CN108899152A - A kind of more insulating layer iron silicon substrate soft magnetic-powder cores and preparation method thereof - Google Patents
A kind of more insulating layer iron silicon substrate soft magnetic-powder cores and preparation method thereof Download PDFInfo
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- CN108899152A CN108899152A CN201810708484.3A CN201810708484A CN108899152A CN 108899152 A CN108899152 A CN 108899152A CN 201810708484 A CN201810708484 A CN 201810708484A CN 108899152 A CN108899152 A CN 108899152A
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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
Abstract
The invention discloses a kind of more insulating layer iron silicon substrate soft magnetic-powder cores and preparation method thereof.Its technical solution is：Ferro-silicium powder is placed in 0.5~3h of stirring under 100~260 DEG C of water vapor, obtains composite powder.Composite powder is dried in vacuo, mold is packed into, the cold moudling under the conditions of 300~1200MPa obtains green body.Green body is placed in high temperature sintering furnace, under vacuum conditions or under the conditions of protective atmosphere, 800~1300 DEG C is warming up to, is sintered 0.5~5h, obtains sintered body.Sintered body is placed in heat-treatment furnace, under vacuum conditions or under the conditions of protective atmosphere, 500~1200 DEG C is warming up to, is heat-treated 0.5~5h, more insulating layer iron silicon substrate soft magnetic-powder cores are made in furnace cooling.Present invention process is simply and with short production cycle, and the insulating coating of prepared more insulating layer iron silicon substrate soft magnetic-powder cores is uniform and thin, and eddy-current loss is low, saturation induction density is high low with coercivity.
Description
Technical field
The invention belongs to iron silicon substrate soft magnetic-powder core technical fields.More particularly to a kind of more insulating layer iron silicon substrate soft magnetic-powder cores and
Preparation method.
Background technique
Iron silicon substrate soft magnetic-powder core is because of its high magnetic permeability, low-loss, low magnetostriction, excellent thermal stability and direct current biasing
Ability, the magnetic element indispensable as power circuit, is widely used in inverter, inductor, transformer and choke coil etc.
In electronic component, it is related to the various fields such as motor, telecommunication, power supply.
It is noted that with the raising of frequency of use, the eddy-current loss grow exponentially of soft magnetic-powder core, and it is magnetic
The insulating wrapped of particle, which is undoubtedly, reduces eddy-current loss most efficient method.On this basis, insulating wrapped is broadly divided into organic
It coats and two kinds of inorganic coating.The machine method for coating of common are is that magnetic-particle and organic coating material are mixed in acetone or alcohol
It is dry after being sufficiently stirred in equal organic solvents, soft magnetic composite powder is obtained, is further compacted and heat treatment obtains soft magnet powder
Core, it is easy to operate, cost is relatively low and covered effect is preferable.However, traditional organic coating material such as phenolic resin, epoxy resin etc.
Heat resistance is poor, and high-temperature heat treatment can not be carried out at 200 DEG C or more and eliminates high temperature residual stress, affects magnetic property.And have
The soft magnetic-powder core of machine material cladding generates heat in long-term work because of eddy-current loss, will lead to organic insulator aging, or even heat
It decomposes, to weaken the insulating properties of soft magnetic-powder core, increase eddy-current loss and influence the stability of soft magnetic-powder core.Therefore, inorganic
Covering material is concerned with its excellent chemical and thermal stability and electrical insulating property.
Common inorganic coating material mainly has phosphate, oxide (Al2O3、MgO、SiO2Deng) and soft magnetic ferrite, it is common
Method for coating be then by simply stirring or magnetic-particle and inorganic insulation are coated material and glue by the physical methods such as ball milling
Agent mixing is tied, high pressure compaction moulding is carried out later, finally obtains soft magnetic-powder core；In addition, there are also co-precipitation and collosol and gels
Equal chemical clading process.The above method for coating, most important purpose be to carry out insulating wrapped to magnetic-particle, and how will be every
The uniform and fine and close cladding of a magnetic-particle is got up, and realizes effective insulation between magnetic-particle, it appears particularly important.
