CN104319049B - Easily face type biphase nanocrystalline high-frequency soft magnetic material and preparation method thereof - Google Patents
Easily face type biphase nanocrystalline high-frequency soft magnetic material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to soft magnetic materials field, be specifically related to one and there is anisotropic 2: 17 type rare earth 3d metal alloys/3d metal biphase nanocrystalline high-frequency soft magnetic material in easy face and preparation method thereof.This soft magnetic materials is by the 2:17 type rare earth 3d metal alloy R of nano-scale2M17Composition compound with 3d metal M, this soft magnetic materials composition is by volume: 2:17 type rare earth 3d metal alloy R2M17Being 5% 95%, remaining is 3d metal M.Show through relevant experimental study, anisotropic 2: the 17 type rare earth 3d metal alloys/3d metal biphase nanocrystalline high-frequency soft magnetic material in easy face of the present invention has the high frequency electromagnetic property being better than prior art, its pcrmeability initial value can reach 1.89, resonant frequency has reached 7GHz, on the premise of ensureing high complex permeability initial value, there is higher resonant frequency, be a kind of good high-frequency soft magnetic material.
Description
Technical field
The invention belongs to soft magnetic materials field, be specifically related to one and there is easy face anisotropic 2:
17 type rare earth-3d metal alloys/3d metal biphase nanocrystalline high-frequency soft magnetic material and preparation side thereof
Method.
Background technology
Along with the fast development of information technology, frequency electromagnetic waves as the important carrier of Information Communication,
The most more and more it is used for the various aspects of human lives and production.High-frequency electron device wide
General application defines the electromagnetic environment of complexity, makes electromagenetic wave radiation day by day increase the impact of environment,
Electromagnetic Interference problem becomes increasingly severe, and this causes the biggest danger to the safety of information
Evil.Electromagnetic pollution not only affects communication, and directly threatens human health, and this just promotes science and technology
Personnel step up electromagnetism interference figure layer, from the electro-magnetic wave absorption material such as stealth technology and microwave dark room
The research and development of material.Wherein, magnetic material, as excellent absorbing material, is that leader studies and answers
Advanced subject.
For the composite for electromagnetic wave shielding, high pcrmeability and high resonant frequency it is
Sample has the essential condition of excellent microwave absorbing property, high resonant frequency ability at high band
Make sample still have high magnetic permeability value at high band, and high magnetic permeability value just can make material full
The condition of foot impedance matching, good impedance matching is the microwave absorbing property that sample has excellence
Premise.The magnetic microwave absorption used the most both at home and abroad is broadly divided into ferrospinel, and six
Angle-style ferrite, magnetic metal powder, magnetic nanometer composite material and easy face type rare earth-3d metallization
Compound is several.Ferrospinel (nickel-zinc ferrite, Journals of Alloys and
Compounds 481 841,2009, Chinese invention patent application 201110210932.5) have suitable
When dielectric constant, but be constrained to the restriction of the Snoek limit, and saturable bead intensity be relatively
Low, its high frequency pcrmeability all ratio is relatively low；Hxagonal ferrite material (Co2Z Barium hexaferrite, IEEE
Transactions on Magnetics 44 2255,2008, Chinese invention patent application
200510046690.5) restriction of the Snoek limit can be broken through, but saturation magnetization is relatively low,
Limit the sample further application at high band；Magnetic metal powder body (carbonyl iron particles,
Journal of Magnetism and Magnetic Materials 321 25,2009) there is high satisfying
And the intensity of magnetization, so the high frequency pcrmeability of material is higher, but due to the relatively low magnetocrystalline of material
Anisotropy field, resonant frequency is the most on the low side；Easily face type rare earth-3d metal alloy (Sm2Fe14B
Compound, Applied Physics A 108 665,2012, Chinese invention patent application
201010230807.6) due to double anisotropic existence, the restriction of the Snoek limit can be broken through,
There is high resonant frequency, but due to rare earth-3d metallic compound saturation magnetization relatively
Low, limit the sample further application at high band.In the prior art, it is difficult to carry simultaneously
The pcrmeability initial value of high sample and resonant frequency.
