CN110090965A - Preparation of high coercive force superfine Sm2Co17Method for producing magnetic powder - Google Patents
Preparation of high coercive force superfine Sm2Co17Method for producing magnetic powder Download PDFInfo
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- CN110090965A CN110090965A CN201910498251.XA CN201910498251A CN110090965A CN 110090965 A CN110090965 A CN 110090965A CN 201910498251 A CN201910498251 A CN 201910498251A CN 110090965 A CN110090965 A CN 110090965A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/0551—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 in the form of particles, e.g. rapid quenched powders or ribbon flakes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/042—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling using a particular milling fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Abstract
The invention discloses a method for preparing high coercive force superfine Sm2Co17The method for producing the magnetic powder comprises the following steps: crushing a 2:17 SmCo magnet into magnetic particles; step two, putting the magnetic particles obtained in the step one into a low-energy ball milling tank, adding grinding balls, a solvent and a surfactant, and then placing the ball milling tank in a low-temperature environment for low-energy ball milling; step three, after the low-energy ball milling in the step two, transferring the content in the ball milling tank into a high-energy ball milling tank, carrying out high-energy ball milling in a low-temperature environment, and taking out the magnet powder after the ball milling is finished to obtain the superfine Sm powder2Co17Magnetic powder; the low-temperature environment is-130 to-20 ℃; the melting point of the solvent is lower than the temperature of the low-temperature environment. Compared with the normal-temperature two-step ball milling technology, the superfine magnetic powder prepared by the method of the invention keeps the integrity of a unit cell structure better and has higher coercive force.
Description
Technical field
The invention belongs to magnetic Nano material fields, and in particular to a kind of to prepare the ultra-fine Sm of high-coercive force2Co17The side of magnetic powder
Method.
Background technique
Rare earth permanent magnet has outstanding magnetic property, and industrial application is extensive, the SmCo including SmCo class5And Sm2Co17, and
The Nd of NdFeB class2Fe14B.Wherein, Sm2Co17Permanent magnetism is second generation rare earth permanent magnet, has excellent comprehensive magnetic energy, especially
With good high-temperature stability, it is used widely in fields such as aerospace, defence and military equipments.However, to permanent magnetism material
The performance requirement of material is also constantly being promoted, improved by changing the structure of material the performance study of rare earth permanent-magnetic material still into
In row.Rare earth permanent magnet nano particle in nanometer due to answering with high magnetocrystalline anisotropy, controllable partial size and excellent magnetism
There are huge potentiality in terms of closing magnetic material and biomedical applications.In recent years, the preparation of this kind of permanent magnetism nano particle causes
Extensive concern, such as SmCo class, NdFeB type nano granular.Common preparation method includes mechanochemistry processing, chemistry conjunction
At, surfactant auxiliary high-energy ball milling etc..Wherein, surfactant auxiliary high-energy ball milling is to obtain hard magnetic SmCo nanometers
A kind of effective technology of grain.
Currently, can get the nanometer SmCo of higher coercivity using the high-energy ball milling that surfactant assists5And
Nd2Fe14B paramagnetic particles.Chinese patent CN201310133182.5, which is disclosed, a kind of prepares rare earth-mistake using low temperature ball grinding method
The method for crossing race's permanent-magnet alloy micro-/ nano particle, first that raw material are cooling, then the ball milling under normal temperature environment, repeats to cool down
And mechanical milling process, Nd is prepared still in low temperature in material in mechanical milling process2Fe14B permanent magnetism micro-nano granules, experiment show
Cryogenic conditions improve Nd obtained2Fe14The yield of nano particle in B permanent magnetism micro-nano granules.Chinese patent
CN201510003975.4 discloses a kind of ball grinding method of multistage friction speed, compared with SmCo made from single speed ball grinding method5
And Pr2Fe14B magnetic flake particle texture degree is stronger, crystal structure is more complete, and wherein the thickness of sheet-like particle arrives several tens
Hundred nanometers.
