CN106583709A - Iron silicon alloy composite powder of core-shell structure and preparation method thereof - Google Patents
Iron silicon alloy composite powder of core-shell structure and preparation method thereof Download PDFInfo
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Abstract
The invention discloses iron silicon alloy composite powder of a core-shell structure and a preparation method thereof and belongs to the technical field of soft magnet composite materials. The internal core of the iron silicon alloy composite powder is composed of iron silicon soft magnet particles, and the outer layers of the soft magnet particles are each wrapped with a layer of dense Al2O3. The preparation method of the composite powder includes the specific steps that iron silicon alloy powder, aluminum powder, ammonium chloride powder and aluminum oxide powder are uniformly mixed, protected by inert gas and subjected to heat treatment for 0.5-5 hours at the temperature of 300-1250 DEG C, and the mixture is cooled to room temperature along with a furnace; then the mixture is placed in an oxidizing atmosphere, and subjected to temperature preservation for 1-3 hours at the temperature of 200-500 DEG C, and the mixture is cooled along with the furnace; and finally, the iron silicon alloy composite powder of the core-shell structure is obtained through ultrasonic cleaning, magnetic separation and vacuum drying. The iron silicon alloy composite powder prepared through the method is high in electrical resistivity, low in loss, good in heat stability and capable of meeting the use requirement of electricity-magnet conversion equipment for development towards high frequency.
Description
Technical field
The invention belongs to soft-magnetic composite material technical field, more particularly, it relates to a kind of iron silicon for possessing core shell structure
Alloy composite powder and preparation method thereof.
Background technology
Metal magnetic powder core be mixed with dielectric by magnetic material powder after, by powder metallurgical production technique prepare
Soft-magnetic composite material.Because the Surface coating of ferromagnetic powder particle one layer of dielectric insulating film, its resistivity ratio alloy is big to be obtained
It is many, therefore eddy-current loss is little, can use at higher frequencies, the inductor filter being widely used at present in telecommunication products
Device, choking-winding and Switching Power Supply iron core, and become one of important component part of soft magnetic materials.In recent years, with main flow electricity
Popularization, the exploitation of high-speed rotation motor and the further application of energy-saving semiconductor power device of machine VFC pattern,
Electricity-standby usage frequency of magnetic converting means just gradually develops to high frequency direction, to ensure power electronics equipment more energy-conservation and little
Type.
Powder core mainly have ferromagnetic powder core, iron-silicon-aluminualloy alloy magnetic powder core, iron-nickel alloy powder core, ferrum-silicon alloy magnetic powder core,
Permalloy powder core etc..Wherein, ferrum-silicon alloy magnetic powder core is used as a kind of NEW TYPE OF COMPOSITE electronic material, due to good full
And the characteristics of magnetic induction intensity, excellent DC superposition characteristic, good temperature stability, low-loss and low cost, quickly
Grow up, and the anti-current device under high current, the power inductor of high energy storage and solar energy, wind energy, hybrid vehicle etc.
It is widely applied in new energy field.Early stage powder core is only required with higher magnetic conductance because operating frequency is than relatively low
Rate and to low-loss require it is not high.But with the applying frequency more and more higher of iron silica magnetic particle core, how to ensure powder core in tool
In the case of having high magnetic permeability, its iron loss is reduced into outstanding problem, this is also the master for limiting iron silica magnetic particle core application at present
Want a difficult problem.
At present, the research both at home and abroad with regard to metal magnetic powder core mainly passes through to select the bag of suitable insulating compound and insulating compound
The methods such as coating process are improving the magnetic property of powder core, and the preparation method of existing metal magnetic powder core usually adopts phosphoric acid, chromium
The acid solutions such as acid are passivated after process to magnetic, add insulating compound, resinae organic binder bond and releasing agent to be well mixed
Jing compression moldings, obtain powder core after heat treatment.Such as, China Patent No. discloses a kind of iron for the application case of CN104233055A
The manufacture method of silicon materials and iron silica magnetic particle core, the manufacture of its iron silica magnetic particle core includes alloy melting, broken, sub-sieve, at surface
Reason, insulating wrapped, plus the operation such as lubricant, compressing, heat treatment, intensive treatment, this application case is first molten using phosphoric acid
Liquid carries out Dunhua process to magnetic, then carries out cladding process to magnetic using silicones organic binder bond.But using above-mentioned side
The iron silica magnetic particle core that method is prepared is coated on magnetic surface when (600-700 DEG C) is heat-treated under higher temperature conditions
Organic insulation agent easily thermally decompose and be carbonized, so as to cause insulating properties decline, high-gradient magnetism can not good, eddy-current loss compared with
Greatly, so affect magnetic core performance stability.And for example, Chinese patent CN201210095855.8 discloses a kind of iron silicon materials
And the manufacture method of the iron silica magnetic particle cores of μ 90, this application case matched somebody with somebody by alloy melting, powder processed, powder reduction, powder classification, granularity
Powder core is prepared than steps such as, powder passivation, insulating wrapped, compression molding, heat treatment and face coats, using party's legal system
The standby iron silica magnetic particle core for obtaining can reduce to a certain extent its core loss, but its operating procedure is relative complex.Additionally, adopting
The passivating solution for being adopted in aforementioned manners or insulating bag covering liquid generally all containing phosphorus or chromium, easily pollute environment, cost of material
Also it is higher.
