CN104001928B - A kind of preparation method of the rare-earth cobalt permanent magnet granule with high remanence ratio - Google Patents
A kind of preparation method of the rare-earth cobalt permanent magnet granule with high remanence ratio Download PDFInfo
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Abstract
The invention provides a kind of preparation method of the rare-earth cobalt permanent magnet granule with high remanence ratio.The method adopts low temperature wet method ball grinding technique, is less than 50 DEG C by controlling organic solvent melting temperature, and ball milling temperature is less than 0 DEG C higher than the melting temperature of organic solvent, and control ball material mass ratio is 8 in mechanical milling process:1～9.5:1, each Ball-milling Time is controlled for 1.5 minutes～5 minutes, total Ball-milling Time is controlled for 1 hour～10 hours, obtain, and the rare-earth cobalt permanent magnet granule with higher remanence ratio, therefore the combination property of rare earth cobalt alloy granule is improve, so as to expand significantly its practical application area.In addition, it is low cost of the present invention, simple to operation, have a good application prospect.
Description
Technical field
The invention belongs to magnetic material preparing technical field, and in particular to a kind of to be prepared with height using low temperature wet ball grinding
The method of the rare cobalt paramagnetic particles of remanence ratio.
Background technology
Rare-earths-cobalt, such as samarium-cobalt, praseodymium-cobalt, and the permanent-magnet alloy granule comprising other doped chemicals etc., in system
The aspects such as standby high temperature high-coercivity magnet, nanocomposite permanent magnets, high storage magnetic recording material, ferrofluid have important grinding
Study carefully and application background.
At present, preparing the method for rare cobalt permanent-magnet alloy granular materialss mainly includes chemical synthesiss, physical deposition methods,
Ball-milling method etc..Wherein, wet ball grinding method is due to low cost, easy to operate, can be mass-produced, the advantages of low for equipment requirements,
Have become it is a kind of it is important, using the most common method for preparing rare cobalt paramagnetic particles.However, due in this kind of alloy
Rare earth element (samarium, praseodymium etc.) is easily aoxidized, and causes the granular materialss permanent magnetism performance for preparing relatively low.
This seminar in the Chinese patent application of Publication No. CN103231066A discloses one kind and prepares rare earth-transition
The method of race's permanent-magnet alloy micro-/ nano granule, the method adopt low temperature ball milling, not only inhibit raw material to aoxidize, improve dilute
The yield of nano-scale particle in soil-transition group permanent-magnet alloy granule, and improve the coercivity of granule.But, the method is simultaneously
The remanence ratio of alloying pellet is not considered.
However, rare cobalt permanent-magnet alloy granule is during formation, due to being produced by the violent shock of abrading-ball high energy
The serious deformation of life, therefore destroy the crystallographic anisotropy inside granule, cause the remanence ratio of alloying pellet that obtains compared with
It is low.
The content of the invention
The technical purpose of the present invention is preparation side disclosed in the Chinese patent application for improving Publication No. CN103231066A
A kind of method, there is provided method for preparing rare cobalt paramagnetic particles, not only has using rare cobalt paramagnetic particles obtained in the method
Higher nano-scale particle content, higher coercivity, and with higher remanence ratio.
In order to realize above-mentioned technical purpose, the present inventor is had been surprisingly found that after many experiments exploration, by Publication No.
Organic solvent in preparation method disclosed in the Chinese patent application of CN103231066A is defined to melting temperature and is less than -50 DEG C
Organic solvent, and ball material mass ratio is limited in mechanical milling process as 8:1～9.5:1, each Ball-milling Time is limited to 1.5 minutes
～5 minutes, total Ball-milling Time be limited to 1 hour～10 it is little in the case of, obtained rare cobalt paramagnetic particles not only with compared with
High nano-scale particle content, higher coercivity, and with higher remanence ratio.
That is, the technical scheme is that：A kind of method of the rare cobalt paramagnetic particles for preparing high remanence ratio, the method
With block or powder rare cobalt permanent-magnet alloy as raw material, raw material is loaded in ball-grinding machine, is deposited in organic solvent
Under conditions, rare cobalt permanent-magnet alloy granule is prepared using low temperature wet ball grinding, is it is characterized in that：Described organic solvent it is molten
Less than -50 DEG C, ball milling temperature is higher than the melting temperature of organic solvent and is less than 0 DEG C point；Also, 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 limited, and the low temperature ball-grinding machine of specialty can be adopted directly to carry out low temperature ball milling,
Low temperature ball milling can be carried out using ball grinder.
