CN104064345A - Method for preparing rare-earth iron permanent-magnet material micro/nano-particles - Google Patents

Method for preparing rare-earth iron permanent-magnet material micro/nano-particles Download PDF

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CN104064345A
CN104064345A CN201410292448.5A CN201410292448A CN104064345A CN 104064345 A CN104064345 A CN 104064345A CN 201410292448 A CN201410292448 A CN 201410292448A CN 104064345 A CN104064345 A CN 104064345A
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ball
organic solvent
earth iron
rare
magnetic material
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张松林
张健
刘立东
杜娟
夏卫星
闫阿儒
刘平
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Ningbo Institute of Material Technology and Engineering of CAS
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Ningbo Institute of Material Technology and Engineering of CAS
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Abstract

The invention provides a method for preparing rare-earth iron permanent-magnet material micro/nano-particles. According to the method, a powdery rare-earth iron permanent-magnet material serving as a raw material is ball-milled in the presence of a surfactant and an organic solvent to obtain the rare-earth iron permanent-magnet material micro/nano-particles, wherein the melting point of the organic solvent is lower than 0 DEG C; the ball milling temperature is equal to or lower than the melting point of the organic solvent. According to the treatment method, the raw material, the surfactant and the low-melting-point organic solvent in a ball milling tank are always kept in a low-temperature state in a ball milling process, so that the energy of the raw material is low, the self-decomposition of the raw material is reduced, high brittleness of the raw material is ensured, the particles are more fined in the ball milling process, and the yield of the nano-particles is increased.

Description

The preparation method of Rare-earth Iron permanent magnetic material micro-/ nano particle
Technical field
The present invention relates to magnetic material preparing technical field, particularly relate to a kind of preparation method of Rare-earth Iron permanent magnetic material micro-/ nano particle.
Background technology
The Rare-earth Iron permanent magnetic material especially micro-/ nano particle of R-Fe-N permanent-magnet alloy has important research and application background at aspects such as preparation nanometer two-phase composite permanent-magnetic material of new generation, bonding or sintered magnet, super-high density magnetic recording material, ferrofluids.
At present, the method for preparing R-Fe-N permanent-magnet alloy particle comprises chemical reduction method, the auxiliary ball-milling method of surfactant etc.But, adopt chemical preparation R-Fe-N permanent-magnet alloy particle very difficult, allow to preparation, the coercive force under its room temperature is also very little.Utilize the auxiliary ball-milling method of surfactant can successfully prepare at normal temperatures micron order and nano level R-Fe-N permanent-magnet alloy particle, but because R-Fe-N is metastable compound, easily decompose, and utilize in the prepared particle of the auxiliary ball-milling method of surfactant nano-scale particle output limited, the coercive force of micron particles is lower.
Summary of the invention
Based on the problems referred to above, the invention provides a kind of preparation method of Rare-earth Iron permanent magnetic material micro-/ nano particle, the method can effectively reduce the decomposition of Rare-earth Iron permanent magnetic material in mechanical milling process, and in the alloying pellet making, the content of nano-scale particle is higher, and the coercive force of micron particles is higher.
For reaching above-mentioned technical purpose, the present invention adopts following technical scheme:
A kind of preparation method of Rare-earth Iron permanent magnetic material micro-/ nano particle, it is raw material that the method adopts pulverous Rare-earth Iron permanent magnetic material, under the condition of surfactant and organic solvent existence, described pulverous Rare-earth Iron permanent magnetic material is carried out to ball-milling treatment and can obtain Rare-earth Iron permanent magnetic material micro-/ nano particle;
The fusing point of wherein said organic solvent is lower than 0 ℃; The temperature of described ball-milling treatment is equal to or less than the fusing point of described organic solvent.
In an embodiment, described ball-milling treatment comprises the steps: therein
(1) described pulverous Rare-earth Iron permanent magnetic material, described surfactant, described organic solvent and abrading-ball are placed in ball grinder, under inert gas shielding, described ball grinder are sealed;
(2) the described ball grinder of good seal is arranged on ball mill, described ball mill is placed in to low temperature environment; Described in when the temperature of described ball grinder is equal to or less than the fusing point of described organic solvent, ball mill brings into operation, and while reaching default Ball-milling Time, ball mill is out of service; The temperature of described low temperature environment is equal to or less than the fusing point of described organic solvent;
(3) micron particles ball-milling treatment being obtained and nano particle are collected and are cleaned and can obtain micron particles and nano particle.
