CN106920608A - The preparation method of high-performance anisotropy nano permanent magnetic material - Google Patents
The preparation method of high-performance anisotropy nano permanent magnetic material Download PDFInfo
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- CN106920608A CN106920608A CN201611120590.7A CN201611120590A CN106920608A CN 106920608 A CN106920608 A CN 106920608A CN 201611120590 A CN201611120590 A CN 201611120590A CN 106920608 A CN106920608 A CN 106920608A
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- magnetic material
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- ball milling
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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
-
- 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
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- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Powder Metallurgy (AREA)
- Hard Magnetic Materials (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The present invention relates to technical field of function materials, and in particular to a kind of preparation method of high-performance anisotropy nano permanent magnetic material.The preparation method of high-performance anisotropy nano permanent magnetic material, the first step, under Ar gas shieldeds, the metalliferous material that will be prepared is put into water jacketed copper crucible, with Medium frequency induction equipment melting hard magnetic alloy ingot；Before melting, 5 × 10 are evacuated down to using mechanical pump‑2 Pa, is filled with high-purity Ar gas, and repetition is vacuumized, and repeats melting time, makes ingot casting composition uniform；Second step, Mechanical Crushing carries out wet ball grinding treatment after hand lapping；3rd step, in the glove box full of Ar gas shieldeds, carries out ball milling.4th step, after ball milling, ultrasonic wave dispersion cleaning is carried out to ball milling product；Centrifugation, rapid thermal treatment, are obtained high-performance anisotropy Sm2Co17Nano permanent magnetic material.The present invention has good application value in terms of high-performance anisotropic permanent-magnetic material with soft or hard magnetic nano composite permanent magnetic material.
Description
Technical field
The present invention relates to technical field of function materials, and in particular to a kind of system of high-performance anisotropy nano permanent magnetic material
Preparation Method.
Background technology
Obvious magnetic anisotropy and stronger coercivity are that permanent-magnet material is different from two of other magnetic materials very
Important index, is also permanent-magnet material researcher and the continuous target pursued of the producer.Prepare these anisotropic permanent magnetism materials
The conventional method of material has HDDR methods, directional solidification method, hot pressing thermal deformation method, mechanical alloying method etc..These methods are each advantageous,
But there is the common feature that technique is relative complex, affecting parameters are more.The end of the year 2006, Texas ,Usa university Liu researchs
Chakka of group et al. reports a kind of addition oleic acid, oleyl amine and prepares permanent magnetism as surfactant auxiliary high-energy ball milling first
The technology of nano particle.At the beginning of 2010, it is tens that Shen et al. is prepared for thickness less than 100nm, thickness using this method
To hundreds of nm, width is several μm, average grain size be 10 nm or so with higher coercivity, obvious magnetic anisotropy,
The PrCo of sheet-like morphology5Nano permanent magnetic material, the room temperature coercivity on its easy magnetizing axis reaches 530.9 kA/m, fully shows
Good prospect of this technology in terms of high anisotropy and high-coercive force permanent magnetism nano particle is prepared.Thereafter, academia's research
Personnel begin attempt to develop high-performance nano permanent-magnet material using this preparation method one after another.
The content of the invention
The present invention is directed to propose a kind of preparation method of high-performance anisotropy nano permanent magnetic material.
Technical program of the present invention lies in：
The preparation method of high-performance anisotropy nano permanent magnetic material, comprises the following steps：
The first step, under Ar gas shieldeds, the metalliferous material that will be prepared is put into water jacketed copper crucible, molten with Medium frequency induction equipment
Refining hard magnetic alloy ingot；Before melting, 5 × 10 are evacuated down to using mechanical pump-2 Pa, is filled with high-purity Ar gas, and repetition is vacuumized fills
Ar gas 5 times；Melting 4 times is repeated, so that ingot casting composition is uniform；
Second step, starting ingot homogenizing annealing 8h at a temperature of 800 DEG C, then by Mechanical Crushing, hand lapping is into granularity
It is 400 mesh fine powder powder, loads ball grinder, carries out wet ball grinding treatment；
3rd step, in the glove box full of Ar gas shieldeds, adds ball milling solvent, and adds surfactant, and ball grinder is by close
Seal is sealed, and is fixed on ball mill after ball milling initial feed is loaded into ball grinder, starts ball mill so that ball milling is initial
Raw material is subject to steel ball high speed generating collision in tank, rapid to crush；
4th step, after ball milling, ultrasonic wave dispersion cleaning is carried out to ball milling product；Nano particle point is carried out using high-speed centrifugation technology
Level, obtains the narrow nanometer paramagnetic particles of particle size distribution；Appropriate rapid thermal treatment finally is carried out to gained powder, is obtained
High-performance anisotropy Sm2Co17Nano permanent magnetic material.
