CN104269238B - High-performance sintered neodymium-iron-boron magnet and preparation method - Google Patents
High-performance sintered neodymium-iron-boron magnet and preparation method Download PDFInfo
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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
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 is come out, widely apply IT, medical treatment, new due to its excellent magnetic property
The fields such as the energy, space flight and aviation.Sintered nd-fe-b magnet is typically by Nd2Fe14B matrix phase, crystal boundary rich-Nd phase and Nd1+εFe4B4Rich
Boron phase composition.Wherein, crystal boundary rich-Nd phase play liquid-phase sintering accelerate compaction while, its composition, structure and distribution
Magnet performance is had a major impact.The coercivity mechanism of Sintered NdFeB magnet is Nucleation Mechanism, and it easily forms instead in grain boundaries
Magnetized domains and reduce magnet coercivity.Research shows, if the heavy rare earth elements such as Dy, Tb can be diffused into crystal boundary, improves crystal boundary
Anisotropy, then magnet coercivity can have and significantly be lifted, magnet remanent magnetism response intensity Br declines seldom simultaneously, and permissible
Effectively reduce the addition of Dy.For this situation, the enterprise of scientific research institution both domestic and external and correlation all carries out one after another oozes Dy, Tb
The research of technology.But, ooze Dy technology and many problems also existed on commercial application, such as：Diffusion depth is limited to be not suitable for
Large scale product；Performance poor controllability during batch production, product stability and uniformity are bad；The professional equipment of grain boundary decision is also
Immature, require further study.Therefore, the preparation that Sintered NdFeB magnet still adopts routine is prepared by current domestic enterprise
Method:Single alloyage or general dual alloy method.Heavy rare earth element cannot be effectively utilized using conventional preparation method, simultaneously
Crystal boundary poor controllability, preparing high performance magnet not only needs higher cost, is difficult to prepare very-high performance magnet simultaneously.
Content of the invention
The invention provides the preparation method of a kind of high performance magnet and high performance magnet.Can not only using the inventive method
Preferably by Dy, Tb Elemental redistribution to crystal boundary, obtain low-cost and high-performance magnet, and original production equipment need not be changed and produced
Industry metaplasia is produced, but also can prepare the magnet of very-high performance.
The technical scheme is that:A kind of performance Nd Fe B sintered magnet, its feature includes 85～97wt% principal phase
Alloy RExFeRemainingMzByWith 3～15wt% crystal boundary Nd-rich phase alloy RESNJFeRemaining, wherein:
RE in main-phase alloy compositionxFor one of LREE Nd and Pr or two kinds, RExFor 28～29wt%, Mz
For add metallic element one of Ga, Cu, Al, Co or more than one, MzFor 0.2～2wt%, B element ByFor 0.95～
1.02wt%, balance of Fe；
RE in crystal boundary Nd-rich phase alloying componentSComprise one of Nd, Dy, Tb or more than one, and include at least
One kind of heavy rare earth element Dy and Tb or two kinds, RESFor 40～80 wt%, and（Dy+Tb）Ratio be 15% ~ RES,NJFor
Add metallic element one of Ga, Cu, Al, Co, Nb, Zr or more than one, NJFor 4～10 wt%, balance of Fe.
The preparation method of performance Nd Fe B sintered magnet, comprises the following steps：
1）, carry out batching weighing according to the composition proportion of main-phase alloy, put into melting in vacuum intermediate-frequency smelting furnace, using speed
Solidifying technique slab, arranges copper roller rotating speed 1.5～2.0m/s, 1420～1430 DEG C of cast temperature, prepared main-phase alloy slab；Principal phase
Alloy casting piece carries out hydrogen and crushes, and controls the oxygen content≤400PPm of broken powder；
2）, carry out batching weighing according to the composition proportion of crystal boundary Nd-rich phase alloy, put in vacuum intermediate-frequency smelting furnace molten
Refining, using conventional strip casting slab, arranges copper roller rotating speed 1.2～1.5m/s, 1440 DEG C～1450 DEG C of cast temperature, crystalline substance is obtained
Boundary's Nd-rich phase alloy casting piece；Crystal boundary richness rare-earth alloy casting slice is carried out hydrogen crush, in the broken powder size of screening hydrogen≤380 μm
Powder；
3）, the crystal boundary Nd-rich phase alloy powder breaking screening through hydrogen is carried out airflow milling under inert gas atmosphere, oxygen contains
Amount controls in 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 broken powder mix in proportion, its
Middle crystal boundary Nd-rich phase alloy fine powder adding proportion is 3wt%～15wt%, by the powder of mixing under inert gas atmosphere again
Carry out airflow milling, control mill room oxygen content≤10 PPm, 2.8～3.0 μm of powder size；
5）, uniform mixed-powder is weighed, insert in mould, plus >=2.0T magnetic field orientating be compressing, green compact are taken out
After Vacuum Package, put into pressurization 150～200Mpa in forcing press, pressurize stands 1～3 minute；
6）, by the green compact after standing through pressurize, put into vacuum≤4.0 × 10-2In the vacuum sintering furnace of Pa, at 1020 DEG C
After sintering 3.5～5.5h at a temperature of～1060 DEG C, carry out 4～6h Ageing Treatment at 450 DEG C～600 DEG C, take from sintering furnace
Go out the neodymium iron boron magnetic body made.
