CN107026002B - The preparation method of Nd Fe B alloys magnet - Google Patents

The preparation method of Nd Fe B alloys magnet Download PDF

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CN107026002B
CN107026002B CN201710245116.5A CN201710245116A CN107026002B CN 107026002 B CN107026002 B CN 107026002B CN 201710245116 A CN201710245116 A CN 201710245116A CN 107026002 B CN107026002 B CN 107026002B
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hydrogen
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CN107026002A (en
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冯招娣
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System In Beijing Jing Magnetoelectricity Work Science And Technology Ltd
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System In Beijing Jing Magnetoelectricity Work Science And Technology Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
    • C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • 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

Abstract

The present invention provides a kind of preparation method of Nd Fe B alloys magnet comprising following steps：The quick-fried powder of master alloying hydrogen and the auxiliary quick-fried powder of alloy hydrogen is made in Nd Fe B alloys magnet sintering raw material respectively；Nd Fe B alloys magnet is made after the quick-fried powder of master alloying hydrogen obtained and the quick-fried powder of auxiliary alloy hydrogen are mixed, wherein the auxiliary quick-fried powder of alloy hydrogen includes Ce；The quality of the auxiliary quick-fried powder of alloy hydrogen is no more than the 10% of the quality of the quick-fried powder of master alloying hydrogen.The Sintered NdFeB magnet of the present invention is mixed with alloying element can be with crystal grain thinning, and replace part Nd using Ce is added in dual alloy normal direction NdFeB material, the consumption for reducing Nd, Dy while obtaining preferable magnetic property greatly reduces the production cost of material, has widened the application field of Ce.

Description

The preparation method of Nd Fe B alloys magnet
Technical field
The invention belongs to magnet preparation field more particularly to a kind of preparation methods of Nd Fe B alloys magnet.
Background technology
Its chemical formula of neodymium iron boron magnetic body is Nd2Fe14B is a kind of artificial permanent magnet, and is had so far most strong The permanent magnet of magnetic force, maximum magnetic energy product (BH) max exceed 10 times of ferrite or more, and in the state of naked magnetic, magnetic force can Reach 3500 Gauss.The advantages of neodymium iron boron magnetic body is cost-effective, small, light-weight, good mechanical property and magnetic The advantages of the features such as property is strong, such high-energy density, makes Nd-Fe-B permanent magnet material be obtained in modern industry and electronic technology extensively General application is known as magnetic king in magnetics circle.Thus, the coke that the preparation of neodymium iron boron magnetic body and extension always give more sustained attention in the industry Point.
Neodymium iron boron magnetic body can be divided into Sintered NdFeB magnet and Agglutinate neodymium-iron-boron magnet, and Sintered NdFeB magnet is current The best permanent-magnet material of magnetic property, is most widely used.But for sintered Nd-Fe-B permanent magnet, there is also corrosion-resistant The defects of performance is poor, mechanical property is not good enough.In the microstructure of sintered NdFeB magnet, rich-Nd phase is to magnetic hardening lifting It acts on, crackle is easy to extend in crystal boundary rich-Nd phase, therefore the mechanical property that improve sintered NdFeB magnet must just improve The obdurability of Grain-Boundary Phase richness Nd.Alloying element is added to prevent or change crack propagation approach with crystal grain thinning, improve NdFeB The processing toughness of magnet.Traditional alloying gimmick is that alloying element is added before melting, is improving magnet strength and toughness Meanwhile it is often bigger to the negative effect of the remanent magnetism of neodymium iron boron magnetic body and magnetic energy product.
With Sintered NdFeB magnet commercial performance be continuously improved, application field is more and more wider, make rare earth metal Nd, The double growth of demand of Pr, Dy and Tb.On the one hand the development for promoting rare earth raw material industry, also results in but then Rare earth resources use imbalance.The overstocked rare earth such as La, Ce how is made full use of, is saved while obtaining preferable magnetic property The resource values such as Dy, Tb obtain perpend.
