CN103426623A - Method for preparing anisotropy nano-crystalline neodymium-iron-boron magnet - Google Patents

Method for preparing anisotropy nano-crystalline neodymium-iron-boron magnet Download PDF

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CN103426623A
CN103426623A CN2013103368082A CN201310336808A CN103426623A CN 103426623 A CN103426623 A CN 103426623A CN 2013103368082 A CN2013103368082 A CN 2013103368082A CN 201310336808 A CN201310336808 A CN 201310336808A CN 103426623 A CN103426623 A CN 103426623A
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magnetic
hydrogen
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pressed compact
dehydrogenation
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CN103426623B (en
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刘颖
李军
郑青
余云萍
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Sichuan University
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Sichuan University
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Abstract

A method for preparing an anisotropy nano-crystalline neodymium-iron-boron magnet comprises the steps that (1) complete hydrogen disproportionate or partial hydrogen disproportionate Nd-Fe-B magnetic powder is prepared; (2) a pressed blank is prepared, the complete hydrogen disproportionate Nd-Fe-B magnetic powder or the partial hydrogen disproportionate Nd-Fe-B magnetic powder prepared in the step (1) is placed in a mold, under the inert gas shielding, pressing is conducted on the magnetic powder at the indoor temperature, and when the pressure intensity received by the magnetic powder is increased to 100MPa-600MPa from 0MPa, pressing is stopped; (3) hot-pressing deformation and dehydrogenation recombination are conducted, so that the temperature of the pressed blank is increased to 680 DEG C-850 DEG C under the vacuum condition, under the conditions that the temperature is 680 DEG C-850 DEG C and the hydrogen partial pressure PH2 satisfies the inequation that 0Pa<PH2<= 1kPa, constant pressure is exerted on the Nd-Fe-B pressed blank so that hot-pressing deformation and dehydrogenation recombination can be conducted, the pressure intensity value is limited in the range that the pressure intensity borne by the Nd-Fe-B hydrogen disproportionate pressed blank in the process of hot-pressing deformation and dehydrogenation ranges from 30MPa to 1.5MPa, and the temperature preservation and pressure preservation time lasts for 5min-120min. The method for preparing the anisotropy nano-crystalline neodymium-iron-boron magnet can improve the performance of the anisotropy nano-crystalline neodymium-iron-boron magnet and reduce energy consumption.

Description

A kind of preparation method of anisotropy nano-crystal neodymium iron boron magnetic body
Technical field
The invention belongs to the rare earth permanent-magnetic material preparation field, particularly a kind of preparation method of anisotropy nano-crystal neodymium iron boron magnetic body.
Background technology
The nanocrystalline Nd-Fe-B magnet of anisotropy has the highest theoretical magnetic energy product, therefore receives much concern.At present, the preparation method of the nanocrystalline Nd-Fe-B magnet of anisotropy mainly contains suction hydrogen-disproportionation-dehydrogenation-recombination method (being called for short the HDDR method) and hot pressing-thermal deformation method.
The standby anisotropy Nd-Fe-B magnet of HDDR legal system, the alloying elements such as the hydrogen dividing potential drop during mainly by the reduction disproportionation or interpolation Co, Ga, Zr obtain anisotropy Nd-Fe-B magnetic, again by anisotropy Nd-Fe-B magnetic with after bonding agent mixes under the effect of externally-applied magnetic field by method moulding such as compacting or injection mouldings, obtain anisotropic bonded magnet.Although this kind of method process is simple, easy-formation, but because the magnetic property that makes magnet adding of bonding agent is generally on the low side, in addition, in the HDDR process, because the suction hydrogen of Nd-Fe-B and dehydrogenation reaction are accompanied by strong heat release and heat absorption phenomenon, make temperature of reaction system produce larger fluctuation, cause Nd-Fe-B magnetic anisotropy lower, and can not stably prepare the finished product magnet of identical performance.
The processing step of hot pressing-thermal deformation method is: (1) applies the high fine and close pressed compact of high pressure (pressure is at least at 300MPa) formation by isotropic Nd-Fe-B magnetic at 600 ℃ ~ 750 ℃ and (sees W. Q. Liu et.al., Structure and magnetic properties of magnetically isotropic and anisotropic Nd – Fe – B permanent magnets prepared by spark plasma sintering technology, J. Appl. Phys., 2010,107 (9): 09A719); (2) pressed compact step (1) formed is greater than 700 ℃ in temperature and exerts pressure and carry out thermal deformation; obtain anisotropy Nd-Fe-B magnet; in thermal deformation process; the pressure range that pressed compact bears changes and (sees Pengpeng Yi et.al between 30 MPa ~ 300 MPa; Enhanced magnetic properties and bending strength of hot deformed Nd – Fe – B magnets with Cu additions; J. Alloys Compds., 2010 (491): 605 – 609; Y. L. Huang et.al, Diffusion of Nd-rich phase in the spark plasma sintered and hot deformed nanocrystalline NdFeB magnets, J. Appl. Phys., 2012,111,033913).The problem that this kind of method exists is: because pressed compact is at the HTHP compacted under, may make that the part crystal grain of Nd-Fe-B pressed compact is excessive and uniformity is poor, thus Nd in the NdFeB magnet that causes obtaining after thermal deformation 2Fe 14The deformation extent of B crystal grain is inhomogeneous, the grain morphology systematicness is poor, the orientation consistency is poor, and has increased energy consumption.
Summary of the invention
The object of the present invention is to provide a kind of new method for preparing the anisotropy nano-crystal neodymium iron boron magnetic body, to obtain anisotropy obviously and the nano-crystal neodymium iron boron magnetic body had excellent magnetic characteristics, and reduce energy consumption, simplify technique.
The preparation method of anisotropy nano-crystal neodymium iron boron magnetic body of the present invention, its processing step is as follows successively:
(1) preparation of hydrogen disproportionation or part hydrogen disproportionation Nd-Fe-B magnetic fully
By the Nd-Fe-B alloy powder at H 2Under atmosphere, in 650 ℃ ~ 820 ℃ insulations, within 5 minutes～60 minutes, inhaled hydrogen-disproportionated reaction, insulation cools to room temperature with the furnace after finishing, and obtaining crystallite dimension is nano level complete hydrogen disproportionation Nd-Fe-B magnetic;
Or by the Nd-Fe-B alloy powder at H 2Under atmosphere, within 5 minutes～60 minutes, inhaled hydrogen-disproportionated reaction in 650 ℃～820 ℃ insulations, after inhaling hydrogen-disproportionated reaction, in vacuum degree<5 * 10 -2Within 1～10 minute, carry out dehydrogenation-recombining reaction in 780 ℃～820 ℃ insulations under the condition of Pa, insulation cools to room temperature with the furnace after finishing, and obtaining crystallite dimension is nano level part hydrogen disproportionation Nd-Fe-B magnetic;
(2) preparation of pressed compact
Complete hydrogen disproportionation Nd-Fe-B magnetic prepared by step (1) or part hydrogen disproportionation Nd-Fe-B magnetic are packed in mould, under inert gas shielding, in room temperature, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 100MPa～600MPa, obtains the hydrogen disproportionation thing pressed compact of Nd-Fe-B;
(3) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (2) is prepared is warming up to 680 ℃～850 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2For 0Pa<P H2Under the condition of≤1kPa, described Nd-Fe-B pressed compact is applied to constant pressure and carry out hot compression deformation-dehydrogenation restructuring, the pressure that bears in thermal deformation-dehydrogenation regrouping process with Nd-Fe-B hydrogen disproportionation thing pressed compact of the value of exerting pressure change and be limited between 30MPa ~ 1.5MPa, the heat-insulation pressure keeping time is 5～120 minutes, heat-insulation pressure keeping cools to room temperature with the furnace after finishing, and obtains the nanocrystalline Nd-Fe-B magnet of anisotropy.
In said method, the initial pressure (maximum pressure) that shape and size and the described pressed compact of the constant pressure that hot compression deformation-dehydrogenation reconstitution steps applies Nd-Fe-B hydrogen disproportionation thing pressed compact by described pressed compact bears in thermal deformation-dehydrogenation regrouping process is determined.Because in hot compression deformation-dehydrogenation regrouping process, Nd-Fe-B hydrogen disproportionation thing pressed compact deforms, and due to stressed constant, its lifting surface area increases, and the pressure born is from diminishing greatly.
In said method, the chemical formula of described Nd-Fe-B alloy powder is Nd xFe 100-x-y-zM yB z, 12≤x≤15,0≤y≤10,5.6≤z≤6 wherein, M is at least one in Co, Ga, Zr, Nb, Cu, Al, Cr, Mo, Ti.
In said method, the preferred Nd of described Nd-Fe-B alloy powder 12.2Fe 81.8B 6, Nd 13.5Fe 80.5B 6, Nd 13.5Fe 80.4Ga 0.5B 5.6, Nd 13.5Fe 73Co 7.5B 6, Nd 12.5Fe 80.5Nb 1B 6, Nd 14Fe 79.4Al 0.6B 6, Nd 15Fe 78Mo 1B 6, Nd 12.2Fe 71.8Co 9.4Ga 0.5Zr 0.1B 6, Nd 13.62Fe 75.7Co 4.45Ga 0.47B 5.76, Nd 14Fe 76Co 3Zr 1B 6, Nd 12.6Fe 72.3Co 8.6Al 0.5B 6.0, Nd 13.5Fe 79.96Al 0.24Nb 0.3B 6, Nd 13Fe 71.86Co 9Al 0.08Cu 0.06B 6, Nd 14.5Fe 76.4Ti 2.5Cr 1B 5.6, Nd 13Fe 71.86Co 9.08Cu 0.06B 6, Nd 13.8Fe 70.6Co 5Mo 3.8Al 1B 5.8, Nd 15Fe 77.9Cu 1.5B 5.6In a kind of.
The method of the invention has following beneficial effect:
1, due to the method for the invention be by after the complete hydrogen disproportionation of Nd-Fe-B alloy powder or part hydrogen disproportionation by the formation pressed compact of colding pressing, again pressed compact hot compression deformation-dehydrogenation restructuring is obtained to the nanocrystalline Nd-Fe-B magnet of anisotropy, thereby the pressed compact crystal grain obtained is tiny, main phase grain oriented nucleation and growth in hot compression deformation-dehydrogenation restructuring, can be formed directly in that grain orientation is obvious and crystallite dimension is tiny (orientation crystal grain width is 80-100nm), uniform anisotropy nano-crystal neodymium iron boron magnetic body (see figure 2), the neodymium iron boron magnetic body of this kind of structure has obvious anisotropy and good magnetic property.
