CN110021467A - A kind of preparation method of Sintered NdFeB magnet - Google Patents

A kind of preparation method of Sintered NdFeB magnet Download PDF

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Publication number
CN110021467A
CN110021467A CN201810022371.8A CN201810022371A CN110021467A CN 110021467 A CN110021467 A CN 110021467A CN 201810022371 A CN201810022371 A CN 201810022371A CN 110021467 A CN110021467 A CN 110021467A
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rare earth
heavy rare
magnetic powder
magnet
sintered ndfeb
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张秋爽
郭帅
闫阿儒
陈仁杰
曹学静
丁广飞
杨潇
曾基灵
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Ningbo Institute of Material Technology and Engineering of CAS
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Ningbo Institute of Material Technology and Engineering of CAS
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/002Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/005Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/06Ferrous alloys, e.g. steel alloys containing aluminium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/10Ferrous alloys, e.g. steel alloys containing cobalt
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/12Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/16Ferrous alloys, e.g. steel alloys containing copper
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets 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
    • H01F1/04Magnets 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
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571Alloys 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
    • H01F1/0575Alloys 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
    • H01F1/0577Alloys 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus 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
    • H01F41/02Apparatus 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
    • H01F41/0253Apparatus 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
    • H01F41/0293Apparatus 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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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Power Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Hard Magnetic Materials (AREA)

Abstract

The invention discloses a kind of preparation methods of Sintered NdFeB magnet, using solution cladding process, by alloy magnetic powder with containing heavy rare earth element organic suspension or organic solution mix, it is evenly coated at heavy rare earth element around magnetic powder particle, then it formed, be sintered tempering, heavy rare earth element is effectively controlled Grain Surface and crystal boundary, can be improved heavy rare earth element in Sintered NdFeB magnet be evenly distributed and diffusion depth, be conducive to improve the magnetic properties such as coercivity.

