CN104001928A - Preparation method for rare earth and cobalt permanent magnetic particles with high remanence ratio - Google Patents
Preparation method for rare earth and cobalt permanent magnetic particles with high remanence ratio Download PDFInfo
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Abstract
The invention provides a preparation method for rare earth and cobalt permanent magnetic particles with the high remanence ratio. According to the method, the low-temperature wet type ball milling technology is adopted; the melting point temperature of organic solvents is controlled to be under minus 50 DEG C; the ball milling temperature is higher than the melting point temperature of the organic solvents and lower than 0 DEG C; in the ball milling process, the mass ratio of ball materials is controlled to be 8:1-9.5:1; the ball milling time of every time is controlled to be within 1.5 minutes to 5 minutes, and the total ball milling time is controlled to be within one hour to ten hours; finally, the rare earth and cobalt permanent magnetic particles with the high nanoscale particle content, the high coercivity and the high remanence ratio are obtained. As a result, the overall performance of the rare earth and cobalt permanent magnetic particles is improved, and the practical application area of the rare earth and cobalt permanent magnetic particles is greatly expanded. In addition, the preparation method has the advantages of being low in cost and easy and convenient to operate and having good application prospects.
Description
Technical field
The invention belongs to magnetic material preparing technical field, be specifically related to a kind of method that adopts the preparation of low temperature wet ball grinding to there is the rare cobalt permanent magnetism particle of high remanence ratio.
Background technology
Rare-earths-cobalt, for example samarium-cobalt, praseodymium-cobalt, and the permanent-magnet alloy particle that comprises other doped chemicals etc., at aspects such as preparing high temperature high-coercive force magnet, nanocomposite permanent magnets, high storage magnetic recording material, ferrofluid, there is important research and application background.
At present, the method for preparing rare cobalt permanent-magnet alloy granular materials mainly comprises chemical synthesis, physical deposition method, ball-milling method etc.Wherein, the advantage such as wet ball grinding method is due to low cost, easy to operate, can be mass-produced, low for equipment requirements, become a kind of important, use the most general method of preparing rare cobalt permanent magnetism particle.Yet, because this class alloy rare earth elements (samarium, praseodymium etc.) is very easily oxidized, cause the granular materials permanent magnetism performance of preparation lower.
A kind of method of preparing rare earth-transition group permanent-magnet alloy micro-/ nano particle is disclosed in the Chinese patent application that this seminar is CN103231066A at publication number, the method adopts low temperature ball milling, not only suppressed raw material oxidation, improve the output of nano-scale particle in rare earth-transition group permanent-magnet alloy particle, and improved the coercivity of particle.But the method is not considered the remanence ratio of alloying pellet.
Yet rare cobalt permanent-magnet alloy particle, in the process forming, produces serious distortion owing to being subject to the violent shock of abrading-ball high energy, therefore destroyed the crystallography anisotropy of granule interior, cause the remanence ratio of the alloying pellet that obtains lower.
Summary of the invention
Technical purpose of the present invention is to improve the disclosed preparation method of Chinese patent application that publication number is CN103231066A, a kind of method of preparing rare cobalt permanent magnetism particle is provided, utilize the rare cobalt permanent magnetism particle that the method makes not only to there is higher nano-scale particle content, higher coercivity, and there is higher remanence ratio.
In order to realize above-mentioned technical purpose, the inventor is unexpected discovery after great many of experiments is explored, organic solvent in the disclosed preparation method of Chinese patent application who is CN103231066A by publication number is defined as melting temperature lower than the organic solvent of-50 ℃, and in mechanical milling process, limiting ball material mass ratio is 8:1～9.5:1, each Ball-milling Time is limited to 1.5 minutes～and 5 minutes, total Ball-milling Time is limited to 1 hour～situation of 10 hours under, the rare cobalt permanent magnetism particle making not only has higher nano-scale particle content, higher coercivity, and there is higher remanence ratio.