For this purpose, scientific and technical personnel have carried out extensive research, such as " a kind of metal soft magnetic powder core inorganic insulation bonding agent and its system
Preparation Method " (CN200710099337.2) patented technology directly mixes magnetic-particle with the inorganic oxide being electrically insulated, preparation
Method is simple, but the effective insulation being difficult to realize between magnetic-particle, and loss reduction is limited, and will cause the group of inorganic coating material
It is poly-, deteriorate magnetic property.And " a kind of method for coating of metal soft magnetic composite material powder and the preparation method of magnet "
(CN201310351622.4) patented technology coats Al on iron particle surface by sol-gel method2O3, the system of sol-gel
Standby process is complicated, and single yield is few, can not expanding production, and material loss is more, higher cost.In addition, a kind of " iron-based soft magnetic
Alloy powder method for coating and soft-magnetic composite material preparation method " (CN201510602786.9) patented technology passes through high-temperature oxydation
Oxide layer is obtained, then iron oxide is gone in pickling, is left containing SiO2、Al2O3And Cr2O3Etc. oxide layers, finally add binder
It is compacted with lubricant, obtains soft-magnetic composite material.The insulating layer of gained soft-magnetic composite material is more uniform, magnetic property compared with
It is good, but preparation process is complicated, operation is not easy, energy and material loss are more and be unfavorable for largely preparing.
Summary of the invention
The present invention is directed to overcome above-mentioned technological deficiency, and it is an object of the present invention to provide a kind of simple process and it is with short production cycle mostly absolutely
The preparation method of edge layer iron silicon substrate soft magnetic-powder core；With the insulating bag of more insulating layer iron silicon substrate soft magnetic-powder cores prepared by the preparation method
Coating is uniform and thin, and eddy-current loss is low, saturation induction density is high low with coercivity.
To achieve the above object, the step of the technical solution adopted by the present invention is：
The first step, composite powder preparation
Ferro-silicium powder is placed in the water vapour, stirs 0.5 under the conditions of steam temperature is 100~260 DEG C
~3h, obtains composite powder.
Second step, cold moudling
The composite powder is dried in vacuo, mold is packed into, the cold moudling under the conditions of 300~1200MPa obtains
Green body.
Third step, sintering
The green body is placed in high temperature sintering furnace, under vacuum conditions or under the conditions of protective atmosphere, it is warming up to 800~
1300 DEG C, it is sintered 0.5~5h, obtains sintered body.
4th step, heat treatment
The sintered body is placed in heat-treatment furnace, under vacuum conditions or under the conditions of protective atmosphere, is warming up to 500
~1200 DEG C, it is heat-treated 0.5~5h, more insulating layer iron silicon substrate soft magnetic-powder cores are made in furnace cooling.
The partial size of the ferro-silicium powder is 1~200 μm, and the Si content of ferro-silicium powder is 1.5~10wt%.
The revolving speed of the stirring is 50~200 revs/min.
The vacuum drying time is 12~36h, and vacuum drying temperature is 40~70 DEG C.
The vacuum degree of the vacuum is 10-2~102Pa。
The protective atmosphere is nitrogen or argon gas.
Due to the adoption of the above technical scheme, the present invention has following advantages compared with prior art：
(1) ferro-silicium powder is placed in 100~260 DEG C of water vapor and stirs by the present invention, by water vapour plus
The superficial oxidation of fast ferro-silicium powder, obtains that kernel is ferro-silicium, shell is ferriferous oxide and elemental silicon mixing clad
Composite powder, it is dry after composite powder cold moudling and high temperature sintering and heat treatment, using the diffusion of high temperature with
And the chemical reaction under high temperature between ferriferous oxide and elemental silicon, so that it is spontaneously formed SiO2And Fe2SiO4More insulating layers of composition are special
Different structure is to get more insulating layer iron silicon substrate soft magnetic-powder cores.The raw materials used in the present invention is only ferro-silicium powder, is not added any viscous
Agent and lubricant etc. are tied, considerably reduces material loss, non-environmental-pollution, and steam oxidation process is simple to operation.Cause
And preparation cost is low and technique is simple, has a good application prospect.