In an embodiment, described ball-milling treatment comprises the steps: therein
(1) described pulverous Rare-earth Iron permanent magnetic material, described surfactant, described organic solvent and abrading-ball are placed in ball grinder, under inert gas shielding, described ball grinder are sealed;
(2) the described ball grinder of good seal is placed in to low temperature environment, until the temperature of described ball grinder is equal to or less than after the fusing point of described organic solvent, takes out and be arranged on ball mill, the temperature of described low temperature environment is equal to or less than the fusing point of described organic solvent;
(3) make described ball mill in normal temperature environment, move 0.1 minute to 10 minutes;
(4) repeating step (2) and (3) are until total Ball-milling Time reaches default Ball-milling Time;
(5) micron particles ball-milling treatment being obtained and nano particle are collected and are cleaned and can obtain micron particles and nano particle.
In an embodiment, described Rare-earth Iron permanent magnetic material is R-Fe-N permanent-magnet alloy therein.
In an embodiment, described organic solvent is alkane organic solvent therein.
In an embodiment, the ratio of quality and the number of copies of described organic solvent and described pulverous Rare-earth Iron permanent magnetic material is 2~11:1 therein.
In an embodiment, described surfactant is oleyl amine, oleic acid therein, the mixture of one or more in sad, octylame, polyoxyethylene laurel ether.
In an embodiment, the ratio of quality and the number of copies of described surfactant and described pulverous Rare-earth Iron permanent magnetic material is 0.1~3:1 therein.
In an embodiment, the fusing point of described organic solvent is 0 ℃ to-210 ℃ therein.
In an embodiment, described default Ball-milling Time is 0.25 hour to 100 hours therein.
Compared with prior art, the invention has the advantages that: processing method of the present invention make raw material, surfactant and low melting point organic solvent in ball grinder in ball-milling treatment process all the time in low-temperature condition, thereby make raw-material energy low, reduced the decomposition of raw material self, and guaranteed that raw material have higher fragility, make particle refinement more in mechanical milling process, improved the output of nano particle.
Accompanying drawing explanation
Fig. 1 is that the granularity of the micron particles in comparative example 1 and embodiment 1 is with the change curve of Ball-milling Time;
Fig. 2 is that the Fe content of the micron particles in comparative example 1 and embodiment 1 is with the change curve of Ball-milling Time;
Fig. 3 is that the remanence ratio of the micron particles in comparative example 1 and embodiment 1 is with the change curve of Ball-milling Time.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described.It should be noted that, in the situation that not conflicting, embodiment and the feature in embodiment in the application can combine mutually.
The present invention improves the existing method of utilizing surfactant auxiliary ball to grind standby Rare-earth Iron permanent magnetic material micro-/ nano particle, is mainly that ball-milling treatment is carried out under cryogenic conditions.
The invention provides a kind of preparation method of Rare-earth Iron permanent magnetic material micro-/ nano particle, it is raw material that this preparation method adopts pulverous Rare-earth Iron permanent magnetic material, under the condition of surfactant and organic solvent existence, described pulverous Rare-earth Iron permanent magnetic material is carried out to ball-milling treatment; The fusing point of wherein said organic solvent is lower than 0 ℃; The temperature of described ball-milling treatment is equal to or less than the fusing point of described organic solvent.
Under low temperature environment, the energy of pulverous Rare-earth Iron permanent magnetic material is very low, under cryogenic conditions, carry out the decomposition that ball milling can reduce Rare-earth Iron permanent magnetic material self, and under cryogenic conditions, raw-material fragility can significantly strengthen, and under low temperature environment, raw material is carried out to ball milling and is more conducive to produce nano particle.Further, in mechanical milling process, the temperature of sample and solvent all can rise, and the fusing point that the temperature of setting ball-milling treatment is equal to or less than organic solvent can reach better cryogenic effect.
