CN106601417B - A kind of core-shell structure iron silicon soft magnetism composite iron core and preparation method thereof - Google Patents
A kind of core-shell structure iron silicon soft magnetism composite iron core and preparation method thereof Download PDFInfo
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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
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
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- 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
- 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
- H01F1/20—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 in the form of particles, e.g. powder
Abstract
The invention discloses a kind of core-shell structure iron silicon soft magnetism composite iron cores and preparation method thereof, belong to iron silicon soft magnetism composite iron core technical field.The preparation method of composite iron core of the invention the steps include: that the silicon powder by the ferro-silicium powder of 90~98wt% and 2~10wt% is uniformly mixed, first under inert gas protection in 800~1150 DEG C of 1~4h of heat preservation；Then 0.5~6h is heat-treated to get the ferro-silicium composite powder of surface oxidation in 500~900 DEG C under oxidizing atmosphere；The inorganic oxide powder of the ferro-silicium composite powder of the surface oxidation of 95~98wt% and 2~5wt% is uniformly mixed, 1~10h of ball milling, compression moulding；1~20h is finally sintered at 950~1300 DEG C, furnace cooling is to get core-shell structure iron silicon soft magnetism composite iron core.Preparation method simple process of the invention, high-efficient, at low cost, the saturation induction density and magnetic conductivity of gained composite iron core are higher, iron loss is lower, and its mechanical strength is more preferable, thermal stability is higher, the service life is longer.
Description
Technical field
It is soft more specifically to a kind of core-shell structure iron silicon the invention belongs to iron silicon soft magnetism composite iron core technical field
Magnetic composite iron core and preparation method thereof.
Background technique
FeSi soft magnetic materials has unique and excellent soft magnet performance, and such as high magnetic conductivity, low magnetic hystersis loss, mangneto are stretched
Contracting coefficient has been more and more widely used almost in zero in the various fields such as telecommunications and new energy, in addition iron, silicon
Element content in the earth's crust is higher, and processing preparation is relatively easy, and cost is relatively low, therefore is constantly subjected to the extensive of domestic and international researcher
Concern.
It is well known that the soft-magnetic composite material as electromagnetic switching device, when operation, meeting is because of surrounding magnetic field
Change and generate vortex, and increases as the raising of applying frequency will lead to soft-magnetic composite material eddy-current loss.Since early stage is soft
Magnetic composite material is mainly used in low frequency, and eddy-current loss is relatively low, therefore studies it to be also just mainly focused on and how mention
Its high magnetic conductivity and it is of less demanding to iron loss.Recently as the universal of mainstream motor frequency conversion control model, high-speed rotation
The exploitation of motor, the further application of energy-saving semiconductor power device, electricity-standby frequency of use of magnetic converting means is just gradually to height
Frequencyization direction is developed, to guarantee that power electronics equipment is more energy efficient and minimizes.Therefore, the high frequency of soft-magnetic composite material how is reduced
Loss is also just at technical problem urgently to be resolved, and wherein the insulating wrapped processing of ferromagnetic particles is domestic and international researcher research
A kind of most methods.
Traditional cladding process is usually first to be passivated processing to ferromagnetic particles surface, then uses organic resin conduct
Insulating compound carries out cladding isolation to ferromagnetic particles.But when using this kind of cladding process, one side ferromagnetic particles easily with passivation
Agent reacts, to reduce insulating wrapped effect；As Chinese patent CN102360660A discloses a kind of iron silica magnetic particle core
And preparation method thereof, the iron that magnetic conductivity is 50 can be made using phosphoric acid as passivator, by binder of phenolic resin for this application
Silica magnetic particle core, but since ferro-silicium powder can generate the oxide of iron with passivator phosphatase reaction, this ferriferous oxide is half
Conductor increases loss so that the isolation effect between ferro-silicium powder particle and particle be made to decline.On the other hand, due to
Organic resin class insulating compound non-refractory, soft-magnetic composite material can only be heat-treated at a lower temperature, so as to cause soft magnetism
The relative density of composite material is lower, intensity difference, stability are difficult to ensure, and its Saturation magnetic sense intensity and relative permeability also compared with
It is low.Such as, application No. is 201310613702.2 application cases to disclose the manufacturer of a kind of iron silicon materials and 55 iron silica magnetic particle core of μ
Method, this application first use phosphoric acid solution to be passivated processing to powder, then carry out using silicone resin as insulating compound to powder exhausted
Edge cladding, molding are heat-treated under the conditions of being placed on 500 ± 30 DEG C, but since heat treatment temperature is excessively high, organic insulation agent
It decomposes substantially, so as to cause being difficult to play its insulation effect.Powder core is at work because long-term vortex heat will lead to simultaneously
Machine insulating compound aging, to influence the stability of powder core performance.
