CN103231066A - Method for producing rare earth-transitional permanent magnet alloy micro/nanoparticles - Google Patents
Method for producing rare earth-transitional permanent magnet alloy micro/nanoparticles Download PDFInfo
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Abstract
The invention provides a method for producing rare earth-transitional permanent magnet alloy micro/nanoparticles. The method for producing the rare earth-transitional permanent magnet alloy micro/nanoparticles is an improvement of an existing surfactant-assisted ball-milling method and changes a ball-milling process of raw materials in a normal temperature into ball milling in a low temperature. Particularly, the method includes placing a ball-milling tank in the low temperature environment to enable the raw materials inside the ball-milling tank to be in a low-temperature state; then performing ball milling in a normal temperature environment and subjecting the raw materials to still being in the low-temperature state in the ball-milling process to guarantee the high brittleness of the raw materials and refine particles obtained from the ball milling, and accordingly to improve the production of nanoparticles; and simultaneously improving the coercivity of magnetic particles due to the fact that more defects and greater stresses exist inside the particles during the low-temperature ball-milling process. According to experiments, the method for producing the rare earth-transitional permanent magnet alloy micro/nanoparticles is low in costs, simple and easy to carry out, effectively improves the content of nanoparticles and the coercivity of microparticles of the rare earth-transitional permanent magnet alloy and has a good application value.
Description
Technical field
The invention belongs to the magnetic material preparing technical field, be specifically related to the method that the auxiliary ball milling of a kind of surfactant prepares rare earth permanent magnet micro-/ nano particle.
Background technology
Rare earth-transition group permanent-magnet alloy micro-/ nano particle, for example Chang Yong rare-earth iron series, Rare-Earth Cobalt are, and the permanent-magnet alloy micro-/ nano particle etc. that comprises other doped chemicals, have important research and application background at aspects such as preparation nanometer two-phase composite permanent-magnetic material of new generation, VHD magnetic recording material, ferrofluids.
At present, the method for preparing rare earth-transition group permanent-magnet alloy particle comprises chemical reduction method, the auxiliary ball-milling method of surfactant etc.But the reduction potential of rare-earth metals is very low as can be known by the outer-shell electron characteristic distributions of rare-earth metals, and common reducing agent in the chemical reaction is as NaBH
4, hydrazine hydrate, polyalcohol, H
2, CO, C etc. can't be reduced to rare-earth metals simple substance, therefore it is very difficult to adopt chemical reduction method to prepare rare earth-transition group permanent-magnet alloy particle, namely allow to preparation, coercivity under its room temperature is also very little, one of reason is that reducing agent can only easily be reduced to simple substance in the reducing metal with Co, Fe etc., and rare earth metal still exists with the form of oxide.Utilize the auxiliary ball-milling method of surfactant can successfully prepare micron order and nano level rare earth-transition group permanent-magnet alloy particle at normal temperatures, but nano-scale particle output is limited in the prepared particle, the coercivity of micron particles is lower.
Summary of the invention
Technical purpose of the present invention is to provide a kind of method for preparing rare earth-transition group permanent-magnet alloy micro-/ nano particle, utilize the output of nano-scale particle in rare earth-transition group permanent-magnet alloy particle that this method makes higher, and the coercivity of micron particles is also higher.
In order to realize above-mentioned technical purpose, after the inventor explores through long-term experiment the existing method of utilizing the auxiliary ball milling of surfactant to prepare rare earth-transition group permanent-magnet alloy micro-/ nano grade particles is improved, that is: raw material mechanical milling process at normal temperatures is improved to carries out ball milling at low temperatures, this be because: under low temperature environment, raw material not only can suppress oxidation, and the significantly enhancing of its fragility, therefore under low temperature environment, raw material are carried out the generation that ball milling is conducive to its nano particle; In addition, compare with the normal temperature ball milling, granule interior exists more defects and bigger stress behind the low temperature ball milling, and coercitive raising has great significance and the increase of defective and stress is to magnetic-particle.