However, being difficult to obtain high-coercive force Sm using the above method2Co17Superfine nano particle.This is because different materials
Coercivity mechanism it is different.Though for example, belonging to SmCo class magnet, SmCo5Coercivity with granularity reduce and increase, as long as
Keep SmCo5The integrality of phase structure, can be obtained high-coercive force, and Sm2Co17It is then different.For 2:17 type SmCo permanent magnet,
In order to improve coercivity and remanent magnetism, the elements such as Cu, Zr and Fe are usually added, alloy system is complicated.In addition, the alloy is micro-
It is made of on seeing cell structure and laminated structure mixing, the coercivity of alloy is strongly depend on the structural integrity of this cellular structure
Property.Work as Sm2Co17After broken, as granularity is gradually reduced, this cellular structure is also destroyed, and coercivity declines to a great extent.Such as
What prepares the Sm of high-coercive force using high energy ball mill method2Co17Superfine nano magnetic powder still faces larger challenge.
Summary of the invention
In view of this, preparing the ultra-fine Sm of high-coercive force one of the objects of the present invention is to provide a kind of2Co17The side of magnetic powder
Method.
Its technical solution is as follows:
It is a kind of to prepare the ultra-fine Sm of high-coercive force2Co17The method of magnetic powder, key are to sequentially include the following steps:
2:17 type SmCo magnet is broken for magnetic particle by step 1；
Step 2, the magnetic particle that step 1 is obtained is put into low energy ball grinder, and abrading-ball, solvent and surface is added
Then ball grinder is placed in progress low energy ball milling under low temperature environment by activating agent；
Content in the low energy ball grinder is transferred to high-energy ball milling in the step 2 after low energy ball milling by step 3
In tank, high-energy ball milling is carried out under low temperature environment, and magnet powder is taken out after the completion of ball milling to get ultra-fine Sm2Co17Magnetic powder；
The low temperature environment temperature is -130--20 DEG C；
The fusing point of the solvent is lower than the temperature of the low temperature environment.
As optimal technical scheme, in above-mentioned steps two, the revolving speed of the low energy ball milling is 150-300r/min；
In the step 3, the revolving speed of the high-energy ball milling is 450-800r/min.
As optimal technical scheme, in above-mentioned steps two, the time of the low energy ball milling is 15-25h.
As optimal technical scheme, in above-mentioned steps three, the time of the high-energy ball milling is 20-40h.
As optimal technical scheme, in above-mentioned steps two and step 3, by weight, the abrading-ball and the magnetic particle or
The ratio of grinding media to material of magnet powder is 10:1.
As optimal technical scheme, in above-mentioned steps two, the low energy ball grinder is placed in incubation chamber, to the incubation chamber
Middle injection liquid nitrogen to the low energy ball grinder is partially submerged, so that the low energy ball grinder keeps low temperature.
As optimal technical scheme, above-mentioned solvent is isohexane.
As optimal technical scheme, the weight ratio of above-mentioned surfactant and the magnetic particle is 3-5:10.
As optimal technical scheme, above-mentioned surfactant is oleic acid.
As optimal technical scheme, in above-mentioned steps one, the SmCo magnet is broken for the magnetic particle of 100-200 mesh.
Detailed description of the invention
Fig. 1 is the demagnetizing curve of magnetic powder prepared by the method for embodiment 2；
Fig. 2 is the XRD spectrum of low temperature low energy ball milling 20h (2a) and low temperature high-energy ball milling 40h (2b) magnetic powder in embodiment 2；
Fig. 3 is low temperature low energy ball milling 20h (3a), low temperature high-energy ball milling 20h (3b) and low temperature high-energy ball milling in embodiment 2
The SEM of magnetic powder after 40h (3c) schemes；
Fig. 4 is the magnetic powder demagnetizing curve of magnetic powder made from reference examples 1；
Fig. 5 is the XRD spectrum of magnetic powder after high-energy ball milling 5h in reference examples 1.