It is described when founding ingot casting, scaling loss during melting is made up to volatile metal Sm.
Described second step wet ball grinding uses planetary ball mill.
Described ball milling solvent is normal heptane.
Described surfactant is the mixture of oleic acid and oleyl amine.
The sealing ring of described ball grinder is teflin ring.
The technical effects of the invention are that：
It is sub-micron that the present invention obtains thickness in 80nm or so, length by the method that surfactant strengthens high-energy ball milling
Level, the high-coercive force Sm with high-specific surface area, high shape anisotropic property and magnetic anisotropy2Co17Nanometer permanent-magnet powder.By
After magnetic field orientating, Sm2Co17Easy magnetizing axis and hard axis direction room temperature coercivity respectively reach 612.9 kA/m and
278.6 kA/m, have application well in terms of high-performance anisotropic permanent-magnetic material with soft or hard magnetic nano composite permanent magnetic material
Value.
Specific embodiment
The preparation method of high-performance anisotropy nano permanent magnetic material, comprises the following steps：
The first step, under Ar gas shieldeds, the metalliferous material that will be prepared is put into water jacketed copper crucible, molten with Medium frequency induction equipment
Refining hard magnetic alloy ingot；Before melting, 5 × 10 are evacuated down to using mechanical pump-2 Pa, is filled with high-purity Ar gas, and repetition is vacuumized fills
Ar gas 5 times；Melting 4 times is repeated, so that ingot casting composition is uniform；
Second step, starting ingot homogenizing annealing 8h at a temperature of 800 DEG C, then by Mechanical Crushing, hand lapping is into granularity
It is 400 mesh fine powder powder, loads ball grinder, carries out wet ball grinding treatment；
3rd step, in the glove box full of Ar gas shieldeds, adds ball milling solvent, and adds surfactant, and ball grinder is by close
Seal is sealed, and is fixed on ball mill after ball milling initial feed is loaded into ball grinder, starts ball mill so that ball milling is initial
Raw material is subject to steel ball high speed generating collision in tank, rapid to crush；
4th step, after ball milling, ultrasonic wave dispersion cleaning is carried out to ball milling product；Nano particle point is carried out using high-speed centrifugation technology
Level, obtains the narrow nanometer paramagnetic particles of particle size distribution；Appropriate rapid thermal treatment finally is carried out to gained powder, is obtained
High-performance anisotropy Sm2Co17Nano permanent magnetic material.
Wherein, it is described when founding ingot casting, scaling loss during melting is made up to volatile metal Sm.Described second step is wet
Method ball milling uses planetary ball mill.Described ball milling solvent is normal heptane.Described surfactant is oleic acid and oleyl amine
Mixture.The sealing ring of described ball grinder is teflin ring.
Embodiment 2
The first step, under Ar gas shieldeds, the metalliferous material that will be prepared is put into water jacketed copper crucible, with Medium frequency induction equipment melting
Hard magnetic alloy ingot；Before melting, 5.5 × 10 are evacuated down to using mechanical pump-2 Pa, is filled with high-purity Ar gas, and repetition is vacuumized fills
Ar gas 5 times；Melting 4 times is repeated, so that ingot casting composition is uniform；
Second step, starting ingot homogenizing annealing 8.5h at a temperature of 800 DEG C, then by Mechanical Crushing, hand lapping granulating
It is 400 mesh fine powder powder to spend, and loads ball grinder, carries out wet ball grinding treatment；
3rd step, in the glove box full of Ar gas shieldeds, adds ball milling solvent, and adds surfactant, and ball grinder is by close
Seal is sealed, and is fixed on ball mill after ball milling initial feed is loaded into ball grinder, starts ball mill so that ball milling is initial
Raw material is subject to steel ball high speed generating collision in tank, rapid to crush；
4th step, after ball milling, ultrasonic wave dispersion cleaning is carried out to ball milling product；Nano particle point is carried out using high-speed centrifugation technology
Level, obtains the narrow nanometer paramagnetic particles of particle size distribution；Appropriate rapid thermal treatment finally is carried out to gained powder, is obtained
High-performance anisotropy Sm2Co17Nano permanent magnetic material.