In above-mentioned, RE in main-phase alloy selects Nd, Pr, is for ensureing that its indiffusion enters without heavy rare earth such as Dy, Tb
Inside principal phase, x selects 28～29wt% to be then because that main-phase alloy composition must be close to neodymium iron boron principal phase composition；Main-phase alloy by
In low generation soft magnetism phase a-Fe easily in fusion process of content of rare earth, suppress the life of a-Fe in melting by adding M element
Become；B adding too much then leads to Nd1+εFe4B4Phase Proportion is too high and reduces principal phase ratio, thus affecting magnet performance；
The heavy rare earth element of vast scale in above-mentioned, must be added in crystal boundary Nd-rich phase alloy, be because the object of the invention
Exactly in order to the heavy rare earth elements such as Dy, Tb be better distributed on border；And the interpolation of N element is then to be formed in magnet crystal boundary
Grain-Boundary Phase, refines main phase grain；
Crystal boundary Nd-rich phase fine powder such as adding proportion<3wt%, then lead to magnet Grain-Boundary Phase very few, penalty；As added
Ratio>15wt%, then lead to Grain-Boundary Phase excessive and situation that is that substantial amounts of Grain-Boundary Phase reunion leads to hydraulic performance decline.
In above-mentioned, only through an abrasive dust, crystal boundary Nd-rich phase alloy is then equal to through abrasive dust twice main-phase alloy；Using
The method is advantageous in that：Refine crystal boundary Nd-rich phase powder size further so as to more effectively wrap up master alloying phase, and
The risk that there is Powder Oxidation during abrasive dust twice independent to crystal boundary Nd-rich phase can be prevented；And can be made by airflow milling process
Powder mixes evenly.
Magnet 1 is prepared using this method）In the case of identical component, fine and close magnetic can be obtained under lower sintering temperature
Body, thus the abnormal grain growth situation that magnet occurs can be controlled because of high temperature sintering；2）More effectively by heavy rare earth Dy, Tb
It is 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 is permissible
Industrialization on existing production line, heavy rare earth grain boundary decision that need not be special is equipped.
Patent accompanying drawing
Below 3 figures be present invention preparation magnet in heavy rare earth element distribution, 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 Fig. 1, is mainly distributed on crystal boundary；
Fig. 3 is the distribution situation of the heavy rare earth element Tb of corresponding Fig. 1, is mainly distributed on 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, point
The number of cloth is corresponding with the numerical value in scale.
Specific embodiment
Embodiment 1：
1）Main-phase alloy presses Nd29.0Co1.0Ga0.2B1.0FeRemaining（Wt%）Proportioning carry out dispensing melting, using rapid hardening technology
Slab, copper roller rotating speed is 1.5m/s, and pouring temperature is 1430 DEG C；Slab carries out hydrogen and crushes, and broken oxygen content in power controls≤
400PPm；
2）Nd pressed by crystal boundary Nd-rich phase alloy25Dy15Cu2.0Al2.0Co3.0FeRemaining（Wt%）Proportion ingredient melting, using speed
Solidifying technology slab, copper roller rotating speed 1.2m/s, cast temperature is 1450 DEG C；Slab hydrogen breaks, and hydrogen breaks powder in Ar environmental protection（O2
≤10PPm）Sieved, sieve aperture is 40 mesh, 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, controls mill room
Oxygen content≤5PPm, 3～3.5 μm of powder size；
4）Crystal boundary Nd-rich phase alloy powder after airflow milling is broken powder with the hydrogen of main-phase alloy mix（Will be above-mentioned
1）With 2）Mixed）, crystal boundary Nd-rich phase alloy powder adding proportion is 8wt%, and main-phase alloy powder is 92 wt%.
Mixed alloy powder forms content：Nd28.68Dy1.20Co1.16Cu0.16Al0.16Ga0.18B0.92FeRemaining（Wt%）.By mixing
Powder carries out airflow milling under Ar gas atmosphere again, controls mill room oxygen content≤10PPm, 3.0 μm of powder size；
5）Uniform mixed-powder is inserted in mould, plus 2.0T magnetic field orientating is compressing, put into after green compact Vacuum Package
In forcing press, pressurize 220Mpa, oil cooling isostatic pressed 1min；
6）Blank after isostatic pressed is ≤4.0 × 10-2It is sintered and timeliness in the vacuum drying oven of Pa, sintering temperature is 1020
DEG C～1060 DEG C, sintering time is 3.5h；Aging technique：500℃×4h.Completion of prescription prepares sintered NdFeB magnet.