In recent years, heat of the inorganic insulation cladding due to being increasingly becoming people's research with excellent insulating properties and thermal stability
Point.Usually used inorganic insulation agent includes mica, kaolin, talcum powder, silica solution and inorganic oxide etc., wherein with inorganic
Oxide using more.It is usually when carrying out insulating wrapped processing to ferromagnetic powder using inorganic insulation agent in the prior art
By ferromagnetic powder, insulating compound and binder mix, be pressed and molded, be heat-treated after obtain soft-magnetic composite material.Such as, China is special
Benefit 201310212031.9 discloses a kind of preparation method of metal soft magnetic powder core, and this application includes raw material sieving, insulating bag
It covers, make the techniques such as magnetic powder, compression moulding, heat treatment and surface spraying to be formed, be specifically to use nano-oxide to metal
Magnetic powder carries out insulating wrapped processing, so as to be effectively improved the thermal stability of gained metal soft magnetic powder core.But using should
When kind method preparation metal soft magnetic powder core, the uniformity and thickness of inorganic insulation clad are difficult to be controlled, so as to cause institute
Soft-magnetic composite material there are still the insulating properties still lower defect of relatively poor, saturation induction density, and its iron loss is still higher.
Additionally due to not can avoid the use of binder, to increase production cost.
Summary of the invention
1. technical problems to be solved by the inivention
The purpose of the present invention, which essentially consists in, overcomes the shortcomings of that the high-frequency loss of existing iron silicon soft magnetism composite iron core is relatively high,
And a kind of core-shell structure iron silicon soft magnetism composite iron core is provided and preparation method thereof.The iron silicon being prepared using method of the invention
Soft magnetism composite iron core not only saturation induction density with higher, relative permeability and consistency, while can also effectively improve
Its insulation performance simultaneously reduces eddy-current loss.
2. technical solution
In order to achieve the above objectives, technical solution provided by the invention are as follows:
A kind of core-shell structure iron silicon soft magnetism composite iron core of the invention, the composite iron core be using ferro-silicium powder as core,
Organosilicate dielectric layer is the core-shell structure of shell, and is isolated between ferro-silicium powder particle by organosilicate dielectric layer.
Further, the organosilicate dielectric layer is MgSiO3、CaSiO3Or Al2(SiO3)3One of or it is a kind of
Above combination.
Further, the saturation induction density of the core-shell structure iron silicon soft magnetism composite iron core is 167~181emu/
G, relative permeability μ (f=100kHz, 0.3V) are 110.7~151.3, iron loss P10/1kFor 15.4~26.3W/kg, P1/10kFor
6.8~11.4W/kg, P0.5/20kFor 3.8~8.4W/kg.
A kind of preparation method of core-shell structure iron silicon soft magnetism composite iron core of the invention, first to ferro-silicium powder surface into
Row siliconising processing, then forms one layer of SiO after aoxidizing2Film, later by the ferro-silicium powder and inorganic oxide after oxidation
Carry out high temperature sintering together to get the iron silicon soft magnetism composite iron core of core-shell structure.
Further, specific step is as follows for the preparation method of core-shell structure iron silicon soft magnetism composite iron core of the invention:
Step 1: ferro-silicium powder and silicon powder are uniformly mixed, under inert gas protection to ferro-silicium powder into
Ferro-silicium powder after siliconising, is then placed under oxidizing atmosphere and carries out oxidation processes, obtain Surface Oxygen by row siliconising heat treatment
The ferro-silicium composite powder of change；
Step 2: the ferro-silicium composite powder and inorganic oxide powder of surface oxidation are uniformly mixed, then lazy
Property gas shield under carry out 1~10h of ball milling, be made with core-shell structure ferro-silicium composite powder；
Step 3: the ferro-silicium composite powder with core-shell structure is pressed under the pressure of 100~1000Mpa
Base, then green compact is placed in sintering furnace 1~15h of sintering at 950~1300 DEG C, and cool to room temperature with the furnace to get nucleocapsid knot
The iron silicon soft magnetism composite iron core of structure.
Further, in the step 1 mass percentage content of ferro-silicium powder and silicon powder be respectively 90~
98%, 2~10%, and the partial size of ferro-silicium powder is less than 150 μm, the Si content of the ferro-silicium powder is 0.5~
10wt%, the partial size of the silicon powder is less than 5 μm.
Further, the mixed-powder that ferro-silicium powder and silicon powder form is placed in 800 in the step 1~
1~4h is kept the temperature at 1150 DEG C, to carry out siliconising processing to ferro-silicium powder, the temperature of oxidation processes is 500~900
DEG C, soaking time is 0.5~6h, cools to room temperature with the furnace later to get the ferro-silicium composite powder of surface oxidation.
Further, the inorganic oxide powder in the step 2 is MgO powder, CaO powder and Al2O3In powder
One or more kinds of combinations, partial size is less than 1 μm, and the ferro-silicium composite powder and inorganic oxide of surface oxidation
The mass percentage content of powder is respectively 95~98%, 2~5%.
Further, inert gas when siliconising is handled in the step 1 uses nitrogen or argon gas, when oxidation processes
Oxidizing atmosphere use air or oxygen.
Further, the ball material mass ratio in the step 2 when ball milling is that (10~30) ︰ 1, the revolving speed of ball mill are
100~500r/min；Sintering furnace in the step 3 is the sintering furnace of vacuum protection or inert gas shielding.
