CN103231066B - A kind of method preparing rare earth-transition race permanent-magnet alloy micro-/ nano particle - Google Patents
A kind of method preparing rare earth-transition race permanent-magnet alloy micro-/ nano particle Download PDFInfo
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Abstract
The invention provides a kind of method preparing rare earth-transition race permanent-magnet alloy micro-/ nano particle.The method improve existing surfactant and assist ball-milling method, raw material mechanical milling process is at normal temperatures improved to ball milling at low temperatures.Be placed in low temperature environment especially by by ball grinder, make the raw material in ball grinder be in low-temperature condition; Then carry out ball milling at normal temperature environment, make raw material in mechanical milling process still be in low-temperature condition, thus ensure raw-material high fragility, make the refinement more of ball milling gained particle, to improve the generation of nano particle; Simultaneously due to the more defects of granule interior existence and larger stress in low temperature mechanical milling process, thus improve the coercivity of magnetic-particle.Experiment confirms, the method cost is low, simple, effectively improves rare earth-transition race permanent-magnet alloy nano-scale particle content, and the coercivity of micron particles, has good using value.
Description
Technical field
The invention belongs to magnetic material preparing technical field, be specifically related to a kind of method that surfactant auxiliary ball grinds standby rare earth permanent magnet micro-/ nano particle.
Background technology
Rare earth-transition race permanent-magnet alloy micro-/ nano particle, such as conventional rare-earth iron series, Rare-Earth Cobalt system, and comprise the permanent-magnet alloy micro-/ nano particle etc. of other doped chemicals, in preparation nanometer two-phase composite permanent-magnetic material of new generation, VHD magnetic recording material, ferrofluid etc., there is important investigation and application background.
At present, prepare rare earth-transition race permanent-magnet alloy particle method comprises chemical reduction method, ball-milling method etc. assisted by surfactant.But very low by the reduction potential of the known rare-earth metals of outer-shell electron characteristic distributions of rare-earth metals, reducing agent common in chemical reaction, as NaBH
4, hydrazine hydrate, polyalcohol, H
2, rare-earth metals cannot be reduced to simple substance by CO, C etc., therefore adopt chemical preparation rare earth-transition race permanent-magnet alloy particle very difficult, namely preparation is allowed to, coercivity under its room temperature is also very little, one of reason is that Co, Fe etc. easily can only be reduced to simple substance in reducing metal by reducing agent, and rare earth metal still exists in the form of the oxide.Surfactant is utilized to assist ball-milling method successfully can prepare micron order and nano level rare earth-transition race permanent-magnet alloy particle at normal temperatures, but nano-scale particle limits throughput in prepared particle, and the coercivity of micron particles is lower.
Summary of the invention
Technical purpose of the present invention is to provide a kind of method preparing rare earth-transition race permanent-magnet alloy micro-/ nano particle, in the rare earth-transition race permanent-magnet alloy particle utilizing the method to obtain, the output of nano-scale particle is higher, and the coercivity of micron particles is also higher.
In order to realize above-mentioned technical purpose, the existing method utilizing surfactant auxiliary ball to grind standby rare earth-transition race permanent-magnet alloy micro-/ nano grade particles is improved by the present inventor after long-term experiment is explored, that is: raw material mechanical milling process is at normal temperatures improved to carries out ball milling at low temperatures, this is because: at low ambient temperatures, raw material can not only suppress oxidation, and its fragility can significantly strengthen, therefore at low ambient temperatures the generation that ball milling is conducive to its nano particle is carried out to raw material; In addition, compared with normal temperature ball milling, after low temperature ball milling there is more defect and larger stress in granule interior, and the increase of defect and stress has great significance to the coercitive raising of magnetic-particle.
