CN104269238A - High-performance sintered neodymium-iron-boron magnet and preparation method - Google Patents

High-performance sintered neodymium-iron-boron magnet and preparation method Download PDF

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CN104269238A
CN104269238A CN201410519324.6A CN201410519324A CN104269238A CN 104269238 A CN104269238 A CN 104269238A CN 201410519324 A CN201410519324 A CN 201410519324A CN 104269238 A CN104269238 A CN 104269238A
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phase alloy
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CN104269238B (en
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徐峰
刘茗
王育平
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Ningbo Ketian Magnetic Industry Co ltd
Ningbo Jintian Copper Group Co Ltd
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Ningbo Ketian Magnet Co Ltd
Ningbo Jintian Copper Group Co Ltd
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Abstract

A high-performance sintered neodymium-iron-boron magnet comprises 85-97wt% of main-phase alloy Rex Fe rest MzBy and 3-15wt% of crystal boundary rich rare earth alloy RESNJ Fe rest; Rex in the main-phase alloy is one or two of light rare earth Nd and Pr; and RES in the crystal boundary rich rare earth alloy comprises one or more than one of Nd, Dy and Tb and at least comprises one or two of heavy rare earth elements comprising Dy and Tb. The preparation method comprises the following steps of respectively performing burdening, smelting, casting and hydrogen decrepitation according to ingredients of the main-phase alloy and ingredients of the crystal boundary rich rare earth phase alloy; performing airflow grinding on crystal boundary rich rare earth phase alloy powder screened by hydrogen decrepitation into fine powder with the size of 2.5-3.5 micrometers; mixing crystal boundary rich rare earth subjected to airflow grinding and main-phase alloy hydrogen decrepitation powder to a scale; performing airflow grinding on the mixture to obtain powder with the size of 2.8-3.0 micrometers; weighing the powder; feeding the powder in molds; performing magnetic-field orientation and compression molding on the powder; maintaining pressure of the powder and standing; and sintering green bodies in a vacuum furnace. Heavy rare earth comprising Dy and Tb is distributed to a crystal boundary of the main-phase alloy, so that the preparation cost of the high-performance magnet is low.

Description

A kind of performance Nd Fe B sintered magnet and preparation method
Technical field
The present invention relates to a kind of high performance sintered magnet and preparation method.
Background technology
Since nineteen eighty-three, sintered Nd-Fe-B was come out, the fields such as IT, medical treatment, new forms of energy, space flight and aviation are applied widely due to the magnetic property of its excellence.Sintered nd-fe-b magnet is generally by Nd 2fe 14b matrix phase, crystal boundary rich-Nd phase and Nd 1+ εfe 4b 4boron-rich phase forms.Wherein, crystal boundary rich-Nd phase is while playing liquid-phase sintering acceleration compaction, and its composition, structure and distribution also have material impact to magnet performance.The coercivity mechanism of Sintered NdFeB magnet is Nucleation Mechanism, and it easily forms magnetic reversal farmland at grain boundaries and reduces magnet coercive force.Research shows, if the heavy rare earth elements such as Dy, Tb can be diffused into crystal boundary, improves the anisotropy of crystal boundary, then magnet coercive force can have and significantly promotes, and magnet remanent magnetism response intensity Br declines seldom simultaneously, and effectively can reduce the addition of Dy.For this situation, scientific research institution both domestic and external and relevant enterprise carry out the research of oozing Dy, Tb technology all one after another.But, ooze Dy technology and also there is many problems in commercial application, such as: diffusion depth is limited is not suitable for large scale product; Performance poor controllability during batch production, product stability and consistency bad; The professional equipment of grain boundary decision is also immature, requires further study.Therefore, the preparation method that Sintered NdFeB magnet still adopts routine prepares in current domestic enterprise: single alloyage or general two alloyages.Adopt conventional preparation method to effectively utilize heavy rare earth element, crystal boundary poor controllability, prepares high performance magnet and not only needs higher cost, be difficult to prepare very-high performance magnet simultaneously simultaneously.
Summary of the invention
The invention provides the preparation method of a kind of high performance magnet and high performance magnet.Adopt the inventive method can not only better by Dy, Tb Elemental redistribution to crystal boundary, acquisition low-cost and high-performance magnet, and original production equipment need not be changed carry out industrialization production, but also the magnet of very-high performance can be prepared.
Technical scheme of the present invention is: a kind of performance Nd Fe B sintered magnet, and its feature comprises 85 ~ 97wt% main-phase alloy RE xfe more thanm zb ywith 3 ~ 15wt% crystal boundary Nd-rich phase alloy RE sn jfe more than, wherein:
RE in main-phase alloy composition xfor the one in light rare earth element Nd and Pr or two kinds, RE xbe 28 ~ 29wt%, M zfor one or more in interpolation metallic element Ga, Cu, Al, Co, M zbe 0.2 ~ 2wt%, B element B ybe 0.95 ~ 1.02wt%, surplus is Fe;
RE in crystal boundary Nd-rich phase alloying component scomprise in Nd, Dy, Tb one or more, and at least comprise the one of heavy rare earth element Dy and Tb or two kinds, RE sbe 40 ~ 80 wt%, and the ratio of (Dy+Tb) is 15% ~ RE s, N jfor one or more in interpolation metallic element Ga, Cu, Al, Co, Nb, Zr, N jbe 4 ~ 10 wt%, surplus is Fe.