3. beneficial effect
Using technical solution provided by the invention, compared with prior art, there is following remarkable result:
(1) a kind of core-shell structure iron silicon soft magnetism composite iron core of the invention, the composite iron core are to be with ferro-silicium powder
Core, organosilicate dielectric layer are the core-shell structure of shell, and are isolated between ferro-silicium powder particle by organosilicate dielectric layer,
Insulating properties between ferro-silicium powder particle is preferable, since the vortex generated when the work of iron silicon soft magnetism composite iron core can be effective
It is limited in organosilicate dielectric cladding region, to can significantly reduce the eddy-current loss and total iron loss of iron silicon soft magnetism composite iron core.
(2) preparation method of a kind of core-shell structure iron silicon soft magnetism composite iron core of the invention, using siliconising-oxidation-chemical combination
The method of cladding first forms one layer of SiO in the surface siliconising of ferro-silicium powder and after aoxidizing2Film recycles SiO2With inorganic oxygen
The combination reaction of compound at high temperature coats organosilicate dielectric layer (MgSiO on ferro-silicium powder surface3、CaSiO3Or Al2
(SiO3)3), so as to obtain the iron silicon soft magnetism composite iron core for having core-shell structure, and each ferro-silicium powder can be effectively ensured
The uniformity of last particle surface cladding insulating layer, has gained iron silicon soft magnetism composite iron core on the basis of with excellent permeability
There is lower iron loss.
(3) preparation method of a kind of core-shell structure iron silicon soft magnetism composite iron core of the invention, gained iron silicon soft magnetism compound iron
The dispersibility of ferro-silicium powder particle preferably, is isolated between ferro-silicium powder particle by organosilicate dielectric layer in core, thus
It can effectively ensure that good insulating properties between ferro-silicium powder particle.The present invention passes through to the work in siliconising and oxidation processes
Skill parameter is controlled, and is control effectively so as to the thickness to clad, and then guarantees gained iron silicon soft magnetism compound iron
The service performance of core.
(4) preparation method of a kind of core-shell structure iron silicon soft magnetism composite iron core of the invention, gained iron silicon soft magnetism compound iron
The surface of ferro-silicium powder is coated with organosilicate dielectric layer in core, to guarantee to bear higher heat treatment temperature, iron
Silicon soft magnetism composite iron core powder compact can be carried out high-temperature heat treatment, so that the relative density of iron silicon soft magnetism composite iron core obviously mentions
The content of height, the ferromagnetic material of unit volume also significantly increases, and the saturation magnetic strength of composite iron core is higher, and thermal stability is good, energy
Improve service life at higher ambient temperatures.
(5) preparation method of a kind of core-shell structure iron silicon soft magnetism composite iron core of the invention, due to not using organic adhesive
Agent and release agent improve production efficiency, and its technological operation is simple to reduce production cost and investment, to environment without
Pollution, is suitable for popularization and application.
Detailed description of the invention
Fig. 1 is a kind of hysteresis loop map of core-shell structure iron silicon soft magnetism composite iron core prepared by embodiment 1；
Fig. 2 is the relative permeability map of core-shell structure iron silicon soft magnetism composite iron core shown in FIG. 1 at different frequencies.
Specific embodiment
To further appreciate that the contents of the present invention, now in conjunction with specific embodiment, the present invention is described in detail.
To avoid repeating, the raw material Unify legislation for being first related to present embodiment is as follows, no longer superfluous in each embodiment
It states:
The partial size of the ferro-silicium powder is less than 150 μm, and the partial size of silicon powder is less than 5 μm, the grain of inorganic oxide powder
Diameter is less than 1 μm.
Embodiment 1
The preparation method of a kind of core-shell structure iron silicon soft magnetism composite iron core of the present embodiment, first to ferro-silicium powder surface
Siliconising processing is carried out, then forms one layer of SiO after aoxidizing2Film, later by the ferro-silicium powder and inorganic oxide after oxidation
Object carries out high temperature sintering together to get the iron silicon soft magnetism composite iron core of core-shell structure, the specific steps of which are as follows:
1) first the silicon powder of the ferro-silicium powder of 90wt% and 10wt% is uniformly mixed, is placed in tube furnace, in argon gas
In 800 DEG C of heat preservation 1.5h under protection, to carry out siliconising processing to ferro-silicium powder；Then by the ferro-silicium powder after siliconising
End is placed under air atmosphere and is heat-treated, and heat treatment temperature is 600 DEG C, and soaking time 0.5h cools to room temperature with the furnace, obtains
To the ferro-silicium composite powder of surface oxidation, i.e., the SiO of one layer of dense uniform is formed on the surface of ferro-silicium powder2It is thin
Film.The Si content (mass fraction) of ferro-silicium powder is 4wt% in the present embodiment.
2) the ferro-silicium composite powder and mass percentage content for the surface oxidation for being 96% by mass percentage content
It is uniformly mixed for 4% MgO powder, then ball milling 1h, ball material mass ratio are 10:1 under protection of argon gas, and drum's speed of rotation is
The ferro-silicium composite powder with core-shell structure is made in 100rpm.
