CN108899152B - Multi-insulation-layer Fe-Si-based soft magnetic powder core and preparation method thereof - Google Patents
Multi-insulation-layer Fe-Si-based soft magnetic powder core and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a multi-insulation-layer iron-silicon-based soft magnetic powder core and a preparation method thereof. The technical scheme is as follows: and (3) placing the iron-silicon alloy powder in a water vapor environment at the temperature of 100-260 ℃ and stirring for 0.5-3 h to obtain the composite powder. And (3) carrying out vacuum drying on the composite powder, loading the composite powder into a mold, and carrying out cold press molding under the condition of 300-1200 MPa to obtain a blank. And (3) placing the green body in a high-temperature sintering furnace, heating to 800-1300 ℃ under a vacuum condition or a protective atmosphere condition, and sintering for 0.5-5 h to obtain a sintered green body. And (3) placing the sintered blank in a heat treatment furnace, heating to 500-1200 ℃ under the vacuum condition or protective atmosphere condition, carrying out heat treatment for 0.5-5 h, and cooling along with the furnace to obtain the multi-insulation-layer iron-silicon-based soft magnetic powder core. The invention has simple process and short production period, and the prepared multi-insulation-layer iron-silicon-based soft magnetic powder core has uniform and thin insulation coating layers, low eddy current loss, high saturation magnetic induction intensity and low coercive force.
Description
Technical Field
The invention belongs to the technical field of iron-silicon-based soft magnetic powder cores. In particular to a multi-insulation layer iron-silicon-based soft magnetic powder core and a preparation method thereof.
Background
The iron-silicon-based soft magnetic powder core is used as an indispensable magnetic element of a power circuit due to high magnetic conductivity, low loss, low magnetostriction, excellent thermal stability and direct current bias capability, is widely applied to electronic components such as inverters, inductors, transformers, chokes and the like, and relates to the fields of motors, telecommunication, power supplies and the like.
It is worth mentioning that the eddy current loss of the soft magnetic powder core increases exponentially with the increase of the frequency of use, and the insulating coating of the magnetic particles is undoubtedly the most effective method for reducing the eddy current loss. On the basis, the insulation coating is mainly divided into an organic coating and an inorganic coating. The common organic coating method is to mix the magnetic particles and the organic coating material in organic solvents such as acetone or ethanol, fully stir and dry the mixture to obtain soft magnetic composite powder, and obtain the soft magnetic powder core through further compaction and heat treatment, and the method has the advantages of simple operation, low cost and good coating effect. However, the conventional organic coating materials such as phenolic resin, epoxy resin and the like have poor heat resistance, and cannot be subjected to high-temperature heat treatment at a temperature of more than 200 ℃ and eliminate high-temperature residual stress, thereby affecting the magnetic performance. And the soft magnetic powder core coated by the organic material generates heat due to eddy current loss in long-term operation, so that the organic insulating layer is aged and even thermally decomposed, the insulativity of the soft magnetic powder core is weakened, the eddy current loss is increased, and the stability of the soft magnetic powder core is influenced. Therefore, the inorganic coating material is receiving attention for its excellent chemical and thermal stability and electrical insulation.
Common inorganic coating materials mainly include phosphate and oxide (Al)2O3、MgO、SiO2Etc.) and soft magnetic ferrite, the common coating method is to mix the magnetic particles with the inorganic insulating coating material and the binder by physical methods such as simple stirring or ball milling, and then to carry out high-strength pressure compaction molding to finally obtain the soft magnetic powder core; in addition, there are chemical coating processes such as coprecipitation and sol-gel. The above coating method mainly aims at insulating and coating the magnetic particles, and how to uniformly and densely coat each magnetic particle to achieve effective insulation between the magnetic particles is very important.
For this reason, technologists have conducted extensive studies, such as "an inorganic insulating adhesive for metal soft magnetic powder core and a method for preparing the same" (CN200710099337.2) patent technology in which magnetic particles are directly mixed with an electrically insulating inorganic oxide, the preparation method is simple, but effective insulation between the magnetic particles is difficult to achieve, loss reduction is limited, and agglomeration of inorganic coating materials is caused, deteriorating magnetic properties. The patent of "a method for coating powder for metallic soft magnetic composite material and a method for preparing magnet" (CN201310351622.4) discloses a method for coating Al on the surface of iron particles by sol-gel method2O3The preparation process of the sol-gel is complex, the single yield is less, the production cannot be expanded, the raw material loss is more, and the cost is higher. In addition, the patent technology of 'an iron-based soft magnetic alloy powder coating method and a soft magnetic composite material preparation method' (CN201510602786.9) obtains an oxide layer by high-temperature oxidation, and then removes iron oxide by acid cleaning to leave SiO-containing powder2、Al2O3And Cr2O3And (5) waiting for the oxide layer, and finally adding a binder and a lubricant for compacting to obtain the soft magnetic composite material. The insulating layer of the obtained soft magnetic composite material is uniform, the magnetic property is good, but the preparation process is complex, the operation is not easy, the energy and raw material loss is more, and the mass preparation is not facilitated.
