CN101154489B - Anti-impact ferrous rare earth permanent magnet and its manufacturing method - Google Patents

Anti-impact ferrous rare earth permanent magnet and its manufacturing method Download PDF

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CN101154489B
CN101154489B CN2007101212017A CN200710121201A CN101154489B CN 101154489 B CN101154489 B CN 101154489B CN 2007101212017 A CN2007101212017 A CN 2007101212017A CN 200710121201 A CN200710121201 A CN 200710121201A CN 101154489 B CN101154489 B CN 101154489B
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rare earth
permanent magnet
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CN101154489A (en
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李卫
王会杰
朱明刚
郭朝晖
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Central Iron and Steel Research Institute
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Abstract

The invention provides a shock resistance iron base rare-earth permanent-magnet material and a preparation method of the same. The chemical composition are that Nd18-25, Re0.5-1.5, TM65-73, M0.1-1 and B5-6, wherein, Re is the lanthanon chosen from Dy and Tb, TM is the transition element chosen from Fe and Co, and M is the microadd element chosen from Nb, Cu and Ti. The preparation method is to increase the proportion of Nd with low hardness and high plasticity in the magnet to improve the ultimate strain energy rate so as to improve the obdurability and shock resistance of magnet. Relative tothe machinable magnet of FeCrCo, the invention prepares the magnet with stronger magnetism and machinable property as well as shock resistance, thereby lowering the processing cost of magnet.

Description

Anti-impact ferrous rare earth permanent magnet and preparation method thereof
Technical field
The invention belongs to the manufacturing field of rare earth permanent-magnetic material, be specially adapted to the preparation of anti-impact ferrous rare earth permanent magnetic material.
Background technology
Rare earth permanent-magnetic material has a wide range of applications in various fields such as space flight navigation, information electronics, the energy, traffic, communication, health cares as important Metallic Functional Materials.In fact, industrial circle never stops the improvement of Nd-Fe-B permanent magnetic material, for example, Chinese patent application 92100958.5 (applying date 1992.01.31) discloses a kind of " rare earth-iron-boron based anisotropy magnet ", be a kind of magnetic anisotropy excellence, and the little R-Fe-B coefficient body of coercitive temperature coefficient.The R-Fe-B based permanent magnet powder that it is crossed by hydrogen treat is made, its component by atomic percent is: R:10-20%, B:3-20%, one or more elements among Ti, V, Nb, Ta, Al and the Si, its total amount is 0.001-5.0%, all the other are that Fe and unavoidable impurities are formed, and it is the collecting structure of the crystal grain of 0.05-20 μ m that average grain diameter is arranged, the crystal grain of the maximum particle diameter/minimum grain size of single crystal grain<2, in structure, account for more than 50% of whole crystal particle volumes, constitute the R-Fe-B anisotropy magnet thus.
Aspect manufacture method, for example Chinese invention patent ZL02158707.8 (applying date 2002.12.26) discloses a kind of " the R-Fe-B based sintered magnet and the manufacture method thereof that contain micro amount of oxygen ", is to adopt inert atmosphere (to comprise N in manufacture process 2Atmosphere) anaerobic technology (ZHOFP) technology under the protection; Control for Oxygen Content in the magnet obtains having the high-quality sintering R-Fe-B magnet of excellent homogeneity in 100~1200ppm scope; after the airflow milling classification, the following superfine powder of 2 μ m can be directly used in makes high-quality R-Fe-B magnet.
But the obdurability of rare earth permanent-magnetic material is very poor, and this has become its deadly defect.Intermetallic compound R 2Fe 14B belongs to square crystal structure, and himself slip system is less, adds the coating of the requisite rich neodymium phase of constituent material permanent magnetism performance, general R 2Fe 14B and rich neodymium ratio mutually are about (weight ratio) 98: 2~93: 7.Rich neodymium phase structure more complicated, because material is a liquid phase sintered material, rich neodymium constitutes the carrying out of liquid phase acceleration of sintering mutually in the sintering process.Rich neodymium generally has two kinds of distributional patterns mutually in sintered magnet: (1) is the thick lamelliform of 1~1.5nm at the place, grain boundary; (2) reunite at crystal boundary corner place, diameter is generally less than 2 microns.Therefore a little less than the rich neodymium of shell shape combines with principal phase, thereby constituted grain-boundary weakness, this makes material be fractured into the master with the edge crystalline substance, has constituted typical brittle fracture.Sintered Nd-Fe-B Magnet shows as low impact resistance.This makes rare earth permanent-magnetic material be difficult to processing, has increased the processing cost of material, reduces the machining accuracy of material; Simultaneously, shock resistance is poor, also makes material fall the limit arrisdefect easily in processes such as production, processing, transportation, assembling, even fracture; Low anti shock and vibration ability influences material stability and fail safe in use.