Biphase nanocrystalline material, since coming out, has been studied widely, but disclosed
In technical field, this kind of material belongs to hard magnetic material, the easy magnetizing axis of rare earth-3d metal alloy with
C direction of principal axis is parallel, and such as Chinese invention patent application 200510087114.5, to disclose one ' dilute
The preparation method of unmanufactured iron series biphase nanocrystalline composite permanent-magnet material '.
Summary of the invention
For the deficiency of current material, it is an object of the invention to provide and a kind of both there is high being total to
Vibration frequency and to have anisotropic 2: 17 types in easy face of high complex permeability initial value dilute
Soil-3d metal alloy/3d metal biphase nanocrystalline high-frequency soft magnetic material and preparation method thereof.This pair
Phase nanocomposite high-frequency soft magnetic material is the rare earth soft magnetic materials that a class is novel, be characterized in by
The 3d metal of high saturation and magnetic intensity and the easy face anisotropic 2 with high resonant frequency:
The spin-exchange-coupled under nano-scale of 17 type rare earth-3d metal alloys becomes to have high saturated magnetization strong
Degree, the two-phase High Frequency Of Recombination soft magnetic materials of high pcrmeability initial value and high resonant frequency.
For achieving the above object, technical scheme is as follows:
A kind of biphase nanocrystalline high-frequency soft magnetic material, this soft magnetic materials is by the 2:17 of nano-scale
Type rare earth-3d metal alloy R2M17Composition compound with 3d metal or metal alloy M, this soft magnetism
Material composition is by volume: 2:17 type rare earth-3d metal alloy R2M17For 5%-95%,
Remaining is 3d metal M；Described 2:17 type rare earth-3d metal alloy R2M17In, R is Ce,
One or both in Nd, Y, Gd, Tb, Dy, Er, Tm or Lu, M is Fe, Co
Or the one in Fe-Co alloy/C.
Described 2:17 type rare earth-3d metal alloy R2M17Direction of easy axis vertical with C axle.
Described soft magnetic materials is that the 2:17 type rare earth-3d metal of the nano-scale by following structure closes
Gold R2M17Composition compound with 3d metal or metal alloy:
Nd2(FeCo)17With FeCo；
Nd2Fe17With Fe.
The preparation method of a kind of biphase nanocrystalline high-frequency soft magnetic material, this preparation method includes following
Step:
A) rare-earth element R and pure 3d metal M are weighed by alloy proportion, by rare-earth element R and pure
3d metal M is smelted into foundry alloy under inert gas shielding, wherein 2:17 type rare earth-3d gold
Belong to alloy R2M17Being 5%-95% by volume, remaining is 3d metal M；
B) melt-quenching method is used to prepare amorphous state, crystalline state nanometer or amorphous and nanocrystalline mixed state
State of quenching alloy；
C) prepared state alloy of quenching carries out airflow milling crush or ball mill crushing process；
D) the soft nanocrystalline magnetic materials powder after pulverizing is put after mixing homogeneously with uncured binding material
Enter in the mould that nonmagnetic substance makes, be placed in magnetic field rotating, until binding material
Solidification.
In step b, the linear velocity of fast melt-quenching is 10-80 meter per second.
In step c, when using airflow milling to crush, state alloy of quenching adds alloy mass 5
The antioxidant of ‰-10 ‰, makes average particle size 1-5 μm through airflow milling under inert gas shielding
Alloy powder；When using ball mill crushing, state alloy of quenching adds alloy mass 5 ‰-10 ‰
Antioxidant and the titanate coupling agent of 1%-5% and ball-milling medium isopropanol or gasoline, will
State of quenching alloy is ground to the mean diameter alloy powder less than 5 μm.
In step d, magnetic field intensity is 0.1-3 tesla, and rotary speed is 5-50 rev/min.
In step d, soft nanocrystalline magnetic materials powder and uncured binding material volume ratio are 1:
9-9:1, described binding material is epoxy resin, paraffin wax, methyl silicone rubber, Kynoar
In one.