(2) ferro-silicium powder is placed in 100~260 DEG C of water vapor by the present invention stirs, and passes through water vapour pair
Ferro-silicium powder carries out accelerated oxidation, and in oxidation process, water vapour comes into full contact with ferro-silicium particle surface layer, makes the conjunction of iron silicon
Gold particle surface quickly forms the mixing clad of ferriferous oxide and elemental silicon, highly shortened the production cycle.
(3) present invention carries out shallow-layer oxidation to ferro-silicium powder surface using water vapour, obtains ferriferous oxide and simple substance
The mixing clad of silicon, so that further oxidation of the water vapour to ferro-silicium powder is prevented, thus clad is uniform and thin, institute
The saturation induction density of more insulating layer iron silicon substrate soft magnetic-powder cores of preparation is higher and coercivity is lower.
(4) insulating materials of more insulating layer iron silicon substrate soft magnetic-powder cores prepared by the present invention is inorganic material, chemical stability
Good and tolerable high temperature, thus high-temperature heat treatment not only promotes the shape of more insulating layers of more insulating layer iron silicon substrate soft magnetic-powder cores
At during which ferriferous oxide has decomposited part Fe, and completely eliminates the internal stress of the factors such as pressure introducing, improves more insulation
Layer iron silicon substrate soft magnetic-powder core saturation induction density and reduce its coercivity.
(5) the ferro-silicium particle of more insulating layer iron silicon substrate soft magnetic-powder cores prepared by the present invention is by SiO2And Fe2SiO4Composition
More insulating layers separate, clad is uniform, therefore is formed by between clad can effectively realize ferro-silicium particle and insulate, thus
Reduce the eddy-current loss of more insulating layer iron silicon substrate soft magnetic-powder cores.
(6) present invention passes through the temperature in the technological parameter of adjusting steam oxidation process, briquetting pressure, high-temperature sintering process
The parameters such as the temperature and time in degree and time, heat treatment process can carry out Effective Regulation to the thickness of clad, to be made
More insulating layer iron silicon substrate soft magnetic-powder cores of different magnetic properties.
Therefore, present invention process simply and with short production cycle, the insulation of prepared more insulating layer iron silicon substrate soft magnetic-powder cores
Clad is uniform and thin, and eddy-current loss is low, saturation induction density is high low with coercivity.
Detailed description of the invention
Fig. 1 is a kind of SEM figure of iron silicon substrate soft magnetic-powder core prepared by the present invention.
Specific embodiment
The invention will be further described with embodiment with reference to the accompanying drawing, not to the limitation of its protection scope.
It is first that technical parameter Unify legislation involved in present embodiment is as follows to avoid repeating, in embodiment not
It repeats again：
The vacuum drying time is 12~36h, and vacuum drying temperature is 40~70 DEG C, vacuum drying vacuum degree
It is 10-2~102Pa。
Vacuum degree under the vacuum condition is 10-2~102Pa。
Embodiment 1
A kind of more insulating layer iron silicon substrate soft magnetic-powder cores and preparation method thereof.It is the step of preparation method described in the present embodiment：
The first step, composite powder preparation
Ferro-silicium powder is placed in water vapour, stirs 0.5 under the conditions of the steam temperature is 100~150 DEG C
~1h, obtains composite powder.
Second step, cold moudling
The composite powder is dried in vacuo, mold is packed into, the cold moudling under the conditions of 300~600MPa obtains
Green body.