; technical scheme of the present invention is: a kind of method of preparing the rare cobalt permanent magnetism particle of high remanence ratio; it is raw material that the method be take block or Powdered rare cobalt permanent-magnet alloy; raw material are packed in ball-grinding machine; under organic solvent existence condition; adopt low temperature wet ball grinding to prepare rare cobalt permanent-magnet alloy particle, it is characterized in that: the fusing point of described organic solvent is lower than-50 ℃, and ball milling temperature is higher than the melting temperature of organic solvent and lower than 0 ℃; And ball material mass ratio is 8:1～9.5:1, total Ball-milling Time is 1 hour～10 hours.
Described low temperature ball milling method is not limit, and can adopt professional low temperature ball-grinding machine directly to carry out low temperature ball milling, can adopt ball grinder to carry out low temperature ball milling yet.
The type of described professional low temperature ball-grinding machine is not limit, and comprises low temperature swing type, planetary, stirring ball mill etc.
When adopting ball grinder to carry out low temperature ball milling, first ball grinder is carried out to freezing processing, then on general milling machine, carry out ball milling, specifically comprise the steps:
(1) ball grinder is placed in to low temperature environment, after the melting temperature that is equal to or less than organic solvent until ball grinder temperature, takes out, under normal temperature environment, be arranged on ball mill ball milling 1.5 minutes～5 minutes; Described ball mill is not limit, and includes but not limited to planetary, three-dimensional vibrating formula, stirring-type, roller ball mill etc.;
(2) repeating step (1), until total Ball-milling Time is 1 hour～10 hours.
Described raw-material size does not have specific requirement, in order to improve grinding efficiency, preferably by raw-material size Control below millimeter magnitude, 50 μ m～800 μ m more preferably.
Described rare cobalt permanent-magnet alloy mainly comprises the systems such as Sm-Co, Pr-Co, Y-Co, La-Co, other doped chemicals of can adulterating in these systems.The permanent-magnet alloy of these systems comprises 1:5 type, 2:17 type, and the compounds such as 1:7 type, for example: SmCo
5, PrCo
5, Sm
2co
17, SmCo
7deng.
Described organic solvent is not limit, such as ethanol, n-hexane, normal heptane, 2-methylpentane etc.
The addition of described organic solvent is not limit, and preferably can infiltrate described raw material, more preferably 1 times～10 times of described raw material quality.
Described ball grinder material and capacity are not limit, and comprise hardened steel and stainless steel 50ml ball grinder; Material quality of grinding balls and size are not limit, and comprise hardened steel 3mm-20mm abrading-ball.
In described mechanical milling process, can also comprise surfactant, can under surfactant existence condition, carry out described low temperature wet ball grinding.Described surfactant is not limit, and comprises oleic acid, oleyl amine, the mixing of one or more in trioctylamine etc.As preferably, described low temperature wet ball grinding carries out under surfactant existence condition.
In sum, the present invention is utilizing wet ball grinding technology to prepare in the process of rare cobalt permanent-magnet alloy particle, by controlling organic solvent melting temperature lower than-50 ℃, and in mechanical milling process, controlling ball material mass ratio is 8:1～9.5:1, each Ball-milling Time is limited to 1.5 minutes～and 5 minutes, total Ball-milling Time is controlled at 1 hour～and 10 hours, obtained and not only there is higher nano-scale particle content, higher coercivity, and there is the rare cobalt permanent magnetism particle of higher remanence ratio.A kind of explanation of its mechanism is: under this ball milling temperature, ball material mass ratio and Ball-milling Time condition, ball milling energy in mechanical milling process is defined, and this ball milling temperature has suppressed movement and the migration of the inner dislocation defects of rare cobalt permanent-magnet alloy, make this rare cobalt permanent-magnet alloy granule interior form larger-size crystal grain and discontinuous crystal boundary, this special microstructure has hindered the rotation of crystal grain in mechanical milling process to a certain extent, at material internal, form higher degree of grain alignment, thereby caused high remanence ratio.
Therefore, preparation method of the present invention can take into account particle size, the coercivity of rare cobalt permanent-magnet alloy particle, and the performance such as remanence ratio, makes the rare cobalt permanent-magnet alloy particle with excellent comprehensive performance, thereby has greatly expanded its practical application area.Secondly, adopt the method for low temperature ball milling to make rare cobalt permanent-magnet alloy particle be not easy to be oxidized, so the method also helps the oxygen content in reduction alloying pellet, and the control of oxygen content have important impact to this class alloy magnetic property.In addition, experiment confirmation, the method cost is low, simple to operation, therefore has a good application prospect.