The technical solution adopted in the present invention is specially: a kind of method for preparing rare earth-transition group permanent-magnet alloy micro-/ nano particle, block or Powdered rare earth-transition group permanent-magnet alloy that this method obtains after with coarse crushing is raw material, raw material are packed in the ball grinder, under surfactant and organic solvent existence condition, carry out ball milling and obtain rare earth-transition group permanent-magnet alloy micro-/ nano particle, it is characterized in that: described organic solvent is the low melting point organic solvent, and its melting temperature is lower than 0 ℃; Detailed process comprises: the ball grinder of rare earth-transition group permanent magnetic alloy powder, surfactant, organic solvent and abrading-ball at first will be housed at the inert gas shielding lower seal, and carry out following steps (1)-(2) then:
(1) ball grinder is placed low temperature environment, treat that the ball grinder temperature is equal to or less than to take out behind the melting temperature of organic solvent under normal temperature environment, to be installed on the ball mill ball milling 0.1 minute～10 minutes;
(2) repeating step (1), reach 0.25 hour～after 100 hours, obtain rare earth-transition group permanent-magnet alloy micro-/ nano particle up to total ball milling time, wherein micron particles is deposited in the ball grinder bottom, nano particle is suspended in the organic solvent, collects and clean this micro-/ nano particle.
Described rare earth-transition group permanent-magnet alloy is not limit, and comprises that rare-earth iron series, Rare-Earth Cobalt are permanent-magnet alloy.Wherein, the Nd-Fe-B permanent-magnet material that the rare-earth iron series permanent-magnet alloy comprises the permanent-magnet material that is made of the Nd-Fe-B element and comprises other doped chemicals, for example 2:14:1 type Nd-Fe-B, i.e. Nd
2Fe
14B etc.; Rare-Earth Cobalt is the Sm-Co permanent-magnet material that permanent-magnet alloy comprises the permanent-magnet material that is made of the Sm-Co element and comprises other doped chemicals, for example 1:5 type Sm-Co, i.e. SmCo
5Deng.
Described organic solvent is the low melting point organic solvent, and its melting temperature is lower than 0 ℃, and as preferably, its melting temperature is between-50 ℃～-150 ℃.Described organic solvent includes but not limited to the alkane organic solvent, for example pentane, n-hexane, 2-methylpentane etc.The addition of described organic solvent is not limit, and preferably can soak into described bulk or Powdered rare earth-transition group permanent-magnet alloy, more preferably 1 times～10 times of described bulk or Powdered rare earth-transition group permanent-magnet alloy quality.
Described kinds of surfactants is not limit, and employed surfactant all can be used for the present invention in the auxiliary ball-milling method of the surfactant under the normal temperature, 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 that the use amount of surface-active effect gets final product, and is preferably 10%～300% of described raw material quality, and more preferably 15%～100%.
Described ball grinder material is not limit, and comprises the ball grinder of stainless steel etc.
Described abrading-ball material 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, and preferred high energy ball mill comprises but do 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 preferred rare earth-transition group permanent-magnet alloy coarse crushing is below the millimeter magnitude, and powder size is preferably 50 μ m～800 μ m in micron dimension.
In the described step (1), ball grinder ball milling 1 minute～8 minutes on ball mill, further preferred ball milling 2 minutes～5 minutes.
In the described step (2), total ball milling time is preferably 0.25 hour～and 100 hours.
In sum, the present invention places low temperature environment to carry out K cryogenic treatment ball grinder, makes raw material, surfactant and low melting point organic solvent in the ball grinder be in low-temperature condition; When this low melting point organic solvent is in curdled appearance, take out this ball grinder and under normal temperature environment, carry out ball milling, treat to carry out K cryogenic treatment again behind the ball milling certain hour, so repeatedly, make raw material in the mechanical milling process, surfactant and organic solvent be in low-temperature condition, thereby guarantee raw-material high fragility, make particle refinement more in the mechanical milling process, to improve the output of nano particle; Simultaneously, because granule interior will exist more defectives and bigger stress in the low temperature mechanical milling process, help to improve the coercivity of magnetic-particle.Experiment confirm, this method cost is low, simple, has effectively improved the generation of rare earth-transition group permanent-magnet alloy nano-scale particle, and the coercivity that has improved micron particles, therefore is a kind of method that applications well is worth that has.
Description of drawings
Fig. 1 be comparative example 1 with embodiment 1 in the ball milling time be the Nd that 2h makes
2Fe
14B micro-/ nano particle picture;
Fig. 2 is the scanning electron microscope diagram of lower floor's particle in comparative example's 1 gained ball milling product;
Fig. 3 is the embodiment 1 gained ball milling product transmission electron microscope figure of particle at the middle and upper levels;
Fig. 4 be comparative example 1 with embodiment 1 in the ball milling time be the Nd that makes behind 0.5h, 1h, 2h and the 4h
2Fe
14The coercivity of B micron particles is with the change curve of ball milling time;
Fig. 5 be comparative example 2 with embodiment 2 in the ball milling time be the SmCo that makes behind 0.5h, 1h, 2h and the 4h
5The coercivity of micron particles is with the change curve of ball milling time.