Therefore, recent domestic researcher begins one's study and replace organic insulation agent to enter powder core using inorganic insulation agent
Row cladding process, conventional inorganic insulation agent includes inorganic phosphate (zinc phosphoric acid, iron phosphate and manganese phosphoric acid), silicate and nothing
Machine oxide etc., wherein most with the application of inorganic insulation agent.Typically by ferromagnetic powder and inorganic insulation in existing research
Agent and binding agent mix, subsequent die forming, and thermally treated acquisition powder core.Such as, Chinese patent CN101089108A is disclosed
A kind of metal soft magnetic powder core inorganic insulation bonding agent and preparation method thereof, this application case is directly using inorganic oxide to iron
Based soft magnetic powder surface carries out insulating wrapped, and heat is steady when carrying out coating process using organic insulation agent such that it is able to be prevented effectively from
Qualitative poor deficiency, but the method using this application case is difficult to ensure that the uniformity that the agent of ferromagnetic particle surface insulation is coated,
So as to cause the insulating properties and stability of product relatively poor, quality is unstable, and its iron loss is still higher.
In sum, the weak point for how overcoming above-mentioned prior art to exist, works out a kind of magnetic conductivity height, iron loss
The excellent ferro-silicium composite powder of little and thermal stability is most important for electricity-standby development of magnetic converting means.
The content of the invention
1. the invention technical problem to be solved
It is an object of the invention to overcome the shortcomings of that above-mentioned prior art is present, there is provided a kind of iron for possessing core shell structure
Silicon alloy composite powder and preparation method thereof.Ensure that ferro-silicium composite powder has using the preparation method of the present invention
While higher electric resistivity, its iron loss can be significantly reduced, the iron loss of gained ferro-silicium composite powder is relatively low, and with compared with
Good heat endurance.
2. technical scheme
To reach above-mentioned purpose, the technical scheme that the present invention is provided is：
A kind of preparation method of ferro-silicium composite powder for possessing core shell structure of the present invention, first passes through heat treatment to iron
Silicon alloy powder carries out aluminising process, then the ferro-silicium powder after aluminising is carried out into oxidation processes, and Jing after magnetic separation is processed
Obtain the ferro-silicium composite powder for possessing core shell structure.
Further, the preparation method of the ferro-silicium composite powder for possessing core shell structure of the invention, its concrete step
It is rapid as follows：
Step one, ferro-silicium powder, aluminium powder, ammonium chloride powder and alumina powder are well mixed and obtain mixed powder
End, mixed-powder is heat-treated under inert gas shielding, and it is 300～1250 DEG C to control heat treatment temperature, temperature retention time
For 0.5～5h, room temperature is then cooled to the furnace, obtain ferro-silicium powder after heat treatment；
Step 2, ferro-silicium powder after heat treatment is placed under oxidizing atmosphere carries out oxidation processes, control oxidation
Treatment temperature is 200～500 DEG C, and temperature retention time is 1～3h, then naturally cools to room temperature with stove, obtains final product the iron silicon after oxidation
Soft magnetic composite powder；
Step 3, gained is aoxidized after iron silicon soft magnetic composite powder carry out at ultrasonic wave cleaning, magnetic separation and vacuum drying
Reason, that is, obtain the ferro-silicium composite powder for possessing core shell structure.
Further, the mass percent of each component is as follows in gained mixed-powder in the step one：Ferro-silicium
80～90wt% of powder, 0.5～2.5wt% of aluminium powder, ammonium chloride 0.1～0.5wt% of powder, 7～19.4wt% of alumina powder.