The preparation method of performance Nd Fe B sintered magnet, comprises the following steps:
1), according to the composition proportion of main-phase alloy carry out batching weighing, put into the melting of vacuum intermediate-frequency smelting furnace, adopt strip casting slab, copper roller rotating speed 1.5 ~ 2.0m/s is set, cast temperature 1420 ~ 1430 DEG C, obtained main-phase alloy slab; Main-phase alloy slab carries out hydrogen fragmentation, the oxygen content≤400PPm of controlled fragmentation powder;
2), batching weighing is carried out according to the composition proportion of crystal boundary Nd-rich phase alloy, put into the melting of vacuum intermediate-frequency smelting furnace, adopt conventional strip casting slab, copper roller rotating speed 1.2 ~ 1.5m/s is set, cast temperature 1440 DEG C ~ 1450 DEG C, obtained crystal boundary Nd-rich phase alloy casting piece; Rich for crystal boundary rare-earth alloy casting slice is carried out hydrogen fragmentation, screening hydrogen breaks in particle size≤powder of 380 μm;
3), by the crystal boundary Nd-rich phase alloy powder breaking screening through hydrogen carry out airflow milling under inert gas atmosphere, Control for Oxygen Content is at 5 below PPm, and the powder particle size after airflow milling controls at 2.5 ~ 3.5 μm;
4), the crystal boundary Nd-rich phase alloy fine powder after airflow milling and main-phase alloy hydrogen are broken powder to mix in proportion, wherein crystal boundary Nd-rich phase alloy fine powder adding proportion is 3wt% ~ 15wt%, the powder of mixing is carried out airflow milling under inert gas atmosphere again, control mill oxygen content≤10, room PPm, particle size 2.8 ~ 3.0 μm;
5), by Homogeneous phase mixing powder weighing, insert in mould, add >=2.0T magnetic field orientating is compressing, and after green compact vacuumize encapsulation, put into forcing press pressurization 150 ~ 200Mpa, pressurize leaves standstill 1 ~ 3 minute;
6), by the green compact after leaving standstill through pressurize, vacuum degree≤4.0 × 10 are put into -2in the vacuum sintering furnace of Pa, sinter 3.5 ~ 5.5h at the temperature of 1020 DEG C ~ 1060 DEG C after, carry out 4 ~ 6h Ageing Treatment at 450 DEG C ~ 600 DEG C, from sintering furnace, take out the neodymium iron boron magnetic body made.
In above-mentioned, the RE in main-phase alloy selects Nd, Pr, and not adding the heavy rare earth such as Dy, Tb is for ensureing that principal phase inside is entered in its indiffusion, and x selects 28 ~ 29wt% to be then because main-phase alloy composition must close to neodymium iron boron principal phase composition; Main-phase alloy easily produces soft magnetism phase a-Fe because content of rare earth is low in fusion process, by adding M element to suppress the generation of a-Fe in melting; B addition is too high, causes Nd 1+ εfe 4b 4phase Proportion is too high and reduce principal phase ratio, thus affects magnet performance;
In above-mentioned, must add the heavy rare earth element of vast scale in crystal boundary Nd-rich phase alloy, be because the object of the invention is exactly in order to the heavy rare earth elements such as Dy, Tb are distributed in border better; The interpolation of N element is then can form Grain-Boundary Phase at magnet crystal boundary, refinement main phase grain;
Crystal boundary Nd-rich phase fine powder as adding proportion <3wt%, then causes magnet Grain-Boundary Phase very few, penalty; As adding proportion >15wt%, then the situation that a large amount of Grain-Boundary Phases is reunited causes hydraulic performance decline to cause Grain-Boundary Phase too much to occur.
In above-mentioned, main-phase alloy is only through an abrasive dust, and crystal boundary Nd-rich phase alloy then equals through twice abrasive dust; The benefit of the method is adopted to be: i.e. further refinement crystal boundary Nd-rich phase particle size, makes its more effective parcel master alloying phase, can prevent again the risk that there is Powder Oxidation during twice abrasive dust independent to crystal boundary Nd-rich phase; And by airflow milling process can make that powder mixes evenly.
Adopt this method prepare magnet 1) identical component when, compactness magnet can be obtained under lower sintering temperature, thus can control the abnormal grain growth situation that magnet occurs because of high temperature sintering; 2) more effectively heavy rare earth Dy, Tb are distributed to crystal boundary and the lower high performance magnet of preparation cost; 3) very-high performance magnet can be prepared.4) the present invention can industrialization on existing production line, heavy rare earth grain boundary decision equipment that need not be special.
patent accompanying drawing
3 figure are the distributions of heavy rare earth element in the magnet prepared of the present invention below, and method of testing is EMPA;
Fig. 1 is magnet heterogeneous microstructure picture, and in figure, white is magnet crystal boundary Nd-rich phase, and black is principal phase;
Fig. 2 is the distribution situation of the heavy rare earth element Dy of corresponding diagram 1, is mainly distributed in crystal boundary;
Fig. 3 is the distribution situation of the heavy rare earth element Tb of corresponding diagram 1, is mainly distributed in crystal boundary.
Note: on the right of Fig. 2 and Fig. 3, the scale of color change represents the distribution abundance in corresponding element each region in FIG, distribution number corresponding with the numerical value in scale.
