CN109065318B - A method of high-frequency soft magnetic material is made based on magnetocrystalline anisotropy energy principle of cancellation - Google Patents
A method of high-frequency soft magnetic material is made based on magnetocrystalline anisotropy energy principle of cancellation Download PDFInfo
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- CN109065318B CN109065318B CN201810771555.4A CN201810771555A CN109065318B CN 109065318 B CN109065318 B CN 109065318B CN 201810771555 A CN201810771555 A CN 201810771555A CN 109065318 B CN109065318 B CN 109065318B
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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
- H01F1/12—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 soft-magnetic materials
- H01F1/33—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 soft-magnetic materials mixtures of metallic and non-metallic particles; metallic particles having oxide skin
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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
- H01F1/12—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 soft-magnetic materials
- H01F1/34—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 soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/36—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 soft-magnetic materials non-metallic substances, e.g. ferrites in the form of particles
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- 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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Abstract
The invention belongs to soft magnetic materials technical field more particularly to a kind of methods based on magnetocrystalline anisotropy energy principle of cancellation production high-frequency soft magnetic material, and general material itself has magnetocrystalline anisotropy energy, and this magnetocrystalline can bring coercivity with performance.Soft magnetic materials produced by the present invention is made of two kinds of material X1 crystal and X2 crystal, by combining both materials, is allowed the magneto-crystalline energy of different crystal orientations to offset each other, has been finally obtained the isotropic material of magneto-crystalline energy.High-frequency soft magnetic material produced by the present invention has lesser crystallite dimension, and crystallite dimension has ideal soft magnetic characteristic, and saturation magnetization is very high, up to 245emu/g generally between 1 nanometer to 1 micron.
Description
Technical field
The invention belongs to soft magnetic materials technical fields, more particularly to a kind of magnetocrystalline anisotropy energy principle of cancellation that is based on to make
The method of high-frequency soft magnetic material.
Background technique
Soft magnetic materials refers to the relatively low ferrimagnet of coercivity, including ferrite, silicon steel sheet, celestial platform alloy, non-
Crystal zone material, nanocrystalline etc. play an important role in terms of many modernizations, these materials by with
In such as power generation and transmission, motor, radio signal and microwave receiving, relay, solenoid, magnetic screen and electromagnet
In.
Soft magnetic materials only works as them by magnetizing force, such as when electric current is flowed through around the conducting wire of soft magnetic core generated magnetic
, they can just show magnetic characteristic.Soft magnetic materials usually is used to amplify related by the electric current generation circuit of magnetic flux with those.
These materials can be used in alternating current (AC) and direct current (DC) circuit.Global soft magnetic materials industry is a mature production
Industry, however, to renewable energy increasingly rely on and become to energy such as the growing interests of total energy Life cycle energy efficiency
Gesture accelerates the research of energy the relevant technologies.New improved amorphous band, nano crystal soft magnetic material are proved to be with higher
Energy efficiency.Therefore, amorphous band has been widely used as in transformer and motor magnetic core.Emerging nanocrystalline magnet core has higher
Efficiency, in future it will be appreciated that there is higher growth.
In traditional ferromagnetic material, the size of coercivity and the included crystal grain of material has relationship, and crystallite dimension must be enough
Greatly, coercivity is just smaller, can just show ideal soft magnetic characteristic in this way.So general soft magnetic materials, crystallite dimension is all
Bigger, the problem of crystallite dimension is directly brought greatly is exactly that frequency response characteristic is poor, and crystallite dimension is bigger, overturns under communicational aspects
Speed it is slower, so frequency characteristic is poorer.
Summary of the invention
In order to solve the above technical problems, the object of the present invention is to provide one kind to be based on magnetocrystalline anisotropy energy principle of cancellation system
Make the method for high-frequency soft magnetic material, there is lesser crystallite dimension, higher percent crystallization in massecuite, ideal soft magnetic characteristic, and be saturated magnetic
It is very high to change intensity.