Further, gained ferro-silicium composite powder be core shell structure, its inner core be iron silicon soft magnetic particles, its shell
Layer is Al2O3Insulating barrier, and Al2O3Insulating barrier is equably wrapped in the surface of iron silicon soft magnetic particles.
Further, the Si contents of the ferro-silicium powder are 0.5～7.5wt%.
Further, NH in the ammonium chloride powder4The mass percentage content of Cl is more than 99.5%, the aluminum oxide
Al in powder2O3Mass percentage content be more than 99%.
Further, the particle diameter of the aluminium powder is less than 1 μm, and the mass percentage content of Al is more than in aluminium powder
99.5%.
Further, the inert gas in the step one using argon gas or nitrogen, adopt by the oxidizing atmosphere in step 2
Use air or oxygen.
Further, the time of ultrasonic wave cleaning is 0.1～1h in the step 4.
A kind of ferro-silicium composite powder for possessing core shell structure of the present invention, the composite powder is the tool using the present invention
What the preparation method of the ferro-silicium composite powder of standby core shell structure was prepared.
3. beneficial effect
The technical scheme provided using the present invention, compared with prior art, with following remarkable result：
(1) preparation method of a kind of ferro-silicium composite powder for possessing core shell structure of the invention, after first aluminising
The mode of oxidation can prepare the ferro-silicium composite powder for possessing core shell structure, and the surface of iron silicon soft magnetic particles is uniformly wrapped
It is covered with the Al of densification2O3Insulating barrier, thereby may be ensured that ferro-silicium composite powder has while with higher magnetic permcability excellent
Good thermal stability and relatively low iron loss, and then disclosure satisfy that the standby use demand to high frequency development of electricity-magnetic converting means.
(2) preparation method of a kind of ferro-silicium composite powder for possessing core shell structure of the invention, it adopts Al2O3Absolutely
Edge layer carries out cladding process to ferro-silicium material, it is to avoid the use of organic insulation agent in prior art, greatly reduces life
Cost and investment are produced, and ferro-silicium composite powder that can be at relatively high temperatures to possessing core shell structure is heat-treated, after being
It is continuous obtain with high-compactness, heat endurance is good, non-oxidizability is strong, the iron silicon magnetic that can work at higher ambient temperatures for a long time
Powder core carries out raw material guarantee.
(3) preparation method of a kind of ferro-silicium composite powder for possessing core shell structure of the invention, by each technique
In technological parameter, the heat treatment temperature, temperature retention time and oxidation temperature and oxidization time when especially aluminising is processed
Control is optimized, such that it is able to ferro-silicium powder surface A l2O3The thickness of insulating barrier control effectively, it is ensured that gained
The performance of ferro-silicium powder.
(4) preparation method of a kind of ferro-silicium composite powder for possessing core shell structure of the invention, its preparation technology letter
It is single, production efficiency, and environmentally safe are improve, cost of material is relatively low, is suitable to promote the use of.
(5) a kind of ferro-silicium composite powder for possessing core shell structure of the invention, excellent by carrying out to its preparation technology
Change design such that it is able to make iron silicon soft magnetic particles coated with uniform have Al2O3Insulating barrier, and then cause ferro-silicium composite powder
The resistivity at end is high, it is good that low, heat endurance is lost.
Description of the drawings
Fig. 1 is the XRD spectrum of the ferro-silicium composite powder for possessing core shell structure in embodiment obtained by preparation.
Specific embodiment
To further appreciate that present disclosure, in conjunction with specific embodiment, the present invention is described in detail.While in order to
Avoid repeating, it is first that the raw material Unify legislation being related in each embodiment is as follows, repeat no more in embodiment：
The aluminium powder particle diameter is less than 1 μm, and the purity (mass percentage content of Al in aluminium powder) of aluminium powder is more than
99.5wt%；
The purity of the ammonium chloride powder is more than 99.5wt%, and the purity of alumina powder is more than 99wt%.
Embodiment 1
A kind of preparation method of ferro-silicium composite powder for possessing core shell structure of the present embodiment, first passes through heat treatment right
Ferro-silicium powder carries out aluminising process, then the ferro-silicium powder after aluminising is carried out into oxidation processes, and Jing magnetic separation is processed
Obtain the ferro-silicium composite powder for possessing core shell structure afterwards, the preparation method is comprised the following steps that：
Step one, first by the ferro-silicium powder of 80wt%, the aluminium powder of 0.5wt%, the ammonium chloride powder of 0.1wt% and
The alumina powder of 19.4wt% is well mixed, then by described mixed-powder be placed at argon gas protection under carry out at high warm
Reason, high-temperature heat treatment temperature setting is 300 DEG C, and temperature retention time is 5h, cools to room temperature with the furnace, obtains iron silicon after heat treatment
Alloy powder, the Si contents of ferro-silicium powder are 0.5wt% in the present embodiment.