2, because the method for the invention is not used bonding agent, and by hot compression deformation-dehydrogenation restructuring, pressed compact is directly changed into to the anisotropy nano-crystal neodymium iron boron magnetic body, thereby with respect to the HDDR method, the magnetic property of anisotropy nano-crystal neodymium iron boron magnetic body can not only be improved, and the finished product magnet can be stably prepared.
3, because adopting cold moudling, the method for the invention prepares the hydrogen disproportionation thing pressed compact of Nd-Fe-B, and the pressure that during hot compression deformation, pressed compact bears is less, thereby, with respect to hot pressing-thermal deformation method, the pressed compact crystal grain that not only obtained is more tiny, even, and capable of reducing energy consumption, simplify the operation.
4, the method for the invention technique of the present invention is simple, energy consumption is lower, not high to equipment requirement, and because the suppression performance of Nd-Fe-B hydrogen disproportionation thing alloy powder is better than the Nd-Fe-B alloy powder that principal phase is the 2:14 phase, under low pressure can produce according to the actual requirements height densification or the fully dense anisotropy Nd-Fe-B magnet product of the various shapes such as sheet, ring-type, strip, be conducive to promote the use of.
The accompanying drawing explanation
Fig. 1 is the XRD figure (perpendicular to pressure direction) of the nanocrystalline Nd-Fe-B magnet of the prepared anisotropy of embodiment 1;
Fig. 2 is the FESEM(field emission scanning electron microscope of the nanocrystalline Nd-Fe-B magnet of the prepared anisotropy of embodiment 1 section) figure (direction of arrow is pressure direction).
Embodiment
Below by embodiment, the preparation method of anisotropy nano-crystal neodymium iron boron magnetic body of the present invention is described further.In following embodiment, the preparation of hydrogen disproportionation or part hydrogen disproportionation Nd-Fe-B magnetic adopts HTO-114 II type horizontal vacuum sintering furnace (Qingdao fully, absolute sincerity Huaqi IDTC company), the hydrogen disproportionation thing pressed compact of Nd-Fe-B adopts YSD-10-1 type bidirectional hydraulic press moulding (Sichuan, the logical magnetic part technology development co. of Mianyang China), hot compression deformation-dehydrogenation reconstitution steps adopts SPS-1050 type discharge plasma sintering instrument (Japan, Sumitomo Shi Tan mining company).
Embodiment 1
The present embodiment is with fast quenching Nd 13.5Fe 73Co 7.5B 6Magnetic is that raw material prepares the anisotropy nanocrystalline magnet, and processing step is as follows:
(1) Nd 13.5Fe 73Co 7.5B 6The preparation of quenched powder
Take metal Nd (purity is 99.5%), DT4 electrical pure iron (purity is 99.95%), ferro-boron (boron content is 19.65%), metal Co (purity is 99.5%) is raw material, according to Nd 13.5Fe 73Co 7.5B 6Alloying component calculates the ingredients by weight (increasing the Nd of 1.5wt% during batching as compensating for loss and damage) of each raw material.Adopt SF2002-4 type vacuum intermediate-frequency induction melting furnace melting Nd Fe B alloys, before heating, first smelting furnace is evacuated to 1 * 10 -2Pa, applying argon gas is to 0.05MPa, then according to the alloying component of calculating, power is adjusted to 38kW and carries out melting, after melting completes, alloy melt poured in ingot mould, obtains plate-cast ingot after cooling.After being ground off to oxide skin, plate-cast ingot is broken for pellet; then put into the copper crucible of LZK-12A type vacuum quick quenching equipment; under argon shield atmosphere; power up to flow to after 600A melts furnace charge and be poured on the copper roller that linear velocity is 28m/s; cooling rear acquisition Nd Fe B alloys strip; after crossing 300 mesh sieves removal fine powders, obtain Nd 13.5Fe 73Co 7.5B 6Rapidly quenched magnetic powder;
(2) preparation of part hydrogen disproportionation Nd-Fe-B magnetic
Fast quenching Nd prepared by step (1) 13.5Fe 73Co 7.5B 6Magnetic is at H 2Under atmosphere, be heated to 800 ℃ of insulations and within 10 minutes, inhaled hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, in vacuum degree<5 * 10 -2Be warming up to 820 ℃ of insulations under the condition of Pa and within 5 minutes, carry out dehydrogenation-recombining reaction, insulation cools to room temperature with the furnace after finishing, and obtains crystallite dimension and (contains principal phase 2:14 phase and disproportionation phase NdH at the part hydrogen disproportionation Nd-Fe-B of 150-200nm magnetic x, Fe 2B, α-Fe);
(3) preparation of pressed compact
Part hydrogen disproportionation Nd-Fe-B magnetic prepared by step (2) is packed in mould, under argon shield, in room temperature, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 300MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B, described pressed compact is cylindrical, is of a size of φ 10mm * 10mm;
(4) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (3) is prepared is warming up to 820 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2Carry out hot compression deformation-dehydrogenation restructuring under the condition of 10Pa, described Nd-Fe-B pressed compact being applied to constant pressure, the value of exerting pressure is 1.5kN, the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact is born in thermal deformation-dehydrogenation regrouping process changes between 20MPa ~ 5.5MPa, the heat-insulation pressure keeping time is 10 minutes, heat-insulation pressure keeping cools to room temperature with the furnace after finishing, the nanocrystalline Nd-Fe-B magnet of anisotropy that to obtain deflection be 73 %, its figure of XRD perpendicular to pressure direction is shown in Fig. 1, FESEM figure is shown in Fig. 2.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.96, and magnetic property is: B r=1.3T, H Ci=602 kA/m, (BH) m=268kJ/m 3.
Embodiment 2
The present embodiment is with fast quenching Nd 13.5Fe 80.4Ga 0.5B 5.6Magnetic is that raw material prepares the anisotropy nanocrystalline magnet, and processing step is as follows:
(1) Nd 13.5Fe 80.4Ga 0.5B 5.6The preparation of quenched powder
Take metal Nd (purity is 99.5%), DT4 electrical pure iron (purity is 99.95%), ferro-boron (boron content is 19.65%), metal Ga(purity is 99.95%) be raw material, according to Nd 13.5Fe 80.4Ga 0.5B 5.6Alloying component calculates the ingredients by weight (increasing the Nd of 1.5wt% during batching as compensating for loss and damage) of each raw material.Adopt SF2002-4 type vacuum intermediate-frequency induction melting furnace melting Nd Fe B alloys, before heating, first smelting furnace is evacuated to 1 * 10 -2Pa, applying argon gas is to 0.05MPa, then according to the alloying component of calculating, power is adjusted to 36kW and carries out melting, after melting completes, alloy melt poured in ingot mould, obtains plate-cast ingot after cooling.After being ground off to oxide skin, plate-cast ingot is broken for pellet; then put into the copper crucible of LZK-12A type vacuum quick quenching equipment; under argon shield atmosphere; power up to flow to after 650A melts furnace charge and be poured on the copper roller that linear velocity is 28m/s; cooling rear acquisition Nd Fe B alloys strip; after crossing 300 mesh sieves and removing fine powder, obtain Nd 13.5Fe 80.4Ga 0.5B 5.6Rapidly quenched magnetic powder.
(2) preparation of part hydrogen disproportionation Nd-Fe-B magnetic
Fast quenching Nd prepared by step (1) 13.5Fe 80.4Ga 0.5B 5.6Magnetic is at H 2Under atmosphere, be heated to 680 ℃ of insulations and within 45 minutes, inhaled hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, in vacuum degree<5 * 10 -2Be warming up to 800 ℃ of insulations under the condition of Pa and within 1 minute, carry out dehydrogenation-recombining reaction, insulation cools to room temperature with the furnace after finishing, and the part hydrogen disproportionation Nd-Fe-B magnetic that obtains crystallite dimension 100-120nm (contains principal phase 2:14 phase and disproportionation phase NdH x, Fe 2B, α-Fe);
(3) preparation of pressed compact
Part hydrogen disproportionation Nd-Fe-B magnetic prepared by step (2) is packed in mould, under argon shield, in room temperature, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 100MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B, described pressed compact is cylindrical, is of a size of φ 10.5mm * 10.5mm;
(4) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (3) is prepared is warming up to 780 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2Carry out hot compression deformation-dehydrogenation restructuring under the condition of 10Pa, described Nd-Fe-B pressed compact being applied to constant pressure, the value of exerting pressure is 2.2kN, the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact is born in thermal deformation-dehydrogenation regrouping process changes between 25MPa ~ 4MPa, the heat-insulation pressure keeping time is 20 minutes, after finishing, heat-insulation pressure keeping cools to room temperature with the furnace, the nanocrystalline Nd-Fe-B magnet of anisotropy that to obtain deflection be 83 %.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.95, and its magnetic property is: B r=1.2 T, H Ci=550 kA/m, (BH) m=2446 kJ/m 3.
Embodiment 3
The present embodiment is with fast quenching Nd 13.5Fe 80.5B 6Magnetic is that raw material prepares the anisotropy nanocrystalline magnet, and processing step is as follows:
(1) Nd 13.5Fe 80.5B 6The quenched powder preparation
Take metal Nd (purity is 99.5%), DT4 electrical pure iron (purity is 99.95%), ferro-boron (boron content is 19.65%) is raw material, the definite Nd according to design 13.5Fe 80.5B 6Alloying component calculates the ingredients by weight (increasing the Nd of 1.5wt% during batching as compensating for loss and damage) of each raw material.Adopt SF2002-4 type vacuum intermediate-frequency induction melting furnace melting Nd Fe B alloys, before heating, first smelting furnace is evacuated to 1 * 10 -2Pa, applying argon gas is to 0.05MPa, then according to the alloying component of calculating, power added to 35kW and carries out melting, after melting completes, alloy melt poured in ingot mould, obtains plate-cast ingot after cooling.After plate-cast ingot is ground off to oxide skin; be broken for pellet; put into the copper crucible of LZK-12A type vacuum quick quenching equipment; under argon shield atmosphere; power up to flow to after 600A melts furnace charge and be poured on the copper roller that linear velocity is 30m/s; cooling rear acquisition Nd Fe B alloys strip, after 300 mesh sieves remove fine powder excessively, obtain Nd 13.5Fe 80.5B 6Rapidly quenched magnetic powder.
