CN108305737A - A kind of compound soft magnetic material and preparation method thereof - Google Patents
A kind of compound soft magnetic material and preparation method thereof Download PDFInfo
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- CN108305737A CN108305737A CN201810090402.3A CN201810090402A CN108305737A CN 108305737 A CN108305737 A CN 108305737A CN 201810090402 A CN201810090402 A CN 201810090402A CN 108305737 A CN108305737 A CN 108305737A
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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
- H01F1/14—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 metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/14766—Fe-Si based alloys
- H01F1/14791—Fe-Si-Al based alloys, e.g. Sendust
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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- 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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Abstract
The present invention relates to a kind of compound soft magnetic materials and preparation method thereof, and the material is in Fe85Si8Al4Ni3Outside is coated with CoFe successively from the inside to the outside2O4Magnetic powder last layer after cladding and silicone layer.The present invention has both the advantages of high magnetic permeability and low core damage.The present invention can be molded when in use according to actually required shape, have a clear superiority when preparing unlike material, is easy to operate, without cutting, non waste edge, cost-effective.The synthetic method of the present invention is simple, of low cost, reaction condition is mild.Laser particle size measurement the result shows that:The Fe that aerosolization obtains85Si8Al4Ni3Powder D50 is about 36 microns.
Description
Technical field
The present invention relates to field of magnetic material, and in particular to a kind of compound soft magnetic material and preparation method thereof.
Background technology
Soft magnetic materials is to be easy magnetization and demagnetization, the low magnetic material of coercivity.Soft magnetic materials requires to have:High magnetic conductance
Rate, high saturation flux density, high resistivity, high stability, low-coercivity, low-loss, low magnetostriction coefficient and low magnetic
Anisotropic crystalline.Soft magnetic materials is widely used in various power equipments and electronic device, electric power, electronic equipment it is small-sized
Change, lightweight, it is energy saving and it is highly sensitive keep people's life more convenient, the influence to environment is smaller and smaller.In soft magnetic materials
In AC applications field, silicon steel sheet occupies very big market within a very long time.These materials have excellent magnetic in direct current
Performance, but under high-frequency ac, will be increased with the increase of frequency and rapidly along with the core damage of vortex, which limits it in height
Use under frequency.Soft magnetic ferrite is widely used in high frequency field, but haves the shortcomings that magnetic flux density is low.
Invention content
In order to solve the above technical problem, the present invention provides a kind of compound soft magnetic materials and preparation method thereof.The present invention's
Compound soft magnetic material is in Fe85Si8Al4Ni3Outside is coated with CoFe successively from the inside to the outside2O4Inorganic coating layer and silicone layer, it
It is generated using in-situ oxidation and has magnetic inorganic oxide clad to magnetic powder particles progress insulating wrapped increase resistance
Rate, to reduce core damage;Organic coating is carried out with organic siliconresin again and increase the intensity of material after molding, and at the same time playing absolutely
Edge act on and further decrease core damage, therefore, compound soft magnetic material prepared by the present invention have both high magnetic permeability and low core damage it is excellent
Point.
Scheme one)
A kind of preparation method of compound soft magnetic material:1) it is 85 according to atomic ratio by Fe powder, Si powder, Al powder and Ni powder:8:
4:3 are uniformly mixed, and are then added in vacuum atomizing stove, and setting temperature is 1800-2200 DEG C, is heated 2-3 hours, then in Ar gas
Protection is lower to be carried out making powder using gas-atomized powder method, is prepared into the Fe with high magnetic permeability85Si8Al4Ni3Powder;
2) ammonia spirit that mass fraction is 2-3% is prepared, is then added according to the ammonia spirit described in every 250-300ml
0.01mol CoCl2·6H2O, later according to every 0.01molCoCl in previous solu2·6H2100g is added in O
Fe85Si8Al4Ni3Powder stirs evenly, and above-mentioned material is added in hydrothermal reaction kettle, after keeping the temperature 1-2 hours at 170-190 DEG C
Cooled to room temperature, filter and with ethanol wash 2 times it is above after be put into 50-70 DEG C of drying of baking oven, acquisition CoFe2O4After cladding
Magnaglo;
3) it at room temperature, sequentially adds silicones, dimethylbenzene and alcohol in the reactor, after the completion of stirring and dissolving, is added
Inorganic oxide CoFe described in step 2)2O4Magnaglo after cladding, finally, by the material of above-mentioned mixing in 60-70 DEG C of constant temperature
Until solvent all evaporates to get the compound soft magnetic material;
Wherein, dimethylbenzene 2-3mL and alcohol 15-17mL is added according to every 2-3g silicones, adds according to every 2-3g silicones
Enter 100-120g CoFe2O4Magnaglo after cladding.