Preferably, as a kind of embodiment, described ball-milling treatment comprises the steps:
(1) described pulverous Rare-earth Iron permanent magnetic material, described surfactant, described organic solvent and abrading-ball are placed in ball grinder, under inert gas shielding, described ball grinder are sealed;
(2) the described ball grinder of good seal is arranged on ball mill, described ball mill is placed in to low temperature environment; Described in when the temperature of described ball grinder is equal to or less than the fusing point of described organic solvent, ball mill brings into operation, and while reaching default Ball-milling Time, ball mill is out of service; The temperature of described low temperature environment is equal to or less than the fusing point of described organic solvent;
(3) micron particles ball-milling treatment being obtained and nano particle are collected and are cleaned and can obtain micron particles and nano particle.After ball-milling treatment finishes, micron particles is deposited in the bottom of ball grinder, and nano particle is suspended in organic solvent, respectively micron particles and nano particle is collected and cleaned to obtain micron particles and nano particle.
Preferably, as a kind of embodiment, described ball-milling treatment comprises the steps:
(1) described pulverous Rare-earth Iron permanent magnetic material, described surfactant, described organic solvent and abrading-ball are placed in ball grinder, under inert gas shielding, described ball grinder are sealed;
(2) the described ball grinder of good seal is placed in to low temperature environment, until the temperature of described ball grinder is equal to or less than after the fusing point of described organic solvent, takes out and be arranged on ball mill, the temperature of described low temperature environment is equal to or less than the fusing point of described organic solvent;
(3) make described ball mill in normal temperature environment, move 0.1 minute to 10 minutes; Ball-milling Time in this step is preferably 1 minute to 8 minutes, is preferably 2 minutes to 5 minutes;
(4) repeating step (2) and (3) are until total Ball-milling Time reaches default Ball-milling Time;
(5) micron particles ball-milling treatment being obtained and nano particle are collected and are cleaned and can obtain micron particles and nano particle.After ball-milling treatment finishes, micron particles is deposited in the bottom of ball grinder, and nano particle is suspended in organic solvent, respectively micron particles and nano particle is collected and cleaned to obtain micron particles and nano particle.
Preferably, as a kind of embodiment, described Rare-earth Iron permanent magnetic material is R-Fe-N permanent-magnet alloy.Described R-Fe-N permanent-magnet alloy comprises R 2(Fe, M) 17n x, R 3(Fe, M) 29n xand R (Fe, M) 12n xpermanent-magnet alloy.
Preferably, as a kind of embodiment, described organic solvent is alkane organic solvent.Any one in pentane, n-hexane, 2-methylpentane for example.
Preferably, as a kind of embodiment, the addition of described organic solvent is not limit, but the addition of organic solvent preferably can infiltrate the pulverous Rare-earth Iron permanent magnetic material adding, the ratio of quality and the number of copies of preferred described organic solvent and described pulverous Rare-earth Iron permanent magnetic material is 2~11:1, and the addition of organic solvent is raw-material quality 1 times to 10 times.
Preferably, as a kind of embodiment, the kind of described surfactant is not limit, and the surfactant using in conventional auxiliary ball-milling method at present all can be used for the present invention.Activating agent in the present embodiment is preferably oleyl amine, oleic acid, the mixture of one or more in sad, octylame, polyoxyethylene laurel ether.The addition of surfactant is not limit, can realize surface-active action, the ratio of quality and the number of copies of preferred described surfactant and described pulverous Rare-earth Iron permanent magnetic material is 0.1~3:1, the quality that is surfactant is raw-material quality 10% to 300%, is preferably 15% to 100%.
Preferably, as a kind of embodiment, the fusing point of described organic solvent is 0 ℃ to-210 ℃, and preferably the fusing point of organic solvent is between-50 ℃ to-210 ℃.
Preferably, as a kind of embodiment, described default Ball-milling Time is 0.25 hour to 100 hours.
The material of ball grinder is not limit, and can adopt the ball grinder of stainless steel.
The material of the abrading-ball using in ball-milling treatment is not limit, and is preferably stainless steel abrading-ball; Abrading-ball is preferably dimensioned to be 3mm to 20mm, and ratio of grinding media to material is not limit, and is preferably 10:1 to 50:1.
The kind of ball mill is not limit, and preferred spheres grinding machine is high energy ball mill, includes but not limited to 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.
The particle diameter of pulverous Rare-earth Iron permanent magnetic material is not limit, and in order to improve grinding efficiency, preferred raw material is of a size of micron dimension, and raw-material particle diameter is preferably 10 μ m to 800 μ m.