3) the ferro-silicium composite powder with core-shell structure is pressed into green compact under the pressure of 100Mpa, then by green compact
It is placed in the sintering furnace of vacuum protection, is sintered 4h under the conditions of 950 DEG C, makes the SiO on ferro-silicium powder surface2Film with it is inorganic
Oxide reacts, and cools to room temperature with the furnace, can obtain core-shell structure iron silicon soft magnetism composite iron core.It is compound obtained by the present embodiment
Iron core is using ferro-silicium powder as core, MgSiO3Insulating layer is the core-shell structure of shell, and leads between ferro-silicium powder particle
Cross MgSiO3Insulating layer is isolated, and through detecting, the saturation induction of the present embodiment preparation gained iron silicon soft magnetism composite iron core is strong
Degree is 169emu/g, and relative permeability μ (f=100kHz, 0.3V) is 111.3, iron loss P10/1kFor 24.3W/kg, P1/10kFor
10.5W/kg P0.5/20kFor 7.8W/kg.Therefore, iron silicon soft magnetism composite iron core can effectively ensure that using the method for the present embodiment
With higher magnetic permcability and while excellent heat stability energy, there is lower high-frequency loss, turn so as to meet electromagnetism
The requirement that changing device develops to high frequency direction.
High-frequency loss for existing soft-magnetic composite material is relatively high, and use organic insulation agent to ferromagnetic material into
The relatively poor problem of the insulating properties and thermal stability of soft magnetism composite iron core obtained by when row insulating wrapped, recent domestic research
Person gradually switchs to research direction in the inorganic insulation cladding processing of ferrimagnet, by using inorganic insulation agent to ferromagnetism
Material carries out cladding processing can be improved the thermal stability of ferrimagnet to a certain extent.Such as Chinese patent
CN101089108A discloses a kind of metal soft magnetic powder core inorganic insulation binder and preparation method thereof, inorganic insulation bonding
Agent is by SiO2、Al2O3、ZrO2, mica powder and water mix, the preparation method of metal soft magnetic powder core includes adding metal magnetic
Enter into bichromate or bichromate and phosphatic mixed liquor and carry out surface passivating treatment, then with insulating adhesive and lubrication
Agent is dried after mixing, is pressed and molded and is obtained powder core after being heat-treated.Though this insulating adhesive is free of organic matter,
It still needs to be passivated processing to magnetic powder with the passivating solution containing chromium during preparation metal soft magnetic powder, so that environmental pollution is easily caused,
And the thickness of clad and uniformity are difficult to control when carrying out cladding processing using this method, it is still higher so as to cause its iron loss.
Chinese patent CN101599334A is using ethyl orthosilicate and ammonium hydroxide etc. as raw material, with the method for collosol and gel in iron silicon
Aluminium magnetic powder surface coats one layer of SiO2Insulating layer, but due to the heavier easy precipitating of magnetic powder in its preparation process, so as to cause magnetic powder
Surface SiO2Cladding is also uneven, therefore the insulating coating method difficulty is larger, it is difficult to guarantee the magnetic property of gained powder.Also have
Researcher attempts to carry out the processing of inorganic insulation cladding to ferromagnetic powder using the method for chemical deposition, and this method is to a certain degree
On the uniformity of clad can be improved, and coating thickness is relatively easy to control, but this method pollution is larger, at high cost, no
It is suitable for popularization and application.
Therefore, a kind of small investment, environmentally protective iron silicon soft magnetism composite iron core preparation method are developed, and guarantees gained iron
It is this several years research emphasis of inventor that silicon soft magnetism composite iron core has lower iron loss on the basis of with magnetic conductivity is increased.
Inventor finally obtains technical solution of the present invention by lot of experiments, i.e., using siliconising-oxidation-chemical combination cladding side
Method first forms one layer of SiO in the surface siliconising of ferro-silicium powder and after aoxidizing2Film, then by the ferro-silicium powder after oxidation
End is sintered together with inorganic oxide powder, can be coated a layer silicate insulating layer on ferro-silicium powder surface, be obtained
To the iron silicon soft magnetism composite iron core of core-shell structure.Since the vortex generated when the work of iron silicon soft magnetism composite iron core can be limited effectively
In organosilicate dielectric cladding region, so as to significantly reduce the eddy-current loss and total iron loss of iron silicon soft magnetism composite iron core, together
This kind of method of Shi Caiyong coats organosilicate dielectric layer on ferro-silicium powder surface, additionally it is possible to the equal of insulating layer cladding be effectively ensured
Even property solves the problems, such as that the inorganic insulation agent of ferro-silicium powder surface is difficult to be evenly coated in the prior art, is further ensured that
Gained composite iron core has lower high-frequency loss.
Meanwhile when preparing iron silicon soft magnetism composite iron core using the method for the present embodiment, in gained iron silicon soft magnetism composite iron core
The dispersibility of ferro-silicium powder particle is relatively good, is not susceptible to reunite, can pass through organosilicate dielectric layer between powder particle
It is effectively isolated, to guarantee that there is good insulating properties between ferro-silicium powder particle.And pass through the iron after aoxidizing
Silicon alloy powder carries out high temperature sintering after carrying out ball-milling treatment together with inorganic oxide again, can be further improved ferro-silicium
The uniformity of dispersibility and the particle surface cladding of powder particle.The present embodiment can be by each in control siliconising and oxidation processes
The range of technological parameter control effectively to the thickness of silicate clad, and the control is easy to operate, that is, uses the present embodiment
Preparation method, the easily tune for realizing ferro-silicium powder surface silicates coating thickness is easily-controllable, overcomes in the prior art
The deficiency that can not be control effectively to the thickness of inorganic insulation clad.Inventor is by many experiments, to siliconising and oxidation
Temperature, soaking time and the ferro-silicium powder of processing and the mixed proportion of silicon powder optimize control, make ferro-silicium powder
The thickness of surface coating layer is in optimized scope, to further ensure the service performance of gained iron silicon soft magnetism composite iron core.