(2) preparation of part hydrogen disproportionation Nd-Fe-B magnetic
Fast quenching Nd prepared by step (1) 13.5Fe 80.5B 6Magnetic is at H 2Under atmosphere, be heated to 750 ℃ of insulations and within 30 minutes, inhaled hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, in vacuum degree<5 * 10 -2Be warming up to 780 ℃ of insulations under the condition of Pa and within 10 minutes, carry out dehydrogenation-recombining reaction, insulation cools to room temperature with the furnace after finishing, and the part hydrogen disproportionation Nd-Fe-B magnetic that to obtain crystallite dimension be 120-140nm (contains principal phase 2:14 phase and disproportionation phase NdH x, Fe 2B, α-Fe);
(3) preparation of pressed compact
Part hydrogen disproportionation Nd-Fe-B magnetic prepared by step (2) is packed in mould, under argon shield, in room temperature, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 270MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B, described pressed compact is cylindrical, is of a size of φ 11mm * 11mm;
(4) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (3) is prepared is warming up to 700 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2Carry out hot compression deformation-dehydrogenation restructuring under the condition of 40Pa, described Nd-Fe-B pressed compact being applied to constant pressure, the value of exerting pressure is 2.7kN, the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact is born in thermal deformation-dehydrogenation regrouping process changes between 28MPa ~ 8.5MPa, the heat-insulation pressure keeping time is 60 minutes, after finishing, heat-insulation pressure keeping cools to room temperature with the furnace, the nanocrystalline Nd-Fe-B magnet of anisotropy that to obtain deflection be 70 %.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.91, and magnetic property is: B r=1.1T, H Ci=600kA/m, (BH) m=235kJ/m 3.
Embodiment 4
The present embodiment is with fast quenching Nd 13.5Fe 73Co 7.5B 6Magnetic is that raw material prepares the anisotropy nanocrystalline magnet, and processing step is as follows:
(1) Nd 13.5Fe 73Co 7.5B 6The quenched powder preparation
The preparation method is with embodiment 1, slightly.
(2) preparation of hydrogen disproportionation Nd-Fe-B magnetic fully
Fast quenching Nd prepared by step (1) 13.5Fe 73Co 7.5B 6Magnetic is at H 2Under atmosphere, in 650 ℃ of insulations, within 60 minutes, inhaled hydrogen-disproportionated reaction, insulation cools to room temperature with the furnace after finishing, and obtaining crystallite dimension is the complete hydrogen disproportionation Nd-Fe-B magnetic of 180-200nm;
(3) preparation of pressed compact
Complete hydrogen disproportionation Nd-Fe-B magnetic prepared by step (2) is packed in mould, under argon shield, in room temperature, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 450MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B, described pressed compact is cylindrical, is of a size of φ 11mm * 11mm;
(4) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (3) is prepared is warming up to 750 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2Carry out hot compression deformation-dehydrogenation restructuring under the condition of 800Pa, described Nd-Fe-B pressed compact being applied to constant pressure, the value of exerting pressure is 2.5kN, the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact is born in thermal deformation-dehydrogenation regrouping process changes between 26MPa ~ 6.5MPa, the heat-insulation pressure keeping time is 60 minutes, after finishing, heat-insulation pressure keeping cools to room temperature with the furnace, the nanocrystalline Nd-Fe-B magnet of anisotropy that to obtain deflection be 75 %.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.92, and its magnetic property is: B r=0.95 T, H Ci=501 kA/m, (BH) m=147 kJ/m 3.
Embodiment 5
The present embodiment is with fast quenching Nd 12.2Fe 71.8Co 9.4Ga 0.5Zr 0.1B 6Magnetic is that raw material prepares the anisotropy nanocrystalline magnet, and processing step is as follows:
(1) Nd 12.2Fe 71.8Co 9.4Ga 0.5Zr 0.1B 6The quenched powder preparation
Take metal Nd (purity is 99.5%), DT4 electrical pure iron (purity is 99.95%), ferro-boron (boron content is 19.65%), metal Co (purity is 99.5%), metal Ga(purity is 99%), metallic Z r(sponge zirconium, purity is 99.5%) be raw material, according to Nd 12.2Fe 63.8Co 17.4Ga 0.5Zr 0.1B 6Alloying component calculates the ingredients by weight (increasing the Nd of 2.5wt% during batching as compensating for loss and damage) of each raw material.Adopt SF2002-4 type vacuum intermediate-frequency induction melting furnace melting Nd Fe B alloys, before heating, first smelting furnace is evacuated to 1 * 10 -2Pa, applying argon gas is to 0.05MPa, then according to the alloying component of calculating, power added to 38kW and carries out melting, after melting completes, alloy melt poured in ingot mould, obtains plate-cast ingot after cooling.After being ground off to oxide skin, plate-cast ingot is broken for pellet; put into the copper crucible of LZK-12A type vacuum quick quenching equipment; under argon shield atmosphere; power up to flow to after 700A melts furnace charge and be poured on the copper roller that linear velocity is 32m/s; cooling rear acquisition Nd Fe B alloys strip; after crossing 300 mesh sieves and removing fine powder, obtain Nd 12.2Fe 71.8Co 9.4Ga 0.5Zr 0.1B 6Rapidly quenched magnetic powder.
(2) preparation of hydrogen disproportionation Nd-Fe-B magnetic fully
Fast quenching Nd prepared by step (1) 12.2Fe 71.8Co 9.4Ga 0.5Zr 0.1B 6Magnetic is at H 2Under atmosphere, in 820 ℃ of insulations, within 5 minutes, inhaled hydrogen-disproportionated reaction, insulation cools to room temperature with the furnace after finishing, and obtaining crystallite dimension is the complete hydrogen disproportionation Nd-Fe-B magnetic of 15-25nm;
(3) preparation of pressed compact
Part hydrogen disproportionation Nd-Fe-B magnetic prepared by step (2) is packed in mould, under argon shield, in room temperature, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 250MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B, described pressed compact is cylindrical, is of a size of φ 12mm * 12mm;
(4) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (3) is prepared is warming up to 800 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2Carry out hot compression deformation-dehydrogenation restructuring under the condition of 500Pa, described Nd-Fe-B pressed compact being applied to constant pressure, the value of exerting pressure is 3.4kN, the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact is born in thermal deformation-dehydrogenation regrouping process changes between 30MPa ~ 7MPa, the heat-insulation pressure keeping time is 30 minutes, after finishing, heat-insulation pressure keeping cools to room temperature with the furnace, the nanocrystalline Nd-Fe-B magnet of anisotropy that to obtain deflection be 77 %.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.99, and its magnetic property is: B r=0.97T, H Ci=483kA/m, (BH) m=152kJ/m 3.
Embodiment 6
The present embodiment is with fast quenching Nd 12.2Fe 81.8B 6Magnetic is that raw material prepares the anisotropy nanocrystalline magnet, and processing step is as follows:
(1) Nd 12.2Fe 81.8B 6The quenched powder preparation
Take metal Nd (purity is 99.5%), DT4 electrical pure iron (purity is 99.95%), ferro-boron (boron content is 19.65%) is raw material, according to Nd 12.2Fe 81.8B 6Alloying component calculates the ingredients by weight (increasing the Nd of 1.0wt% during batching as compensating for loss and damage) of each raw material.Adopt SF2002-4 type vacuum intermediate-frequency induction melting furnace melting Nd Fe B alloys, before heating, first smelting furnace is evacuated to 1 * 10 -2Pa, applying argon gas is to 0.05MPa, then according to the alloying component of calculating, power added to 36kW and carries out melting, after melting completes, alloy melt poured in ingot mould, obtains plate-cast ingot after cooling.After being ground off to oxide skin, plate-cast ingot is broken for pellet; put into the copper crucible of LZK-12A type vacuum quick quenching equipment; under argon shield atmosphere; power up to flow to after 650A melts furnace charge and be poured on the copper roller that linear velocity is 32m/s; cooling rear acquisition Nd Fe B alloys strip; after crossing 300 mesh sieves and removing fine powder, obtain Nd 12.2Fe 81.8B 6Rapidly quenched magnetic powder.
(2) preparation of part hydrogen disproportionation Nd-Fe-B magnetic
Fast quenching Nd prepared by step (1) 12.2Fe 81.8B 6Magnetic is at H 2Under atmosphere, within 10 minutes, inhaled hydrogen-disproportionated reaction in 780 ℃ of insulations, after inhaling hydrogen-disproportionated reaction, in vacuum degree<5.0 * 10 -2Be warming up to 820 ℃ under the Pa condition, be incubated 5 minutes and carry out dehydrogenation-recombining reaction, after insulation finishes, cool to room temperature with the furnace, the part hydrogen disproportionation products that to obtain crystallite dimension be 120-160nm (has principal phase 2:14 phase and disproportionation phase NdH x, Fe 2B, α-Fe mixes);
(3) preparation of pressed compact
Part hydrogen disproportionation Nd-Fe-B magnetic prepared by step (2) is packed in mould, under argon shield, in room temperature, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 460MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B, described pressed compact is cylindrical, is of a size of φ 13mm * 13mm;
(4) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (3) is prepared is warming up to 850 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2Carry out hot compression deformation-dehydrogenation restructuring under the condition of 50Pa, described Nd-Fe-B pressed compact being applied to constant pressure, the value of exerting pressure is 1kN, the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact is born in thermal deformation-dehydrogenation regrouping process changes between 7.5MPa ~ 1.5MPa, the heat-insulation pressure keeping time is 5 minutes, after finishing, heat-insulation pressure keeping cools to room temperature with the furnace, the nanocrystalline Nd-Fe-B magnet of anisotropy that to obtain deflection be 80 %.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.96, and magnetic property is: B r=1.03T, H Ci=398kA/m, (BH) m=166kJ/m 3.
Embodiment 7
The present embodiment is with annealing ingot casting Nd 12.2Fe 81.8B 6Magnetic is that raw material prepares the anisotropy nanocrystalline magnet, and processing step is as follows:
(1) annealing ingot casting Nd 12.2Fe 81.8B 6The preparation of magnetic
Prepare Nd according to the described method of step (1) in embodiment 6 12.2Fe 81.8B 6Plate-cast ingot, by the Nd made 12.2Fe 81.8B 6Thin plate, putting into the SDZK high-temperature vacuum sintering furnace, is evacuated to 1 * 10 -3Pass into the high-purity argon gas of 0.02MPa after Pa, be warming up to 1100 ℃ of insulation 12 h and carry out the homogenizing annealing processing under argon shield, the thin plate annealing ingot casting Mechanical Crushing that processing is obtained, cross 300 mesh sieves and remove fine powder, and ingot casting Nd obtains annealing 12.2Fe 81.8B 6Broken magnetic.