The technical solution adopted in the present invention is specially: a kind of method preparing rare earth-transition race permanent-magnet alloy micro-/ nano particle, the method with the bulk obtained after coarse crushing or Powdered rare earth-transition race permanent-magnet alloy for raw material, raw material are loaded in ball grinder, under surfactant and organic solvent existence condition, carry out ball milling obtain rare earth-transition race permanent-magnet alloy micro-/ nano particle, it is characterized in that: described organic solvent is low melting point organic solvent, and its melting temperature is lower than 0 DEG C; Detailed process comprises: first the ball grinder of rare earth-transition race permanent magnetic alloy powder, surfactant, organic solvent and abrading-ball will be housed at inert gas shielding lower seal, then carry out following steps (1)-(2):
(1) ball grinder is placed in low temperature environment, takes out after the melting temperature that ball grinder temperature is equal to or less than organic solvent and under normal temperature environment, to be arranged on ball mill ball milling 0.1 minute ~ 10 minutes;
(2) step (1) is repeated, until after always Ball-milling Time reaches 0.25 hour ~ 100 hours, obtain rare earth-transition race permanent-magnet alloy micro-/ nano particle, wherein micron particles is deposited in bottom ball grinder, nanoparticle suspension in organic solvent, is collected and cleans this micro-/ nano particle.
Described rare earth-transition race permanent-magnet alloy is not limit, and comprises rare-earth iron series, Rare-Earth Cobalt system permanent-magnet alloy.Wherein, rare-earth iron series permanent-magnet alloy comprises the permanent-magnet material be made up of Nd-Fe-B element and the Nd-Fe-B permanent-magnet material comprising other doped chemicals, such as 2:14:1 type Nd-Fe-B, i.e. Nd
2fe
14b etc.; Rare-Earth Cobalt system permanent-magnet alloy comprises the permanent-magnet material be made up of Sm-Co element and the Sm-Co permanent-magnet material comprising other doped chemicals, such as 1:5 type Sm-Co, i.e. SmCo
5deng.
Described organic solvent is low melting point organic solvent, and its melting temperature is lower than 0 DEG C, and as preferably, its melting temperature is between-50 DEG C ~-150 DEG C.Described organic solvent includes but not limited to alkane organic solvent, such as pentane, n-hexane, 2-methylpentane etc.The addition of described organic solvent is not limit, and preferably can infiltrate described bulk or Powdered rare earth-transition race permanent-magnet alloy, more preferably described bulk or 1 times ~ 10 times of Powdered rare earth-transition race permanent-magnet alloy quality.
Described kinds of surfactants is not limit, and the surfactant under normal temperature assists the surfactant used in ball-milling method all to can be used for the present invention, includes but not limited to oleyl amine, oleic acid, sad, octylame, polyoxyethylene laurel ether etc.The addition of described surfactant is not limit, and can realize the use amount of surface-active action, is preferably 10% ~ 300% of described raw material quality, more preferably 15% ~ 100%.
Described ball grinder material is not limit, and comprises the ball grinder etc. of stainless steel.
Described Material quality of grinding balls is not limit, and is preferably stainless steel abrading-ball etc.; Abrading-ball is preferably dimensioned to be 3mm ~ 20mm; Ball material mass ratio is not limit, and is preferably 10:1 ~ 50:1.
Described ball mill kind is not limit, preferred high energy ball mill, comprises but does not limit planetary high-energy ball mill, three-dimensional vibrating type high energy ball mill, agitating type high energy ball mill, roll type high energy ball mill etc.
Described raw material size does not have specific requirement, and in order to improve grinding efficiency, the block size after the permanent-magnet alloy coarse crushing of preferred rare earth-transition race is below millimeter magnitude, and powder size, in micron dimension, is preferably 50 μm ~ 800 μm.
In described step (1), ball grinder ball milling 1 minute ~ 8 minutes on ball mill, further preferred ball milling 2 minutes ~ 5 minutes.
In described step (2), total Ball-milling Time is preferably 0.25 hour ~ 100 hours.
In sum, ball grinder is placed in low temperature environment and carries out K cryogenic treatment by the present invention, makes the raw material in ball grinder, surfactant and low melting point organic solvent be in low-temperature condition; Take out this ball grinder when this low melting point organic solvent is in curdled appearance and carry out ball milling under normal temperature environment, K cryogenic treatment is re-started after ball milling certain hour, so repeatedly, raw material in mechanical milling process, surfactant and organic solvent is made to be in low-temperature condition, thus ensure raw-material high fragility, make particle refinement more in mechanical milling process, to improve the output of nano particle; Meanwhile, because granule interior will exist more defects and larger stress in low temperature mechanical milling process, contribute to the coercivity improving magnetic-particle.Experiment confirms, the method cost is low, simple, effectively improves the generation of rare earth-transition race permanent-magnet alloy nano-scale particle, and improves the coercivity of micron particles, is therefore a kind of method having applications well and be worth.