Inventor also passes through many experiments and optimizes control to the range of parameter each in sintering process and the partial size of each powder, so as to
With guarantee clad compactness and its with the bond strength of powder particle.
In addition, the present embodiment is by being coated with organosilicate dielectric layer on the surface of ferro-silicium powder, to guarantee gained
Iron silicon soft magnetism composite iron core is able to bear higher heat treatment temperature, and iron silicon soft magnetism composite iron core powder compact can be carried out high warm
Processing, so that the relative density of iron silicon soft magnetism composite iron core significantly improves, the content of the ferromagnetic material of unit volume is also obvious
Increase, the saturation magnetic strength of composite iron core is higher, and thermal stability is good, can improve service life at higher ambient temperatures.And by
In the present embodiment without using organic binder and release agent, to reduce production cost and investment, production efficiency is improved,
And its technological operation is simple, no pollution to the environment is suitable for popularization and application.
Embodiment 2
A kind of preparation method of the core-shell structure iron silicon soft magnetism composite iron core of the present embodiment, the specific steps of which are as follows:
1) first the silicon powder of the ferro-silicium powder of 92wt% and 8wt% is uniformly mixed, is placed in tube furnace, protected in argon gas
1h is kept the temperature under the conditions of 850 DEG C under shield, to carry out siliconising heat treatment to ferro-silicium powder；Then the iron silicon after siliconising is closed
Bronze end is placed under oxygen atmosphere and is heat-treated, and heat treatment temperature is 500 DEG C, and soaking time 1.5h cools to room with the furnace
Temperature obtains the ferro-silicium composite powder of surface oxidation.The Si content (mass fraction) of ferro-silicium powder is in the present embodiment
2wt%.
2) CaO powder of the ferro-silicium composite powder of the surface oxidation of 95wt% and 5wt% is uniformly mixed, is then existed
Ball milling 3h under nitrogen protection, ball material mass ratio are 15:1, drum's speed of rotation 200rpm, and the iron silicon with core-shell structure is made and closes
Golden composite powder.
3) the ferro-silicium composite powder that will be provided with core-shell structure is pressed into green compact under the pressure of 300Mpa, then by green compact
It is placed in the sintering furnace of vacuum protection, is sintered 1h under the conditions of 1050 DEG C, cools to room temperature with the furnace, core-shell structure iron silicon can be obtained
Soft magnetism composite iron core.
Composite iron core obtained by the present embodiment is using ferro-silicium powder as core, CaSiO3Insulating layer is the core-shell structure of shell,
And pass through CaSiO between ferro-silicium powder particle3Insulating layer is isolated, and through detecting, the present embodiment preparation gained iron silicon is soft
The saturation induction density of magnetic composite iron core is 167emu/g, and relative permeability μ (f=10kHz, 0.3V) is 110.7, iron loss
P10/1kFor 26.3W/kg, P1/10kFor 11.4W/kg, P0.5/20kFor 8.4W/kg.
Embodiment 3
A kind of preparation method of the core-shell structure iron silicon soft magnetism composite iron core of the present embodiment, the specific steps of which are as follows:
1) first the silicon powder of the ferro-silicium powder of 93wt% and 7wt% is uniformly mixed, is placed in tube furnace, protected in nitrogen
2.5h is kept the temperature under the conditions of 950 DEG C under shield, to carry out siliconising heat treatment to ferro-silicium powder；Then by the iron silicon after siliconising
Alloy powder is placed under oxygen atmosphere and is heat-treated, and heat treatment temperature is 750 DEG C, and soaking time 3h cools to room with the furnace
Temperature obtains the ferro-silicium composite powder of surface oxidation.The Si content (mass fraction) of ferro-silicium powder is in the present embodiment
0.5wt%.
2) by the ferro-silicium composite powder of the surface oxidation of 98wt% and the Al of 2wt%2O3Powder is uniformly mixed, then
Ball milling 4h under protection of argon gas, ball material mass ratio are 25:1, drum's speed of rotation 350rpm, and the iron silicon with core-shell structure is made
Alloy composite powder.
3) the ferro-silicium composite powder with core-shell structure is pressed into green compact under the pressure of 500Mpa, then by green compact
It is placed in the sintering furnace of inert gas shielding, is sintered 8h under the conditions of 1150 DEG C, cools to room temperature with the furnace, core-shell structure can be obtained
Iron silicon soft magnetism composite iron core.
Composite iron core obtained by the present embodiment is using ferro-silicium powder as core, Al2(SiO3)3Insulating layer is the nucleocapsid knot of shell
Structure, and pass through Al between ferro-silicium powder particle2(SiO3)3Insulating layer is isolated.Through detecting, the present embodiment preparation gained
The saturation induction density of core-shell structure iron silicon soft magnetism composite iron core be 172emu/g, relative permeability μ (f=100kHz,
It 0.3V) is 140.1, iron loss P10/1kFor 22.5W/kg, P1/10kFor 8.9W/kg, P0.5/20kFor 6.2W/kg.