The type of the low temperature ball-grinding machine of described specialty is not limited, including low temperature swing type, planetary, stirring ball mill
Deng.
When low temperature ball milling being carried out using ball grinder, ball grinder is carried out into freezing processing first, then in general milling machine
On carry out ball milling, specifically include following steps：
(1) ball grinder is placed in into low temperature environment, is taken after ball grinder temperature is equal to or less than the melting temperature of organic solvent
Go out, ball milling 1.5 minutes～5 minutes on ball mill are arranged under normal temperature environment；Described ball mill is not limited, including but not limited to
Planetary, three-dimensional vibrating formula, stirring-type, roller ball mill etc.；
(2) repeat step (1), until total Ball-milling Time is 1 hour～10 hours.
The size of described raw material does not have specific requirement, in order to improve grinding efficiency, preferably by the size control of raw material
Make below millimeter magnitude, more preferably 50 μm～800 μm.
Described rare cobalt permanent-magnet alloy mainly includes the systems such as Sm-Co, Pr-Co, Y-Co, La-Co, these bodies
Can adulterate in system other doped chemicals.The permanent-magnet alloy of these systems includes 1:5 types, 2:17 types, 1:The chemical combination such as 7 types
Thing, for example：SmCo5, PrCo5, Sm2Co17, SmCo7Deng.
Described organic solvent is not limited, for example ethanol, normal hexane, normal heptane, 2- methylpentanes etc..
The addition of described organic solvent is not limited, and is preferably able to infiltrate described raw material, more preferably described
1 times～10 times of raw material quality.
Described ball grinder material and capacity are not limited, including hardened steel and rustless steel 50ml ball grinders；Material quality of grinding balls and chi
It is very little not limit, including hardened steel 3mm-20mm abrading-balls.
Surfactant can also be included in described mechanical milling process, you can to carry out under surfactant existence condition
Described low temperature wet ball grinding.Described surfactant is not limited, including one or more in Oleic acid, oleyl amine, trioctylamine etc.
Mixing.Preferably, described low temperature wet ball grinding is carried out under surfactant existence condition.
In sum, the present invention is passed through during rare cobalt permanent-magnet alloy granule is prepared using wet ball grinding technology
Control organic solvent melting temperature is less than -50 DEG C, and control ball material mass ratio is 8 in mechanical milling process:1～9.5:1, every time
Ball-milling Time is limited to 1.5 minutes～5 minutes, and total Ball-milling Time is controlled at 1 hour～10 hours, obtains not only with higher
Nano-scale particle content, higher coercivity, and the rare cobalt paramagnetic particles with higher remanence ratio.A kind of solution of its mechanism
Releasing is：Under the conditions of the ball milling temperature, ball material mass ratio and Ball-milling Time, the ballmilling energy in mechanical milling process is defined, and is somebody's turn to do
Ball milling temperature inhibits the movement and migration of dislocation defects inside rare cobalt permanent-magnet alloy so that the rare cobalt permanent magnetism is closed
Gold grain is internally formed larger-size crystal grain and discontinuous crystal boundary, and this special microstructure is hindered to a certain extent
Rotation of the crystal grain in mechanical milling process, defines higher degree of grain alignment in material internal, so as to result in high remanence ratio.
Therefore, preparation method of the invention can take into account the particle size of rare cobalt permanent-magnet alloy granule, coercivity, with
And the performance such as remanence ratio, the rare cobalt permanent-magnet alloy granule with excellent comprehensive performance is obtained, so as to expand significantly its reality
Application.Secondly, make rare cobalt permanent-magnet alloy granule that oxidation, therefore the party to be less likely to occur using the method for low temperature ball milling
Method also helps the oxygen content reduced in alloying pellet, and the control of oxygen content has important shadow to this kind of alloy magnetic property
Ring.In addition, it is experimentally confirmed that the method low cost, simple to operation, therefore have a good application prospect.
Description of the drawings
Fig. 1 is comparative example 1 and SmCo in embodiment 15Granule remanence ratio is with the change curve of Ball-milling Time；
Fig. 2 is comparative example 3 and PrCo in embodiment 35Granule remanence ratio is with the change curve of Ball-milling Time.
