CN106601416B - A kind of iron silicon soft magnetic composite powder of multi-layer core-shell structure and preparation method thereof - Google Patents

A kind of iron silicon soft magnetic composite powder of multi-layer core-shell structure and preparation method thereof Download PDF

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CN106601416B
CN106601416B CN201611214913.9A CN201611214913A CN106601416B CN 106601416 B CN106601416 B CN 106601416B CN 201611214913 A CN201611214913 A CN 201611214913A CN 106601416 B CN106601416 B CN 106601416B
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powder
soft magnetic
composite powder
iron silicon
shell structure
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CN106601416A (en
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吴朝阳
李�杰
郑力
李光强
樊希安
王万林
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Wuhan University of Science and Engineering WUSE
Anhui University of Technology AHUT
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Wuhan University of Science and Engineering WUSE
Anhui University of Technology AHUT
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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
    • 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
    • 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

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  • Dispersion Chemistry (AREA)
  • Engineering & Computer Science (AREA)
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  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Soft Magnetic Materials (AREA)
  • Powder Metallurgy (AREA)

Abstract

Iron silicon soft magnetic composite powder the invention discloses a kind of multi-layer core-shell structure and preparation method thereof, belongs to soft magnetic composite powder technical field.The composite powder of the present invention includes inner core and is coated on the shell of inner core outer layer, its inner core is iron silicon soft magnetic particles, and the external sheath of soft magnetic particles has Fe3Si, Fe3The outside of Si is coated with SiO2Insulating layer.The preparation method of the above-mentioned composite powder of the present invention, its step are：Ferro-silicium powder and nano silica fume are uniformly mixed, is placed in the stove of starvation and keeps the temperature 1~5h in 900~1150 DEG C, cool to room temperature with the furnace；Finally it is placed in rotary tube furnace, 0.5~2h, and furnace cooling is kept the temperature at 200~450 DEG C under oxidizing atmosphere, up to the iron silicon soft magnetic composite powder of multi-layer core-shell structure.The preparation method technique of the present invention is simple, and the cycle is short, and cost is low, and preparing gained iron silicon soft magnetic composite powder has higher resistivity and excellent heat endurance, and its iron loss is lower, and service life is longer.

Description

A kind of iron silicon soft magnetic composite powder of multi-layer core-shell structure and preparation method thereof
Technical field
The invention belongs to soft magnetic composite powder technical field, more specifically to a kind of iron silicon of multi-layer core-shell structure Soft magnetic composite powder and preparation method thereof.
Background technology
Metal magnetic powder core be by ferromagnetism powder and dielectric through mix, suppress and be heat-treated and made of a kind of soft magnetism Composite material.Common metal magnetic powder core has ferromagnetic powder core, iron-silicon-aluminualloy alloy magnetic powder core, iron-nickel alloy powder core, ferro-silicium Powder core, permalloy powder core etc..Wherein iron silica magnetic particle core mainly substitutes ferrocart core, low 80% left side of loss ratio ferrocart core The right side, can use under the high-frequency of more than 8kHz.In recent years, turn with the popularization of mainstream motor frequency conversion control model, at a high speed The exploitation of dynamic motor and the further application of energy-saving semiconductor power device, electricity-standby frequency of use of magnetic converting means are just gradual Develop to high frequency direction, to ensure that power electronics equipment is more energy efficient and minimizes.
It is well known that the powder core as electromagnetic switching device operation when, can because surrounding magnetic field change and Vortex is produced, and the raising of applying frequency can cause the increase of powder core eddy-current loss.Eddy-current loss not only reduces powder core Performance, while substantial amounts of Joule heat can be produced, therefore reduce application of the eddy-current loss for powder core in electromagnetic switching device With regard to most important.At present, in order to reduce the energy loss as caused by eddy-current loss, it is common practice to ferromagnetic in powder core Property powder particle surface coat the higher organic or inorganic megohmite insulant of a layer resistivity.
Common organic insulation agent mainly has epoxy resin, silicone resin and phenolic resin etc..Such as, Chinese Patent Application No. A kind of manufacture method of iron silicon materials and iron silica magnetic particle core is disclosed for 201410445569.9 application case, this application first makes Ferro-silicium powder is coated as insulating compound by the use of silicone resin and zinc stearate, epoxy is immersed in after compressing Heavy insulation is carried out in resin.But organic insulation agent is used to carry out the iron silica magnetic particle core that cladding processing is prepared, in higher temperatures Under the conditions of degree during (600-700 DEG C) heat treatment, the resin for being coated on magnetic powder surface is easily thermally decomposed and is carbonized, so as to cause magnetic The insulating properties of powder core declines, high-gradient magnetism energy is bad, eddy-current loss is larger.In addition, cladding processing is carried out using organic insulation agent When also result in powder core at work because long-term eddy-current loss is generated heat so that organic matter aging, so as to influence magnetic powder core performance Stability.
