CN103426623B - A kind of preparation method of anisotropy nano-crystalline neodymium-iron-boronmagnet magnet - Google Patents

A kind of preparation method of anisotropy nano-crystalline neodymium-iron-boronmagnet magnet Download PDF

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CN103426623B
CN103426623B CN201310336808.2A CN201310336808A CN103426623B CN 103426623 B CN103426623 B CN 103426623B CN 201310336808 A CN201310336808 A CN 201310336808A CN 103426623 B CN103426623 B CN 103426623B
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pressed compact
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disproportionation
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CN103426623A (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

The preparation method of anisotropy nano-crystalline neodymium-iron-boronmagnet magnet: the preparation of (1) complete hydrogen disproportionation or part hydrogen disproportionation Nd-Fe-B magnetic; (2) preparation of pressed compact, complete hydrogen disproportionation Nd-Fe-B magnetic step (1) prepared or part hydrogen disproportionation Nd-Fe-B magnetic load in mould, in room temperature, magnetic is exerted pressure under inert gas shielding, when the pressure suffered by magnetic is from 0? stop exerting pressure after MPa is increased to 100MPa ~ 600MPa; (3) hot compression deformation-dehydrogenation restructuring, is warming up to 680 DEG C ~ 850 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P by pressed compact h2for 0Pa < P h2under the condition of≤1kPa, constant pressure is applied to described Nd-Fe-B pressed compact and carries out hot compression deformation-dehydrogenation restructuring, force value of exerting pressure change between 30MPa ~ 1.5MPa with the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact bears in thermal deformation-dehydrogenation regrouping process and be limited, the heat-insulation pressure keeping time is 5 ~ 120 minutes.The preparation method of anisotropy nano-crystalline neodymium-iron-boronmagnet magnet of the present invention, can improve the performance of anisotropic neodymium iron boron magnetic body, and reduce energy consumption.<!--1-->

Description

A kind of preparation method of anisotropy nano-crystalline neodymium-iron-boronmagnet magnet
Technical field
The invention belongs to rare earth permanent-magnetic material preparation field, particularly a kind of preparation method of anisotropy nano-crystalline neodymium-iron-boronmagnet magnet.
Background technology
Anisotropy nanocrystalline Nd-Fe-B magnet 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 HDDR method) and hot pressing-thermal deformation method.
HDDR legal system is for anisotropy Nd-Fe-B magnet, anisotropy Nd-Fe-B magnetic is obtained mainly through alloying elements such as hydrogen dividing potential drop during reduction disproportionation or interpolation Co, Ga, Zr, shaping by methods such as compacting or injection mouldings under the effect of externally-applied magnetic field after again anisotropy Nd-Fe-B magnetic being mixed with bonding agent, namely obtain anisotropic bonded magnet.Although this kind of method process is simple, easy-formation, but because adding of bonding agent makes the magnetic property of magnet generally on the low side, in addition, in HDDR process, because the suction hydrogen of Nd-Fe-B and dehydrogenation reaction are along with strong heat release and endothermic thermal event, make temperature of reaction system produce larger fluctuation, cause Nd-Fe-B magnetic anisotropy lower, and stably can not prepare the finished product magnet of identical performance.
The processing step of hot pressing-thermal deformation method is: isotropic Nd-Fe-B magnetic is applied high pressure (pressure is at least at 300MPa) at 600 DEG C ~ 750 DEG C and forms high fine and close pressed compact (see W.Q.Liuet.al. by (1), Structureandmagneticpropertiesofmagneticallyisotropicand anisotropicNd – Fe – Bpermanentmagnetspreparedbysparkplasmasinteringtechnolog y, J.Appl.Phys., 2010,107 (9): 09A719); (2) pressed compact step (1) formed is greater than 700 DEG C 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 (see PengpengYiet.al between 30MPa ~ 300MPa; Enhancedmagneticpropertiesandbendingstrengthofhotdeforme dNd – Fe – BmagnetswithCuadditions; J.AlloysCompds., 2010 (491): 605 – 609; Y.L.Huanget.al, DiffusionofNd-richphaseinthesparkplasmasinteredandhotdef ormednanocrystallineNdFeBmagnets, J.Appl.Phys., 2012,111,033913).This kind of method Problems existing is: because pressed compact is shaping at high temperature under high pressure, may make that the portion crystal of Nd-Fe-B pressed compact is excessive and uniformity is poor, thus Nd in the NdFeB magnet obtained after causing thermal deformation 2fe 14the deformation extent of B crystal grain is uneven, grain morphology systematicness is poor, orientation consistency is poor, and adds energy consumption.
Summary of the invention
The object of the present invention is to provide a kind of new method preparing anisotropy nano-crystalline neodymium-iron-boronmagnet magnet, to obtain the nano-crystal neodymium iron boron magnetic body that anisotropy is obvious and have excellent magnetic characteristics, and reduce energy consumption, Simplified flowsheet.
The preparation method of anisotropy nano-crystalline neodymium-iron-boronmagnet magnet of the present invention, its processing step is as follows successively:
(1) preparation of complete hydrogen disproportionation or part hydrogen disproportionation Nd-Fe-B magnetic
By Nd-Fe-B alloy powder at H 2under atmosphere, within 5 minutes ~ 60 minutes, carry out suction hydrogen-disproportionated reaction in 650 DEG C ~ 820 DEG C insulations, cool to room temperature with the furnace after insulation terminates, obtaining crystallite dimension is nano level complete hydrogen disproportionation Nd-Fe-B magnetic;
Or by Nd-Fe-B alloy powder at H 2under atmosphere, within 5 minutes ~ 60 minutes, carry out suction hydrogen-disproportionated reaction in 650 DEG C ~ 820 DEG C insulations, after inhaling hydrogen-disproportionated reaction, at vacuum degree < 5 × 10 -2within 1 ~ 10 minute, carry out dehydrogenation-recombining reaction in 780 DEG C ~ 820 DEG C insulations under the condition of Pa, cool to room temperature with the furnace after insulation terminates, 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 step (1) prepared or part hydrogen disproportionation Nd-Fe-B magnetic load in mould, in room temperature, magnetic is exerted pressure under inert gas shielding, stop exerting pressure after the pressure suffered by magnetic is increased to 100MPa ~ 600MPa from 0MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B;
(3) hot compression deformation-dehydrogenation restructuring
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (2) is warming up to 680 DEG C ~ 850 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2for 0Pa < P h2under the condition of≤1kPa, constant pressure is applied to described Nd-Fe-B pressed compact and carries out hot compression deformation-dehydrogenation restructuring, force value of exerting pressure change between 30MPa ~ 1.5MPa with the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact bears in thermal deformation-dehydrogenation regrouping process and be limited, the heat-insulation pressure keeping time is 5 ~ 120 minutes, cool to room temperature with the furnace after heat-insulation pressure keeping terminates, obtain the nanocrystalline Nd-Fe-B magnet of anisotropy.
In said method, the initial pressure (maximum pressure) that the constant pressure that hot compression deformation-dehydrogenation reconstitution steps applies Nd-Fe-B hydrogen disproportionation thing pressed compact is born in thermal deformation-dehydrogenation regrouping process by shape and size and the described pressed compact of described pressed compact 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 then 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, wherein 12≤x≤15,0≤y≤10,5.6≤z≤6, 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 one.