The beneficial effects of the present invention is:
Show through relevant experimental study, anisotropic 2: the 17 type rare earths in easy face of the present invention
-3d metal alloy/3d metal biphase nanocrystalline high-frequency soft magnetic material has the height being better than prior art
Frequently electromagnetic performance, its pcrmeability initial value can reach 1.89, and resonant frequency has reached 7GHz,
On the premise of ensureing high complex permeability initial value, there is higher resonant frequency, be a kind of
Good high-frequency soft magnetic material.
Accompanying drawing explanation
Fig. 1 is XRD diffraction spectrogram before and after present example 1 material orientation.
Fig. 2 is before and after the material paraffin of present example 1 is composite orientation prepared by binding agent
Complex permeability is with the change of frequency.
Fig. 3 be the material paraffin of present example 2 be composite plural number magnetic conductance prepared by binding agent
Rate is with the change of frequency.
Fig. 4 be the material paraffin of present example 3 be composite plural number magnetic conductance prepared by binding agent
Rate is with the change of frequency.
Detailed description of the invention
Below in conjunction with the accompanying drawings and embodiment, the detailed description of the invention of the present invention is made the most in detail
Describe.
The biphase nanocrystalline high-frequency soft magnetic material of the present invention is by the 2:17 type rare earth of nano-scale
-3d metal alloy R2M17Composition compound with 3d metal M, this soft magnetic materials composition is by volume
For: 2:17 type rare earth-3d metal alloy R2M17For 5%-95%, remaining is 3d metal M,
Wherein, the one during R is Ce, Nd, Y, Gd, Tb, Dy, Er, Tm or Lu or two
Kind, M is the one in Fe, Co or Fe-Co alloy/C, and described 2:17 type rare earth-3d gold
Belong to alloy R2M17Direction of easy axis vertical with C axle.
The preparation method of the biphase nanocrystalline high-frequency soft magnetic material of the present invention, comprises the following steps:
A) rare-earth element R and pure 3d metal M are weighed by alloy proportion, by rare-earth element R and pure 3d
Metal M is smelted into foundry alloy under inert gas shielding, wherein 2:17 type rare earth-3d metal
Alloy R2M17Being 5%-95% by volume, remaining is 3d metal M；
B) melt-quenching method is used to prepare amorphous state, crystalline state nanometer or amorphous and nanocrystalline mixed state
State of quenching alloy, the linear velocity of fast melt-quenching is 10-80 meter per second；
C) prepared melt spun alloy carries out airflow milling crush or ball mill crushing, wherein, use air-flow
When galling broken, state alloy of quenching adds the antioxidant of alloy mass 5 ‰-10 ‰, at indifferent gas
Average particle size 1-5 μm alloy powder is made through airflow milling under body protection；When using ball mill crushing,
In state alloy of quenching, the antioxidant of interpolation alloy mass 5 ‰-10 ‰ and the titanate esters of 1%-5% are even
Joining agent and ball-milling medium isopropanol or gasoline, state of quenching alloy is ground to mean diameter less than 5
The alloy powder of μm；
D) the soft nanocrystalline magnetic materials powder after pulverizing is put after mixing homogeneously with uncured binding material
Enter nonmagnetic substance make mould in, be placed in the magnetic field of 0.1-3 tesla, with 5-50 turn/
Minute rotating speed rotate, until binding material solidify, wherein, soft nanocrystalline magnetic materials powder
Last Yu uncured binding material volume ratio is 1:9-9:1, and described binding material is asphalt mixtures modified by epoxy resin
Fat, paraffin wax, methyl silicone rubber, the one in Kynoar.
Embodiment 1
The biphase nanocrystalline high-frequency soft magnetic material of embodiment 1 is dilute by the 2:17 type of nano-scale
Soil-3d metal alloy R2M17Composition compound with 3d metal M, this soft magnetic materials composition R2M17:
M is 50:50 (volume ratio).