Comparative example 1A：
1) customary preparation methods are adopted, composition is Nd28.68Dy1.2Co1.16Cu0.16Al0.16Ga0.18B0.92FeRemaining（I.e. embodiment
The composition of alloy powder after mixing in 1）, using conventional rapid hardening technology：Copper roller rotating speed 1.2～1.5m/s, 1440 DEG C of cast temperature
～1460 DEG C；Slab hydrogen breaks, and hydrogen breaks powder O2≤ 800PPm, H2≤800PPm；
2) the broken powder of hydrogen carries out airflow milling, controls 3.0～3.5 μm of powder particle size；
3) powder through airflow milling is loaded mould, be molded in the magnetic field of 2.0T, be molded green compact Vacuum Package, after encapsulation
Blank carry out oil cooling isostatic pressed 1～3min in 200～250MPa；
4) blank after isostatic pressed is ≤4.0 × 10-2It is sintered and timeliness under Pa vacuum condition, 1020 DEG C of sintering temperature
～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）Using customary preparation methods, composition is Nd28Dy1.6Co1.2Cu0.2Al0.2Ga0.2B0.95FeRemainingUsing conventional rapid hardening skill
Art：Copper roller rotating speed 1.2～1.5m/s, 1440 DEG C～1460 DEG C of cast temperature；Slab hydrogen breaks, and hydrogen breaks powder O2≤ 800PPm, H2≤
800PPm；
2）Hydrogen breaks powder and carries out airflow milling, controls 3.0～3.5 μm of powder particle size；
3）Powder after airflow milling is loaded mould, is molded in the magnetic field of 2.0T, be molded green compact Vacuum Package, after encapsulation
Blank carry out oil cooling isostatic pressed 1～3min in 200～250MPa；
4）Isostatic pressed blank is ≤4.0 × 10-2In 1045 DEG C × 3.5h of sintering under Pa vacuum condition；Aging technique, 500 DEG C
×4h.Sintered NdFeB magnet is prepared after completion of prescription.
Table 1A difference sintering temperature density contrast table
Can see from above-mentioned contrast table, be obtained under 1020 DEG C～1050 DEG C of sintering temperature using the inventive method
Nd-Fe-B magnet steel, its density will significantly greater than adopt the magnet steel that conventional method is obtained.It is obtained under 1060 DEG C of sintering temperature
Although Nd-Fe-B magnet steel consistency is identical, using the prepared Nd-Fe-B magnet steel abnormal grain growth of conventional method, affect magnet
Performance.Therefore, using the present invention, in the case of identical component, compactness magnet can be obtained under lower sintering temperature, because
And the abnormal grain growth situation that magnet occurs can be controlled because of high temperature sintering.
Table 1B magnetic property and Dy content balance table
Can see from above-mentioned contrast table, the close neodymium-iron-boron of magnetic property is obtained using the inventive method and conventional method
Steel, the content of its heavy rare earth Dy have dropped 0.4wt%, reduces cost.Therefore, this method being capable of the lower high property of preparation cost
Can magnet.
Embodiment 2：
1）Main-phase alloy is according to Nd28.5FeRemainingCu0.2Ga0.2B1.0（Wt%）Proportioning carries out dispensing melting, using rapid hardening technology
Slab, copper roller rotating speed is 1.8m/s, and pouring temperature is 1425 DEG C；Slab carries out hydrogen and crushes, and broken oxygen content in power controls≤
400PPm；
2）Crystal boundary Nd-rich phase alloy is according to Nd45Dy25Tb10Nb1.0Al2.0Co3.0FeRemaining（Wt%）Proportioning carries out dispensing and melts
Refining, using rapid hardening technology slab, copper roller rotating speed 1.2m/s, cast temperature is 1450 DEG C；Slab hydrogen breaks, and hydrogen breaks powder and protects in Ar
In environment（O2≤10PPm）Sieved, sieve aperture is 40 mesh, 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, controls mill room
Oxygen content≤5PPm, 3.0～3.5 μm of powder size；
4）Crystal boundary Nd-rich phase alloy powder after airflow milling and main-phase alloy hydrogen are broken powder mix（Will be above-mentioned
1）With 2）Mixed）, crystal boundary Nd-rich phase alloy adding proportion is 5wt%, and main-phase alloy is 95 wt%；Mixed conjunction
Bronze end composition content be：Nd29.33Dy1.25Tb0.50Co0.50Cu0.19Al0.10Ga0.19Nb0.05B0.95FeRemaining（Wt%）, will mix
Alloy powder carry out airflow milling under Ar gas atmosphere again, control mill room oxygen content≤10PPm, powder size 2.8～3.0 μ
m；
5）Uniformly mixed powder is put in mould plus 2.0T magnetic field orientating is compressing, put after green compact Vacuum Package
Enter in forcing press, pressurize 220MPa, oil cooling isostatic pressed 1min；
6）Blank after isostatic pressed is ≤4.0 × 10-2It is sintered and timeliness under the vacuum condition of Pa, sintering temperature is
1020 DEG C～1050 DEG C, sintering time is 4.5h；Aging technique：480℃×4h.Completion of prescription prepares Sintered NdFeB magnetic
Body.