The method of the invention has following beneficial effect:
1, due to the method for the invention be by after complete for Nd-Fe-B alloy powder hydrogen disproportionation or part hydrogen disproportionation by formation pressed compact of colding pressing, again pressed compact hot compression deformation-dehydrogenation restructuring is obtained the nanocrystalline Nd-Fe-B magnet of anisotropy, thus obtained pressed compact crystal grain is tiny, main phase grain oriented nucleation and growth in hot compression deformation-dehydrogenation restructuring, can be formed directly in grain orientation obviously and crystallite dimension tiny (orientation die width is 80-100nm), uniform anisotropy nano-crystalline neodymium-iron-boronmagnet magnet (see figure 2), the neodymium iron boron magnetic body of this kind of structure has obvious anisotropy and excellent magnetic property.
2, because the method for the invention does not use bonding agent, and by hot compression deformation-dehydrogenation restructuring, pressed compact is directly changed into anisotropy nano-crystalline neodymium-iron-boronmagnet magnet, thus relative to HDDR method, the magnetic property of anisotropy nano-crystalline neodymium-iron-boronmagnet magnet can not only be improved, and can stably prepare finished product magnet.
3, because the method for the invention adopts cold moudling to prepare the hydrogen disproportionation thing pressed compact of Nd-Fe-B, and the pressure that during hot compression deformation, pressed compact bears is less, thus relative to hot pressing-thermal deformation method, not only obtained pressed compact crystal grain 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 be better than the Nd-Fe-B alloy powder that principal phase is 2:14 phase due to the suppression performance of Nd-Fe-B hydrogen disproportionation thing alloy powder, under low pressure can produce the height densification of the various shapes such as sheet, ring-type, strip or fully dense anisotropy Nd-Fe-B magnet product according to the actual requirements, be conducive to promoting the use of.
Accompanying drawing explanation
Fig. 1 is XRD figure (perpendicular to pressure direction) of the nanocrystalline Nd-Fe-B magnet of anisotropy prepared by embodiment 1;
Fig. 2 is the FESEM(field emission scanning electron microscope of the anisotropy nanocrystalline Nd-Fe-B magnet section prepared by embodiment 1) figure (direction of arrow is pressure direction).
Embodiment
Below by embodiment, the preparation method to anisotropy nano-crystalline neodymium-iron-boronmagnet magnet of the present invention is described further.In following embodiment, the preparation of complete hydrogen disproportionation or part hydrogen disproportionation Nd-Fe-B magnetic adopts HTO-114 II type horizontal vacuum sintering furnace (Qingdao, company of absolute sincerity Huaqi IDTC), the hydrogen disproportionation thing pressed compact of Nd-Fe-B adopts the shaping (Sichuan of YSD-10-1 type bidirectional hydraulic press, 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 anisotropy nanocrystalline magnet prepared by raw material, and processing step is as follows:
(1) Nd 13.5fe 73co 7.5b 6the preparation of quenched powder
With metal Nd (purity is for 99.5%), DT4 electrical pure iron (purity is for 99.95%), ferro-boron (Boron contents is for 19.65%), metal Co (purity is for 99.5%) for 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, power, to 0.05MPa, is then adjusted to 38kW according to the alloying component calculated and carries out melting, pour in ingot mould, obtain plate-cast ingot after cooling after melting completes by alloy melt by applying argon gas.Pellet is broken for after plate-cast ingot being ground off oxide skin; then the copper crucible of LZK-12A type vacuum quick quenching equipment is put into; under argon atmosphere; power up flow to 600A make load melting after be poured on copper roller that linear velocity is 28m/s; Nd Fe B alloys strip is obtained after cooling; after crossing 300 mesh sieves removal fine powders, namely obtain Nd 13.5fe 73co 7.5b 6rapidly quenched magnetic powder;
(2) preparation of part hydrogen disproportionation Nd-Fe-B magnetic
By fast quenching Nd prepared by step (1) 13.5fe 73co 7.5b 6magnetic is at H 2under atmosphere, be heated to 800 DEG C of insulations and within 10 minutes, carry out suction hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, at vacuum degree < 5 × 10 -2be warming up to 820 DEG C of insulations under the condition of Pa and carry out dehydrogenation-recombining reaction in 5 minutes, cool to room temperature with the furnace after insulation terminates, obtain the part hydrogen disproportionation Nd-Fe-B magnetic of crystallite dimension at 150-200nm (containing 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 step (2) prepared loads in mould, in room temperature, magnetic is exerted pressure under argon shield, stop exerting pressure after the pressure suffered by magnetic is increased to 300MPa from 0MPa, 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
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (3) is warming up to 820 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2hot compression deformation-dehydrogenation restructuring is carried out for applying constant pressure to described Nd-Fe-B pressed compact under the condition of 10Pa, force 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, room temperature is cooled to the furnace after heat-insulation pressure keeping terminates, obtain the nanocrystalline Nd-Fe-B magnet of anisotropy that deflection is 73%, its XRD figure perpendicular to pressure direction is shown in Fig. 1, and 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=602kA/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 anisotropy nanocrystalline magnet prepared by raw material, and processing step is as follows:
(1) Nd 13.5fe 80.4ga 0.5b 5.6the preparation of quenched powder
With metal Nd (purity is for 99.5%), DT4 electrical pure iron (purity is for 99.95%), ferro-boron (Boron contents is for 19.65%), metal Ga(purity for 99.95%) for 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, power, to 0.05MPa, is then adjusted to 36kW according to the alloying component calculated and carries out melting, pour in ingot mould, obtain plate-cast ingot after cooling after melting completes by alloy melt by applying argon gas.Pellet is broken for after plate-cast ingot being ground off oxide skin; then the copper crucible of LZK-12A type vacuum quick quenching equipment is put into; under argon atmosphere; power up flow to 650A make load melting after be poured on copper roller that linear velocity is 28m/s; Nd Fe B alloys strip is obtained after cooling; cross after 300 mesh sieves remove fine powder, namely obtain Nd 13.5fe 80.4ga 0.5b 5.6rapidly quenched magnetic powder.
(2) preparation of part hydrogen disproportionation Nd-Fe-B magnetic
By fast quenching Nd prepared by step (1) 13.5fe 80.4ga 0.5b 5.6magnetic is at H 2under atmosphere, be heated to 680 DEG C of insulations and within 45 minutes, carry out suction hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, at vacuum degree < 5 × 10 -2be warming up to 800 DEG C of insulations under the condition of Pa and carry out dehydrogenation-recombining reaction in 1 minute, cool to room temperature with the furnace after insulation terminates, obtain the part hydrogen disproportionation Nd-Fe-B magnetic of crystallite dimension 100-120nm (containing 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 step (2) prepared loads in mould, in room temperature, magnetic is exerted pressure under argon shield, stop exerting pressure after the pressure suffered by magnetic is increased to 100MPa from 0MPa, 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
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (3) is warming up to 780 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2hot compression deformation-dehydrogenation restructuring is carried out for applying constant pressure to described Nd-Fe-B pressed compact under the condition of 10Pa, force 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, cool to room temperature with the furnace after heat-insulation pressure keeping terminates, obtain the nanocrystalline Nd-Fe-B magnet of anisotropy that deflection is 83%.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.95, and its magnetic property is: B r=1.2T, H ci=550kA/m, (BH) m=2446kJ/m 3.
