CN113299451A - FeNi nano particle/epoxy resin composite coated iron-silicon magnetic powder core and preparation method thereof - Google Patents
FeNi nano particle/epoxy resin composite coated iron-silicon magnetic powder core and preparation method thereof Download PDFInfo
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- CN113299451A CN113299451A CN202110498150.XA CN202110498150A CN113299451A CN 113299451 A CN113299451 A CN 113299451A CN 202110498150 A CN202110498150 A CN 202110498150A CN 113299451 A CN113299451 A CN 113299451A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F3/00—Cores, Yokes, or armatures
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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
- H01F1/032—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 hard-magnetic materials
- H01F1/04—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 hard-magnetic materials metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
Abstract
The invention discloses a FeNi nano particle/epoxy resin composite coated iron-silicon magnetic powder core, and a preparation method thereof comprises a powder mixing step, a modification step, an insulation coating step, a drying step, a compression molding step and a vacuum annealing treatment step. The invention takes the iron-silicon powder as a main body, a FeNi nano-particle/epoxy resin coating layer is constructed on the surface, and compared with the existing related products, the obtained iron-silicon magnetic powder core has the advantages of low magnetic loss, high magnetic conductivity, high product density, lower cost and the like.
Description
Technical Field
The invention belongs to the technical field of composite soft magnetic materials, and particularly relates to a FeNi nano particle/epoxy resin composite coated iron-silicon magnetic powder core and a preparation method thereof.
Background
The soft magnetic composite material (also called magnetic powder core) is a soft magnetic material which is obtained by using magnetic powder as a raw material, coating an insulating medium layer on the surface of the powder, pressing the powder into a required shape by adopting a powder metallurgy process, and performing heat treatment, and plays the role of information and energy coupling transmission and conversion in various devices. Due to the characteristics of high saturation magnetic flux density, high magnetic permeability, low loss and the like, the metal soft magnetic powder core conforms to the trend that electronic components are continuously developed towards high frequency, miniaturization, large current, low loss and high power, is widely applied to the industries of new energy, aerospace, intelligent terminals and the like, and has wide market prospect.
The iron-silicon magnetic powder core has excellent magnetic properties such as good direct current superposition characteristic, high frequency, low loss, high frequency stability and the like due to high resistivity, low magnetostriction coefficient and almost zero magnetocrystalline anisotropy coefficient of the alloy, so that the iron-silicon magnetic powder core particularly meets the technical requirements of low-voltage strong current, high power density and high frequency at present. However, the Fe-6.5% Si alloy is hard and brittle, and it is difficult to obtain a high-density Fe-Si magnetic powder core under high pressure, which results in high loss and serious heat generation, and is not beneficial to energy conservation and high efficiency of devices. Patent CN103824670B discloses a method for preparing an iron-silicon magnetic powder core by adding trace elements of Ni or Co on the basis of iron-silicon; although the loss is low, the preparation steps are complex, the cost is high, and the direct current bias performance of the magnetic powder core is poor. Therefore, it is necessary to further design and manufacture an iron-silicon magnetic powder core with excellent comprehensive performance, simple preparation process and low cost so as to meet the use requirements of rapidly developed electronic components.
Since the FeNi magnetic nanoparticles have a very large specific surface area, the use of the nano magnetic particles alone to prepare the magnetic powder core results in a large amount of non-magnetic substances contained in the magnetic powder core and a decrease in density, which drastically deteriorates the magnetic properties of the magnetic powder core and fails to exert the excellent soft magnetic properties of the magnetic nanoparticles. Meanwhile, the magnetic powder core using the nano magnetic particles as the metal matrix has the problems of complicated preparation process, high cost and the like.
Disclosure of Invention
The invention mainly aims to provide a FeNi nano particle/FeSi composite magnetic powder core and a preparation method thereof aiming at the defects in the prior art; the FeSi alloy powder is coated and modified by using a composite coating material formed by FeNi nano-particles and epoxy resin, so that the density and the effective magnetic conductivity of the FeSi magnetic powder core are effectively improved, and the loss is reduced.