Embodiment 4
A kind of preparation method of the core-shell structure iron silicon soft magnetism composite iron core of the present embodiment, the specific steps of which are as follows:
1) first the silicon powder of the ferro-silicium powder of 94wt% and 6wt% is uniformly mixed, is placed in tube furnace, protected in nitrogen
3h is kept the temperature under the conditions of 980 DEG C under shield, to carry out siliconising heat treatment to ferro-silicium powder；Then the iron silicon after siliconising is closed
Bronze end is placed under air atmosphere and is heat-treated, and heat treatment temperature is 900 DEG C, and soaking time 3.5h cools to room with the furnace
Temperature obtains the ferro-silicium composite powder of surface oxidation.The Si content (mass fraction) of ferro-silicium powder is in the present embodiment
10wt%.
2) (MgO+CaO) powder of the ferro-silicium composite powder of the surface oxidation of 97wt% and 3wt% are uniformly mixed,
Then ball milling 5h, ball material mass ratio are 30:1, drum's speed of rotation 500rpm under protection of argon gas, are made with core-shell structure
Ferro-silicium composite powder.
3) the ferro-silicium composite powder that will be provided with core-shell structure is pressed into green compact under the pressure of 700Mpa, then by green compact
It is placed in the sintering furnace of inert gas shielding, is sintered 15h under the conditions of 1300 DEG C, cools to room temperature with the furnace, nucleocapsid knot can be obtained
Structure iron silicon soft magnetism composite iron core.
Composite iron core obtained by the present embodiment is using ferro-silicium powder as core, (MgSiO3+CaSiO3) insulating layer be shell core
Shell structure, and pass through (MgSiO between ferro-silicium powder particle3+CaSiO3) insulating layer is isolated.Through detecting, the present embodiment
The saturation induction density of preparation gained iron silicon soft magnetism composite iron core is 170emu/g；Relative permeability μ (f=100kHz,
It 0.3V) is 134.6；Iron loss P10/1kFor 22W/kg, P1/10kFor 7.2W/kg, P0.5/20kFor 5.2W/kg.
Embodiment 5
A kind of preparation method of the core-shell structure iron silicon soft magnetism composite iron core of the present embodiment, the specific steps of which are as follows:
1) first the silicon powder of the ferro-silicium powder of 95wt% and 5wt% is uniformly mixed, is placed in tube furnace, protected in nitrogen
3.5h is kept the temperature under the conditions of 1050 DEG C under shield；Then it is heat-treated in air atmosphere, heat treatment temperature is 550 DEG C, heat preservation
Time is 5.5h, cools to room temperature with the furnace, obtains the ferro-silicium composite powder of surface oxidation.Ferro-silicium powder in the present embodiment
The Si content (mass fraction) at end is 7wt%.
2) by the ferro-silicium composite powder of the surface oxidation of 95wt% and the (MgO+Al of 5wt%2O3) powder mixing is
Even, then ball milling 6h, ball material mass ratio are 18:1, drum's speed of rotation 250rpm under nitrogen protection, and being made has nucleocapsid knot
The ferro-silicium composite powder of structure.
3) the ferro-silicium composite powder that will be provided with core-shell structure is pressed into green compact under the pressure of 1000Mpa, then will pressure
Base is placed in the sintering furnace of inert gas shielding, is sintered 10h under the conditions of 1000 DEG C, is cooled to room temperature with the furnace, can obtain nucleocapsid
Structural iron silicon soft magnetism composite iron core.
Composite iron core obtained by the present embodiment is using ferro-silicium powder as core, (MgSiO3+Al2(SiO3)3) insulating layer be shell
Core-shell structure, and between ferro-silicium powder particle pass through (MgSiO3+Al2(SiO3)3) insulation layer insulating be isolated.
Through detecting, the saturation induction density of the present embodiment preparation gained core-shell structure iron silicon soft magnetism composite iron core is 175emu/g；Phase
It is 128.6 to magnetic permeability μ (f=100kHz, 0.3V)；Iron loss P10/1kFor 17.6W/kg, P1/10kFor 8.4W/kg, P0.5/20kFor
4.5W/kg。
Embodiment 6
A kind of preparation method of the core-shell structure iron silicon soft magnetism composite iron core of the present embodiment, the specific steps of which are as follows:
1) first the silicon powder of the ferro-silicium powder of 96wt% and 4wt% is uniformly mixed, is placed in tube furnace, protected in argon gas
4h is kept the temperature under the conditions of 1100 DEG C under shield；Then it is heat-treated in air atmosphere, heat treatment temperature is 870 DEG C, when heat preservation
Between be 6h, cool to room temperature with the furnace, obtain the ferro-silicium composite powder of surface oxidation.Ferro-silicium powder in the present embodiment
Si content (mass fraction) is 8wt%.
2) by (CaO+Al of the ferro-silicium composite powder and 2wt% through surface oxidation of 98wt%2O3) powder mixing is
Even, then ball milling 7h, ball material mass ratio are 13:1, drum's speed of rotation 410rpm under nitrogen protection, and being made has nucleocapsid knot
The ferro-silicium composite powder of structure.