Embodiment 3
The present embodiment is with fast quenching Nd 13.5fe 80.5b 6magnetic is that anisotropy nanocrystalline magnet prepared by raw material, and processing step is as follows:
(1) Nd 13.5fe 80.5b 6prepared by quenched powder
With metal Nd (purity is for 99.5%), DT4 electrical pure iron (purity is for 99.95%), ferro-boron (Boron contents is for 19.65%) for raw material, according to designing the Nd determined 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, power, to 0.05MPa, is then added to 35kW according to the alloying component calculated and carries out melting, pour in ingot mould, obtain plate-cast ingot after cooling after melting completes by alloy melt by applying argon gas.After plate-cast ingot is ground off oxide skin; be broken for pellet; put into the copper crucible of LZK-12A type vacuum quick quenching equipment; under argon atmosphere; power up flow to 600A make load melting after be poured on copper roller that linear velocity is 30m/s; cooling obtains Nd Fe B alloys strip afterwards, after 300 mesh sieves remove fine powder excessively, namely obtains Nd 13.5fe 80.5b 6rapidly quenched magnetic powder.
(2) preparation of part hydrogen disproportionation Nd-Fe-B magnetic
By fast quenching Nd prepared by step (1) 13.5fe 80.5b 6magnetic is at H 2under atmosphere, be heated to 750 DEG C of insulations and within 30 minutes, carry out suction hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, at vacuum degree < 5 × 10 -2be warming up to 780 DEG C of insulations under the condition of Pa and carry out dehydrogenation-recombining reaction in 10 minutes, cool to room temperature with the furnace after insulation terminates, obtaining crystallite dimension is that the part hydrogen disproportionation Nd-Fe-B magnetic of 120-140nm is (containing 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 step (2) prepared loads in mould, in room temperature, magnetic is exerted pressure under argon shield, stop exerting pressure after the pressure suffered by magnetic is increased to 270MPa from 0MPa, 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
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (3) is warming up to 700 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2hot compression deformation-dehydrogenation restructuring is carried out for applying constant pressure to described Nd-Fe-B pressed compact under the condition of 40Pa, force 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, cool to room temperature with the furnace after heat-insulation pressure keeping terminates, obtain the nanocrystalline Nd-Fe-B magnet of anisotropy that deflection is 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 anisotropy nanocrystalline magnet prepared by raw material, and processing step is as follows:
(1) Nd 13.5fe 73co 7.5b 6prepared by quenched powder
Preparation method, with embodiment 1, omits.
(2) preparation of complete hydrogen disproportionation Nd-Fe-B magnetic
By fast quenching Nd prepared by step (1) 13.5fe 73co 7.5b 6magnetic is at H 2under atmosphere, within 60 minutes, carry out suction hydrogen-disproportionated reaction in 650 DEG C of insulations, cool to room temperature with the furnace after insulation terminates, obtain the complete hydrogen disproportionation Nd-Fe-B magnetic that crystallite dimension is 180-200nm;
(3) preparation of pressed compact
Complete hydrogen disproportionation Nd-Fe-B magnetic step (2) prepared loads in mould, in room temperature, magnetic is exerted pressure under argon shield, stop exerting pressure after the pressure suffered by magnetic is increased to 450MPa from 0MPa, 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
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (3) is warming up to 750 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2hot compression deformation-dehydrogenation restructuring is carried out for applying constant pressure to described Nd-Fe-B pressed compact under the condition of 800Pa, force 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, cool to room temperature with the furnace after heat-insulation pressure keeping terminates, obtain the nanocrystalline Nd-Fe-B magnet of anisotropy that deflection is 75%.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.92, and its magnetic property is: B r=0.95T, H ci=501kA/m, (BH) m=147kJ/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 anisotropy nanocrystalline magnet prepared by raw material, and processing step is as follows:
(1) Nd 12.2fe 71.8co 9.4ga 0.5zr 0.1b 6prepared by quenched powder
With metal Nd (purity is for 99.5%), DT4 electrical pure iron (purity is for 99.95%), ferro-boron (Boron contents is for 19.65%), metal Co (purity is for 99.5%), metal Ga(purity for 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, power, to 0.05MPa, is then added to 38kW according to the alloying component calculated and carries out melting, pour in ingot mould, obtain plate-cast ingot after cooling after melting completes by alloy melt by applying argon gas.Pellet is broken for after plate-cast ingot being ground off oxide skin; put into the copper crucible of LZK-12A type vacuum quick quenching equipment; under argon atmosphere; power up flow to 700A make load melting after be poured on copper roller that linear velocity is 32m/s; Nd Fe B alloys strip is obtained after cooling; cross after 300 mesh sieves remove fine powder, namely obtain Nd 12.2fe 71.8co 9.4ga 0.5zr 0.1b 6rapidly quenched magnetic powder.
(2) preparation of complete hydrogen disproportionation Nd-Fe-B magnetic
By fast quenching Nd prepared by step (1) 12.2fe 71.8co 9.4ga 0.5zr 0.1b 6magnetic is at H 2under atmosphere, within 5 minutes, carry out suction hydrogen-disproportionated reaction in 820 DEG C of insulations, cool to room temperature with the furnace after insulation terminates, obtain the complete hydrogen disproportionation Nd-Fe-B magnetic that crystallite dimension is 15-25nm;
(3) preparation of pressed compact
Part hydrogen disproportionation Nd-Fe-B magnetic step (2) prepared loads in mould, in room temperature, magnetic is exerted pressure under argon shield, stop exerting pressure after the pressure suffered by magnetic is increased to 250MPa from 0MPa, 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
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (3) is warming up to 800 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2hot compression deformation-dehydrogenation restructuring is carried out for applying constant pressure to described Nd-Fe-B pressed compact under the condition of 500Pa, force 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, cool to room temperature with the furnace after heat-insulation pressure keeping terminates, obtain the nanocrystalline Nd-Fe-B magnet of anisotropy that deflection is 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 anisotropy nanocrystalline magnet prepared by raw material, and processing step is as follows:
(1) Nd 12.2fe 81.8b 6prepared by quenched powder
With metal Nd (purity is for 99.5%), DT4 electrical pure iron (purity is for 99.95%), ferro-boron (Boron contents is for 19.65%) for 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, power, to 0.05MPa, is then added to 36kW according to the alloying component calculated and carries out melting, pour in ingot mould, obtain plate-cast ingot after cooling after melting completes by alloy melt by applying argon gas.Pellet is broken for after plate-cast ingot being ground off oxide skin; put into the copper crucible of LZK-12A type vacuum quick quenching equipment; under argon atmosphere; power up flow to 650A make load melting after be poured on copper roller that linear velocity is 32m/s; Nd Fe B alloys strip is obtained after cooling; cross after 300 mesh sieves remove fine powder, namely obtain Nd 12.2fe 81.8b 6rapidly quenched magnetic powder.