In a word, the obdurability difference has not only increased the production cost of rare earth permanent-magnetic material, and seriously restricts the further expansion of material range of application.
Summary of the invention
The objective of the invention is to: a kind of anti-impact ferrous rare earth permanent magnet is provided.
Another object of the present invention is to: the preparation method that a kind of above-mentioned anti-impact ferrous rare earth permanent magnet is provided.
To achieve these goals, the present invention is achieved in that
A kind of anti-impact ferrous rare earth permanent magnet, it comprises the Nd of high rigidity 2Fe 14B, the chemical composition of this permanent magnet by atomic percent is: Nd 18-25, Re 0.5-1.5, TM 65-73, M 0.1-1, B 5-6, wherein Re is the rare earth element that is selected from Dy, Tb, TM is the transition element that is selected from Fe, Co, and M is the trace additives that is selected from Nb, Cu, Ti, and all the other are inevitable trace impurity; Wherein, this permanent magnet also comprises the rich rare earth precipitate of high-ductility.
The rich rare earth precipitate of high-ductility is rich neodymium phase.
Nd 2Fe 14B is 90: 10~80: 20 with rich neodymium volume ratio mutually.
The room temperature fracture toughness scope of permanent magnet is 6~8.5MPam -1/2, the bending strength scope is 360~420MPa, the maximum magnetic flux performance is not less than 23MGOe.
A kind of powder sintered preparation method of anti-impact ferrous rare earth permanent magnet comprises that batching, smelting, fast quenching obtain quick setting belt, and with this quick setting belt fragmentation, this permanent magnet is by Nd 2Fe 14B is composited mutually with rich neodymium, the chemical composition of rare-earth permanent magnet by atomic percent is: Nd 18-25, Re 0.5-1.5, TM 65-73, M 0.1~1, B 5-6, wherein Re is the rare earth element that is selected from Dy, Tb, TM is the transition element that is selected from Fe, Co, and M is the trace additives that is selected from Nb, Cu, Ti, and all the other are inevitable trace impurity;
This method also comprises the steps:
A. the rapid-hardening flake powder of fragmentation is inhaled hydrogen and dehydrogenation processing;
B. in alignment magnetic field, powder is carried out moulding;
C. adopt the malleation sintering;
D. adjusting the magnet two-phase by tempering distributes.
The granularity of rapid-hardening flake powder is 3.2~4.5 μ m.
The desorption temperature of dehydrogenation step is 550~650 ℃, and dehydrogenation pressure is 2 * 10 -3Pa.
In the magnetic field powder is carried out comprising also magnet is waited static pressure that pressure is 200MPa after the forming step.
When the sintering temperature of sintering step was 1000~1200 ℃, the time was 60~120 minutes, and the maintenance argon pressure is 0.2MPa.
Tempering step is sample to be quenched after 60~120 minutes 850~950 ℃ of insulations, carries out Quenching Treatment 560~650 ℃ of insulations after 120 minutes then.
Also add the low melting point liquid phase powder in the rapid-hardening flake powder, low melting point liquid phase powder and rapid-hardening flake proportion of powder are about 0.1-0.7: 99.3-99.9, this low melting point liquid phase powder is rich rare earth compound or rare earth hydride.
Described low melting point liquid phase powder is DyH x, (Dy, Nd) H xIn at least a, wherein X is 2.
A kind of discharge sintering preparation method of anti-impact ferrous rare earth permanent magnet comprises that batching, smelting, fast quenching obtain quick setting belt, and with this quick setting belt fragmentation, this permanent magnet is by Nd 2Fe 14B is composited mutually with rich neodymium, the chemical composition of rare-earth permanent magnet by atomic percent is: Nd 18-25, Re 0.5-1.5, Fe 65-73, M 0.1~1, B 5-6, wherein Re is the rare earth element that is selected from Dy, Tb, TM is the transition element that is selected from Fe, Co, and M is the trace additives that is selected from Nb, Cu, Ti, and all the other are inevitable trace impurity;
This method also comprises the steps:
A. earlier with the magnetic orientation, be orientated a 1.5~2.5T; Press down then, it is 100~250MPa that pressure is controlled at, and passes to big electric current simultaneously;
B. make magnet temperature rise to 550~900 ℃, magnet is depressed into theoretical density, after hot pressing is finished, use the high pressure argon gas that magnet is cooled off fast;
C. the intact sample of sintering is carried out tempering.
Hot pressing carries out under protective atmosphere.