Specific embodiment
Below in conjunction with the accompanying drawings with embodiment, the present invention is further elucidated.It should be understood that these embodiments are merely to illustrate
The present invention, rather than limit the scope of the present invention.
Comparative example 1:
The present embodiment is the comparative example of following embodiments 1.
In the present embodiment, it is 200 μm～400 μm powders SmCo that raw material is the granularity obtained after coarse crushing5Material
Material.The raw material is prepared as by SmCo using wet ball grinding5Granule, preparation method are as follows：
(1) three-dimensional vibrating Spex8000D type high energy ball mills are chosen, in stainless steel jar mill, then raw material is loaded
The low melting point organic solvent 2- methylpentanes of 4 times of raw material qualities are added, the rustless steel of a diameter of 6.5mm and 9.5mm is added
Abrading-ball, ratio of grinding media to material are 9：1；
(2) ball grinder that will be equipped with raw material, abrading-ball, organic solvent is sealed in Ar gas glove boxs, then by ball grinder
Be installed on ball mill, set Ball-milling Time, carry out ball milling at normal temperatures, ball grinder is removed after Ball-milling Time reaches, obtained
Ball milling product is poured in observation bottle；
Specifically preparation process is：Set respectively Ball-milling Time as 1 hour, 2 hours, 4 hours, 6 hours, 8 hours, it is 10 little
When, 12 hours, repeat the above steps (1) and (2), obtain ball milling 1 hour, 2 hours, 4 hours, 6 hours, 8 hours, 10 hours,
The ball milling product of 12 hours.
Embodiment 1：
In the present embodiment, raw material, selected ball mill, ball grinder, organic solvent and consumption, abrading-ball size and ball material
It is more identical with above-mentioned comparative example 1 than, ball grinder sealing means.Except that prepared by the method using low temperature ball milling
SmCo5Granule, preparation method are as follows：
After ball grinder sealing is intact proceed as follows to realize low temperature ball milling：
(1) it is identical with the step (1) in comparative example；
(2) raw material, abrading-ball, the ball grinder of organic solvent be will be equipped with and is placed in sub-cooled in liquid nitrogen, treat ball grinder temperature
Take out after less than -150 DEG C, ball milling 5 minutes on ball mill are arranged under normal temperature environment；
(3) Ball-milling Time is set, repeat step (2) removes ball after total Ball-milling Time reaches the Ball-milling Time of setting
Grinding jar, obtains ball milling product and pours in observation bottle；
Specifically preparation process is：Set respectively Ball-milling Time as 1 hour, 2 hours, 4 hours, 6 hours, 8 hours, it is 10 little
When, 12 hours, repeat the above steps (1) and (2), obtain ball milling 1 hour, 2 hours, 4 hours, 6 hours, 8 hours, 10 hours,
The ball milling product of 12 hours.
Ball milling product to obtaining in above-mentioned comparative example 1 and embodiment 1 is tested as follows：
(1) the ball milling Product samples obtained in above-mentioned comparative example 1 and embodiment 1 are contrasted, the ball milling product
Particle is, lower floor's granule is SmCo5Micron dimension, it is intensive, be deposited in bottom of bottle, and upper strata granule is SmCo5Nanometer amount
Level, suspend in organic solvent, in embodiment 1 the nano-particle yield of low temperature ball milling apparently higher than in comparative example 1 in phase
With the nano-particle of room temperature ball milling under experiment condition.
(2) a small amount of lower floor SmCo is taken in the ball milling product for obtaining in above-mentioned comparative example 1 and embodiment 1 respectively5It is micro-
Rice grain sample is carried out coercivity and is tested with remanence ratio, and the method for testing for being adopted is filled for powder is mixed with AB gum resin
To in polyfluortetraethylene pipe of the internal diameter for 3mm, it is orientated in magnetic field of the magnetic field intensity for 2.7T, after colloid is fully cured molding
Which is taken out from polyfluortetraethylene pipe, its hysteresis curve is tested using vibrating specimen magnetometer, obtain coercivity, remanent magnetism and satisfy
And the intensity of magnetization, test condition is identical.Test result shows as follows：
A (), under identical Ball-milling Time, the coercivity of the micron particle obtained by the low temperature ball milling in embodiment 1 is bright
The aobvious coercivity higher than the micron particle obtained by the room temperature ball milling in comparative example 1 under same experimental conditions；
B it is remanence ratio that () calculates remanent magnetism with the ratio of saturation magnetization, and the remanence ratio for obtaining is as shown in figure 1, can from Fig. 1
Will become apparent from：When total Ball-milling Time is 1 hour～10 hours, the SmCo obtained by the low temperature ball milling in embodiment 15
The remanence ratio of grain is apparently higher than the SmCo obtained by the room temperature ball milling in comparative example 1 under same experimental conditions5Granule
Remanence ratio；But, after total Ball-milling Time is more than 10 hours, the SmCo obtained by the low temperature ball milling in embodiment 15Granule
Remanence ratio decline, less than the SmCo obtained by the room temperature ball milling in comparative example 1 under same experimental conditions5Granule
Remanence ratio；
(3) oxygen content survey is carried out to the powder sample obtained in above-mentioned comparison example 1 and example 1 using oxygen-nitrogen analyzer
Examination, test result show：Under same experimental conditions and Ball-milling Time, the SmCo that low temperature ball milling is obtained5The oxygen content of granule is bright
The aobvious sample obtained less than room temperature ball milling.