Specific embodiment
The invention will be further described with attached drawing with reference to embodiments.
(1) preparation of magnetic powder
Embodiment 1
Taking ingredient is Sm (CobalFe0.07Cu0.088Zr0.025)7.5Samarium-cobalt alloy, by the alloy breaks down be 200 mesh powder.
It weighs broken powder 10g to be put into low energy ball grinder, while being put into 100g abrading-ball, 30ml isohexane and 3g oleic acid is added,
Low energy ball grinder is sealed.The low energy ball grinder is equipped with shaft, which is connected on the output shaft of rotary mill.Specifically
Ground, rotary mill output shaft stretch out its shell, then connect again with shaft.Incubation chamber is arranged outside low energy ball grinder simultaneously.
After ball milling 5h, liquid nitrogen is injected into incubation chamber, and partially submerged ball grinder, after stablizing, environment temperature in incubation chamber is measured and is maintained at
About -126 DEG C.After the revolving speed ball milling 15h of 200r/min, ball grinder temperature is waited to be warmed to room temperature, takes out powder, liquid and mill
Ball is put into high-energy ball milling tank.Using planetary high-energy ball mill, high-energy ball milling, while ring are carried out with the revolving speed of 450r/min
Border temperature is maintained at -20 DEG C.After ball milling 40h, powder is taken out.
Embodiment 2
Taking ingredient is Sm (CobalFe0.1Cu0.08Zr0.03)8.3Samarium-cobalt alloy, by the alloy breaks down be 100 mesh powder.Claim
It takes broken powder 10g to be put into low energy ball grinder, while being put into 100g abrading-ball, 30ml isohexane and 3g oleic acid is added.It will
Low energy ball grinder is sealed, and the mounting means with rotary mill is placed in incubation chamber with embodiment 1.Liquid nitrogen is infused
Enter incubation chamber, and partially submerged ball grinder, measures environment temperature in incubation chamber and be maintained at about -130 DEG C.After ball milling 20h, to ball milling
Tank temperature degree is warmed to room temperature, and takes out powder, liquid and abrading-ball, is put into progress low temperature high-energy ball milling in high-energy ball milling tank.Revolving speed 600r/
Min, while environment temperature is maintained at -60 DEG C.After high-energy ball milling 20h, taking-up powder keeps sample to be detected；After ball milling 40h, powder is taken out
End detection.
Reference examples 1
Taking ingredient is Sm (CobalFe0.1Cu0.08Zr0.03)8.3Samarium-cobalt alloy, by alloy breaks down be 100 mesh powder.It takes brokenly
Powder 10g after broken is put into ball grinder, while being put into 100g abrading-ball, 30ml isohexane.Ball grinder is sealed, high energy is put into
Room temperature high-energy ball milling, revolving speed 600r/min are carried out in ball grinder.After ball milling 1h and 5h, taking-up powder keeps sample to be detected respectively.
Reference examples 2
Taking ingredient is Sm (CobalFe0.1Cu0.08Zr0.03)8.3Samarium-cobalt alloy, by alloy breaks down be 100 mesh powder.It takes brokenly
Powder 10g after broken is put into ball grinder, while 100g abrading-ball, 30ml normal heptane, 3g oleic acid is added.Ball grinder is sealed,
It is put into rotary mill, with the revolving speed ball milling of 200r/min.After ball milling 20h, powder, liquid and abrading-ball are taken out, high energy is put into
High-energy ball milling is carried out in ball grinder.After the revolving speed ball milling 40h of 600r/min, powder detection is taken out.
Reference examples 3
Taking ingredient is Sm (CobalFe0.1Cu0.08Zr0.03)8.3Samarium-cobalt alloy, by alloy breaks down be 100 mesh powder.It takes brokenly
Powder 5g after broken is put into ball grinder, while 50g abrading-ball, 20ml isohexane, 1.5g oleic acid is added.Ball grinder is sealed,
It is put into progress low temperature high-energy ball milling in high-energy ball milling tank.With the revolving speed ball milling of 600r/min, while environment temperature is maintained at -60
DEG C, after ball milling 50h, take out powder.