Step 2, the ferro-silicium powder by gained after heat treatment are placed in tubular annealing stove, carry out in air atmosphere
Oxidation processes, oxidation temperature is set to 250 DEG C, and temperature retention time is 1h, then naturally cools to room temperature with stove, obtains final product oxidation
Iron silicon soft magnetic composite powder afterwards.
Step 3, ferro-silicium powder after heat treatment is cleaned into 0.1h with ultrasonic wave, filtered, vacuum drying is obtained final product
To the ferro-silicium composite powder for possessing core shell structure.The ferro-silicium composite powder prepared using the method for the present embodiment
For core shell structure, its inner core is iron silicon soft magnetic particles, and its shell is Al2O3Insulating barrier, and Al2O3Insulating barrier is equably wrapped up
In the surface of iron silicon soft magnetic particles, thereby may be ensured that ferro-silicium composite powder has while with higher magnetic permcability excellent
Good thermal stability and relatively low iron loss, and then disclosure satisfy that the standby use demand to high frequency development of electricity-magnetic converting means.
As seen from Figure 1, the ferro-silicium composite powder for possessing core shell structure prepared by the present embodiment comprises only Al2O3With iron silicon
Two kinds of thing phases of alloy.
With the standby development to high frequency direction of electricity-magnetic converting means, except requiring that powder core should have higher magnetic conductivity,
Also higher requirement is proposed to its iron loss, how ensures that powder core guarantees that it has on the basis of with higher magnetic permcability
Relatively low iron loss is the technical barrier for being badly in need of solving in powder core application process.For the technical problem, domestic and international researcher
Extensive research is expanded, and research is concentrated mainly on the cladding process aspect of insulating compound.Existing ferro-silicium composite powder leads to
Cladding process is carried out frequently with organic insulation agent, but organic insulation agent is easily thermally decomposed when being heat-treated at relatively high temperatures
And carbonization, and powder core at work because of the heating of long-term eddy-current loss, to be also easily caused organic insulation agent aging, so as to affect magnetic
The stability of core performance.
In order to avoid the aging impact to powder core heat endurance performance is decomposed in organic insulation agent, existing researcher will study
Direction switchs to replace organic insulation agent to carry out powder core cladding process using inorganic insulation agent, and inventor is also devoted to always this
The research in direction, and achieve certain achievement.Patent such as Chinese Patent Application No. 201410354869.6 discloses a kind of tool
There is ferrous alloy powder core of nucleocapsid heterojunction structure and preparation method thereof, it is specifically by iron(-)base powder and inorganic oxide
Powder is mixed, and ball-milling treatment is carried out under inert gas shielding, and the ferrous alloy composite powder after ball milling loads graphite jig, then
Insert and be sintered in plasma activated sintering stove and cooling treatment, obtain final product the ferrous alloy magnetic with nucleocapsid heterojunction structure
Core.Inventor has found in research process, can improve ferro-silicium to a certain extent using the method for this application case and be combined
The uniformity of the consistency, heat endurance and insulating compound cladding of powder, but because ferro-silicium material is powder, still cannot keep away
Powder can occur agglomeration during ball milling free, so as to be difficult to that the uniform of ferromagnetic particle surface insulation agent cladding is effectively ensured
Property, and the thickness of clad is not easy to control.
Inventor passes through this 2 years long-time research, and combines a large amount of theoretical and interpretations, finally found that, adopts
With the preparation method of the present invention, i.e., first aluminising process is carried out to ferro-silicium powder, then by the ferro-silicium powder after aluminising
Oxidation processes are carried out, such that it is able in the Al of one layer of densification of ferromagnetic particle coated with uniform2O3Insulating barrier, and then improve
The resistivity of iron silica flour grain, simultaneously because vortex is limited in insulating wrapped area, reduces the operating of vortex in cladding region
Radius, can be greatly lowered eddy-current loss.Wherein, can have by adding a certain proportion of alumina powder in mixed-powder
Effect prevents aluminium powder from sintering, and by the addition of ammonium chloride powder the aluminising speed of ferro-silicium powder can be effectively improved, and
The addition of itself also will not be impacted to the performance of gained ferro-silicium powder, easily be separated by subsequent treatment.Adopt
Ferro-silicium powder can also be prevented effectively from the method for the present invention and agglomeration occurs, it is ensured that Al2O3The uniformity of insulating barrier and
Compactness.Simultaneously can be to Al by control aluminising and oxidation technology parameter2O3The thickness of insulating barrier control effectively, the control
Mode processed is simple, and inventor is also optimized design by many experiments to aluminising and oxidation technology parameter, such that it is able to effective
Ensure the performance of final gained ferro-silicium composite powder.