Disclosure of Invention
The invention aims to overcome the technical defects and provides a preparation method of a multi-insulation-layer iron-silicon-based soft magnetic powder core with simple process and short production period; the multi-insulation-layer iron-silicon-based soft magnetic powder core prepared by the preparation method has the advantages of uniform and thin insulation coating layer, low eddy current loss, high saturation magnetic induction intensity and low coercive force.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
first step, composite powder preparation
And (3) placing the iron-silicon alloy powder into the water vapor, and stirring for 0.5-3 h at the water vapor temperature of 100-260 ℃ to obtain the composite powder.
Second step, cold press forming
And (3) carrying out vacuum drying on the composite powder, loading the composite powder into a mold, and carrying out cold press molding under the condition of 300-1200 MPa to obtain a blank body.
Third step, sintering
And (3) placing the blank body in a high-temperature sintering furnace, heating to 800-1300 ℃ under a vacuum condition or a protective atmosphere condition, and sintering for 0.5-5 h to obtain a sintered blank body.
Fourth, heat treatment
And (3) placing the sintered blank in a heat treatment furnace, heating to 500-1200 ℃ under the vacuum condition or protective atmosphere condition, carrying out heat treatment for 0.5-5 h, and cooling along with the furnace to obtain the multi-insulation-layer iron-silicon-based soft magnetic powder core.
The particle size of the iron-silicon alloy powder is 1-200 mu m, and the Si content of the iron-silicon alloy powder is 1.5-10 wt%.
The rotating speed of the stirring is 50-200 revolutions per minute.
The vacuum drying time is 12-36 h, and the vacuum drying temperature is 40-70 ℃.
The vacuum degree of the vacuum is 10-2～102Pa。
The protective atmosphere is nitrogen or argon.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following advantages:
(1) the method comprises the steps of placing iron-silicon alloy powder in a water vapor environment at 100-260 ℃ for stirring, accelerating the surface oxidation of the iron-silicon alloy powder through water vapor to obtain composite powder with an iron-silicon alloy core and an iron oxide and simple substance silicon mixed coating layer on a shell, carrying out cold press molding, high-temperature sintering and heat treatment on the dried composite powder, and carrying out spontaneous SiO formation on the composite powder by utilizing the diffusion effect at high temperature and the chemical reaction between the iron oxide and the simple substance silicon at high temperature2And Fe2SiO4The multi-insulation layer special structure is formed, and the multi-insulation layer iron-silicon-based soft magnetic powder core is obtained. The raw materials used in the invention are only iron-silicon alloy powder, and no binder, lubricant and the like are added, so that the raw material loss is greatly reduced, the environment pollution is avoided, and the steam oxidation process is simple and easy to operate. Therefore, the preparation cost is low, the process is simple, and the application prospect is good.
(2) According to the invention, the iron-silicon alloy powder is placed in a water vapor environment at 100-260 ℃ and stirred, the iron-silicon alloy powder is subjected to accelerated oxidation through water vapor, and in the oxidation process, the water vapor is fully contacted with the surface layer of the iron-silicon alloy particles, so that a mixed coating layer of iron oxide and simple substance silicon is rapidly formed on the surface of the iron-silicon alloy particles, and the production period is greatly shortened.
(3) According to the invention, the surface of the iron-silicon alloy powder is subjected to shallow oxidation by adopting water vapor to obtain the mixed coating layer of the iron oxide and the elemental silicon, so that the iron-silicon alloy powder is prevented from being further oxidized by the water vapor, the coating layer is uniform and thin, and the prepared multi-insulation-layer iron-silicon-based soft magnetic powder core has higher saturation magnetic induction intensity and lower coercive force.
(4) The insulating material of the multi-insulating-layer Fe-Si-based soft magnetic powder core prepared by the invention is an inorganic material, has good chemical stability and can resist high temperature, so that the high-temperature heat treatment not only promotes the formation of the multi-insulating layer of the multi-insulating-layer Fe-Si-based soft magnetic powder core, but also completely eliminates the internal stress caused by factors such as pressure and the like during the formation of the multi-insulating layer Fe-Si-based soft magnetic powder core, improves the saturation magnetic induction intensity of the multi-insulating-layer Fe-Si-based soft magnetic powder core and reduces the coercive force of the multi.