Description

A kind of preparation method of Sintered NdFeB magnet
Technical field
The present invention relates to the sintering technology fields of rare-earth permanent magnet, more particularly to a kind of preparation of Sintered NdFeB magnet Method.
Background technique
Sintered NdFeB rear-earth permanent magnet be up to the present it is found that magnetic energy product highest, most widely used permanent magnetism material Material.To meet new-energy automobile and wind-power electricity generation to the market demand of high performance magnet, Sintered NdFeB magnet is in market segment Application further expansion.The raising of coercivity and magnetic energy product has pushed sintered permanent magnet being skyrocketed through in motor market.
It is a kind of raising magnet coercive that current people generally study that heavy rare earth element is added in Sintered NdFeB magnet The method of power and magnetic energy product.The technological means of addition includes: molten alloy method, dual alloy method, grain boundary decision method.In recent years, brilliant Boundary's diffusion method significantly improves coercivity because it is not in the case where influencing remanent magnetism, it is considered to be state-of-the art efficient using heavy The effective ways of rare earth.
Grain boundary decision method refer to magnet surface deposit heavy rare earth compound, after heat treatment, make heavy rare earth element along Grain boundary decision is to the intracorporal method of magnetic.Heavy rare earth element is mainly distributed on crystal boundary and Grain Surface, and the heavy rare earth of intra-die Content is low, forms the shell structurre of high magnetocrystalline anisotropy field, so that coercivity is substantially improved and does not lose remanent magnetism, also very great Cheng The utilization rate of heavy rare earth is improved on degree.
Common grain boundary decision method has magnetron sputtering, surface coating, electrophoretic deposition.But these grain boundary decision methods are all only It is to be carried out on magnet surface layer, diffusion depth is limited, and the general thickness for spreading magnet is no more than 6mm, and diffusion depth is no more than 500 μ m.In addition, there is also magnetic powder the problem of being unevenly distributed with heavy rare earth element easy to reunite for existing method.Therefore, it is dilute how to improve weight The distributing homogeneity and grain boundary decision depth of earth elements are current research hotspots.
Summary of the invention
Status in view of the above technology, the present invention provides a kind of preparation methods of Sintered NdFeB magnet, using solution packet Cover method, by alloy magnetic powder with containing heavy rare earth element organic suspension or organic solution mix, coat heavy rare earth element uniformly Around magnetic powder particle, forming, sintering and tempering processing is then carried out, can be improved heavy rare earth element in Sintered NdFeB magnet Be evenly distributed and diffusion depth, be conducive to the raising of magnetic property.
That is, the technical solution of the present invention is as follows: a kind of preparation method of Sintered NdFeB magnet, includes the following steps:
The molecular formula Nd of neodymium iron boron magnetic bodyaMbFe100-a-b-cBc, wherein a, b, c represent the mass fraction of each corresponding element, and And one of 20≤a≤33,0≤b≤10,0.8≤c≤1, M La, Ce, Pr, Dy, Tb, Ga, Co, Cu, Al, Nb element or It is several;It is broken with after airflow milling through hydrogen according to the molecular formula preparing metal raw material and mixed smelting of neodymium iron boron magnetic body, obtain alloy magnetic Powder;
Organic compound containing heavy rare earth metal or halide are mixed with organic solvent, obtain organic suspension or molten Liquid, wherein the quality of heavy rare earth metal accounts for the mass percent of the alloy magnetic powder less than 10%;
The alloy magnetic powder is uniformly mixed with organic suspension or solution, and under vacuum or inert gas shielding, So that organic solvent is volatilized completely, obtains mixing magnetic powder;
The mixing magnetic powder is subjected to magnetic field orientating and is pressed into blank magnet;
Blank magnet is put into vacuum sintering furnace and is sintered, is then quickly cooled down, is carried out at second annealing heat later Reason.
As a kind of implementation, the sintering process are as follows: be warming up to blank magnet with 5 DEG C/min-30 DEG C/min 300 DEG C -400 DEG C, and -3 hours 1 hour are kept the temperature, 500 DEG C -650 DEG C are then heated to, and keep the temperature -3 hours 1 hour, Zhi Housheng Temperature keeps the temperature -3 hours 1 hour to 700 DEG C -850 DEG C, is finally warming up to 900-1090 DEG C and is sintered -6 hours 1 hour.
Preferably, the secondary tempering heat treatment are as follows: keep the temperature -3 hours 1 hour at 850 DEG C -950 DEG C first, then It is filled with argon gas and is cooled to room temperature fastly, then be warming up to 450 DEG C -580 DEG C and keep the temperature -3 hours 1 hour.
Organic compound containing heavy rare earth element, shared weight ratio are 0.1-10%.
The organic solvent includes formic acid, ether, tributyl phosphate, acetone, benzene, toluene, ethyl alcohol, propyl alcohol, isopropanol, just One or more of hexane, dioxane and tetrahydrofuran etc., wherein acetone, ether, propyl alcohol, isopropanol, ethyl alcohol are all AR It analyzes pure.
Preferably, the quality of suspension or solution accounts for when the alloy magnetic powder is mixed with organic suspension or solution The quality of alloy magnetic powder is greater than 10%.
Preferably, the quality of the heavy rare earth organic compound accounts for the 0.1%- of suspension or solution quality 90.0%, the quality of the heavy rare earth organohalogen compounds accounts for the 0.1%-90.0% of suspension or solution quality.
Preferably, the mass fraction of Al is 0.2~3.0 in the molecular formula of the neodymium iron boron magnetic body, Co, Nb and Ga member The mass fraction that the mass fraction of element is 0.2~4.0, Cu is 0.1~6.0.
The heavy rare earth metal include gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), One of lutetium (Lu) and yttrium (Y) etc. are several.
Compared with prior art, the invention has the following advantages:
(1) heavy rare earth compound is distributed in organic solvent, is uniformly mixed after suspension or solution is made with magnetic powder, so that Heavy rare earth element can be equably coated to around magnetic powder particle, effectively inhibited magnetic powder to reunite and asked with what heavy rare earth was unevenly distributed Topic.
