainable magnetic property of neodymium iron boron magnetic body addition 1~3wt% dysprosium institute of method preparation.
Specific embodiment
The present invention will be further described with reference to the examples below.
Total embodiment
A kind of no heavy rare earth sintered NdFeB, raw material include main-phase alloy and auxiliary phase alloy.
Each element mass component is Pr in the main-phase alloyaNdbTMcFe100-a-b-c-dBd, wherein TM Nb, Al, Cu, One or more of Co, Ni, Ga, Zr；27≤a, b≤32,0≤c≤10,0.7≤d≤1.1, remaining is for Fe and unavoidably Impurity.
Each element mass component is Nd in the auxiliary phase alloymFenAlloy, m+n=1.
The quality of auxiliary phase alloy is the 0.5-4wt% of main-phase alloy.
The preparation method of the no heavy rare earth sintered NdFeB the following steps are included:
1) it the preparation of main-phase alloy: successively broken is made by rapid hardening furnace rejection tablet, hydrogen crushing treatment and air-flow milling；Main-phase alloy Average particle size is 2-5 μm.
2) preparation of auxiliary phase alloy: Nd and Fe are placed in heating and melting in quartz ampoule according to the ratio and obtain closing melt, melting temperature 1300~1450 DEG C of degree, argon atmospher pressure are 20kPa~30kPa；It pushes alloy molten solution by Ar gas through crucible bottom aperture It is ejected into high-speed rotating water cooling molybdenum roller surface, forms rapid tempering belt；Rapid tempering belt is placed in high energy ball mill again and is prepared into averagely The particle that granularity is 0.5-1.5 μm, obtains auxiliary phase alloy.
3) mixing: main-phase alloy and auxiliary phase alloy are mixed in proportion；
4) it is orientated: the oriented moulding under magnetic field；
5) it suppresses: being pressed into blank；
4) sintering tempering: sintering temperature is 1040~1100 DEG C, vacuum degree 10-1~10-5Pa, sintering time 2-8h.Tempering Processing is divided into two sections, 850~950 DEG C of the tempering temperature of first segment, 1~3h of time；Second segment tempering temperature is 480~550 DEG C, 3~6h of time.
Embodiment 1
1) main-phase alloy (Pr0.25Nd0.75)27Fe69.38Nb0.1Co1.5Cu0.15Al0.7Ga0.2B0.97Preparation: successively pass through rapid hardening Furnace rejection tablet, hydrogen crushing treatment and air-flow milling broken are made；The average particle size of main-phase alloy is 3.2 μm.
2) auxiliary phase alloy Nd0.55Fe0.45Preparation: by Nd and Fe be placed according to the ratio heating and melting in quartz ampoule obtain closing it is molten Liquid, 1350 DEG C of smelting temperature, argon atmospher pressure is 25kPa；It pushes alloy molten solution by Ar gas through crucible bottom small hole injection To high-speed rotating water cooling molybdenum roller surface, rapid tempering belt is formed；Rapid tempering belt is placed in high energy ball mill again and is prepared into average particle size For 0.9 μm of particle, auxiliary phase alloy is obtained.
3) mixing: main-phase alloy is uniformly mixed at 100: 1 in proportion with auxiliary phase alloy；
4) it is orientated: the oriented moulding under magnetic field；
5) it suppresses: being pressed into blank；
4) sintering tempering: sintering temperature is 1065 DEG C, vacuum degree 10-3Pa, sintering time 4.5h.Tempering is divided into two Section, 900 DEG C of the tempering temperature of first segment, time 2h；Second segment tempering temperature is 515 DEG C, time 4h.
Embodiment 2
1) main-phase alloy (Pr0.25Nd0.75)27Fe69.38Nb0.1Co1.5Cu0.15Al0.7Ga0.2B0.97Preparation: successively pass through rapid hardening Furnace rejection tablet, hydrogen crushing treatment and air-flow milling broken are made；The average particle size of main-phase alloy is 3.1 μm.
2) auxiliary phase alloy Nd0.6Fe0.4Preparation: by Nd and Fe be placed according to the ratio heating and melting in quartz ampoule obtain closing it is molten Liquid, 1400 DEG C of smelting temperature, argon atmospher pressure is 28kPa；It pushes alloy molten solution by Ar gas through crucible bottom small hole injection To high-speed rotating water cooling molybdenum roller surface, rapid tempering belt is formed；Rapid tempering belt is placed in high energy ball mill again and is prepared into average particle size For 0.9 μm of particle, auxiliary phase alloy is obtained.