(2) preparation of part hydrogen disproportionation Nd-Fe-B magnetic
Annealing ingot casting Nd prepared by step (1) 12.2Fe 81.8B 6Broken magnetic is at H 2Under atmosphere, be heated to 750 ℃ of insulations and within 30 minutes, inhaled hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, in vacuum degree<5 * 10 -2Be warming up to 800 ℃ of insulations under the condition of Pa and within 5 minutes, carry out dehydrogenation-recombining reaction, insulation cools to room temperature with the furnace after finishing, and the part hydrogen disproportionation Nd-Fe-B magnetic that to obtain crystallite dimension be 120-160nm (contains principal phase 2:14 phase and disproportionation phase NdH x, Fe 2B, α-Fe);
(3) preparation of pressed compact
Part hydrogen disproportionation Nd-Fe-B magnetic prepared by step (2) is packed in mould, under argon shield, in room temperature, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 270MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B, described pressed compact is cylindrical, is of a size of φ 11mm * 11mm;
(4) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (3) is prepared is warming up to 780 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2Carry out hot compression deformation-dehydrogenation restructuring under the condition of 200Pa, described Nd-Fe-B pressed compact being applied to constant pressure, the value of exerting pressure is 1.2kN, the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact is born in thermal deformation-dehydrogenation regrouping process changes between 13MPa ~ 3MPa, the heat-insulation pressure keeping time is 30 minutes, after finishing, heat-insulation pressure keeping cools to room temperature with the furnace, the nanocrystalline Nd-Fe-B magnet of anisotropy that to obtain deflection be 75.6 %.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.90, and its magnetic property is: B r=1.2 T, H Ci=530 kA/m, (BH) m=234 kJ/m 3.
Embodiment 8
The present embodiment is with annealing ingot casting Nd 12.2Fe 71.8Co 9.4Ga 0.5Zr 0.1B 6Magnetic is that raw material prepares the anisotropy nanocrystalline magnet, and processing step is as follows:
(1) annealing ingot casting Nd 12.2Fe 71.8Co 9.4Ga 0.5Zr 0.1B 6Magnetic
Prepare Nd according to the described method of step (1) in embodiment 5 12.2Fe 71.8Co 9.4Ga 0.5Zr 0.1B 6Plate-cast ingot, by the Nd made 12.2Fe 71.8Co 9.4Ga 0.5Zr 0.1B 6Thin plate, putting into the SDZK high-temperature vacuum sintering furnace, is evacuated to 1 * 10 -3Pass into the high-purity argon gas of 0.02MPa after Pa, be warming up to 1120 ℃ of insulations and within 16 hours, carry out the homogenizing annealing processing under argon shield, the thin plate that processing is obtained annealing ingot casting Mechanical Crushing, cross 300 mesh sieves and remove fine powder, and ingot casting Nd must anneal 12.2Fe 71.8Co 9.4Ga 0.5Zr 0.1B 6Magnetic.
(2) preparation of part hydrogen disproportionation Nd-Fe-B magnetic
Annealing ingot casting Nd prepared by step (1) 12.2Fe 71.8Co 9.4Ga 0.5Zr 0.1B 6Magnetic is at H 2Under atmosphere, be heated to 800 ℃ of insulations and within 10 minutes, inhaled hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, in vacuum degree<5 * 10 -2Be warming up to 820 ℃ of insulations under the condition of Pa and within 3 minutes, carry out dehydrogenation-recombining reaction, insulation cools to room temperature with the furnace after finishing, and obtains the part hydrogen disproportionation Nd-Fe-B magnetic that crystallite dimension is less than 140-160nm and (contains principal phase 2:14 phase and disproportionation phase NdH x, Fe 2B, α-Fe);
(3) preparation of pressed compact
Part hydrogen disproportionation Nd-Fe-B magnetic prepared by step (2) is packed in mould, under argon shield, in room temperature, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 150MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B, described pressed compact is cylindrical, is of a size of φ 10mm * 10mm;
(4) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (3) is prepared is warming up to 750 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2Carry out hot compression deformation-dehydrogenation restructuring under the condition of 100Pa, described Nd-Fe-B pressed compact being applied to constant pressure, the value of exerting pressure is 1.6kN, the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact is born in thermal deformation-dehydrogenation regrouping process changes between 20MPa ~ 6.5MPa, the heat-insulation pressure keeping time is 30 minutes, after finishing, heat-insulation pressure keeping cools to room temperature with the furnace, the nanocrystalline Nd-Fe-B magnet of anisotropy that to obtain deflection be 68 %.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.90, and its magnetic property is: B r=1.14T, H Ci=490 kA/m, (BH) m=190 kJ/m 3.
Embodiment 9
The present embodiment is with annealing ingot casting Nd 13.5Fe 73Co 7.5B 6Magnetic is that raw material prepares the anisotropy nanocrystalline magnet, and processing step is as follows:
(1) annealing ingot casting Nd 13.5Fe 73Co 7.5B 6Magnetic
Prepare Nd according to the described method of step (1) in embodiment 1 13.5Fe 73Co 7.5B 6Plate-cast ingot, by the Nd made 13.5Fe 73Co 7.5B 6Thin plate, putting into the SDZK high-temperature vacuum sintering furnace, is evacuated to 1 * 10 -3Pass into the high-purity argon gas of 0.02MPa after Pa, be warming up to 1100 ℃ of insulations and within 14 hours, carry out the homogenizing annealing processing under argon shield, the thin plate that processing is obtained annealing ingot casting Mechanical Crushing, cross 300 mesh sieves and remove fine powder, and ingot casting Nd must anneal 13.5Fe 73Co 7.5B 6Magnetic.
(2) preparation of part hydrogen disproportionation Nd-Fe-B magnetic
Annealing ingot casting Nd prepared by step (1) 13.5Fe 73Co 7.5B 6Magnetic is at H 2Under atmosphere, be heated to 780 ℃ of insulations and within 15 minutes, inhaled hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, in vacuum degree<5 * 10 -2Be warming up to 820 ℃ of insulations under the condition of Pa and within 3 minutes, carry out dehydrogenation-recombining reaction, insulation cools to room temperature with the furnace after finishing, and the part hydrogen disproportionation Nd-Fe-B magnetic that obtains crystallite dimension 160-180nm (contains principal phase 2:14 phase and disproportionation phase NdH x, Fe 2B, α-Fe);
(3) preparation of pressed compact
Part hydrogen disproportionation Nd-Fe-B magnetic prepared by step (2) is packed in mould, under argon shield, in room temperature, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 400MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B, described pressed compact is cylindrical, is of a size of φ 10mm * 10mm;
(4) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (3) is prepared is warming up to 680 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2Carry out hot compression deformation-dehydrogenation restructuring under the condition of 1kPa, described Nd-Fe-B pressed compact being applied to constant pressure, the value of exerting pressure is 1.8kN, the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact is born in thermal deformation-dehydrogenation regrouping process changes between 22MPa ~ 7MPa, the heat-insulation pressure keeping time is 120 minutes, after finishing, heat-insulation pressure keeping cools to room temperature with the furnace, the nanocrystalline Nd-Fe-B magnet of anisotropy that to obtain deflection be 65 %.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.86, and magnetic property is: B r=0.96 T, H Ci=557kA/m, (BH) m=162 kJ/m 3.
Embodiment 10
The present embodiment is with annealing ingot casting Nd 13.62Fe 75.7Co 4.45Ga 0.47B 5.76Magnetic is that raw material prepares the anisotropy nanocrystalline magnet, and processing step is as follows:
(1) annealing ingot casting Nd 13.62Fe 75.7Co 4.45Ga 0.47B 5.76Preparation
Take metal Nd (purity is 99.5%), DT4 electrical pure iron (purity is 99.95%), ferro-boron (boron content is 19.65%), metal Co (purity is 99.5%), metal Ga(purity is 99%) be raw material, according to Nd 12.2Fe 63.8Co 17.4Ga 0.5Zr 0.1B 6Alloying component calculates the ingredients by weight (increasing the Nd of 2.5wt% during batching as compensating for loss and damage) of each raw material.Adopt SF2002-4 type vacuum intermediate-frequency induction melting furnace melting Nd Fe B alloys, before heating, first smelting furnace is evacuated to 1 * 10 -2Pa, applying argon gas is to 0.05MPa, then according to the alloying component of calculating, power added to 38kW and carries out melting, after melting completes, alloy melt poured in ingot mould, obtains plate-cast ingot after cooling.By the Nd made 13.62Fe 75.7Co 4.45Ga 0.47B 5.76Thin plate, putting into the SDZK high-temperature vacuum sintering furnace, is evacuated to 1 * 10 -3Pass into the high-purity argon gas of 0.02MPa after Pa, be warming up to 1120 ℃ of insulations and within 14 hours, carry out the homogenizing annealing processing under argon shield, the thin plate that processing is obtained annealing ingot casting Mechanical Crushing, cross 300 mesh sieves and remove fine powder, and ingot casting Nd must anneal 13.62Fe 75.7Co 4.45Ga 0.47B 5.76Magnetic.
(2) preparation of hydrogen disproportionation Nd-Fe-B magnetic fully
Annealing ingot casting Nd prepared by step (1) 13.62Fe 75.7Co 4.45Ga 0.47B 5.76Magnetic is at H 2Under atmosphere, in 800 ℃ of insulations, within 15 minutes, inhaled hydrogen-disproportionated reaction, insulation cools to room temperature with the furnace after finishing, and obtaining crystallite dimension is the complete hydrogen disproportionation Nd-Fe-B magnetic of 40-90nm;
(3) preparation of pressed compact
Complete hydrogen disproportionation Nd-Fe-B magnetic prepared by step (2) is packed in mould, under argon shield, in room temperature, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 420MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B, described pressed compact is cylindrical, is of a size of φ 12mm * 12mm;
(4) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (3) is prepared is warming up to 750 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2Carry out hot compression deformation-dehydrogenation restructuring under the condition of 30Pa, described Nd-Fe-B pressed compact being applied to constant pressure, the value of exerting pressure is 3.5kN, the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact is born in thermal deformation-dehydrogenation regrouping process changes between 30MPa ~ 9MPa, the heat-insulation pressure keeping time is 45 minutes, after finishing, heat-insulation pressure keeping cools to room temperature with the furnace, the nanocrystalline Nd-Fe-B magnet of anisotropy that to obtain deflection be 70 %.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.91, and its magnetic property is: B r=0.93T, H Ci=600kA/m, (BH) m=159kJ/m 3.