Al is adopted in the present embodiment2O3Insulating barrier carries out cladding process to ferro-silicium material, it is to avoid have in prior art
The use of machine insulating compound, greatly reduces production cost and investment, and iron silicon that can be at relatively high temperatures to possessing core shell structure is closed
Golden composite powder is heat-treated, be it is follow-up obtain with high-compactness, heat endurance is good, non-oxidizability is strong, can exist for a long time
The iron silica magnetic particle core worked under higher environment temperature carries out raw material guarantee, and its preparation process is simple, improves production efficiency,
Environmentally safe, cost of material is relatively low, is suitable to promote the use of.
Embodiment 2
A kind of preparation method of ferro-silicium composite powder for possessing core shell structure of the present embodiment, it is concretely comprised the following steps：
Step one, first by the ferro-silicium powder of 81wt%, the aluminium powder of 0.9wt%, the ammonium chloride powder of 0.3wt% and
The alumina powder of 17.8wt% is well mixed, then described mixed-powder is placed in carry out under nitrogen protection at high warm
Reason, high-temperature heat treatment temperature setting is 450 DEG C, and temperature retention time is 1.5h, cools to room temperature with the furnace, obtains iron after heat treatment
Silicon alloy powder, the Si contents of ferro-silicium powder are 2wt% in the present embodiment.
Step 2, the ferro-silicium powder by gained after heat treatment are placed in tubular annealing stove, carry out under oxygen atmosphere
Oxidation processes, oxidation temperature is set to 300 DEG C, and temperature retention time is 1.5h, then naturally cools to room temperature with stove, obtains final product oxygen
Iron silicon soft magnetic composite powder after change.
Step 3, the ferro-silicium powder after heat treatment is cleaned into 0.3h with ultrasonic wave, filtered, vacuum drying,
Obtain the ferro-silicium composite powder for possessing core shell structure.The ferro-silicium composite powder prepared using the method for the present embodiment
End is core shell structure, and its stratum nucleare is ferromagnetic iron silicon grain, and its inner core is iron silicon soft magnetic particles, and its shell is Al2O3Insulation
Layer, and Al2O3Insulating barrier is equably wrapped in the surface of iron silicon soft magnetic particles, thereby may be ensured that ferro-silicium composite powder exists
There is excellent thermal stability and relatively low iron loss while with higher magnetic permcability, and then disclosure satisfy that electricity-magnetic conversion
Equip the use demand to high frequency development.
Embodiment 3
A kind of preparation method of ferro-silicium composite powder for possessing core shell structure of the present embodiment, its concrete steps is such as
Under：
Step one, first by the ferro-silicium powder of 82wt%, the aluminium powder of 1.7wt%, the ammonium chloride powder of 0.3wt% and
The alumina powder of 16wt% is well mixed, then by described mixed-powder be placed at argon gas protection under carry out high-temperature heat treatment,
High-temperature heat treatment temperature setting is 600 DEG C, and temperature retention time is 4h, cools to room temperature with the furnace, and the iron silicon for obtaining after heat treatment is closed
Bronze end, the Si contents of ferro-silicium powder are 4.5wt% in the present embodiment.
Step 2, the ferro-silicium powder after heat treatment is placed in into tubular annealing stove, is carried out under oxygen atmosphere
Oxidation processes, oxidation temperature is set to 350 DEG C, and temperature retention time is 2h, then naturally cools to room temperature with stove, obtains final product oxygen
Iron silicon soft magnetic composite powder after change.