Embodiment
embodiment 1:
1) main-phase alloy presses Nd 29.0co 1.0ga 0.2b 1.0fe more than(wt%) proportioning carries out batching melting, and adopt rapid hardening technology slab, copper roller rotating speed is 1.5m/s, and pouring temperature is 1430 DEG C; Slab carries out hydrogen fragmentation, broken oxygen content in power control≤400PPm;
2) Nd pressed by crystal boundary Nd-rich phase alloy 25dy 15cu 2.0al 2.0co 3.0fe more than(wt%) proportion ingredient melting, adopt rapid hardening technology slab, copper roller rotating speed 1.2m/s, cast temperature is 1450 DEG C; Slab hydrogen breaks, and hydrogen breaks powder (O in Ar protection of the environment 2≤ 10PPm) sieve, sieve aperture is 40 orders, and the Nd-rich phase hydrogen filtering out granularity≤380 μm breaks powder;
3) the crystal boundary Nd-rich phase alloy powder breaking screening through hydrogen is carried out airflow milling under Ar gas atmosphere, control mill room oxygen content≤5PPm, particle size 3 ~ 3.5 μm;
4) the crystal boundary Nd-rich phase alloy powder after airflow milling and the hydrogen of main-phase alloy are broken powder to mix (by above-mentioned 1) and 2) mix), crystal boundary Nd-rich phase alloy powder adding proportion is 8wt%, and main-phase alloy powder is 92 wt%.Mixed alloy powder composition content is: Nd 28.68dy 1.20co 1.16cu 0.16al 0.16ga 0.18b 0.92fe more than(wt%).The powder of mixing is carried out airflow milling again under Ar gas atmosphere, controls mill room oxygen content≤10PPm, particle size 3.0 μm;
5) Homogeneous phase mixing powder is inserted in mould, add 2.0T magnetic field orientating compressing, after green compact Vacuum Package, put into forcing press, pressurization 220Mpa, oil cooling isostatic pressed 1min;
6) blank after isostatic pressed is ≤4.0 × 10 -2carry out in the vacuum furnace of Pa sintering and timeliness, sintering temperature is 1020 DEG C ~ 1060 DEG C, and sintering time is 3.5h; Aging technique: 500 DEG C × 4h.Completion of prescription prepares sintered NdFeB magnet.
comparative example 1A:
1) adopt customary preparation methods, composition is Nd 28.68dy 1.2co 1.16cu 0.16al 0.16ga 0.18b 0.92fe more than(namely in embodiment 1, mixing the composition of rear alloy powder), adopt conventional rapid hardening technology: copper roller rotating speed 1.2 ~ 1.5m/s, cast temperature 1440 DEG C ~ 1460 DEG C; Slab hydrogen breaks, and hydrogen breaks powder O 2≤ 800PPm, H 2≤ 800PPm;
2) hydrogen breaks powder and carries out airflow milling, controls powder particle size 3.0 ~ 3.5 μm;
3) powder through airflow milling is loaded mould, shaping in the magnetic field of 2.0T, shaping green compact Vacuum Package, the blank after encapsulation carries out oil cooling isostatic pressed 1 ~ 3min at 200 ~ 250MPa;
4) blank after isostatic pressed is ≤4.0 × 10 -2carry out under Pa vacuum condition sintering and timeliness, sintering temperature 1020 DEG C ~ 1060 DEG C, sintering time 3.5h; Aging technique, 500 DEG C × 4h.Sintered NdFeB magnet is prepared after completion of prescription.
comparative example 1B:
1) adopt customary preparation methods, composition is Nd 28dy 1.6co 1.2cu 0.2al 0.2ga 0.2b 0.95fe more thanadopt conventional rapid hardening technology: copper roller rotating speed 1.2 ~ 1.5m/s, cast temperature 1440 DEG C ~ 1460 DEG C; Slab hydrogen breaks, and hydrogen breaks powder O 2≤ 800PPm, H 2≤ 800PPm;
2) hydrogen breaks powder and carries out airflow milling, controls powder particle size 3.0 ~ 3.5 μm;
3) powder after airflow milling is loaded mould, shaping in the magnetic field of 2.0T, shaping green compact Vacuum Package, the blank after encapsulation carries out oil cooling isostatic pressed 1 ~ 3min at 200 ~ 250MPa;
4) isostatic pressed blank is ≤4.0 × 10 -2at sintering 1045 DEG C × 3.5h under Pa vacuum condition; Aging technique, 500 DEG C × 4h.Sintered NdFeB magnet is prepared after completion of prescription.
Table 1A different sintering temperature density contrast table
Can see from above-mentioned contrast table, adopt the Nd-Fe-B magnet steel that the inventive method is obtained under the sintering temperature of 1020 DEG C ~ 1050 DEG C, its density obviously will be greater than the magnet steel adopting conventional method obtained.Although Nd-Fe-B magnet steel density obtained under the sintering temperature of 1060 DEG C is identical, adopts the Nd-Fe-B magnet steel abnormal grain growth that conventional method is obtained, affect magnet performance.Therefore, adopt the present invention, when identical component, compactness magnet can be obtained under lower sintering temperature, thus can control the abnormal grain growth situation that magnet occurs because of high temperature sintering.
Table 1B magnetic property and Dy content balance table
Can see from above-mentioned contrast table, adopt the inventive method and conventional method to obtain the close Nd-Fe-B magnet steel of magnetic property, the content of its heavy rare earth Dy have dropped 0.4wt%, reduces cost.Therefore, this method can the lower high performance magnet of preparation cost.
embodiment 2:
1) main-phase alloy is according to Nd 28.5fe more thancu 0.2ga 0.2b 1.0(wt%) proportioning carries out batching melting, and adopt rapid hardening technology slab, copper roller rotating speed is 1.8m/s, and pouring temperature is 1425 DEG C; Slab carries out hydrogen fragmentation, broken oxygen content in power control≤400PPm;
2) crystal boundary Nd-rich phase alloy is according to Nd 45dy 25tb 10nb 1.0al 2.0co 3.0fe more than(wt%) proportioning carries out batching melting, and adopt rapid hardening technology slab, copper roller rotating speed 1.2m/s, cast temperature is 1450 DEG C; Slab hydrogen breaks, and hydrogen breaks powder (O in Ar protection of the environment 2≤ 10PPm) sieve, sieve aperture is 40 orders, and the Nd-rich phase hydrogen filtering out granularity≤380 μm breaks powder;
3) the crystal boundary Nd-rich phase alloy powder breaking screening through hydrogen is carried out airflow milling in Ar gas atmosphere, control mill room oxygen content≤5PPm, particle size 3.0 ~ 3.5 μm;
4) the crystal boundary Nd-rich phase alloy powder after airflow milling and main-phase alloy hydrogen are broken powder to mix (by above-mentioned 1) and 2) mix), crystal boundary Nd-rich phase alloy adding proportion is 5wt%, and main-phase alloy is 95 wt%; The composition content of mixed alloy powder is: Nd 29.33dy 1.25tb 0.50co 0.50cu 0.19al 0.10ga 0.19nb 0.05b 0.95fe more than(wt%), the alloy powder of mixing is carried out airflow milling again under Ar gas atmosphere, control mill room oxygen content≤10PPm, particle size 2.8 ~ 3.0 μm;
5) powder after Homogeneous phase mixing being put into mould, to add 2.0T magnetic field orientating compressing, puts into forcing press after green compact Vacuum Package, pressurization 220MPa, oil cooling isostatic pressed 1min;
6) blank after isostatic pressed is ≤4.0 × 10 -2carry out under the vacuum condition of Pa sintering and timeliness, sintering temperature is 1020 DEG C ~ 1050 DEG C, and sintering time is 4.5h; Aging technique: 480 DEG C × 4h.Completion of prescription prepares sintered NdFeB magnet.
