CN113593877A - Method for preparing nano-scale high-performance composite magnet material - Google Patents
Method for preparing nano-scale high-performance composite magnet material Download PDFInfo
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- 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
- H01F41/02—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 for manufacturing cores, coils, or magnets
- H01F41/0253—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 for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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- 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
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- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0576—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together pressed, e.g. hot working
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- H01F1/047—Alloys characterised by their composition
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- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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- 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
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0579—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B with exchange spin coupling between hard and soft nanophases, e.g. nanocomposite spring magnets
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Abstract
The invention discloses a method for preparing a nanometer-level high-performance composite magnet material, which comprises the following steps: weighing raw materials according to a certain stoichiometric ratio, grinding and mixing the raw materials, and pressing the powder into blocks; presintering the pressed blocks at a certain temperature to form a precursor; cleaning a precursor, drying, putting the precursor serving as a target on a target support of a beaker, filling an isopropyl alcohol solution which is 5-10 mm higher than the precursor, placing the beaker on a rotary platform, adopting third harmonic of Nd, namely YAG laser as an ablation laser light source, and focusing a laser pulse light beam on the surface of the precursor for ablation to generate a mixed solution containing nano-scale particle precipitates; and filtering the precipitate of the mixed solution, repeatedly cleaning and drying to obtain the nano-grade high-performance composite permanent magnet material. The method has simple preparation process, and the prepared composite nanocrystalline permanent magnet has clean surface and good chemical activity, and simultaneously effectively inhibits structural deformity and improves the magnetic property of the nanocrystalline magnet.
Description
Technical Field
The invention particularly relates to a method for preparing a nano-scale high-performance composite magnet material.
Background
The composite nanocrystalline magnetic material is a novel two-phase permanent magnetic material developed in recent years. It is characterized by that the hard magnetic phase with high magnetocrystalline anisotropy and soft magnetic phase with high saturation magnetization produce strong magnetic exchange coupling action on the nano scale, so that the magnet can present obvious remanence enhancement effect (Mr/Ms > 0.5). At present, the research on the high-performance composite nanocrystalline magnetic material is less, and therefore, a preparation method of the high-performance composite nanocrystalline magnetic material is needed to be provided.
Disclosure of Invention
In view of the above situation, the present invention provides a method for preparing a nanoscale high-performance composite magnet material in order to overcome the defects of the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for preparing a nanoscale high-performance composite magnet material comprises the following steps:
(1) a burdening stage: weighing raw materials according to a certain stoichiometric ratio, grinding and mixing the raw materials, and pressing the powder into blocks;
(2) and (3) pre-burning stage: presintering the pressed blocks at a certain temperature to form a precursor;
(3) an ablation stage: cleaning of the precursor, 80oC ~120 oCDrying, placing the dried target material as a target material on a target material bracket of a beaker, filling an isopropyl alcohol solution which is 5-10 mm higher than the precursor, placing the beaker on a rotating platform, adopting third harmonic of an Nd-YAG laser as an ablation laser light source, focusing a laser pulse light beam on the surface of the precursor for ablation, and generating a mixed solution containing nano-scale particle precipitates;
(4) a separation stage: and filtering the precipitate of the mixed solution, repeatedly cleaning and drying to obtain the nano-grade high-performance composite permanent magnet material. Further, In the step (1), the raw materials comprise Nd, Dy, Tb, In, Fe and Co powder, NbFe powder, FeB powder and FeCrCo alloy powder subjected to induction melting, wherein the mass fraction of B In the FeB powder is 19.83%; the mass fraction of Nb in the NbFe powder is 66.3 percent; the FeCrCo alloy powder contains 24.7w% of Cr, 12.9wt% of Co, 1.1 wt% of Si and the balance of Fe.
Further, in the step (1), the length and the width of the pressed block are respectively 12-25 mm, and the thickness is 3-6 mm.