Accompanying drawing explanation
Fig. 1 is SmCo in comparative example 1 and embodiment 1
5particle remanence ratio is along with the change curve of Ball-milling Time;
Fig. 2 is PrCo in comparative example 3 and embodiment 3
5particle remanence ratio is along 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 for the present invention is described, limit the scope of the invention and be not used in.
Comparative example 1:
The present embodiment is the comparative example of following embodiment 1.
In the present embodiment, raw material are that the granularity obtaining after coarse crushing is the Powdered SmCo of 200 μ m～400 μ m
5material.Adopt wet ball grinding that these raw material are prepared as to SmCo
5particle, preparation method is as follows:
(1) choose three-dimensional vibrating Spex8000D type high energy ball mill, raw material are packed in stainless steel jar mill, then add the low melting point organic solvent 2-methylpentane of 4 times of raw material qualities, then to add diameter be the stainless steel abrading-ball of 6.5mm and 9.5mm, ratio of grinding media to material is 9:1;
(2) ball grinder that raw material, abrading-ball, organic solvent are housed is sealed in Ar gas glove box, then ball grinder is installed on ball mill, sets Ball-milling Time, carry out at normal temperatures ball milling, after Ball-milling Time reaches, take off ball grinder, obtain ball milling product and pour in observation bottle;
Concrete preparation process is: setting respectively Ball-milling Time is 1 hour, 2 hours, 4 hours, 6 hours, 8 hours, 10 hours, 12 hours, repeat above-mentioned steps (1) and (2), the obtain ball milling ball milling product of 1 hour, 2 hours, 4 hours, 6 hours, 8 hours, 10 hours, 12 hours.
Embodiment 1:
In the present embodiment, raw material, selected ball mill, ball grinder, organic solvent and consumption, abrading-ball size and ratio of grinding media to material, ball grinder sealing means are identical with above-mentioned comparative example 1.Difference is to adopt the method for low temperature ball milling to prepare SmCo
5particle, preparation method is as follows:
After ball grinder sealing is intact, proceed as follows to realize low temperature ball milling:
(1) identical with the step (1) in comparative example;
(2) ball grinder that raw material, abrading-ball, organic solvent are housed is placed in to liquid nitrogen sub-cooled, after ball grinder temperature is lower than-150 ℃, takes out, under normal temperature environment, be arranged on ball mill ball milling 5 minutes;
(3) set Ball-milling Time, repeating step (2), until total Ball-milling Time takes off ball grinder after reaching the Ball-milling Time of setting, obtains ball milling product and pours into and observe in bottle;
Concrete preparation process is: setting respectively Ball-milling Time is 1 hour, 2 hours, 4 hours, 6 hours, 8 hours, 10 hours, 12 hours, repeat above-mentioned steps (1) and (2), the obtain ball milling ball milling product of 1 hour, 2 hours, 4 hours, 6 hours, 8 hours, 10 hours, 12 hours.
The ball milling product obtaining in above-mentioned comparative example 1 and embodiment 1 is tested as follows:
(1) the ball milling product sample obtaining in above-mentioned comparative example 1 and embodiment 1 is contrasted, this ball milling product is suspended particulate, and lower floor's particle is SmCo
5micron dimension, intensive, be deposited in bottle at the bottom of, and upper strata particle is SmCo
5nanometer scale, is suspended in organic solvent, in embodiment 1 the nano particle output of low temperature ball milling apparently higher than in comparative example 1 under same experimental conditions the nano particle of normal temperature ball milling.