(2) preparation of part hydrogen disproportionation Nd-Fe-B magnetic
By fast quenching Nd prepared by step (1) 12.2fe 81.8b 6magnetic is at H 2under atmosphere, within 10 minutes, carry out suction hydrogen-disproportionated reaction in 780 DEG C of insulations, after inhaling hydrogen-disproportionated reaction, at vacuum degree < 5.0 × 10 -2be warming up to 820 DEG C under Pa condition, be incubated and carry out dehydrogenation-recombining reaction in 5 minutes, cool to room temperature with the furnace after insulation terminates, obtaining crystallite dimension is that the part hydrogen disproportionation products of 120-160nm (namely 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 step (2) prepared loads in mould, in room temperature, magnetic is exerted pressure under argon shield, stop exerting pressure after the pressure suffered by magnetic is increased to 460MPa from 0MPa, 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
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (3) is warming up to 850 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2hot compression deformation-dehydrogenation restructuring is carried out for applying constant pressure to described Nd-Fe-B pressed compact under the condition of 50Pa, force 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, cool to room temperature with the furnace after heat-insulation pressure keeping terminates, obtain the nanocrystalline Nd-Fe-B magnet of anisotropy that deflection is 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 the ingot casting Nd that anneals 12.2fe 81.8b 6magnetic is that anisotropy nanocrystalline magnet prepared by raw material, and processing step is as follows:
(1) anneal ingot casting Nd 12.2fe 81.8b 6the preparation of magnetic
Nd is prepared according to step (1) described method in embodiment 6 12.2fe 81.8b 6plate-cast ingot, by obtained Nd 12.2fe 81.8b 6thin plate, putting into SDZK high-temperature vacuum sintering furnace, is evacuated to 1 × 10 -3pass into the high-purity argon gas of 0.02MPa after Pa, under argon shield, be warming up to 1100 DEG C of insulation 12h carry out homogenizing annealing process, will the thin plate annealing ingot casting Mechanical Crushing obtained be processed, and cross 300 mesh sieves and remove fine powder, namely obtain annealing ingot casting Nd 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 DEG C of insulations and within 30 minutes, carry out suction hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, at vacuum degree < 5 × 10 -2be warming up to 800 DEG C of insulations under the condition of Pa and carry out dehydrogenation-recombining reaction in 5 minutes, cool to room temperature with the furnace after insulation terminates, obtaining crystallite dimension is that the part hydrogen disproportionation Nd-Fe-B magnetic of 120-160nm is (containing 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 step (2) prepared loads in mould, in room temperature, magnetic is exerted pressure under argon shield, stop exerting pressure after the pressure suffered by magnetic is increased to 270MPa from 0MPa, 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
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (3) is warming up to 780 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2hot compression deformation-dehydrogenation restructuring is carried out for applying constant pressure to described Nd-Fe-B pressed compact under the condition of 200Pa, force 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, cool to room temperature with the furnace after heat-insulation pressure keeping terminates, obtain the nanocrystalline Nd-Fe-B magnet of anisotropy that deflection is 75.6%.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.90, and its magnetic property is: B r=1.2T, H ci=530kA/m, (BH) m=234kJ/m 3.
Embodiment 8
The present embodiment is with the ingot casting Nd that anneals 12.2fe 71.8co 9.4ga 0.5zr 0.1b 6magnetic is that anisotropy nanocrystalline magnet prepared by raw material, and processing step is as follows:
(1) anneal ingot casting Nd 12.2fe 71.8co 9.4ga 0.5zr 0.1b 6magnetic
Nd is prepared according to step (1) described method in embodiment 5 12.2fe 71.8co 9.4ga 0.5zr 0.1b 6plate-cast ingot, by obtained Nd 12.2fe 71.8co 9.4ga 0.5zr 0.1b 6thin plate, putting into 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 DEG C of insulations and carry out homogenizing annealing process in 16 hours under argon shield, will process the thin plate annealing ingot casting Mechanical Crushing obtained, cross 300 mesh sieves and remove fine powder, must anneal ingot casting Nd 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 DEG C of insulations and within 10 minutes, carry out suction hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, at vacuum degree < 5 × 10 -2be warming up to 820 DEG C of insulations under the condition of Pa and carry out dehydrogenation-recombining reaction in 3 minutes, cool to room temperature with the furnace after insulation terminates, obtain crystallite dimension and be less than the part hydrogen disproportionation Nd-Fe-B magnetic of 140-160nm (containing 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 step (2) prepared loads in mould, in room temperature, magnetic is exerted pressure under argon shield, stop exerting pressure after the pressure suffered by magnetic is increased to 150MPa from 0MPa, 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
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (3) is warming up to 750 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2hot compression deformation-dehydrogenation restructuring is carried out for applying constant pressure to described Nd-Fe-B pressed compact under the condition of 100Pa, force 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, cool to room temperature with the furnace after heat-insulation pressure keeping terminates, obtain the nanocrystalline Nd-Fe-B magnet of anisotropy that deflection is 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=490kA/m, (BH) m=190kJ/m 3.
Embodiment 9
The present embodiment is with the ingot casting Nd that anneals 13.5fe 73co 7.5b 6magnetic is that anisotropy nanocrystalline magnet prepared by raw material, and processing step is as follows:
(1) anneal ingot casting Nd 13.5fe 73co 7.5b 6magnetic
Nd is prepared according to step (1) described method in embodiment 1 13.5fe 73co 7.5b 6plate-cast ingot, by obtained Nd 13.5fe 73co 7.5b 6thin plate, putting into 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 DEG C of insulations and carry out homogenizing annealing process in 14 hours under argon shield, will process the thin plate annealing ingot casting Mechanical Crushing obtained, cross 300 mesh sieves and remove fine powder, must anneal ingot casting Nd 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 DEG C of insulations and within 15 minutes, carry out suction hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, at vacuum degree < 5 × 10 -2be warming up to 820 DEG C of insulations under the condition of Pa and carry out dehydrogenation-recombining reaction in 3 minutes, cool to room temperature with the furnace after insulation terminates, obtain the part hydrogen disproportionation Nd-Fe-B magnetic of crystallite dimension 160-180nm (containing 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 step (2) prepared loads in mould, in room temperature, magnetic is exerted pressure under argon shield, stop exerting pressure after the pressure suffered by magnetic is increased to 400MPa from 0MPa, 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
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (3) is warming up to 680 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2hot compression deformation-dehydrogenation restructuring is carried out for applying constant pressure to described Nd-Fe-B pressed compact under the condition of 1kPa, force 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, cool to room temperature with the furnace after heat-insulation pressure keeping terminates, obtain the nanocrystalline Nd-Fe-B magnet of anisotropy that deflection is 65%.After tested, the relative density of prepared anisotropy Nd-Fe-B magnet is: 0.86, and magnetic property is: B r=0.96T, H ci=557kA/m, (BH) m=162kJ/m 3.
Embodiment 10
The present embodiment is with the ingot casting Nd that anneals 13.62fe 75.7co 4.45ga 0.47b 5.76magnetic is that anisotropy nanocrystalline magnet prepared by raw material, and processing step is as follows:
(1) anneal ingot casting Nd 13.62fe 75.7co 4.45ga 0.47b 5.76preparation
With metal Nd (purity is for 99.5%), DT4 electrical pure iron (purity is for 99.95%), ferro-boron (Boron contents is for 19.65%), metal Co (purity is for 99.5%), metal Ga(purity for 99%) for 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, power, to 0.05MPa, is then added to 38kW according to the alloying component calculated and carries out melting, pour in ingot mould, obtain plate-cast ingot after cooling after melting completes by alloy melt by applying argon gas.By obtained Nd 13.62fe 75.7co 4.45ga 0.47b 5.76thin plate, putting into 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 DEG C of insulations and carry out homogenizing annealing process in 14 hours under argon shield, will process the thin plate annealing ingot casting Mechanical Crushing obtained, cross 300 mesh sieves and remove fine powder, must anneal ingot casting Nd 13.62fe 75.7co 4.45ga 0.47b 5.76magnetic.