comparative example 2A:
1) adopt customary preparation methods, composition is Nd 29.33dy 1.25tb 0.5co 0.5cu 0.19al 0.1ga 0.19nb 0.05b 0.95fe more than(wt%) (composition of rear alloy powder namely in embodiment 2, is mixed); Adopt conventional rapid hardening technology: copper roller rotating speed 1.2 ~ 1.5m/s, cast temperature 1440 DEG C ~ 1460 DEG C; Slab hydrogen breaks, and hydrogen breaks powder O 2≤ 800PPm, H 2≤ 800PPm;
2) hydrogen breaks powder and carries out airflow milling, controls powder particle size 3.0 ~ 3.5 μm;
3) powder after airflow milling is loaded mould, shaping in the magnetic field of 2.0T, shaping green compact Vacuum Package, the blank after encapsulation carries out oil cooling isostatic pressed 1 ~ 3min at 200 ~ 250MPa;
4) isostatic pressed blank is ≤4.0 × 10 -2carrying out sintering and timeliness under Pa vacuum condition, sintering temperature 1020 DEG C ~ 1050 DEG C, sintering time 4.5h; Aging technique, 480 DEG C × 4h.Sintered NdFeB magnet is prepared after completion of prescription.
comparative example 2B:
1) adopt customary preparation methods, composition is Nd 29.5dy 1.8tb 0.5co 0.5cu 0.19al 0.10ga 0.19nb 0.05b 0.95fe more than(wt%); Adopt conventional rapid hardening technology: copper roller rotating speed 1.2 ~ 1.5m/s, cast temperature 1440 DEG C ~ 1460 DEG C; Slab hydrogen breaks, and hydrogen breaks powder O 2≤ 800PPm, H 2≤ 800PPm;
2) hydrogen breaks powder and carries out airflow milling, powder particle size 3.0 ~ 3.5 μm;
3) airflow milling powder is loaded mould, shaping in the magnetic field of 2.0T, shaping green compact Vacuum Package, the blank after encapsulation carries out oil cooling isostatic pressed 1 ~ 3min at 200 ~ 250MPa;
Isostatic pressed blank is ≤4.0 × 10 -2at sintering 1040 DEG C × 4.5h under Pa vacuum condition; Aging technique, 480 DEG C × 4h.Sintered NdFeB magnet is prepared after completion of prescription.
Table 2A different sintering temperature density contrast table
Can see from above-mentioned contrast table, adopt the Nd-Fe-B magnet steel that the inventive method is obtained under the sintering temperature of 1020 DEG C ~ 1040 DEG C, its density is greater than the magnet steel adopting conventional method obtained.Although Nd-Fe-B magnet steel density obtained under the sintering temperature of 1050 DEG C is identical, adopts the Nd-Fe-B magnet steel abnormal grain growth that conventional method is obtained, affect magnet performance.Therefore, adopt the present invention, when identical component, compactness magnet can be obtained under lower sintering temperature, thus can control the abnormal grain growth situation that magnet occurs because of high temperature sintering.
Table 2B magnetic property and Dy content balance table
Can see from above-mentioned contrast table, adopt the inventive method and conventional method to obtain the close Nd-Fe-B magnet steel of magnetic property, the content of its heavy rare earth Dy have dropped 0.55%, reduces cost.Therefore, this method can the lower high performance magnet of preparation cost.
embodiment 3:
1) main-phase alloy is according to Pr 7nd 21fe more thanal 0.2co 1.0b 1.0(wt%) proportioning carries out batching melting, and adopt rapid hardening technology slab, copper roller rotating speed is 2.0m/s, and pouring temperature is 1425 DEG C; Slab carries out hydrogen fragmentation, broken oxygen content in power control≤400PPm;
2) crystal boundary Nd-rich phase alloy is according to Nd 30dy 20zr 1.0ga 2cu 2fe more than(wt%) proportioning carries out batching melting, and adopt rapid hardening technology slab, copper roller rotating speed 1.4m/s, cast temperature is 1450 DEG C; Slab hydrogen breaks, and hydrogen breaks powder (O in Ar protection of the environment 2≤ 10PPm) sieve, sieve aperture is 40 orders, and the Nd-rich phase hydrogen filtering out granularity≤380 μm breaks powder;
3) the crystal boundary Nd-rich phase alloy powder breaking screening through hydrogen is carried out airflow milling under Ar gas atmosphere, control mill room oxygen content≤5PPm, particle size 3.0 μm;
4) the crystal boundary Nd-rich phase alloy powder after airflow milling and main-phase alloy hydrogen are broken powder to mix (by above-mentioned 1) and 2) mix), Nd-rich phase alloy powder adding proportion is 15wt%, and main-phase alloy is 85 wt%; Mixed alloy powder composition content is: Nd 22.35pr 5.95dy 3.0co 0.85cu 0.3al 0.17ga 0.3zr 0.15b 0.85fe more than(wt%).Under Ar gas atmosphere, the alloy powder of mixing is carried out airflow milling again, control mill room oxygen content≤10PPm, particle size 2.8 μm;
5) powder after Homogeneous phase mixing is inserted in mould to add 2.0T magnetic field orientating compressing, put into forcing press after green compact Vacuum Package, pressurization 220MPa, oil cooling isostatic pressed 1min;
6) blank after isostatic pressed is ≤4.0 × 10 -2carry out under the vacuum condition of Pa sintering and timeliness, sintering temperature is 1020 DEG C ~ 1050 DEG C, and sintering time is 4.5h; Aging technique: 520 DEG C × 4h.Completion of prescription prepares sintered NdFeB magnet.