Third step, sintering
The green body is placed in high temperature sintering furnace, is warming up to 800~900 DEG C under vacuum conditions, is sintered 0.5~1h,
Obtain sintered body.
4th step, heat treatment
The sintered body is placed in heat-treatment furnace, is warming up to 900~1200 DEG C under vacuum conditions, heat treatment 4.5
More insulating layer iron silicon substrate soft magnetic-powder cores are made in~5h, furnace cooling.
The partial size of the ferro-silicium powder is 1~60 μm, and the Si content of ferro-silicium powder is 1.5~6wt%.
The revolving speed of the stirring is 50~100 revs/min.
The protective atmosphere is nitrogen.
Embodiment 2
A kind of more insulating layer iron silicon substrate soft magnetic-powder cores and preparation method thereof.It is the step of preparation method described in the present embodiment：
The first step, composite powder preparation
Ferro-silicium powder is placed in water vapour, the steam temperature be 130~180 DEG C under the conditions of stirring 1~
1.5h obtains composite powder.
Second step, cold moudling
The composite powder is dried in vacuo, mold is packed into, the cold moudling under the conditions of 450~750MPa obtains
Green body.
Third step, sintering
The green body is placed in high temperature sintering furnace, 900~1000 DEG C are warming up under the conditions of protective atmosphere, sintering
1.5~2h obtains sintered body.
4th step, heat treatment
The sintered body is placed in heat-treatment furnace, is warming up to 800~1100 DEG C under the conditions of protective atmosphere, at heat
3.5~4h is managed, more insulating layer iron silicon substrate soft magnetic-powder cores are made in furnace cooling.
The partial size of the ferro-silicium powder is 35~95 μm, and the Si content of ferro-silicium powder is 3~7wt%.
The revolving speed of the stirring is 75~125 revs/min.
The protective atmosphere is argon gas.
Embodiment 3
A kind of more insulating layer iron silicon substrate soft magnetic-powder cores and preparation method thereof.It is the step of preparation method described in the present embodiment：
The first step, composite powder preparation
Ferro-silicium powder is placed in water vapour, stirs 1.5 under the conditions of the steam temperature is 160~210 DEG C
~2h, obtains composite powder.
Second step, cold moudling
The composite powder is dried in vacuo, mold is packed into, the cold moudling under the conditions of 600~900MPa obtains
Green body.
Third step, sintering
The green body is placed in high temperature sintering furnace, is warming up to 1000~1100 DEG C under vacuum conditions, sintering 2.5~
3h obtains sintered body.
4th step, heat treatment
The sintered body is placed in heat-treatment furnace, is warming up to 700~1000 DEG C under vacuum conditions, heat treatment 2.5
More insulating layer iron silicon substrate soft magnetic-powder cores are made in~3h, furnace cooling.
The partial size of the ferro-silicium powder is 70~130 μm, and the Si content of ferro-silicium powder is 4~8wt%.
The revolving speed of the stirring is 100~150 revs/min.
The protective atmosphere is argon gas.
Embodiment 4
A kind of more insulating layer iron silicon substrate soft magnetic-powder cores and preparation method thereof.It is the step of preparation method described in the present embodiment：
The first step, composite powder preparation
Ferro-silicium powder is placed in water vapour, the steam temperature be 190~240 DEG C under the conditions of stirring 2~
2.5h obtains composite powder.
Second step, cold moudling
The composite powder is dried in vacuo, mold is packed into, the cold moudling under the conditions of 750~1050MPa obtains
Green body.
Third step, sintering
The green body is placed in high temperature sintering furnace, 1100~1200 DEG C are warming up under the conditions of protective atmosphere, sintering
3.5~4h obtains sintered body.
4th step, heat treatment
The sintered body is placed in heat-treatment furnace, is warming up to 600~900 DEG C under the conditions of protective atmosphere, at heat
1.5~2h is managed, more insulating layer iron silicon substrate soft magnetic-powder cores are made in furnace cooling.