Described tempering step is: quench 850~950 ℃ of insulations 60~120 minutes and to sample, 700~750 ℃ are incubated 60~120 minutes and sample are carried out Water Quenching, quench after 120 minutes 560~650 ℃ of insulations then.
In sum, key of the present invention is: by improving composition, improve the moulding proportion that resembles in the magnet.Utilize the burning hot compression technology of sintering to prepare the theoretical density magnet, be equipped with optimum tempering process simultaneously, strengthen the bond strength between principal phase and the crystal boundary phase.By increasing moulding phase proportion in the magnet, and strengthen combine with the plasticity richness rare earth way of intensity of main phase grain, prepare the anti-impact ferrous rare earth permanent magnetic material.Under the prerequisite that keeps than high magnetic characteristics, increase substantially the shock resistance vibrations performance of magnet.
Particularly, the present invention is carrying out following improvement aspect composition and the manufacture method two:
Improve about composition
Commercial sintering (Nd, R)-bending strength of Fe-B is generally at 220~300MPa, and fracture toughness is at 4.5 ± 0.5MPaM -1/2, impact toughness is about 3.5kJ/m 2, shock resistance is lower.For fragile material, under many circumstances, its destruction is to be subjected to a percussion, therefore improve the sintered magnet obdurability primary be the shock resistance that will improve magnet.
Can process permanent magnet and generally include three kinds: 1) FeCrCo-type, such magnet magnetic property especially coercive force is very low; 2) PtCo-type, the price of such magnet are its fatal shortcomings; 3) bonded permanent magnet, the magnetic property of such magnet is very low, 50% of normally similar sintered magnet performance.
The permanent magnet of the present invention's preparation will realize that its shock resistance is significantly increased than commercial magnet, and the raising of mechanical property will effectively reduce the destruction of magnet in processing and use, improves the processability and the reliability of magnet greatly.
In sum, be to utilize and follow plastic history to improve magnet strength and fracture toughness in the magnet impact failure according to the solution that above-mentioned purpose proposed.Because in plastic history, the energy that magnet absorbs is much higher.Plasticity mainly is rich neodymium phase mutually in the magnet, and plasticity in the magnet destructive process plastic deformation takes place, and absorbs energy and reduces the purpose that stress is concentrated thereby reach, thereby improve magnet strength and fracture toughness.By improving ratio and the principal phase and plasticity internal stress enhancement effect mutually of plasticity phase in the magnet, can effectively improve the energy that magnet absorbed before destroying, and then improve the shock resistance of magnet greatly, prepare the rare earth permanent-magnetic material that has high magnetic characteristics and impact resistance concurrently.
The chemical analysis of anti-impact ferrous rare earth permanent magnet (atom %): (NdHRe) 18-25(FeTM) 67- 77M 0.1-2B 5-6, wherein HRe represents heavy rare earth, and TM represents transition element, and M represents other trace additives, and all the other are because the trace impurity that material purity brought.
Nd in the prior art 2Fe 14B is about 98: 2 with rich neodymium part by weight mutually~and 93: 7, the Nd among the present invention 2Fe 14The B principal phase is about 90: 10 with rich neodymium volume ratio mutually~and 80: 20.
The preparation method improves
The invention provides powder sintered and two kinds of preparation methods of discharge sintering.
Anti-impact ferrous rare earth permanent magnet adopts powder sintered preparation method, and concrete preparation technology is:
After the above-mentioned anti-impact ferrous rare earth permanent magnetism meal component preparation, in vaccum sensitive stove, under argon shield, carry out melting.Adopt rapid hardening technology that alloy is made rapid-hardening flake.Adopt rapid-hardening flake to compare the cooling rate that can improve alloy cast ingot with common ingot casting, the microstructure of refinement ingot casting among the present invention.For obtaining principal phase, final magnet creates precondition with mutually even, the tiny microstructure of rich neodymium.Carry out the hydrogen fragmentation then, in pulverizing process, mix a small amount of low melting point liquid phase.
The powder sintered preparation technology of anti-impact ferrous rare earth permanent magnet is:
1, carries out proportioning according to component ratio, utilize induction furnace that alloying component is smelted.After smelting is finished molten steel injected in the water cooled copper mould and cool off, perhaps molten steel is carried out rapid hardening and handle, be prepared into rapid-hardening flake, rolling speed is 1~5m/s.