comparative example 3A:
1) adopt customary preparation methods, composition is Nd 22.35pr 5.95dy 3.0co 0.85cu 0.3al 0.17ga 0.3zr 0.15b 0.85fe more than(wt.%) (composition of rear alloy powder namely in embodiment 3, is mixed); Adopt conventional rapid hardening technology: copper roller rotating speed 1.2 ~ 1.5m/s, cast temperature 1440 DEG C ~ 1460 DEG C; Slab hydrogen breaks, and hydrogen breaks powder O 2≤ 800PPm, H 2≤ 800PPm;
2) hydrogen breaks powder and carries out airflow milling, controls powder particle size 3.0 ~ 3.5 μm;
3) powder after airflow milling is loaded mould, shaping in the magnetic field of 2.0T, shaping green compact Vacuum Package, the blank after encapsulation carries out oil cooling isostatic pressed 1 ~ 3min at 200 ~ 250MPa;
4) isostatic pressed blank is ≤4.0 × 10 -2carry out under Pa vacuum condition sintering and timeliness, sintering temperature at 1020 DEG C ~ 1050 DEG C, sintering time 4.5h; Aging technique, 520 DEG C × 4h.Sintered NdFeB magnet is prepared after completion of prescription.
comparative example 3B:
1) adopt customary preparation methods, composition is Nd 22.4pr 5.6dy 4.0co 1.0cu 0.3al 0.2ga 0.3zr 0.15b 0.85fe more than(wt.%); Adopt conventional rapid hardening technology: copper roller rotating speed 1.2 ~ 1.5m/s, cast temperature 1440 DEG C ~ 1460 DEG C; Slab hydrogen breaks, and hydrogen breaks powder O 2≤ 800PPm, H 2≤ 800PPm;
2) hydrogen breaks powder and carries out airflow milling, controls powder particle size 3.0 ~ 3.5 μm;
3) powder after airflow milling is loaded mould, shaping in the magnetic field of 2.0T, shaping green compact Vacuum Package, the blank after encapsulation carries out oil cooling isostatic pressed 1 ~ 3min at 200 ~ 250MPa;
Isostatic pressed blank is ≤4.0 × 10 -2at sintering 1045 DEG C × 3.5h under Pa vacuum condition; Aging technique, 480 DEG C × 4h.Sintered NdFeB magnet is prepared after completion of prescription.
Table 3A different sintering temperature density contrast table
Can see from above-mentioned contrast table, adopt the Nd-Fe-B magnet steel that the inventive method is obtained under the sintering temperature of 1020 DEG C ~ 1050 DEG C, its density is greater than the magnet steel adopting conventional method obtained.Therefore, adopt the present invention, when identical component, compactness magnet can be obtained under lower sintering temperature, thus can control the abnormal grain growth situation that magnet occurs because of high temperature sintering.
Table 3B magnetic property and Dy content balance table
Can see from above-mentioned contrast table, adopt the inventive method and conventional method to obtain the close Nd-Fe-B magnet steel of magnetic property, the content of its heavy rare earth Dy have dropped 0.5%, reduces cost.Therefore, this method can the lower high performance magnet of preparation cost.
embodiment 4:
1) main-phase alloy is according to Nd 28.5fe more thanco 1.0b 1.0(wt%) proportioning carries out batching melting, and adopt rapid hardening technology slab, copper roller rotating speed is 1.8m/s, and pouring temperature is 1420 DEG C; Slab carries out hydrogen fragmentation, broken oxygen content in power control≤400PPm;
2) crystal boundary Nd-rich phase alloy is according to Nd 35dy 20nb 1.0ga 2cu 2fe more than(wt%) proportioning carries out batching melting, and adopt rapid hardening technology slab, copper roller rotating speed 1.5m/s, cast temperature is 1450 DEG C; Slab hydrogen breaks, and hydrogen breaks powder (O in Ar protection of the environment 2≤ 10PPm) sieve, sieve aperture is 40 orders, and the Nd-rich phase hydrogen filtering out granularity≤380 μm breaks powder;
3) the crystal boundary Nd-rich phase alloy powder breaking screening through hydrogen is carried out airflow milling under Ar gas atmosphere, control mill room O 2≤ 5PPm, particle size 3.0 μm;
4) the crystal boundary Nd-rich phase alloy powder after airflow milling and main-phase alloy hydrogen are broken powder to mix (by above-mentioned 1) and 2) mix), Nd-rich phase alloy powder adding proportion is 3wt%, and main-phase alloy is 97wt%; Mixed alloy powder composition content is: Nd 28.83dy 1.00co 0.95cu 0.10ga 0.10nb 0.05b 0.95fe more than(wt%), under Ar gas atmosphere, the alloy powder of mixing is carried out airflow milling again, control mill room oxygen content≤10PPm, particle size 2.8 μm;
5) powder after Homogeneous phase mixing is inserted in mould to add 2.0T magnetic field orientating compressing, put into forcing press after green compact Vacuum Package, pressurization 220MPa, oil cooling isostatic pressed 3min;
6) blank after isostatic pressed is ≤4.0 × 10 -2carry out under the vacuum condition of Pa sintering and timeliness, sintering temperature is 1045 DEG C, and sintering time is 5.5h; Aging technique: 485 DEG C × 4h.Completion of prescription prepares sintered NdFeB magnet, and magnet has superelevation remanent magnetism and magnetic energy product, and performance is as following table 4.
