CN103567446B - A kind of Toughening-type rare earth permanent-magnetic material and preparation method thereof - Google Patents
A kind of Toughening-type rare earth permanent-magnetic material and preparation method thereof Download PDFInfo
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Abstract
The invention provides the preparation method of a kind of Toughening-type rare earth permanent-magnetic material, comprise the following steps: S1, employing ingot casting or rapid hardening rejection tablet technique prepare RE permanent magnetic alloy, obtain alloy powder through broken, grinding；S2, toward alloy powder adds toughener and organic additive, and mix homogeneously；Described toughener is selected from SiC whisker, CuO whisker, TiC whisker, Si3N4Whisker, AlN whisker, TiO2Whisker, SnO2At least one in whisker；S3, mixed system is carried out that magnetic field orientating is compressing and isostatic pressed, after sintering and being tempered, obtain rare earth permanent-magnetic material.Present invention also offers the Toughening-type rare earth permanent-magnetic material using this preparation method to prepare.The preparation method that the present invention provides, on the premise of keeping magnetic property to be basically unchanged, can significantly improve toughness and the processing characteristics of RE permanent magnetic alloy, thus prepare the rare earth permanent-magnetic material that mechanical property been significantly enhanced.
Description
Technical field
The invention belongs to field of magnetic material, the preparation method particularly relating to a kind of Toughening-type rare earth permanent-magnetic material and the rare earth permanent-magnetic material prepared by this preparation method.
Background technology
Nineteen eighty-three, SUMITOMO CHEMICAL metal company has invented Nd-Fe-B permanent magnet material first.Since coming out, Nd-Fe-B permanent magnet material is owing to having the advantages such as the resources reserve of high energy product, the price of relative moderate and abundance, particularly neodymium iron boron has the highest ratio of performance to price, therefore become and manufacture that usefulness is high, volume is little, the ideal material of the magnetic function device of light weight, many applications are produced revolutionary impacts.
Nd2Fe14B is tetragonal crystal system, and its crystal structure is complicated, and slip system is little, does not therefore have yield deformation, and this just determines Nd2Fe14B series compound is fragile material.And the Brittleness of neodymium iron boron greatly limit its application, the processing such as grinding section, spark cutting, laser can only be carried out, and the course of processing easily cause broken, fall the defective products such as corner, raised product cost.
By adding iron fiber or other fibrous metal silk in sintered NdFeB magnetic powder in prior art, it not only can not play toughness reinforcing effect, can react with Nd Fe B alloys in sintering process on the contrary and cause neodymium iron boron component segregation, even destroy its tetragonal crystal structure, cause magnetic property to reduce.
Disclosing the preparation method of a kind of motor sintered NdFeB improving processability in CN201110347367, it is by adding antimony, copper and titanium elements during alloy melting in neodymium iron boron, to improve the mechanical property of alloy.But in the method, for modified metallic element and alloy compositions melting simultaneously, the metal element content that thus be accordingly used in modification is unsuitable too high, otherwise can cause alloying component segregation, when but content is relatively low its to improve effect the most limited, can not effectively strengthen the toughness of alloy so that the processing characteristics of alloy product is the most poor.
CN200810249555 disclosing a kind of boron nitride nano-tube Grain-Boundary Phase interpolation and prepares tough magnets method, the steps include: 1) main-phase alloy uses casting technique to make neodymium iron boron cast ingot alloy, and crystal-boundary phase alloy uses rapid quenching technique to make rapid tempering belt；2) by main-phase alloy and crystal-boundary phase alloy powder process respectively；3) boron nitride nano-tube is added in crystal-boundary phase alloy powder；4) mixed main-phase alloy and crystal-boundary phase alloy powder are compressing in magnetic field；5) in high vacuum sintering furnace, sintered magnet is made.The method is dual alloy method, complex process；It addition, the boron nitride nano-tube cost used is high, it is unfavorable for producing volume production；And using the bending strength ＜ 300MPa of magnet that the method prepares, it is the most very limited that its toughness improves effect.
Summary of the invention
The present invention solves poor toughness that prior art middle rare earth permanent magnet material exists, modified effect is limited during toughening modifying and the technical problem of complex process.
The invention provides the preparation method of a kind of Toughening-type rare earth permanent-magnetic material, comprise the following steps:
S1, employing ingot casting or rapid hardening rejection tablet technique prepare RE permanent magnetic alloy, then obtain, through broken, grinding, the alloy powder that particle diameter is 3-5 μm；
S2, toward 100 weight portion alloy powders add toughener and the organic additive of 0.01-1 weight portion of 0.02-2 weight portion, and mix homogeneously；Described toughener is selected from SiC whisker, CuO whisker, TiC whisker, Si3N4Whisker, AlN whisker, TiO2Whisker, SnO2At least one in whisker；
S3, the mixed system obtained by S2 carry out that magnetic field orientating is compressing and isostatic pressed, are then sintered and are tempered, obtaining described Toughening-type rare earth permanent-magnetic material.