The specific embodiment
Below in conjunction with accompanying drawing and embodiment, further illustrate the present invention.It should be understood that these embodiment only are used for explanation the present invention, limit the scope of the invention and be not used in.
The comparative example 1:
Present embodiment is the comparative example of following embodiment 1.
In the present embodiment, raw material are the Powdered Nd through obtaining after the coarse crushing
2Fe
14B material, its particle size are 200 μ m～400 μ m.Be Nd with 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 packed in the stainless steel jar mill, the oleyl amine surfactant that adds raw material quality 50% then, and the low melting point organic solvent 2-methylpentane of 3.5 times of raw material qualities, the stainless steel abrading-ball, the ratio of grinding media to material that add diameter again and be 6.5mm and 9.5mm are 15:1.The ball grinder that raw material, abrading-ball, surfactant, organic solvent are housed is sealed in glove box, and protective gas is high-purity Ar gas, carries out following steps then:
At normal temperatures, ball grinder is installed to carries out ball milling on the ball mill, treat that ball milling takes off ball grinder successively after 0.5 hour, 1 hour, 2 hours and 4h hour, the ball milling product is poured into observed in the bottle.
Embodiment 1:
In the present embodiment, raw material used among raw material and the above-mentioned comparative example 1 are identical.Be Nd with 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 packed in the stainless steel jar mill, the oleyl amine surfactant that adds raw material quality 50% then, and the low melting point organic solvent 2-methylpentane of 3.5 times of raw material qualities, the stainless steel abrading-ball, the ratio of grinding media to material that add diameter again and be 6.5mm and 9.5mm are 15:1.The ball grinder that raw material, abrading-ball, surfactant, organic solvent are housed is sealed in glove box, and protective gas is high-purity Ar gas, carries out following steps (1)-(2) then:
(1) ball grinder is placed the liquid nitrogen K cryogenic treatment, treat to take out after the ball grinder temperature remains below-150 ℃, under normal temperature environment, be installed on the ball mill ball milling 5 minutes;
(2) repeating step (1) takes off ball grinder successively after total ball milling time reaches 0.5 hour, 1 hour, 2 hours and 4 hours, the ball milling product is poured into observed in the bottle.
Observe respectively among above-mentioned comparative example 1 and the embodiment 1 through ball milling after 0.5 hour, 1 hour, 2 hours and 4 hours gained ball milling product compare.Wherein, the outside drawing of the ball milling product that ball milling obtained after 2 hours as shown in Figure 1, right bottle be gained ball milling product among the comparative example 1, left side bottle be gained ball milling product among the embodiment 1, through observe and measurement after 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 side bottle and the right bottle, the ball milling product is the suspended particulate that levels is separated, lower floor's particle is intensive, be deposited in bottle at the bottom of, the upper strata particle is suspended in the organic solvent.
Take a morsel in right bottle and left side bottle respectively lower floor's particulate samples and upper strata particulate samples observed under SEM and transmission electron microscope.In the right bottle observation figure of lower floor's particle as shown in Figure 2, the Nd-Fe-B of the lower floor permanent magnetism particle that produces behind the normal temperature ball milling as can be seen is micron dimension; Observation and Fig. 2 of lower floor's particle are similar in the left side bottle, and the Nd-Fe-B of lower floor permanent magnetism particle that demonstration produces behind the low temperature ball milling is micron dimension.In a left side bottle observation figure of lower floor's particle as shown in Figure 3, the upper strata Nd-Fe-B permanent magnetism particle that produces behind the low temperature ball milling as can be seen is nanometer scale; Right bottle observation and Fig. 3 of particle at the middle and upper levels is similar, and the upper strata Nd-Fe-B particle that demonstration produces behind the 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 side bottle and right bottle can obviously be found out the nano-scale particle number showed increased that left side bottle suspends at the middle and upper levels, and the concentration of upper strata aaerosol solution is higher, namely produce more nano particle and be suspended in the organic solvent behind the low temperature ball milling; And right bottle suspended particulate rareness at the middle and upper levels, the concentration of upper strata aaerosol solution is very low, namely only produces a spot of nano particle and be suspended in the organic solvent behind the normal temperature ball milling.Therefore, the sample of the nano-powder output of low temperature ball milling normal temperature ball milling under the 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 side bottle and right bottle respectively carries out the coercivity test, the method of testing that adopts is for to be fixed on powder sample on the specimen holder of vibrating specimen magnetometer, utilize vibrating specimen magnetometer to test its demagnetizing curve, obtain coercivity value, test condition is identical.Test result can obviously find out from Fig. 4 as shown in Figure 4, at identical ball milling under the time, and the Nd that obtains by the low temperature ball milling among the embodiment 1
2Fe
14The coercivity of B micron particles is apparently higher than the Nd that obtains by the normal temperature ball milling among the comparative example 1 under same experimental conditions
2Fe
14The coercivity of B micron particles.