Further, in the step (2), the temperature in the pre-sintering stage is 1000-1300 ℃, and the pre-sintering time is 2-5 hours. The temperature of the pre-sintering stage is set to be 1000-1300 ℃, so that the flow of a crystal boundary phase is facilitated, and the magnetic performance is improved.
Further, in the step (3), the Nd-YAG laser is a nanosecond solid laser, the laser frequency is 10 Hz, the wavelength is 1064nm, the pulse width is 7ns, the laser pulse intensity is 100-250 mJ/pulse, and the spot diameter is 1 mm. The laser parameters are set to the above values, which facilitates melting of the material and formation of nanoparticles.
Further, in the step (3), the laser pulse light beam is focused on the surface of the precursor to be ablated for 10-20 min.
Further, in the step (3), an ultrasonic cleaning agent is used for cleaning the precursor, and the ultrasonic cleaning agent is ethanol.
Further, in the step (3), the beaker is placed on a rotating platform with the rotating speed of 20 r/min.
Further, in the step (4), a centrifugal machine is adopted for filtering, the speed is 5000-15000 rpm, and the centrifugation is carried out for 10-30 min.
Further, in the step (4), the drying temperature is 150 DEGoC。
The invention has the beneficial effects that:
(1) the chemical composition of the composite permanent magnet material is Nd2Fe14The preparation method of the invention can generate extreme environments such as high temperature and high pressure at room temperature, and the particles from the target material and the solution medium can generate various reactions in the extreme environments of high temperature and high pressure, and the liquid has good cooling effect, can realize the rapid cooling of high temperature plasma, has simple preparation process, ensures that the prepared composite nanocrystalline permanent magnet has clean surface and good chemical activity, and effectively inhibits the junctionThe structure is deformed, and the magnetic performance of the nanocrystalline magnet is improved.
(2) Compared with a rapid quenching method, the novel laser liquid phase ablation nano composite permanent magnet material has the advantages of simpler preparation method, easier control of the environment and good cooling effect of liquid, can realize rapid cooling of high-temperature plasma, protects the nano composite permanent magnet material, obtains a uniformly distributed nano microcrystal structure, and obtains a microstructure as shown in figure 2.
(3) In the invention, the ablated magnet grain boundary phase has a cleaner surface and higher chemical activity, and the composite phase can generate strong exchange coupling effect on the nano-crystalline scale to obtain higher theoretical maximum energy product.
Drawings
FIG. 1 is a schematic diagram of the preparation process of the present invention.
FIG. 2 is a TEM image of a nanocomposite magnet material produced by the present invention.
Detailed Description
The technical solutions of the present invention are further described in detail below with reference to the accompanying drawings, and it should be noted that the detailed description is only for describing the present invention, and should not be construed as limiting the present invention.
Example 1
A method for preparing a nano-scale composite magnet material by a liquid-phase laser ablation method comprises the following steps:
(1) a burdening stage: the atomic number ratio is Nd: dy: fe: nb: co: b = 9: 0.4: 80.24: 0.36: 3: 6, converting the atomic number ratio into a mass ratio, then weighing metal powder materials Nd, Dy, Tb, In, Fe, Co, FeB (the mass fraction of B In FeB is 19.83%) and NbFe (the mass fraction of Nb In NbFe is 66.3%), adding FeCrCo alloy powder (Cr 24.7w%, Co 12.9wt%, Si 1.1 wt% and the balance Fe) prepared by induction melting or other melting methods, fully grinding and mixing, and pressing the raw material powder into blocks with the length of 15mm, the width of 15mm and the thickness of 4mm under the pressure of 15 MPa;
in the embodiment, the FeCrCo alloy powder is prepared by an induction melting method, which is a conventional method in the prior art, and the invention does not improve the method. In this embodiment, the raw material is pressed into a block, in other embodiments, other shapes or other sizes of blocks may be pressed.