Comparative example 2:
The present embodiment is the comparative example of following embodiments 2.
In the present embodiment, raw material is identical with comparative example 1.
The raw material is prepared as by SmCo using wet ball grinding5Preparation side in granule, preparation method and comparative example 1
Method is essentially identical, except that in step (1), the ratio of grinding media to material for adopting is for 8：1, in step (2), Ball-milling Time is 4 points
Clock.
Embodiment 2：
In the present embodiment, raw material is identical with comparative example 2.
The raw material is prepared as by SmCo using wet ball grinding5Preparation method base in granule, preparation method and embodiment 1
This is identical, except that in step (1), the ratio of grinding media to material for adopting is for 8：1, in step (2), Ball-milling Time is 4 minutes.
Ball milling product to obtaining in above-mentioned comparative example 2 and embodiment 2 is tested as follows：
(1) the ball milling Product samples obtained in above-mentioned comparative example 2 and embodiment 2 are contrasted, the ball milling product
Particle is, lower floor's granule is SmCo5Micron dimension, it is intensive, be deposited in bottom of bottle, and upper strata granule is SmCo5Nanometer amount
Level, suspend in organic solvent, in embodiment 2 the nano-particle yield of low temperature ball milling apparently higher than in comparative example 2 in phase
With the nano-particle of room temperature ball milling under experiment condition.
(2) a small amount of lower floor SmCo is taken in the ball milling product for obtaining in above-mentioned comparative example 2 and embodiment 2 respectively5It is micro-
Rice grain sample is carried out coercivity and is tested with remanence ratio, and the method for testing for being adopted is filled for powder is mixed with AB gum resin
To in polyfluortetraethylene pipe of the internal diameter for 3mm, it is orientated in magnetic field of the magnetic field intensity for 2.7T, after colloid is fully cured molding
Which is taken out from polyfluortetraethylene pipe, its hysteresis curve is tested using vibrating specimen magnetometer, obtain coercivity, remanent magnetism and satisfy
And the intensity of magnetization, test condition is identical.Test result shows as follows：
A (), under identical Ball-milling Time, the coercivity of the micron particle obtained by the low temperature ball milling in embodiment 2 is bright
The aobvious coercivity higher than the micron particle obtained by the room temperature ball milling in comparative example 2 under same experimental conditions；
B it is remanence ratio that () calculates remanent magnetism with the ratio of saturation magnetization, and the remanence ratio result for obtaining shows：When total ball milling
When time is -10 hours 1 hour, the SmCo obtained by the low temperature ball milling in embodiment 25The remanence ratio of granule apparently higher than
The SmCo obtained by the room temperature ball milling in comparative example 2 under same experimental conditions5The remanence ratio of granule；But, when total ball
After time consuming was more than 10 hours, the SmCo obtained by the low temperature ball milling in embodiment 25The remanence ratio of granule declines, less than
The SmCo obtained by the room temperature ball milling in comparative example 2 under same experimental conditions5The remanence ratio of granule；
(3) oxygen content survey is carried out to the powder sample obtained in above-mentioned comparison example 2 and example 2 using oxygen-nitrogen analyzer
Examination, test result shows, under same experimental conditions and Ball-milling Time, the SmCo that low temperature ball milling is obtained5The oxygen content of granule is obvious
Less than the sample obtained by room temperature ball milling.
Comparative example 3:
The present embodiment is the comparative example of following embodiments 3.