In order to achieve the purpose, the invention adopts the technical scheme that:
the FeNi nano particle/epoxy resin composite coated iron-silicon magnetic powder core has a core-shell structure, wherein the core is iron-silicon powder, and a coating modification material formed by FeNi nano particles and epoxy resin is coated on the surface of the iron-silicon powder to form a shell.
In the scheme, the alloy component of the iron-silicon powder is Fe-6.5 wt.% Si, and the grain diameter is-200 meshes; the particle size of the FeNi nano-particles is 1-100 nm.
In the scheme, the mass ratio of the iron silicon powder to the FeNi nano particles is (4-19): 1.
The preparation method of the FeNi nano particle/epoxy resin composite coated iron-silicon magnetic powder core comprises the following steps:
1) powder mixing: uniformly mixing iron silicon powder and FeNi nano particles to obtain mixed powder;
2) modification treatment: adding a silane coupling agent-ethanol solution into the mixed powder for magnetic powder surface treatment, and drying;
3) insulating and coating: adding the mixed powder obtained by the surface treatment in the step 2) into an epoxy resin-acetone solution, and continuously stirring until acetone is completely volatilized to obtain coated powder;
4) drying the obtained coated powder, adding a lubricant into the obtained dried powder, and uniformly stirring to obtain lubricating powder; then compression molding is carried out to obtain a magnetic powder core blank;
5) and (3) vacuum annealing treatment: and annealing the magnetic powder core blank to obtain the iron-silicon magnetic powder core.
In the scheme, the particle size of the iron-silicon powder is-200 meshes; the particle size of the FeNi nano-particles is 1-100 nm.
In the scheme, the mass ratio of the iron silicon powder to the FeNi nano particles is (4-19): 1.
Preferably, the mass ratio of the iron silicon powder to the FeNi nanoparticles is (17-18): 1
In the scheme, the adding amount of the silane coupling agent-ethanol solution is 2-6% of the mass of the mixed powder; wherein the silane coupling agent accounts for 2-10% of the mass of the silane coupling agent-ethanol solution.
In the scheme, the adding amount of the epoxy resin-acetone solution is 1-3% of the mass of the mixed powder obtained by surface treatment, wherein the weight percentage of the epoxy resin in the epoxy resin-acetone solution is 1-5%.
In the scheme, the drying temperature is 50-150 ℃ and the drying time is 30-60 min.
In the scheme, the lubricant is one or more of stearate, molybdenum disulfide, hexagonal boron nitride and aluminum stearate; the addition amount of the lubricant is 0.3-0.6% of the weight of the dried powder.
In the scheme, the molding pressure adopted in the compression molding step is 1600-2200MPa, and the pressure maintaining time is 30-120 s.
In the scheme, the annealing step adopts a vacuum condition or a protective atmosphere, and the protective atmosphere can be inert gases such as nitrogen, argon and the like; the annealing temperature is 400-700 ℃, and the heat preservation time is 30-60 min.
Compared with the prior art, the invention has the beneficial effects that:
1) book (I)The invention firstly proposes to construct a FeNi nano-particle/epoxy resin coating layer on the surface of the iron-silicon powder to prepare a FeNi nano-particle/FeSi composite magnetic powder core; the obtained magnetic powder core has the optimal comprehensive performance that the density is 6.7g/cm3Above 10kHz, the effective magnetic conductivity can reach more than 87, and the unit volume loss Pcv(50kHz,100mT)Can reach 650mW/cm3The following; a brand new idea can be provided for the preparation of the high-performance iron-silicon magnetic powder core;
2) the FeNi nano particle/FeSi composite magnetic powder core obtained by the invention has the advantages that the density of the composite magnetic powder core is obviously improved by playing the filling role of a small amount of FeNi nano particles, the internal magnetic domain structure of the powder core is optimized, and finally the effective magnetic conductivity of the composite magnetic powder core can reach the level equivalent to that of the FeNi magnetic powder core. This may provide an alternative to some high cost FeNi magnetic powder core applications.
3) The preparation method provided by the invention is simple, convenient to operate and suitable for popularization and application.