Accompanying drawing explanation
Fig. 1 is comparative example 1 is the Nd that 2h obtains with Ball-milling Time in embodiment 1
2fe
14b micro-/ nano particle picture;
Fig. 2 is the scanning electron microscope diagram of lower floor's particle in comparative example 1 gained ball milling product;
Fig. 3 is the transmission electron microscope figure of embodiment 1 gained ball milling product particle at the middle and upper levels;
Fig. 4 is comparative example 1 is Nd obtained after 0.5h, 1h, 2h and 4h with Ball-milling Time in embodiment 1
2fe
14the change curve of the coercivity Ball-milling Time of B micron particles;
Fig. 5 is comparative example 2 is SmCo obtained after 0.5h, 1h, 2h and 4h with Ball-milling Time in embodiment 2
5the change curve of the coercivity Ball-milling Time of micron particles.
Detailed description of the invention
Below in conjunction with accompanying drawing and embodiment, illustrate the present invention further.It should be understood that these embodiments are only for illustration of the present invention, and be not used in and limit the scope of the invention.
Comparative example 1:
The present embodiment is the comparative example of following embodiment 1.
In the present embodiment, raw material are the Powdered Nd obtained after coarse crushing
2fe
14b material, its particle size is 200 μm ~ 400 μm.Be Nd by this raw material ball milling
2fe
14the process of B permanent-magnet alloy micro-/ nano particle is as follows.
Choose three-dimensional vibrating type high energy ball mill, raw material are loaded in stainless steel jar mill, then the oleyl amine surfactant of raw material quality 50% is added, and the low melting point organic solvent 2-methylpentane of 3.5 times of raw material qualities, then add stainless steel abrading-ball that diameter is 6.5mm and 9.5mm, ratio of grinding media to material is 15:1.By be equipped with raw material, abrading-ball, surfactant, organic solvent ball grinder seal in glove box, protective gas is high-purity Ar gas, then carries out following steps:
At normal temperatures, ball grinder is installed on ball mill and carries out ball milling, take off ball grinder until ball milling successively after 0.5 hour, 1 hour, 2 hours and 4h hour, ball milling product is poured into and observes in bottle.
Embodiment 1:
In the present embodiment, raw material are identical with raw material used in above-mentioned comparative example 1.Be Nd by this raw material ball milling
2fe
14the process of B permanent-magnet alloy micro-/ nano particle is as follows.
Choose three-dimensional vibrating type high energy ball mill, raw material are loaded in stainless steel jar mill, then the oleyl amine surfactant of raw material quality 50% is added, and the low melting point organic solvent 2-methylpentane of 3.5 times of raw material qualities, then add stainless steel abrading-ball that diameter is 6.5mm and 9.5mm, ratio of grinding media to material is 15:1.By be equipped with raw material, abrading-ball, surfactant, organic solvent ball grinder seal in glove box, protective gas is high-purity Ar gas, then carries out following steps (1)-(2):
(1) ball grinder is placed in liquid nitrogen K cryogenic treatment, remains on after lower than-150 DEG C until ball grinder temperature and take out, under normal temperature environment, to be arranged on ball mill ball milling 5 minutes;
(2) repeat step (1), until total Ball-milling Time takes off ball grinder after reaching 0.5 hour, 1 hour, 2 hours and 4 hours successively, ball milling product is poured into and observes in bottle.
Observe respectively in above-mentioned comparative example 1 and embodiment 1 through ball milling after 0.5 hour, 1 hour, 2 hours and 4 hours gained ball milling product contrast.Wherein, as shown in Figure 1, right bottle is gained ball milling product in comparative example 1 to the outside drawing of the ball milling product that ball milling obtained after 2 hours, and left bottle is gained ball milling product in embodiment 1, after observing and measuring, draw following result.