2, alloy cast ingot is inhaled hydrogen and handle, ingot casting is put into closed container and is evacuated to 2 * 10 -1Pa.Feed H 2To 1.5 * 10 5Pa, magnetic is inhaled the hydrogen fragmentation.After fragmentation is finished magnetic is carried out dehydrogenation and handle, desorption temperature is 550~650 ℃, and dehydrogenation pressure is 2 * 10 -3Pa.
3, the alloyed powder of getting after the dehydrogenation carries out airflow milling, and gas is high pure nitrogen or argon gas, and the temperature of airflow milling process is 20 ℃~40 ℃.Mix a small amount of antioxidant (the antioxidant main component is methyl palmitate and toluene) in the alloyed powder to increase abrasive dust efficient, prevent that magnetic from merging once more and magnetic is protected, the ratio that antioxidant accounts for magnetic is about (weight %) 0.1-0.2%.Then, low melting point liquid phase (rich rare earth compound or rare earth hydride) mixed with certain proportion together carry out abrasive dust, the low melting point liquid phase mainly comprises: DyH x, (Dy, Nd) H x, all in pulverizing process, mix with alloy cast ingot with powder morphology.PrH xIts fusing point is 931 ℃, (Pr, Nd) H xFusing point increase and increase along with Nd content, scope is: 931 ℃~1010 ℃.Low melting point liquid phase and principal phase ratio are about 0.5: 99.5.Granularity of magnet powder is adjusted to 3.2~4.5 μ m.
4, under nitrogen or argon shield, carry out weighing, moulding in being orientated a magnetic field that is 1.5~5T.
5, static pressure such as magnet is carried out, pressure is 200MPa.
6, the sample that static pressure such as will pass through is put into sintering furnace, and sintering temperature is 1010 ℃~1120 ℃, and sintering time is 60~120 minutes.Sintering adopts the malleation sintering, pours argon gas after reaching sintering temperature, and the maintenance argon pressure is 0.2Mpa, behind the sintering sample is carried out Quenching Treatment to room temperature.
7, the intact sample of sintering is carried out tempering, quench, quench after 120 minutes 560~650 ℃ of insulations then 850~950 ℃ of insulations 60~120 minutes and to sample.
Anti-impact ferrous rare earth permanent magnet also can adopt the preparation method of discharge sintering, specifically prepares the worker Skill is:
1, carries out proportioning according to component ratio, utilize induction furnace that alloying component is smelted.After smelting is finished molten steel injected in the water cooled copper mould and cool off, perhaps molten steel is carried out rapid hardening and handle, be prepared into rapid-hardening flake, rolling speed is 1~5m/s.
2, coarse crushing alloyed powder at first carries out airflow milling then, and gas is high pure nitrogen or argon gas.The temperature of airflow milling process is 20 ℃~40 ℃, and the ratio that antioxidant accounts for magnetic is about (weight %) one thousandth, and antioxidant is methyl palmitate or toluene.
Low melting point liquid phase (rich rare earth compound or rare earth hydride) mixed with certain proportion carry out abrasive dust together.The low melting point liquid phase mainly comprises: DyH x, (Dy, Nd) H x, all in pulverizing process, mix with alloy cast ingot with powder morphology.PrH xIts fusing point is 931 ℃, (Dy, Nd) H xFusing point increase and increase along with Nd content, scope is: 931 ℃~1010 ℃.Low melting point liquid phase and principal phase ratio are about 0.5: 99.5.Granularity of magnet powder is adjusted to 3.2~4.5 μ m.
3, quenched powder is put into mould, mode of heating adopts the way of discharge heating.
4, at first with the magnet orientation, orientation 1.5~2.5T.Press down then, it is 100~250MPa that pressure is controlled at, and passes to big electric current simultaneously, makes magnet temperature rise to 700~900 ℃, and magnet is depressed into theoretical density.Use the high pressure argon gas that magnet is cooled off fast after hot pressing is finished, this process is all carried out under inert gas shielding or in the vacuum.
5, the intact sample of sintering is carried out tempering, quench, quench after 120 minutes 560~650 ℃ of insulations then 850~950 ℃ of insulations 60~120 minutes and to sample.