Embodiment 11
The present embodiment is with annealing ingot casting Nd 13.5Fe 80.4Ga 0.5B 5.6Magnetic is that raw material prepares the anisotropy nanocrystalline magnet, and processing step is as follows:
(1) annealing ingot casting Nd 13.5Fe 80.4Ga 0.5B 5.6Preparation
Prepare Nd according to the described method of step (1) in embodiment 2 13.5Fe 80.4Ga 0.5B 5.6Plate-cast ingot, by the Nd made 13.5Fe 80.4Ga 0.5B 5.6Thin plate putting into the SDZK high-temperature vacuum sintering furnace, be evacuated to 1 * 10 -3Pass into the high-purity argon gas of 0.02MPa after Pa, be warming up to 1080 ℃ of insulations and within 12 hours, carry out the homogenizing annealing processing under argon shield, the thin plate that processing is obtained annealing ingot casting Mechanical Crushing, cross 300 mesh sieves and remove fine powder, and ingot casting Nd must anneal 13.5Fe 80.4Ga 0.5B 5.6Magnetic.
(2) preparation of hydrogen disproportionation Nd-Fe-B magnetic fully
Annealing ingot casting Nd prepared by step (1) 13.5Fe 80.4Ga 0.5B 5.6Magnetic is at H 2Under atmosphere, in 780 ℃ of insulations, within 25 minutes, inhaled hydrogen-disproportionated reaction, insulation cools to room temperature with the furnace after finishing, and obtaining crystallite dimension is the complete hydrogen disproportionation Nd-Fe-B magnetic of 80-120nm;
(3) preparation of pressed compact
Complete hydrogen disproportionation Nd-Fe-B magnetic prepared by step (2) is packed in mould, under argon shield, in room temperature, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 600MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B, described pressed compact is cylindrical, is of a size of φ 12mm * 12mm;
(4) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (3) is prepared is warming up to 800 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2Carry out hot compression deformation-dehydrogenation restructuring under the condition of 10Pa, described Nd-Fe-B pressed compact being applied to constant pressure, the value of exerting pressure is 2kN, the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact is born in thermal deformation-dehydrogenation regrouping process changes between 20MPa ~ 6MPa, the heat-insulation pressure keeping time is 10 minutes, after finishing, heat-insulation pressure keeping cools to room temperature with the furnace, the nanocrystalline Nd-Fe-B magnet of anisotropy that to obtain deflection be 67 %.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.96, and magnetic property is: B r=0.86T, H Ci=530kA/m, (BH) m=125 kJ/m 3.
Embodiment 12
The present embodiment is with annealing ingot casting Nd 14Fe 76Co 3Zr 1B 6Magnetic is that raw material prepares the anisotropy nanocrystalline magnet, and processing step is as follows:
(1) annealing ingot casting Nd 14Fe 76Co 3Zr 1B 6Preparation
Take metal Nd (purity is 99.5%), DT4 electrical pure iron (purity is 99.95%), ferro-boron (boron content is 19.65%), metal Co (purity is 99.5%), metallic Z r(sponge zirconium, purity is 99.5%) be raw material, according to Nd 14Fe 76Co 3Zr 1B 6Alloying component calculates the ingredients by weight (increasing the Nd of 2.0wt% during batching as compensating for loss and damage) of each raw material.Adopt SF2002-4 type vacuum intermediate-frequency induction melting furnace melting Nd Fe B alloys, before heating, first smelting furnace is evacuated to 10 -2Pa, applying argon gas is to 0.05MPa, then according to the alloying component of calculating, power added to 38kW and carries out melting, after melting completes, alloy melt poured in ingot mould, obtains plate-cast ingot after cooling.By the Nd made 14Fe 76Co 3Zr 1B 6Thin plate putting into the SDZK high-temperature vacuum sintering furnace, be evacuated to 1 * 10 -3Pass into the high-purity argon gas of 0.02MPa after Pa, be warming up to 1160 ℃ of insulations and within 16 hours, carry out the homogenizing annealing processing under argon shield, the thin plate that processing is obtained annealing ingot casting Mechanical Crushing, cross 300 mesh sieves and remove fine powder, and ingot casting Nd must anneal 14Fe 76Co 3Zr 1B 6Magnetic.
(2) preparation of hydrogen disproportionation Nd-Fe-B magnetic fully
Annealing ingot casting Nd prepared by step (1) 14Fe 76Co 3Zr 1B 6Magnetic is at H 2Under atmosphere, in 750 ℃ of insulations, within 60 minutes, inhaled hydrogen-disproportionated reaction, insulation cools to room temperature with the furnace after finishing, and obtains the complete hydrogen disproportionation Nd-Fe-B magnetic of crystallite dimension 140-160nm;
(3) preparation of pressed compact
Complete hydrogen disproportionation Nd-Fe-B magnetic prepared by step (2) is packed in mould, under argon shield, in room temperature, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 500MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B, described pressed compact is cylindrical, is of a size of φ 12mm * 12mm;
(4) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (3) is prepared is warming up to 780 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2Carry out hot compression deformation-dehydrogenation restructuring under the condition of 30Pa, described Nd-Fe-B pressed compact being applied to constant pressure, the value of exerting pressure is 1.6kN, the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact is born in thermal deformation-dehydrogenation regrouping process changes between 14MPa ~ 4MPa, the heat-insulation pressure keeping time is 15 minutes, after finishing, heat-insulation pressure keeping cools to room temperature with the furnace, the nanocrystalline Nd-Fe-B magnet of anisotropy that to obtain deflection be 72 %.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.93, and its magnetic property is: B r=0.98T, H Ci=557.7kA/m, (BH) m=172kJ/m 3.
Embodiment 13
The present embodiment is with fast quenching Nd 12.5Fe 80.5Nb 1B 6Magnetic is that raw material prepares the anisotropy nanocrystalline magnet, and processing step is as follows:
(1) Nd 12.5Fe 80.5Nb 1B 6The preparation of quenched powder
Take metal Nd (purity is 99.5%), DT4 electrical pure iron (purity is 99.95%), ferro-boron (boron content is 19.65%), ferro-niobium (Nb content is 50%) is raw material, according to Nd 12.5Fe 80.5Nb 1B 6Alloying component, calculate the ingredients by weight (increasing the Nd of 2.0wt% during batching as compensating for loss and damage) of each raw material.Adopt SF2002-4 type vacuum intermediate-frequency induction melting furnace melting Nd Fe B alloys, before heating, first smelting furnace is evacuated to 1 * 10 -2Pa, applying argon gas is to 0.05MPa, then according to the alloying component of calculating, power added to the 36kW melting, after melting completes, alloy melt poured in ingot mould, obtains plate-cast ingot after cooling.After being ground off to oxide skin, plate-cast ingot is broken for pellet; put into the copper crucible of LZK-12A type vacuum quick quenching equipment; under argon shield atmosphere; power up to flow to after 650A melts furnace charge and be poured on the copper roller that linear velocity is 32m/s; cooling rear acquisition Nd Fe B alloys strip; after crossing 300 mesh sieves and removing fine powder, obtain Nd 12.5Fe 80.5Nb 1B 6Rapidly quenched magnetic powder.
(2) preparation of hydrogen disproportionation Nd-Fe-B magnetic fully
Fast quenching Nd prepared by step (1) 12.5Fe 80.5Nb 1B 6Magnetic is at H 2Under atmosphere, in 780 ℃ of insulations, within 30 minutes, inhaled hydrogen-disproportionated reaction, insulation cools to room temperature with the furnace after finishing, and obtaining crystallite dimension is the complete hydrogen disproportionation Nd-Fe-B magnetic of 110-150nm;
(3) preparation of pressed compact
Complete hydrogen disproportionation Nd-Fe-B magnetic prepared by step (2) is packed in mould, under argon shield, in room temperature, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 250MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B, described pressed compact is cylindrical, is of a size of φ 12.5mm * 12.5mm;
(4) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (3) is prepared is warming up to 850 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2Carry out hot compression deformation-dehydrogenation restructuring under the condition of 0.0005Pa, described Nd-Fe-B pressed compact being applied to constant pressure, the value of exerting pressure is 3.7kN, the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact is born in thermal deformation-dehydrogenation regrouping process changes between 30MPa ~ 7.5MPa, the heat-insulation pressure keeping time is 10 minutes, after finishing, heat-insulation pressure keeping cools to room temperature with the furnace, the nanocrystalline Nd-Fe-B magnet of anisotropy that to obtain deflection be 75 %.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.97, and magnetic property is: B r=1.13T, H Ci=358kA/m, (BH) m=158kJ/m 3.
Embodiment 14
The present embodiment is with annealing ingot casting Nd 12.6Fe 72.3Co 8.6Al 0.5B 6.0Magnetic is that raw material prepares the anisotropy nanocrystalline magnet, and processing step is as follows:
(1) annealing ingot casting Nd 12.6Fe 72.3Co 8.6Al 0.5B 6.0The preparation of magnetic
Take metal Nd (purity is 99.5%), DT4 electrical pure iron (purity is 99.95%), ferro-boron (boron content is 19.65%), metal Co (purity is 99.5%), metal A l(purity is 99%) be raw material, according to Nd 12.6Fe 72.3Co 8.6Al 0.5B 6.0Alloying component calculates the ingredients by weight (increase the Nd of 2.5wt% during batching, 3% Al is as compensating for loss and damage) of each raw material.Adopt SF2002-4 type vacuum intermediate-frequency induction melting furnace melting Nd Fe B alloys, before heating, first smelting furnace is evacuated to 10 -2Pa, applying argon gas is to 0.05MPa, then according to the alloying component of calculating, power added to 38kW and carries out melting, after melting completes, alloy melt poured in ingot mould, obtains plate-cast ingot after cooling.By the Nd made 12.6Fe 72.3Co 8.6Al 0.5B 6.0Thin plate putting into the SDZK high-temperature vacuum sintering furnace, be evacuated to 1 * 10 -3Pass into the high-purity argon gas of 0.02MPa after Pa, be warming up to 1140 ℃ of insulations and within 16 hours, carry out the homogenizing annealing processing under argon shield, the thin plate that processing is obtained annealing ingot casting Mechanical Crushing, cross 300 mesh sieves and remove fine powder, and ingot casting Nd must anneal 12.6Fe 72.3Co 8.6Al 0.5B 6.0Magnetic.