(2) SmCo of lower floor takes a morsel in the ball milling product obtaining in above-mentioned comparative example 1 and embodiment 1 respectively
5micron particles sample carries out coercivity and remanence ratio test, the method of testing adopting is for to mix powder with AB gum resin, be filled in the polyfluortetraethylene pipe that internal diameter is 3mm, in the magnetic field that is 2.7T in magnetic field intensity, be orientated, after the complete curing molding of colloid, it is taken out from polyfluortetraethylene pipe, utilize vibrating specimen magnetometer to test its hysteresis curve, obtain coercivity, remanent magnetism and saturation magnetization, test condition is identical.Test result shows below:
(a), under identical Ball-milling Time, the coercivity of the micron particles obtaining by the low temperature ball milling in embodiment 1 is apparently higher than the coercivity of the micron particles obtaining by the normal temperature ball milling in comparative example 1 under same experimental conditions;
(b) ratio of calculating remanent magnetism and saturation magnetization is remanence ratio, and the remanence ratio obtaining as shown in Figure 1, can obviously be found out from Fig. 1: when total Ball-milling Time is 1 hour～10 hours, and the SmCo obtaining by the low temperature ball milling in embodiment 1
5the remanence ratio of particle is apparently higher than the SmCo obtaining by the normal temperature ball milling in comparative example 1 under same experimental conditions
5the remanence ratio of particle; But, when total Ball-milling Time was greater than after 10 hours, the SmCo obtaining by the low temperature ball milling in embodiment 1
5the remanence ratio of particle declines, lower than the SmCo obtaining by the normal temperature ball milling in comparative example 1 under same experimental conditions
5the remanence ratio of particle;
(3) utilize oxygen-nitrogen analyzer to carry out oxygen content test to the powder sample obtaining in above-mentioned comparison example 1 and example 1, test result shows: under same experimental conditions and Ball-milling Time, and the SmCo that low temperature ball milling obtains
5the oxygen content of particle is starkly lower than the sample that normal temperature ball milling obtains.
Comparative example 2:
The present embodiment is the comparative example of following embodiment 2.
In the present embodiment, raw material are identical with comparative example 1.
Adopt wet ball grinding that these raw material are prepared as to SmCo
5particle, the preparation method in preparation method and comparative example 1 is basic identical, and difference is in step (1), and the ratio of grinding media to material of employing is 8:1, and in step (2), Ball-milling Time is 4 minutes.
Embodiment 2:
In the present embodiment, raw material are identical with comparative example 2.
Adopt wet ball grinding that these raw material are prepared as to SmCo
5particle, the preparation method in preparation method and embodiment 1 is basic identical, and difference is in step (1), and the ratio of grinding media to material of employing is 8:1, and in step (2), Ball-milling Time is 4 minutes.
The ball milling product obtaining in above-mentioned comparative example 2 and embodiment 2 is tested as follows:
(1) the ball milling product sample obtaining in above-mentioned comparative example 2 and embodiment 2 is contrasted, this ball milling product is suspended particulate, and lower floor's particle is SmCo
5micron dimension, intensive, be deposited in bottle at the bottom of, and upper strata particle is SmCo
5nanometer scale, is suspended in organic solvent, in embodiment 2 the nano particle output of low temperature ball milling apparently higher than in comparative example 2 under same experimental conditions the nano particle of normal temperature ball milling.
(2) SmCo of lower floor takes a morsel in the ball milling product obtaining in above-mentioned comparative example 2 and embodiment 2 respectively
5micron particles sample carries out coercivity and remanence ratio test, the method of testing adopting is for to mix powder with AB gum resin, be filled in the polyfluortetraethylene pipe that internal diameter is 3mm, in the magnetic field that is 2.7T in magnetic field intensity, be orientated, after the complete curing molding of colloid, it is taken out from polyfluortetraethylene pipe, utilize vibrating specimen magnetometer to test its hysteresis curve, obtain coercivity, remanent magnetism and saturation magnetization, test condition is identical.Test result shows below:
(a), under identical Ball-milling Time, the coercivity of the micron particles obtaining by the low temperature ball milling in embodiment 2 is apparently higher than the coercivity of the micron particles obtaining by the normal temperature ball milling in comparative example 2 under same experimental conditions;
(b) ratio of calculating remanent magnetism and saturation magnetization is remanence ratio, and the remanence ratio result obtaining shows: when total Ball-milling Time is 1 hour-10 hours, and the SmCo obtaining by the low temperature ball milling in embodiment 2
5the remanence ratio of particle is apparently higher than the SmCo obtaining by the normal temperature ball milling in comparative example 2 under same experimental conditions
5the remanence ratio of particle; But, when total Ball-milling Time was greater than after 10 hours, the SmCo obtaining by the low temperature ball milling in embodiment 2
5the remanence ratio of particle declines, lower than the SmCo obtaining by the normal temperature ball milling in comparative example 2 under same experimental conditions
5the remanence ratio of particle;
(3) utilize oxygen-nitrogen analyzer to carry out oxygen content test to the powder sample obtaining in above-mentioned comparison example 2 and example 2, test result demonstration, under same experimental conditions and Ball-milling Time, the SmCo that low temperature ball milling obtains
5the oxygen content of particle is starkly lower than the sample that normal temperature ball milling obtains.