(5) The multi-insulation layer iron silicon prepared by the inventionIron-silicon alloy particle coating SiO based on soft magnetic powder core2And Fe2SiO4The formed multiple insulating layers are separated, and the coating layers are uniform, so that the formed coating layers can effectively realize insulation among iron-silicon alloy particles, and the eddy current loss of the iron-silicon-based soft magnetic powder core with the multiple insulating layers is reduced.
(6) The invention can effectively regulate and control the thickness of the coating layer by adjusting the technological parameters of the steam oxidation process, the forming pressure, the temperature and time in the high-temperature sintering process, the temperature and time in the heat treatment process and the like, thereby preparing the multi-insulation-layer iron-silicon-based soft magnetic powder core with different magnetic properties.
Therefore, the invention has simple process and short production period, and the prepared multi-insulation-layer iron-silicon-based soft magnetic powder core has uniform and thin insulation coating layers, low eddy current loss, high saturation magnetic induction intensity and low coercive force.
Drawings
FIG. 1 is an SEM image of an iron-silicon-based soft magnetic powder core prepared by the present invention.
Detailed Description
The invention is further described with reference to the following figures and examples, without limiting its scope.
In order to avoid repetition, the technical parameters related to this specific embodiment are uniformly described as follows, and are not described in detail in the embodiments:
the vacuum drying time is 12-36 h, the vacuum drying temperature is 40-70 ℃, and the vacuum degree of the vacuum drying is 10-2～102Pa。
The vacuum degree under the vacuum condition is 10-2～102Pa。
Example 1
A multi-insulation layer Fe-Si-based soft magnetic powder core and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
first step, composite powder preparation
And (3) placing the iron-silicon alloy powder into steam, and stirring for 0.5-1 h at the steam temperature of 100-150 ℃ to obtain the composite powder.
Second step, cold press forming
And (3) carrying out vacuum drying on the composite powder, loading the composite powder into a mold, and carrying out cold press molding under the condition of 300-600 MPa to obtain a blank.
Third step, sintering
And placing the blank in a high-temperature sintering furnace, heating to 800-900 ℃ under a vacuum condition, and sintering for 0.5-1 h to obtain a sintered blank.
Fourth, heat treatment
And (3) placing the sintered blank in a heat treatment furnace, heating to 900-1200 ℃ under a vacuum condition, carrying out heat treatment for 4.5-5 h, and cooling along with the furnace to obtain the multi-insulation-layer Fe-Si-based soft magnetic powder core.
The particle size of the iron-silicon alloy powder is 1-60 mu m, and the Si content of the iron-silicon alloy powder is 1.5-6 wt%.
The rotating speed of the stirring is 50-100 revolutions per minute.
The protective atmosphere is nitrogen.
Example 2
A multi-insulation layer Fe-Si-based soft magnetic powder core and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
first step, composite powder preparation
And (3) placing the iron-silicon alloy powder into steam, and stirring for 1-1.5 h under the condition that the temperature of the steam is 130-180 ℃ to obtain the composite powder.
Second step, cold press forming
And (3) carrying out vacuum drying on the composite powder, loading the composite powder into a mold, and carrying out cold press molding under the condition of 450-750 MPa to obtain a blank body.
Third step, sintering
And placing the green body in a high-temperature sintering furnace, heating to 900-1000 ℃ under the protective atmosphere condition, and sintering for 1.5-2 h to obtain a sintered green body.
Fourth, heat treatment
And (3) placing the sintered blank in a heat treatment furnace, heating to 800-1100 ℃ under the protective atmosphere condition, carrying out heat treatment for 3.5-4 h, and cooling along with the furnace to obtain the multi-insulation-layer Fe-Si-based soft magnetic powder core.
The particle size of the iron-silicon alloy powder is 35-95 mu m, and the Si content of the iron-silicon alloy powder is 3-7 wt%.
The rotating speed of the stirring is 75-125 revolutions per minute.
The protective atmosphere is argon.
Example 3
A multi-insulation layer Fe-Si-based soft magnetic powder core and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
first step, composite powder preparation
And (3) placing the iron-silicon alloy powder into water vapor, and stirring for 1.5-2 h at the temperature of 160-210 ℃ to obtain the composite powder.
Second step, cold press forming
And (3) carrying out vacuum drying on the composite powder, loading the composite powder into a mold, and carrying out cold press molding under the condition of 600-900 MPa to obtain a blank.
Third step, sintering
And placing the green body in a high-temperature sintering furnace, heating to 1000-1100 ℃ under a vacuum condition, and sintering for 2.5-3 h to obtain a sintered green body.