In recent years, inorganic insulation cladding since its excellent insulating properties and heat endurance gradually replace organic insulation cladding and As the hot spot of people's research.The inorganic insulation agent often used include inorganic phosphate (zinc phosphoric acid, iron phosphate and manganese phosphoric acid), Silicate and inorganic oxide etc..General preparation process is to mix ferromagnetic powder with insulating compound and binding agent, with rear mold Pressing formation, last thermally treated acquisition powder core.Such as, it is entitled " a kind of metal soft magnetic powder core with inorganic insulation bonding agent and its The patent application case of preparation method " (CN101089108A) is directly real to iron-based soft magnetic powder surface using inorganic oxide The processing of row insulating wrapped, but it is directly simply to be mixed ferromagnetic powder with insulating compound, so as to be difficult to ensure that each Ferromagnetic particle surface can coat last layer insulating compound, and ferromagnetic particle is easily reunited, so as to cause insulating wrapped Agent skewness, poor insulativity, the stability of product are poor, quality is unstable and iron loss is higher.
In addition, document " preparation of the 6.5%Si high silicon steel cores of heterojunction structure containing nucleocapsid and magnetic property " (functional material, 44.10(2013):One kind 1431-1436.) is reported by the way that ferromagnetic powder is carried out high-temperature oxydation under oxidizing atmosphere, from And make the method for powder Surface Creation inorganic oxide dielectric film.Can effectively it be carried to a certain extent using the method in the document Its high resistivity, but it is difficult to ensure that the uniformity of gained ferromagnetic powder surface inorganic oxide dielectric film, and the thickness of dielectric film Degree is also difficult to control, so as to limit the application of the technology.
In conclusion the above problem existing for ferromagnetic powder surface insulation layer cladding all seriously restricts iron silica magnetic particle core Development and application, therefore, how to ensure iron silicon soft magnetic composite powder while possessing high magnetic permeability with relatively low vortex Loss and excellent heat endurance are the technical barriers that those skilled in the art are badly in need of solving.
The content of the invention
1. technical problems to be solved by the inivention
It is an object of the invention to overcome use the prior art prepare gained iron silicon soft magnetic composite powder existing for it is above-mentioned not A kind of foot, there is provided iron silicon soft magnetic composite powder of multi-layer core-shell structure and preparation method thereof.Method using the present invention can Preparing one kind has high saturated magnetic induction, high resistivity, and the iron of the multi-layer core-shell structure low, heat endurance is good is lost Silicon soft magnetic composite powder, so as to meet existing electricity-standby requirement of magnetic converting means.
2. technical solution
To reach above-mentioned purpose, technical solution provided by the invention is：
A kind of iron silicon soft magnetic composite powder of multi-layer core-shell structure of the present invention, the composite powder are by inner core and cladding In the multi-layer core-shell structure that the shell of inner core outer layer forms, its inner core is iron silicon soft magnetic particles, the outer layer bag of soft magnetic particles It is covered with Fe3Si, Fe3The outside of Si is coated with SiO2Insulating layer.
Further, the saturation induction density of the composite powder is 153~174emu/g, and coercivity is 5~8Oe, Resistivity is 4.3 × 10-5~3.1 × 10-4Ω·m。
The preparation method of the iron silicon soft magnetic composite powder of a kind of multi-layer core-shell structure of the present invention, first by ferro-silicium powder Siliconising heat treatment is carried out, is subsequently placed under oxidizing atmosphere and carries out oxidation processes, and by controlling rational siliconising heat treatment and oxygen Change treatment process, so as to obtain the iron silicon soft magnetic composite powder for possessing multi-layer core-shell structure.
Further, a kind of preparation method of the iron silicon soft magnetic composite powder of multi-layer core-shell structure of the invention is specific Step is as follows：
Step 1: ferro-silicium powder and nano silica fume are uniformly mixed, then by gained mixed-powder in starvation Under conditions of carry out high-temperature heat treatment, heat treatment temperature is 900~1150 DEG C, and soaking time is 1~5h, is cooled to the furnace afterwards Room temperature, obtains the ferro-silicium powder after siliconising is heat-treated；
Step 2: the ferro-silicium powder after siliconising is heat-treated is heated to the heating rate of 10~30 DEG C/min 200~450 DEG C, 0.5~2h then is kept the temperature in 200~450 DEG C under oxidizing atmosphere, cools to room temperature with the furnace afterwards, i.e., much The iron silicon soft magnetic composite powder of layer core shell structure.