3) mixing: main-phase alloy is uniformly mixed at 100: 2 in proportion with auxiliary phase alloy；
4) it is orientated: the oriented moulding under magnetic field；
5) it suppresses: being pressed into blank；
4) sintering tempering: sintering temperature is 1065 DEG C, vacuum degree 10-3Pa, sintering time 4h.Tempering is divided into two sections, 900 DEG C of the tempering temperature of first segment, time 2.5h；Second segment tempering temperature is 515 DEG C, time 4.5h.
Embodiment 3
1) main-phase alloy (Pr0.25Nd0.75)27Fe69.38Nb0.1Co1.5Cu0.15Al0.7Ga0.2B0.97Preparation: successively pass through rapid hardening Furnace rejection tablet, hydrogen crushing treatment and air-flow milling broken are made；The average particle size of main-phase alloy is 3.3 μm.
2) auxiliary phase alloy Nd0.65Fe0.35Preparation: by Nd and Fe be placed according to the ratio heating and melting in quartz ampoule obtain closing it is molten Liquid, 1330 DEG C of smelting temperature, argon atmospher pressure is 22kPa；It pushes alloy molten solution by Ar gas through crucible bottom small hole injection To high-speed rotating water cooling molybdenum roller surface, rapid tempering belt is formed；Rapid tempering belt is placed in high energy ball mill again and is prepared into average particle size For 0.9 μm of particle, auxiliary phase alloy is obtained.
3) mixing: main-phase alloy is uniformly mixed at 100: 3 in proportion with auxiliary phase alloy；
4) it is orientated: the oriented moulding under magnetic field；
5) it suppresses: being pressed into blank；
4) sintering tempering: sintering temperature is 1065 DEG C, vacuum degree 10-3Pa, sintering time 5h.Tempering is divided into two sections, 900 DEG C of the tempering temperature of first segment, time 2h；Second segment tempering temperature is 515 DEG C, time 5h.
Comparative example 1 (without auxiliary phase)
Prepared composition is (Pr0.25Nd0.75)27Fe69.38Nb0.1Co1.5Cu0.15Al0.7Ga0.2B0.97Magnet, using strip casting It is made, subsequent hydrogen is broken, airflow milling powder, and powder mean particle sizes are 3.2 μm.In magnetic field after oriented moulding, it is put into vacuum-sintering It is sintered respectively at 1065 DEG C in furnace, 910 DEG C × 2h+520 DEG C × 4h tempering.
The magnet performance result after sintering tempering are as follows: Br=13.6Gs, Hcj=17.3kOe, (BH) max= 45.3MOeGs。
Comparative example 2 (without auxiliary phase, directly improves Nd and Fe ratio) in main phase
Prepared composition is Pr6.75Nd21.25Fe68.38Nb0.1Co1.5Cu0.15Al0.7Ga0.2B0.97Magnet, using strip casting system , subsequent hydrogen is broken, and in airflow milling powder, powder mean particle sizes are 3.2 μm.In magnetic field after oriented moulding, it is put into vacuum-sintering It is sintered respectively at 1065 DEG C in furnace, 910 DEG C × 2h+520 DEG C × 4h tempering.
The magnet performance result after sintering tempering are as follows: Br=13.4Gs, Hcj=17.6kOe, (BH) max= 43.3MOeGs。
Comparative example 3 (is added with heavy rare earth Dy)
Prepared composition is (Pr0.25Nd0.75)27Fe68.38Dy1Nb0.1Co1.5Cu0.15Al0.7Ga0.2B0.97Magnet, using rapid hardening work Skill is made, and subsequent hydrogen is broken, airflow milling powder, and powder mean particle sizes are 3.1 μm.In magnetic field after oriented moulding, it is put into vacuum burning Respectively in 1065 DEG C of vacuum-sintering 4h, 910 DEG C × 2h+520 DEG C × 4h temperings in freezing of a furnace.
The magnet performance result after sintering tempering are as follows: Br=13.3Gs, Hcj=18.3kOe, (BH) max= 43.2MOeGs。
Comparative example 4 (is added with heavy rare earth Dy)
Prepared composition is (Pr0.25Nd0.75)27Fe67.38Dy2Nb0.1Co1.5Cu0.15Al0.7Ga0.2B0.97Magnet, using rapid hardening work Skill is made, and subsequent hydrogen is broken, airflow milling powder, and powder mean particle sizes are 3.1 μm.In magnetic field after oriented moulding, it is put into vacuum burning Respectively in 1065 DEG C of vacuum-sintering 4h, 910 DEG C × 2h+520 DEG C × 4h temperings in freezing of a furnace.