(2) And (3) pre-burning stage: pressing the pressed blocks at 1200oC, pre-burning for 1h to form a precursor;
(3) an ablation stage: the temperature of the precursor is reduced to 30 DEGoC, cleaning the precursor for 30min by using an ultrasonic cleaning agent (such as chromatographic pure ethanol) 80 minoC ~120 oCDrying, placing the dried mixture on a target material bracket of a beaker, filling isopropanol which is 10mm higher than the precursor, placing the beaker on a magnetic stirrer with the rotating speed of 20 r/min, adopting Nd, namely third harmonic wave of a YAG laser as an ablation laser light source, the laser frequency is 10 Hz, the wavelength is 1064nm, the pulse width is 7ns, the laser pulse intensity is 100 mJ/pulse, the spot diameter is 1mm, focusing a laser pulse light beam on the surface of the precursor to ablate for 15min, and generating a mixed solution containing nano-particle precipitates;
(4) a separation stage: filtering the precipitate of the mixed solution with a centrifuge at 8000rpm, repeatedly cleaning for 5 times, centrifuging for 30min, and then at 150%oDrying for 2h under the condition of C to obtain nano-grade high-performance Nd2Fe14B/FeCrCo composite magnetic material.
Compared with the material prepared by a rapid quenching method, the nano composite permanent magnet prepared by the invention still has a coercive force control mechanism as a nucleation mechanism, but has smaller crystal grain size, the average grain diameter of 10 nm-150 nm, stronger exchange coupling strength and 19.1 MGOe magnetic energy product, improves 17% of the magnetic energy product of the material obtained by high-energy ball milling (16.3 MGOe), obviously improves the comprehensive magnetic property and is safer in the preparation process.
Example 2
A method for preparing a nano-scale composite magnet material by a liquid-phase laser ablation method comprises the following steps:
(1) a burdening stage: the atomic number ratio is Nd: dy: fe: nb: co: b = 9: 0.4: 80.24: 0.36: 3: 6, converting the atomic number ratio into a mass ratio, then weighing metal powder materials Nd, Dy, Tb, In, Fe, Co, FeB (the mass fraction of B In FeB is 19.83%) and NbFe (the mass fraction of Nb In NbFe is 66.3%), adding FeCrCo alloy powder (Cr 24.7w%, Co 12.9wt%, Si 1.1 wt% and the balance Fe) prepared by induction melting or other melting methods, fully grinding and mixing, and pressing the raw material powder into blocks with the width of 12mm and the height of 5mm under the pressure of 15 MPa;
(2) and (3) pre-burning stage: pressing the pressed blocks at 1200oC, pre-burning for 1h to form a precursor;
(3) an ablation stage: the temperature of the precursor is reduced to 20 DEGoC, cleaning the precursor for 30min by using an ultrasonic cleaning agent (such as chromatographic pure ethanol) 80 minoC ~120 oCDrying, placing the dried mixture on a target material bracket of a beaker, filling 5mm of isopropyl alcohol to submerge the precursor, placing the beaker on a magnetic stirrer with the rotation speed of 20 r/min, adopting Nd, namely third harmonic wave of a YAG laser as an ablation laser light source, the laser frequency is 10 Hz, the wavelength is 1064nm, the pulse width is 7ns, the laser pulse intensity is 100 mJ/pulse, the spot diameter is 1mm, and focusing a laser pulse light beam on the surface of the precursor to ablate for 20min to generate a mixed solution containing nano-particle precipitates;
(4) a separation stage: filtering the precipitate with centrifuge at 10000rpm for 30min, and repeatedly cleaning for 5 times, and then centrifuging at 150 deg.CoDrying for 3h under the condition of C to obtain nano-grade high-performance Nd2Fe14B/FeCrCo composite magnetic material.
The coercive force control mechanism of the nano composite permanent magnet obtained by the embodiment is still a nucleation mechanism, but the nano composite permanent magnet has smaller grain size, the average grain diameter of 20 nm-120 nm, stronger exchange coupling strength and 22.3 MGOe magnetic energy product, obviously improved comprehensive magnetic property and safer preparation process.