Comparative example 2A：
1）Using customary preparation methods, composition is Nd29.33Dy1.25Tb0.5Co0.5Cu0.19Al0.1Ga0.19Nb0.05B0.95FeRemaining
（Wt%）（The composition of alloy powder after mixing in embodiment 2）；Using conventional rapid hardening technology：Copper roller rotating speed 1.2～1.5m/s,
1440 DEG C～1460 DEG C of cast temperature；Slab hydrogen breaks, and hydrogen breaks powder O2≤ 800PPm, H2≤800PPm；
2）Hydrogen breaks powder and carries out airflow milling, controls 3.0～3.5 μm of powder particle size；
3）Powder after airflow milling is loaded mould, is molded in the magnetic field of 2.0T, be molded green compact Vacuum Package, after encapsulation
Blank carry out oil cooling isostatic pressed 1～3min in 200～250MPa；
4）Isostatic pressed blank is ≤4.0 × 10-2Being sintered and timeliness under Pa vacuum condition, 1020 DEG C of sintering temperature～
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）Using customary preparation methods, composition is Nd29.5Dy1.8Tb0.5Co0.5Cu0.19Al0.10Ga0.19Nb0.05B0.95FeRemaining
（Wt%）；Using conventional rapid hardening technology：Copper roller rotating speed 1.2～1.5m/s, 1440 DEG C～1460 DEG C of cast temperature；Slab hydrogen breaks,
Hydrogen breaks powder O2≤ 800PPm, H2≤800PPm；
2）Hydrogen breaks powder and carries out airflow milling, 3.0～3.5 μm of powder particle size；
3）Airflow milling powder is loaded mould, is molded in the magnetic field of 2.0T, be molded green compact Vacuum Package, the base after encapsulation
Material carries out oil cooling isostatic pressed 1～3min in 200～250MPa；
Isostatic pressed blank is ≤4.0 × 10-2In 1040 DEG C × 4.5h of sintering under Pa vacuum condition；Aging technique, 480 DEG C ×
4h.Sintered NdFeB magnet is prepared after completion of prescription.
Table 2A difference sintering temperature density contrast table
Can see from above-mentioned contrast table, be obtained under 1020 DEG C～1040 DEG C of sintering temperature using the inventive method
Nd-Fe-B magnet steel, its density is greater than the magnet steel being obtained using conventional method.The neodymium iron being obtained under 1050 DEG C of sintering temperature
Although boron magnet steel consistency is identical, using the prepared Nd-Fe-B magnet steel abnormal grain growth of conventional method, affect magnet performance.
Therefore, using the present invention, in the case of identical component, compactness magnet can be obtained under lower sintering temperature, thus can
With the abnormal grain growth situation controlling magnet to occur because of high temperature sintering.
Table 2B magnetic property and Dy content balance table
Can see from above-mentioned contrast table, the close neodymium-iron-boron of magnetic property is obtained using the inventive method and conventional method
Steel, the content of its heavy rare earth Dy have dropped 0.55%, reduces cost.Therefore, this method being capable of the lower high-performance of preparation cost
Magnet.
Embodiment 3：
1）Main-phase alloy is according to Pr7Nd21FeRemainingAl0.2Co1.0B1.0（Wt%）Proportioning carries out dispensing melting, using rapid hardening skill
Art slab, copper roller rotating speed is 2.0m/s, and pouring temperature is 1425 DEG C；Slab carries out hydrogen and crushes, and broken oxygen content in power controls
≤400PPm；
2）Crystal boundary Nd-rich phase alloy is according to Nd30Dy20Zr1.0Ga2Cu2FeRemaining（Wt%）Proportioning carries out dispensing melting, adopts
Rapid hardening technology slab, copper roller rotating speed 1.4m/s, cast temperature is 1450 DEG C；Slab hydrogen breaks, and hydrogen breaks powder in Ar environmental protection
（O2≤10PPm）Sieved, sieve aperture is 40 mesh, 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, controls mill room
Oxygen content≤5PPm, 3.0 μm of powder size；
4）Crystal boundary Nd-rich phase alloy powder after airflow milling and main-phase alloy hydrogen are broken powder mix（Will be above-mentioned
1）With 2）Mixed）, Nd-rich phase alloy powder adding proportion is 15wt%, and main-phase alloy is 85 wt%；Mixed conjunction
Golden powder constituent content is：Nd22.35Pr5.95Dy3.0Co0.85Cu0.3Al0.17Ga0.3Zr0.15B0.85FeRemaining（Wt%）.In Ar gas gas
Under atmosphere, the alloy powder of mixing is carried out airflow milling again, control mill room oxygen content≤10PPm, 2.8 μm of powder size；
5）Uniformly mixed powder is inserted in mould plus 2.0T magnetic field orientating is compressing, put after green compact Vacuum Package
Enter in forcing press, pressurize 220MPa, oil cooling isostatic pressed 1min；
6）Blank after isostatic pressed is ≤4.0 × 10-2It is sintered and timeliness under the vacuum condition of Pa, sintering temperature is
1020 DEG C～1050 DEG C, sintering time is 4.5h；Aging technique：520℃×4h.Completion of prescription prepares Sintered NdFeB magnetic
Body.