Further, the mass percentage content of ferro-silicium powder is 90 in gained mixed-powder in the step 1 ~99.5%, the mass percentage content of nano silica fume is 0.5~10%.
Further, mixed-powder is placed in high-temperature vacuum furnace, inert atmosphere protection stove or reduction in the step 1 High-temperature heat treatment is carried out in atmosphere protection stove.
Further, the ferro-silicium powder after siliconising is heat-treated in the step 2 is placed in rotary tube furnace progress Oxidation processes, and the rotating speed of during insulation rotary tube furnace is 2~7RPM.
Further, the particle diameter of the ferro-silicium powder is less than 150 μm, and the Si contents of ferro-silicium powder are 0.5~7.0wt%.
Further, the particle diameter of the nano silica fume is less than 200nm, and the mass fraction of the Si in nano silica fume is more than 99.5wt%.
Further, the oxidizing atmosphere in the step 2 is air or oxygen.
3. beneficial effect
Using technical solution provided by the invention, compared with prior art, there is following remarkable result：
(1) the iron silicon soft magnetic composite powder of a kind of multi-layer core-shell structure of the invention, the composite powder be by inner core and Be coated on the multi-layer core-shell structure of the shell composition of inner core outer layer, its inner core be iron silicon soft magnetic particles, soft magnetic particles outside Layer is coated with Fe3Si, Fe3The outside of Si is coated with SiO2Insulating layer, so as to which iron silicon soft magnetic composite powder is effectively ensured at the same time With higher saturation induction density, relatively low eddy-current loss and excellent heat endurance, existing electricity-magnetic conversion disclosure satisfy that Equip the requirement developed to high frequency direction.
(2) preparation method of the iron silicon soft magnetic composite powder of a kind of multi-layer core-shell structure of the invention, after first siliconising The mode of oxidation carries out cladding processing to iron silicon soft magnetic particles, and the uniformity of gained clad is preferable, while reasonable by controlling Siliconising heat treatment and oxidation processing technique, consequently facilitating be controlled the thickness of clad, and ensure to obtain multi-layer core-shell The iron silicon soft magnetic composite powder of structure, make gained composite powder on the basis of with compared with high saturated magnetic induction still with compared with Low eddy-current loss and excellent heat endurance.
(3) preparation method of the iron silicon soft magnetic composite powder of a kind of multi-layer core-shell structure of the invention, it prepares gained iron The most external of silicon soft magnetic composite powder is coated with one layer of fine and close SiO2Insulating layer, avoid organic insulation agent in the prior art and The use of binding agent, at relatively high temperatures can be heat-treated the iron silicon soft magnetic composite powder of multi-layer core-shell structure, be follow-up Obtain with high-compactness, heat endurance is good, inoxidizability is strong, the iron silica magnetic particle that can work at higher ambient temperatures for a long time Core carries out raw material guarantee.
(4) preparation method of the iron silicon soft magnetic composite powder of a kind of multi-layer core-shell structure of the invention, the letter of its operating procedure It is single, reduce production cost and investment, improve production efficiency, and it is environmentally safe, it is easy to utilize.
Brief description of the drawings
Fig. 1 is a kind of SEM figures of the iron silicon soft magnetic composite powder for multi-layer core-shell structure that the embodiment of the present invention 1 is prepared Picture and its corresponding line scanning spectra；
Fig. 2 is the hysteresis curve figure of the iron silicon soft magnetic composite powder of the multi-layer core-shell structure shown in Fig. 1.
Embodiment
To further appreciate that present disclosure, in conjunction with specific embodiment, the present invention is described in detail.
It is first that the raw material Unify legislation involved in each embodiment is as follows to avoid repeating, repeated no more in embodiment：It is described The particle diameter of ferro-silicium powder is less than 150 μm, and the particle diameter of nano silica fume is less than 200nm, and the purity (matter of the Si in nano silica fume Amount fraction) it is more than 99.5wt%, by optimizing control to the particle diameter of ferro-silicium powder and nano silica fume, so as to be conducive to Ensure the compactness and intensity of gained iron silicon soft magnetic granules surface coating layer.
Embodiment 1
The preparation method of the iron silicon soft magnetic composite powder of a kind of multi-layer core-shell structure of the present embodiment, first by ferro-silicium powder End carries out siliconising heat treatment, is subsequently placed under oxidizing atmosphere and carries out oxidation processes, and by control rational siliconising be heat-treated and Oxidation processing technique, so as to obtain the iron silicon soft magnetic composite powder for possessing multi-layer core-shell structure.The preparation method it is specific Step is as follows：
Step 1: it is respectively that the ferro-silicium powder of 90wt% and the nano silica fume of 10wt% mix by mass percentage content Close uniformly, gained mixed-powder then is placed in high-temperature vacuum furnace carries out high-temperature heat treatment, and heat treatment temperature is 900 DEG C, insulation Time is 1.5h, cools to room temperature with the furnace afterwards, obtains the ferro-silicium powder after siliconising is heat-treated, and ferro-silicium powder The distribution of siliconising layer is than more uniform.The Si contents (mass fraction) of ferro-silicium powder are 2.0wt% in the present embodiment.