Invention content
To solve the above problems, the present invention provides a kind of preparation method of Nd Fe B alloys magnet comprising following steps：
The quick-fried powder of master alloying hydrogen and the auxiliary quick-fried powder of alloy hydrogen is made in Nd Fe B alloys magnet sintering raw material respectively；
Nd Fe B alloys magnet is made after the quick-fried powder of master alloying hydrogen obtained and the quick-fried powder of auxiliary alloy hydrogen are mixed, wherein
The auxiliary quick-fried powder of alloy hydrogen includes Ce；
The quality of the auxiliary quick-fried powder of alloy hydrogen is no more than the 10% of the quality of the quick-fried powder of master alloying hydrogen.
Preferably, in the preparation method of the Nd Fe B alloys magnet,
The NbFeB sintered raw material include purity be 99.5% neodymium metal, metal dysprosium, metallic aluminium, pure iron, Ce with And the ferro-boron of boracic mass fraction 19.5%.
Preferably, in the preparation method of the Nd Fe B alloys magnet, the NbFeB sintered raw material are made Master alloying slab and auxiliary alloy casting piece,
The master alloying slab and the auxiliary alloy casting piece are subjected to hydrogen respectively and break the obtained master alloying of airflow milling processing The quick-fried powder of hydrogen and the auxiliary quick-fried powder of alloy hydrogen；
The quick-fried powder of the master alloying hydrogen and the quick-fried powder of the auxiliary alloy hydrogen are mixed to be placed under nitrogen protection, neodymium iron boron conjunction is made Golden magnet green compact；
The Nd Fe B alloys magnet green compact is sintered obtained Nd Fe B alloys magnet.
Preferably, in the preparation method of the Nd Fe B alloys magnet,
The composition of the master alloying slab is Nd13.05Dy0.23Fe80.12B6.5, thickness 0.15-0.45mm；
The composition of the auxiliary alloy casting piece is Nd38.2Ce11.8Fe44.88Al4.12B, thickness 0.15-0.45mm.
Preferably, in the preparation method of the Nd Fe B alloys magnet, the average grain diameter of the quick-fried powder of master alloying hydrogen It it is 3-4 μm, the average grain diameter of the auxiliary quick-fried powder of alloy hydrogen is 3-4 μm.
Preferably, in the preparation method of the Nd Fe B alloys magnet, the mixing uses three-dimensional material mixer, mixing Time is 1.5-3.5h.
Preferably, in the preparation method of the Nd Fe B alloys magnet, the uniformly mixed master alloying hydrogen is quick-fried The compression moulding in the alignment magnetic field of >=1.5T of powder and the auxiliary quick-fried powder of alloy hydrogen, it is 4.6 to obtain density using isostatic cool pressing ~4.8g/cm3The Nd Fe B alloys magnet green compact.
Preferably, in the preparation method of the Nd Fe B alloys magnet, when sintering, sintering temperature is 1050 DEG C~ 1100 DEG C of 2~8h of heat preservation, in 800 DEG C~920 DEG C 2~5h of level-one tempering heat preservation；450 DEG C~580 DEG C second annealings heat preservation 3~ 4h。
Beneficial effects of the present invention：
Compared with prior art, rich rare earth can partly be replaced by Ce being added in present invention dual alloy normal direction NdFeB material Nd in phase reduces the consumption of Nd, and the Ce being added with this method occupies grain boundary sites first, greatly reduces expansions of the Dy to crystal boundary It dissipates, reduces the loss of Dy, relatively traditional alloying gimmick effectively improves the coercivity of magnet.In addition, the price of Ce is low In the farther price far below Dy of the price of Nd, so greatly reducing the production cost of material, the profit of rare earth resources is alleviated With imbalance.
The present invention uses pairing gold process, and melting master alloying and the auxiliary alloy of Grain-Boundary Phase, pass through the collaboration of main and auxiliary alloy respectively Effect, so as to get NdFeB magnets have higher coercivity, remanent magnetism and magnetic energy product, processing performance good and at low cost.