Present invention also offers a kind of Toughening-type rare earth permanent-magnetic material, described Toughening-type rare earth permanent-magnetic material preparation method provided by the present invention prepares.
In the preparation method of the Toughening-type rare earth permanent-magnetic material that the present invention provides, by using SiC, CuO, TiC, Si of high-melting-point, whisker level that toughness is high3N4、AlN、TiO2、SnO2As the toughener of RE permanent magnetic alloy, in sintering process can effective crystal grain thinning, thus improve toughness of material；In combination with compound transmission, crackle bridging, the crack deflection of whisker and extract effect etc. and strengthen mechanism, the toughness of rare earth permanent-magnetic material can be further enhanced, obtain the Toughening-type rare earth permanent-magnetic material that the present invention provides.
Detailed description of the invention
The invention provides the preparation method of a kind of Toughening-type rare earth permanent-magnetic material, comprise the following steps:
S1, employing ingot casting or rapid hardening rejection tablet technique prepare RE permanent magnetic alloy, then obtain, through broken, grinding, the alloy powder that particle diameter is 3-5 μm；
S2, toward 100 weight portion alloy powders add toughener and the organic additive of 0.01-1 weight portion of 0.02-2 weight portion, and mix homogeneously；Described toughener is selected from SiC whisker, CuO whisker, TiC whisker, Si3N4Whisker, AlN whisker, TiO2Whisker, SnO2At least one in whisker；
S3, the mixed system obtained by S2 carry out that magnetic field orientating is compressing and isostatic pressed, are then sintered and are tempered, obtaining described Toughening-type rare earth permanent-magnetic material.
Specifically, in the present invention, consisting of of described RE permanent magnetic alloy: REaFe(100-a-b-c)BbMc, wherein 9at%≤a≤18at%, 5at%≤b≤8at%, 0≤c≤15at%；At least one in Nd, Pr, Dy, Tb, Ho, Ga of RE, at least one in Co, Al, Cu, Zr, Ni, Sn, Ga, Nb, Mo, Ti of M.
In the present invention, being that hydrogen is broken or broken by crusher in crushing, preferably hydrogen by the method that RE permanent magnetic alloy is broken, its crushing effect is more preferably.The broken method of described hydrogen is known to those skilled in the art, RE permanent magnetic alloy ingot casting or rapid hardening rejection tablet technique prepared loads in hydrogen crushing furnace, after evacuation, it is filled with high-purity hydrogen, under 0.02-1.2MPa hydrogen pressure, inhale hydrogen 0.5-5h, hearing the cracker of alloy, can detect that the temperature of container is constantly raising simultaneously, this is to form hydride volumetric expansion after RE permanent magnetic alloy inhales hydrogen and burst, then dehydrogenase 12-10h at 450-650 DEG C, obtains flour.Described known to those skilled in the art by the method for crusher in crushing, carry out coarse crushing for example with jaw crusher, broken in then being carried out by middle disintegrating machine.
In the present invention, hydrogen flour after broken is crushed by described grinding further, thus completes the pulverizing process of alloy.The method of described grinding is airflow milling or ball milling, preferably airflow milling.The method of airflow milling powder is known to those skilled in the art, and it, for utilizing air-flow that powder particle is accelerated to supersonic speed, is allowed to mutually clash and crush.Flour after being crushed by airflow milling makes the alloy powder that mean diameter is 3-5 μm.
In the preparation method of the Toughening-type rare earth permanent-magnetic material that the present invention provides, by using SiC, CuO, TiC, Si of high-melting-point, whisker level that toughness is high3N4、AlN、TiO2、SnO2As the toughener of RE permanent magnetic alloy, in sintering process can effective crystal grain thinning, thus improve toughness of material；In combination with compound transmission, crackle bridging, the crack deflection of whisker and extract effect etc. and strengthen mechanism, the toughness of rare earth permanent-magnetic material can be further enhanced, obtain the Toughening-type rare earth permanent-magnetic material that the present invention provides.
In the present invention, described whisker is the chopped fiber by high-purity crystal growth, and its diameter is generally micron or systems.As a kind of preferred implementation of the present invention, in the present invention, the whisker length of described toughener is 1-50 μm.