The present invention by introducing plasticity Nd preferably, effectively increases the plastic deformation that magnet took place for improving the obdurability of permanent magnet before destroying, increase the fracture interface energy simultaneously, thereby the critical strain that has effectively increased magnet can release rate.Overcome principal phase hardness height to a certain extent, the shortcoming that fragility is big has increased the obdurability of magnet.
Add copper and increase the liquid phase flowable, copper adds in the alloying ingredient stage with simple substance form, also other raw material together melting form alloy.Copper can form the low melting point liquid phase with neodymium metal, and the low melting point liquid phase can promote magnet to shrink in sintering process, improves the wetness degree between the principal phase particle, and then strengthens the bond strength between the principal phase particle, thereby increases the mechanical strength of magnet.Add the low melting point liquid phase or add with its hydride form in pulverizing process, liquid phase contains higher content of rare earth.Add a spot of antioxidant in pulverizing process, main component is the mixture of toluene and methyl palmitate, claims powder, die mould then, and the orientation field is 2~3T, and again sample being carried out pressure is static pressure processing such as 20MPa.To wait the intact sample of static pressure to carry out the shove charge sintering, 300 ℃, 800 ℃ to the sample processing that outgases, vacuum degree reaches 2 * 10 -3Shi Shengwen, sintering temperature is 1010 ℃~1125 ℃, sintering time is 60~120 minutes.It is 0.2Mpa that sintering process adopts the malleation sintering pressure, after temperature is reduced to room temperature, sample is carried out tempering, tempering is a second annealing, comprise 850~950 ℃ of insulations 60~120 minutes and sample quenched, 700~750 ℃ are incubated 60~120 minutes and sample are carried out Water Quenching, quench after 120 minutes 500~650 ℃ of insulations at last.After heat treatment is finished sample is carried out machining, it is saturated under magnetic field sample to be magnetized at last.
Compared with prior art, beneficial effect of the present invention is: the more commercial magnet of anti-impact ferrous rare earth permanent magnetic material has higher shock resistance, vibration performance, can resist the requirement of impact to magnet magnetic property stability.Can bear higher acceleration percussion, be particularly suitable for the special occasions that some is had relatively high expectations to the material shock resistance, have the excellent magnetism energy simultaneously.Owing to introduce the plasticity phase in a large number in RE permanent magnetic alloy, thereby improved the obdurability of magnet, have excellent intrinsic magnetic properties simultaneously and can and have very high coercive force.
Embodiment
Table 1 is the concrete chemical composition of the alloy of anti-impact ferrous rare earth permanent magnet of the present invention; Table 2,3 and 4 is the preparation technology of anti-impact ferrous rare earth permanent magnet of the present invention; Table 5 is the every performance and the prior art performance comparison table of the embodiment of the invention; Table 6 is a drop weight method to the magnetic property of magnet commonly used and the contrast of shock resistance, and wherein sample is of a size of Φ 10 * 4mm 2The comparison that table 7 is permanent magnet of the present invention and FeCrCo can process the permanent magnetism magnetic property.
Table 1: the anti-impact ferrous rare earth permanent magnetic material chemical composition (atom %) of the embodiment of the invention
Table 2: embodiment of the invention anti-impact ferrous rare earth permanent magnetic material preparation technology
Figure B2007101212017D00112
Table 3: embodiment of the invention shock resistance (Nd, R)-Fe-B rare-earth permanent magnet hot pressing preparation technology
Table 4: embodiment of the invention anti-impact ferrous rare earth permanent magnetic material preparation technology
Figure B2007101212017D00121
Table 5: the performance comparison of embodiment of the invention anti-impact ferrous rare earth permanent magnet and prior art
Figure B2007101212017D00122
Annotate: in an embodiment, 1 (1)+3 (1) refers to that composition combines with technology in the table 3 in the table 1, all the other and the like.
Table 6: the contrast of magnet commonly used and anti-impact ferrous rare earth permanent magnetic material magnetic property and shock resistance
Table 7: the contrast of invention magnet and machinability FeCrCo magnet
Figure B2007101212017D00132

Claims (13)

1. anti-impact ferrous rare earth permanent magnet, it comprises the Nd of high rigidity 2Fe 14B is characterized in that:
The chemical composition of this permanent magnet by atomic percent is: Nd 18-25, Re 0.5-1.5, TM65-73, M 0.1-1, B 5-6, wherein Re is the rare earth element that is selected from Dy, Tb, TM is the transition element that is selected from Fe, Co, M is the trace additives that is selected from Nb, Cu, Ti, and all the other are inevitable trace impurity;
Wherein, this permanent magnet also comprises the rich rare earth precipitate of high-ductility, and this richness rare earth precipitate is rich neodymium phase, Nd 2Fe 14B is 90: 10~80: 20 with rich neodymium volume ratio mutually.