A kind of soft magnetic materials proposed by the present invention, including two kinds of ferrimagnets, ferrimagnet are that X1 crystal and X2 are brilliant
Body, X1 crystal and X2 crystal are BCT structure, are a kind of body-centered cubic structure (the Body Center of elongation
Tetragonal), the characteristics of such BCT crystal is with the magnetic anisotropy energy along some crystallographic axis, and crystallographic axis here is used
Abc axis indicates, orthogonal between each axis, and angle is kept for 90 °, and the magnetocrystalline anisotropy energy of X1 crystal is along a axis or b axis or c-axis side
To the magnetocrystalline anisotropy energy of X2 crystal is along the plane vertical with X1 crystal magnetocrystalline anisotropy energy, by controlling X1 crystal
Size with X2 crystal is respectively 1~1000nm, and the proportion of control X1 crystal and X2 crystal makes the magnetocrystalline anisotropy energy of the two
It offsets each other, shows ideal soft magnetic characteristic.
Further, X1 crystal includes α "-Fe16N2、α”-Fe16(NC)2Or (Fe1-xZx)16N2Or (Fe1-xZx)16
(NC)2, wherein Z includes one of Ni, Co, Mn, Zn, Nd.
Further, X2 crystal includes Fe8C、Fe8O、Fe8B、Fe8Al、Fe8One of Si.
It is another object of the present invention to propose the preparation method of above-mentioned soft magnetism, use pure iron for raw material, ball milling is at iron powder, so
C, O are added afterwards2, iron oxide, ferrous oxide, B, Al or Si, continue ball milling, add ammonium nitrate or ammonium nitrate and Fe, Co or
Zn continues ball milling, is annealed to obtain soft magnetic materials after ball milling.
Further, when ball milling iron powder, 1000 revs/min to 2000 revs/min of revolving speed, ball milling 1 hour to 100 at room temperature
Hour.
Further, C, O is added2, iron oxide, ferrous oxide, after B, Al or Si, 1000 revs/min to 2000 of revolving speed
Rev/min, continue ball milling 1 hour to 100 hours at room temperature.
Further, after ammonium nitrate or ammonium nitrate and Fe, Co or Zn being added, 1000 revs/min to 2000 revs/min of revolving speed
Clock continues ball milling 1 hour to 100 hours at room temperature.
Further, annealing temperature is 150~300 DEG C.
Further, annealing gas pressure maintains 1 atmosphere and is depressed between 50 atmospheric pressure.
Further, annealing atmosphere is hydrogen or nitrogen.
Further, annealing time is 0.5 hour to 200 hours.
Further, before annealing, material is sealed with aluminium-foil paper, places into annealing furnace.
The invention also provides above-mentioned soft magnetic materials to prepare inductance, transformer, inverter, RF tag (RFID), electricity
Electrical automobile, nuclear magnetic resonance equipment, wind-power electricity generation, the application in drive motor.
The operation principle schematic diagram of soft magnetic materials produced by the present invention is as shown in Figure 3.
According to the above aspect of the present invention, the present invention has at least the following advantages: general material itself has magnetocrystalline anisotropy energy, and
This magnetocrystalline can bring coercivity with performance.Soft magnetic materials produced by the present invention is by two kinds of material X1 crystal and X2 crystal structure
At allowing the magneto-crystalline energy of different crystal orientations to offset each other, finally obtained magneto-crystalline energy respectively to same by combining both materials
The material of property.
High-frequency soft magnetic material produced by the present invention, has lesser crystallite dimension, and crystallite dimension is generally micro- at 1 nanometer to 1
Between rice, therefore there is ideal soft magnetic characteristic, and saturation magnetization is very high, up to 245emu/g.
Detailed description of the invention
Fig. 1 is soft magnetic materials magnetocrystalline anisotropy energy curve graph made from embodiment 1.
Fig. 2 is the magnetization curve of soft magnetic materials made from embodiment 1.
Fig. 3 is the operation principle schematic diagram of soft magnetic materials.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.
The person that is not specified actual conditions in embodiment, carries out according to conventional conditions or manufacturer's recommended conditions.Agents useful for same
Or production firm person is not specified in instrument, being can be with conventional products that are commercially available.
Embodiment 1
(1) starting material is pure iron, and market is directly bought, and purity is 98% to 99%, contains micro Mn or C, matter
Amount is 100 grams, and first by the method for ball milling, iron is worn into iron powder, when ball milling, using planetary ball mill, type
Number RP200,1000 revs/min of revolving speed, ball milling 20 hours under room ambient conditions；
(2) 1 gram of carbon is added into ball grinder, continues ball milling 60 hours, room temperature, 1000 revs/min of revolving speed；
(3) 0.5 gram of solid of ammonium nitrate of crystallization is added into ball grinder, continues ball milling 20 hours, room temperature, revolving speed 1000
Rev/min；
(4) material of milled is taken out from ball grinder, after being sealed with aluminium-foil paper, is put into annealing furnace and anneals, moves back
Fiery temperature is 200 DEG C, and annealing gas pressure maintains 1 atmospheric pressure, and annealing atmosphere is nitrogen, and annealing time is 4 hours；
(5) sample is taken out in the glove box full of nitrogen.