Comparative example 3A：
1）Using customary preparation methods, composition is Nd22.35Pr5.95Dy3.0Co0.85Cu0.3Al0.17Ga0.3Zr0.15B0.85FeRemaining
（Wt.%）（The composition of alloy powder after mixing in embodiment 3）；Using conventional rapid hardening technology：Copper roller rotating speed 1.2～1.5m/
S, 1440 DEG C～1460 DEG C of cast temperature；Slab hydrogen breaks, and hydrogen breaks powder O2≤ 800PPm, H2≤800PPm；
2）Hydrogen breaks powder and carries out airflow milling, controls 3.0～3.5 μm of powder particle size；
3）Powder after airflow milling is loaded mould, is molded in the magnetic field of 2.0T, be molded green compact Vacuum Package, after encapsulation
Blank carry out oil cooling isostatic pressed 1～3min in 200～250MPa；
4）Isostatic pressed blank is ≤4.0 × 10-2Be sintered and timeliness under Pa vacuum condition, sintering temperature 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）Using customary preparation methods, composition is Nd22.4Pr5.6Dy4.0Co1.0Cu0.3Al0.2Ga0.3Zr0.15B0.85FeRemaining
（Wt.%）；Using conventional rapid hardening technology：Copper roller rotating speed 1.2～1.5m/s, 1440 DEG C～1460 DEG C of cast temperature；Slab hydrogen breaks,
Hydrogen breaks powder O2≤ 800PPm, H2≤800PPm；
2）Hydrogen breaks powder and carries out airflow milling, controls 3.0～3.5 μm of powder particle size；
3）Powder after airflow milling is loaded mould, is molded in the magnetic field of 2.0T, be molded green compact Vacuum Package, after encapsulation
Blank carry out oil cooling isostatic pressed 1～3min in 200～250MPa；
Isostatic pressed blank is ≤4.0 × 10-2In 1045 DEG C × 3.5h of sintering under Pa vacuum condition；Aging technique, 480 DEG C ×
4h.Sintered NdFeB magnet is prepared after completion of prescription.
Table 3A difference sintering temperature density contrast table
Can see from above-mentioned contrast table, be obtained under 1020 DEG C～1050 DEG C of sintering temperature using the inventive method
Nd-Fe-B magnet steel, its density is greater than the magnet steel being obtained using conventional method.Therefore, using the present invention, in the feelings of identical component
Under condition, compactness magnet can be obtained under lower sintering temperature, thus the crystalline substance that magnet occurs because of high temperature sintering can be controlled
Grain abnormal growth situation.
Table 3B magnetic property and Dy content balance table
Can see from above-mentioned contrast table, the close neodymium-iron-boron of magnetic property is obtained using the inventive method and conventional method
Steel, the content of its heavy rare earth Dy have dropped 0.5%, reduces cost.Therefore, this method being capable of the lower high-performance of preparation cost
Magnet.
Embodiment 4：
1）Main-phase alloy is according to Nd28.5FeRemainingCo1.0B1.0（Wt%）Proportioning carries out dispensing melting, using the casting of rapid hardening technology
Piece, copper roller rotating speed is 1.8m/s, and pouring temperature is 1420 DEG C；Slab carries out hydrogen and crushes, and broken oxygen content in power controls≤
400PPm；
2）Crystal boundary Nd-rich phase alloy is according to Nd35Dy20Nb1.0Ga2Cu2FeRemaining（Wt%）Proportioning carries out dispensing melting, adopts
Rapid hardening technology slab, copper roller rotating speed 1.5m/s, cast temperature is 1450 DEG C；Slab hydrogen breaks, and hydrogen breaks powder in Ar environmental protection
（O2≤10PPm）Sieved, sieve aperture is 40 mesh, 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, controls mill room
O2≤ 5PPm, 3.0 μm of powder size；
4）Crystal boundary Nd-rich phase alloy powder after airflow milling and main-phase alloy hydrogen are broken powder mix（Will be above-mentioned
1）With 2）Mixed）, Nd-rich phase alloy powder adding proportion is 3wt%, and main-phase alloy is 97wt%；Mixed alloy
Powder constituent content is：Nd28.83Dy1.00Co0.95Cu0.10Ga0.10Nb0.05B0.95FeRemaining（Wt%）, will mix under Ar gas atmosphere
Alloy powder carry out airflow milling again, control mill room oxygen content≤10PPm, 2.8 μm of powder size；
5）Uniformly mixed powder is inserted in mould plus 2.0T magnetic field orientating is compressing, put after green compact Vacuum Package
Enter in forcing press, pressurize 220MPa, oil cooling isostatic pressed 3min；
6）Blank after isostatic pressed is ≤4.0 × 10-2It is sintered and timeliness under the vacuum condition of Pa, sintering temperature is
1045 DEG C, sintering time is 5.5h；Aging technique：485℃×4h.Completion of prescription prepares sintered NdFeB magnet, and magnet has
There are superelevation remanent magnetism and magnetic energy product, performance such as table 4 below.
Table 4 magnet performance table
Comparative example 4
1）Using customary preparation methods, composition is Nd28.83Dy1.0Co0.95Cu0.1Ga0.1Nb0.05B0.95FeRemaining（Wt%）；Using
Conventional rapid hardening technology：Copper roller rotating speed 1.2～1.5m/s, 1440 DEG C～1460 DEG C of cast temperature；Slab hydrogen breaks, and hydrogen breaks powder O2≤
800PPm, H2≤800PPm；
2）Hydrogen breaks powder and carries out airflow milling, controls 3.0～3.5 μm of powder particle size；
3）Powder after airflow milling is loaded mould, is molded in the magnetic field of 2.0T, be molded green compact Vacuum Package, after encapsulation
Blank carry out oil cooling isostatic pressed 1～3min in 200～250MPa；
Isostatic pressed blank is ≤4.0 × 10-2In 1045 DEG C × 3.5h of sintering 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/cm3, do not have
Be magnetic energy.