Scheme two)
A kind of compound soft magnetic material, the compound soft magnetic material prepared by a kind of compound soft magnetic material.
The principle of the present invention:The present invention is generated using in-situ oxidation has magnetic inorganic oxide CoFe2O4Clad is to magnetic
Property powder particle carry out insulating wrapped increase resistivity, to reduce core damage.Organic coating is carried out with organic siliconresin to be added to
The intensity of material after type, and can equally reduce core damage.Therefore, the inorganic-organic two-coat with low core damage is prepared
FeSiAlNi base compound soft magnetic materials have important practical value.
The prior art before relatively, the invention has the advantages that:
1. the FeSiAlNi base compound soft magnetic materials of the present invention have both the advantages of high magnetic permeability and low core damage.
2. especially core damage is lower in high frequency for product of the present invention.
3. the FeSiAlNi bases compound soft magnetic material of the present invention can be molded when in use according to actually required shape, preparing
It has a clear superiority when unlike material, is easy to operate, without cutting, non waste edge, cost-effective.
4. the synthetic method of the present invention is simple, of low cost, reaction condition is mild.
Specific implementation mode
Description of the drawings
Fig. 1, Fe85Si8Al4Ni3The laser particle size measurement figure of powder.
Fig. 2, Fe85Si8Al4Ni3The scanning electron microscope (SEM) photograph of powder.
The surface sweeping electron microscope of Fig. 3, product of the present invention.
Fig. 4, Fe85Si8Al4Ni3Powder surface inorganic oxide treated x-ray photoelectron spectroscopy analysis chart.(a、b、c
It is Co2p combination energy collection of illustrative plates, Fe2p combination energy collection of illustrative plates, O1s combination energy collection of illustrative plates respectively)
The hysteresis loop of Fig. 5, product of the present invention and 130i-1P.
Fig. 6, product of the present invention and the cores of 130i-1P at different frequencies damage.
The each component raw material of following embodiment is purchased from dealer.Atomization plant is Britain PSI used by experiment
The close coupling vacuum atomizing stove of company's manufacture, atomization gas are high pressure pure argon.Powder by atomization atomization belongs to machinery powder method,
It is the method for directly smashing liquid metals or alloy and powder being made, application is relatively broad.For gas-atomized powder technique, it is transmitted to
The energy of metal stream is bigger, and the powder of preparation is more tiny, and the process of gas-atomized powder is actually the mistake of droplet shape retrieval
The shape order of journey, droplet is different according to the difference at a distance from nozzle, is followed successively by cylinder, cone, slice-shaped, frenulum
Shape, spherical shape.
Embodiment 1
A kind of preparation method of compound soft magnetic material:
A kind of preparation method of compound soft magnetic material:1) it is 85 according to atomic ratio by Fe powder, Si powder, Al powder and Ni powder:8:
4:3 are uniformly mixed in addition vacuum atomizing stove, and setting temperature is 1800 DEG C, keeps the temperature 2 hours, and gas is then used under Ar gas shieldeds
Powder by atomization technique carries out spraying and powder making, is prepared into the Fe with high magnetic permeability85Si8Al4Ni3Powder;
2) ammonia spirit that mass fraction is 2% is prepared, then adds 0.01mol according to the ammonia spirit described in every 250ml
CoCl2·6H2O, later according to every 0.01molCoCl2·6H2100g Fe are added in O85Si8Al4Ni3Powder stirs evenly, will be upper
It states material to be added in hydrothermal reaction kettle, cooled to room temperature after keeping the temperature 1 hour at 170 DEG C filters and with after ethanol wash 3 times
50 DEG C of dryings of baking oven are put into, inorganic oxide CoFe is obtained2O4Magnaglo after cladding;
3) it at room temperature, sequentially adds silicones, dimethylbenzene and alcohol in the reactor, after the completion of stirring and dissolving, is added
Inorganic oxide CoFe2O4Magnaglo after cladding, finally, by the material of above-mentioned mixing in 70 DEG C of constant temperature until solvent all steams
Hair to get;
Wherein, dimethylbenzene 2mL and alcohol 15mL is added according to every 2g silicones, it is inorganic that 100g is added according to every 2g silicones
Aoxidize CoFe2O4Magnaglo after cladding.