The preparation method of the biphase nanocrystalline high-frequency soft magnetic material of embodiment 1, comprises the following steps:
A) 6.7621g Nd, 21.3467g Fe and 22.5271g Co, Nd are weighed2(FeCo)17
It is 50:50 with the volume ratio of FeCo, under argon shield, is smelted into two-phase foundry alloy；
B) melt-quenching method is used to prepare amorphous state, crystalline state nanometer or amorphous and nanocrystalline mixed state
State of quenching alloy, fast quenching linear velocity is 30 meter per seconds；
C) prepared melt spun alloy carrying out ball mill crushing, concrete operations are to be existed by prepared melt spun alloy
Grind to form the granule of about 50-60 micron with agate mortar under normal hexane protection；Then by granule
100ml isopropanol and 0.2ml phthalate ester coupling agent and 0.05ml is added with planetary ball mill
Antioxidant wet grinding, wherein, coupling agent is the 2% of alloy mass, and antioxidant is alloy mass
5 ‰, ratio of grinding media to material is 20: 1, and ball milling speed is 400 revs/min, uses rotating alternately
The mode of ball milling, separating ball time consuming is 1 hour, and ball milling total time is set as 16 hours；
D) finally sample is dried, obtain Nd2(FeCo)17/ FeCo soft nanocrystalline magnetic materials powder；
E) paraffin that soft nanocrystalline magnetic materials powder and normal hexane dilute is mixed with volume ratio for 1:1
Closing uniformly, (internal diameter is 3.04mm, outward to be put into mould prepared by nonmagnetic substance after drying
Footpath is 7.00mm) in, mould is placed in baking oven 90 DEG C and is incubated 15 minutes, make paraffin melting,
Then mould being put into magnetic field to be rotationally oriented, alignment magnetic field size is 1.2 teslas, rotates speed
Degree is about 20 revs/min, continues to make sample solidify completely in 20 minutes, then under 1Mpa pressure
Compressing, finally take out test.Its X-ray diffraction spectrogram is listed in Fig. 1, high-gradient magnetism energy
See Fig. 2.
As shown in Figure 1, there are two kinds of phase structures in the material obtained by this example 1, one is pure
2: 17 type rare earth-3d metal alloy Nd2(FeCo)17Phase, another kind is pure 3d metal
M FeCo phase, through being repeatedly orientated, occurs in that Nd clearly2(FeCo)17(006)
Diffraction maximum strengthens phenomenon, and other diffraction maximum disappears substantially, and the diffraction maximum of FeCo does not occurs substantially
Change.Understand the present embodiment 1 resulting materials and there is the feature of in-plane anisotropy at normal temperatures.
As shown in Figure 2, after material is compound with paraffin, pcrmeability initial value can reach 5, resonance
Frequency has reached 7GHz, has higher on the premise of ensureing high complex permeability initial value
Resonant frequency, be a kind of good high-frequency soft magnetic material.
Comparative example 1
The soft nanocrystalline magnetic materials powder of preparation in embodiment 1 step d is diluted with normal hexane
Paraffin with volume ratio for 1:1 mix homogeneously, (internal diameter is 3.04 to put it into mould after drying
Mm, external diameter is 7.00mm) in, compressing under 1Mpa pressure, then take out test.
It is found that magnetic field rotating orientation further improves the complex permeability value of sample so that sample
Product have higher magnetic permeability value under high resonant frequency.
Embodiment 2
The biphase nanocrystalline high-frequency soft magnetic material of embodiment 2 is dilute by the 2:17 type of nano-scale
Soil-3d metal alloy R2M17Composition compound with 3d metal M, this soft magnetic materials composition R2M17:
M is 5:95 (volume ratio).