In like manner, the ball milling product that ball milling is obtained after 0.5 hour, 1 hour, 4 hours carries out above-mentioned observation and test, obtains result same as described above.
The comparative example 2:
Present embodiment is the comparative example of following embodiment 2.
In the present embodiment, raw material are the Powdered SmCo through obtaining after the coarse crushing
5Material, its particle size are 200 μ m～400 μ m.Be SmCo with 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 packed in the stainless steel jar mill, the oleyl amine surfactant that adds raw material quality 50% then, and the low melting point organic solvent 2-methylpentane of 3.5 times of raw material qualities, the stainless steel abrading-ball, the ratio of grinding media to material that add diameter again and be 6.5mm and 9.5mm are 15:1.The ball grinder that raw material, abrading-ball, surfactant, organic solvent are housed is sealed in glove box, and protective gas is high-purity Ar gas, carries out following steps then:
At normal temperatures, ball grinder is installed to carries out ball milling on the ball mill, treat that ball milling takes off ball grinder successively after 1 hour, 2 hours and 4h hour, the ball milling product is poured into observed in the bottle.
Embodiment 2:
In the present embodiment, raw material used among raw material and the above-mentioned comparative example 2 are identical.Be SmCo with 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 packed in the stainless steel jar mill, the oleyl amine surfactant that adds raw material quality 50% then, and low-melting organic solvent 2-methylpentane of 3.5 times of raw material qualities, the stainless steel abrading-ball, the ratio of grinding media to material that add diameter again and be 6.5mm and 9.5mm are 15:1.The ball grinder that raw material, abrading-ball, surfactant, organic solvent are housed is sealed in glove box, and protective gas is high-purity Ar gas, carries out following steps (1)-(2) then:
(1) ball grinder is placed the liquid nitrogen K cryogenic treatment, treat to take out after the ball grinder temperature remains below-150 ℃, under normal temperature environment, be installed on the ball mill ball milling 5 minutes;
(2) repeating step (1) takes off ball grinder successively after total ball milling time reaches 1 hour, 2 hours and 4h hour, the ball milling product is poured into observed in the bottle.
Observe respectively among above-mentioned comparative example 2 and the embodiment 2 through ball milling gained ball milling product and comparing 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 shown in Figure 1, draws following result after observing and measuring.
(1) normal temperature ball milling and low temperature ball milling all obtain SmCo
5Permanent-magnet alloy micro-/ nano particle
Similar shown in Figure 1, the ball milling product that obtains among above-mentioned comparative example 2 and the embodiment 2 is the suspended particulate that levels is separated, lower floor's particle is intensive, be deposited in bottle at the bottom of, the upper strata particle is suspended in the organic solvent.Through SEM and transmission electron microscope observation, the SmCo of lower floor
5The permanent magnetism particle is micron dimension; Upper strata SmCo
5The permanent magnetism particle is nanometer scale.
(2) SmCo that obtains of low temperature ball milling
5Permanent-magnet alloy nano particle showed increased
The ball milling product that obtains among comparative example 2 and the embodiment 2, obtain the nano-scale particle number showed increased that embodiment 2 gained ball milling products suspend at the middle and upper levels, the concentration of upper strata aaerosol solution is higher, namely produces more nano particle and be suspended in the organic solvent behind the low temperature ball milling; And comparative example's 2 gained ball milling products suspended particulate rareness at the middle and upper levels, the concentration of upper strata aaerosol solution is very low, namely only produces a spot of nano particle and be suspended in the organic solvent behind the normal temperature ball milling.Therefore, the sample of the nano-powder output of low temperature ball milling normal temperature ball milling under the 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 carry out coercivity test, the method of testing that adopts is for to be fixed on powder sample on the specimen holder of vibrating specimen magnetometer, utilize vibrating specimen magnetometer to test its demagnetizing curve, obtain coercivity value, test condition is identical.Test result can obviously find out from Fig. 5 as shown in Figure 5, at identical ball milling under the time, and the SmCo that obtains by the low temperature ball milling among the embodiment 2
5The coercivity of micron particles is apparently higher than the SmCo that obtains by the normal temperature ball milling among the comparative example 2 under same experimental conditions
5The coercivity of micron particles.