In the present embodiment, it is 200 μm～400 μm powders PrCo that raw material is the granularity obtained after coarse crushing5Material
Material.The raw material is prepared as by PrCo using wet ball grinding5Granule, preparation process are as follows：
(1) three-dimensional vibrating type high energy ball mill is chosen, raw material is loaded in hardened steel ball grinder, raw material is subsequently adding
The oleyl amine surfactant of quality 30%, and the low melting point organic solvent normal heptane of 8 times of raw material qualities, add a diameter of
The hardened steel abrading-ball of 4mm, 6.5mm and 9.5mm, ratio of grinding media to material are 8.5：1；
(2) will be equipped with raw material, abrading-ball, surfactant, organic solvent ball grinder it is close in high-purity Ar gas glove box
Envelope, is then installed to ball grinder on ball mill, sets Ball-milling Time, carries out ball milling at normal temperatures, after Ball-milling Time reaches
Ball grinder is removed, ball milling product is obtained and is poured in observation bottle；
Specifically preparation process is：Ball-milling Time is set respectively as 1.17 hours, 2 hours, 3 hours and 4 hours, in repetition
Step (1) and (2) are stated, the ball milling ball milling product of 1.17 hours, 2 hours, 3 hours and 4 hours is obtained.
Embodiment 3：
In the present embodiment, raw material, selected ball mill, ball grinder, organic solvent and consumption, surfactant and use
Amount, abrading-ball size and ratio of grinding media to material, ball grinder sealing means are identical with above-mentioned comparative example 3.Except that using low
The method of warm ball milling prepares PrCo5Granule, preparation method are as follows：
After ball grinder sealing is intact proceed as follows to realize low temperature ball milling：
(1) it is identical with the step (1) in comparative example；
(2) will be equipped with raw material, abrading-ball, the ball grinder of surfactant, organic solvent be placed in sub-cooled in liquid nitrogen,
Take out after ball grinder temperature is held below -90 DEG C, ball milling 3 minutes on ball mill are arranged under normal temperature environment；
(3) Ball-milling Time is set, repeat step (2) removes ball after total Ball-milling Time reaches the Ball-milling Time of setting
Grinding jar, the ball milling product for obtaining are poured in observation bottle；
Specifically preparation process is：Ball-milling Time is set respectively as 1.17 hours, 2 hours, 3 hours and 4 hours, in repetition
Step (1) and (2) are stated, the ball milling ball milling product of 1.17 hours, 2 hours, 3 hours and 4 hours is obtained.
Ball milling product to obtaining in above-mentioned comparative example 3 and embodiment 3 is tested as follows：
(1) the ball milling Product samples obtained in above-mentioned comparative example 3 and embodiment 3 are contrasted, the ball milling product
Particle is, lower floor's granule is PrCo5Micron dimension, it is intensive, be deposited in bottom of bottle, and upper strata granule is PrCo5Nanometer amount
Level, suspend in organic solvent, in embodiment 3 the nano-particle yield of low temperature ball milling apparently higher than in comparative example 3 in phase
With the nano-particle of room temperature ball milling under experiment condition.
(2) a small amount of lower floor PrCo is taken in the ball milling product for obtaining in above-mentioned comparative example 3 and embodiment 3 respectively5It is micro-
Rice grain sample is carried out coercivity and is tested with remanence ratio, and the method for testing for being adopted is filled for powder is mixed with AB gum resin
To in polyfluortetraethylene pipe of the internal diameter for 3mm, it is orientated in magnetic field of the magnetic field intensity for 2.7T, after colloid is fully cured molding
Which is taken out from polyfluortetraethylene pipe, its hysteresis curve is tested using vibrating specimen magnetometer, obtain coercivity value, remanent magnetism with
Saturation magnetization, test condition are identical.Test result shows as follows：
A (), under identical Ball-milling Time, the coercivity of the micron particle obtained by the low temperature ball milling in embodiment 3 is bright
The aobvious coercivity higher than the micron particle obtained by the room temperature ball milling in comparative example 3 under same experimental conditions；
B it is remanence ratio that () calculates the ratio of remanent magnetism and saturation magnetization, the remanence ratio result for obtaining as shown in Fig. 2 from
Can see in Fig. 2：The PrCo obtained by the low temperature ball milling in embodiment 35The remanence ratio of granule is apparently higher than in identical reality
The PrCo obtained by the room temperature ball milling in comparative example 3 under the conditions of testing5The remanence ratio of granule.