(2) preparation of part hydrogen disproportionation Nd-Fe-B magnetic
Annealing ingot casting Nd prepared by step (1) 12.6Fe 72.3Co 8.6Al 0.5B 6.0Magnetic is at H 2Under atmosphere, be heated to 800 ℃ of insulations and within 15 minutes, inhaled hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, in vacuum degree<5 * 10 -2Be warming up to 820 ℃ of insulations under the condition of Pa and within 5 minutes, carry out dehydrogenation-recombining reaction, insulation cools to room temperature with the furnace after finishing, and the part hydrogen disproportionation Nd-Fe-B magnetic that to obtain crystallite dimension be 160-200nm (contains principal phase 2:14 phase and disproportionation phase NdH x, Fe 2B, α-Fe);
(3) preparation of pressed compact
Part hydrogen disproportionation Nd-Fe-B magnetic prepared by step (2) is packed in mould, under argon shield, in room temperature, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 500MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B, described pressed compact is cylindrical, is of a size of φ 12mm * 12mm;
(4) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (3) is prepared is warming up to 750 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2Carry out hot compression deformation-dehydrogenation restructuring under the condition of 500Pa, described Nd-Fe-B pressed compact being applied to constant pressure, the value of exerting pressure is 2.8kN, the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact is born in thermal deformation-dehydrogenation regrouping process changes between 25MPa ~ 8MPa, the heat-insulation pressure keeping time is 30 minutes, after finishing, heat-insulation pressure keeping cools to room temperature with the furnace, the nanocrystalline Nd-Fe-B magnet of anisotropy that to obtain deflection be 68.5 %.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.89, and its magnetic property is: B r=1.07T, H Ci=500 kA/m, (BH) m=205 kJ/m 3.
Embodiment 15
The present embodiment is with annealing ingot casting Nd 15Fe 78Mo 1B 6Magnetic is that raw material prepares the anisotropy nanocrystalline magnet, and processing step is as follows:
(1) annealing ingot casting Nd 15Fe 78Mo 1B 6Preparation
Take metal Nd (purity is 99.5%), DT4 electrical pure iron (purity is 99.95%), ferro-boron (boron content is 19.65%), molybdenum-iron (Mo content is 60%) is raw material, according to Nd 15Fe 78Mo 1B 6Alloying component calculates the ingredients by weight (increasing the Nd of 2.5wt% during batching as compensating for loss and damage) of each raw material.Adopt SF2002-4 type vacuum intermediate-frequency induction melting furnace melting Nd Fe B alloys, before heating, first smelting furnace is evacuated to 10 -2Pa, applying argon gas is to 0.05MPa, then according to the alloying component of calculating, power added to 40kW and carries out melting, after melting completes, alloy melt poured in ingot mould, obtains plate-cast ingot after cooling.By the Nd made 15Fe 78Mo 1B 6Thin plate putting into the SDZK high-temperature vacuum sintering furnace, be evacuated to 1 * 10 -3Pass into the high-purity argon gas of 0.02MPa after Pa, be warming up to 1200 ℃ of insulations and within 16 hours, carry out the homogenizing annealing processing under argon shield, the thin plate that processing is obtained annealing ingot casting Mechanical Crushing, cross 300 mesh sieves and remove fine powder, and ingot casting Nd must anneal 15Fe 78Mo 1B 6Magnetic.
(2) preparation of hydrogen disproportionation Nd-Fe-B magnetic fully
Annealing ingot casting Nd prepared by step (1) 15Fe 78Mo 1B 6Magnetic is at H 2Under atmosphere, in 820 ℃ of insulations, within 30 minutes, inhaled hydrogen-disproportionated reaction, insulation cools to room temperature with the furnace after finishing, and obtaining crystallite dimension is the complete hydrogen disproportionation Nd-Fe-B magnetic of 200-250nm;
(3) preparation of pressed compact
Complete hydrogen disproportionation Nd-Fe-B magnetic prepared by step (2) is packed in mould, under argon shield, in room temperature, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 550MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B, described pressed compact is cylindrical, is of a size of φ 13mm * 13mm;
(4) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (3) is prepared is warming up to 850 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2Carry out hot compression deformation-dehydrogenation restructuring under the condition of 0.001Pa, described Nd-Fe-B pressed compact being applied to constant pressure, the value of exerting pressure is 3.3kN, the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact is born in thermal deformation-dehydrogenation regrouping process changes between 25MPa ~ 5MPa, the heat-insulation pressure keeping time is 20 minutes, after finishing, heat-insulation pressure keeping cools to room temperature with the furnace, the nanocrystalline Nd-Fe-B magnet of anisotropy that to obtain deflection be 81 %.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.97, and magnetic property is: B r=1.02T, H Ci=320kA/m, (BH) m=155kJ/m 3.
Embodiment 16
The present embodiment is with fast quenching Nd 13.5Fe 79.96Al 0.24Nb 0.3B 6Magnetic is that raw material prepares the anisotropy nanocrystalline magnet, and processing step is as follows:
(1) Nd 13.5Fe 79.96Al 0.24Nb 0.3B 6The preparation of quenched powder
Take metal Nd (purity is 99.5%), DT4 electrical pure iron (purity is 99.95%), ferro-boron (boron content is 19.65%), ferro-niobium (Nb content is 50%), metal A l(purity is 99%) be raw material, according to Nd 13.5Fe 79.96Al 0.24Nb 0.3B 6Alloying component calculates the ingredients by weight (increase the Nd of 2.0wt% during batching, the Al of 3.0wt% is as compensating for loss and damage) of each raw material.Adopt SF2002-4 type vacuum intermediate-frequency induction melting furnace melting Nd Fe B alloys, before heating, first smelting furnace is evacuated to 10 -2Pa; applying argon gas is to 0.05MPa; then according to the alloying component of calculating, power is added to 34kW and carry out melting; after melting completes, alloy melt is poured in ingot mould; obtain plate-cast ingot after cooling; after being ground off to oxide skin, plate-cast ingot is broken for pellet; put into the copper crucible of LZK-12A type vacuum quick quenching equipment; under argon shield atmosphere; power up to flow to after 650A melts furnace charge and be poured on the copper roller that linear velocity is 32m/s; cooling rear acquisition Nd Fe B alloys strip, after 300 mesh sieves remove fine powder excessively, obtain Nd 13.5Fe 79.96Al 0.24Nb 0.3B 6Rapidly quenched magnetic powder.
(2) preparation of part hydrogen disproportionation Nd-Fe-B magnetic
Annealing ingot casting Nd prepared by step (1) 13.5Fe 79.96Al 0.24Nb 0.3B 6Magnetic is at H 2Under atmosphere, be heated to 780 ℃ of insulations and within 40 minutes, inhaled hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, in vacuum degree<5 * 10 -2Be warming up to 800 ℃ of insulations under the condition of Pa and within 6 minutes, carry out dehydrogenation-recombining reaction, insulation cools to room temperature with the furnace after finishing, and the part hydrogen disproportionation Nd-Fe-B magnetic that to obtain crystallite dimension be 250-270nm (contains principal phase 2:14 phase and disproportionation phase NdH x, Fe 2B, α-Fe);
(3) preparation of pressed compact
Part hydrogen disproportionation Nd-Fe-B magnetic prepared by step (2) is packed in mould, under argon shield, in room temperature, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 300MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B, described pressed compact is cylindrical, is of a size of φ 10mm * 10mm;
(4) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (3) is prepared is warming up to 820 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2Carry out hot compression deformation-dehydrogenation restructuring under the condition of 0.001Pa, described Nd-Fe-B pressed compact being applied to constant pressure, the value of exerting pressure is 1.4kN, the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact is born in thermal deformation-dehydrogenation regrouping process changes between 17.5MPa ~ 4MPa, the heat-insulation pressure keeping time is 30 minutes, after finishing, heat-insulation pressure keeping cools to room temperature with the furnace, the nanocrystalline Nd-Fe-B magnet of anisotropy that to obtain deflection be 77 %.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.92, and magnetic property is: B r=1.04T, H Ci=590kA/m, (BH) m=190kJ/m 3.
Embodiment 17
The present embodiment is with annealing ingot casting Nd 13Fe 71.86Co 9Al 0.08Cu 0.06B 6Magnetic is that raw material prepares the anisotropy nanocrystalline magnet, and processing step is as follows:
(1) annealing ingot casting Nd 13Fe 71.86Co 9Al 0.08Cu 0.06B 6Preparation
Take metal Nd (purity is 99.5%), DT4 electrical pure iron (purity is 99.95%), ferro-boron (boron content is 19.65%), metal A l(purity is 99%), metal Cu(purity is 99%), metal Co (purity is 99.5%) is raw material, according to Nd 13Fe 71.86Co 9Al 0.08Cu 0.06B 6Alloying component calculates the ingredients by weight (increase the Nd of 3.0wt% during batching, the Al of 3.0wt% is as compensating for loss and damage) of each raw material.Adopt SF2002-4 type vacuum intermediate-frequency induction melting furnace melting Nd Fe B alloys, before heating, first smelting furnace is evacuated to 10 -2Pa, applying argon gas is to 0.05MPa, then according to the alloying component of calculating, power added to 38kW and carries out melting, after melting completes, alloy melt poured in ingot mould, obtains plate-cast ingot after cooling.By the Nd made 13Fe 71.86Co 9Al 0.08Cu 0.06B 6Thin plate putting into the SDZK high-temperature vacuum sintering furnace, be evacuated to 1 * 10 -3Pass into the high-purity argon gas of 0.02MPa after Pa, be warming up to 1150 ℃ of insulations and within 18 hours, carry out the homogenizing annealing processing under argon shield, the thin plate that processing is obtained annealing ingot casting Mechanical Crushing, cross 300 mesh sieves and remove fine powder, and ingot casting Nd must anneal 13Fe 71.86Co 9Al 0.08Cu 0.06B 6Magnetic.
(2) preparation of hydrogen disproportionation Nd-Fe-B magnetic fully
Annealing ingot casting Nd prepared by step (1) 13Fe 71.86Co 9Al 0.08Cu 0.06B 6Magnetic is at H 2Under atmosphere, in 800 ℃ of insulations, within 45 minutes, inhaled hydrogen-disproportionated reaction, insulation cools to room temperature with the furnace after finishing, and obtaining crystallite dimension is the complete hydrogen disproportionation Nd-Fe-B magnetic of 200-220nm;
(3) preparation of pressed compact
Part hydrogen disproportionation Nd-Fe-B magnetic prepared by step (2) is packed in mould, under argon shield, in room temperature, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 550MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B, described pressed compact is cylindrical, is of a size of φ 13mm * 13mm;
(4) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (3) is prepared is warming up to 820 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2Carry out hot compression deformation-dehydrogenation restructuring under the condition of 30Pa, described Nd-Fe-B pressed compact being applied to constant pressure, the value of the exerting pressure 3.2kN of institute, the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact is born in thermal deformation-dehydrogenation regrouping process changes between 24MPa ~ 5.4MPa, the heat-insulation pressure keeping time is 30 minutes, after finishing, heat-insulation pressure keeping cools to room temperature with the furnace, the nanocrystalline Nd-Fe-B magnet of anisotropy that to obtain deflection be 78 %.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.95, and magnetic property is: B r=1.10T, H Ci=450kA/m, (BH) m=185kJ/m 3.