Table 4 magnet performance table
comparative example 4
1) adopt customary preparation methods, composition is Nd 28.83dy 1.0co 0.95cu 0.1ga 0.1nb 0.05b 0.95fe more than(wt%); Adopt conventional rapid hardening technology: copper roller rotating speed 1.2 ~ 1.5m/s, cast temperature 1440 DEG C ~ 1460 DEG C; Slab hydrogen breaks, and hydrogen breaks powder O 2≤ 800PPm, H 2≤ 800PPm;
2) hydrogen breaks powder and carries out airflow milling, controls powder particle size 3.0 ~ 3.5 μm;
3) powder after airflow milling is loaded mould, shaping in the magnetic field of 2.0T, shaping green compact Vacuum Package, the blank after encapsulation carries out oil cooling isostatic pressed 1 ~ 3min at 200 ~ 250MPa;
Isostatic pressed blank is ≤4.0 × 10 -2at sintering 1045 DEG C × 3.5h under Pa vacuum condition; Aging technique, 480 DEG C × 4h.Sintered NdFeB magnet is prepared after completion of prescription.This magnet is difficult to densified sintering product, and magnet density is less than 7.0g/cm 3, there is no magnetic property.
Can be found out by above-mentioned contrast, adopt same recipe, can be obtained the magnet with superelevation remanent magnetism and magnetic energy product by the inventive method, and adopt conventional method, then the neodymium iron boron magnetic body prepared does not have magnetic property.Reason is: preparation superelevation remanent magnetism and magnetic energy product magnet, must ensure magnet composition Rare-Earth Content close to principal phase component content (26.8wt%) to obtain a high proportion of principal phase, and crystal boundary Nd-rich phase content is less.Adopt customary preparation methods, crystal boundary Nd-rich phase freely distributes, and there will be the situation of skewness, and thus cause liquid-phase sintering in sintering process insufficient, magnet density is low.And adopting the present invention, crystal boundary Nd-rich phase very can be evenly distributed on crystal boundary, thus improves sintering densification behavior, even if also can obtain high-compactness magnet when crystal boundary Nd-rich phase ratio is less.Therefore, the inventive method is adopted can to obtain the superelevation magnetic property magnet simultaneously with high remanent magnetism and high energy product.
embodiment 5:
1) main-phase alloy is according to Nd 28.5fe more thanco 1.0b 1.0(wt%) proportioning carries out batching melting, and adopt rapid hardening technology slab, copper roller rotating speed is 1.8m/s, and pouring temperature is 1420 DEG C; Slab carries out hydrogen fragmentation, broken oxygen content in power control≤400PPm;
2) crystal boundary Nd-rich phase alloy is according to Dy 25tb 20co 2.0ga 2.0cu 2.0al 4.0fe more than(wt%) proportioning carries out batching melting, and adopt rapid hardening technology slab, copper roller rotating speed 1.3m/s, cast temperature is 1445 DEG C; Slab hydrogen breaks, and hydrogen breaks powder (O in Ar protection of the environment 2≤ 10PPm) sieve, sieve aperture is 40 orders, and the Nd-rich phase alloy hydrogen filtering out granularity≤380 μm breaks powder;
3) the crystal boundary Nd-rich phase alloy powder breaking screening through hydrogen is carried out airflow milling under Ar Buchholz protection, mill room O 2≤ 5PPm, particle size 3.5 μm;
4) the crystal boundary Nd-rich phase alloy powder after airflow milling and main-phase alloy hydrogen are broken powder to mix (by above-mentioned 1) and 2) mix), Nd-rich phase alloy powder adding proportion is 10wt%, and main-phase alloy is 90wt%; Mixed alloy powder composition content is: Nd 25.65dy 2.50tb 2.00co 1.10cu 0.20ga 0.20al 0.40b 0.95fe more than(wt%), under Ar gas atmosphere, the alloy powder of mixing is carried out airflow milling again, control mill room oxygen content≤10PPm, particle size 3.0 μm;
5) powder after Homogeneous phase mixing is inserted in mould to add 2.0T magnetic field orientating compressing, put into forcing press after green compact Vacuum Package, pressurization 220MPa, oil cooling isostatic pressed 2min;
6) blank after isostatic pressed is ≤4.0 × 10 -2carry out under the vacuum condition of Pa sintering and timeliness, sintering temperature is 1045 DEG C, and sintering time is 3.5h; Aging technique: 485 DEG C × 4h.Completion of prescription prepares sintered NdFeB magnet, and magnet has high remanent magnetism and high-coercive force, and performance is as following table 5.
comparative example 5
1) adopt customary preparation methods, composition is Nd 25.65dy 2.5tb 2.0co 1.1cu 0.2ga 0.2al 0.4b 0.95fe more than(wt%); Adopt conventional rapid hardening technology: copper roller rotating speed 1.2 ~ 1.5m/s, cast temperature 1440 DEG C ~ 1460 DEG C; Slab hydrogen breaks, and hydrogen breaks powder O 2≤ 800PPm, H 2≤ 800PPm;
2) hydrogen breaks powder and carries out airflow milling, controls powder particle size 3.0 ~ 3.5 μm;
3) powder after airflow milling is loaded mould, shaping in the magnetic field of 2.0T, shaping green compact Vacuum Package, the blank after encapsulation carries out oil cooling isostatic pressed 1 ~ 3min at 200 ~ 250MPa;
Isostatic pressed blank is ≤4.0 × 10 -2at sintering 1045 DEG C × 3.5h under Pa vacuum condition; Aging technique, 480 DEG C × 4h.Sintered NdFeB magnet is prepared after completion of prescription.Magnet performance is in table 5
Table 5 magnet performance contrast table
As can be seen from above-mentioned contrast table, the neodymium iron boron magnetic body that the neodymium iron boron magnetic body adopting identical material prescription to be obtained by the inventive method is obtained compared to conventional method, its remanent magnetism improves 0.15kGs, and coercive force improves 2.3kOe.Adopting customary preparation methods, enter into principal phase because Dy, Tb heavy rare earth element more, therefore, as improved magnet coercive force by adding heavy rare earth, then can sacrifice remanent magnetism; If improve remanent magnetism by improving principal phase ratio, that coercive force level will decline.So, the formula of the present embodiment, if adopt conventional method will prepare the magnet that coercive force level reaches 20.5kOe, the content of heavy rare earth Dy or Tb then must be increased in batching, and the increase of Dy or Tb can cause remanent magnetism to decline, remanent magnetism does not reach the level of 13.75kGs, cannot obtain the magnet that existing high remanent magnetism has again high-coercive force.Adopt the present invention, because Dy, Tb heavy rare earth can be evenly distributed on crystal boundary, seldom enter principal phase, therefore can obtain the magnet of the superelevation magnetic property simultaneously with high remanent magnetism and high-coercive force.
