CN104646677A - Preparation method of magnetic powder - Google Patents
Preparation method of magnetic powder Download PDFInfo
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- CN104646677A CN104646677A CN201510003975.4A CN201510003975A CN104646677A CN 104646677 A CN104646677 A CN 104646677A CN 201510003975 A CN201510003975 A CN 201510003975A CN 104646677 A CN104646677 A CN 104646677A
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Abstract
The invention provides a preparation method of magnetic powder. The method comprises the following steps: (a) adding a magnetic material, milling balls, an organic solvent and a selectively added surfactant into a ball milling tank; (b) sealing the ball milling tank, and then, carrying out ball milling, wherein a ball milling process is of speed-gradually-increased staged ball milling and at least comprises two ball milling stages, and the time of ball milling of each stage is 0.5-24 hours; (c) taking out the milling balls, pouring a ball-milled product into a vessel, flushing and drying, thereby obtaining the magnetic powder. Compared with the traditional single-speed-adopted ball milling manner, the preparation method has the advantages that the magnetic powder with higher texture degree and more-complete crystal structure can be obtained due to a multistage different-speed ball milling method; the preparation method of the magnetic powder, provided by the invention, is simple in steps, new equipment is not required to be added, and implementation can be achieved by only changing ball milling speed during ball milling and controlling corresponding ball milling time, so that the application is very extensive.
Description
Technical field
The present invention relates to field of magnetic material, relate more specifically to a kind of small-size magnetic raw powder's production technology.
Background technology
Along with modern development, much new field requires that raw-material size is the smaller the better, even little of nano-scale and following.Such as need little size to increase the magnetic refrigerating field of heat exchange, need little size obtain the permanent magnetism field of high-coercive force and need little size to reduce the electromagnetic arts etc. of eddy-current loss.Although chemically can synthesize the little material to nanoscale, output is considerably less, and chemical reagent also can cause certain pollution to material.Therefore, the main still physics of method producing small scale particle at present in enormous quantities is broken, such as ball milling, airflow milling etc.Because the final size size of fragmentation and the power of grinding are directly proportional, so less particle will be obtained just need higher energy.High energy proposes certain requirement to equipment on the one hand, next the more important thing is that high energy can destroy the crystal structure of material, for the application of portion of material, material is not only needed to keep a little size, secondly material is also needed to keep a complete crystal structure, particularly in rare earth permanent-magnetic material, unbodied material does not almost have performance.Therefore high-energy ball milling is except being applied in except in specific material, is mainly used in alloying process.
But lead his team to use the surfactant nano particle of smaller particle size of having assisted the mode of ball milling to prepare along with professor Liu Ping of the development, particularly branch school, Arlington of texas,U.S university in 2006 (The University of Texas at Arlington) of ball grinding technique.The method that ball milling prepares small size powder is subject to extensive concern both domestic and external again, because surfactant generally uses in liquid environment, so the effect slowing down impact force can be played, therefore surfactant assists ball milling often to use high-energy ball milling to reach the object reducing particle size, secondly, surfactant itself also can play the effect preventing cold welding, so can prepare more short grained material, particularly needs the rare earth permanent-magnetic material of full die.And on this basis, US Patent No. 2012/0021219A1 it is also proposed a kind of preparation method using surfactant auxiliary ball to grind standby magnetic Nano sheet.Because the fragility of material during low temperature can increase, so Chinese patent CN103231066A it is also proposed a kind of use low temperature to add method that surfactant auxiliary ball grinds standby rare earth-transition race permanent-magnet alloy micrometer/nanometer particle afterwards, the method can obtain the less magnetic Nano sheet of granularity.
Even if but employ the auxiliary mechanical milling process (also comprise low temperature and assist ball milling) of surfactant, material crystal structure after ball milling still obtains and destroys significantly, for needing the material keeping complete crystal structure as far as possible, particularly permanent magnetism class material (high magnetocrystalline anisotropy), all need the later stage very strict heat treatment etc. eliminate the negative effect that this crystal structure defects brings.