Be can be seen that by above-mentioned contrast and adopt same recipe, can be obtained with superelevation remanent magnetism by the inventive method and
The magnet of magnetic energy product, and adopt conventional method, then the neodymium iron boron magnetic body prepared does not have magnetic property.Reason is:Preparation superelevation remains
Magnetic and magnetic energy product magnet, it is necessary to assure magnet composition Rare-Earth Content is close to principal phase component content（26.8wt%）To obtain high ratio
The principal phase of example, and crystal boundary Nd-rich phase content is less.Using customary preparation methods, crystal boundary Nd-rich phase be freely distributed it may appear that
The situation of skewness, thus results in that liquid-phase sintering in sintering process is insufficient, and magnet density is low.And adopt the present invention, brilliant
Boundary's Nd-rich phase highly uniform can be distributed in crystal boundary, thus improving sintering densification behavior, even if in crystal boundary Nd-rich phase ratio
Also high-compactness magnet can be obtained in the case of less.Therefore, can be obtained using the inventive method and there is high remanent magnetism and height simultaneously
The superelevation magnetic property magnet of magnetic energy product.
Embodiment 5：
1）Main-phase alloy is according to Nd28.5FeRemainingCo1.0B1.0（Wt%）Proportioning carries out dispensing melting, using the casting of rapid hardening technology
Piece, copper roller rotating speed is 1.8m/s, and pouring temperature is 1420 DEG C；Slab carries out hydrogen and crushes, and broken oxygen content in power controls≤
400PPm；
2）Crystal boundary Nd-rich phase alloy is according to Dy25Tb20Co2.0Ga2.0Cu2.0Al4.0FeRemaining（Wt%）Proportioning carries out dispensing and melts
Refining, using rapid hardening technology slab, copper roller rotating speed 1.3m/s, cast temperature is 1445 DEG C；Slab hydrogen breaks, and hydrogen breaks powder and protects in Ar
In environment（O2≤10PPm）Sieved, sieve aperture is 40 mesh, 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 gas shield, grinds room O2≤
5PPm, 3.5 μm of powder size；
4）Crystal boundary Nd-rich phase alloy powder after airflow milling and main-phase alloy hydrogen are broken powder mix（Will be above-mentioned
1）With 2）Mixed）, Nd-rich phase alloy powder adding proportion is 10wt%, and main-phase alloy is 90wt%；Mixed alloy
Powder constituent content is：Nd25.65Dy2.50Tb2.00Co1.10Cu0.20Ga0.20Al0.40B0.95FeRemaining（Wt%）, under Ar gas atmosphere
The alloy powder of mixing is carried out airflow milling again, control mill room oxygen content≤10PPm, 3.0 μm of powder size；
5）Uniformly mixed powder is inserted in mould plus 2.0T magnetic field orientating is compressing, put after green compact Vacuum Package
Enter in forcing press, pressurize 220MPa, oil cooling isostatic pressed 2min；
6）Blank after isostatic pressed is ≤4.0 × 10-2It is sintered and timeliness under the vacuum condition of Pa, sintering temperature is
1045 DEG C, sintering time is 3.5h；Aging technique：485℃×4h.Completion of prescription prepares sintered NdFeB magnet, and magnet has
There are high remanent magnetism and high-coercive force, performance such as table 5 below.
Comparative example 5
1）Using customary preparation methods, composition is Nd25.65Dy2.5Tb2.0Co1.1Cu0.2Ga0.2Al0.4B0.95FeRemaining（Wt%）；
Using conventional rapid hardening technology：Copper roller rotating speed 1.2～1.5m/s, 1440 DEG C～1460 DEG C of cast temperature；Slab hydrogen breaks, and hydrogen breaks powder
O2≤ 800PPm, H2≤800PPm；
2）Hydrogen breaks powder and carries out airflow milling, controls 3.0～3.5 μm of powder particle size；
3）Powder after airflow milling is loaded mould, is molded in the magnetic field of 2.0T, be molded green compact Vacuum Package, after encapsulation
Blank carry out oil cooling isostatic pressed 1～3min in 200～250MPa；
Isostatic pressed blank is ≤4.0 × 10-2In 1045 DEG C × 3.5h of sintering under Pa vacuum condition；Aging technique, 480 DEG C ×
4h.Sintered NdFeB magnet is prepared after completion of prescription.Magnet performance is shown in Table 5
Table 5 magnet performance contrast table
As can be seen that the neodymium-iron-boron that the inventive method is obtained is passed through using identical material prescription from above-mentioned contrast table
The neodymium iron boron magnetic body that body is obtained compared to conventional method, its remanent magnetism improves 0.15kGs, and coercivity improves 2.3kOe.Using
Customary preparation methods, enter in principal phase because Dy, Tb heavy rare earth element is more, therefore, are such as improved by adding heavy rare earth
Magnet coercivity, then can sacrifice remanent magnetism；If improving remanent magnetism by improving principal phase ratio, that coercivity level will decline.
So, the formula of the present embodiment, if the magnet that coercivity level reaches 20.5kOe will be prepared using conventional method, necessary
Increase the content of heavy rare earth Dy or Tb in dispensing, and the increase of Dy or Tb can lead to remanent magnetism to decline, remanent magnetism does not reach
The level of 13.75kGs, existing high remanent magnetism cannot be obtained the magnet of high-coercive force again.Using the present invention, because Dy, Tb weight is dilute
Soil can be evenly distributed on crystal boundary, seldom enter principal phase, the superelevation magnetic simultaneously with high remanent magnetism and high-coercive force therefore can be obtained
The magnet of energy.