By specific embodiment, be illustrated below.The raw material adopting in following examples is commercially available, and equipment is also commercially available.
Comparative example 1:
Raw material is pulverous Sm 2fe 17n x, its particle size is 20 μ m~40 μ m.Choose three-dimensional vibrating type high energy ball mill.By this raw material ball milling, be that the process of permanent magnetic material micro-/ nano particle is as follows:
(1) above-mentioned raw materials is packed in stainless steel jar mill, then add surfactant and organic solvent, wherein surfactant is oleic acid, the addition of oleic acid be raw material quality 30%, organic solvent is 2-methylpentane, the addition of organic solvent is 3.5 times of material quality, then to add diameter be the stainless steel abrading-ball of 6.5mm and 9.5mm, and ratio of grinding media to material is 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;
(2) at normal temperatures, ball grinder is installed to and on ball mill, carries out ball milling.
Until ball milling, after 0.5 hour, 1 hour, 2 hours and 4h hour, take off successively ball grinder, ball milling product is poured into and observed in bottle.
Embodiment 1:
In the present embodiment, surfactant and the addition thereof of raw material used, interpolation are identical with comparative example 1 with organic solvent and addition thereof.The preparation method of the present embodiment is as follows:
(1) above-mentioned raw materials is packed in stainless steel jar mill, then add surfactant and organic solvent, wherein surfactant is oleic acid, the addition of oleic acid be raw material quality 30%, organic solvent is 2-methylpentane, the addition of organic solvent is 3.5 times of material quality, then to add diameter be the stainless steel abrading-ball of 6.5mm and 9.5mm, and ratio of grinding media to material is 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;
(2) ball grinder is placed in to liquid nitrogen K cryogenic treatment, after ball grinder temperature remains on lower than-150 ℃, takes out;
(3) under normal temperature environment, be arranged on ball mill ball milling 5 minutes;
(4) repeating step (2) and (3), until total Ball-milling Time takes off ball grinder after reaching 0.5 hour, 1 hour, 2 hours and 4 hours successively, pour ball milling product to observe in bottle into.
Observe respectively in above-mentioned comparative example 1 and embodiment 1 through ball milling after 0.5 hour, 1 hour, 2 hours and 4 hours gained ball milling product contrast.After observing and measuring, draw following result.
The normal temperature ball milling of comparative example 1 and the low temperature ball milling of embodiment 1 all can obtain Sm2Fe17Nx permanent-magnet alloy micro-/ nano particle
The granularity of the micro-/ nano particle that as shown in Figure 1, the low temperature ball milling of embodiment 1 obtains is less.
Fig. 2 calculates Sm by XRD 2fe 17n xthe content balance curve chart of Fe in powder, can obviously see the Sm that the low temperature ball milling of embodiment 1 obtains 2fe 17n xin micro-/ nano particulate samples, the content of Fe is less than the sample of the normal temperature ball milling of comparative example 1, and Fe is mainly derived from, Sm in the low temperature ball grinding method of this explanation embodiment 1 2fe 17n xpermanent-magnet alloy decomposition amount is fewer than the normal temperature ball milling decomposition amount of comparative example 1.
Fig. 3 is the Sm that the normal temperature ball milling of comparative example 1 and the low temperature ball milling of embodiment 1 obtain 2fe 17n xthe correlation curve figure of the remanence ratio of permanent-magnet alloy micro-/ nano particle can obviously find out from Fig. 3, under identical Ball-milling Time, and the Sm obtaining by the low temperature ball milling in embodiment 1 2fe 17n xthe Sm that the remanence ratio of micron particles obtains apparently higher than the normal temperature ball milling in comparative example 1 under same experimental conditions 2fe 17n xthe remanence ratio of micron particles.The Sm that low temperature ball milling of the present invention obtains is described 2fe 17n xthe remanence ratio of permanent-magnet alloy micron particles is higher.