3) the ferro-silicium composite powder that will be provided with core-shell structure is pressed into green compact under the pressure of 400Mpa, then by green compact
It is placed in the sintering furnace of vacuum protection, is sintered 5h under the conditions of 1100 DEG C, cools to room temperature with the furnace, core-shell structure iron silicon can be obtained
Soft magnetism composite iron core.
Composite iron core obtained by the present embodiment is using ferro-silicium powder as core, (CaSiO3+Al2(SiO3)3) insulating layer be shell
Core-shell structure, and between ferro-silicium powder particle pass through (CaSiO3+Al2(SiO3)3) insulating layer is isolated.Through detecting,
The saturation induction density of the present embodiment preparation gained core-shell structure iron silicon soft magnetism composite iron core is 181emu/g (such as Fig. 1 institute
Show)；Relative permeability μ (f=100kHz, 0.3V) is 151.3；Iron loss P10/1kFor 15.4W/kg, P1/10kFor 6.8W/kg,
P0.5/20kFor 3.8W/kg.
Embodiment 7
A kind of preparation method of the core-shell structure iron silicon soft magnetism composite iron core of the present embodiment, the specific steps of which are as follows:
1) first the silicon powder of the ferro-silicium powder of 97wt% and 3wt% is uniformly mixed, is placed in tube furnace, protected in argon gas
1.2h is kept the temperature under the conditions of 1150 DEG C under shield；Then it is heat-treated under oxygen atmosphere, heat treatment temperature is 720 DEG C, heat preservation
Time is 1.4h, cools to room temperature with the furnace, obtains the ferro-silicium composite powder of surface oxidation.Ferro-silicium powder in the present embodiment
The Si content (mass fraction) at end is 10wt%.
2) by (MgO+CaO+Al of the ferro-silicium composite powder and 4.5wt% through surface oxidation of 95.5wt%2O3) mixed
It closing powder to be uniformly mixed, then ball milling 8.5h under protection of argon gas, ball material mass ratio is 29:1, drum's speed of rotation 240rpm,
The ferro-silicium composite powder with core-shell structure is made.
3) the ferro-silicium composite powder that will be provided with core-shell structure is pressed into green compact under the pressure of 800Mpa, then by green compact
It is placed in the sintering furnace of inert gas shielding, is sintered 15h under the conditions of 970 DEG C, cools to room temperature with the furnace, core-shell structure can be obtained
Iron silicon soft magnetism composite iron core.
Composite iron core obtained by the present embodiment is using ferro-silicium powder as core, (MgSiO3+CaSiO3+Al2(SiO3)3) compound
Insulating layer is the core-shell structure of shell, and passes through (MgSiO between ferro-silicium powder particle3+CaSiO3+Al2(SiO3)3) compound exhausted
Edge layer is isolated.Through detecting, the saturation induction density of the present embodiment preparation gained core-shell structure iron silicon soft magnetism composite iron core
For 175emu/g；Relative permeability μ (f=100kHz, 0.3V) is 140.4；Iron loss P10/1kFor 20.2W/kg, P1/10kFor 8.2W/
Kg, P0.5/20kFor 6W/kg.
Embodiment 8
A kind of preparation method of the core-shell structure iron silicon soft magnetism composite iron core of the present embodiment, the specific steps of which are as follows:
1) first the silicon powder of the ferro-silicium powder of 98wt% and 2wt% is uniformly mixed, is placed in tube furnace, protected in nitrogen
2.2h is kept the temperature under the conditions of 1070 DEG C under shield；Then it is heat-treated under oxygen atmosphere, heat treatment temperature is 640 DEG C, heat preservation
Time is 4.7h, cools to room temperature with the furnace, obtains the ferro-silicium composite powder of surface oxidation.Ferro-silicium powder in the present embodiment
The Si content (mass fraction) at end is 3wt%.
2) the MgO powder of the ferro-silicium composite powder and 2.5wt% through surface oxidation of 97.5wt% is uniformly mixed,
Then ball milling 10h, ball material mass ratio are 16:1, drum's speed of rotation 500rpm under nitrogen protection, and being made has core-shell structure
Ferro-silicium composite powder.
3) the ferro-silicium composite powder that will be provided with core-shell structure is pressed into green compact under the pressure of 200Mpa, then by green compact
It is placed in the sintering furnace of vacuum protection, is sintered 14h under the conditions of 1250 DEG C, cools to room temperature with the furnace, core-shell structure iron can be obtained
Silicon soft magnetism composite iron core.
The present embodiment preparation gained composite iron core is using ferro-silicium powder as core, MgSiO3Insulating layer is the nucleocapsid knot of shell
Structure, and pass through MgSiO between ferro-silicium powder particle3Insulating layer is isolated.Through detecting, iron silicon soft magnetism obtained by the present embodiment
The saturation induction density of composite iron core is 172emu/g；Relative permeability μ (f=100kHz, 0.3V) is 119.0；Iron loss
P10/1kFor 25.4W/kg, P1/10kFor 7.8W/kg, P0.5/20kFor 7.6W/kg.