Drawings
FIG. 1 is a scanning electron micrograph of a product obtained in example 3 of the present invention;
FIG. 2 shows the permeability of the products obtained in examples 1 to 4 as a function of frequency.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
In the following examples, iron silicon powder was used which was supplied by Baokui Cycloco and had an alloy composition of Fe-6.5 wt.% Si and a particle size of-200 mesh; the FeNi nanoparticles are provided by Ningbo broad New nanometer materials company, and the particle size of the FeNi nanoparticles is 1-100 nm.
In the following examples, the epoxy resin used was supplied by Sichuan Longhua adhesive practice Co., Ltd., model No. W-6 c.
In the following examples, the silane coupling agent KH-550 used was provided by national reagent.
Example 1
A FeNi nano particle/epoxy resin composite coated iron-silicon magnetic powder core is prepared by the following steps:
1) uniformly dry-mixing iron silicon powder and FeNi nano particles according to the weight ratio of 95:5, wherein the dosage of the iron silicon powder is 19g, and the dosage of the FeNi nano particles is 1 g; the material mixing time is 20min, and the material mixing speed is 30 r/min;
2) weighing 2g of silane coupling agent, adding the silane coupling agent into 10ml of absolute ethyl alcohol, and ultrasonically stirring for 5min to obtain a silane coupling agent-ethyl alcohol solution; adding the obtained mixed powder into a prepared silane coupling agent-absolute ethyl alcohol solution, and carrying out ultrasonic stirring reaction for 10 min; then putting the mixture into a vacuum dryer for drying, wherein the drying temperature is set at 60 ℃, and the drying time is 1 h;
3) adding epoxy resin accounting for 1.5% of the dried powder mass into 10ml of acetone solution, and performing ultrasonic dispersion for 1min to obtain epoxy resin-acetone solution;
4) adding the dried powder obtained in the step 2) into a prepared epoxy resin-acetone solution, continuously stirring until acetone is completely volatilized, and continuously drying the powder coated with the insulation, wherein the drying temperature is set at 60 ℃ and the drying time is 1 h; weighing zinc stearate accounting for 0.5% of the weight of the obtained dried powder, uniformly mixing the zinc stearate with the obtained powder in a dry mode, and maintaining the pressure for 60s under the condition of 1800MPa to obtain a magnetic powder core blank;
5) putting the obtained magnetic ring blank into a vacuum annealing furnace, and keeping the vacuum degree at 10-3And under the condition, preserving heat for 1h at the temperature of 500 ℃ to obtain the FeNi nano particle/epoxy resin composite coated iron-silicon magnetic powder core.
Example 2
The preparation method of the FeNi nano particle/epoxy resin composite coated iron-silicon magnetic powder core is only different from that of the embodiment 1 in that: the mass ratio of the iron silicon powder to the FeNi nanoparticles in the step 1) is 90:10, wherein the using amount of the iron silicon powder is 18g, and the using amount of the FeNi nanoparticles is 2 g.
Example 3
The preparation method of the FeNi nano particle/epoxy resin composite coated iron-silicon magnetic powder core is only different from that of the embodiment 1 in that: the mass ratio of the iron silicon powder to the FeNi nanoparticles in the step 1) is 85:5, wherein the using amount of the iron silicon powder is 17g, and the using amount of the FeNi nanoparticles is 3 g.
Example 4
The preparation method of the FeNi nano particle/epoxy resin composite coated iron-silicon magnetic powder core is only different from that of the embodiment 1 in that: the mass ratio of the iron silicon powder to the FeNi nanoparticles in the step 1) is 80:20, wherein the using amount of the iron silicon powder is 16g, and the using amount of the FeNi nanoparticles is 4 g.
The scanning electron micrograph of the product obtained in example 3 is shown in FIG. 1, and the result shows that: the FeNi nano particles are uniformly and densely embedded on the epoxy resin layer on the surface of the large-particle iron-silicon powder.
The results of the permeability changes with frequency of the products obtained in examples 1 to 4 are shown in FIG. 2.
Comparative example 1
A method for preparing an iron-silicon magnetic powder core, which is different from the example 1 only in that: iron silicon powder (20g) was used in step 1) in total, and no FeNi nanoparticles were added.