Step 3, the ferro-silicium powder after heat treatment is cleaned into 0.5h with ultrasonic wave, filtered, vacuum drying,
Obtain the ferro-silicium composite powder for possessing core shell structure.The ferro-silicium composite powder prepared using the method for the present embodiment
End is core shell structure, and its inner core is iron silicon soft magnetic particles, and its shell is Al2O3Insulating barrier, and Al2O3Insulating barrier is equably wrapped
The surface of iron silicon soft magnetic particles is wrapped in, thereby may be ensured that ferro-silicium composite powder has while with higher magnetic permcability
Excellent thermal stability and relatively low iron loss, so disclosure satisfy that electricity-magnetic converting means it is standby to high frequency development using needing
Ask.
Embodiment 4
A kind of preparation method of ferro-silicium composite powder for possessing core shell structure of the present embodiment, its concrete steps is such as
Under：
Step one, first by the ferro-silicium powder of 83wt%, the aluminium powder of 2.5wt%, the ammonium chloride powder of 0.5wt% and
The alumina powder of 14wt% is well mixed, then by described mixed-powder be placed at argon gas protection under carry out high-temperature heat treatment,
High-temperature heat treatment temperature setting is 750 DEG C, and temperature retention time is 3h, cools to room temperature with the furnace, and the iron silicon for obtaining after heat treatment is closed
Bronze end, the Si contents of ferro-silicium powder are 5wt% in the present embodiment.
Step 2, the ferro-silicium powder after heat treatment is placed in into tubular annealing stove, is carried out in air atmosphere
Oxidation processes, oxidation temperature is set to 400 DEG C, and temperature retention time is 1.5h, then naturally cools to room temperature with stove, is obtained final product
Iron silicon soft magnetic composite powder after oxidation.
Step 3, the ferro-silicium powder after heat treatment is cleaned into 0.7h with ultrasonic wave, filtered, vacuum drying,
Obtain the ferro-silicium composite powder for possessing core shell structure.The ferro-silicium composite powder prepared using the method for the present embodiment
End is core shell structure, and its inner core is iron silicon soft magnetic particles, and its shell is Al2O3Insulating barrier, and Al2O3Insulating barrier is equably wrapped
The surface of iron silicon soft magnetic particles is wrapped in, thereby may be ensured that ferro-silicium composite powder has while with higher magnetic permcability
Excellent thermal stability and relatively low iron loss, so disclosure satisfy that electricity-magnetic converting means it is standby to high frequency development using needing
Ask.
Embodiment 5
A kind of preparation method of ferro-silicium composite powder for possessing core shell structure of the present embodiment, its concrete steps is such as
Under：
Step one, first by the ferro-silicium powder of 85wt%, the aluminium powder of 0.7wt%, the ammonium chloride powder of 0.1wt% and
The alumina powder of 14.2wt% is well mixed, then by described mixed-powder be placed at argon gas protection under carry out at high warm
Reason, high-temperature heat treatment temperature setting is 900 DEG C, and temperature retention time is 2.5h, cools to room temperature with the furnace, obtains iron after heat treatment
Silicon alloy powder, the Si contents of ferro-silicium powder are 7.5wt% in the present embodiment.
Step 2, the ferro-silicium powder after heat treatment is placed in into tubular annealing stove, is carried out under oxygen atmosphere
Oxidation processes, oxidation temperature is set to 450 DEG C, and temperature retention time is 1h, then naturally cools to room temperature with stove, obtains final product oxygen
Iron silicon soft magnetic composite powder after change.
Step 3, the ferro-silicium powder after heat treatment is cleaned into 0.2h with ultrasonic wave, filtered, vacuum drying,
Obtain the ferro-silicium composite powder for possessing core shell structure.The ferro-silicium composite powder prepared using the method for the present embodiment
End is core shell structure, and its inner core is iron silicon soft magnetic particles, and its shell is Al2O3Insulating barrier, and Al2O3Insulating barrier is equably wrapped
The surface of iron silicon soft magnetic particles is wrapped in, thereby may be ensured that ferro-silicium composite powder has while with higher magnetic permcability
Excellent thermal stability and relatively low iron loss, so disclosure satisfy that electricity-magnetic converting means it is standby to high frequency development using needing
Ask.
Embodiment 6
A kind of preparation method of ferro-silicium composite powder for possessing core shell structure of the present embodiment, its concrete steps is such as
Under：
Step one, first by the ferro-silicium powder of 86wt%, the aluminium powder of 1wt%, the ammonium chloride powder of 0.4wt% and
The alumina powder of 12.6wt% is well mixed, then described mixed-powder is placed in carry out under nitrogen protection at high warm
Reason, high-temperature heat treatment temperature setting is 1050 DEG C, and temperature retention time is 3h, cools to room temperature with the furnace, obtains iron after heat treatment
Silicon alloy powder, the Si contents of ferro-silicium powder are 6wt% in the present embodiment.