The present inventor is by the discovery of further experiment, and in the present invention, described toughener is selected from SiC whisker and the mixture of CuO whisker.In the case of more preferably, on the basis of the gross mass of toughener, wherein brilliant and CuO whisker the mass ratio of SiC is 1:(1-5).
As it was previously stated, in the present invention, on the basis of the alloy powder of 100 weight portions, the consumption 0.02-2 weight portion of toughener, more preferably 0.1-0.3 weight portion.
In the present invention, described organic additive is the existing various organic additives prepared and commonly use in RE permanent magnetic alloy, its Main Function includes: the lubricity of raising powder, to improve the magnetic field orientating molding degree of orientation, intercepts powder particles simultaneously and contacts with oxygen, prevent alloy powder oxidized.Therefore, described organic additive includes but not limited to various lubricant commonly used in the prior art and/or antioxidant.Wherein, one or more during described antioxidant is selected from polyethylene oxide alkyl ethers, poly(ethylene oxide) mono fatty acid ester or poly(ethylene oxide) allyl ether.Described lubricant can use the mixture of oleic acid, stearic acid and their salt, polyhydric alcohol, Polyethylene Glycol, sorbitol and anhydro sorbitol and glyceryl stearate.In the present invention, described lubricant, antioxidant also can directly use commercial products, the present invention to be not particularly limited.
The method that mixed system is orientated in magnetic field compressing blank is conventional method, under preferable case, is compressed to blank in magnetic field orientating moulding press.The compressing condition of described magnetic field orientating is: carry out being orientated compressing in the Constant charge soil or pulsed magnetic field of 1.5-5T.The condition of described isostatic pressed is: at 170-220MPa isostatic pressed, the compressing blank obtained is kept 15-120s.
In this step S3, blank is positioned in sintering furnace, sinters 2-6 hour at 1000-1200 DEG C, use low-temperature sintering can be prevented effectively from blank crystal grain and grow up faster.Cavity it is provided with in described sintering furnace, cavity inner wall ring-type molybdenum filament cincture at certain intervals, energising makes molybdenum filament generate heat, then mainly it is applied on blank with thermal-radiating form, heating blank, described blank i.e. die mould block, shape is with the processing external form of required permanent magnet as reference.The step of described tempering is: first carries out one-level tempering at 800-1000 DEG C, and keeps 1-4h, then carry out second annealing at 400-600 DEG C, and keeps 1-4h.Rare earth permanent-magnetic material is conducive to obtain good microstructure through two-stage temper.
In the present invention, the step of described sintering and tempering is preferably carried out under vacuum or inert gas shielding.Described noble gas can be any gas being not involved in reaction, preferably one or more in group 0 element gas.
Present invention also offers a kind of Toughening-type rare earth permanent-magnetic material, described Toughening-type rare earth permanent-magnetic material preparation method provided by the present invention prepares.
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearer, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
Embodiment 1
(1) using casting ingot process to prepare Nd Fe B alloys block, its composition is (PrNd)12.64Dy1.47Fe77.79B6Co1.2Al0.5Cu0.2Ga0.2.Then Nd Fe B alloys block is used and under 1.0MPa hydrogen pressure, inhale dehydrogenation 6h at hydrogen 1.5h, and 560 DEG C, obtain hydrogen flour；Then by hydrogen flour being ground to form the alloy powder that granularity is 3～4 μm.
(2) this alloy powder 100 weight portion is taken, being subsequently adding 0.1 weight portion SiC whisker (a length of 1-50 μm) and 0.1 weight portion antioxidant and lubricant, use American three-dimensional material mixer batch mixing, batch mixing rotating speed is 30r/min, mixing time is 2h, obtains mixed system.
(3) mixed system is orientated in the Constant charge soil of 1.5-2T compressing, and through 190MPa isostatic pressed keep 15s, obtain blank.By blank under argon shield, proceed to 1070 DEG C of sintering 4.5h in vacuum sintering furnace, and carry out one-level tempering 2h, then second annealing 3h at 490 DEG C at 900 DEG C, obtain the rare earth permanent-magnetic material 1 of the present embodiment.
Comparative example 1
Using step same as in Example 1 to prepare the rare earth permanent-magnetic material DS1 of this comparative example, difference is:
In step (2), in 100 weight portion alloy powders, only add 0.1 weight portion antioxidant and lubricant, be added without SiC whisker；Then using American three-dimensional material mixer batch mixing, batch mixing rotating speed is 30r/min, and mixing time is 2h, obtains mixed system.
By above-mentioned steps, obtain the rare earth permanent-magnetic material DS1 of this comparative example.