Embodiment 18
The present embodiment is with annealing ingot casting Nd 14.5Fe 76.4Ti 2.5Cr 1B 5.6Magnetic is that raw material prepares the anisotropy nanocrystalline magnet, and processing step is as follows:
(1) annealing ingot casting Nd 14.5Fe 76.4Ti 2.5Cr 1B 5.6Preparation
Take metal Nd (purity is 99.5%), DT4 electrical pure iron (purity is 99.95%), ferro-boron (boron content is 19.65%), ferrotianium (Ti content 30.0%), ferrochrome (Cr content is 65.0%) is raw material, according to Nd 14.5Fe 76.4Ti 2.5Cr 1B 5.6Alloying component calculates the ingredients by weight (increasing the Nd of 3wt% during batching as compensating for loss and damage) of each raw material.Adopt SF2002-4 type vacuum intermediate-frequency induction melting furnace melting Nd Fe B alloys, before heating, first smelting furnace is evacuated to 10 -2Pa, applying argon gas is to 0.05MPa, then according to the alloying component of calculating, power added to 40kW and carries out melting, after melting completes, alloy melt poured in ingot mould, obtains plate-cast ingot after cooling.By the Nd made 14.5Fe 76.4Ti 2.5Cr 1B 5.6Thin plate putting into the SDZK high-temperature vacuum sintering furnace, be evacuated to 1 * 10 -3Pass into the high-purity argon gas of 0.02MPa after Pa, be warming up to 1200 ℃ of insulations and within 22 hours, carry out the homogenizing annealing processing under argon shield, the thin plate that processing is obtained annealing ingot casting Mechanical Crushing, cross 300 mesh sieves and remove fine powder, and ingot casting Nd must anneal 14.5Fe 76.4Ti 2.5Cr 1B 5.6Magnetic.
(2) preparation of part hydrogen disproportionation Nd-Fe-B magnetic
Annealing ingot casting Nd prepared by step (1) 14.5Fe 76.4Ti 2.5Cr 1B 5.6Magnetic is at H 2Under atmosphere, be heated to 800 ℃ of insulations and within 30 minutes, inhaled hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, in vacuum degree<5 * 10 -2Be warming up to 820 ℃ of insulations under the condition of Pa and within 7 minutes, carry out dehydrogenation-recombining reaction, insulation cools to room temperature with the furnace after finishing, and the part hydrogen disproportionation Nd-Fe-B magnetic that to obtain crystallite dimension be 220-270nm (contains principal phase 2:14 phase and disproportionation phase NdH x, Fe 2B, α-Fe);
(3) preparation of pressed compact
Part hydrogen disproportionation Nd-Fe-B magnetic prepared by step (2) is packed in mould, under argon shield, in room temperature, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 550MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B, described pressed compact is cylindrical, is of a size of φ 12mm * 12mm;
(4) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (3) is prepared is warming up to 820 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2Carry out hot compression deformation-dehydrogenation restructuring under the condition of 10Pa, described Nd-Fe-B pressed compact being applied to constant pressure, the value of the exerting pressure 3kN of institute, the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact is born in thermal deformation-dehydrogenation regrouping process changes between 26MPa ~ 5.5MPa, the heat-insulation pressure keeping time is 35 minutes, after finishing, heat-insulation pressure keeping cools to room temperature with the furnace, the nanocrystalline Nd-Fe-B magnet of anisotropy that to obtain deflection be 78 %.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.96, and its magnetic property is: B r=1.17T, H Ci=650 kA/m, (BH) m=249 kJ/m 3.
Embodiment 19
The present embodiment is with fast quenching Nd 14Fe 79.4Al 0.6B 6Magnetic is that raw material prepares the anisotropy nanocrystalline magnet, and processing step is as follows:
(1) Nd 14Fe 79.4Al 0.6B 6The preparation of quenched powder
Take metal Nd (purity is 99.5%), DT4 electrical pure iron (purity is 99.95%), ferro-boron (boron content is 19.65%), metal A l(purity is 99%) be raw material, according to Nd 14Fe 79.4Al 0.6B 6Alloying component calculates the ingredients by weight (increase the Nd of 2.0wt% during batching, the Al of 3.0wt% is as compensating for loss and damage) of each raw material.Adopt SF2002-4 type vacuum intermediate-frequency induction melting furnace melting Nd Fe B alloys, before heating, first smelting furnace is evacuated to 10 -2Pa, applying argon gas is to 0.05MPa, then according to the alloying component of calculating, power added to 32kW and carries out melting, after melting completes, alloy melt poured in ingot mould, obtains plate-cast ingot after cooling.After being ground off to oxide skin, plate-cast ingot is broken for pellet; put into the copper crucible of LZK-12A type vacuum quick quenching equipment; under argon shield atmosphere; power up to flow to after 650A melts furnace charge and be poured on the copper roller that linear velocity is 34m/s; cooling rear acquisition Nd Fe B alloys strip; after crossing 300 mesh sieves and removing fine powder, obtain Nd 14Fe 79.4Al 0.6B 6Rapidly quenched magnetic powder.
(2) preparation of part hydrogen disproportionation Nd-Fe-B magnetic
Annealing ingot casting Nd prepared by step (1) 14Fe 79.4Al 0.6B 6Magnetic is at H 2Under atmosphere, be heated to 780 ℃ of insulations and within 45 minutes, inhaled hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, in vacuum degree<5 * 10 -2Be warming up to 820 ℃ of insulations under the condition of Pa and within 5 minutes, carry out dehydrogenation-recombining reaction, insulation cools to room temperature with the furnace after finishing, and the part hydrogen disproportionation Nd-Fe-B magnetic that to obtain crystallite dimension be 250-280nm (contains principal phase 2:14 phase and disproportionation phase NdH x, Fe 2B, α-Fe);
(3) preparation of pressed compact
Part hydrogen disproportionation Nd-Fe-B magnetic prepared by step (2) is packed in mould, under argon shield, in room temperature, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 300MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B, described pressed compact is cylindrical, is of a size of φ 12.5mm * 12.5mm;
(4) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (3) is prepared is warming up to 850 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2Carry out hot compression deformation-dehydrogenation restructuring under the condition of 0.0001Pa, described Nd-Fe-B pressed compact being applied to constant pressure, the value of exerting pressure is 3kN, the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact is born in thermal deformation-dehydrogenation regrouping process changes between 24MPa ~ 5MPa, the heat-insulation pressure keeping time is 20 minutes, after finishing, heat-insulation pressure keeping cools to room temperature with the furnace, the nanocrystalline Nd-Fe-B magnet of anisotropy that to obtain deflection be 80%.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.97, and magnetic property is: B r=1.01T, H Ci=297kA/m, (BH) m=125kJ/m 3.
Embodiment 20
The present embodiment is with annealing ingot casting Nd 15Fe 77.9Cu 1.5B 5.6Magnetic is that raw material prepares the anisotropy nanocrystalline magnet, and processing step is as follows:
(1) annealing ingot casting Nd 15Fe 77.9Cu 1.5B 5.6Preparation
Take metal Nd (purity is 99.5%), DT4 electrical pure iron (purity is 99.95%), ferro-boron (boron content is 19.65%), metal Cu(purity is 99%) be raw material, according to Nd 15Fe 77.9Cu 1.5B 5.6Alloying component calculates the ingredients by weight (increasing the Nd of 3wt% during batching as compensating for loss and damage) of each raw material.Adopt SF2002-4 type vacuum intermediate-frequency induction melting furnace melting Nd Fe B alloys, before heating, first smelting furnace is evacuated to 10 -2Pa, applying argon gas is to 0.05MPa, then according to the alloying component of calculating, power added to 32kW and carries out melting, after melting completes, alloy melt poured in ingot mould, obtains plate-cast ingot after cooling.By the Nd made 15Fe 77.9Cu 1.5B 5.6Thin plate putting into the SDZK high-temperature vacuum sintering furnace, be evacuated to 1 * 10 -3Pass into the high-purity argon gas of 0.02MPa after Pa, be warming up to 1200 ℃ of insulations and within 12 hours, carry out the homogenizing annealing processing under argon shield, the thin plate that processing is obtained annealing ingot casting Mechanical Crushing, cross 300 mesh sieves and remove fine powder, and ingot casting Nd must anneal 15Fe 77.9Cu 1.5B 5.6Magnetic.
(2) preparation of part hydrogen disproportionation Nd-Fe-B magnetic
Annealing ingot casting Nd prepared by step (1) 15Fe 77.9Cu 1.5B 5.6Magnetic is at H 2Under atmosphere, be heated to 780 ℃ of insulations and within 60 minutes, inhaled hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, in vacuum degree<5 * 10 -2Be warming up to 820 ℃ of insulations under the condition of Pa and within 5 minutes, carry out dehydrogenation-recombining reaction, insulation cools to room temperature with the furnace after finishing, and the part hydrogen disproportionation Nd-Fe-B magnetic that to obtain crystallite dimension be 280-350nm (contains principal phase 2:14 phase and disproportionation phase NdH x, Fe 2B, α-Fe);
(3) preparation of pressed compact
Part hydrogen disproportionation Nd-Fe-B magnetic prepared by step (2) is packed in mould, under argon shield, in room temperature, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 300MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B, described pressed compact is cylindrical, is of a size of φ 10mm * 10mm;
(4) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (3) is prepared is warming up to 820 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2Carry out hot compression deformation-dehydrogenation restructuring under the condition of 10Pa, described Nd-Fe-B pressed compact being applied to constant pressure, the value of exerting pressure is 2.4kN, the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact is born in thermal deformation-dehydrogenation regrouping process changes between 30MPa ~ 4.5MPa, the heat-insulation pressure keeping time is 30 minutes, after finishing, heat-insulation pressure keeping cools to room temperature with the furnace, the nanocrystalline Nd-Fe-B magnet of anisotropy that to obtain deflection be 85 %.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.98, and its magnetic property is: B r=0.98T, H Ci=350 kA/m, (BH) m=142 kJ/m 3.