Step 2: the ferro-silicium powder after siliconising is heat-treated is placed in rotary tube furnace, with the heating of 10 DEG C/min Speed is heated to 200 DEG C, then keeps the temperature 0.5h in 200 DEG C under oxidizing atmosphere, and the rotating speed of during insulation rotary tube furnace is 2RPM, cools to room temperature with the furnace afterwards, up to the iron silicon soft magnetic composite powder of multi-layer core-shell structure.What the present embodiment was prepared Composite powder is by inner core and is coated on the multi-layer core-shell structure that the shell of inner core outer layer forms, its inner core is soft for iron silicon Magnetic particle, the external sheath of soft magnetic particles have Fe3Si, Fe3The outside of Si is coated with SiO2Insulating layer, so as to be effectively ensured Iron silicon soft magnetic composite powder has higher saturation induction density, relatively low eddy-current loss and excellent heat endurance at the same time, It disclosure satisfy that the standby requirement developed to high frequency direction of existing electricity-magnetic converting means.The SEM of composite powder obtained by the present embodiment Image and its corresponding line scanning spectra with reference to Fig. 1 analyses respectively as shown in Figure 1, understand that iron silicon soft magnetism obtained by the present embodiment is answered Close powder and comprise only tri- kinds of elements of Fe, Si, O, and the outermost layer of powder is by SiO2Coat even compact.
Develop as electricity-magnetic converting means is standby to high frequency direction, existing powder core can cause its vortex in application process Loss increase, so as to influence its performance, limits its application in electricity-magnetic converting means is standby.In order to effectively reduce magnetic powder The eddy-current loss of core, domestic and international researcher be typically directed to ferromagnetism powder particle surface coat higher organic of a layer resistivity or The research of inorganic insulation agent.But since because generating heat aging phenomenon easily occurs for organic insulation agent in use, so as to cause magnetic The thermal stability of powder core is poor, so as to promote the research of inorganic insulation agent cladding processing.Inventor also has been devoted to lead to The processing of inorganic insulation agent cladding is crossed to reduce the research of powder core eddy-current loss, e.g., filed in 24 days July in 2014 of inventor The patent of Application No. 201410354869.6 discloses a kind of ferrous alloy powder core and its system with nucleocapsid heterojunction structure Preparation Method, this application carry out ball by mixing iron(-)base powder and inorganic oxide powder under inert gas shielding Mill processing, then the ferrous alloy composite powder after ball milling is placed in plasma activated sintering stove be sintered and cooling at Reason, it is hereby achieved that the ferrous alloy powder core with nucleocapsid heterojunction structure.Using the method in the patent to a certain degree On can improve ferro-silicium composite powder consistency, heat endurance and insulating compound cladding uniformity, but still be difficult to have Effect ensures the uniformity of ferromagnetic particle surface insulation agent cladding, and the thickness of clad is not easy to control, gained powder core Eddy-current loss is still higher, it is difficult to meets the standby use demand developed to high frequency direction of electricity-magnetic converting means.
Therefore, how to ensure that the uniformity of inorganic insulation agent cladding and its easily-controllable property of coating thickness are that inventor is grinding The technological difficulties overcome are needed during studying carefully, this be also limit one of the application of inorganic insulation agent coating technology it is main because Element.Inventor passes through lot of experiments and theory analysis, finally found that the method using the present embodiment, that is, after using first siliconising The mode of oxidation carries out cladding processing to iron silicon soft magnetic particles, so as to which iron silicon soft magnetic particles surface coating layer is effectively ensured Uniformity, while by siliconizing treatment processes parameter and subsequent oxidation technological parameter, especially to siliconising heat treatment temperature and time And the temperature and time of subsequent oxidation processing is adjusted, so as to control effectively to the thickness of gained clad, Solve the uniformity and thickness of clad when using inorganic insulation agent iron silicon soft magnetic particles are carried out with cladding processing in the prior art The unmanageable problem of degree, and then ensure that the performance of gained iron silicon soft magnetic composite powder.Inventor is also by a large amount of real Research is tested to siliconizing treatment processes parameter and subsequent oxidation technological parameter, such as siliconising heat treatment temperature, soaking time, oxidation processes temperature Degree, heating rate and soaking time optimize, it is hereby achieved that the iron silicon soft magnetism with multi-layer core-shell structure is compound Powder.Wherein, since the external sheath of iron silicon soft magnetic particles has Fe3Si phases, so as to be conducive to improve the interaction coupling of magnetic particle Cooperation is used, and ensures that it has higher saturation induction density.And since ferromagnetic particle outermost layer is by inorganic SiO2Insulating layer Uniformly cladding, so as to effectively improve the resistivity of iron silica flour grain, simultaneously because vortex is limited in insulating wrapped area, subtracts The operating radius of vortex is lacked, eddy-current loss can be greatly lowered.Therefore, it is prepared using the method for the present embodiment compound Powder is on the basis of with compared with high saturated magnetic induction still with relatively low eddy-current loss and excellent heat endurance.This Outside, since the most external of gained iron silicon soft magnetic composite powder is coated with one layer of fine and close SiO2Insulating layer, so as to avoid existing Organic insulation agent and the use of binding agent in technology, can be at relatively high temperatures to the iron silicon soft magnetic composite powder of multi-layer core-shell structure It is heat-treated, for follow-up acquisition has high-compactness, heat endurance is good, inoxidizability is strong, can be for a long time in higher environment temperature The iron silica magnetic particle core of the lower work of degree has carried out raw material guarantee.