embodiment 6:
1) main-phase alloy is according to Nd 29.0fe more thanco 1.0b 1.0(wt%) proportioning carries out batching melting, and adopt rapid hardening technology slab, copper roller rotating speed is 1.8m/s, and pouring temperature is 1420 DEG C; Slab carries out hydrogen fragmentation, broken oxygen content in power control≤400PPm;
2) crystal boundary Nd-rich phase alloy is according to Dy 20tb 30co 3.0ga 2.0cu 2.0al 4.0fe more than(wt%) proportioning carries out batching melting, and adopt rapid hardening technology slab, copper roller rotating speed 1.3m/s, cast temperature is 1445 DEG C; Slab hydrogen breaks, and hydrogen breaks powder (O in Ar protection of the environment 2≤ 10PPm) sieve, sieve aperture is 40 orders, and the Nd-rich phase hydrogen filtering out granularity≤380 μm breaks powder;
3) the crystal boundary Nd-rich phase alloy powder breaking screening through hydrogen is carried out airflow milling under Ar Buchholz protection, control mill room O 2≤ 5PPm, particle size 3.5 μm;
4) the crystal boundary Nd-rich phase alloy powder after airflow milling and main-phase alloy hydrogen are broken powder to mix (by above-mentioned 1) and 2) mix), Nd-rich phase alloy powder adding proportion is 12wt%, and main-phase alloy is 88wt%; Mixed alloy powder composition content is: Nd 25.52dy 2.40tb 3.60co 1.24cu 0.24ga 0.24al 0.48b 0.88fe more than(wt%), under Ar gas atmosphere, the alloy powder of mixing is carried out airflow milling again, control mill room oxygen content≤10PPm, particle size 3.0 μm;
5) powder after Homogeneous phase mixing is inserted in mould to add 2.0T magnetic field orientating compressing, put into forcing press after green compact Vacuum Package, pressurization 220MPa, oil cooling isostatic pressed 3min;
6) blank after isostatic pressed is ≤4.0 × 10 -2carry out under the vacuum condition of Pa sintering and timeliness, sintering temperature is 1045 DEG C, and sintering time is 3.5h; Aging technique: 485 DEG C × 4h.Completion of prescription prepares sintered NdFeB magnet, and magnet has high remanent magnetism and ultra-high coercive force, and performance is as following table 6.Magnet institutional framework as shown in Figure 1, the distribution of Dy as the distribution of Fig. 2, Tb as shown in Figure 3.
comparative example 6
1) adopt customary preparation methods, composition is Nd 25.52dy 2.40tb 3.60co 1.24cu 0.24ga 0.24al 0.48b 0.88fe more than(wt.%); Adopt conventional rapid hardening technology: copper roller rotating speed 1.2 ~ 1.5m/s, cast temperature 1440 DEG C ~ 1460 DEG C; Slab hydrogen breaks, and hydrogen breaks powder O 2≤ 800PPm, H 2≤ 800PPm;
2) hydrogen breaks powder and carries out airflow milling, controls powder particle size 3.0 ~ 3.5 μm;
3) powder after airflow milling is loaded mould, shaping in the magnetic field of 2.0T, shaping green compact Vacuum Package, the blank after encapsulation carries out oil cooling isostatic pressed 1 ~ 3min at 200 ~ 250MPa;
Isostatic pressed blank is ≤4.0 × 10 -2at sintering 1045 DEG C × 3.5h under Pa vacuum condition; Aging technique, 480 DEG C × 4h.Sintered NdFeB magnet is prepared after completion of prescription.Magnet performance is in table 6.
Table 6 magnet performance contrast table
As can be seen from above-mentioned contrast table, adopt identical material prescription, the neodymium iron boron magnetic body that the neodymium iron boron magnetic body obtained by the inventive method is obtained compared to commonsense method, its remanent magnetism improves 0.25kGs, and coercive force improves 2.5kOe.Adopting customary preparation methods, enter into principal phase because Dy, Tb heavy rare earth element more, therefore, as improved magnet coercive force by adding heavy rare earth, then can sacrifice remanent magnetism; If improve remanent magnetism by improving principal phase ratio, that coercive force level will decline.So, the formula of the present embodiment, if adopt commonsense method will prepare the magnet that coercive force level reaches 30.5kOe, the content of heavy rare earth Dy or Tb then must be increased in batching, and the increase of Dy or Tb, remanent magnetism then can be caused to decline, do not reach the level of 12.85kGs, the magnet that existing high remanent magnetism has again high-coercive force cannot be obtained.Adopt the inventive method can obtain the magnet of the superelevation magnetic property simultaneously with high remanent magnetism and high-coercive force.