The preparation method of the biphase nanocrystalline high-frequency soft magnetic material of embodiment 2, comprises the following steps:
A) 6.2723g Nd and 43.7277g Fe, Nd are weighed2Fe17It is 5:95 with the volume ratio of Fe,
Two-phase foundry alloy it is smelted under argon shield；
B) melt-quenching method is used to prepare amorphous state, crystalline state nanometer or amorphous and nanocrystalline mixed state
State of quenching alloy, fast quenching linear velocity is 80 meter per seconds；
C) prepared melt spun alloy carrying out ball mill crushing, concrete operations are to be existed by prepared melt spun alloy
Grind to form the granule of about 50-60 micron with agate mortar under normal hexane protection；Then by granule
100ml isopropanol and 0.1ml phthalate ester coupling agent and 0.05ml is added with planetary ball mill
Antioxidant wet grinding, wherein, coupling agent is the 1% of alloy mass, and antioxidant is alloy mass
5 ‰, ratio of grinding media to material is 20: 1, and ball milling speed is 400 revs/min, uses rotating alternately
The mode of ball milling, separating ball time consuming is 1 hour, and ball milling total time is set as 16 hours；
D) finally sample is dried, obtain Nd2Fe17/ Fe soft nanocrystalline magnetic materials powder；
E) paraffin that soft nanocrystalline magnetic materials powder and normal hexane dilute is mixed with volume ratio for 1:9
Closing uniformly, (internal diameter is 3.04mm, outward to be put into mould prepared by nonmagnetic substance after drying
Footpath is 7.00mm) in, mould is placed in baking oven 90 DEG C and is incubated 15 minutes, make paraffin melting,
Then mould being put into magnetic field to be rotationally oriented, alignment magnetic field size is 0.1 tesla, rotates speed
Degree is about 5 revs/min, continues to make sample solidify completely in 20 minutes, then presses under 1Mpa pressure
Make type, finally take out test.High-gradient magnetism can be shown in Fig. 3.
From the figure 3, it may be seen that after material is compound with paraffin, pcrmeability initial value can reach 2.72,
Resonant frequency has reached 12.72GHz, has on the premise of ensureing high complex permeability initial value
There is higher resonant frequency, be a kind of good high-frequency soft magnetic material.
Embodiment 3
The biphase nanocrystalline high-frequency soft magnetic material of embodiment 3 is dilute by the 2:17 type of nano-scale
Soil-3d metal alloy R2M17Composition compound with 3d metal M, this soft magnetic materials composition R2M17:
M is 95:5 (volume ratio).
The preparation method of the biphase nanocrystalline high-frequency soft magnetic material of embodiment 1, comprises the following steps:
A) 11.6216g Nd, 38.3784g Fe, Nd are weighed2Fe17It is 95:5 with the volume ratio of Fe,
Two-phase foundry alloy it is smelted under argon shield；
B) melt-quenching method is used to prepare amorphous state, crystalline state nanometer or amorphous and nanocrystalline mixed state
State of quenching alloy, fast quenching linear velocity is 10 meter per seconds；
C) prepared melt spun alloy carrying out ball mill crushing, concrete operations are to be existed by prepared melt spun alloy
Grind to form the granule of about 50-60 micron with agate mortar under normal hexane protection；Then by granule
Crushing by airflow milling, add 0.1ml antioxidant, wherein, antioxidant is alloy mass
10‰；
D) collection obtains Nd2Fe17/ Fe soft nanocrystalline magnetic materials powder particle；
E) paraffin that soft nanocrystalline magnetic materials powder and normal hexane dilute is mixed with volume ratio for 9:1
Closing uniformly, (internal diameter is 3.04mm, outward to be put into mould prepared by nonmagnetic substance after drying
Footpath is 7.00mm) in, mould is placed in baking oven 90 DEG C and is incubated 15 minutes, make paraffin melting,
Then mould being put into magnetic field to be rotationally oriented, alignment magnetic field size is 3.0 teslas, rotates speed
Degree is about 50 revs/min, continues to make sample solidify completely in 20 minutes, then under 1Mpa pressure
Compressing, finally take out test.High-gradient magnetism can be shown in Fig. 4.
As shown in Figure 4, after material is compound with paraffin, pcrmeability initial value can reach 1.89,
Resonant frequency has reached 12.72GHz, has on the premise of ensureing high complex permeability initial value
There is higher resonant frequency, be a kind of good high-frequency soft magnetic material.
Claims (7)
1. a biphase nanocrystalline high-frequency soft magnetic material, it is characterised in that:
This soft magnetic materials is by the 2:17 type rare earth-3d metal alloy R of nano-scale2M17Composition compound with 3d metal or metal alloy M, wherein said 2:17 type rare earth-3d metal alloy R2M17Direction of easy axis vertical with C axle, this soft magnetic materials composition is by volume: 2:17 type rare earth-3d metal alloy R2M17For 5%-95%, remaining is 3d metal M；Described 2:17 type rare earth-3d metal alloy R2M17In, R is one or both in Ce, Nd, Y, Gd, Tb, Dy, Er, Tm or Lu, and M is the one in Fe, Co or Fe-Co alloy/C.