The partial size of the ferro-silicium powder is 105~165 μm, and the Si content of ferro-silicium powder is 5~9wt%.
The revolving speed of the stirring is 125~175 revs/min.
The protective atmosphere is argon gas.
Embodiment 5
A kind of more insulating layer iron silicon substrate soft magnetic-powder cores and preparation method thereof.It is the step of preparation method described in the present embodiment：
The first step, composite powder preparation
Ferro-silicium powder is placed in water vapour, stirs 2.5 under the conditions of the steam temperature is 220~260 DEG C
~3h, obtains composite powder.
Second step, cold moudling
The composite powder is dried in vacuo, mold is packed into, the cold moudling under the conditions of 900~1200MPa obtains
Green body.
Third step, sintering
The green body is placed in high temperature sintering furnace, is warming up to 1200~1300 DEG C under vacuum conditions, sintering 4.5~
5h obtains sintered body.
4th step, heat treatment
The sintered body is placed in heat-treatment furnace, is warming up to 500~800 DEG C under the conditions of protective atmosphere, at heat
0.5~1h is managed, more insulating layer iron silicon substrate soft magnetic-powder cores are made in furnace cooling.
The partial size of the ferro-silicium powder is 140~200 μm, and the Si content of ferro-silicium powder is 7~10wt%.
The revolving speed of the stirring is 150~200 revs/min.
The protective atmosphere is nitrogen.
Present embodiment has following advantages compared with prior art：
(1) ferro-silicium powder is placed in 100~260 DEG C of water vapor and stirs by the present invention, by water vapour plus
The superficial oxidation of fast ferro-silicium powder, obtains that kernel is ferro-silicium, shell is ferriferous oxide and elemental silicon mixing clad
Composite powder, it is dry after composite powder cold moudling and high temperature sintering and heat treatment, using the diffusion of high temperature with
And the chemical reaction under high temperature between ferriferous oxide and elemental silicon, so that it is spontaneously formed SiO2And Fe2SiO4More insulating layers of composition are special
Different structure is to get more insulating layer iron silicon substrate soft magnetic-powder cores.The raw materials used in the present invention is only ferro-silicium powder, is not added any viscous
Agent and lubricant etc. are tied, considerably reduces material loss, non-environmental-pollution, and steam oxidation process is simple to operation.Cause
And preparation cost is low, technique is simple and reproducible, has a good application prospect.
(2) ferro-silicium powder is placed in 100~260 DEG C of water vapor by the present invention stirs, and passes through water vapour pair
Ferro-silicium powder carries out accelerated oxidation, and in oxidation process, water vapour comes into full contact with ferro-silicium particle surface layer, makes the conjunction of iron silicon
Gold particle surface quickly forms the mixing clad of ferriferous oxide and elemental silicon, highly shortened the production cycle.
(3) present invention carries out shallow-layer oxidation to ferro-silicium powder surface using water vapour, obtains ferriferous oxide and simple substance
The mixing clad of silicon, so that further oxidation of the water vapour to ferro-silicium powder is prevented, thus clad is uniform and thin, such as
Shown in Fig. 1, Fig. 1 is that a kind of SEM of more insulating layer iron silicon substrate soft magnetic-powder cores prepared by embodiment 3 schemes (backscatter images), from Fig. 1
It can be seen that：Clad between iron silicon particle is uniform and relatively thin, the saturation magnetic of prepared more insulating layer iron silicon substrate soft magnetic-powder cores
Induction is higher and coercivity is lower.
(4) insulating materials of more insulating layer iron silicon substrate soft magnetic-powder cores prepared by the present invention is inorganic material, chemical stability
Good and tolerable high temperature, thus high-temperature heat treatment not only promotes the shape of more insulating layers of more insulating layer iron silicon substrate soft magnetic-powder cores
At during which ferriferous oxide has decomposited part Fe, and completely eliminates the internal stress of the factors such as pressure introducing, improves more insulation
Layer iron silicon substrate soft magnetic-powder core saturation induction density and reduce its coercivity.