Embodiment 2:
Raw material is pulverous Sm 3fe 29n x, its particle size is 20 μ m~40 μ m.Adopt three-dimensional vibrating type high energy ball mill.The preparation method of the present embodiment is as follows:
(1) above-mentioned raw materials is packed in stainless steel jar mill, then add surfactant and organic solvent, wherein surfactant is oleyl amine, the addition of oleyl amine is 10% (mass percent) of the quality of raw material, organic solvent is pentane, the addition of organic solvent is 1 times of material quality, then to add diameter be the stainless steel abrading-ball of 3.0mm and 9.5mm, and ratio of grinding media to material is 10:1.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;
(2) ball grinder is placed in to liquid nitrogen K cryogenic treatment, until ball grinder temperature, remains on after being equal to or less than-129.8 ℃ and take out;
(3) under normal temperature environment, be arranged on ball mill ball milling 0.1 minute;
(4) repeating step (2) and (3), until total Ball-milling Time takes off ball grinder after reaching 0.25 hour, can obtain Sm 3fe 29n xmicro-/ nano particle.
Embodiment 3:
Raw material is pulverous SmFe 12n x, its particle size is 10 μ m~100 μ m.Adopt three-dimensional vibrating type high energy ball mill.The preparation method of the present embodiment is as follows:
(1) above-mentioned raw materials is packed in stainless steel jar mill, then add surfactant and organic solvent, wherein surfactant is sad, the addition of oleyl amine and raw material identical in quality, organic solvent is n-hexane, the addition of organic solvent is 5 times of material quality, then to add diameter be the stainless steel abrading-ball of 6.0mm and 9.5mm, and ratio of grinding media to material is 20:1.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;
(2) ball grinder is placed in to liquid nitrogen K cryogenic treatment, after ball grinder temperature remains on lower than-110 ℃, takes out;
(3) under normal temperature environment, be arranged on ball mill ball milling 1 minute;
(4) repeating step (2) and (3), until total Ball-milling Time takes off ball grinder while reaching 10 hours, can obtain SmFe 12n xmicro-/ nano particle.
Embodiment 4:
Raw material is pulverous Sm 2fe 17n x, its particle size is 40 μ m~100 μ m.Adopt three-dimensional vibrating type high energy ball mill.The preparation method of the present embodiment is as follows:
(1) above-mentioned raw materials is packed in stainless steel jar mill, then add surfactant and organic solvent, wherein surfactant is octylame, the addition of octylame is 10% (mass percent) of the quality of raw material, organic solvent is pentane, the addition of organic solvent is 2 times of material quality, then to add diameter be the stainless steel abrading-ball of 10mm and 20mm, and ratio of grinding media to material is 30:1.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;
(2) ball grinder is placed in to liquid nitrogen K cryogenic treatment, after ball grinder temperature remains on lower than-150 ℃, takes out;
(3) under normal temperature environment, be arranged on ball mill ball milling 2 minutes;
(4) repeating step (2) and (3), until total Ball-milling Time takes off ball grinder while reaching 50 hours, can obtain Sm 2fe 17n xmicro-/ nano particle.
Embodiment 5:
Raw material is pulverous Sm 2fe 17n x, its particle size is 40 μ m~100 μ m.Adopt three-dimensional vibrating type high energy ball mill.The preparation method of the present embodiment is as follows:
(1) above-mentioned raw materials is packed in stainless steel jar mill, then add surfactant and organic solvent, wherein surfactant is polyoxyethylene laurel ether, the addition of polyoxyethylene laurel ether is 15% (mass percent) of the quality of raw material, organic solvent is pentane, the addition of organic solvent is 10 times of material quality, then to add diameter be the stainless steel abrading-ball of 6.0mm and 9.5mm, and ratio of grinding media to material is 50:1.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;
(2) ball grinder is placed in to liquid nitrogen K cryogenic treatment, after ball grinder temperature remains on lower than-150 ℃, takes out;
(3) under normal temperature environment, be arranged on ball mill ball milling 10 minutes;
(4) repeating step (2) and (3), until total Ball-milling Time takes off ball grinder while reaching 100 hours, can obtain Sm 2fe 17n xmicro-/ nano particle.