(2) performance detection of magnetic powder
Powder prepared by Example 2, reference examples 1 and reference examples 2 respectively tests its demagnetizing curve and determines coercivity,
According to magnetic property as a result, characterizing its crystal structure using X-ray diffraction analysis method (XRD), it is imaged using scanning electron microscopy
(SEM) morphology microstructure is observed.
Fig. 1 is the demagnetizing curve of magnetic powder made from embodiment 2.Initial breaking apart powder coercivity is close to 20kOe, when low temperature is low
After energy ball milling 20h, magnetic powder coercivity is about 16kOe；In conjunction with Fig. 2 (a) it is found that magnetic powder is still by Sm at this time2Co17Phase composition, by Fig. 3
(a) it is found that granular size is about 1-2 μm at this time.After high-energy ball milling 20h, magnetic powder coercivity is about 13KOe, is known by Fig. 3 (b)
Granular size is about 300-500nm at this time；After high-energy ball milling 40h, magnetic powder coercivity is about 9.9kOe, the magnetic known to Fig. 2 (b)
Powder main phase is still Sm2Co17, know that granular size is about 100nm by Fig. 3 (c).
Fig. 4 is the magnetic powder demagnetizing curve of magnetic powder made from reference examples 1.After high-energy ball milling 1h, powder coercivity is reduced to
About 6kOe.After high-energy ball milling 5h, powder coercivity is about 3kOe, at this point, by the XRD spectrum of Fig. 5 it is found that the hard magnetic phase of powder
Sm2Co17It disappears substantially, powder is decrystallized.
In reference examples 2, magnetic powder obtained after high-energy ball milling 40h, measuring its coercivity is 7.8kOe.In reference examples 3, low temperature
After high-energy ball milling 50h, powder size is close with embodiment 2 and reference examples 2 at 0.3 μm, but powder coercivity only has at this time
5.6kOe.As shown in table 1.
Magnetic powder coercivity changes after 1 room temperature of table and low temperature ball milling
Powder made from comparing embodiment 2 and reference examples 2, although all through two step ball milling system of low energy ball milling and high-energy ball milling
It is standby, but coercivity of the coercivity less than low temperature high-energy ball milling sample of sample is made in room temperature ball milling.Comparing embodiment 2 and reference examples
Powder made from 3, although all using low temperature ball grinding method, and in powder size made from one step ball milling of low temperature high energy and example 1
Powder size is almost the same, but powder coercivity is far below powder made from embodiment 2 at this time.
The generation for speculating the phenomenon is the result of low temperature and two step ball-milling technologies synergistic effect.Firstly, magnetic under low-temperature condition
Particulate brittleness is stronger, is easier to that brittle crush occurs, and grain structure destruction is less；Secondly, in mechanical milling process, surfactant
Play an important role, when preparing magnetic powder only with low temperature high-energy ball milling, surfactant possibly can not in conjunction with dispersed-powder,
Magnetic powder grain structure integrality in mechanical milling process is caused to go to pot, so that coercivity be made to reduce.
The utility model has the advantages that the present invention creates low temperature environment using 2:17 type SmCo as raw material, using liquid nitrogen, using surfactant
The two step method ball grinding technique that the low energy ball milling and high-energy ball milling of auxiliary combine, successfully be made partial size down to 100nm ultra-fine magnetic
Powder.Compared with room temperature two-step method ball grinding technique or low temperature ball grinding technique, super-fine magnetic powder made from method of the invention is preferably
The integrality of cell configuration is maintained, product coercivity is higher.
Finally, it should be noted that foregoing description is only the preferred embodiment of the present invention, the ordinary skill people of this field
Member under the inspiration of the present invention, without prejudice to the purpose of the present invention and the claims, can make multiple similar tables
Show, such transformation is fallen within the scope of protection of the present invention.