Comparative example 3:
The present embodiment is the comparative example of following embodiment 3.
In the present embodiment, raw material are that the granularity obtaining after coarse crushing is the Powdered PrCo of 200 μ m～400 μ m
5material.Adopt wet ball grinding that these raw material are prepared as to PrCo
5particle, preparation process is as follows:
(1) choose three-dimensional vibrating type high energy ball mill, raw material are packed in hardened steel ball grinder, then the oleyl amine surfactant that adds raw material quality 30%, and the low melting point organic solvent normal heptane of 8 times of raw material qualities, then to add diameter be that hardened steel abrading-ball, the ratio of grinding media to material of 4mm, 6.5mm and 9.5mm is 8.5:1;
(2) ball grinder that raw material, abrading-ball, surfactant, organic solvent are housed is sealed in high-purity Ar gas glove box, then ball grinder is installed on ball mill, set Ball-milling Time, carry out at normal temperatures ball milling, after Ball-milling Time reaches, take off ball grinder, obtain ball milling product and pour in observation bottle;
Concrete preparation process is: setting respectively Ball-milling Time is 1.17 hours, 2 hours, 3 hours and 4 hours, repeats above-mentioned steps (1) and (2), the ball milling product of obtain ball milling 1.17 hours, 2 hours, 3 hours and 4 hours.
Embodiment 3:
In the present embodiment, raw material, selected ball mill, ball grinder, organic solvent and consumption, surfactant and consumption, abrading-ball size and ratio of grinding media to material, ball grinder sealing means are identical with above-mentioned comparative example 3.Difference is to adopt the method for low temperature ball milling to prepare PrCo
5particle, preparation method is as follows:
After ball grinder sealing is intact, proceed as follows to realize low temperature ball milling:
(1) identical with the step (1) in comparative example;
(2) by be equipped with raw material, abrading-ball,, the ball grinder of surfactant, organic solvent is placed in liquid nitrogen sub-cooled, after ball grinder temperature remains on lower than-90 ℃, takes out, and is arranged on ball mill ball milling 3 minutes under normal temperature environment;
(3) set Ball-milling Time, repeating step (2), until total Ball-milling Time takes off ball grinder after reaching the Ball-milling Time of setting, the ball milling product obtaining is poured into and is observed in bottle;
Concrete preparation process is: setting respectively Ball-milling Time is 1.17 hours, 2 hours, 3 hours and 4 hours, repeats above-mentioned steps (1) and (2), the ball milling product of obtain ball milling 1.17 hours, 2 hours, 3 hours and 4 hours.
The ball milling product obtaining in above-mentioned comparative example 3 and embodiment 3 is tested as follows:
(1) the ball milling product sample obtaining in above-mentioned comparative example 3 and embodiment 3 is contrasted, this ball milling product is suspended particulate, and lower floor's particle is PrCo
5micron dimension, intensive, be deposited in bottle at the bottom of, and upper strata particle is PrCo
5nanometer scale, is suspended in organic solvent, in embodiment 3 the nano particle output of low temperature ball milling apparently higher than in comparative example 3 under same experimental conditions the nano particle of normal temperature ball milling.