Summary of the invention
Therefore, the object of this invention is to provide a kind of preparation method that can obtain the small-particulate materials of lower crystal structure defects.Preparation method of the present invention can overcome the shortcoming of prior art, improved by simple on the basis of existing technology, obtain the small-particulate materials (micron is to nanometer) with complete crystal structure more of texture degree stronger (magnetic anisotropy is stronger).
To achieve these goals, the invention provides a kind of preparation method of magnetic powder, the method comprises the following steps:
A the surfactant of magnetic material and abrading-ball, organic solvent and selective interpolation joins in ball grinder by ();
B () carries out ball milling after being sealed by ball grinder, wherein, the process of ball milling is the ball milling stage by stage of speed increase, comprises at least two ball milling stages, and the Ball-milling Time in each stage is 0.5 ~ 24 hour;
C () takes out abrading-ball, pour in container by ball milling product, obtains magnetic powder after rinsing drying.
According to preparation method provided by the invention, preferably, described mechanical milling process comprises at least three ball milling stages, more preferably comprises at least four ball milling stages.
According to preparation method provided by the invention, wherein, the Ball-milling Time in each stage is preferably 1 ~ 20 hour, is more preferably 3 ~ 15 hours.
As described in the present invention, " ball milling stage by stage of speed increase " refers to: mechanical milling process is divided at least two stages, to the last stage from first stage, ball milling speed increases successively.The amplitude that the present invention increases for each stage ball milling speed is not particularly limited, the amplitude that each stage speed increases can be the same or different, as long as adopt " ball milling stage by stage of speed increase " of the present invention mode, namely effectively can strengthen the texture degree of small-particulate materials and improve the integrality of crystal structure.
According to preparation method provided by the invention, wherein, the ball milling speed of first stage can be 1 ~ 200rpm, and the ball milling speed of second stage can be 100 ~ 300rpm.When described method comprises at least three ball milling stages, the ball milling speed of three phases can be 200 ~ 400rpm.When described method comprises at least four ball milling stages, the ball milling speed of the last stage can for being greater than 400rpm.Wherein, the Ball-milling Time in each stage can be the same or different.
According to preparation method provided by the invention, wherein, described magnetic material can be rare earth permanent-magnetic material or the non-rare earth permanent-magnetic material of Mn base.The average particle size particle size being applied to the magnetic material of the inventive method can be 1 to 400 microns.
Preferably, described rare earth compound comprises R-T system rare earth permanent-magnetic material, wherein R represents one or more in Y, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, and T represents one or more the combination in one or more and Cu, Zr, Al, Ga, Nb, Hf, B, N, the C in one or more or Fe, Co, Ni, the Mn in transition elements Fe, Co, Ni, Mn.
Preferably, the non-rare earth permanent-magnetic material of described Mn base can comprise Mn-Al, Mn-Ga and Mn-Bi.
According to preparation method provided by the invention, wherein, the organic solvent that described organic solvent can be commonly used for this area, such as ethanol, acetone, normal heptane etc.
According to preparation method provided by the invention, wherein, described surfactant can be cationic, anionic, nonionic surface active agent or their any combination.
Preferably, described surfactant is one or more in oleic acid, oleyl amine, trioctylamine, polyvinylpyrrolidone, sad and aliphatic acid polyethenoxy ether.
According to preparation method provided by the invention, wherein, the consumption of described organic solvent can be 5% ~ 2000% of magnetic material mass, preferably fills it up with whole ball mill container (ball grinder).The consumption of described surfactant can be 15% ~ 45% of magnetic material mass.
Compared to the ball milling method of the single speed of traditional use, the ball grinding method of multistage friction speed of the present invention can obtain the Magnaglo that texture degree is stronger, crystal structure is more complete.Magnaglo preparation method step of the present invention is simple, does not need to add new equipment, only needs in the process of ball milling, to change ball milling speed and control corresponding Ball-milling Time and can realize, therefore applies widely.The method can be used for high-performance and low-cost soft/production of Hard Magnetic coupling magnet and two (many) principal phases permanent-magnet alloy, also can be used for preparing microwave absorbing material and magnetic refrigerating material.