In sample, Fe16(NC)2Crystallite dimension be 100 rans, Fe8The crystallite dimension of C be 50 rans, two
The molar ratio of person is 1:1.2, and the saturation magnetization and magnetocrystalline anisotropy energy of two kinds of materials are shown in Table 1.
Table 1
| Sample | Saturation magnetization | Magnetocrystalline anisotropy energy |
| Fe16(NC)2 | 2.3μB/Fe | 1.6×107erg/cm3 |
| Fe8C | 2.1μB/Fe | -1.4×107erg/cm3 |
As it can be seen from table 1 Fe16(NC)2Saturation magnetization and Fe8The saturation magnetization of C is very close, still
Magnetocrystalline anisotropy energy is different, if we define Fe16(NC)2Magnetocrystalline anisotropy energy along c-axis direction, magnetic at this moment
Anisotropic crystalline can be positive value；According to the definition of above-mentioned crystallographic axis, Fe8The magnetocrystalline anisotropy energy of C is just along ab plane, at this time
Magnetocrystalline anisotropy energy is negative value.Since the saturation magnetization numerical value of two kinds of materials is close, the crystal structure distribution of the two and
Electron cloud state is all very close, so when the crystallite dimension of both reasonable control, if the crystal grain side between two kinds of materials
In the case that boundary's thickness is smaller, there is hydridization in the electron cloud of the two outer layer, and the electron cloud of two kinds of materials is caused phase mutual coupling occur
Cooperation is used, and is intercoupled；After coupling, original saturation magnetization is still maintained；But due to the magnetocrystalline of the two
The distribution of anisotropic energy is not identical, and in orthogonal state, the magnetocrystalline anisotropy energy that final macro manifestations come out is very low, so
Show ideal soft magnetic characteristic.
As change Fe8C and Fe16(NC)2Fig. 1 is shown in volume ratio, the influence to soft magnetic materials magnetocrystalline anisotropy energy, from Fig. 1
In as can be seen that with the two content difference, apparent become is presented in the magnetocrystalline anisotropy energy that soft magnetic materials aggregate performance goes out
Change trend, when the two content is 50% or so, magnetocrystalline anisotropy energy numerical value is reduced to zero, and corresponding is optimal soft
Magnetic characteristic.
The magnetization curve of soft magnetic materials is shown in Fig. 2, figure it is seen that the soft magnetic materials that the present embodiment is prepared has
Ideal soft magnetic characteristic, and saturation magnetization is very high, up to 245emu/g.
The expression formula of the maximum operating frequency (being also cutoff frequency) of soft magnetic materials is as follows:
Wherein, fgIt is maximum operating frequency, d represents the diameter of crystal grain, ρelResistivity is represented, μ represents magnetic conductivity, μoIt represents
Space permeability, μdcRepresent relative permeability.
Pair of maximum operating frequency corresponding to the soft magnetic materials that table 2 is prepared for conventional soft magnetic materials and the present embodiment
Than results, it can be seen that the highest frequency of soft magnetic materials produced by the present invention can reach 3000GHz, significantly larger than conventional soft magnetic
The corresponding working frequency of material.
Table 2
Table 3 is the characteristic for the soft magnetic materials that the present embodiment is prepared.
The characteristic of 3 soft magnetic materials of table
| Variable | Characterisitic parameter |
| Density | 6.9-7.0g/cm3 |
| Young's modulus | 160-200GPa |
| Curie temperature | >500℃ |
| Resistivity | 200-300μΩ-cm |
| Saturation magnetization | 245emu/g |
| Coercivity | 1-5Oe |
| Magnetic conductivity | 8000-10000 |
Although the present invention has been described by way of example and in terms of the preferred embodiments, it is not intended to limit the invention, any to be familiar with this skill
The people of art can do various change and modification, therefore protection model of the invention without departing from the spirit and scope of the present invention
Enclosing subject to the definition of the claims.