Embodiment 6：
1）Main-phase alloy is according to Nd29.0FeRemainingCo1.0B1.0（Wt%）Proportioning carries out dispensing melting, using the casting of rapid hardening technology
Piece, copper roller rotating speed is 1.8m/s, and pouring temperature is 1420 DEG C；Slab carries out hydrogen and crushes, and broken oxygen content in power controls≤
400PPm；
2）Crystal boundary Nd-rich phase alloy is according to Dy20Tb30Co3.0Ga2.0Cu2.0Al4.0FeRemaining（Wt%）Proportioning carries out dispensing and melts
Refining, using rapid hardening technology slab, copper roller rotating speed 1.3m/s, cast temperature is 1445 DEG C；Slab hydrogen breaks, and hydrogen breaks powder and protects in Ar
In environment（O2≤10PPm）Sieved, sieve aperture is 40 mesh, 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 shield, controls mill room
O2≤ 5PPm, 3.5 μm of powder size；
4）Crystal boundary Nd-rich phase alloy powder after airflow milling and main-phase alloy hydrogen are broken powder mix（Will be above-mentioned
1）With 2）Mixed）, Nd-rich phase alloy powder adding proportion is 12wt%, and main-phase alloy is 88wt%；Mixed alloy
Powder constituent content is：Nd25.52Dy2.40Tb3.60Co1.24Cu0.24Ga0.24Al0.48B0.88FeRemaining（Wt%）, under Ar gas atmosphere
The alloy powder of mixing is carried out airflow milling again, control mill room oxygen content≤10PPm, 3.0 μm of powder size；
5）Uniformly mixed powder is inserted in mould plus 2.0T magnetic field orientating is compressing, put after green compact Vacuum Package
Enter in forcing press, pressurize 220MPa, oil cooling isostatic pressed 3min；
6）Blank after isostatic pressed is ≤4.0 × 10-2It is sintered and timeliness under the vacuum condition of Pa, sintering temperature is
1045 DEG C, sintering time is 3.5h；Aging technique：485℃×4h.Completion of prescription prepares sintered NdFeB magnet, and magnet has
There are high remanent magnetism and ultra-high coercive force, performance such as table 6 below.Magnet institutional framework is as shown in figure 1, distribution such as Fig. 2 of Dy, the distribution of Tb
As shown in Figure 3.
Comparative example 6
1）Using customary preparation methods, composition is Nd25.52Dy2.40Tb3.60Co1.24Cu0.24Ga0.24Al0.48B0.88FeRemaining
（Wt.%）；Using conventional rapid hardening technology：Copper roller rotating speed 1.2～1.5m/s, 1440 DEG C～1460 DEG C of cast temperature；Slab hydrogen breaks,
Hydrogen breaks powder O2≤ 800PPm, H2≤800PPm；
2）Hydrogen breaks powder and carries out airflow milling, controls 3.0～3.5 μm of powder particle size；
3）Powder after airflow milling is loaded mould, is molded in the magnetic field of 2.0T, be molded green compact Vacuum Package, after encapsulation
Blank carry out oil cooling isostatic pressed 1～3min in 200～250MPa；
Isostatic pressed blank is ≤4.0 × 10-2In 1045 DEG C × 3.5h of sintering under Pa vacuum condition；Aging technique, 480 DEG C ×
4h.Sintered NdFeB magnet is prepared after completion of prescription.Magnet performance is shown in Table 6.
Table 6 magnet performance contrast table
As can be seen that adopting identical material prescription from above-mentioned contrast table, the neodymium iron boron being obtained by the inventive method
The neodymium iron boron magnetic body that magnet is obtained compared to commonsense method, its remanent magnetism improves 0.25kGs, and coercivity improves 2.5kOe.Adopt
With customary preparation methods, enter in principal phase because Dy, Tb heavy rare earth element is more, therefore, such as carried by adding heavy rare earth
High magnet coercivity, then can sacrifice remanent magnetism；If by improve principal phase ratio improve remanent magnetism, that coercivity level will under
Fall.So, the formula of the present embodiment, if the magnet that coercivity level reaches 30.5kOe will be prepared using commonsense method, must
The content of heavy rare earth Dy or Tb must be increased in dispensing, and the increase of Dy or Tb, then remanent magnetism can be led to decline, do not reach
The level of 12.85kGs, existing high remanent magnetism cannot be obtained the magnet of high-coercive force again.Can be obtained simultaneously using the inventive method
There is the magnet of the superelevation magnetic property of high remanent magnetism and high-coercive force.