(2) preparation of complete hydrogen disproportionation Nd-Fe-B magnetic
Annealing ingot casting Nd prepared by step (1) 13.62fe 75.7co 4.45ga 0.47b 5.76magnetic is at H 2under atmosphere, within 15 minutes, carry out suction hydrogen-disproportionated reaction in 800 DEG C of insulations, cool to room temperature with the furnace after insulation terminates, obtain the complete hydrogen disproportionation Nd-Fe-B magnetic that crystallite dimension is 40-90nm;
(3) preparation of pressed compact
Complete hydrogen disproportionation Nd-Fe-B magnetic step (2) prepared loads in mould, in room temperature, magnetic is exerted pressure under argon shield, stop exerting pressure after the pressure suffered by magnetic is increased to 420MPa from 0MPa, 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
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (3) is warming up to 750 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2hot compression deformation-dehydrogenation restructuring is carried out for applying constant pressure to described Nd-Fe-B pressed compact under the condition of 30Pa, force 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, cool to room temperature with the furnace after heat-insulation pressure keeping terminates, obtain the nanocrystalline Nd-Fe-B magnet of anisotropy that deflection is 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 the ingot casting Nd that anneals 13.5fe 80.4ga 0.5b 5.6magnetic is that anisotropy nanocrystalline magnet prepared by raw material, and processing step is as follows:
(1) anneal ingot casting Nd 13.5fe 80.4ga 0.5b 5.6preparation
Nd is prepared according to step (1) described method in embodiment 2 13.5fe 80.4ga 0.5b 5.6plate-cast ingot, by obtained Nd 13.5fe 80.4ga 0.5b 5.6thin plate putting into 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 DEG C of insulations and carry out homogenizing annealing process in 12 hours under argon shield, will process the thin plate annealing ingot casting Mechanical Crushing obtained, cross 300 mesh sieves and remove fine powder, must anneal ingot casting Nd 13.5fe 80.4ga 0.5b 5.6magnetic.
(2) preparation of complete hydrogen disproportionation Nd-Fe-B magnetic
Annealing ingot casting Nd prepared by step (1) 13.5fe 80.4ga 0.5b 5.6magnetic is at H 2under atmosphere, within 25 minutes, carry out suction hydrogen-disproportionated reaction in 780 DEG C of insulations, cool to room temperature with the furnace after insulation terminates, obtain the complete hydrogen disproportionation Nd-Fe-B magnetic that crystallite dimension is 80-120nm;
(3) preparation of pressed compact
Complete hydrogen disproportionation Nd-Fe-B magnetic step (2) prepared loads in mould, in room temperature, magnetic is exerted pressure under argon shield, stop exerting pressure after the pressure suffered by magnetic is increased to 600MPa from 0MPa, 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
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (3) is warming up to 800 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2hot compression deformation-dehydrogenation restructuring is carried out for applying constant pressure to described Nd-Fe-B pressed compact under the condition of 10Pa, force 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, cool to room temperature with the furnace after heat-insulation pressure keeping terminates, obtain the nanocrystalline Nd-Fe-B magnet of anisotropy that deflection is 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=125kJ/m 3.
Embodiment 12
The present embodiment is with the ingot casting Nd that anneals 14fe 76co 3zr 1b 6magnetic is that anisotropy nanocrystalline magnet prepared by raw material, and processing step is as follows:
(1) anneal ingot casting Nd 14fe 76co 3zr 1b 6preparation
With metal Nd (purity is for 99.5%), DT4 electrical pure iron (purity is for 99.95%), ferro-boron (Boron contents is for 19.65%), metal Co (purity is for 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, power, to 0.05MPa, is then added to 38kW according to the alloying component calculated and carries out melting, pour in ingot mould, obtain plate-cast ingot after cooling after melting completes by alloy melt by applying argon gas.By obtained Nd 14fe 76co 3zr 1b 6thin plate putting into 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 DEG C of insulations and carry out homogenizing annealing process in 16 hours under argon shield, will process the thin plate annealing ingot casting Mechanical Crushing obtained, cross 300 mesh sieves and remove fine powder, must anneal ingot casting Nd 14fe 76co 3zr 1b 6magnetic.
(2) preparation of complete hydrogen disproportionation Nd-Fe-B magnetic
Annealing ingot casting Nd prepared by step (1) 14fe 76co 3zr 1b 6magnetic is at H 2under atmosphere, within 60 minutes, carry out suction hydrogen-disproportionated reaction in 750 DEG C of insulations, cool to room temperature with the furnace after insulation terminates, obtain 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 step (2) prepared loads in mould, in room temperature, magnetic is exerted pressure under argon shield, stop exerting pressure after the pressure suffered by magnetic is increased to 500MPa from 0MPa, 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
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (3) is warming up to 780 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2hot compression deformation-dehydrogenation restructuring is carried out for applying constant pressure to described Nd-Fe-B pressed compact under the condition of 30Pa, force 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, cool to room temperature with the furnace after heat-insulation pressure keeping terminates, obtain the nanocrystalline Nd-Fe-B magnet of anisotropy that deflection is 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 anisotropy nanocrystalline magnet prepared by raw material, and processing step is as follows:
(1) Nd 12.5fe 80.5nb 1b 6the preparation of quenched powder
With metal Nd (purity is for 99.5%), DT4 electrical pure iron (purity is for 99.95%), ferro-boron (Boron contents is for 19.65%), ferro-niobium (Nb content is for 50%) for raw material, according to Nd 12.5fe 80.5nb 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 1 × 10 -2pa, power, to 0.05MPa, is then added to 36kW melting according to the alloying component calculated, pours in ingot mould, obtain plate-cast ingot after cooling after melting completes by alloy melt by applying argon gas.Pellet is broken for after plate-cast ingot being ground off oxide skin; put into the copper crucible of LZK-12A type vacuum quick quenching equipment; under argon atmosphere; power up flow to 650A make load melting after be poured on copper roller that linear velocity is 32m/s; Nd Fe B alloys strip is obtained after cooling; cross after 300 mesh sieves remove fine powder, namely obtain Nd 12.5fe 80.5nb 1b 6rapidly quenched magnetic powder.