(2) compared with traditional grain boundary decision method, solution cladding process can not only guarantee heavy rare earth organic compound point The heavy rare earth product overwhelming majority after solution is located at grain boundaries, is effectively formed the heavy rare earth shell with high magnetocrystalline anisotropy, subtracts Magnetization coupling between small main phase grain, and may also be ensured that around each crystal grain there is heavy rare earth element package, favorably In heavy rare earth element during the sintering process using liquid phase crystal boundary as diffusion admittance, it is uniformly dispersed in Grain Surface and crystal boundary, is dashed forward The size limitation for having broken grain boundary decision solves the problems, such as that heavy rare earth element is only spread in magnet surface shallow-layer.
Detailed description of the invention
Fig. 1 is the backscatter images and each element mapping of the magnetic powder in embodiment 1 using the preparation of solution cladding process;
Fig. 2 is the demagnetizing curve of embodiment 1 with Sintered NdFeB magnet obtained in comparative example 1;
Fig. 3 is the demagnetizing curve of embodiment 2 with Sintered NdFeB magnet obtained in comparative example 2.
Specific embodiment
Below with reference to embodiment, present invention is further described in detail, it should be pointed out that embodiment described below purport It is being convenient for the understanding of the present invention, and is not playing any restriction effect to it.
Embodiment 1:
In the present embodiment, the preparation process of Sintered NdFeB magnet is as follows:
(1) neodymium iron boron Nd rapid hardening: is prepared using raw material mixed smelting, copper roller casting33FebalB0.95Cu0.2Rapid-hardening flake, copper roller Revolving speed about 1.4m/s, resulting rapid-hardening flake thickness are 300 μm or so.
(2) powder processed: rapid-hardening flake hydrogen is broked into the neodymium iron boron alloy powder that average grain diameter is 0.1mm-1mm, then uses powder Hydrogen breaks technique and the magnetic powder that average grain diameter is about 2.0 μm is made.
(3) mixing: heavy rare earth organic compound is dissolved in organic solvent, and ultrasonic disperse, obtains mixture.Heavy rare earth Organic compound is isopropanol dysprosium, and organic solvent is dehydrated alcohol.Then mixture is mixed with magnetic powder made from step (2), It stirs evenly, wherein heavy rare earth organic compound accounts for the 2.1% of magnetic powder total weight, under vacuum or inert gas shielding, makes Organic solvent volatilization is complete.
In Fig. 1, upper row from left to right the first width figure be the magnetic powder obtained after above-mentioned processing back scattering figure, remaining five width figure is The mapping of each element scanned through energy disperse spectroscopy.It will be seen from figure 1 that each element is evenly coated at around magnetic powder, it is brilliant Grain surface layer and this structure of crystal boundary enrichment heavy rare earth member be conducive to during the sintering process heavy rare earth element using liquid phase crystal boundary as Diffusion admittance is uniformly dispersed in Grain Surface and crystal boundary, breaks through the size limitation of grain boundary decision.
(4) form: the magnetic powder that step (3) is obtained magnetic field orientating in forming press forms, and blank is made.Vacuum sealing Afterwards, blank is compacted using cold isostatic press, to further increase green density.
(5) it is sintered: the blank magnet that step (4) obtains is placed in vacuum sintering furnace, under vacuum conditions (< 10-1Pa), 320 DEG C are warming up to 10 DEG C/min, and keeps the temperature 2 hours, guarantees remaining organic solvent volatilization completely, heavy rare earth organic compound It decomposes completely and product is made to be detached from magnet.It then heats to 580 DEG C and keeps the temperature 2 hours, it is ensured that dehydrogenation is complete.Then 800 are warming up to DEG C heat preservation 2 hours, be warming up to later 1045 DEG C be sintered 2 hours.Argon gas is finally passed through to be rapidly cooled.
(6) it is tempered: the magnet temperature that step (5) obtains being risen into 900 DEG C of progress level-one tempering first, keep the temperature 2 hours;So After be passed through argon gas rapid cooling.Then it is warming up to 500 DEG C of progress second annealings again and keeps the temperature 2 hours, obtains Sintered NdFeB magnet.
Comparing embodiment 1:
In the present embodiment, the preparation process of Sintered NdFeB magnet is substantially the same manner as Example 1, the difference is that this reality It applies and does not add heavy rare earth organic compound in example, prepare base magnet, specific preparation process is as follows:
(1) neodymium iron boron Nd rapid hardening: is prepared using raw material mixed smelting, copper roller casting33FebalB0.95Cu0.2Rapid-hardening flake, copper roller Revolving speed about 1.4m/s, resulting rapid-hardening flake thickness are 300 μm or so.
(2) powder processed: rapid-hardening flake hydrogen is broked into the neodymium iron boron alloy powder that average grain diameter is 0.1mm-1mm, then uses powder Hydrogen breaks technique and the magnetic powder that average grain diameter is about 2.0 μm is made.
(3) form: the magnetic powder that step (2) is obtained magnetic field orientating in forming press forms, and blank is made.Vacuum sealing Afterwards, blank is compacted using cold isostatic press, to further increase green density.
(4) it is sintered: the blank magnet that step (3) obtains is placed in vacuum sintering furnace, under vacuum conditions (< 10-1Pa), 320 DEG C are warming up to 10 DEG C/min, and keeps the temperature 2 hours, guarantees remaining organic solvent volatilization completely, heavy rare earth organic compound It decomposes completely and product is made to be detached from magnet.It then heats to 580 DEG C and keeps the temperature 2 hours, it is ensured that dehydrogenation is complete.Then 800 are warming up to DEG C heat preservation 2 hours, be warming up to later 1045 DEG C be sintered 2 hours.Argon gas is finally passed through to be rapidly cooled.
(5) it is tempered: the magnet temperature that step (4) obtains being risen into 900 DEG C of progress level-one tempering first, keep the temperature 2 hours;So After be passed through argon gas rapid cooling.Then it is warming up to 500 DEG C of progress second annealings again and keeps the temperature 2 hours, obtains Sintered NdFeB magnet.