2. anti-impact ferrous rare earth permanent magnet as claimed in claim 1 is characterized in that: the room temperature fracture toughness scope of described permanent magnet is 6~8.5MPam -1/2, the bending strength scope is 360~420MPa, the maximum magnetic flux performance is not less than 23MGOe.
3. the powder sintered preparation method of an anti-impact ferrous rare earth permanent magnet comprises that batching, smelting, fast quenching obtain quick setting belt, with this quick setting belt fragmentation, it is characterized in that:
This permanent magnet is by Nd 2Fe 14B is composited Nd mutually with rich neodymium 2Fe 14B is 90: 10~80: 20 with rich neodymium volume ratio mutually, the chemical composition of rare-earth permanent magnet by atomic percent is: Nd18-25, Re 0.5-1.5, TM 65-73, M 0.1~1, B 5-6, wherein Re is the rare earth element that is selected from Dy, Tb, TM is the transition element that is selected from Fe, Co, and M is the trace additives that is selected from Nb, Cu, Ti, and all the other are inevitable trace impurity;
This method also comprises the steps:
A. the rapid-hardening flake powder of fragmentation is inhaled hydrogen and dehydrogenation processing;
B. in alignment magnetic field, powder is carried out moulding;
C. adopt the malleation sintering;
D. adjusting the magnet two-phase by tempering distributes.
4. preparation method according to claim 3 is characterized in that: the granularity of described rapid-hardening flake powder is 3.2~4.5 μ m.
5. preparation method according to claim 3 is characterized in that: the desorption temperature of described dehydrogenation step is 550~650 ℃, and dehydrogenation pressure is 2 * 10 -3Pa.
6. preparation method according to claim 3 is characterized in that: in the described magnetic field powder is carried out comprising also magnet is waited static pressure that pressure is 200MPa after the forming step.
7. preparation method according to claim 3 is characterized in that: when the sintering temperature of described sintering step was 1000~1200 ℃, the time was 60~120 minutes, and the maintenance argon pressure is 0.2MPa.
8. preparation method according to claim 3 is characterized in that: described tempering step carries out Quenching Treatment 560~650 ℃ of insulations after 120 minutes then for sample being quenched after 60~120 minutes 850~950 ℃ of insulations.
9. preparation method according to claim 3, it is characterized in that: also add the low melting point liquid phase powder in the described rapid-hardening flake powder, low melting point liquid phase powder and rapid-hardening flake proportion of powder are 0.1-0.7: 99.3-99.9, and this low melting point liquid phase powder is rich rare earth compound or rare earth hydride.
10. preparation method according to claim 9 is characterized in that: described low melting point liquid phase powder is DyH x, (Dy, Nd) H xIn at least a, wherein X is 2.
11. the discharge sintering preparation method of an anti-impact ferrous rare earth permanent magnet comprises that batching, smelting, fast quenching obtain quick setting belt, with this quick setting belt fragmentation, it is characterized in that:
This permanent magnet is by Nd 2Fe 14B is composited Nd mutually with rich neodymium 2Fe 14B is 90: 10~80: 20 with rich neodymium volume ratio mutually, the chemical composition of rare-earth permanent magnet by atomic percent is: Nd18-25, Re 0.5-1.5, Fe 65-73, M 0.1~1, B 5-6, wherein Re is the rare earth element that is selected from Dy, Tb, TM is the transition element that is selected from Fe, Co, and M is the trace additives that is selected from Nb, Cu, Ti, and all the other are inevitable trace impurity;
This method also comprises the steps:
A. earlier with the magnetic orientation, be orientated a 1.5~2.5T; Press down then, it is 100~250MPa that pressure is controlled at, and passes to big electric current simultaneously;
B. make magnet temperature rise to 550~900 ℃, magnet is depressed into theoretical density, after hot pressing is finished, use the high pressure argon gas that magnet is cooled off fast;
C. the intact sample of sintering is carried out tempering.
12. preparation method according to claim 11 is characterized in that: described hot pressing carries out under protective atmosphere.
13. preparation method according to claim 11, it is characterized in that: described tempering step is: quench 850~950 ℃ of insulations 60~120 minutes and to sample, 700~750 ℃ are incubated 60~120 minutes and sample are carried out Water Quenching, quench after 120 minutes 560~650 ℃ of insulations then.
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