Claims (10)
1. a kind of prepare the ultra-fine Sm of high-coercive force2Co17The method of magnetic powder, it is characterised in that sequentially include the following steps:
2:17 type SmCo magnet is broken for magnetic particle by step 1；
Step 2, the magnetic particle that step 1 is obtained is put into low energy ball grinder, and abrading-ball, solvent and surface-active is added
Then ball grinder is placed in progress low energy ball milling under low temperature environment by agent；
Content in the low energy ball grinder is transferred in high-energy ball milling tank by step 3 in the step 2 after low energy ball milling,
High-energy ball milling is carried out under low temperature environment, and magnet powder is taken out after the completion of ball milling to get ultra-fine Sm2Co17Magnetic powder；
The low temperature environment temperature is -130--20 DEG C；
The fusing point of the solvent is lower than the temperature of the low temperature environment.
2. a kind of the ultra-fine Sm of high-coercive force is prepared according to claim 12Co17The method of magnetic powder, it is characterised in that: described
In step 2, the revolving speed of the low energy ball milling is 150-300r/min；
In the step 3, the revolving speed of the high-energy ball milling is 450-800r/min.
3. a kind of the super Sm of high-coercive force is prepared according to claim 1 or 22Co17The method of magnetic powder, it is characterised in that: institute
It states in step 2, the time of the low energy ball milling is 15-25h.
4. a kind of the ultra-fine Sm of high-coercive force is prepared according to claim 1 or 22Co17The method of magnetic powder, it is characterised in that:
In the step 3, the time of the high-energy ball milling is 20-40h.
5. a kind of the ultra-fine Sm of high-coercive force is prepared according to claim 1 or 22Co17The method of magnetic powder, it is characterised in that:
In the step 2 and step 3, by weight, the abrading-ball is 10:1 with the ratio of grinding media to material of the magnetic particle or magnet powder.
6. a kind of the ultra-fine Sm of high-coercive force is prepared according to claim 1 or 22Co17The method of magnetic powder, it is characterised in that:
In the step 2, the low energy ball grinder is placed in incubation chamber, liquid nitrogen is injected into the incubation chamber to the low energy ball milling
Tank is partially submerged, so that the low energy ball grinder keeps low temperature.
7. a kind of the ultra-fine Sm of high-coercive force is prepared according to claim 12Co17The method of magnetic powder, it is characterised in that: described
Solvent is isohexane.
8. a kind of the ultra-fine Sm of high-coercive force is prepared according to claim 12Co17The method of magnetic powder, it is characterised in that: described
The weight ratio of surfactant and the magnetic particle is 3-5:10.
9. a kind of the ultra-fine Sm of high-coercive force is prepared according to claim 82Co17The method of magnetic powder, it is characterised in that: described
Surfactant is oleic acid.
10. a kind of the ultra-fine Sm of high-coercive force is prepared according to claim 12Co17The method of magnetic powder, it is characterised in that: institute
It states in step 1, the SmCo magnet is broken for the magnetic particle of 100-200 mesh.
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| CN111243804A (en) * | 2019-11-29 | 2020-06-05 | 南京安德海睿智能科技有限公司 | Rare earth permanent magnet with hydrogen resistance and preparation method thereof |
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| CN111243804A (en) * | 2019-11-29 | 2020-06-05 | 南京安德海睿智能科技有限公司 | Rare earth permanent magnet with hydrogen resistance and preparation method thereof |
| CN111243804B (en) * | 2019-11-29 | 2023-10-17 | 南京安德海睿智能科技有限公司 | Rare earth permanent magnet with hydrogen resistance and preparation method thereof |
| CN111097916A (en) * | 2020-01-09 | 2020-05-05 | 北京矿冶科技集团有限公司 | Preparation method of superfine high-purity rhenium powder |
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