It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (10)
1. A method for preparing a nano-grade high-performance composite magnet material is characterized by comprising the following steps:
(1) a burdening stage: weighing raw materials according to a certain stoichiometric ratio, grinding and mixing the raw materials, and pressing the powder into blocks;
(2) and (3) pre-burning stage: presintering the pressed blocks at a certain temperature to form a precursor;
(3) an ablation stage: cleaning a precursor, drying, putting the precursor serving as a target on a target support of a beaker, filling an isopropyl alcohol solution which is 5-10 mm higher than the precursor, placing the beaker on a rotary platform, adopting third harmonic of Nd, namely YAG laser as an ablation laser light source, and focusing a laser pulse light beam on the surface of the precursor for ablation to generate a mixed solution containing nano-scale particle precipitates;
(4) a separation stage: and filtering the precipitate of the mixed solution, repeatedly cleaning and drying to obtain the nano-grade high-performance composite permanent magnet material.
2. A method for producing a nano-scale high performance composite magnet material as claimed In claim 1, wherein In the step (1), the raw materials include Nd, Dy, Tb, In, Fe, Co powders, NbFe powders, FeB powders and induction-smelted FeCrCo alloy powders, wherein the mass fraction of B In the FeB powders is 19.83%; the mass fraction of Nb in the NbFe powder is 66.3 percent; the FeCrCo alloy powder contains 24.7w% of Cr, 12.9wt% of Co, 1.1 wt% of Si and the balance of Fe.
3. The method for producing a nano-scale high performance composite magnetic material as claimed in claim 1, wherein in the step (1), the length and width of the pressed block are 12 to 25mm, respectively, and the thickness is 3 to 6 mm.
4. The method for preparing a nano-scale high-performance composite magnet material according to claim 1, wherein in the step (2), the temperature in the pre-sintering stage is 1000 to 1300 ℃, and the pre-sintering time is 2 to 5 hours.
5. The method according to claim 1, wherein in the step (3), the Nd-YAG laser is a nanosecond solid laser, the laser frequency is 10 Hz, the wavelength is 1064nm, the pulse width is 7ns, the laser pulse intensity is 100-250 mJ/pulse, and the spot diameter is 1 mm.
6. The method for preparing a nano-scale high-performance composite magnet material according to claim 1, wherein in the step (3), a laser pulse light beam is focused on the surface of the precursor for ablation for 10-20 min.
7. The method for preparing a nano-scale high-performance composite magnet material according to claim 1, wherein in the step (3), the precursor is cleaned by using an ultrasonic cleaning agent, and the ultrasonic cleaning agent is ethanol.
8. The method for producing a nano-scale high performance composite magnetic material as claimed in claim 1, wherein in the step (3), the beaker is placed on a rotating platform with a rotating speed of 20 r/min.
9. The method for preparing a nano-scale high-performance composite magnet material according to claim 1, wherein the step (4) is performed by using a centrifuge at a speed of 5000-15000 rpm.
10. The method for producing a nano-scale high-performance composite magnetic material as claimed in claim 1, wherein the drying temperature in the step (4) is 150 ℃oC。
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107045911A (en) * | 2017-03-27 | 2017-08-15 | 河北工业大学 | Nd Fe B thin strip magnets and preparation method thereof |
| CN107464646A (en) * | 2017-09-27 | 2017-12-12 | 杭州天时亿科技有限公司 | A kind of preparation method of high evenness adhesive bond Ru-Fe-Mn |
| CN112582167A (en) * | 2020-12-31 | 2021-03-30 | 杨方宗 | Method for preparing nano-scale rare earth magnetic refrigeration material by laser ablation |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107045911A (en) * | 2017-03-27 | 2017-08-15 | 河北工业大学 | Nd Fe B thin strip magnets and preparation method thereof |
| CN107464646A (en) * | 2017-09-27 | 2017-12-12 | 杭州天时亿科技有限公司 | A kind of preparation method of high evenness adhesive bond Ru-Fe-Mn |
| CN112582167A (en) * | 2020-12-31 | 2021-03-30 | 杨方宗 | Method for preparing nano-scale rare earth magnetic refrigeration material by laser ablation |
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