The magnetic property of iron silicon soft magnetic composite powder manufactured in the present embodiment is detected using VSM, the results showed that, this reality Applying composite powder obtained by example has an excellent soft magnet performance, its saturation induction density is 153emu/g (as shown in Figure 2), coercive Power is 7Oe.The resistivity of powder is tested using resistivity tester, the results showed that, composite powder obtained by the present embodiment With higher resistivity, its resistivity is 3.1 × 10-4Ω·m。
Embodiment 2
The preparation method of the iron silicon soft magnetic composite powder of a kind of multi-layer core-shell structure of the present embodiment, first by ferro-silicium powder End carries out siliconising heat treatment, is subsequently placed under oxidizing atmosphere and carries out oxidation processes, and by control rational siliconising be heat-treated and Oxidation processing technique, so as to obtain the iron silicon soft magnetic composite powder for possessing multi-layer core-shell structure.The preparation method it is specific Step is as follows：
Step 1: be first uniformly mixed the high-purity nm silica flour of the ferro-silicium powder of 92wt% and 8wt%, then by described in Mixed-powder be placed in inert atmosphere protection stove and carry out high-temperature heat treatment, between heat treatment temperature is 950 DEG C, soaking time is 1h, cools to room temperature with the furnace afterwards, obtains the ferro-silicium powder after siliconising is heat-treated.Ferro-silicium powder in the present embodiment Si contents (mass fraction) be 0.5wt%.
Step 2: the ferro-silicium powder after siliconising is heat-treated is placed in rotary tube furnace, with the heating of 20 DEG C/min Speed is warming up to 300 DEG C, keeps the temperature 1h under the conditions of 300 DEG C under oxygen atmosphere, and during insulation rotary tube furnace rotating speed is 4RPM, Then with stove cooled to room temperature, up to the iron silicon soft magnetic composite powder of multi-layer core-shell structure.What the present embodiment was prepared Composite powder is by inner core and is coated on the multi-layer core-shell structure that the shell of inner core outer layer forms, its inner core is soft for iron silicon Magnetic particle, the external sheath of soft magnetic particles have Fe3Si, Fe3The outside of Si is coated with SiO2Insulating layer.
The magnetic property of iron silicon soft magnetic composite powder manufactured in the present embodiment is detected using VSM, the results showed that, this reality Composite powder obtained by applying example has excellent soft magnet performance, its saturation induction density is 158emu/g, coercivity 7Oe.Adopt Powder resistivity is tested with resistivity tester, the results showed that powder has higher resistivity, its resistivity is 2.0 ×10-4Ω·m。
Embodiment 3
A kind of preparation method of the iron silicon soft magnetic composite powder of multi-layer core-shell structure of the present embodiment, its specific steps is such as Under：
Step 1: be first uniformly mixed the high-purity nm silica flour of the ferro-silicium powder of 93wt% and 7wt%, then by described in Mixed-powder be placed in protection of reducing atmosphere stove and carry out high-temperature heat treatment, between heat treatment temperature is 1000 DEG C, soaking time For 2h, room temperature is cooled to the furnace afterwards, obtain the ferro-silicium powder after siliconising is heat-treated.Ferro-silicium powder in the present embodiment The Si contents (mass fraction) at end are 7.0wt%.