Accompanying drawing explanation
Below, describe embodiment of the present invention in detail by reference to the accompanying drawings, wherein:
The scanning electron microscope (SEM) photograph of the magnetic powder that Fig. 1 embodiment of the present invention 1 is obtained;
The x-ray diffraction pattern of the magnetic powder that Fig. 2 embodiment of the present invention 1 is obtained;
The hysteresis curve of the magnetic powder that Fig. 3 embodiment of the present invention 1 is obtained.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is further described in detail, the embodiment provided only in order to illustrate the present invention, instead of in order to limit the scope of the invention.
embodiment 1
1, the SmCo after coarse crushing is taken
5material 5g (particle size is less than 400 μm), load stainless steel jar mill, then add the stainless steel abrading-ball (80g of the 20g of 8mm, 5mm) of 100g, and 1ml oleic acid and 1ml oleyl amine are as surfactant, finally add 100ml normal heptane as organic solvent.
2, the ball grinder that magnetic material, abrading-ball, surfactant and organic solvent are housed is sealed in glove box.The ball grinder of good seal is contained on GN-2 type high energy ball mill, ball milling 5 hours under the voltage of 30v (about 150 revs/min); Then ball milling 10 hours under the voltage of 40v (about 200 revs/min); Then ball milling 15 hours under the voltage of 50v (about 250 revs/min).
3, take out abrading-ball, the ball milling product after ball milling is poured in centrifuge tube, use normal heptane to rinse 5 times, then dry, namely arrive magnetic powder of the present invention.
product characterizes
1, the magnetic powder that the present embodiment is obtained is put into ESEM to measure, result as shown in Figure 1.It is thick that visible the inventive method can obtain 50 ~ 200nm, the nanometer sheet of 1 ~ 2 μm long.
2, the magnetic powder that the present embodiment is obtained is put into x-ray diffractometer and measure crystal structure, as shown in Figure 2, it has stronger diffraction maximum as seen, illustrates and has than more complete degree of crystallinity.
3, dried magnetic powder and nonmagnetic epoxide-resin glue (must answer health (Devcon) No. 14270 two component epoxy glue) are mixed, then orientation under magnetic field, measures the XRD (as shown in Figure 2) of composite and the hysteresis curve (as shown in Figure 3) of different directions after waiting epoxy resin cure.The result of XRD shown in Fig. 2 can be found out, except (001), (002) diffraction crystal face almost can't see other diffraction maximum outward, the ratio approach infinity of its (002) diffraction maximum and (111) diffraction maximum (be can't see (111 diffraction maximum), is illustrated that this material has the very strong degree of orientation.In Fig. 3, direction of easy axis represents the direction that direction of measurement is parallel to magnetic field orientating, and hard direction represents the direction of direction of measurement perpendicular to magnetic field orientating.The hysteresis curve of different directions also illustrates that the magnetic Nano sheet obtained through the inventive method has very strong texture (magnetic anisotropy).
comparative example 1
This comparative example adopts traditional single speed ball milling, for contrasting with the embodiment of the present invention 1.
1, the SmCo after coarse crushing is taken
5material 5g (particle size is less than 400 μm), load stainless steel jar mill, then add 100g stainless steel abrading-ball (80g of the 20g of 8mm, 5mm), and 1ml oleic acid and 1ml oleyl amine are as surfactant, finally add 100ml normal heptane as organic solvent.
2, the ball grinder that magnetic material, abrading-ball, surfactant and organic solvent are housed is sealed in glove box.The ball grinder of good seal is contained on GN-2 type high energy ball mill, ball milling 30 hours under the voltage of 50v (about 250 revs/min).Take out abrading-ball, the ball milling product after ball milling is poured in centrifuge tube, use normal heptane to rinse 5 times, then dry.
Measure the character of magnetic powder, result is as shown in table 1.
Measurement result can be found out, although also can obtain the nanometer sheet of 50 ~ 200nm through disposable long-time ball milling, its degree of orientation, texture degree, coercivity all present decline clearly.
comparative example 2
Result in result of the present invention and existing document is contrasted further, by document 1 (Anisotropic SmCo
5nanoflakes by surfactant-assisted high energy ballmilling, JOURNAL OF APPLIED PHYSICS 107,09A721 (2010)) and document 2 (The effect of flake thickness on anisotropic SmCo
5nanoflakes/submicronflakes with high energy product, JOURNAL OFAPPLIED PHYSICS 109,07A762 (2011)) in data also arrange in Table 1.