(5) the ferro-silicium particle of more insulating layer iron silicon substrate soft magnetic-powder cores prepared by the present invention is by SiO2And Fe2SiO4Composition
More insulating layers separate, clad is uniform.From Fig. 1 it can also be seen that：Ferro-silicium particle is by with SiO2Based on SiO2-
Fe2SiO4More insulating layers separate, therefore are formed by between clad can effectively realize ferro-silicium particle and insulate, to reduce more
The eddy-current loss of insulating layer iron silicon substrate soft magnetic-powder core.
(5) present invention passes through the temperature in the technological parameter of adjusting steam oxidation process, briquetting pressure, high-temperature sintering process
The parameters such as the temperature and time in degree and time, heat treatment process can carry out Effective Regulation to the thickness of clad, to be made
More insulating layer iron silicon substrate soft magnetic-powder cores of different magnetic properties.
Therefore, present invention process simply and with short production cycle, the insulation of prepared more insulating layer iron silicon substrate soft magnetic-powder cores
Clad is uniform and thin, and eddy-current loss is low, saturation induction density is high low with coercivity.
Claims (7)
1. a kind of preparation method of more insulating layer iron silicon substrate soft magnetic-powder cores, it is characterised in that the step of preparation method is：
The first step, composite powder preparation
Ferro-silicium powder is placed in water vapour, 0.5~3h is stirred under the conditions of the steam temperature is 100~260 DEG C,
Obtain composite powder；
Second step, cold moudling
The composite powder is dried in vacuo, mold is packed into, the cold moudling under the conditions of 300~1200MPa obtains base
Body；
Third step, sintering
The green body is placed in high temperature sintering furnace, is warming up to 800~1300 under vacuum conditions or under the conditions of protective atmosphere
DEG C, it is sintered 0.5~5h, obtains sintered body；
4th step, heat treatment
The sintered body is placed in heat-treatment furnace, it is warming up to 500 under vacuum conditions or under the conditions of protective atmosphere~
1200 DEG C, it is heat-treated 0.5~5h, more insulating layer iron silicon substrate soft magnetic-powder cores are made in furnace cooling.
2. the preparation method of more insulating layer iron silicon substrate soft magnetic-powder cores according to claim 1, it is characterised in that the iron silicon
The partial size of alloy powder is 1~200 μm, and the Si content of ferro-silicium powder is 1.5~10wt%.
3. the preparation method of more insulating layer iron silicon substrate soft magnetic-powder cores according to claim 1, it is characterised in that the stirring
Revolving speed be 50~200 revs/min.
4. the preparation method of more insulating layer iron silicon substrate soft magnetic-powder cores according to claim 1, it is characterised in that the vacuum
The dry time is 12~36h, and vacuum drying temperature is 40~70 DEG C.
5. the preparation method of more insulating layer iron silicon substrate soft magnetic-powder cores according to claim 1, it is characterised in that described is true
Empty vacuum degree is 10-2~102Pa。
6. the preparation method of more insulating layer iron silicon substrate soft magnetic-powder cores according to claim 1, it is characterised in that the protection
Property atmosphere be nitrogen or argon gas.
7. a kind of more insulating layer iron silicon substrate soft magnetic-powder cores, it is characterised in that：More insulating layer iron silicon substrate soft magnetic-powder cores are bases
More insulating layer iron of the preparation method preparation of more insulating layer iron silicon substrate soft magnetic-powder cores described in any one of claim 1~6
Silicon substrate soft magnetic-powder core.
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| CN112420309A (en) * | 2019-08-21 | 2021-02-26 | Tdk株式会社 | Dust core |
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| CN108899152B (en) | 2019-12-24 |
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