(2) PrCo of lower floor takes a morsel in the ball milling product obtaining in above-mentioned comparative example 3 and embodiment 3 respectively
5micron particles sample carries out coercivity and remanence ratio test, the method of testing adopting is for to mix powder with AB gum resin, be filled in the polyfluortetraethylene pipe that internal diameter is 3mm, in the magnetic field that is 2.7T in magnetic field intensity, be orientated, after the complete curing molding of colloid, it is taken out from polyfluortetraethylene pipe, utilize vibrating specimen magnetometer to test its hysteresis curve, obtain coercivity value, remanent magnetism and saturation magnetization, test condition is identical.Test result shows below:
(a), under identical Ball-milling Time, the coercivity of the micron particles obtaining by the low temperature ball milling in embodiment 3 is apparently higher than the coercivity of the micron particles obtaining by the normal temperature ball milling in comparative example 3 under same experimental conditions;
(b) ratio that calculates remanent magnetism and saturation magnetization is remanence ratio, the remanence ratio result obtaining as shown in Figure 2, as can see from Figure 2: the PrCo obtaining by the low temperature ball milling in embodiment 3
5the remanence ratio of particle is apparently higher than the PrCo obtaining by the normal temperature ball milling in comparative example 3 under same experimental conditions
5the remanence ratio of particle.
(3) utilize oxygen-nitrogen analyzer to carry out oxygen content test to the powder sample obtaining in above-mentioned comparative example 3 and embodiment 3, test result demonstration, under same experimental conditions and Ball-milling Time, the PrCo that low temperature ball milling obtains
5the oxygen content of particle is starkly lower than the sample that normal temperature ball milling obtains.
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 any modifications of making within the scope of principle of the present invention, supplement or similar fashion substitutes etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a preparation method with the rare cobalt permanent magnetism particle of high remanence ratio, block or the Powdered rare cobalt permanent-magnet alloy of take is raw material, raw material are packed in ball-grinding machine, under organic solvent existence condition, adopt low temperature wet ball grinding to prepare rare cobalt permanent-magnet alloy particle, it is characterized in that: the melting temperature of described organic solvent is lower than-50 ℃, ball milling temperature higher than the melting temperature of organic solvent lower than 0 ℃; And ball material mass ratio is 8:1～9.5:1, total Ball-milling Time is 1 hour～10 hours.
2. the preparation method with the rare cobalt permanent magnetism particle of high remanence ratio as claimed in claim 1, is characterized in that: described raw-material diameter is 50 μ m～800 μ m.
3. the preparation method with the rare cobalt permanent magnetism particle of high remanence ratio as claimed in claim 1, is characterized in that: described rare cobalt permanent-magnet alloy is Sm-Co, Pr-Co, Y-Co, or La-Co system.
4. the preparation method with the rare cobalt permanent magnetism particle of high remanence ratio as claimed in claim 1, is characterized in that: described organic solvent is ethanol, n-hexane, normal heptane, 2-methylpentane.
5. the preparation method with the rare cobalt permanent magnetism particle of high remanence ratio as claimed in claim 1, is characterized in that: the quality that adds of described organic solvent is 1 times～10 times of described raw material quality.
6. the preparation method with the rare cobalt permanent magnetism particle of high remanence ratio as claimed in claim 1, is characterized in that: described Material quality of grinding balls is hardened steel.
7. the preparation method of the rare cobalt permanent magnetism particle with high remanence ratio as described in arbitrary claim in claim 1 to 6, is characterized in that: described ball-grinding machine is low temperature ball-grinding machine, or ball grinder;
When adopting ball grinder to carry out low temperature ball milling, first ball grinder is carried out to freezing processing, then on general milling machine, carry out ball milling, specifically comprise the steps:
(1) ball grinder is placed in to low temperature environment, after the melting temperature that is equal to or less than organic solvent until ball grinder temperature, takes out, under normal temperature environment, be arranged on ball mill ball milling 1.5 minutes～5 minutes; Described ball mill is not limit, and includes but not limited to planetary, three-dimensional vibrating formula, stirring-type, roller ball mill etc.;
(2) repeating step (1), until total Ball-milling Time is 1 hour～10 hours.
8. the preparation method with the rare cobalt permanent magnetism particle of high remanence ratio as claimed in claim 7, is characterized in that: described ball grinder material is hardened steel, stainless steel.