(2) preparation of complete hydrogen disproportionation Nd-Fe-B magnetic
By fast quenching Nd prepared by step (1) 12.5fe 80.5nb 1b 6magnetic is at H 2under atmosphere, within 30 minutes, carry out suction hydrogen-disproportionated reaction in 780 DEG C of insulations, cool to room temperature with the furnace after insulation terminates, obtain the complete hydrogen disproportionation Nd-Fe-B magnetic that crystallite dimension is 110-150nm;
(3) preparation of pressed compact
Complete hydrogen disproportionation Nd-Fe-B magnetic step (2) prepared loads in mould, in room temperature, magnetic is exerted pressure under argon shield, stop exerting pressure after the pressure suffered by magnetic is increased to 250MPa from 0MPa, 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
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (3) is warming up to 850 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2hot compression deformation-dehydrogenation restructuring is carried out for applying constant pressure to described Nd-Fe-B pressed compact under the condition of 0.0005Pa, force 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, cool to room temperature with the furnace after heat-insulation pressure keeping terminates, obtain the nanocrystalline Nd-Fe-B magnet of anisotropy that deflection is 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 the ingot casting Nd that anneals 12.6fe 72.3co 8.6al 0.5b 6.0magnetic is that anisotropy nanocrystalline magnet prepared by raw material, and processing step is as follows:
(1) anneal ingot casting Nd 12.6fe 72.3co 8.6al 0.5b 6.0the preparation of magnetic
With metal Nd (purity is for 99.5%), DT4 electrical pure iron (purity is for 99.95%), ferro-boron (Boron contents is for 19.65%), metal Co (purity is for 99.5%), metal A l(purity for 99%) for 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, the Al of 3% 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, power, to 0.05MPa, is then added to 38kW according to the alloying component calculated and carries out melting, pour in ingot mould, obtain plate-cast ingot after cooling after melting completes by alloy melt by applying argon gas.By obtained Nd 12.6fe 72.3co 8.6al 0.5b 6.0thin plate putting into 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 DEG C of insulations and carry out homogenizing annealing process in 16 hours under argon shield, will process the thin plate annealing ingot casting Mechanical Crushing obtained, cross 300 mesh sieves and remove fine powder, must anneal ingot casting Nd 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 DEG C of insulations and within 15 minutes, carry out suction hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, at vacuum degree < 5 × 10 -2be warming up to 820 DEG C of insulations under the condition of Pa and carry out dehydrogenation-recombining reaction in 5 minutes, cool to room temperature with the furnace after insulation terminates, obtaining crystallite dimension is that the part hydrogen disproportionation Nd-Fe-B magnetic of 160-200nm is (containing 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 step (2) prepared loads in mould, in room temperature, magnetic is exerted pressure under argon shield, stop exerting pressure after the pressure suffered by magnetic is increased to 500MPa from 0MPa, 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
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (3) is warming up to 750 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2hot compression deformation-dehydrogenation restructuring is carried out for applying constant pressure to described Nd-Fe-B pressed compact under the condition of 500Pa, force 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, cool to room temperature with the furnace after heat-insulation pressure keeping terminates, obtain the nanocrystalline Nd-Fe-B magnet of anisotropy that deflection is 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=500kA/m, (BH) m=205kJ/m 3.
Embodiment 15
The present embodiment is with the ingot casting Nd that anneals 15fe 78mo 1b 6magnetic is that anisotropy nanocrystalline magnet prepared by raw material, and processing step is as follows:
(1) anneal ingot casting Nd 15fe 78mo 1b 6preparation
With metal Nd (purity is for 99.5%), DT4 electrical pure iron (purity is for 99.95%), ferro-boron (Boron contents is for 19.65%), molybdenum-iron (Mo content is for 60%) for 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, power, to 0.05MPa, is then added to 40kW according to the alloying component calculated and carries out melting, pour in ingot mould, obtain plate-cast ingot after cooling after melting completes by alloy melt by applying argon gas.By obtained Nd 15fe 78mo 1b 6thin plate putting into 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 DEG C of insulations and carry out homogenizing annealing process in 16 hours under argon shield, will process the thin plate annealing ingot casting Mechanical Crushing obtained, cross 300 mesh sieves and remove fine powder, must anneal ingot casting Nd 15fe 78mo 1b 6magnetic.
(2) preparation of complete hydrogen disproportionation Nd-Fe-B magnetic
Annealing ingot casting Nd prepared by step (1) 15fe 78mo 1b 6magnetic is at H 2under atmosphere, within 30 minutes, carry out suction hydrogen-disproportionated reaction in 820 DEG C of insulations, cool to room temperature with the furnace after insulation terminates, obtain the complete hydrogen disproportionation Nd-Fe-B magnetic that crystallite dimension is 200-250nm;
(3) preparation of pressed compact
Complete hydrogen disproportionation Nd-Fe-B magnetic step (2) prepared loads in mould, in room temperature, magnetic is exerted pressure under argon shield, stop exerting pressure after the pressure suffered by magnetic is increased to 550MPa from 0MPa, 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
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (3) is warming up to 850 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2hot compression deformation-dehydrogenation restructuring is carried out for applying constant pressure to described Nd-Fe-B pressed compact under the condition of 0.001Pa, force 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, cool to room temperature with the furnace after heat-insulation pressure keeping terminates, obtain the nanocrystalline Nd-Fe-B magnet of anisotropy that deflection is 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 anisotropy nanocrystalline magnet prepared by raw material, and processing step is as follows:
(1) Nd 13.5fe 79.96al 0.24nb 0.3b 6the preparation of quenched powder
With metal Nd (purity is for 99.5%), DT4 electrical pure iron (purity is for 99.95%), ferro-boron (Boron contents is for 19.65%), ferro-niobium (Nb content is for 50%), metal A l(purity for 99%) for 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 calculated, power is added to 34kW and carry out melting; after melting completes, alloy melt is poured in ingot mould; plate-cast ingot is obtained after cooling; pellet is broken for after plate-cast ingot being ground off oxide skin; put into the copper crucible of LZK-12A type vacuum quick quenching equipment; under argon atmosphere; power up flow to 650A make load melting after be poured on copper roller that linear velocity is 32m/s; cooling obtains Nd Fe B alloys strip afterwards, after 300 mesh sieves remove fine powder excessively, namely obtains 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 DEG C of insulations and within 40 minutes, carry out suction hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, at vacuum degree < 5 × 10 -2be warming up to 800 DEG C of insulations under the condition of Pa and carry out dehydrogenation-recombining reaction in 6 minutes, cool to room temperature with the furnace after insulation terminates, obtaining crystallite dimension is that the part hydrogen disproportionation Nd-Fe-B magnetic of 250-270nm is (containing 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 step (2) prepared loads in mould, in room temperature, magnetic is exerted pressure under argon shield, stop exerting pressure after the pressure suffered by magnetic is increased to 300MPa from 0MPa, 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
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (3) is warming up to 820 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2hot compression deformation-dehydrogenation restructuring is carried out for applying constant pressure to described Nd-Fe-B pressed compact under the condition of 0.001Pa, force 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, cool to room temperature with the furnace after heat-insulation pressure keeping terminates, obtain the nanocrystalline Nd-Fe-B magnet of anisotropy that deflection is 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 the ingot casting Nd that anneals 13fe 71.86co 9al 0.08cu 0.06b 6magnetic is that anisotropy nanocrystalline magnet prepared by raw material, and processing step is as follows:
(1) anneal ingot casting Nd 13fe 71.86co 9al 0.08cu 0.06b 6preparation
With metal Nd (purity is for 99.5%), DT4 electrical pure iron (purity is for 99.95%), ferro-boron (Boron contents is for 19.65%), metal A l(purity for 99%), Ni metal (purity is for 99%), metal Co (purity is for 99.5%) for 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, power, to 0.05MPa, is then added to 38kW according to the alloying component calculated and carries out melting, pour in ingot mould, obtain plate-cast ingot after cooling after melting completes by alloy melt by applying argon gas.By obtained Nd 13fe 71.86co 9al 0.08cu 0.06b 6thin plate putting into 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 DEG C of insulations and carry out homogenizing annealing process in 18 hours under argon shield, will process the thin plate annealing ingot casting Mechanical Crushing obtained, cross 300 mesh sieves and remove fine powder, must anneal ingot casting Nd 13fe 71.86co 9al 0.08cu 0.06b 6magnetic.