Fourth, heat treatment
And (3) placing the sintered blank in a heat treatment furnace, heating to 700-1000 ℃ under a vacuum condition, carrying out heat treatment for 2.5-3 h, and cooling along with the furnace to obtain the multi-insulation-layer Fe-Si-based soft magnetic powder core.
The particle size of the iron-silicon alloy powder is 70-130 mu m, and the Si content of the iron-silicon alloy powder is 4-8 wt%.
The rotating speed of the stirring is 100-150 revolutions per minute.
The protective atmosphere is argon.
Example 4
A multi-insulation layer Fe-Si-based soft magnetic powder core and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
first step, composite powder preparation
And (3) placing the iron-silicon alloy powder into water vapor, and stirring for 2-2.5 hours at the temperature of 190-240 ℃ of the water vapor to obtain the composite powder.
Second step, cold press forming
And (3) carrying out vacuum drying on the composite powder, loading the composite powder into a mold, and carrying out cold press molding under the condition of 750-1050 MPa to obtain a blank body.
Third step, sintering
And placing the green body in a high-temperature sintering furnace, heating to 1100-1200 ℃ under the protective atmosphere condition, and sintering for 3.5-4 h to obtain a sintered green body.
Fourth, heat treatment
And (3) placing the sintered blank in a heat treatment furnace, heating to 600-900 ℃ under the protective atmosphere condition, carrying out heat treatment for 1.5-2 h, and cooling along with the furnace to obtain the multi-insulation-layer Fe-Si-based soft magnetic powder core.
The particle size of the iron-silicon alloy powder is 105-165 mu m, and the Si content of the iron-silicon alloy powder is 5-9 wt%.
The rotating speed of the stirring is 125-175 revolutions per minute.
The protective atmosphere is argon.
Example 5
A multi-insulation layer Fe-Si-based soft magnetic powder core and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
first step, composite powder preparation
And (3) placing the iron-silicon alloy powder into steam, and stirring for 2.5-3 h at the steam temperature of 220-260 ℃ to obtain the composite powder.
Second step, cold press forming
And (3) carrying out vacuum drying on the composite powder, loading the composite powder into a mold, and carrying out cold press molding under the condition of 900-1200 MPa to obtain a blank body.
Third step, sintering
And (3) placing the blank body in a high-temperature sintering furnace, heating to 1200-1300 ℃ under a vacuum condition, and sintering for 4.5-5 h to obtain a sintered blank body.
Fourth, heat treatment
And (3) placing the sintered blank in a heat treatment furnace, heating to 500-800 ℃ under the protective atmosphere condition, carrying out heat treatment for 0.5-1 h, and cooling along with the furnace to obtain the multi-insulation-layer Fe-Si-based soft magnetic powder core.
The particle size of the iron-silicon alloy powder is 140-200 mu m, and the Si content of the iron-silicon alloy powder is 7-10 wt%.
The rotating speed of the stirring is 150-200 revolutions per minute.
The protective atmosphere is nitrogen.
Compared with the prior art, the specific implementation mode has the following advantages:
(1) the method comprises the steps of placing iron-silicon alloy powder in a water vapor environment at 100-260 ℃ for stirring, accelerating the surface oxidation of the iron-silicon alloy powder through water vapor to obtain composite powder with an iron-silicon alloy core and an iron oxide and simple substance silicon mixed coating layer on a shell, carrying out cold press molding, high-temperature sintering and heat treatment on the dried composite powder, and carrying out spontaneous SiO formation on the composite powder by utilizing the diffusion effect at high temperature and the chemical reaction between the iron oxide and the simple substance silicon at high temperature2And Fe2SiO4The multi-insulation layer special structure is formed, and the multi-insulation layer iron-silicon-based soft magnetic powder core is obtained. The raw materials used in the invention are only iron-silicon alloy powder, and no binder, lubricant and the like are added, so that the raw material loss is greatly reduced, the environment pollution is avoided, and the steam oxidation process is simple and easy to operate. Therefore, the preparation cost is low, the process is simple and easy, the repeatability is good, and the application prospect is good.
(2) According to the invention, the iron-silicon alloy powder is placed in a water vapor environment at 100-260 ℃ and stirred, the iron-silicon alloy powder is subjected to accelerated oxidation through water vapor, and in the oxidation process, the water vapor is fully contacted with the surface layer of the iron-silicon alloy particles, so that a mixed coating layer of iron oxide and simple substance silicon is rapidly formed on the surface of the iron-silicon alloy particles, and the production period is greatly shortened.