Part is illustrated to embody by further advantage, target and the feature of the present invention by following, and part will also be by this The research and practice of invention and be understood by the person skilled in the art.
Specific implementation mode
The present invention is described in further detail below, to enable those skilled in the art being capable of evidence with reference to specification word To implement.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or more The presence or addition of a other elements or combinations thereof.
The present invention provides a kind of preparation methods of Nd Fe B alloys magnet, include the following steps, first by certain purity Neodymium metal, metal dysprosium, metallic aluminium, pure iron, Ce and ferro-boron as raw material, utilize vacuum rapid hardening rejection tablet equipment that neodymium iron boron is made Permanent-magnet material master alloying slab and auxiliary alloy casting piece；Main and auxiliary alloy casting piece is crushed respectively and obtains powder；Auxiliary alloy powder is pressed Certain mass percent is uniformly mixed into master alloying powder, and mixed dual alloy powder is through magnetic field orientating and isostatic cool pressing Obtain compacting green compact；It handles to obtain Sintered NdFeB magnet through sintering and second annealing again.
Embodiment 1
1. using purity for 99.5% neodymium metal, metal dysprosium, metallic aluminium, pure iron, Ce and the (quality point of boracic 19.5% Number) ferro-boron be used as raw material, NdFeB rare earth permanent-magnetic materials master alloying and richness rare earth auxiliary alloy are made with rapid hardening thin slice technique.It is main The composition of alloy casting piece is Nd13.05Dy0.23Fe80.12B6.5, thickness 0.15-0.45mm；The composition of auxiliary alloy casting piece is Nd38.2Ce11.8Fe44.88Al4.12B, thickness 0.15-0.45mm.
2. above-mentioned neodymium iron boron master alloying slab is carried out hydrogen respectively with auxiliary alloy casting piece to break, and air-flow is carried out respectively and is ground Powder obtains auxiliary alloy material feed powder of the average grain diameter in 3-4 μm of neodymium iron boron master alloying material powder and average grain diameter at 3-4 μm End.
3 are added to the auxiliary alloy powder of 3wt% in master alloying material powder, by three-dimensional material mixer by two kinds of alloyed powders End is uniformly mixed, and mixes powder time 2h；
4. by the compression moulding in the alignment magnetic field of >=1.5T of uniformly mixed powder, density is obtained using isostatic cool pressing For 4.6g/cm3Green compact；
5. blank is placed in vacuum sintering furnace the sintering 8h at 1060 DEG C, it is tempered 4h in 900 DEG C of level-ones, in 540 DEG C of two levels It is tempered 3.5h, it is Nd to obtain ingredient30.3Dy0.55Fe67.32B1.04Ce0.73Al0.05Sintered NdFeB magnet.
Sintered NdFeB magnet is prepared into the standard specimen of D10*10 (mm), with the lossless survey of NIM-10000H AC permanent magnet materials It tries instrument and carries out magnetic property measurement, performance is listed in Table 1 below.
Table 1：The obtained properties of product of the present invention and traditional handicraft correction data
Performance Hcj/KOe Br/KGs (BH)max/MGOe Crystal grain/μm Passing rate of processing
Traditional handicraft 16.45~17.18 12.46~12.61 39.75~40.28 6.19 89.1%~92.33%
The present invention 18.2~18.57 13.17~13.32 42.3~43.4 5.38 93.67%~95.45%
As it can be seen from table 1 the technique that the Nd-Fe-B permanent magnet of this method preparation is more traditional, magnetic property is good, crystal grain ruler It is very little refinement and passing rate of processing significantly improve.