(1) normal temperature ball milling and low temperature ball milling all obtain Nd
2fe
14b permanent-magnet alloy micro-/ nano particle
In left bottle and right bottle, ball milling product is the suspended particulate that levels is separated, lower floor's particle is intensive, to be deposited in bottle at the bottom of, upper strata particle suspends in organic solvent.
Take a morsel in right bottle and left bottle respectively lower floor's particulate samples and upper strata particulate samples is observed under SEM and transmission electron microscope.The observation figure of You Pingzhong lower floor particle as shown in Figure 2, can find out that the lower floor Nd-Fe-B paramagnetic particles that produces after normal temperature ball milling is micron dimension; Observation and Fig. 2 of Zuo Pingzhong lower floor particle are similar, and showing the lower floor Nd-Fe-B paramagnetic particles that produces after low temperature ball milling is micron dimension.The observation figure of Zuo Pingzhong lower floor particle as shown in Figure 3, can find out that the upper strata Nd-Fe-B paramagnetic particles that produces after low temperature ball milling is nanometer scale; Right bottle at the middle and upper levels the observation of particle and Fig. 3 similar, showing the upper strata Nd-Fe-B particle produced after normal temperature ball milling is nanometer scale.
(2) Nd that obtains of low temperature ball milling
2fe
14b permanent-magnet alloy nano particle showed increased
Contrast left bottle and right bottle, obviously can find out the nano-scale particle number showed increased that left bottle suspends at the middle and upper levels, the concentration of upper strata aaerosol solution is higher, namely after low temperature ball milling, produces more nanoparticle suspension in organic solvent; And right bottle suspended particulate is at the middle and upper levels rare, the concentration of upper strata aaerosol solution is very low, namely after normal temperature ball milling, only produces a small amount of nanoparticle suspension in organic solvent.Therefore, the nano-powder output of low temperature ball milling is apparently higher than the sample of normal temperature ball milling under same experimental conditions.
(3) Nd that obtains of low temperature ball milling
2fe
14the coercivity of B permanent-magnet alloy micron particles improves
The lower floor's micron particles sample that takes a morsel in left bottle and right bottle respectively carries out coercivity test, the method of testing adopted is be fixed on the specimen holder of vibrating specimen magnetometer by powder sample, utilize vibrating specimen magnetometer to test its demagnetizing curve, obtain coercivity value, test condition is identical.Test result as shown in Figure 4, can obviously be found out from Fig. 4, under identical Ball-milling Time, and the Nd obtained by the low temperature ball milling in embodiment 1
2fe
14the coercivity of B micron particles apparently higher than under same experimental conditions by Nd that the normal temperature ball milling in comparative example 1 obtains
2fe
14the coercivity of B micron particles.
In like manner, above-mentioned observation and test are carried out to the ball milling product that ball milling obtains after 0.5 hour, 1 hour, 4 hours, obtains result same as described above.
Comparative example 2:
The present embodiment is the comparative example of following embodiment 2.
In the present embodiment, raw material are the Powdered SmCo obtained after coarse crushing
5material, its particle size is 200 μm ~ 400 μm.Be SmCo by this raw material ball milling
5the process of permanent-magnet alloy micro-/ nano particle is as follows.
Choose three-dimensional vibrating type high energy ball mill, raw material are loaded in stainless steel jar mill, then the oleyl amine surfactant of raw material quality 50% is added, and the low melting point organic solvent 2-methylpentane of 3.5 times of raw material qualities, then add stainless steel abrading-ball that diameter is 6.5mm and 9.5mm, ratio of grinding media to material is 15:1.By be equipped with raw material, abrading-ball, surfactant, organic solvent ball grinder seal in glove box, protective gas is high-purity Ar gas, then carries out following steps:
At normal temperatures, ball grinder is installed on ball mill and carries out ball milling, take off ball grinder until ball milling successively after 1 hour, 2 hours and 4h hour, ball milling product is poured into and observes in bottle.
Embodiment 2:
In the present embodiment, raw material are identical with raw material used in above-mentioned comparative example 2.Be SmCo by this raw material ball milling
5the process of permanent-magnet alloy micro-/ nano particle is as follows.