Claims (9)
1. the preparation method of performance Nd Fe B sintered magnet, the composition of wherein performance Nd Fe B sintered magnet includes 85～
97wt% main-phase alloy RExFeRemainingMzByWith 3～15wt% crystal boundary Nd-rich phase alloy RESNJFeRemaining, wherein:
RE in main-phase alloy compositionxFor one of LREE Nd and Pr or two kinds, RExFor 28～29wt%, MzFor adding
Plus metallic element one of Ga, Cu, Al, Co or more than one, MzFor 0.2～2wt%, B element ByFor 0.95～
1.02wt%, balance of Fe；
RE in crystal boundary Nd-rich phase alloying componentSComprise one of Nd, Dy, Tb or more than one, and include at least heavy rare earth
One kind of element Dy and Tb or two kinds, RESFor 40～80 wt%, and（Dy+Tb）Ratio be 15% ~ RES,NJFor adding gold
Belong to element one of Ga, Cu, Al, Co, Nb, Zr or more than one, NJFor 4～10 wt%, balance of Fe；
Preparation method comprises the following steps：
1）, carry out batching weighing according to the composition proportion of main-phase alloy, put into melting in vacuum intermediate-frequency smelting furnace, using rapid hardening work
Skill slab, arranges copper roller rotating speed 1.5～2.0m/s, 1420～1430 DEG C of cast temperature, prepared main-phase alloy slab；Main-phase alloy
Slab carries out hydrogen and crushes, and controls the oxygen content≤400PPm of broken powder；
2）, carry out batching weighing according to the composition proportion of crystal boundary Nd-rich phase alloy, put into melting in vacuum intermediate-frequency smelting furnace, adopt
With conventional strip casting slab, copper roller rotating speed 1.2～1.5m/s, 1440 DEG C～1450 DEG C of cast temperature are set, and prepared crystal boundary is rich
Rare-earth phase alloy casting piece；Crystal boundary richness rare-earth alloy casting slice is carried out hydrogen crush, screening hydrogen breaks the powder of powder size≤380 μm；
3）, the crystal boundary Nd-rich phase alloy powder breaking screening through hydrogen is carried out airflow milling, oxygen content control under inert gas atmosphere
In 5 below PPm, the powder particle size after airflow milling controls at 2.5～3.5 μm system；
4）, the crystal boundary Nd-rich phase alloy fine powder after airflow milling and main-phase alloy hydrogen broken powder mix in proportion, wherein brilliant
Boundary's Nd-rich phase alloy fine powder adding proportion is 3wt%～15wt%, and the powder of mixing is carried out under inert gas atmosphere again
Airflow milling, controls mill room oxygen content≤10 PPm, 2.8～3.0 μm of powder size；
5）, the uniform mixed-powder after airflow milling again is weighed, insert in mould, plus >=2.0T magnetic field orientating be pressed into
Type, after green compact vacuumize encapsulation, puts into pressurization 150～200Mpa in forcing press, pressurize stands 1～3 minute；
6）, by the green compact after standing through pressurize, put into vacuum≤4.0 × 10-2In the vacuum sintering furnace of Pa, 1020 DEG C～
After sintering 3.5～5.5h at a temperature of 1060 DEG C, carry out 4～6h Ageing Treatment at 450 DEG C～600 DEG C, take out from sintering furnace
The neodymium iron boron magnetic body made.
2. the preparation method of performance Nd Fe B sintered magnet according to claim 1, is characterized in that high-performance Ne-Fe-B
The composition content of magnet, Nd for 28.68wt%, Dy for 1.20wt%, Co for 1.16wt%, Cu for 0.16wt%, Al is
0.16wt%, Ga are 0.18 wt%, B is 0.92wt%, balance of Fe.
3. the preparation method of performance Nd Fe B sintered magnet according to claim 1, is characterized in that high-performance Ne-Fe-B
The composition content of magnet, Nd be 28.83 wt%, Dy be 1.00wt%, Co be 0.95wt%, Cu be 0.10wt%, Ga be 0.10
Wt%, Nb are 0.05 wt%, B is 0.95wt%, balance of Fe.
4. the preparation method of performance Nd Fe B sintered magnet according to claim 1, is characterized in that high-performance Ne-Fe-B
The composition content of magnet, Nd for 25.65 wt%, Dy for 2.50 wt%, Tb for 2.00 wt%, Co for 1.10 wt%, Cu is
0.20 wt%, Ga is 0.20 wt%, Al is 0.95 wt%, balance of Fe for 0.40 wt%, B.
5. the preparation method of performance Nd Fe B sintered magnet according to claim 1, is characterized in that high-performance Ne-Fe-B
The composition content of magnet, Nd for 25.52 wt%, Dy for 2.40 wt%, Co for 1.14 wt%, Cu for 0.24 wt%, Ga is
0.24 wt%, Al is 0.48 wt%, B is 0.88 wt%, balance of Fe.
6. the preparation method of performance Nd Fe B sintered magnet according to claim 1 is it is characterised in that step 1）Middle master
Phase alloy composition passes through at least one generation for suppressing a-Fe in melting in addition element Ga, Cu, Al, Co.
7. the preparation method of performance Nd Fe B sintered magnet according to claim 1 is it is characterised in that step 1）Middle master
Phase alloy rapid hardening slab technique sets copper roller rotating speed as 1.8m/s, and cast temperature is 1420 DEG C.
8. the preparation method of performance Nd Fe B sintered magnet according to claim 1 is it is characterised in that step 2）Middle crystalline substance
The screening that boundary's Nd-rich phase hydrogen breaks powder is under inert gas shielding, controls O2≤ 10PPm, is sieved by 40 eye mesh screens.
9. the preparation method of performance Nd Fe B sintered magnet according to claim 1 is it is characterised in that step 6）In true
1020 DEG C～1040 DEG C of empty stove sintering temperature, sinters 3.5～4.5 hours.
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