Embodiment 2
(1) using rapid hardening rejection tablet technique to prepare Nd Fe B alloys thin slice, its composition is (PrNd)10.65Dy3.5Fe77.46B5.9Co1.73Al0.5Cu0.16Nb0.1.Then Nd Fe B alloys thin slice is used and under 1.1MPa hydrogen pressure, inhale dehydrogenation 8h at hydrogen 2.5h, and 500 DEG C, obtain hydrogen flour；Then by hydrogen flour being ground to form the alloy powder that granularity is 3～4 μm.
(2) this alloy powder 100 weight portion is taken, it is subsequently adding 0.1 weight portion SiC whisker (a length of 1-50 μm), the CuO whisker (a length of 1-50 μm) of 0.1 weight portion and 0.1 weight portion antioxidant and lubricant, use American three-dimensional material mixer batch mixing, batch mixing rotating speed is 30r/min, mixing time is 2h, obtains mixed system.
(3) mixed system is orientated in the Constant charge soil of 1.5-2T compressing, and through 190MPa isostatic pressed keep 15s, obtain blank.By blank under argon shield, proceed to 1080 DEG C of sintering 4.5h in vacuum sintering furnace, and carry out one-level tempering 2h, then second annealing 3.5h at 550 DEG C at 900 DEG C, obtain the rare earth permanent-magnetic material 2 of the present embodiment.
Comparative example 2
Using step same as in Example 2 to prepare the rare earth permanent-magnetic material DS1 of this comparative example, difference is:
In step (2), in 100 weight portion alloy powders, only add 0.1 weight portion antioxidant and lubricant, be added without SiC whisker, CuO whisker；Then using American three-dimensional material mixer batch mixing, batch mixing rotating speed is 30r/min, and mixing time is 2h, obtains mixed system.
By above-mentioned steps, obtain the rare earth permanent-magnetic material DS2 of this comparative example.
Embodiment 3
Using step same as in Example 1 to prepare the rare earth permanent-magnetic material DS1 of the present embodiment, difference is:
In step (2), in 100 weight portion alloy powders, only add 2 weight portion TiC whiskers (a length of 1-50 μm), 0.3 weight portion antioxidant and lubricant；Then using American three-dimensional material mixer batch mixing, batch mixing rotating speed is 30r/min, and mixing time is 2h, obtains mixed system.
By above-mentioned steps, obtain the rare earth permanent-magnetic material 3 of the present embodiment.
Embodiment 4
Using step same as in Example 1 to prepare the rare earth permanent-magnetic material DS1 of the present embodiment, difference is:
In step (2), in 100 weight portion alloy powders, only add 0.01 weight portion TiO2Whisker (a length of 1-50 μm), 0.01 weight portion AlN whisker (a length of 1-50 μm) and 0.01 weight portion antioxidant and lubricant；Then using American three-dimensional material mixer batch mixing, batch mixing rotating speed is 30r/min, and mixing time is 2h, obtains mixed system.
By above-mentioned steps, obtain the rare earth permanent-magnetic material 4 of the present embodiment.
Embodiment 5
Using step same as in Example 1 to prepare the rare earth permanent-magnetic material DS1 of the present embodiment, difference is:
In step (2), in 100 weight portion alloy powders, only add 0.05 weight portion SiC whisker (a length of 1-50 μm), 0.25 weight portion CuO whisker (a length of 1-50 μm) and 0.03 weight portion antioxidant and lubricant；Then using American three-dimensional material mixer batch mixing, batch mixing rotating speed is 30r/min, and mixing time is 2h, obtains mixed system.
By above-mentioned steps, obtain the rare earth permanent-magnetic material 5 of the present embodiment.
Comparative example 3
Method disclosed in CN201110347367 embodiment one is used to prepare the Nd Fe B alloys sample DS3 of this comparative example.
Comparative example 4
Method disclosed in CN200810249555 embodiment 1 is used to prepare the Nd Fe B alloys sample DS4 of this comparative example.
Performance test
1-5 and DS1-DS4 is processed as the specification piece of 60mm (length) × 6mm (wide) × 5mm (high), and its camber 5mm direction is differently-oriented directivity.Microcomputer controlled electronic universal tester (model C MT5105) is used to carry out three-point bending resistance strength test, loading span is 40mm, compression rate is 0.1mm/min, and compression aspect is parallel to neodymium iron boron differently-oriented directivity, records the three-point bending resistance average strength (σ of each magnet samplebb).Test result is as shown in table 1.