The performance of the ferrosilicon magnetic powder cores prepared in examples 1 to 4 and comparative example 1 was tested under the experimental conditions (100mT, 50kHz), and the test results are shown in table 1 below.
TABLE 1 results of performance test of the ferrite cores obtained in examples and comparative examples
| Numbering | ρ(g/cm3) | μ | Pcv *(mW/cm3) |
| Example 1 | 6.457 | 74.5 | 714 |
| Example 2 | 6.608 | 83.9 | 665.6 |
| Example 3 | 6.710 | 87.7 | 647.9 |
| Example 4 | 6.528 | 72.6 | 683.3 |
| Comparative example 1 | 6.254 | 61.0 | 831.4 |
The results show that compared with the iron-silicon magnetic powder core which is insulated only by using epoxy resin, the density of the iron-silicon magnetic powder core adopting the FeNi nano-particle-epoxy resin composite coating method is remarkably increased, the effective magnetic conductivity is improved by nearly 44%, and the loss is reduced by nearly 22% under the same condition; the magnetic conductivity of the iron-silicon magnetic powder core can be effectively improved, the loss of the iron-silicon magnetic powder core is reduced, and meanwhile, the preparation cost is effectively reduced.
The above-mentioned embodiments only express the specific embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (9)
1. The FeNi nano particle/epoxy resin composite coated iron-silicon magnetic powder core is characterized by having a core-shell structure, wherein the core is iron-silicon powder, and a coating modification material formed by FeNi nano particles and epoxy resin is coated on the surface of the iron-silicon powder to form a shell.
2. The ferrosilicon magnetic powder core according to claim 1, wherein the grain size of the ferrosilicon powder is-200 mesh; the particle size of the FeNi nano-particles is 1-100 nm.
3. The preparation method of the FeNi nanoparticle/epoxy resin composite coated iron-silicon magnetic powder core as claimed in any one of claims 1 to 2, characterized by comprising the following steps:
1) powder mixing: uniformly mixing iron silicon powder and FeNi nano particles to obtain mixed powder;
2) modification treatment: adding a silane coupling agent-ethanol solution into the mixed powder for magnetic powder surface treatment, and drying;
3) insulating and coating: adding the mixed powder obtained by the surface treatment in the step 2) into an epoxy resin-acetone solution, and continuously stirring until acetone is completely volatilized to obtain coated powder;
4) drying the obtained coated powder, adding a lubricant into the obtained dried powder, and uniformly stirring to obtain lubricating powder; then compression molding is carried out to obtain a magnetic powder core blank;
5) and (3) vacuum annealing treatment: and annealing the magnetic powder core blank to obtain the iron-silicon magnetic powder core.
4. The preparation method according to claim 3, wherein the mass ratio of the iron silicon powder to the FeNi nanoparticles is (4-19): 1.
5. The preparation method according to claim 3, wherein the silane coupling agent is added in an amount of 8 to 11% by mass of the mixed powder; wherein the silane coupling agent accounts for 2-10% of the mass of the silane coupling agent-ethanol solution.
6. The preparation method according to claim 3, wherein the amount of the epoxy resin added is 1 to 3% by mass of the mixed powder obtained by the surface treatment, and the epoxy resin accounts for 1 to 5% by mass of the epoxy resin-acetone solution.
7. The preparation method according to claim 3, wherein the lubricant is one or more of stearate, molybdenum disulfide, hexagonal boron nitride and aluminum stearate; the addition amount of the lubricant is 0.3-0.6% of the weight of the dried powder.
8. The method according to claim 3, wherein the molding pressure used in the molding step is 1600-2200MPa, and the dwell time is 30-120 s.
9. The method according to claim 3, wherein the annealing step uses vacuum conditions or a protective atmosphere; the annealing temperature is 400-700 ℃, and the heat preservation time is 30-60 min.
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| CN115312316A (en) * | 2022-08-23 | 2022-11-08 | 湖南大学 | Low-loss soft magnetic composite material for high frequency and high power and preparation method thereof |
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