Step 2, the ferro-silicium powder after heat treatment is placed in into tubular annealing stove, is carried out in air atmosphere
Oxidation processes, oxidation temperature is set to 500 DEG C, and temperature retention time is 1.5h, then naturally cools to room temperature with stove, is obtained final product
Iron silicon soft magnetic composite powder after oxidation.
Step 3, the ferro-silicium powder after heat treatment is cleaned into 0.4h with ultrasonic wave, filtered, vacuum drying,
Obtain the ferro-silicium composite powder for possessing core shell structure.The ferro-silicium composite powder prepared using the method for the present embodiment
End is core shell structure, and its inner core is iron silicon soft magnetic particles, and its shell is Al2O3Insulating barrier, and Al2O3Insulating barrier is equably wrapped
The surface of iron silicon soft magnetic particles is wrapped in, thereby may be ensured that ferro-silicium composite powder has while with higher magnetic permcability
Excellent thermal stability and relatively low iron loss, so disclosure satisfy that electricity-magnetic converting means it is standby to high frequency development using needing
Ask.
Embodiment 7
A kind of preparation method of ferro-silicium composite powder for possessing core shell structure of the present embodiment, its concrete steps is such as
Under：
Step one, first by the ferro-silicium powder of 88wt%, the aluminium powder of 2wt%, the ammonium chloride powder of 0.2wt% and
The alumina powder of 9.8wt% is well mixed, then by described mixed-powder be placed at argon gas protection under carry out high-temperature heat treatment,
High-temperature heat treatment temperature setting is 1250 DEG C, and temperature retention time is 0.5h, cools to room temperature with the furnace, obtains iron silicon after heat treatment
Alloy powder, the Si contents of ferro-silicium powder are 6.5wt% in the present embodiment.
Step 2, the ferro-silicium powder after heat treatment is placed in into tubular annealing stove, is carried out under oxygen atmosphere
Oxidation processes, oxidation temperature is set to 200 DEG C, and temperature retention time is 3h, then naturally cools to room temperature with stove, obtains final product oxygen
Iron silicon soft magnetic composite powder after change.
Step 3, the ferro-silicium powder after heat treatment is cleaned into 1h with ultrasonic wave, filtered, vacuum drying is obtained
To the ferro-silicium composite powder for possessing core shell structure.The ferro-silicium composite powder prepared using the method for the present embodiment
For core shell structure, its inner core is iron silicon soft magnetic particles, and its shell is Al2O3Insulating barrier, and Al2O3Insulating barrier is equably wrapped up
In the surface of iron silicon soft magnetic particles, thereby may be ensured that ferro-silicium composite powder has while with higher magnetic permcability excellent
Good thermal stability and relatively low iron loss, and then disclosure satisfy that the standby use demand to high frequency development of electricity-magnetic converting means.
Embodiment 8
A kind of preparation method of ferro-silicium composite powder for possessing core shell structure of the present embodiment, its concrete steps is such as
Under：
Step one, first by the ferro-silicium powder of 90wt%, the aluminium powder of 2.5wt%, the ammonium chloride powder of 0.5wt% and
The alumina powder of 7wt% is well mixed, then described mixed-powder is placed in carry out under nitrogen protection high-temperature heat treatment, high
Warm treatment temperature is set to 700 DEG C, and temperature retention time is 1h, cools to room temperature with the furnace, obtains ferro-silicium after heat treatment
Powder, the Si contents of ferro-silicium powder are 7.5wt% in the present embodiment.
Step 2, the ferro-silicium powder after heat treatment is placed in into tubular annealing stove, is carried out under oxygen atmosphere
Oxidation processes, oxidation temperature is set to 360 DEG C, and temperature retention time is 1.7h, then naturally cools to room temperature with stove, is obtained final product
Iron silicon soft magnetic composite powder after oxidation.
Step 3, the ferro-silicium powder after heat treatment is cleaned into 0.6h with ultrasonic wave, filtered, vacuum drying,
Obtain the ferro-silicium composite powder for possessing core shell structure.The ferro-silicium composite powder prepared using the method for the present embodiment
End is core shell structure, and its inner core is iron silicon soft magnetic particles, and its shell is Al2O3Insulating barrier, and Al2O3Insulating barrier is equably wrapped
The surface of iron silicon soft magnetic particles is wrapped in, thereby may be ensured that ferro-silicium composite powder has while with higher magnetic permcability
Excellent thermal stability and relatively low iron loss, so disclosure satisfy that electricity-magnetic converting means it is standby to high frequency development using needing
Ask.