By with the results contrast reported in document 1 and 2, also can find out that the present invention uses no matter the multistep magnetic powder that ball milling obtains stage by stage is coercivity significantly, or texture degree or the degree of orientation are all higher than the ball milling result using a traditional step constant speed at present.
embodiment 2
1, the SmCo after coarse crushing is taken
5material 5g (particle size is less than 400 μm), loads stainless steel jar mill, then adds 100g stainless steel abrading-ball (80g of the 20g of 8mm, 5mm), finally add 100ml normal heptane as organic solvent.
2, the ball grinder that magnetic material, abrading-ball and organic solvent are housed is sealed in glove box.The ball grinder of good seal is contained on GN-2 type high energy ball mill, ball milling 1 hour under the voltage of 30v (about 150 revs/min), then ball milling 2 hours under the voltage of 40v (about 200 revs/min), then ball milling 4 hours under the voltage of 50v (about 250 revs/min).
3, take out abrading-ball, pour in centrifuge tube by the ball milling product after ball milling, use normal heptane to rinse 5 times, then drying obtains magnetic powder of the present invention.
The measurement result of the magnetic powder that the present embodiment obtains is as shown in table 1.
comparative example 3
1, the SmCo after coarse crushing is taken
5material 5g (particle size is less than 400 μm), loads stainless steel jar mill, then adds 100g stainless steel abrading-ball (80g of the 20g of 8mm, 5mm), finally add 100ml normal heptane as organic solvent.
2, the ball grinder that magnetic material, abrading-ball and organic solvent are housed is sealed in glove box.The ball grinder of good seal is contained on GN-2 type high energy ball mill, ball milling 7 hours under the voltage of 50v (about 250 revs/min).
3, take out abrading-ball, pour in centrifuge tube by the ball milling product after ball milling, use normal heptane to rinse 5 times, then drying obtains magnetic powder.
The character of the magnetic powder that this comparative example obtains is in table 1.
Can be found out by contrast, do not use the particle of surfactant ball milling to have larger granularity, less coercivity and remanent magnetism, but under the same conditions, multistep stage by stage ball milling still show the magnetic property more outstanding than a step constant speed ball milling.
embodiment 3
1, the Pr after coarse crushing is taken
2fe
14b material 5g (particle size is less than 400 μm), load stainless steel jar mill, then add 100g stainless steel abrading-ball (80g of the 20g of 8mm, 5mm), and 1ml oleic acid and 1ml oleyl amine are as surfactant, finally add 100ml normal heptane as organic solvent.
2, the ball grinder that magnetic material, abrading-ball, surfactant and organic solvent are housed is sealed in glove box.The ball grinder of good seal is contained on GN-2 type high energy ball mill, ball milling 1 hour under the voltage of 30v (about 150 revs/min), ball milling 1 hour under the voltage of 40v (about 200 revs/min), ball milling 2 hours under the voltage of 50v (about 250 revs/min), then ball milling 2 hours under the voltage of 60v (about 300 revs/min).
3, take out abrading-ball, pour in centrifuge tube by the ball milling product after ball milling, use normal heptane to rinse 5 times, then drying obtains magnetic powder of the present invention.
The measurement result of the magnetic powder that the present embodiment obtains is as shown in table 1.
comparative example 4
1, the Pr after coarse crushing is taken
2fe
14b material 5g (particle size is less than 400 μm), load stainless steel jar mill, then add 100g stainless steel abrading-ball (80g of the 20g of 8mm, 5mm), and 1ml oleic acid and 1ml oleyl amine are as surfactant, finally add the normal heptane of 100ml as organic solvent.
2, the ball grinder that magnetic material, abrading-ball, surfactant and organic solvent are housed is sealed in glove box.The ball grinder of good seal is contained on GN-2 type high energy ball mill, ball milling 6 hours under the voltage of 60v (about 250 revs/min).
3, take out abrading-ball, pour in centrifuge tube by the ball milling product after ball milling, use normal heptane to rinse 5 times, then drying obtains magnetic powder.
The character of the magnetic powder that this comparative example obtains is in table 1.