Step 2: the ferro-silicium powder after siliconising is heat-treated is placed in rotary tube furnace, with the heating of 25 DEG C/min Speed is warming up to 350 DEG C, keeps the temperature 2h under the conditions of 350 DEG C in air atmosphere, and during insulation rotary tube furnace rotating speed is 5RPM, Then with stove cooled to room temperature, up to the iron silicon soft magnetic composite powder of multi-layer core-shell structure.What the present embodiment was prepared Composite powder is by inner core and is coated on the multi-layer core-shell structure that the shell of inner core outer layer forms, its inner core is soft for iron silicon Magnetic particle, the external sheath of soft magnetic particles have Fe3Si, Fe3The outside of Si is coated with SiO2Insulating layer.
The magnetic property of iron silicon soft magnetic composite powder manufactured in the present embodiment is detected using VSM, the results showed that, this reality Composite powder obtained by applying example has excellent soft magnet performance, its saturation induction density is 159emu/g, coercivity 6Oe.Adopt Powder resistivity is tested with resistivity tester, the results showed that powder has higher resistivity, its resistivity is 1.0 ×10-4Ω·m。
Embodiment 4
A kind of preparation method of the iron silicon soft magnetic composite powder of multi-layer core-shell structure of the present embodiment, its specific steps is such as Under：
Step 1: be first uniformly mixed the high-purity nm silica flour of the ferro-silicium powder of 94wt% and 6wt%, then by described in Mixed-powder be placed in high-temperature vacuum furnace and carry out high-temperature heat treatment, heat treatment temperature is arranged to 1100 DEG C, and soaking time is 2.5h, cools to room temperature with the furnace, obtains the ferro-silicium powder after siliconising is heat-treated.Ferro-silicium powder in the present embodiment Si contents (mass fraction) are 5.0wt%.
Step 2: the ferro-silicium powder after siliconising is heat-treated is placed in rotary tube furnace, with 30 DEG C/min's Heating rate is warming up to 400 DEG C, keeps the temperature 0.5h, during insulation rotary tube furnace rotating speed under the conditions of 400 DEG C in air atmosphere For 6RPM, then with stove cooled to room temperature, up to the iron silicon soft magnetic composite powder of multi-layer core-shell structure.It is prepared by the present embodiment Obtained composite powder is by inner core and is coated on the multi-layer core-shell structure that the shell of inner core outer layer forms, its inner core is Iron silicon soft magnetic particles, the external sheath of soft magnetic particles have Fe3Si, Fe3The outside of Si is coated with SiO2Insulating layer.
The magnetic property of iron silicon soft magnetic composite powder manufactured in the present embodiment is detected using VSM, the results showed that, this reality Composite powder obtained by applying example has excellent soft magnet performance, its saturation induction density is 163emu/g, coercivity 7Oe.Adopt Powder resistivity is tested with resistivity tester, the results showed that powder has higher resistivity, its resistivity is 9.1 ×10-5Ω·m。
Embodiment 5
A kind of preparation method of the iron silicon soft magnetic composite powder of multi-layer core-shell structure of the present embodiment, its specific steps is such as Under：
Step 1: be first uniformly mixed the high-purity nm silica flour of the ferro-silicium powder of 95wt% and 5wt%, then by described in Mixed-powder be placed in high-temperature vacuum furnace and carry out high-temperature heat treatment, heat treatment temperature is arranged between 1150 DEG C, soaking time For 3h, room temperature is cooled to the furnace, obtain the ferro-silicium powder after siliconising is heat-treated.Ferro-silicium powder in the present embodiment Si contents (mass fraction) are 3.5wt%.
Step 2: the ferro-silicium powder after siliconising is heat-treated is placed in rotary tube furnace, with the heating of 10 DEG C/min Speed is warming up to 450 DEG C, keeps the temperature 0.9h under the conditions of 450 DEG C under oxygen atmosphere, and during insulation rotary tube furnace rotating speed is 7RPM, then with stove cooled to room temperature, up to the iron silicon soft magnetic composite powder of multi-layer core-shell structure.The present embodiment is prepared into To composite powder is by inner core and is coated on the multi-layer core-shell structure that the shell of inner core outer layer forms, its inner core is iron Silicon soft magnetic particles, the external sheath of soft magnetic particles have Fe3Si, Fe3The outside of Si is coated with SiO2Insulating layer.
The magnetic property of iron silicon soft magnetic composite powder manufactured in the present embodiment is detected using VSM, the results showed that, this reality Composite powder obtained by applying example has excellent soft magnet performance, its saturation induction density is 165emu/g, coercivity 6Oe.Adopt Powder resistivity is tested with resistivity tester, the results showed that powder has higher resistivity, its resistivity is 7.4 ×10-5Ω·m。
Embodiment 6
A kind of preparation method of the iron silicon soft magnetic composite powder of multi-layer core-shell structure of the present embodiment, its specific steps is such as Under：
Step 1: be first uniformly mixed the high-purity nm silica flour of the ferro-silicium powder of 97wt% and 3wt%, then by described in Mixed-powder be placed in inert atmosphere protection stove and carry out high-temperature heat treatment, heat treatment temperature is arranged between 900 DEG C, during insulation Between be 3.5h, cool to room temperature with the furnace, obtain the ferro-silicium powder after siliconising is heat-treated.Ferro-silicium powder in the present embodiment The Si contents (mass fraction) at end are 5.0wt%.