Table 1
| Sample | σbb/MPa |
| 1 | 353 |
| DS1 | 267 |
| 2 | 376 |
| DS2 | 239 |
| 3 | 195 |
| 4 | 324 |
| 5 | 362 |
| DS3 | 278 |
| DS4 | 286 |
From upper table 1,1 compares it can be seen that use whisker level toughener toughness reinforcing to RE permanent magnetic alloy in the preparation method of present invention offer with the test result of DS1,2 and DS2, can significantly improve the processing characteristics of alloy.
Can be seen that from the test result of 1-5 with DS3, DS4, toughness and the magnetic property of alloy can be effectively ensured in the preparation method that the present invention provides, and modified metal element adds during alloy melting in DS3, alloying component segregation is more or less caused to cause magnetic property to reduce；On the one hand complex process, relatively costly in DS4；On the other hand to improve effect the most very limited for the method toughness.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all any amendment, equivalent and improvement etc. made within the spirit and principles in the present invention, should be included within the scope of the present invention.
Claims (9)
1. the preparation method of a Toughening-type rare earth permanent-magnetic material, it is characterised in that comprise the following steps:
S1, employing ingot casting or rapid hardening rejection tablet technique prepare RE permanent magnetic alloy, then obtain the alloy powder that particle diameter is 3-5 μm, consisting of of described RE permanent magnetic alloy: RE through broken, grindingaFe(100-a-b-c)BbMc, wherein 9at%≤a≤18at%, 5at%≤b≤8at%, 0≤c≤15at%；At least one in Nd, Pr, Dy, Tb, Ho, Ga of RE, at least one in Co, Al, Cu, Zr, Ni, Sn, Ga, Nb, Mo, Ti of M；
S2, toward 100 weight portion alloy powders add toughener and the organic additive of 0.01-1 weight portion of 0.02-2 weight portion, and mix homogeneously；Described toughener is selected from SiC whisker, CuO whisker, TiC whisker, Si3N4Whisker, AlN whisker, TiO2Whisker, SnO2At least one in whisker, described organic additive includes antioxidant and/or lubricant；
S3, the mixed system obtained by S2 carry out that magnetic field orientating is compressing and isostatic pressed, are then sintered and are tempered, obtaining described Toughening-type rare earth permanent-magnetic material.
Preparation method the most according to claim 1, it is characterised in that in step S1, described in be broken for hydrogen broken, the broken condition of hydrogen is: by RE permanent magnetic alloy under 0.02-1.2MPa hydrogen pressure, inhaling hydrogen 0.5-5h, at 450-650 DEG C, dehydrogenase 12-10h, obtains flour；The method of described grinding is airflow milling or ball milling.
Preparation method the most according to claim 1, it is characterised in that in step S2, the whisker length of described toughener is 1-50 μm.
4., according to the preparation method described in claim 1 or 3, it is characterised in that in step S2, described toughener is selected from SiC whisker and the mixture of CuO whisker；On the basis of the gross mass of toughener, wherein brilliant and CuO whisker the mass ratio of SiC is 1:(1-5).
Preparation method the most according to claim 4, it is characterised in that on the basis of the alloy powder of 100 weight, the consumption of toughener is 0.1-0.3 weight portion.
Preparation method the most according to claim 1, it is characterised in that in step S3, the compressing condition of described magnetic field orientating is: carry out being orientated compressing in the Constant charge soil or pulsed magnetic field of 1.5-5T；The condition of described isostatic pressed is: at 170-220MPa isostatic pressed, the compressing blank obtained is kept 15-120s.
Preparation method the most according to claim 1, it is characterised in that the condition of described sintering is: sintering temperature is 1000-1200 DEG C, sintering time is 2-6 hour；The step of described tempering is: first carries out one-level tempering at 800-1000 DEG C, and keeps 1-4h, then carry out second annealing at 400-600 DEG C, and keeps 1-4h.
8. according to the preparation method described in claim 1 or 7, it is characterised in that described sintering and tempering are carried out under vacuum or inert gas shielding.
9. a Toughening-type rare earth permanent-magnetic material, it is characterised in that described Toughening-type rare earth permanent-magnetic material is prepared by the preparation method described in any one of claim 1-8.
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| CN105427988A (en) * | 2015-11-27 | 2016-03-23 | 宁波科星材料科技有限公司 | High temperature resistant samarium cobalt permanent magnet and preparation method thereof |
| CN106252011B (en) * | 2016-08-29 | 2019-01-29 | 浙江东阳东磁稀土有限公司 | A kind of method that the compound addition of Grain-Boundary Phase improves coercivity of sintered ndfeb |
| CN106910586B (en) * | 2017-05-03 | 2019-08-27 | 南京信息工程大学 | A kind of magnetic composite and preparation method |
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