Choose three-dimensional vibrating type high energy ball mill, raw material are loaded in stainless steel jar mill, then the oleyl amine surfactant of raw material quality 50% is added, and the organic solvent 2-methylpentane of the low melting point of 3.5 times of raw material qualities, then add stainless steel abrading-ball that diameter is 6.5mm and 9.5mm, ratio of grinding media to material is 15:1.By be equipped with raw material, abrading-ball, surfactant, organic solvent ball grinder seal in glove box, protective gas is high-purity Ar gas, then carries out following steps (1)-(2):
(1) ball grinder is placed in liquid nitrogen K cryogenic treatment, remains on after lower than-150 DEG C until ball grinder temperature and take out, under normal temperature environment, to be arranged on ball mill ball milling 5 minutes;
(2) repeat step (1), until total Ball-milling Time takes off ball grinder after reaching 1 hour, 2 hours and 4h hour successively, ball milling product is poured into and observes in bottle.
Observe respectively in above-mentioned comparative example 2 and embodiment 2 through ball milling gained ball milling product contrasting after 0.5 hour, 1 hour, 2 hours and 4 hours.Wherein, the outside drawing of the ball milling product that ball milling obtained after 2 hours is similar to Figure 1, after observing and measuring, draw following result.
(1) normal temperature ball milling and low temperature ball milling all obtain SmCo
5permanent-magnet alloy micro-/ nano particle
Similar to Figure 1, the ball milling product obtained in above-mentioned comparative example 2 and embodiment 2 is the suspended particulate that levels is separated, lower floor's particle is intensive, to be deposited in bottle at the bottom of, upper strata particle suspends in organic solvent.Through SEM and transmission electron microscope observation, lower floor SmCo
5paramagnetic particles is micron dimension; Upper strata SmCo
5paramagnetic particles is nanometer scale.
(2) SmCo that obtains of low temperature ball milling
5permanent-magnet alloy nano particle showed increased
The ball milling product obtained in comparative example 2 and embodiment 2, obtain the nano-scale particle number showed increased that embodiment 2 gained ball milling product suspends at the middle and upper levels, the concentration of upper strata aaerosol solution is higher, namely after low temperature ball milling, produces more nanoparticle suspension in organic solvent; And comparative example 2 gained ball milling product suspended particulate is at the middle and upper levels rare, the concentration of upper strata aaerosol solution is very low, namely after normal temperature ball milling, only produces a small amount of nanoparticle suspension in organic solvent.Therefore, the nano-powder output of low temperature ball milling is apparently higher than the sample of normal temperature ball milling under same experimental conditions.
(3) SmCo that obtains of low temperature ball milling
5the coercivity of permanent-magnet alloy micron particles improves
Take a morsel respectively comparative example 2 and embodiment 2 gained micron particles carries out coercivity test, the method of testing adopted is be fixed on the specimen holder of vibrating specimen magnetometer by powder sample, vibrating specimen magnetometer is utilized to test its demagnetizing curve, obtain coercivity value, test condition is identical.Test result as shown in Figure 5, can obviously be found out from Fig. 5, under identical Ball-milling Time, and the SmCo obtained by the low temperature ball milling in embodiment 2
5the coercivity of micron particles apparently higher than under same experimental conditions by SmCo that the normal temperature ball milling in comparative example 2 obtains
5the coercivity of micron particles.
In like manner, above-mentioned observation and test are carried out to the ball milling product that ball milling obtains after 0.5 hour, 1 hour, 4 hours, obtains result same as described above.
Above-described embodiment has been described in detail technical scheme of the present invention; be understood that and the foregoing is only specific embodiments of the invention; be not limited to the present invention; all make in spirit of the present invention any amendment, supplement or similar fashion substitute etc., all should be included within protection scope of the present invention.