9. the preparation method of the rare cobalt permanent magnetism particle with high remanence ratio as described in arbitrary claim in claim 1 to 6, is characterized in that: under surfactant existence condition, carry out described low temperature wet ball grinding.
10. the preparation method with the rare cobalt permanent magnetism particle of high remanence ratio as claimed in claim 9, is characterized in that: described surfactant is one or more the mixing in oleic acid, oleyl amine, trioctylamine.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104576022A (en) * | 2014-12-03 | 2015-04-29 | 中国科学院宁波材料技术与工程研究所 | Preparation method of rare earth permanent magnet |
| CN104646677A (en) * | 2015-01-05 | 2015-05-27 | 中国科学院物理研究所 | Preparation method of magnetic powder |
| 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 |
| 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 |
| CN113084180A (en) * | 2021-04-14 | 2021-07-09 | 宁波中乌新材料产业技术研究院有限公司 | Preparation method of titanium alloy spherical powder |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5376395A (en) * | 1976-12-17 | 1978-07-06 | Seiko Instr & Electronics Ltd | Manufacturing of rare-earth cobalt magnet |
| US20040065173A1 (en) * | 2002-10-02 | 2004-04-08 | The Boeing Company | Method for preparing cryomilled aluminum alloys and components extruded and forged therefrom |
| CN1555949A (en) * | 2004-01-08 | 2004-12-22 | 北京科技大学 | Method of preparing nano powderusing liquid nitrogen low temperature ball mill |
| CN102403118A (en) * | 2011-11-23 | 2012-04-04 | 北京航空航天大学 | Preparation method of anisotropic samarium cobalt-based nanocrystalline rare earth permanent magnet |
| CN102784920A (en) * | 2012-07-19 | 2012-11-21 | 河北工程大学 | Method for preparing rare earth permanent-magnet alloy nanosheet-shaped powder |
| CN103231066A (en) * | 2013-04-16 | 2013-08-07 | 中国科学院宁波材料技术与工程研究所 | Method for producing rare earth-transitional permanent magnet alloy micro/nanoparticles |
-
2014
- 2014-05-23 CN CN201410223780.6A patent/CN104001928B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5376395A (en) * | 1976-12-17 | 1978-07-06 | Seiko Instr & Electronics Ltd | Manufacturing of rare-earth cobalt magnet |
| US20040065173A1 (en) * | 2002-10-02 | 2004-04-08 | The Boeing Company | Method for preparing cryomilled aluminum alloys and components extruded and forged therefrom |
| CN1555949A (en) * | 2004-01-08 | 2004-12-22 | 北京科技大学 | Method of preparing nano powderusing liquid nitrogen low temperature ball mill |
| CN102403118A (en) * | 2011-11-23 | 2012-04-04 | 北京航空航天大学 | Preparation method of anisotropic samarium cobalt-based nanocrystalline rare earth permanent magnet |
| CN102784920A (en) * | 2012-07-19 | 2012-11-21 | 河北工程大学 | Method for preparing rare earth permanent-magnet alloy nanosheet-shaped powder |
| CN103231066A (en) * | 2013-04-16 | 2013-08-07 | 中国科学院宁波材料技术与工程研究所 | Method for producing rare earth-transitional permanent magnet alloy micro/nanoparticles |
Non-Patent Citations (2)
| Title |
|---|
| ZHANG SONGLIN ET AL.: "Sm2Fe17Nx nanoflakes prepared by surfactant assisted cryomilling", 《JOURNAL OF APPLIED PHYSICS》 * |
| ZHANG SONGLIN ET AL.: "Sm2Fe17Nx nanoflakes prepared by surfactant assisted cryomilling", 《JOURNAL OF APPLIED PHYSICS》, vol. 115, no. 17, 10 January 2014 (2014-01-10), XP012180363, DOI: doi:10.1063/1.4861204 * |
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| CN104576022B (en) * | 2014-12-03 | 2017-06-27 | 中国科学院宁波材料技术与工程研究所 | The preparation method of rare-earth permanent magnet |
| CN104646677A (en) * | 2015-01-05 | 2015-05-27 | 中国科学院物理研究所 | Preparation method of magnetic powder |
| 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 |
| 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 |
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