(2) preparation of complete hydrogen disproportionation Nd-Fe-B magnetic
Annealing ingot casting Nd prepared by step (1) 13fe 71.86co 9al 0.08cu 0.06b 6magnetic is at H 2under atmosphere, within 45 minutes, carry out suction hydrogen-disproportionated reaction in 800 DEG C of insulations, cool to room temperature with the furnace after insulation terminates, obtain the complete hydrogen disproportionation Nd-Fe-B magnetic that crystallite dimension is 200-220nm;
(3) preparation of pressed compact
Part hydrogen disproportionation Nd-Fe-B magnetic step (2) prepared loads in mould, in room temperature, magnetic is exerted pressure under argon shield, stop exerting pressure after the pressure suffered by magnetic is increased to 550MPa from 0MPa, 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
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (3) is warming up to 820 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2hot compression deformation-dehydrogenation restructuring is carried out for applying constant pressure to described Nd-Fe-B pressed compact under the condition of 30Pa, the force value 3.2kN that exerts pressure, 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, cool to room temperature with the furnace after heat-insulation pressure keeping terminates, obtain the nanocrystalline Nd-Fe-B magnet of anisotropy that deflection is 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 the ingot casting Nd that anneals 14.5fe 76.4ti 2.5cr 1b 5.6magnetic is that anisotropy nanocrystalline magnet prepared by raw material, and processing step is as follows:
(1) anneal ingot casting Nd 14.5fe 76.4ti 2.5cr 1b 5.6preparation
With metal Nd (purity is for 99.5%), DT4 electrical pure iron (purity is for 99.95%), ferro-boron (Boron contents is for 19.65%), ferrotianium (Ti content 30.0%), ferrochrome (Cr content is for 65.0%) for 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, power, to 0.05MPa, is then added to 40kW according to the alloying component calculated and carries out melting, pour in ingot mould, obtain plate-cast ingot after cooling after melting completes by alloy melt by applying argon gas.By obtained Nd 14.5fe 76.4ti 2.5cr 1b 5.6thin plate putting into 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 DEG C of insulations and carry out homogenizing annealing process in 22 hours under argon shield, will process the thin plate annealing ingot casting Mechanical Crushing obtained, cross 300 mesh sieves and remove fine powder, must anneal ingot casting Nd 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 DEG C of insulations and within 30 minutes, carry out suction hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, at vacuum degree < 5 × 10 -2be warming up to 820 DEG C of insulations under the condition of Pa and carry out dehydrogenation-recombining reaction in 7 minutes, cool to room temperature with the furnace after insulation terminates, obtaining crystallite dimension is that the part hydrogen disproportionation Nd-Fe-B magnetic of 220-270nm is (containing 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 step (2) prepared loads in mould, in room temperature, magnetic is exerted pressure under argon shield, stop exerting pressure after the pressure suffered by magnetic is increased to 550MPa from 0MPa, 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
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (3) is warming up to 820 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2hot compression deformation-dehydrogenation restructuring is carried out for applying constant pressure to described Nd-Fe-B pressed compact under the condition of 10Pa, the force value 3kN that exerts pressure, 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, cool to room temperature with the furnace after heat-insulation pressure keeping terminates, obtain the nanocrystalline Nd-Fe-B magnet of anisotropy that deflection is 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=650kA/m, (BH) m=249kJ/m 3.
Embodiment 19
The present embodiment is with fast quenching Nd 14fe 79.4al 0.6b 6magnetic is that anisotropy nanocrystalline magnet prepared by raw material, and processing step is as follows:
(1) Nd 14fe 79.4al 0.6b 6the preparation of quenched powder
With metal Nd (purity is for 99.5%), DT4 electrical pure iron (purity is for 99.95%), ferro-boron (Boron contents is for 19.65%), metal A l(purity for 99%) for 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, power, to 0.05MPa, is then added to 32kW according to the alloying component calculated and carries out melting, pour in ingot mould, obtain plate-cast ingot after cooling after melting completes by alloy melt by applying argon gas.Pellet is broken for after plate-cast ingot being ground off oxide skin; put into the copper crucible of LZK-12A type vacuum quick quenching equipment; under argon atmosphere; power up flow to 650A make load melting after be poured on copper roller that linear velocity is 34m/s; Nd Fe B alloys strip is obtained after cooling; cross after 300 mesh sieves remove fine powder, namely 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 DEG C of insulations and within 45 minutes, carry out suction hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, at vacuum degree < 5 × 10 -2be warming up to 820 DEG C of insulations under the condition of Pa and carry out dehydrogenation-recombining reaction in 5 minutes, cool to room temperature with the furnace after insulation terminates, obtaining crystallite dimension is that the part hydrogen disproportionation Nd-Fe-B magnetic of 250-280nm is (containing 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 step (2) prepared loads in mould, in room temperature, magnetic is exerted pressure under argon shield, stop exerting pressure after the pressure suffered by magnetic is increased to 300MPa from 0MPa, 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
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (3) is warming up to 850 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2hot compression deformation-dehydrogenation restructuring is carried out for applying constant pressure to described Nd-Fe-B pressed compact under the condition of 0.0001Pa, force 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, cool to room temperature with the furnace after heat-insulation pressure keeping terminates, obtain the nanocrystalline Nd-Fe-B magnet of anisotropy that deflection is 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 the ingot casting Nd that anneals 15fe 77.9cu 1.5b 5.6magnetic is that anisotropy nanocrystalline magnet prepared by raw material, and processing step is as follows:
(1) anneal ingot casting Nd 15fe 77.9cu 1.5b 5.6preparation
With metal Nd (purity is for 99.5%), DT4 electrical pure iron (purity is for 99.95%), ferro-boron (Boron contents is for 19.65%), Ni metal (purity is for 99%) for 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, power, to 0.05MPa, is then added to 32kW according to the alloying component calculated and carries out melting, pour in ingot mould, obtain plate-cast ingot after cooling after melting completes by alloy melt by applying argon gas.By obtained Nd 15fe 77.9cu 1.5b 5.6thin plate putting into 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 DEG C of insulations and carry out homogenizing annealing process in 12 hours under argon shield, will process the thin plate annealing ingot casting Mechanical Crushing obtained, cross 300 mesh sieves and remove fine powder, must anneal ingot casting Nd 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 DEG C of insulations and within 60 minutes, carry out suction hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, at vacuum degree < 5 × 10 -2be warming up to 820 DEG C of insulations under the condition of Pa and carry out dehydrogenation-recombining reaction in 5 minutes, cool to room temperature with the furnace after insulation terminates, obtaining crystallite dimension is that the part hydrogen disproportionation Nd-Fe-B magnetic of 280-350nm is (containing 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 step (2) prepared loads in mould, in room temperature, magnetic is exerted pressure under argon shield, stop exerting pressure after the pressure suffered by magnetic is increased to 300MPa from 0MPa, 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
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (3) is warming up to 820 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2hot compression deformation-dehydrogenation restructuring is carried out for applying constant pressure to described Nd-Fe-B pressed compact under the condition of 10Pa, force 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, cool to room temperature with the furnace after heat-insulation pressure keeping terminates, obtain the nanocrystalline Nd-Fe-B magnet of anisotropy that deflection is 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=350kA/m, (BH) m=142kJ/m 3.