In conjunction with the embodiments 1-8 it can be concluded that, can be prepared into using method of the invention and provide high magnetic strength, high-densit
Degree, good insulating performance, low iron loss and excellent heat stability iron silicon soft magnetism composite iron core, gained iron silicon soft magnetism composite iron core
Saturation induction density is 167~181emu/g；Relative permeability μ (f=100kHz, 0.3V) is 110.7~151.3；Iron loss
P10/1kFor 15.4~26.3W/kg, P1/10kFor 6.8~11.4W/kg, P0.5/20kFor 3.8~8.4W/kg, and its preparation process letter
Single, small investment, high production efficiency, no pollution to the environment can satisfy what existing electromagnetic switching device developed to high frequency direction
Requirement, and be suitable for popularization and application.
Claims (9)
1. a kind of preparation method of core-shell structure iron silicon soft magnetism composite iron core, it is characterised in that: first to ferro-silicium powder surface
Siliconising processing is carried out, then forms one layer of SiO after aoxidizing2Film, later by the ferro-silicium powder and inorganic oxide after oxidation
Object carries out high temperature sintering together to get the iron silicon soft magnetism composite iron core of core-shell structure, and the inorganic oxide powder is MgO powder
End, CaO powder and Al2O3One of powder or more than one combination.
2. a kind of preparation method of core-shell structure iron silicon soft magnetism composite iron core according to claim 1, it is characterised in that: institute
Composite iron core is stated as the core-shell structure using ferro-silicium powder as core, organosilicate dielectric layer for shell, and ferro-silicium powder particle
Between be isolated by organosilicate dielectric layer, the organosilicate dielectric layer be MgSiO3、CaSiO3Or Al2(SiO3)3In
One or more kinds of combinations.
3. a kind of preparation method of core-shell structure iron silicon soft magnetism composite iron core according to claim 2, it is characterised in that: institute
The saturation induction density for stating core-shell structure iron silicon soft magnetism composite iron core is 167 ~ 181emu/g, at f=100kHz, 0.3V
Relative permeability μ be 110.7 ~ 151.3, iron loss P10/1kFor 15.4 ~ 26.3W/kg, P1/10kFor 6.8 ~ 11.4W/kg, P0.5/20k
For 3.8 ~ 8.4W/kg.
4. a kind of preparation method of core-shell structure iron silicon soft magnetism composite iron core according to claim 1, which is characterized in that its
Specific step is as follows:
Step 1: ferro-silicium powder and silicon powder are uniformly mixed, ferro-silicium powder is seeped under inert gas protection
Ferro-silicium powder after siliconising, is then placed under oxidizing atmosphere and carries out oxidation processes, obtain surface oxidation by silicon heat treatment
Ferro-silicium composite powder；
Step 2: the ferro-silicium composite powder and inorganic oxide powder of surface oxidation are uniformly mixed, then in indifferent gas
Body protection is lower to carry out 1 ~ 10h of ball milling, and the ferro-silicium composite powder with core-shell structure is made；
Step 3: the ferro-silicium composite powder with core-shell structure is pressed into base under the pressure of 100 ~ 1000Mpa, then will
Green compact is placed in sintering furnace is sintered 1 ~ 15h at 950 ~ 1300 DEG C, and it is soft to get the iron silicon of core-shell structure to cool to room temperature with the furnace
Magnetic composite iron core.
5. a kind of preparation method of core-shell structure iron silicon soft magnetism composite iron core according to claim 4, it is characterised in that: institute
Stating the mass percentage content of ferro-silicium powder and silicon powder in step 1 is respectively 90 ~ 98%, 2 ~ 10%, and ferro-silicium powder
Partial size less than 150 μm, the Si content of the ferro-silicium powder is 0.5 ~ 10wt%, and the partial size of the silicon powder is less than 5 μm.
6. a kind of preparation method of core-shell structure iron silicon soft magnetism composite iron core according to claim 4 or 5, feature exist
In: the mixed-powder that ferro-silicium powder and silicon powder form is placed in 1 ~ 4h of heat preservation at 800 ~ 1150 DEG C in the step 1, from
And siliconising processing is carried out to ferro-silicium powder, the temperature of oxidation processes is 500 ~ 900 DEG C, and soaking time is 0.5 ~ 6h, it
Cool to room temperature with the furnace afterwards to get the ferro-silicium composite powder of surface oxidation.
7. a kind of preparation method of core-shell structure iron silicon soft magnetism composite iron core according to claim 6, it is characterised in that: institute
The partial size of the inorganic oxide powder in step 2 is stated less than 1 μm, and the ferro-silicium composite powder of surface oxidation and inorganic oxygen
The mass percentage content of compound powder is respectively 95 ~ 98%, 2 ~ 5%.
8. a kind of preparation method of core-shell structure iron silicon soft magnetism composite iron core according to claim 7, it is characterised in that: institute
Inert gas when siliconising in step 1 is handled is stated using nitrogen or argon gas, oxidizing atmosphere when oxidation processes uses air or oxygen
Gas.
9. a kind of preparation method of core-shell structure iron silicon soft magnetism composite iron core according to claim 7, it is characterised in that: institute
Ball material mass ratio when stating ball milling in step 2 is that (10 ~ 30) ︰ 1, the revolving speed of ball mill are 100 ~ 500r/min；The step 3
In sintering furnace be vacuum protection or inert gas shielding sintering furnace.
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