Embodiment 21
The present embodiment is with annealing ingot casting Nd 13.8Fe 70.6Co 5Mo 3.8Al 1B 5.8Magnetic is that raw material prepares the anisotropy nanocrystalline magnet, and processing step is as follows:
(1) annealing ingot casting Nd 13.8Fe 70.6Co 5Mo 3.8Al 1B 5.8Preparation
Take metal Nd (purity is 99.5%), DT4 electrical pure iron (purity is 99.95%), ferro-boron (boron content is 19.65%), metal Co (purity is 99%), molybdenum-iron (Mo content is 60%), metal A l(purity is 99%) be raw material, according to Nd 13.8Fe 70.6Co 5Mo 3.8Al 1B 5.8Alloying component calculates the ingredients by weight (increase the Nd of 3.0wt% during batching, the Al of 3.0wt% is as compensating for loss and damage) of each raw material.Adopt SF2002-4 type vacuum intermediate-frequency induction melting furnace melting Nd Fe B alloys, before heating, first smelting furnace is evacuated to 10 -2Pa, applying argon gas is to 0.05MPa, then according to the alloying component of calculating, power added to 38kW and carries out, and after melting completes, alloy melt poured in ingot mould, obtains plate-cast ingot after cooling.By the Nd made 13.8Fe 70.6Co 5Mo 3.8Al 1B 5.8Thin plate, putting into the SDZK high-temperature vacuum sintering furnace, is evacuated to 1 * 10 -3Pass into the high-purity argon gas of 0.02MPa after Pa, be warming up to 1200 ℃ of insulations and within 16 hours, carry out the homogenizing annealing processing under argon shield, the thin plate that processing is obtained annealing ingot casting Mechanical Crushing, cross 300 mesh sieves and remove fine powder, and ingot casting Nd must anneal 13.8Fe 70.6Co 5Mo 3.8Al 1B 5.8Magnetic.
(2) preparation of part hydrogen disproportionation Nd-Fe-B magnetic
Annealing ingot casting Nd prepared by step (1) 13.8Fe 70.6Co 5Mo 3.8Al 1B 5.8Magnetic is at H 2Under atmosphere, be heated to 780 ℃ of insulations and within 45 minutes, inhaled hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, in vacuum degree<5 * 10 -2Be warming up to 820 ℃ of insulations under the condition of Pa and within 5 minutes, carry out dehydrogenation-recombining reaction, insulation cools to room temperature with the furnace after finishing, and the part hydrogen disproportionation Nd-Fe-B magnetic that to obtain crystallite dimension be 260-300nm (contains principal phase 2:14 phase and disproportionation phase NdH x, Fe 2B, α-Fe);
(3) preparation of pressed compact
Part hydrogen disproportionation Nd-Fe-B magnetic prepared by step (2) is packed in mould, under argon shield, in room temperature, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 600MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B, described pressed compact is cylindrical, is of a size of φ 12mm * 12mm;
(4) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (3) is prepared is warming up to 820 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2Be 0.001 time described Nd-Fe-B pressed compact to be applied to constant pressure to carry out hot compression deformation-dehydrogenation restructuring, the value of exerting pressure is 2.7kN, the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact is born in thermal deformation-dehydrogenation regrouping process changes between 24MPa ~ 5.3MPa, the heat-insulation pressure keeping time is 20 minutes, after finishing, heat-insulation pressure keeping cools to room temperature with the furnace, the nanocrystalline Nd-Fe-B magnet of anisotropy that to obtain deflection be 78 %.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.97, and magnetic property is: B r=1.04T, H Ci=303kA/m, (BH) m=147kJ/m 3.
Embodiment 22
The present embodiment is with fast quenching Nd 13Fe 71.86Co 9.08Cu 0.06B 6Magnetic is that raw material prepares the anisotropy nanocrystalline magnet, and processing step is as follows:
(1) Nd 13Fe 71.86Co 9.08Cu 0.06B 6The preparation of quenched powder
Take metal Nd (purity is 99.5%), DT4 electrical pure iron (purity is 99.95%), ferro-boron (boron content is 19.65%), metal Co (purity is 99%), metal Cu(purity is 99%) be raw material, according to Nd 13Fe 71.86Co 9.08Cu 0.06B 6Alloying component, calculate the ingredients by weight (increasing the Nd of 2.0wt% during batching as compensating for loss and damage) of each raw material.Adopt SF2002-4 type vacuum intermediate-frequency induction melting furnace melting Nd Fe B alloys, before heating, first smelting furnace is evacuated to 10 -2Pa, applying argon gas is to 0.05MPa, then according to the alloying component of calculating, power added to 34kW and carries out, and after melting completes, alloy melt poured in ingot mould, obtains plate-cast ingot after cooling.After being ground off to oxide skin, plate-cast ingot is broken for pellet; put into the crucible of LZK-12A type vacuum quick quenching equipment; under argon shield atmosphere; power up to flow to after 700A melts furnace charge and be poured on the copper roller that linear velocity is 34m/s; cooling rear acquisition Nd Fe B alloys strip; after crossing 300 mesh sieves and removing fine powder, obtain Nd 13Fe 71.86Co 9.08Cu 0.06B 6Rapidly quenched magnetic powder.
(2) preparation of hydrogen disproportionation Nd-Fe-B magnetic fully
Annealing ingot casting Nd prepared by step (1) 13Fe 71.86Co 9Al 0.08Cu 0.06B 6Magnetic is at H 2Under atmosphere, in 800 ℃ of insulations, within 20 minutes, inhaled hydrogen-disproportionated reaction, insulation cools to room temperature with the furnace after finishing, and obtaining crystallite dimension is the complete hydrogen disproportionation Nd-Fe-B magnetic of 180-200nm;
(3) preparation of pressed compact
Complete hydrogen disproportionation Nd-Fe-B magnetic prepared by step (2) is packed in mould, under argon shield, in room temperature, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 350MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B, described pressed compact is cylindrical, is of a size of φ 11mm * 11mm;
(4) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (3) is prepared is warming up to 820 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2Carry out hot compression deformation-dehydrogenation restructuring under the condition of 500Pa, described Nd-Fe-B pressed compact being applied to constant pressure, the value of exerting pressure is 2.9kN, the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact is born in thermal deformation-dehydrogenation regrouping process changes between 30MPa ~ 7.2MPa, the heat-insulation pressure keeping time is 30 minutes, after finishing, heat-insulation pressure keeping cools to room temperature with the furnace, the nanocrystalline Nd-Fe-B magnet of anisotropy that to obtain deflection be 76.5 %.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.96, and magnetic property is: B r=0.99T, H Ci=458kA/m, (BH) m=165kJ/m 3.

Claims (3)

1. the preparation method of an anisotropy nano-crystal neodymium iron boron magnetic body is characterized in that processing step is as follows successively:
(1) preparation of hydrogen disproportionation or part hydrogen disproportionation Nd-Fe-B magnetic fully
By the Nd-Fe-B alloy powder at H 2Under atmosphere, in 650 ℃ ~ 820 ℃ insulations, within 5 minutes～60 minutes, inhaled hydrogen-disproportionated reaction, insulation cools to room temperature with the furnace after finishing, and obtaining crystallite dimension is nano level complete hydrogen disproportionation Nd-Fe-B magnetic;
Or by the Nd-Fe-B alloy powder at H 2Under atmosphere, within 5 minutes～60 minutes, inhaled hydrogen-disproportionated reaction in 650 ℃～820 ℃ insulations, after inhaling hydrogen-disproportionated reaction, in vacuum degree<5 * 10 -2Within 1～10 minute, carry out dehydrogenation-recombining reaction in 780 ℃～820 ℃ insulations under the condition of Pa, insulation cools to room temperature with the furnace after finishing, and obtaining crystallite dimension is nano level part hydrogen disproportionation Nd-Fe-B magnetic;
(2) preparation of pressed compact
Complete hydrogen disproportionation Nd-Fe-B magnetic prepared by step (1) or part hydrogen disproportionation Nd-Fe-B magnetic are packed in mould, under room temperature, inert gas shielding, magnetic is exerted pressure, the pressure suffered when magnetic stops exerting pressure from 0 MPa increases to 100MPa～600MPa, obtains the hydrogen disproportionation thing pressed compact of Nd-Fe-B;
(3) hot compression deformation-dehydrogenation restructuring
The Nd-Fe-B hydrogen disproportionation thing pressed compact that step (2) is prepared is warming up to 680 ℃～850 ℃ under vacuum condition, then at this temperature and hydrogen dividing potential drop P H2For 0Pa<P H2Under the condition of≤1kPa, described Nd-Fe-B pressed compact is applied to constant pressure and carry out hot compression deformation-dehydrogenation restructuring, the pressure that bears in thermal deformation-dehydrogenation regrouping process with Nd-Fe-B hydrogen disproportionation thing pressed compact of the value of exerting pressure change and be limited between 30MPa ~ 1.5MPa, the heat-insulation pressure keeping time is 5～120 minutes, heat-insulation pressure keeping cools to room temperature with the furnace after finishing, and obtains the anisotropy nano-crystal neodymium iron boron magnetic body.
2. the preparation method of anisotropy nano-crystal neodymium iron boron magnetic body according to claim 1, the chemical formula that it is characterized in that described Nd-Fe-B alloy powder is Nd xFe 100-x-y-zM yB z, 12≤x≤15,0≤y≤10,5.6≤z≤6 wherein, M is at least one in Co, Ga, Zr, Nb, Cu, Al, Cr, Mo, Ti.
3. the preparation method of described anisotropy nano-crystal neodymium iron boron magnetic body according to claim 2, is characterized in that described Nd-Fe-B alloy powder is Nd 12.2Fe 81.8B 6, Nd 13.5Fe 80.5B 6, Nd 13.5Fe 80.4Ga 0.5B 5.6, Nd 13.5Fe 73Co 7.5B 6, Nd 12.5Fe 80.5Nb 1B 6, Nd 14Fe 79.4Al 0.6B 6, Nd 15Fe 78Mo 1B 6, Nd 12.2Fe 71.8Co 9.4Ga 0.5Zr 0.1B 6, Nd 13.62Fe 75.7Co 4.45Ga 0.47B 5.76, Nd 14Fe 76Co 3Zr 1B 6, Nd 12.6Fe 72.3Co 8.6Al 0.5B 6.0, Nd 13.5Fe 79.96Al 0.24Nb 0.3B 6, Nd 13Fe 71.86Co 9Al 0.08Cu 0.06B 6, Nd 14.5Fe 76.4Ti 2.5Cr 1B 5.6, Nd 13Fe 71.86Co 9.08Cu 0.06B 6, Nd 13.8Fe 70.6Co 5Mo 3.8Al 1B 5.8, Nd 15Fe 77.9Cu 1.5B 5.6In a kind of.
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