Embodiment 2
1. using purity for 99.5% neodymium metal, metal dysprosium, metallic aluminium, pure iron, Ce and the (quality point of boracic 19.5% Number) ferro-boron be used as raw material, NdFeB rare earth permanent-magnetic materials master alloying and richness rare earth auxiliary alloy are made with rapid hardening thin slice technique.It is main The composition of alloy casting piece is Nd13.05Dy0.23Fe80.12B6.5, thickness 0.15-0.45mm.The composition of auxiliary alloy casting piece is Nd38.2Ce11.8Fe44.88Al4.12B, thickness 0.15-0.45mm.
2. above-mentioned neodymium iron boron master alloying slab is carried out hydrogen respectively with auxiliary alloy casting piece to break, and air-flow is carried out respectively and is ground Powder obtains auxiliary alloy material feed powder of the average grain diameter in 3-4 μm of neodymium iron boron master alloying material powder and average grain diameter at 3-4 μm End.
3. the auxiliary alloy powder of 6wt% is added in master alloying material powder, by three-dimensional material mixer by two kinds of alloys Powder is uniformly mixed, and mixes powder time 2.2h；
4. by the compression moulding in the alignment magnetic field of >=1.5T of uniformly mixed powder, density is obtained using isostatic cool pressing For 4.7g/cm3Green compact；
5. blank is placed in vacuum sintering furnace the sintering 8h at 1055 DEG C, it is tempered 4h in 900 DEG C of level-ones, in 520 DEG C of two levels It is tempered 3.5h, it is Nd to obtain ingredient31.38Dy0.53Fe65.58B1.01Ce1.41Al0.09Sintered NdFeB magnet.
Sintered NdFeB magnet is prepared into the standard specimen of D10*10 (mm), with the lossless survey of NIM-10000H AC permanent magnet materials It tries instrument and carries out magnetic property measurement, performance is listed in Table 2 below.
Table 2：The obtained properties of product of the present invention and traditional handicraft correction data
Performance Hcj/KOe Br/KGs (BH)max/MGOe Crystal grain/μm Passing rate of processing
Traditional handicraft 14.12~14.56 12.88~12.97 39.23~40.01 6.38 90.57%~93.86%
The present invention 15.38~16.01 13.26~13.43 41.08~42.72 5.52 95.22~97.3%
From table 2 it can be seen that the technique that the Nd-Fe-B permanent magnet of this method preparation is more traditional, magnetic property is good, crystal grain ruler It is very little refinement and passing rate of processing significantly improve.
Embodiment 3
1. using purity for 99.5% neodymium metal, metal dysprosium, metallic aluminium, pure iron, Ce and the (quality point of boracic 19.5% Number) ferro-boron be used as raw material, NdFeB rare earth permanent-magnetic materials master alloying and richness rare earth auxiliary alloy are made with rapid hardening thin slice technique.It is main The composition of alloy casting piece is Nd13.05Dy0.23Fe80.12B6.5, thickness 0.15-0.45mm.The composition of auxiliary alloy casting piece is Nd38.2Ce11.8Fe44.88Al4.12B, thickness 0.15-0.45mm.
2. above-mentioned neodymium iron boron master alloying slab is carried out hydrogen respectively with auxiliary alloy casting piece to break, and air-flow is carried out respectively and is ground Powder obtains auxiliary alloy material feed powder of the average grain diameter in 3-4 μm of neodymium iron boron master alloying material powder and average grain diameter at 3-4 μm End.
3. the auxiliary alloy powder of 10wt% is added in master alloying material powder, by three-dimensional material mixer by two kinds of alloys Powder is uniformly mixed, and mixes powder time 2.5h；
4. by the compression moulding in the alignment magnetic field of >=1.5T of uniformly mixed powder, density is obtained using isostatic cool pressing For 4.78g/cm3Green compact；
5. blank is placed in vacuum sintering furnace the sintering 8h at 1050 DEG C, it is tempered 4h in 900 DEG C of level-ones, in 560 DEG C of two levels It is tempered 3.5h, it is Nd to obtain ingredient32.69Dy0.5Fe63.48B0.96Ce2.22Al0.15Sintered NdFeB magnet.