Above-described embodiment 1 is obtained with magnet sample obtained in comparative example 1 by wire cutting and machine toolingCylinder.The remanent magnetism, coercivity and magnetic energy product of both samples are tested using magnetic property measuring instrument, Fig. 2 is to obtain Demagnetizing curve, it can be seen that compared with comparative example 1, in embodiment 1 add heavy rare earth organic compound, magnet rectify Stupid power enhancing, and there is no deteriorate because of heavy rare earth diffusion for squareness.Specific magnetic property comparing result such as table 1.
Table 1
Embodiment 2:
In the present embodiment, the preparation process of Sintered NdFeB magnet is as follows:
(1) neodymium iron boron (Pr rapid hardening: is prepared using raw material mixed smelting, copper roller casting0.2Nd0.8)30.5Al0.2Cu0.04FebalB1Rapid-hardening flake, copper roller revolving speed about 1.4m/s, 300 μm or so of resulting rapid-hardening flake thickness.
(2) powder processed: rapid-hardening flake hydrogen is broked into the neodymium iron boron alloy powder that average grain diameter is less than 1mm, then breaks powder with hydrogen The powder that average grain diameter is about 3 μm is made in technique.
(3) mixing: under anhydrous and oxygen-free environment, heavy rare earth halide being dissolved in organic solvent, and obtaining concentration is 2g/L's Solution.Heavy rare earth halide is terbium chloride, and organic solvent is dehydrated alcohol.Then magnetic powder made from solution and step (2) is mixed It closes, ultrasonic disperse is uniform, and wherein heavy rare earth halide accounts for the .0.33% of magnetic powder total weight, in vacuum or inert gas shielding Under, keep solvent volatilization complete.
The back scattering figure of the magnetic powder obtained after above-mentioned processing, and the EDS maps of each element scanned through energy disperse spectroscopy Scheme it is similar to Figure 1, display each element be evenly coated at around magnetic powder, this structure be conducive to during the sintering process heavy rare earth member Element is uniformly dispersed in entire magnet using liquid phase crystal boundary as diffusion admittance, breaks through the size limitation of grain boundary decision.
(4) form: blank is made in the magnetic powder that step (3) is obtained oriented moulding in forming press.After vacuum sealing, benefit Blank is compacted with cold isostatic press, to further increase green density.
(5) it is sintered: the blank magnet that step (4) obtains is placed in vacuum sintering furnace, under vacuum conditions (< 10-1Pa), 320 DEG C are warming up to 10 DEG C/min, and keeps the temperature 2 hours, guarantees that residual organic solvent volatilization is complete.Then heat to 580 DEG C of guarantors Temperature 2 hours, it is ensured that dehydrogenation is complete.Then 800 DEG C are warming up to and keeps the temperature 2 hours, 1050 DEG C is warming up to later and is sintered 2 hours.Finally Argon gas is passed through to be rapidly cooled.
(6) it is tempered: the magnet temperature that step (5) obtains being risen into 900 DEG C of progress level-one tempering first, keep the temperature 2 hours;So After be passed through argon gas rapid cooling.Then 500 DEG C of progress second annealings are warming up to and keep the temperature 2 hours, obtain Sintered NdFeB magnet.
Comparing embodiment 2:
In the present embodiment, the preparation process of Sintered NdFeB magnet is substantially the same manner as Example 2, the difference is that this reality It applies and does not add heavy rare earth compound in example, prepare base magnet, specific preparation process is as follows:
(1) neodymium iron boron (Pr rapid hardening: is prepared using raw material mixed smelting, copper roller casting0.2Nd0.8)30.5Al0.2Cu0.04FebalB1Rapid-hardening flake, copper roller revolving speed about 1.4m/s, 300 μm or so of resulting rapid-hardening flake thickness.
(2) powder processed: rapid-hardening flake hydrogen is broked into the neodymium iron boron alloy powder that average grain diameter is less than 1mm, then breaks powder with hydrogen The powder that average grain diameter is about 3 μm is made in technique.
(3) form: blank is made in the magnetic powder that step (2) is obtained oriented moulding in forming press.After vacuum sealing, benefit Blank is compacted with cold isostatic press, to further increase green density.
(4) it is sintered: the blank magnet that step (3) obtains is placed in vacuum sintering furnace, under vacuum conditions (< 10-1Pa), 320 DEG C are warming up to 10 DEG C/min, and keeps the temperature 2 hours, guarantees that residual organic solvent volatilization is complete.Then heat to 580 DEG C of guarantors Temperature 2 hours, it is ensured that dehydrogenation is complete.Then 800 DEG C are warming up to and keeps the temperature 2 hours, 1050 DEG C is warming up to later and is sintered 2 hours.Finally Argon gas is passed through to be rapidly cooled.
(5) it is tempered: the magnet temperature that step (4) obtains being risen into 900 DEG C of progress level-one tempering first, keep the temperature 2 hours;So After be passed through argon gas rapid cooling.Then 500 DEG C of progress second annealings are warming up to and keep the temperature 2 hours, obtain Sintered NdFeB magnet.
Above-described embodiment 1 is obtained with magnet sample obtained in comparative example 1 by wire cutting and machine toolingCylinder.Using magnetic property measuring instrument test both samples room temperature magnetic property and different temperatures under obtain As shown in table 2, the demagnetization that Fig. 3 is is bent for residual magnetism temperature coefficient and coercive force temperature coefficient (25 DEG C -100 DEG C of temperature range) Line.As can be seen that the magnet coercivity promotion for being added to heavy rare earth halide in embodiment 2 is bright compared with comparative example 2 It is aobvious, and remanent magnetism has almost no change, while still remain high squareness.
Table 2
Technical solution of the present invention is described in detail in embodiment described above, it should be understood that the above is only For specific embodiments of the present invention, it is not intended to restrict the invention, all any modifications made in spirit of the invention, Supplement or similar fashion substitution etc., should all be included in the protection scope of the present invention.