Surfactant oleic acid, oleyl amine have carried out effective induction and control to the mechanical milling process of cast alloy, at least rise
Following key effect is arrived：(1) crystal grain thinning：Surfactant effectively reduces various materials in traditional mechanical milling process
The ball milling lower limit to be produced；(2) prevent from reuniting：Surfactant is in time carried out the new particle for producing in mechanical milling process
Isolate and be distributed in solvent and effectively prevent the reunion between particle；(3) anti-oxidation：Surfactant is tightly adsorbed
And be coated on new generation, on the ball milling particle exterior surface that chemism is high, effective anti-oxidation magnet loss phenomenon；(4) lead to
Anisotropy：Due to the inducing action of surfactant, ball milling product internal grain produces specific oriented growth, and outside it
Sheet-like morphology is formd in sight, so as to produce stronger magnetocrystalline and shape anisotropy, obvious magnetic anisotropy is ultimately formed；
(5) crystal formation is kept：Prevent excess destruction of the crystal grain in mechanical milling process, it is ensured that ball milling product have preferable coercivity and
Remanent magnetism.
It is Asia that the present invention obtains thickness in 80nm or so, length by the method that surfactant strengthens high-energy ball milling
Micron order, the high-coercive force Sm with high-specific surface area, high shape anisotropic property and magnetic anisotropy2Co17Nanometer permanent-magnet powder.
By after magnetic field orientating, Sm2Co17Easy magnetizing axis and hard axis direction room temperature coercivity respectively reach 612.9 kA/m and
278.6 kA/m, have application well in terms of high-performance anisotropic permanent-magnetic material with soft or hard magnetic nano composite permanent magnetic material
Value.
Claims (6)
1. the preparation method of high-performance anisotropy nano permanent magnetic material, it is characterised in that：Comprise the following steps：
The first step, under Ar gas shieldeds, the metalliferous material that will be prepared is put into water jacketed copper crucible, molten with Medium frequency induction equipment
Refining hard magnetic alloy ingot；Before melting, 5 × 10 are evacuated down to using mechanical pump-2 Pa, is filled with high-purity Ar gas, and repetition is vacuumized fills
Ar gas 5 times；Melting 4 times is repeated, so that ingot casting composition is uniform；
Second step, starting ingot homogenizing annealing 8h at a temperature of 800 DEG C, then by Mechanical Crushing, hand lapping is into granularity
It is 400 mesh fine powder powder, loads ball grinder, carries out wet ball grinding treatment；
3rd step, in the glove box full of Ar gas shieldeds, adds ball milling solvent, and adds surfactant, and ball grinder is by close
Seal is sealed, and is fixed on ball mill after ball milling initial feed is loaded into ball grinder, starts ball mill so that ball milling is initial
Raw material is subject to steel ball high speed generating collision in tank, rapid to crush；
4th step, after ball milling, ultrasonic wave dispersion cleaning is carried out to ball milling product；Nano particle point is carried out using high-speed centrifugation technology
Level, obtains the narrow nanometer paramagnetic particles of particle size distribution；Appropriate rapid thermal treatment finally is carried out to gained powder, is obtained
High-performance anisotropy Sm2Co17Nano permanent magnetic material.
2. the preparation method of high-performance anisotropy nano permanent magnetic material according to claim 1, it is characterised in that：It is described
When founding ingot casting, scaling loss during melting is made up to volatile metal Sm.
3. the preparation method of high-performance anisotropy nano permanent magnetic material according to claim 1, it is characterised in that：It is described
Second step wet ball grinding use planetary ball mill.
4. the preparation method of high-performance anisotropy nano permanent magnetic material according to claim 1, it is characterised in that：It is described
Ball milling solvent be normal heptane.
5. the preparation method of high-performance anisotropy nano permanent magnetic material according to claim 1, it is characterised in that：It is described
Surfactant be the mixture of oleic acid and oleyl amine.
6. the preparation method of high-performance anisotropy nano permanent magnetic material according to claim 1, it is characterised in that：It is described
Ball grinder sealing ring be teflin ring.
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| CN201611120590.7A CN106920608A (en) | 2016-12-08 | 2016-12-08 | The preparation method of high-performance anisotropy nano permanent magnetic material |
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| CN201611120590.7A CN106920608A (en) | 2016-12-08 | 2016-12-08 | The preparation method of high-performance anisotropy nano permanent magnetic material |
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| CN106920608A true CN106920608A (en) | 2017-07-04 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN115106534A (en) * | 2022-08-30 | 2022-09-27 | 西安稀有金属材料研究院有限公司 | Preparation method of multi-powder uniformly-dispersed sintered anode foil |
-
2016
- 2016-12-08 CN CN201611120590.7A patent/CN106920608A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN115106534A (en) * | 2022-08-30 | 2022-09-27 | 西安稀有金属材料研究院有限公司 | Preparation method of multi-powder uniformly-dispersed sintered anode foil |
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