Claims (10)

1. a performance Nd Fe B sintered magnet, its feature comprises 85 ~ 97wt% main-phase alloy RE xfe more thanm zb ywith 3 ~ 15wt% crystal boundary Nd-rich phase alloy RE sn jfe more than, wherein:
RE in main-phase alloy composition xfor the one in light rare earth element Nd and Pr or two kinds, RE xbe 28 ~ 29wt%, M zfor one or more in interpolation metallic element Ga, Cu, Al, Co, M zbe 0.2 ~ 2wt%, B element B ybe 0.95 ~ 1.02wt%, surplus is Fe;
RE in crystal boundary Nd-rich phase alloying component scomprise in Nd, Dy, Tb one or more, and at least comprise the one of heavy rare earth element Dy and Tb or two kinds, RE sbe 40 ~ 80 wt%, and the ratio of (Dy+Tb) is 15% ~ RE s, N jfor one or more in interpolation metallic element Ga, Cu, Al, Co, Nb, Zr, N jbe 4 ~ 10 wt%, surplus is Fe.
2. a kind of performance Nd Fe B sintered magnet according to claim 1, it is characterized in that the composition content of high-performance neodymium-iron-boron magnet, Nd is 28.68wt%, Dy be 1.20wt%, Co be 1.16wt%, Cu be 0.16wt%, Al be 0.16wt%, Ga be 0.18 wt%, B is 0.92wt%, surplus is Fe.
3. a kind of performance Nd Fe B sintered magnet according to claim 1, it is characterized in that the composition content of high-performance neodymium-iron-boron magnet, Nd is 28.83 wt%, Dy be 1.00wt%, Co be 0.95wt%, Cu be 0.10wt%, Ga be 0.10 wt%, Nb be 0.05 wt%, B is 0.95wt%, surplus is Fe.
4. a kind of performance Nd Fe B sintered magnet according to claim 1, it is characterized in that the composition content of high-performance neodymium-iron-boron magnet, Nd is 25.65 wt%, Dy be 2.50 wt%, Tb be 2.00 wt%, Co be 1.10 wt%, Cu be 0.20 wt%, Ga be 0.20 wt%, Al be 0.40 wt%, B is 0.95 wt%, surplus is Fe.
5. a kind of performance Nd Fe B sintered magnet according to claim 1, it is characterized in that the composition content of high-performance neodymium-iron-boron magnet, Nd is 25.52 wt%, Dy be 2.40 wt%, Co be 1.14 wt%, Cu be 0.24 wt%, Ga be 0.24 wt%, Al be 0.48 wt%, B is 0.88 wt%, surplus is Fe.
6. the preparation method of performance Nd Fe B sintered magnet, comprises the following steps:
1), according to the composition proportion of main-phase alloy carry out batching weighing, put into the melting of vacuum intermediate-frequency smelting furnace, adopt strip casting slab, copper roller rotating speed 1.5 ~ 2.0m/s is set, cast temperature 1420 ~ 1430 DEG C, obtained main-phase alloy slab; Main-phase alloy slab carries out hydrogen fragmentation, the oxygen content≤400PPm of controlled fragmentation powder;
2), batching weighing is carried out according to the composition proportion of crystal boundary Nd-rich phase alloy, put into the melting of vacuum intermediate-frequency smelting furnace, adopt conventional strip casting slab, copper roller rotating speed 1.2 ~ 1.5m/s is set, cast temperature 1440 DEG C ~ 1450 DEG C, obtained crystal boundary Nd-rich phase alloy casting piece; Rich for crystal boundary rare-earth alloy casting slice is carried out hydrogen fragmentation, screening hydrogen breaks in particle size≤powder of 380 μm;
3), by the crystal boundary Nd-rich phase alloy powder breaking screening through hydrogen carry out airflow milling under inert gas atmosphere, Control for Oxygen Content is at 5 below PPm, and the powder particle size after airflow milling controls at 2.5 ~ 3.5 μm;
4), the crystal boundary Nd-rich phase alloy fine powder after airflow milling and main-phase alloy hydrogen are broken powder to mix in proportion, wherein crystal boundary Nd-rich phase alloy fine powder adding proportion is 3wt% ~ 15wt%, the powder of mixing is carried out airflow milling under inert gas atmosphere again, control mill oxygen content≤10, room PPm, particle size 2.8 ~ 3.0 μm;
5), by Homogeneous phase mixing powder weighing, insert in mould, add >=2.0T magnetic field orientating is compressing, and after green compact vacuumize encapsulation, put into forcing press pressurization 150 ~ 200Mpa, pressurize leaves standstill 1 ~ 3 minute;
6), by the green compact after leaving standstill through pressurize, vacuum degree≤4.0 × 10 are put into -2in the vacuum sintering furnace of Pa, sinter 3.5 ~ 5.5h at the temperature of 1020 DEG C ~ 1060 DEG C after, carry out 4 ~ 6h Ageing Treatment at 450 DEG C ~ 600 DEG C, from sintering furnace, take out the neodymium iron boron magnetic body made.
7. the preparation method of a kind of performance Nd Fe B sintered magnet according to claim 6, is characterized in that in step 1), main-phase alloy composition suppresses the generation of a-Fe in melting by least one in Addition ofelements Ga, Cu, Al, Co.
8. the preparation method of a kind of performance Nd Fe B sintered magnet according to claim 6, it is characterized in that in step 1), main-phase alloy rapid hardening slab technique sets copper roller rotating speed as 1.8m/s, cast temperature is 1420 DEG C.
9. the preparation method of a kind of performance Nd Fe B sintered magnet according to claim 6, is characterized in that step 2) in the screening of breaking powder of crystal boundary Nd-rich phase hydrogen be under inert gas shielding, control O 2≤ 10PPm, is sieved by 40 eye mesh screens.
10. the preparation method of a kind of performance Nd Fe B sintered magnet according to claim 6, is characterized in that vacuum furnace sintering temperature 1020 DEG C ~ 1040 DEG C in step 6), sinters 3.5 ~ 4.5 hours.
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