Step 2: the ferro-silicium powder after siliconising is heat-treated is placed in rotary tube furnace, with the heating of 23 DEG C/min Speed is warming up to 280 DEG C, in air atmosphere, 1.3h is kept the temperature under the conditions of 280 DEG C, during insulation rotary tube furnace rotating speed is 2.5RPM, then with stove cooled to room temperature, up to the iron silicon soft magnetic composite powder of multi-layer core-shell structure.It is prepared by the present embodiment Obtained composite powder is by inner core and is coated on the multi-layer core-shell structure that the shell of inner core outer layer forms, its inner core is Iron silicon soft magnetic particles, the external sheath of soft magnetic particles have Fe3Si, Fe3The outside of Si is coated with SiO2Insulating layer.
The magnetic property of iron silicon soft magnetic composite powder manufactured in the present embodiment is detected using VSM, the results showed that, this reality Composite powder obtained by applying example has excellent soft magnet performance, its saturation induction density is 168emu/g, coercivity 6Oe.Adopt Powder resistivity is tested with resistivity tester, the results showed that powder has higher resistivity, its resistivity is 4.3 ×10-5Ω·m。
Embodiment 7
A kind of preparation method of the iron silicon soft magnetic composite powder of multi-layer core-shell structure of the present embodiment, its specific steps is such as Under：
Step 1: be first uniformly mixed the high-purity nm silica flour of the ferro-silicium powder of 98.5wt% and 1.5wt%, then will The mixed-powder, which is placed in protection of reducing atmosphere stove, carries out high-temperature heat treatment, and heat treatment temperature is arranged between 1120 DEG C, Soaking time is 4h, cools to room temperature with the furnace, obtains the ferro-silicium powder after siliconising is heat-treated.Iron silicon closes in the present embodiment The Si contents (mass fraction) at bronze end are 6.5wt%.
Step 2: the ferro-silicium powder after siliconising is heat-treated is placed in rotary tube furnace, with 30 DEG C/min's Heating rate is warming up to 380 DEG C, keeps the temperature 0.8h, during insulation rotary tube furnace rotating speed under the conditions of 380 DEG C under oxygen atmosphere For 5RPM, then with stove cooled to room temperature, up to the iron silicon soft magnetic composite powder of multi-layer core-shell structure.It is prepared by the present embodiment Obtained composite powder is by inner core and is coated on the multi-layer core-shell structure that the shell of inner core outer layer forms, its inner core is Iron silicon soft magnetic particles, the external sheath of soft magnetic particles have Fe3Si, Fe3The outside of Si is coated with SiO2Insulating layer.
The magnetic property of iron silicon soft magnetic composite powder manufactured in the present embodiment is detected using VSM, the results showed that, this reality Composite powder obtained by applying example has excellent soft magnet performance, its saturation induction density is 174emu/g, coercivity 5Oe.Adopt Powder resistivity is tested with resistivity tester, the results showed that powder has higher resistivity, its resistivity is 5.2 ×10-5Ω·m。
Embodiment 8
A kind of preparation method of the iron silicon soft magnetic composite powder of multi-layer core-shell structure of the present embodiment, its specific steps is such as Under：
Step 1: be first uniformly mixed the high-purity nm silica flour of the ferro-silicium powder of 99.5wt% and 0.5wt%, then will The mixed-powder, which is placed in inert atmosphere protection stove, carries out high-temperature heat treatment, and heat treatment temperature is arranged between 1070 DEG C, Soaking time is 5h, cools to room temperature with the furnace, obtains the ferro-silicium powder after siliconising is heat-treated.Iron silicon closes in the present embodiment The Si contents (mass fraction) at bronze end are 2.5wt%.
Step 2: the ferro-silicium powder after siliconising is heat-treated is placed in rotary tube furnace, with 18 DEG C/min's Heating rate is warming up to 410 DEG C, keeps the temperature 0.5h, during insulation rotary tube furnace rotating speed under the conditions of 410 DEG C in air atmosphere For 4.5RPM, then with stove cooled to room temperature, up to the iron silicon soft magnetic composite powder of multi-layer core-shell structure.The present embodiment system Standby obtained composite powder is by inner core and is coated on the multi-layer core-shell structure that the shell of inner core outer layer forms, its inner core For iron silicon soft magnetic particles, the external sheath of soft magnetic particles has Fe3Si, Fe3The outside of Si is coated with SiO2Insulating layer.