Claims (9)
1. one kind is improved the coercitive method of rare earth-transition race permanent-magnet alloy micro-/ nano particle, with the bulk obtained after coarse crushing or Powdered rare earth-transition race permanent-magnet alloy for raw material, raw material are loaded in ball grinder, under surfactant and organic solvent existent condition, carry out ball milling obtain rare earth-transition race permanent-magnet alloy micro-/ nano particle, it is characterized in that: described organic solvent is the alkane organic solvent of low melting point, and its melting temperature is lower than 0 DEG C; Detailed process comprises: first the ball grinder of rare earth-transition race permanent magnetic alloy powder, surfactant, organic solvent and abrading-ball will be housed at inert gas shielding lower seal, then carry out following steps (1)-(2):
(1) ball grinder is placed in low temperature environment, takes out after the melting temperature that ball grinder temperature is equal to or less than organic solvent and under normal temperature environment, to be arranged on ball mill ball milling 0.1 minute ~ 10 minutes;
(2) step (1) is repeated, until after always Ball-milling Time reaches 0.25 hour ~ 100 hours, obtain rare earth-transition race permanent-magnet alloy micro-/ nano particle, wherein micron particles is deposited in bottom ball grinder, nanoparticle suspension in organic solvent, is collected and cleans this micro-/ nano particle.
2. the coercitive method of raising rare earth-transition race permanent-magnet alloy micro-/ nano particle according to claim 1, is characterized in that: described rare earth-transition race permanent-magnet alloy comprises rare-earth iron series and Rare-Earth Cobalt system permanent-magnet alloy.
3. the coercitive method of raising rare earth-transition race permanent-magnet alloy micro-/ nano particle according to claim 1, is characterized in that: the addition of described organic solvent is 1 times ~ 10 times of raw material quality.
4. the coercitive method of raising rare earth-transition race permanent-magnet alloy micro-/ nano particle according to claim 1, it is characterized in that: described surfactant comprises oleyl amine, oleic acid, one or more the mixture in sad, octylame, polyoxyethylene laurel ether.
5. the coercitive method of raising rare earth-transition race permanent-magnet alloy micro-/ nano particle according to claim 1, is characterized in that: the addition of described surfactant is 10% ~ 300% of raw material quality.
6. the coercitive method of raising rare earth-transition race permanent-magnet alloy micro-/ nano particle according to claim 1, is characterized in that: described ball mill is high energy ball mill.
7. the coercitive method of raising rare earth-transition race permanent-magnet alloy micro-/ nano particle according to claim arbitrary in claim 1 to 6, is characterized in that: the melting temperature of described organic solvent is between 0 DEG C ~-150 DEG C.
8. the coercitive method of raising rare earth-transition race permanent-magnet alloy micro-/ nano particle according to claim arbitrary in claim 1 to 6, is characterized in that: in described step (1), ball grinder ball milling 1 minute ~ 8 minutes on ball mill.
9. the coercitive method of raising rare earth-transition race permanent-magnet alloy micro-/ nano particle according to claim arbitrary in claim 1 to 6, is characterized in that: in described step (1), ball grinder ball milling 2 minutes ~ 5 minutes on ball mill.
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| CN104064345A (en) * | 2014-06-25 | 2014-09-24 | 中国科学院宁波材料技术与工程研究所 | Method for preparing rare-earth iron permanent-magnet material micro/nano-particles |
| CN106158201B (en) * | 2015-03-31 | 2018-07-24 | 中国科学院宁波材料技术与工程研究所 | Magnetic anisotropy rare-earth iron-boron permanent-magnet alloy submicron particles and preparation method thereof |
| CN105414555A (en) * | 2015-11-17 | 2016-03-23 | 中国科学院宁波材料技术与工程研究所 | Method for preparing micron/nano particles of rare earth-transition group permanent magnetic alloy |
| CN105702406B (en) * | 2016-04-06 | 2018-02-09 | 同济大学 | A kind of MnAlC bases high coercive force permanent-magnetic material and preparation method thereof |
| CN113631511B (en) * | 2019-03-06 | 2023-11-24 | 罗伯特·博世有限公司 | Magnetic refrigeration module and preparation method thereof |
| CN110090965B (en) * | 2019-06-10 | 2022-05-13 | 重庆理工大学 | Preparation of high coercive force superfine Sm2Co17Method for producing magnetic powder |
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