Embodiment 2
A kind of preparation method of compound soft magnetic material:1) it is 85 according to atomic ratio by Fe powder, Si powder, Al powder and Ni powder:8:
4:3 are uniformly mixed in addition vacuum atomizing stove, and setting temperature is 2200 DEG C, keeps the temperature 3 hours, and gas is then used under Ar gas shieldeds
Powder by atomization technique carries out spraying and powder making, is prepared into the Fe with high magnetic permeability85Si8Al4Ni3Powder;
2) ammonia spirit that mass fraction is 3% is prepared, then adds 0.01mol according to the ammonia spirit described in every 300ml
CoCl2·6H2O, later according to every 0.01molCoCl2·6H2100g Fe are added in O85Si8Al4Ni3Powder stirs evenly, will be upper
It states material to be added in hydrothermal reaction kettle, cooled to room temperature after keeping the temperature 2 hours at 190 DEG C filters and with after ethanol wash 3 times
70 DEG C of dryings of baking oven are put into, inorganic oxide CoFe is obtained2O4Magnaglo after cladding;
3) it at room temperature, sequentially adds silicones, dimethylbenzene and alcohol in the reactor, after the completion of stirring and dissolving, is added
Inorganic oxide CoFe2O4Magnaglo after cladding, finally, by the material of above-mentioned mixing in 60 DEG C of constant temperature until solvent all steams
Hair to get;
Wherein, according to every 2-3g silicones be added dimethylbenzene 3mL and alcohol 17mL, according to every 3g silicones be added 120g without
Machine aoxidizes CoFe2O4Magnaglo after cladding.
Embodiment 3
A kind of preparation method of compound soft magnetic material:1) it is 85 according to atomic ratio by Fe powder, Si powder, Al powder and Ni powder:8:
4:3 are uniformly mixed in addition vacuum atomizing stove, and setting temperature is 1800-2200 DEG C, 2.5 hours is kept the temperature, then in Ar gas shieldeds
It is lower that spraying and powder making is carried out using gas-atomized powder technique, it is prepared into the Fe with high magnetic permeability85Si8Al4Ni3Powder;
2) ammonia spirit that mass fraction is 2.5% is prepared, is then added according to the ammonia spirit described in every 280ml
0.01mol CoCl2·6H2O, later according to every 0.01molCoCl2·6H2100g Fe are added in O85Si8Al4Ni3Powder, stirring
Uniformly, above-mentioned material is added in hydrothermal reaction kettle, cooled to room temperature after keeping the temperature 1-2 hours at 180 DEG C filters and uses wine
Fine purifiation is put into 60 DEG C of dryings of baking oven after washing 3 times, obtain inorganic oxide CoFe2O4Magnaglo after cladding;
3) it at room temperature, sequentially adds silicones, dimethylbenzene and alcohol in the reactor, after the completion of stirring and dissolving, is added
Inorganic oxide CoFe2O4Magnaglo after cladding, finally, by the material of above-mentioned mixing in 65 DEG C of constant temperature until solvent all steams
Hair to get;
Wherein, dimethylbenzene 2.5mL and alcohol 16mL is added according to every 2.5g silicones, is added according to every 2.5g silicones
110g inorganic oxides CoFe2O4Magnaglo after cladding.
The low core being prepared damage FeSiAlNi base compound soft magnetic materials are subjected to laser particle size measurement, as a result such as Fig. 1 institutes
Show, the Fe that aerosolization obtains85Si8Al4Ni3Powder D50 is about 36 microns.