(3) oxygen content is carried out to the powder sample obtained in above-mentioned comparative example 3 and embodiment 3 using oxygen-nitrogen analyzer
Test, test result shows, under same experimental conditions and Ball-milling Time, the PrCo that low temperature ball milling is obtained5The oxygen content of granule is bright
The aobvious sample obtained less than room temperature ball milling.
Embodiment described above has been described in detail to technical scheme, it should be understood that the above is only
For the specific embodiment of the present invention, the present invention is not limited to, all any modifications made in the spirit of the present invention,
Supplementary or similar fashion replacement etc., should be included within the scope of the present invention.
Claims (10)
1. a kind of method for improving rare cobalt paramagnetic particles remanence ratio, with block or powder rare cobalt permanent-magnet alloy be
Raw material, by raw material load ball-grinding machine in, under organic solvent existence condition, using low temperature wet ball grinding prepare rare earth-
Co permanent magnetic alloy granule, is characterized in that：The melting temperature of described organic solvent is less than -50 DEG C, and ball milling temperature is higher than organic molten
The melting temperature of agent and be less than 0 DEG C；Also, ball material mass ratio is 8:1～9.5:1, each Ball-milling Time be limited to 1.5 minutes～
5 minutes, total Ball-milling Time was 1 hour～10 hours.
2. the method for improving rare cobalt paramagnetic particles remanence ratio as claimed in claim 1, is characterized in that：Described powder rare earth-
A diameter of 50 μm～800 μm of Co permanent magnetic alloy material.
3. the method for improving rare cobalt paramagnetic particles 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 systems.
4. the method for improving rare cobalt paramagnetic particles remanence ratio as claimed in claim 1, is characterized in that：Described is organic molten
Agent is ethanol, normal hexane, normal heptane, 2- methylpentanes.
5. the method for improving rare cobalt paramagnetic particles remanence ratio as claimed in claim 1, is characterized in that：Described is organic molten
The addition quality of agent is 1 times～10 times of described raw material quality.
6. the method for improving rare cobalt paramagnetic particles remanence ratio as claimed in claim 1, is characterized in that：In described ball milling
The material of the abrading-ball for using is hardened steel.
7. the method for the raising rare cobalt paramagnetic particles remanence ratio as described in any claim in claim 1 to 6, which is special
Levying is：Described ball-grinding machine is low temperature ball-grinding machine；
When low temperature ball milling being carried out using ball grinder, ball grinder is carried out into freezing processing first, it is then enterprising in general milling machine
Row ball milling, specifically includes following steps：
(1) ball grinder is placed in into low temperature environment, is taken out after ball grinder temperature is equal to or less than the melting temperature of organic solvent,
Ball milling 1.5 minutes～5 minutes on ball mill are arranged under normal temperature environment；Described ball mill is not limited, including but not limited to planet
Formula, three-dimensional vibrating formula, stirring-type, roller ball mill；
(2) repeat step (1), until total Ball-milling Time is 1 hour～10 hours.
8. the method for improving rare cobalt paramagnetic particles remanence ratio as claimed in claim 7, is characterized in that：Described ball grinder
Material is hardened steel, rustless steel.
9. the method for the raising rare cobalt paramagnetic particles remanence ratio as described in any claim in claim 1 to 6, which is special
Levying is：Described low temperature wet ball grinding is carried out under surfactant existence condition.
10. the method for improving rare cobalt paramagnetic particles remanence ratio as claimed in claim 9, is characterized in that：Live on described surface
Property agent is Oleic acid, oleyl amine, the mixing of one or more in trioctylamine.
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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 |
| CN104646677B (en) * | 2015-01-05 | 2017-08-01 | 中国科学院物理研究所 | A kind of 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 |
| 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 |
| 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 |
| 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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| JPS5376395A (en) * | 1976-12-17 | 1978-07-06 | Seiko Instr & Electronics Ltd | Manufacturing of rare-earth cobalt magnet |
| US6902699B2 (en) * | 2002-10-02 | 2005-06-07 | 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 |
| CN102403118B (en) * | 2011-11-23 | 2013-05-08 | 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 |
| CN103231066B (en) * | 2013-04-16 | 2015-09-30 | 中国科学院宁波材料技术与工程研究所 | A kind of method preparing rare earth-transition race permanent-magnet alloy micro-/ nano particle |
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