Claims (11)
1. a kind of soft magnetic materials, it is characterised in that: including two or more ferromagnetism ingredient, the ferromagnetism ingredient is
X1 crystal and X2 crystal, the X1 crystal and X2 crystal are body-centered cubic structure, and the crystallographic axis of the X1 crystal and X2 crystal is used
Abc axis indicates, orthogonal between each axis of abc axis, and angle is kept for 90 °, the magnetocrystalline anisotropy energy of the X1 crystal along a axis or
The magnetocrystalline anisotropy energy in b axis or c-axis direction, the X2 crystal is put down along vertical with the X1 crystal magnetocrystalline anisotropy energy
The size of face, the X1 crystal and X2 crystal is respectively 1~1000nm, when preparing soft magnetic materials, using certain preparation side
Method, making soft magnetic materials includes two kinds of crystal of X1 and X2, and corresponding crystallite dimension is 1-1000nm, at this point, the magnetic of two kinds of crystal
Anisotropic crystalline can be coefficient as a result, the overall magnetocrystalline opposite sex of prepared soft magnetic materials is enable to offset each other.
2. a kind of soft magnetic materials, it is characterised in that: including two kinds of ferrimagnets, the ferrimagnet is that X1 crystal and X2 are brilliant
Body, the X1 crystal and X2 crystal are body-centered cubic structure, and the crystallographic axis of the X1 crystal and X2 crystal is indicated with abc axis, abc
Orthogonal between each axis of axis, angle is kept for 90 °, the magnetocrystalline anisotropy energy of the X1 crystal along a axis or b axis or c-axis direction,
The magnetocrystalline anisotropy energy of the X2 crystal is along the plane vertical with the X1 crystal magnetocrystalline anisotropy energy, the X1 crystal
Size with X2 crystal is respectively 1~1000nm.
3. soft magnetic materials according to claim 1, it is characterised in that: X1 crystal includes α "-Fe16N2、α”-Fe16(NC)2、
(Fe1-xZx)16N2Or (Fe1-xZx)16(NC)2, wherein Z includes one of Ni, Co, Mn, Zn, Nd；X2 crystal includes Fe8C、
Fe8O、Fe8B、Fe8Al、Fe8One of Si.
4. soft magnetic materials according to claim 2, it is characterised in that: X1 crystal includes α "-Fe16N2、α”-Fe16(NC)2、
(Fe1-xZx)16N2Or (Fe1-xZx)16(NC)2, wherein Z includes one of Ni, Co, Mn, Zn, Nd；X2 crystal includes Fe8C、
Fe8O、Fe8B、Fe8Al、Fe8One of Si.
5. the preparation method of the described in any item soft magnetic materials of claim 1-4, it is characterised in that: use pure iron for raw material, ball
Iron powder is worn into, C, O is then added2, iron oxide, ferrous oxide, B, Al or Si, continue ball milling, add ammonium nitrate or nitric acid
After one of ammonium and Fe, Co, Zn, continues ball milling, annealed to obtain soft magnetic materials after ball milling.
6. the preparation method of soft magnetic materials according to claim 5, it is characterised in that: when ball milling iron powder, 1000 turns of revolving speed/
Minute to 2000 revs/min, ball milling 1 hour to 100 hours at room temperature.
7. the preparation method of soft magnetic materials according to claim 5, it is characterised in that: C, O is added2, iron oxide, oxidation it is sub-
After iron, B, Al or Si, 1000 revs/min to 2000 revs/min of revolving speed, continue ball milling 1 hour to 100 hours at room temperature.
8. the preparation method of soft magnetic materials according to claim 5, it is characterised in that: ammonium nitrate or ammonium nitrate is added
With after one of Fe, Co, Zn, 1000 revs/min to 2000 revs/min of revolving speed, continue at room temperature ball milling 1 hour to 100 small
When.
9. the preparation method of soft magnetic materials according to claim 5, it is characterised in that: annealing temperature is 150~300 DEG C,
Annealing gas pressure maintains 1 atmosphere and is depressed between 50 atmospheric pressure.
10. the preparation method of soft magnetic materials according to claim 5, it is characterised in that: annealing atmosphere be hydrogen or nitrogen,
Annealing time is 0.5 hour to 200 hours.
11. the described in any item soft magnetic materials of claim 1-4 are preparing inductance, transformer, inverter, RF tag, electronic
Automobile, nuclear magnetic resonance equipment, wind-power electricity generation, the application in drive motor.
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| JP4146769B2 (en) * | 2003-08-08 | 2008-09-10 | 日立マクセル株式会社 | Magnetic recording medium |
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