Embodiment 21
The present embodiment is with the ingot casting Nd that anneals 13.8fe 70.6co 5mo 3.8al 1b 5.8magnetic is that anisotropy nanocrystalline magnet prepared by raw material, and processing step is as follows:
(1) anneal ingot casting Nd 13.8fe 70.6co 5mo 3.8al 1b 5.8preparation
With metal Nd (purity is for 99.5%), DT4 electrical pure iron (purity is for 99.95%), ferro-boron (Boron contents is for 19.65%), metal Co (purity is for 99%), molybdenum-iron (Mo content is for 60%), metal A l(purity for 99%) for 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, power, to 0.05MPa, is then added to 38kW according to the alloying component calculated and carries out, pour in ingot mould, obtain plate-cast ingot after cooling after melting completes by alloy melt by applying argon gas.By obtained Nd 13.8fe 70.6co 5mo 3.8al 1b 5.8thin plate, putting into 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 DEG C of insulations and carry out homogenizing annealing process in 16 hours under argon shield, will process the thin plate annealing ingot casting Mechanical Crushing obtained, cross 300 mesh sieves and remove fine powder, must anneal ingot casting Nd 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 DEG C of insulations and within 45 minutes, carry out suction hydrogen-disproportionated reaction, after inhaling hydrogen-disproportionated reaction, at vacuum degree < 5 × 10 -2be warming up to 820 DEG C of insulations under the condition of Pa and carry out dehydrogenation-recombining reaction in 5 minutes, cool to room temperature with the furnace after insulation terminates, obtaining crystallite dimension is that the part hydrogen disproportionation Nd-Fe-B magnetic of 260-300nm is (containing 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 step (2) prepared loads in mould, in room temperature, magnetic is exerted pressure under argon shield, stop exerting pressure after the pressure suffered by magnetic is increased to 600MPa from 0MPa, 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
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (3) is warming up to 820 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2be apply constant pressure to described Nd-Fe-B pressed compact 0.001 time to carry out hot compression deformation-dehydrogenation restructuring, force 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, cool to room temperature with the furnace after heat-insulation pressure keeping terminates, obtain the nanocrystalline Nd-Fe-B magnet of anisotropy that deflection is 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 anisotropy nanocrystalline magnet prepared by raw material, and processing step is as follows:
(1) Nd 13fe 71.86co 9.08cu 0.06b 6the preparation of quenched powder
With metal Nd (purity is for 99.5%), DT4 electrical pure iron (purity is for 99.95%), ferro-boron (Boron contents is for 19.65%), metal Co (purity is for 99%), Ni metal (purity is for 99%) for raw material, according to Nd 13fe 71.86co 9.08cu 0.06b 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, power, to 0.05MPa, is then added to 34kW according to the alloying component calculated and carries out, pour in ingot mould, obtain plate-cast ingot after cooling after melting completes by alloy melt by applying argon gas.Pellet is broken for after plate-cast ingot being ground off oxide skin; put into the crucible of LZK-12A type vacuum quick quenching equipment; under argon atmosphere; power up flow to 700A make load melting after be poured on copper roller that linear velocity is 34m/s; Nd Fe B alloys strip is obtained after cooling; cross after 300 mesh sieves remove fine powder, namely obtain Nd 13fe 71.86co 9.08cu 0.06b 6rapidly quenched magnetic powder.
(2) preparation of complete hydrogen disproportionation Nd-Fe-B magnetic
Annealing ingot casting Nd prepared by step (1) 13fe 71.86co 9al 0.08cu 0.06b 6magnetic is at H 2under atmosphere, within 20 minutes, carry out suction hydrogen-disproportionated reaction in 800 DEG C of insulations, cool to room temperature with the furnace after insulation terminates, obtain the complete hydrogen disproportionation Nd-Fe-B magnetic that crystallite dimension is 180-200nm;
(3) preparation of pressed compact
Complete hydrogen disproportionation Nd-Fe-B magnetic step (2) prepared loads in mould, in room temperature, magnetic is exerted pressure under argon shield, stop exerting pressure after the pressure suffered by magnetic is increased to 350MPa from 0MPa, 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
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (3) is warming up to 820 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2hot compression deformation-dehydrogenation restructuring is carried out for applying constant pressure to described Nd-Fe-B pressed compact under the condition of 500Pa, force 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, cool to room temperature with the furnace after heat-insulation pressure keeping terminates, obtain the nanocrystalline Nd-Fe-B magnet of anisotropy that deflection is 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. a preparation method for anisotropy nano-crystalline neodymium-iron-boronmagnet magnet, is characterized in that processing step is as follows successively:
(1) preparation of complete hydrogen disproportionation or part hydrogen disproportionation Nd-Fe-B magnetic
By Nd-Fe-B alloy powder at H 2under atmosphere, within 5 minutes ~ 60 minutes, carry out suction hydrogen-disproportionated reaction in 650 DEG C ~ 820 DEG C insulations, cool to room temperature with the furnace after insulation terminates, obtaining crystallite dimension is nano level complete hydrogen disproportionation Nd-Fe-B magnetic;
Or by Nd-Fe-B alloy powder at H 2under atmosphere, within 5 minutes ~ 60 minutes, carry out suction hydrogen-disproportionated reaction in 650 DEG C ~ 820 DEG C insulations, after inhaling hydrogen-disproportionated reaction, at vacuum degree < 5 × 10 -2within 1 ~ 10 minute, carry out dehydrogenation-recombining reaction in 780 DEG C ~ 820 DEG C insulations under the condition of Pa, cool to room temperature with the furnace after insulation terminates, 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 step (1) prepared or part hydrogen disproportionation Nd-Fe-B magnetic load in mould, under room temperature, inert gas shielding, magnetic is exerted pressure, stop exerting pressure after the pressure suffered by magnetic is increased to 100MPa ~ 600MPa from 0MPa, obtain the hydrogen disproportionation thing pressed compact of Nd-Fe-B;
(3) hot compression deformation-dehydrogenation restructuring
Nd-Fe-B hydrogen disproportionation thing pressed compact prepared by step (2) is warming up to 680 DEG C ~ 850 DEG C, under vacuum then at this temperature and hydrogen dividing potential drop P h2for 0Pa < P h2under the condition of≤1kPa, constant pressure is applied to described Nd-Fe-B hydrogen disproportionation thing pressed compact and carries out hot compression deformation-dehydrogenation restructuring, force value of exerting pressure change between 30MPa ~ 1.5MPa with the pressure that Nd-Fe-B hydrogen disproportionation thing pressed compact bears in thermal deformation-dehydrogenation regrouping process and be limited, the heat-insulation pressure keeping time is 5 ~ 120 minutes, cool to room temperature with the furnace after heat-insulation pressure keeping terminates, obtain anisotropy nano-crystalline neodymium-iron-boronmagnet magnet.
2. the preparation method of anisotropy nano-crystalline neodymium-iron-boronmagnet magnet according to claim 1, is characterized in that the chemical formula of described Nd-Fe-B alloy powder is Nd xfe 100-x-y-zm yb z, wherein 12≤x≤15,0≤y≤10,5.6≤z≤6, M is at least one in Co, Ga, Zr, Nb, Cu, Al, Cr, Mo, Ti.
3. the preparation method of described anisotropy nano-crystalline neodymium-iron-boronmagnet magnet 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 one.
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CN108115139B (en) * 2016-11-28 2021-07-27 罗伯特·博世有限公司 Method and apparatus for producing thermally deformed magnet
CN108428542B (en) * 2017-02-14 2020-06-12 中国科学院宁波材料技术与工程研究所 Preparation method of high-performance anisotropic neodymium iron boron magnet under liquid-phase-free condition
CN111091944B (en) * 2019-12-31 2021-06-04 浙江大学 Lanthanum-cerium-yttrium-rich multi-main-phase fine-grain rare earth permanent magnet material and preparation method thereof
CN111968851A (en) * 2020-09-23 2020-11-20 赣州富尔特电子股份有限公司 Method for preparing anisotropic neodymium iron boron magnetic powder by directionally crushing thermal deformation magnet
CN116682661A (en) * 2023-05-12 2023-09-01 燕山大学 Preparation method of neodymium-iron-boron permanent magnet material

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