In conjunction with the embodiments knowable to 1-8, the resistivity of the ferro-silicium composite powder prepared using the method for the present invention
High, the low, heat endurance of loss is good, disclosure satisfy that the standby use demand to high frequency development of electricity-magnetic converting means, and its preparation technology
Simply, production efficiency is improve, and environmentally safe, cost of material is relatively low, is suitable to promote the use of.Colleague's gained ferro-silicium
Composite powder can be heat-treated at relatively high temperatures, be that follow-up acquisition has that high-compactness, heat endurance be good, non-oxidizability
By force, the iron silica magnetic particle core that can be worked at higher ambient temperatures for a long time carries out raw material guarantee.
Claims (10)
1. a kind of preparation method of the ferro-silicium composite powder for possessing core shell structure, it is characterised in that：First pass through heat treatment right
Ferro-silicium powder carries out aluminising process, then the ferro-silicium powder after aluminising is carried out into oxidation processes, and Jing magnetic separation is processed
The ferro-silicium composite powder for possessing core shell structure is obtained afterwards.
2. the preparation method of a kind of ferro-silicium composite powder for possessing core shell structure according to claim 1, its feature
It is that it is comprised the following steps that：
Step one, ferro-silicium powder, aluminium powder, ammonium chloride powder and alumina powder are well mixed obtain mixed-powder, will
Mixed-powder is heat-treated under inert gas shielding, controls heat treatment temperature for 300～1250 DEG C, and temperature retention time is 0.5
～5h, then cools to room temperature with the furnace, obtains ferro-silicium powder after heat treatment；
Step 2, ferro-silicium powder after heat treatment is placed under oxidizing atmosphere carries out oxidation processes, control oxidation processes
Temperature is 200～500 DEG C, and temperature retention time is 1～3h, then naturally cools to room temperature with stove, obtains final product the iron silicon soft magnetism after oxidation
Composite powder；
Step 3, gained is aoxidized after iron silicon soft magnetic composite powder carry out ultrasonic wave cleaning, magnetic separation and vacuum drying treatment, i.e.,
Obtain the ferro-silicium composite powder for possessing core shell structure.
3. the preparation method of a kind of ferro-silicium composite powder for possessing core shell structure according to claim 2, its feature
It is：The mass percent of each component is as follows in gained mixed-powder in the step one：Ferro-silicium 80～90wt% of powder,
0.5～2.5wt% of aluminium powder, ammonium chloride 0.1～0.5wt% of powder, 7～19.4wt% of alumina powder.
4. the preparation side of a kind of ferro-silicium composite powder for possessing core shell structure according to any one of claim 1-3
Method, it is characterised in that：Gained ferro-silicium composite powder is core shell structure, and its inner core is iron silicon soft magnetic particles, and its shell is
Al2O3Insulating barrier, and Al2O3Insulating barrier is equably wrapped in the surface of iron silicon soft magnetic particles.
5. the preparation side of a kind of ferro-silicium composite powder for possessing core shell structure according to any one of claim 1-3
Method, it is characterised in that：The Si contents of the ferro-silicium powder are 0.5～7.5wt%.
6. the preparation side of a kind of ferro-silicium composite powder for possessing core shell structure according to any one of claim 1-3
Method, it is characterised in that：NH in the ammonium chloride powder4The mass percentage content of Cl is more than 99.5%, the alumina powder
Middle Al2O3Mass percentage content be more than 99%.
7. the preparation method of a kind of ferro-silicium composite powder for possessing core shell structure according to claim 4, its feature
It is：The particle diameter of the aluminium powder is less than 1 μm, and the mass percentage content of Al is more than 99.5% in aluminium powder.
8. the preparation method of a kind of ferro-silicium composite powder for possessing core shell structure according to claim 7, its feature
It is：Inert gas in the step one adopts air or oxygen using argon gas or nitrogen, the oxidizing atmosphere in step 2.
9. the preparation method of a kind of ferro-silicium composite powder for possessing core shell structure according to claim 8, its feature
It is：The time of ultrasonic wave cleaning is 0.1～1h in the step 4.
10. a kind of ferro-silicium composite powder for possessing core shell structure, it is characterised in that：The composite powder is to adopt claim
What the method any one of 1-9 was prepared.
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