Embodiment 6
Raw material is pulverous Sm 2fe 17n x, its particle size is 40 μ m~100 μ m.Adopt three-dimensional vibrating type high energy ball mill.The preparation method of the present embodiment is as follows:
(1) above-mentioned raw materials is packed in stainless steel jar mill, then add surfactant and organic solvent, wherein surfactant is the mixture of polyoxyethylene laurel ether and oleic acid, the addition of surfactant is 300% (mass percent) of the quality of raw material, organic solvent is pentane, the addition of organic solvent is 10 times of material quality, then to add diameter be the stainless steel abrading-ball of 6.0mm and 9.5mm, and ratio of grinding media to material is 10:1.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;
(2) ball grinder is placed in to liquid nitrogen K cryogenic treatment, after ball grinder temperature remains on lower than-150 ℃, takes out;
(3) under normal temperature environment, be arranged on ball mill ball milling 10 minutes;
(4) repeating step (2) and (3), until total Ball-milling Time takes off ball grinder while reaching 100 hours, can obtain Sm 2fe 17n xmicro-/ nano particle.
The above embodiment has only expressed several execution mode of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection range of patent of the present invention should be as the criterion with claims.

Claims (10)

1. the preparation method of a Rare-earth Iron permanent magnetic material micro-/ nano particle, it is characterized in that, adopting pulverous Rare-earth Iron permanent magnetic material is raw material, under the condition of surfactant and organic solvent existence, described pulverous Rare-earth Iron permanent magnetic material is carried out to ball-milling treatment and can obtain Rare-earth Iron permanent magnetic material micro-/ nano particle;
The fusing point of wherein said organic solvent is lower than 0 ℃; The temperature of described ball-milling treatment is equal to or less than the fusing point of described organic solvent.
2. preparation method according to claim 1, is characterized in that, described ball-milling treatment comprises the steps:
(1) described pulverous Rare-earth Iron permanent magnetic material, described surfactant, described organic solvent and abrading-ball are placed in ball grinder, under inert gas shielding, described ball grinder are sealed;
(2) the described ball grinder of good seal is arranged on ball mill, described ball mill is placed in to low temperature environment; Described in when the temperature of described ball grinder is equal to or less than the fusing point of described organic solvent, ball mill brings into operation, and while reaching default Ball-milling Time, ball mill is out of service; The temperature of described low temperature environment is equal to or less than the fusing point of described organic solvent;
(3) micron particles ball-milling treatment being obtained and nano particle are collected and are cleaned and can obtain micron particles and nano particle.
3. preparation method according to claim 1, is characterized in that, described ball-milling treatment comprises the steps:
(1) described pulverous Rare-earth Iron permanent magnetic material, described surfactant, described organic solvent and abrading-ball are placed in ball grinder, under inert gas shielding, described ball grinder are sealed;
(2) the described ball grinder of good seal is placed in to low temperature environment, until the temperature of described ball grinder is equal to or less than after the fusing point of described organic solvent, takes out and be arranged on ball mill, the temperature of described low temperature environment is equal to or less than the fusing point of described organic solvent;
(3) make described ball mill in normal temperature environment, move 0.1 minute to 10 minutes;
(4) repeating step (2) and (3) are until total Ball-milling Time reaches default Ball-milling Time;
(5) micron particles ball-milling treatment being obtained and nano particle are collected and are cleaned and can obtain micron particles and nano particle.
4. preparation method according to claim 1, is characterized in that, described Rare-earth Iron permanent magnetic material is R-Fe-N permanent-magnet alloy.
5. preparation method according to claim 1, is characterized in that, described organic solvent is alkane organic solvent.
6. preparation method according to claim 1, is characterized in that, the ratio of quality and the number of copies of described organic solvent and described pulverous Rare-earth Iron permanent magnetic material is 2~11:1.
7. preparation method according to claim 1, is characterized in that, described surfactant is oleyl amine, oleic acid, the mixture of one or more in sad, octylame, polyoxyethylene laurel ether.
8. preparation method according to claim 1, is characterized in that, the ratio of quality and the number of copies of described surfactant and described pulverous Rare-earth Iron permanent magnetic material is 0.1~3:1.
9. preparation method according to claim 1, is characterized in that, the fusing point of described organic solvent is 0 ℃ to-210 ℃.
10. according to the preparation method described in claim 2 or 3, it is characterized in that, described default Ball-milling Time is 0.25 hour to 100 hours.
CN201410292448.5A 2014-06-25 2014-06-25 Method for preparing rare-earth iron permanent-magnet material micro/nano-particles Pending CN104064345A (en)

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