Sintered NdFeB magnet is prepared into the standard specimen of D10*10 (mm), with the lossless survey of NIM-10000H AC permanent magnet materials It tries instrument and carries out magnetic property measurement, performance is listed in Table 3 below.
Table 3：The obtained properties of product of the present invention and traditional handicraft correction data
Performance Hcj/KOe Br/KGs (BH)max/MGOe Crystal grain/μm Passing rate of processing
Traditional handicraft 12.12~12.56 11.49~11.73 35.82~36.75 6.51 91.15%~94.3%
The present invention 13.71~14.26 12.86~13.1 37.52~38.06 5.73 96.5~98.2%
From table 3 it can be seen that the technique that the Nd-Fe-B permanent magnet of this method preparation is more traditional, magnetic property is good, crystal grain ruler It is very little refinement and passing rate of processing significantly improve.
Fig. 1 is conventional alloys gimmick, i.e., neodymium iron boron magnetic body prepared by alloying element is added before melting, and metallographic observation goes out The phenomenon that having showed abnormal grain growth, average grain size are 6.14~7.3 μm, and largest grain size is 18~26 μm.
Fig. 2 is neodymium iron boron magnetic body prepared by the inventive method, it is found that the crystallite dimension of magnet is tiny, and relatively uniform.
This illustrates that the addition of auxiliary alloy Nd-rich phase improves the microscopic structure of neodymium iron boron magnetic body to a certain extent, effectively Crystallite dimension has been refined, crystal grain in irregular shape is made to greatly reduce or disappear, has made closer between crystal grain, grain boundaries toughness carries Height promotes the promotion of magnet comprehensive performance.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited In specific details and legend shown and described herein.

Claims (1)

1. the preparation method of Nd Fe B alloys magnet, which is characterized in that include the following steps：
Master alloying slab and auxiliary alloy casting piece is made in the NbFeB sintered raw material, the NbFeB sintered raw material include The ferro-boron of neodymium metal, metal dysprosium, metallic aluminium, pure iron, Ce and boracic mass fraction 19.5% that purity is 99.5%；The master The composition of alloy casting piece is Nd13.05Dy0.23Fe80.12B6.5, thickness 0.15-0.45mm；The composition of the auxiliary alloy casting piece is Nd38.2Ce11.8Fe44.88Al4.12B, thickness 0.15-0.45mm；
It is quick-fried that the master alloying slab and the auxiliary alloy casting piece are subjected to the broken obtained master alloying hydrogen of airflow milling processing of hydrogen respectively Powder and the auxiliary quick-fried powder of alloy hydrogen；The auxiliary quick-fried powder of alloy hydrogen includes Ce；The quality of the auxiliary quick-fried powder of alloy hydrogen is no more than institute State the 10% of the quality of the quick-fried powder of master alloying hydrogen；The average grain diameter of the quick-fried powder of master alloying hydrogen is 3-4 μm, the auxiliary quick-fried powder of alloy hydrogen Average grain diameter be 3-4 μm；
The quick-fried powder of the master alloying hydrogen and the quick-fried powder of the auxiliary alloy hydrogen are mixed, the mixing uses three-dimensional material mixer, incorporation time For 1.5-3.5h,
The uniformly mixed quick-fried powder of the master alloying hydrogen and the auxiliary quick-fried powder of alloy hydrogen are placed under nitrogen protection, taking in >=1.5T The compression moulding into magnetic field, it is 4.6~4.8g/cm to obtain density using isostatic cool pressing3The Nd Fe B alloys magnet pressure Base；
The Nd Fe B alloys magnet green compact is sintered obtained Nd Fe B alloys magnet, sintering temperature is 1050 DEG C~1100 DEG C 2~8h of heat preservation, in 800 DEG C~920 DEG C level-ones tempering heat preservation, 2~5h；3~4h is kept the temperature in 450 DEG C~580 DEG C second annealings.
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