Table 1
Can be found out by above embodiment and comparative example, multistep of the present invention stage by stage ball grinding method is not only applicable to Sm-Co system, and also can show coercivity for systems such as R-Fe-B increases, the features such as remanence ratio enhancing.
These are only the preferred embodiments of the present invention, be not limited to the present invention.To those skilled in the art, the present invention can have various modifications and variations, within the spirit and principles in the present invention all, and any amendment done, equivalent replacement, improvement etc., all should be included within right of the present invention.
Claims (10)
1. a preparation method for magnetic powder, the method comprises the following steps:
A the surfactant of magnetic material and abrading-ball, organic solvent and selective interpolation joins in ball grinder by ();
B () carries out ball milling after being sealed by ball grinder, wherein, the process of ball milling is the ball milling stage by stage of speed increase, at least comprises two ball milling stages, and the Ball-milling Time in each stage is 0.5 ~ 24 hour;
C () takes out abrading-ball, pour in container by ball milling product, obtains magnetic powder after rinsing drying.
2. preparation method according to claim 1, wherein, described mechanical milling process comprises at least three ball milling stages, preferably includes at least four ball milling stages.
3. preparation method according to claim 1 and 2, wherein, the Ball-milling Time in each stage is 1 ~ 20 hour, is preferably 3 ~ 15 hours.
4. preparation method according to any one of claim 1 to 3, wherein, the ball milling speed of the first stage of mechanical milling process is 1 ~ 200rpm, and the ball milling speed of second stage is 100 ~ 300rpm.
5. preparation method according to any one of claim 1 to 4, wherein, the ball milling speed of the three phases of mechanical milling process is 200 ~ 400rpm.
6. preparation method according to any one of claim 1 to 5, wherein, the ball milling speed of the last stage of mechanical milling process is for being greater than 400rpm.
7. preparation method according to any one of claim 1 to 6, wherein, described magnetic material is rare earth permanent-magnetic material or the non-rare earth permanent-magnetic material of Mn base.
8. preparation method according to any one of claim 1 to 7, wherein, described organic solvent is selected from ethanol, acetone and normal heptane; Preferably, described surfactant is cationic, anionic, nonionic surface active agent or their any combination.
9. preparation method according to any one of claim 1 to 8, wherein, described surfactant is one or more in oleic acid, oleyl amine, trioctylamine, polyvinylpyrrolidone, sad and aliphatic acid polyethenoxy ether.
10. preparation method according to any one of claim 1 to 9, wherein, the consumption of described organic solvent is 5% ~ 2000% of magnetic material mass, preferably fills it up with whole ball grinder; Preferably, the consumption of described surfactant is 15% ~ 45% of magnetic material mass.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107803505A (en) * | 2017-10-22 | 2018-03-16 | 苏州南尔材料科技有限公司 | A kind of 3d printings prepare the preparation method of Mn-Bi-Al permanent-magnet material |
| CN108831659A (en) * | 2018-09-10 | 2018-11-16 | 重庆科技学院 | It is a kind of to prepare a nanometer method and nanometer permanent magnetism powder for neodymium iron nitrogen permanent-magnet powder |
| CN110090965A (en) * | 2019-06-10 | 2019-08-06 | 重庆理工大学 | Preparation of high coercive force superfine Sm2Co17Method for producing magnetic powder |
| CN112359211A (en) * | 2020-11-16 | 2021-02-12 | 江苏集萃安泰创明先进能源材料研究院有限公司 | Method for recycling waste amorphous nanocrystalline iron core and amorphous nanocrystalline powder core |
| CN113517124A (en) * | 2021-04-22 | 2021-10-19 | 中国计量大学 | Preparation method of high-performance anisotropic rare-earth-free permanent magnet |
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| CN112359211A (en) * | 2020-11-16 | 2021-02-12 | 江苏集萃安泰创明先进能源材料研究院有限公司 | Method for recycling waste amorphous nanocrystalline iron core and amorphous nanocrystalline powder core |
| CN113517124A (en) * | 2021-04-22 | 2021-10-19 | 中国计量大学 | Preparation method of high-performance anisotropic rare-earth-free permanent magnet |
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