(3) In the invention, water vapor is used for shallow oxidation of the surface of the iron-silicon alloy powder to obtain a mixed coating layer of iron oxide and elemental silicon, so that further oxidation of the iron-silicon alloy powder by the water vapor is prevented, and thus the coating layer is uniform and thin, as shown in fig. 1, fig. 1 is an SEM (back scattering image) of the multi-insulation-layer iron-silicon-based soft magnetic powder core prepared in example 3, and as can be seen from fig. 1: the coating layers among the iron-silicon particles are uniform and thin, and the prepared multi-insulation-layer iron-silicon-based soft magnetic powder core is high in saturation magnetic induction intensity and low in coercive force.
(4) The insulating material of the multi-insulating-layer Fe-Si-based soft magnetic powder core prepared by the invention is an inorganic material, has good chemical stability and can resist high temperature, so that the high-temperature heat treatment not only promotes the formation of the multi-insulating layer of the multi-insulating-layer Fe-Si-based soft magnetic powder core, but also completely eliminates the internal stress caused by factors such as pressure and the like during the formation of the multi-insulating layer Fe-Si-based soft magnetic powder core, improves the saturation magnetic induction intensity of the multi-insulating-layer Fe-Si-based soft magnetic powder core and reduces the coercive force of the multi.
(5) The Fe-Si alloy particle coating SiO of the multi-insulation layer Fe-Si-based soft magnetic powder core prepared by the invention2And Fe2SiO4The formed multiple insulating layers are separated, and the coating layers are uniform. As can also be seen from fig. 1: the iron-silicon alloy particles being coated with SiO2Predominantly of SiO2-Fe2SiO4The multiple insulating layers are separated, so that the formed coating layer can effectively realize insulation among iron-silicon alloy particles, and the eddy current loss of the iron-silicon-based soft magnetic powder core with the multiple insulating layers is reduced.
(5) The invention can effectively regulate and control the thickness of the coating layer by adjusting the technological parameters of the steam oxidation process, the forming pressure, the temperature and time in the high-temperature sintering process, the temperature and time in the heat treatment process and the like, thereby preparing the multi-insulation-layer iron-silicon-based soft magnetic powder core with different magnetic properties.
Therefore, the invention has simple process and short production period, and the prepared multi-insulation-layer iron-silicon-based soft magnetic powder core has uniform and thin insulation coating layers, low eddy current loss, high saturation magnetic induction intensity and low coercive force.
Claims (7)
1. A preparation method of a multi-insulation layer Fe-Si-based soft magnetic powder core is characterized by comprising the following steps:
first step, composite powder preparation
Placing iron-silicon alloy powder into water vapor, and stirring for 0.5-3 h at the temperature of 100-260 ℃ to obtain composite powder;
second step, cold press forming
Vacuum drying the composite powder, putting the powder into a mold, and performing cold press molding under the condition of 300-1200 MPa to obtain a blank body;
third step, sintering
Placing the green body in a high-temperature sintering furnace, heating to 800-1300 ℃ under a vacuum condition or a protective atmosphere condition, and sintering for 0.5-5 h to obtain a sintered green body;
fourth, heat treatment
And (3) placing the sintered blank in a heat treatment furnace, heating to 500-1200 ℃ under the vacuum condition or protective atmosphere condition, carrying out heat treatment for 0.5-5 h, and cooling along with the furnace to obtain the multi-insulation-layer iron-silicon-based soft magnetic powder core.
2. The method of preparing a multi-insulation layer Fe-Si-based soft magnetic powder core according to claim 1, wherein the grain size of the Fe-Si alloy powder is 1 to 200 μm, and the Si content of the Fe-Si alloy powder is 1.5 to 10 wt%.
3. The method for preparing a multi-insulation layer Fe-Si-based soft magnetic powder core according to claim 1, wherein the stirring speed is 50 to 200 rpm.
4. The method for preparing a multi-insulation layer Fe-Si-based soft magnetic powder core according to claim 1, wherein the vacuum drying time is 12 to 36 hours, and the temperature of the vacuum drying is 40 to 70 ℃.
5. The method for preparing multi-insulation layer Fe-Si-based soft magnetic powder core as claimed in claim 1, wherein the degree of vacuum of said vacuum is 10-2～102Pa。
6. The method for preparing a multi-insulation layer fe-si based soft magnetic powder core according to claim 1, wherein the protective atmosphere is nitrogen or argon.
7. A many insulating layers silica-based soft magnetic powder core which characterized in that: the multi-insulation-layer Fe-Si-based soft magnetic powder core is prepared by the preparation method of the multi-insulation-layer Fe-Si-based soft magnetic powder core according to any one of claims 1 to 6.
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