Claims (8)

1. a kind of preparation method of Sintered NdFeB magnet, it is characterized in that: including the following steps:
The molecular formula Nd of neodymium iron boron magnetic bodyaMbFe100-a-b-cBc, wherein a, b, c represent the mass fraction of each corresponding element, and 20 ≤ a≤33,0≤b≤10,0.8≤c≤1, one of M La, Ce, Pr, Dy, Tb, Ga, Co, Cu, Al, Nb element or several Kind;It is broken with after airflow milling through hydrogen according to the molecular formula preparing metal raw material and mixed smelting of neodymium iron boron magnetic body, obtain alloy magnetic Powder;
Organic compound containing heavy rare earth metal or halide are mixed with organic solvent, obtain organic suspension or solution, Wherein the quality of heavy rare earth metal accounts for the mass percent of the alloy magnetic powder less than 10%;
The alloy magnetic powder is uniformly mixed with organic suspension or solution, and under vacuum or inert gas shielding, makes to have Solvent is volatilized completely, obtains mixing magnetic powder;
The mixing magnetic powder is subjected to magnetic field orientating and is pressed into blank magnet;
Blank magnet is put into vacuum sintering furnace and is sintered, is then quickly cooled down, carries out secondary tempering heat treatment later.
2. the preparation method of Sintered NdFeB magnet as described in claim 1, it is characterized in that: the sintering process are as follows: will Blank magnet is warming up to 300 DEG C -400 DEG C with 5 DEG C/min-30 DEG C/min, and keeps the temperature -3 hours 1 hour, then heats to 500 DEG C -650 DEG C, and -3 hours 1 hour are kept the temperature, it is warming up to 700 DEG C -850 DEG C later, and keep the temperature -3 hours 1 hour, is finally warming up to 900-1090 DEG C is sintered -6 hours 1 hour.
3. the preparation method of Sintered NdFeB magnet as described in claim 1, it is characterized in that: the secondary tempering heat treatment Are as follows: -3 hours 1 hour are kept the temperature at 850 DEG C -950 DEG C first, argon gas is then charged with and is cooled to room temperature fastly, then be warming up to 450 DEG C -580 DEG C heat preservation -3 hours 1 hour.
4. the preparation method of Sintered NdFeB magnet as described in claim 1, it is characterized in that: containing the organic of heavy rare earth element In compound or halide, the mass percentage of heavy rare earth element is 10-90%.
5. the preparation method of Sintered NdFeB magnet as described in claim 1, it is characterized in that: the alloy magnetic powder with it is organic When suspension or solution mix, the quality of suspension or solution accounts for alloy magnetic powder quality greater than 50%.
6. the preparation method of Sintered NdFeB magnet as described in claim 1, it is characterized in that: the heavy rare earth organic compound The quality of object accounts for the 0.1%-90.0% of suspension or solution quality;The quality of the heavy rare earth organohalogen compounds accounts for suspension Or the 0.1%-90.0% of solution quality.
7. the preparation method of the Sintered NdFeB magnet as described in any claim in claim 1 to 6, it is characterized in that: institute The organic solvent stated includes formic acid, ether, tributyl phosphate, acetone, benzene, toluene, ethyl alcohol, propyl alcohol, isopropanol, n-hexane, dioxy One or more of six rings and tetrahydrofuran etc..
8. the preparation method of the Sintered NdFeB magnet as described in any claim in claim 1 to 6, it is characterized in that: institute The heavy rare earth metal stated includes one of gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium or several.
CN201810022371.8A 2018-01-10 2018-01-10 A kind of preparation method of Sintered NdFeB magnet Pending CN110021467A (en)