The magnet performance result after sintering tempering are as follows: Br=13.1Gs, Hcj=20.3kOe, (BH) max= 41.8MOeGs。
Performance comparison
The magnetic property control of magnet obtained by table 1, each embodiment and comparative example
Performance indicator Br(kGs) Hcj(kOe) (BH)m(MGOe)
Comparative example 1 13.6 17.3 45.3
Comparative example 2 13.4 17.6 43.3
Comparative example 3 13.3 18.3 43.2
Comparative example 4 13.1 20.3 41.8
Embodiment 1 13.54 19.7 45.2
Embodiment 2 13.52 20.8 44.9
Embodiment 3 13.48 20.6 44.7
By upper table data comparison it is found that producing (comparative example 1) without heavy rare earth method using conventional, when remanent magnetism reaches 13.6kGs, rectify Stupid power 17.3kOe.(comparative example 2) coercivity slightly promotes (17.6kOe) after adding a certain amount of Nd in fusion process, but surplus Magnetic reduces (13.4kGs).Remanent magnetism reduces while Dy (the comparative example 3 and 4) coercivity of addition 1% and 2% is promoted in melting It is more.And after using method addition NdFe alloy of the invention, remanent magnetism reaches 13.52kGs, coercivity 20.8kOe, in remanent magnetism base Coercivity improves 3kOe under the premise of this is undiminished.Therefore, NdmFenMust be added in the form of auxiliary phase alloy, without It can directly increase accordingly the content of Nd and Fe element in main-phase alloy, if directly added in main phase, and can not play State technical effect.
Raw materials used in the present invention, equipment is unless otherwise noted the common raw material, equipment of this field；In the present invention Method therefor is unless otherwise noted the conventional method of this field.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way, it is all according to the present invention Technical spirit any simple modification, change and equivalent transformation to the above embodiments, still fall within the technology of the present invention side The protection scope of case.

Claims (8)

1. a kind of no heavy rare earth sintered NdFeB, which is characterized in that raw material includes main-phase alloy and auxiliary phase alloy；
Each element mass component is Pr in the main-phase alloyaNdbTMcFe100-a-b-c-dBd, wherein TM Nb, Al, Cu, Co, One or more of Ni, Ga, Zr；27≤a, b≤32,0≤c≤10,0.7≤d≤1.1, remaining is for Fe and inevitably Impurity；
Each element mass component is Nd in the auxiliary phase alloymFenAlloy, m+n=1；
The quality of auxiliary phase alloy is the 0.5-4wt% of main-phase alloy.
2. a kind of no heavy rare earth sintered NdFeB as described in claim 1, which is characterized in that preparation method includes following step It is rapid:
1) it the preparation of main-phase alloy: successively broken is made by rapid hardening furnace rejection tablet, hydrogen crushing treatment and air-flow milling；
2) it the preparation of auxiliary phase alloy: is successively made through fast quenching, high-energy ball milling；
3) mixing: main-phase alloy and auxiliary phase alloy are mixed in proportion；
4) it is orientated: the oriented moulding under magnetic field；
5) it suppresses: being pressed into blank；
4) sintering tempering.
3. a kind of no heavy rare earth sintered NdFeB as claimed in claim 2, which is characterized in that the average grain of the main-phase alloy Degree is greater than the average particle size of auxiliary phase alloy.
4. a kind of no heavy rare earth sintered NdFeB as claimed in claim 3, which is characterized in that the average grain of the main-phase alloy Degree is 2-5 μm.
5. a kind of no heavy rare earth sintered NdFeB as claimed in claim 4, which is characterized in that the average grain of the auxiliary phase alloy Degree is 0.5-1.5 μm.
6. a kind of no heavy rare earth sintered NdFeB as claimed in claim 2, which is characterized in that step 3) specifically comprises the processes of: Nd and Fe are placed in heating and melting in quartz ampoule according to the ratio to obtain closing melt, 1300 ~ 1450 DEG C of smelting temperature, argon atmospher pressure is 20kPa~30kPa；It pushes alloy molten solution by Ar gas through crucible bottom small hole injection to high-speed rotating water cooling molybdenum roller surface, Form rapid tempering belt；Rapid tempering belt is placed in high energy ball mill again and is prepared into particle, obtains auxiliary phase alloy.
7. a kind of no heavy rare earth sintered NdFeB as claimed in claim 2, which is characterized in that in step 4), sintering temperature is 1040 ~ 1100 DEG C, vacuum degree 10-1~10-5Pa, sintering time 2-8h.
8. a kind of no heavy rare earth sintered NdFeB as described in claim 2 or 6, which is characterized in that in step 4), tempering It is divided into two sections, 850 ~ 950 DEG C of the tempering temperature of first segment, 1 ~ 3h of time；Second segment tempering temperature is 480 ~ 550 DEG C, the time 3 ~ 6h。
CN201810815001.XA 2018-07-23 2018-07-23 A kind of no heavy rare earth sintered NdFeB Pending CN108987017A (en)

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Application publication date: 20181211