2. biphase nanocrystalline high-frequency soft magnetic material as claimed in claim 1, it is characterised in that:
Described soft magnetic materials is the 2:17 type rare earth-3d metal alloy R of the nano-scale by following structure2M17Composition compound with 3d metal or metal alloy:
Nd2(FeCo)17With FeCo；
Nd2Fe17With Fe.
3. the preparation method of a biphase nanocrystalline high-frequency soft magnetic material as claimed in claim 1, it is characterised in that:
This preparation method comprises the following steps:
A) weigh rare-earth element R and pure 3d metal M by alloy proportion, rare-earth element R and pure 3d metal M are smelted into foundry alloy under inert gas shielding, wherein 2:17 type rare earth-3d metal alloy R2M17Being 5%-95% by volume, remaining is 3d metal M；
B) melt-quenching method is used to prepare the state alloy of quenching of amorphous state, crystalline state nanometer or amorphous and nanocrystalline mixed state；
C) prepared state alloy of quenching carries out airflow milling crush or ball mill crushing process；
D) the soft nanocrystalline magnetic materials powder after pulverizing puts into, after mixing homogeneously with uncured binding material, the mould that nonmagnetic substance makes, and is placed in magnetic field rotating, until binding material solidifies.
4. the preparation method of biphase nanocrystalline high-frequency soft magnetic material as claimed in claim 3, it is characterised in that:
In step b, the linear velocity of fast melt-quenching is 10-80 meter per second.
5. the preparation method of biphase nanocrystalline high-frequency soft magnetic material as claimed in claim 3, it is characterised in that:
In step c, when using airflow milling to crush, state alloy of quenching adds the antioxidant of alloy mass 5 ‰-10 ‰, under inert gas shielding, makes average particle size 1-5 μm alloy powder through airflow milling；When using ball mill crushing, state alloy of quenching adds the antioxidant of alloy mass 5 ‰-10 ‰ and the titanate coupling agent of 1%-5% and ball-milling medium isopropanol or gasoline, state alloy of quenching is ground to the mean diameter alloy powder less than 5 μm.
6. the preparation method of biphase nanocrystalline high-frequency soft magnetic material as claimed in claim 3, it is characterised in that:
In step d, magnetic field intensity is 0.1-3 tesla, and rotary speed is 5-50 rev/min.
7. the preparation method of biphase nanocrystalline high-frequency soft magnetic material as claimed in claim 3, it is characterised in that:
In step d, soft nanocrystalline magnetic materials powder and uncured binding material volume ratio are 1:9-9:1, and described binding material is epoxy resin, paraffin wax, methyl silicone rubber, the one in Kynoar.
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| JP3470032B2 (en) * | 1997-12-22 | 2003-11-25 | 信越化学工業株式会社 | Rare earth permanent magnet material and manufacturing method thereof |
| CN1805084A (en) * | 2006-01-18 | 2006-07-19 | 哈尔滨工业大学 | Preparation method of nanometer biphase Nd2Fe14B/alpha-Fe permanent magnetic powder |
| CN101104896A (en) * | 2007-07-30 | 2008-01-16 | 浙江大学 | Fibre composite reinforcement Cu-Fe-RE alloy and preparation method thereof |
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| JP3470032B2 (en) * | 1997-12-22 | 2003-11-25 | 信越化学工業株式会社 | Rare earth permanent magnet material and manufacturing method thereof |
| CN1805084A (en) * | 2006-01-18 | 2006-07-19 | 哈尔滨工业大学 | Preparation method of nanometer biphase Nd2Fe14B/alpha-Fe permanent magnetic powder |
| CN101104896A (en) * | 2007-07-30 | 2008-01-16 | 浙江大学 | Fibre composite reinforcement Cu-Fe-RE alloy and preparation method thereof |
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