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Cited By (6)

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CN115020058A (en) * 2022-08-05 2022-09-06 京磁材料科技股份有限公司 Low-cost double-low-temperature-coefficient rare earth permanent magnet and preparation method thereof

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CN110473685A (en) * 2019-08-27 2019-11-19 安徽省瀚海新材料股份有限公司 A method of neodymium iron boron magnetic body is prepared using rare earth alloy modification
CN110473685B (en) * 2019-08-27 2020-09-11 安徽省瀚海新材料股份有限公司 Method for preparing neodymium-iron-boron magnet by modifying rare earth alloy
EP3827916A1 (en) 2019-11-28 2021-06-02 Yantai Shougang Magnetic Materials Inc. A manufacturing method of sintered nd-fe-b permanent magnet
CN111029074A (en) * 2019-12-30 2020-04-17 江西师范大学 Preparation method of sintered rare earth iron boron permanent magnet material for regulating grain boundary
CN111029074B (en) * 2019-12-30 2022-05-17 江西师范大学 Preparation method of sintered rare earth iron boron permanent magnet material for regulating grain boundary
CN111613404A (en) * 2020-06-01 2020-09-01 福建省长汀金龙稀土有限公司 Neodymium-iron-boron magnet material, raw material composition, preparation method and application thereof
CN111968819A (en) * 2020-09-09 2020-11-20 宁波科田磁业有限公司 Low-heavy rare earth high-performance sintered neodymium-iron-boron magnet and preparation method thereof
CN115020058A (en) * 2022-08-05 2022-09-06 京磁材料科技股份有限公司 Low-cost double-low-temperature-coefficient rare earth permanent magnet and preparation method thereof

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