By Fe made from step 1)85Si8Al4Ni3Powder and the low core damage FeSiAlNi base composite soft-magnetics being finally prepared
Material does scanning electron microscope, as a result as shown in Figure 2,3:The Fe that aerosolization obtains85Si8Al4Ni3The substantially spherically-shaped particle of powder, surface
Smooth, homogeneous grain diameter, but the powder rough surface and surface layer organic coating layer after coating are, it is apparent that and still keep spherical
Granule-morphology.
As shown in figure 4, x-ray photoelectron spectroscopy analysis can obtain:The chemical valence of particle surface clad after being coated after oxidation
State be respectively Co be+divalent, Fe be+trivalent, O be-divalent, show Fe85Si8Al4Ni3Particle surface is aoxidized and is generated with magnetic
The CoFe of property2O4Inorganic coating layer.
Test results are shown in figure 5 for the strong magnetic meter of vibrating example:Number with He Genasi purchases is that 130i-1P samples are opposite
Than coercivity of the invention is smaller, sensitive to external magnetic field reaction, quick, is conducive to product miniaturization.
Compression moulding, pressing pressure have been carried out to two kinds of powder of product of the present invention and 130i-1P using briquetting process
For 1200MPa, samples outer diameter 45.18mm, internal diameter 34.08mm, height is respectively 4.68mm and 4.30mm.It is molded to reduce
Caused internal stress anneals 2h to the loop sample after compression moulding under 550 DEG C, argon atmosphere, then uses coiling
Method has carried out Dynamic magnetic property test to loop sample, and test magnetic field intensity is 50mT, and test results are shown in figure 6, as a result table
It is bright:Before 50KHz, the core damage of two kinds of materials is not much different, and as frequency increases, the core damage of 130i-1P rises obviously, and
The core of FeSiAlNi base compound soft magnetic materials damages compared with 130i-1P, and gently and under high frequency core damage is lower for variation.When 100KHz,
130i-1P cores damage is 250.61W/Kg, and the core of FeSiAlNi base compound soft magnetic materials damage is only 153.74W/Kg, therewith phase
Than core damage is only the 61% of 130i-1P.Therefore, the present invention has been successfully prepared under a kind of high frequency with low core damage
FeSiAlNi base compound soft magnetic materials make it in high-frequency range using more advantage.
Claims (2)
1. a kind of preparation method of compound soft magnetic material, it is characterised in that:1) by Fe powder, Si powder, Al powder and Ni powder according to atom
Than being 85:8:4:3 are uniformly mixed, and are then added in vacuum atomizing stove, and setting temperature is 1800-2200 DEG C, is heated 2-3 hours,
Then it carries out making powder using gas-atomized powder method under Ar gas shieldeds, is prepared into the Fe with high magnetic permeability85Si8Al4Ni3Powder
End;
2) ammonia spirit that mass fraction is 2-3% is prepared, is then added according to the ammonia spirit described in every 250-300ml
0.01mol CoCl2·6H2O, later according to every 0.01molCoCl in previous solu2·6H2100g is added in O
Fe85Si8Al4Ni3Powder stirs evenly, and above-mentioned material is added in hydrothermal reaction kettle, after keeping the temperature 1-2 hours at 170-190 DEG C
Cooled to room temperature, filter and with ethanol wash 2 times it is above after be put into 50-70 DEG C of drying of baking oven, acquisition CoFe2O4After cladding
Magnaglo;
3) it at room temperature, sequentially adds silicones, dimethylbenzene and alcohol in the reactor, after the completion of stirring and dissolving, step is added
2) CoFe described in2O4Magnaglo after cladding, finally, by the material of above-mentioned mixing in 60-70 DEG C of constant temperature until solvent is whole
Evaporation is to get the compound soft magnetic material;
Wherein, dimethylbenzene 2-3mL and alcohol 15-17mL is added according to every 2-3g silicones, is added according to every 2-3g silicones
100-120g CoFe2O4Magnaglo after cladding.
2. a kind of compound soft magnetic material, it is characterised in that:By a kind of preparation method of compound soft magnetic material described in claim 1
The compound soft magnetic material of preparation.
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CN113192717A (en) * | 2021-04-22 | 2021-07-30 | 兰州大学 | Metal soft magnetic composite material and preparation method thereof |
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