The magnetic property of iron silicon soft magnetic composite powder manufactured in the present embodiment is detected using VSM, the results showed that, this reality Composite powder obtained by applying example has excellent soft magnet performance, its saturation induction density is 172emu/g, coercivity 8Oe.Adopt Powder resistivity is tested with resistivity tester, the results showed that powder has higher resistivity, its resistivity is 4.4 ×10-5Ω·m。
1-8 can be drawn in conjunction with the embodiments, and it is high, electric that saturation induction density can be prepared in method using the present invention The iron silicon soft magnetic composite powder that resistance rate is high, eddy-current loss is low and heat endurance is good, so as to meet that existing electricity-magnetic converting means is standby to height The requirement that frequencyization direction is developed, and its preparation process is simple, production cost and investment are low, production efficiency is high, to environment without Pollution, gained composite powder can meet the requirement to work at higher ambient temperatures for a long time.

Claims (9)

  1. A kind of 1. iron silicon soft magnetic composite powder of multi-layer core-shell structure, it is characterised in that：The composite powder is by inner core and bag The multi-layer core-shell structure of the shell composition of inner core outer layer is overlying on, its inner core is iron silicon soft magnetic particles, the outer layer of soft magnetic particles It is coated with Fe3Si, Fe3The outside of Si is coated with SiO2Insulating layer, the saturation induction density of the composite powder for 153~ 174emu/g, coercivity are 5~8Oe, and resistivity is 4.3 × 10-5~3.1 × 10-4Ω·m。
  2. 2. a kind of preparation method of the iron silicon soft magnetic composite powder of multi-layer core-shell structure as claimed in claim 1, its feature exist In：Ferro-silicium powder is first subjected to siliconising heat treatment, is subsequently placed under oxidizing atmosphere and carries out oxidation processes, and is closed by controlling The siliconising heat treatment of reason and oxidation processing technique, so as to obtain the iron silicon soft magnetic composite powder for possessing multi-layer core-shell structure.
  3. 3. a kind of preparation method of the iron silicon soft magnetic composite powder of multi-layer core-shell structure according to claim 2, its feature It is, it is comprised the following steps that：
    Step 1: ferro-silicium powder and nano silica fume are uniformly mixed, then by gained mixed-powder in the bar of starvation High-temperature heat treatment is carried out under part, heat treatment temperature is 900~1150 DEG C, and soaking time is 1~5h, cools to room with the furnace afterwards Temperature, obtains the ferro-silicium powder after siliconising is heat-treated；
    Step 2: the ferro-silicium powder after siliconising is heat-treated is heated to 200 with the heating rate of 10~30 DEG C/min~ 450 DEG C, 0.5~2h then is kept the temperature in 200~450 DEG C under oxidizing atmosphere, room temperature is cooled to the furnace afterwards, up to multi-layer core-shell The iron silicon soft magnetic composite powder of structure.
  4. 4. a kind of preparation method of the iron silicon soft magnetic composite powder of multi-layer core-shell structure according to claim 3, its feature It is：The mass percentage content of ferro-silicium powder is 90~99.5% in gained mixed-powder in the step 1, nanometer The mass percentage content of silica flour is 0.5~10%.
  5. 5. a kind of preparation method of the iron silicon soft magnetic composite powder of multi-layer core-shell structure according to claim 3 or 4, it is special Sign is：Mixed-powder is placed in high-temperature vacuum furnace, inert atmosphere protection stove or protection of reducing atmosphere stove in the step 1 Carry out high-temperature heat treatment.
  6. 6. a kind of preparation method of the iron silicon soft magnetic composite powder of multi-layer core-shell structure according to claim 3 or 4, it is special Sign is：Ferro-silicium powder after siliconising is heat-treated in the step 2 is placed in rotary tube furnace and carries out oxidation processes, and The rotating speed of during insulation rotary tube furnace is 2~7RPM.
  7. 7. a kind of preparation method of the iron silicon soft magnetic composite powder of multi-layer core-shell structure according to claim 6, its feature It is：The particle diameter of the ferro-silicium powder is less than 150 μm, and the Si contents of ferro-silicium powder are 0.5~7.0wt%.
  8. 8. a kind of preparation method of the iron silicon soft magnetic composite powder of multi-layer core-shell structure according to claim 6, its feature It is：The particle diameter of the nano silica fume is less than 200nm, and the mass fraction of the Si in nano silica fume is more than 99.5wt%.
  9. 9. a kind of preparation method of the iron silicon soft magnetic composite powder of multi-layer core-shell structure according to claim 8, its feature It is：Oxidizing atmosphere in the step 2 is air or oxygen.
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