In like manner, the ball milling product that ball milling is obtained after 0.5 hour, 1 hour, 4 hours carries out above-mentioned observation and test, obtains result same as described above.
Above-described embodiment has been described in detail technical scheme of the present invention; be understood that the above only is specific embodiments of the invention; be not limited to the present invention; all any modifications of in principle scope of the present invention, making, replenish or similar fashion substitutes etc., all should be included within protection scope of the present invention.
Claims (10)
1. method for preparing rare earth-transition group permanent-magnet alloy micro-/ nano particle, block or Powdered rare earth-transition group permanent-magnet alloy that this method obtains after with coarse crushing is raw material, raw material are packed in the ball grinder, under the condition of surfactant and organic solvent existence, carry out ball milling and obtain rare earth-transition group permanent-magnet alloy micro-/ nano particle, it is characterized in that: described organic solvent is the low melting point organic solvent, and its melting temperature is lower than 0 ℃; Detailed process comprises: the ball grinder of rare earth-transition group permanent magnetic alloy powder, surfactant, organic solvent and abrading-ball at first will be housed at the inert gas shielding lower seal, and carry out following steps (1)-(2) then:
(1) ball grinder is placed low temperature environment, treat that the ball grinder temperature is equal to or less than to take out behind the melting temperature of organic solvent under normal temperature environment, to be installed on the ball mill ball milling 0.1 minute～10 minutes;
(2) repeating step (1), reach 0.25 hour～after 100 hours, obtain rare earth-transition group permanent-magnet alloy micro-/ nano particle up to total ball milling time, wherein micron particles is deposited in the ball grinder bottom, nano particle is suspended in the organic solvent, collects and clean this micro-/ nano particle.
2. the method for preparing rare earth-transition group permanent-magnet alloy micro-/ nano particle according to claim 1, it is characterized in that: described rare earth-transition group permanent-magnet alloy comprises that rare-earth iron series and Rare-Earth Cobalt are permanent-magnet alloy.
3. the method for preparing rare earth-transition group permanent-magnet alloy micro-/ nano particle according to claim 1, it is characterized in that: described organic solvent is low-melting alkane organic solvent.
4. the method for preparing rare earth-transition group permanent-magnet alloy micro-/ nano particle according to claim 1, it is characterized in that: the addition of described organic solvent is 1 times～10 times of raw material quality.
5. the method for preparing rare earth-transition group permanent-magnet alloy micro-/ nano particle according to claim 1 is characterized in that: described surfactant package oil scraper amine, oleic acid, the mixture of one or more in sad, octylame, the polyoxyethylene laurel ether.
6. the method for preparing rare earth-transition group permanent-magnet alloy micro-/ nano particle according to claim 1, it is characterized in that: the addition of described surfactant is 10%～300% of raw material quality.
7. the method for preparing rare earth-transition group permanent-magnet alloy micro-/ nano particle according to claim 1, it is characterized in that: described ball mill is high energy ball mill.
8. according to the described method for preparing rare earth-transition group permanent-magnet alloy micro-/ nano particle of arbitrary claim in the claim 1 to 7, it is characterized in that: the melting temperature of described organic solvent is between 0 ℃～-150 ℃.
9. according to the described method for preparing rare earth-transition group permanent-magnet alloy micro-/ nano particle of arbitrary claim in the claim 1 to 7, it is characterized in that: in the described step (1), ball grinder ball milling 1 minute～8 minutes on ball mill.
10. according to the described method for preparing rare earth-transition group permanent-magnet alloy micro-/ nano particle of arbitrary claim in the claim 1 to 6, it is characterized in that: in the described step (1), ball grinder ball milling 2 minutes～5 minutes on ball mill.
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| CN106158201A (en) * | 2015-03-31 | 2016-11-23 | 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 |
| 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 |
| CN105702406A (en) * | 2016-04-06 | 2016-06-22 | 同济大学 | MnAlC-based high coercive force permanent magnetic material and preparation method thereof |
| 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 |
| WO2020177093A1 (en) * | 2019-03-06 | 2020-09-10 | 罗伯特·博世有限公司 | Magnetic refrigeration module and preparation method therefor |
| 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 |
| 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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