Iron-based amorphous soft magnetic alloy magnetic core material and preparation method thereof
阅读说明：本技术 一种铁基非晶软磁合金磁芯材料及其制备方法 (Iron-based amorphous soft magnetic alloy magnetic core material and preparation method thereof ) 是由 邓毕力 罗顶飞 王玉川 徐敏义 潘振海 于 2020-12-21 设计创作，主要内容包括：本发明提供一种铁基非晶软磁合金磁芯材料及其制备方法,所述磁芯材料具有以下分子式：Fe-aSi-bM-cB-dP-eC-f,a+b+c+d+f＝100,所述M元素为Co、Zr、Nb、Cu中的一种或几种,所述磁芯材料外还具有NiCo-2O-4纳米线层,所述纳米NiCo-2O-4纳米线层外采用化学气象沉积一层厚度为5μm～10μm的聚苯胺薄膜,NiCo-2O-4纳米线层中的NiCo-2O-4纳米线的直径为50nm～100nm,厚度为3mm～8mm。本发明提供的制备方法制备得到的具有分子式Fe-aSi-bM-cB-dP-eC-f的铁基非晶软磁合金磁芯材料具有饱和磁化强度高、介电损耗较小且具有一定绝缘的能力的同时不影响其磁导率的优异性能。(The invention provides an iron-based amorphous soft magnetic alloy magnetic core material and a preparation method thereof, wherein the magnetic core material has the following molecular formula: fe a Si b M c B d P e C f The a + b + c + d + f is 100, the M element is one or more of Co, Zr, Nb and Cu, and NiCo is also arranged outside the magnetic core material 2 O 4 A nanowire layer of said nano NiCo 2 O 4 A layer of polyaniline film and NiCo with the thickness of 5-10 mu m is deposited outside the nanowire layer by adopting chemical vapor deposition 2 O 4 NiCo in nanowire layer 2 O 4 The diameter of the nano wire is 50 nm-100 nm, and the thickness is 3 mm-8 mm. The Fe molecular formula prepared by the preparation method provided by the invention a Si b M c B d P e C f The iron-based amorphous soft magnetic alloy magnetic core material has high saturation magnetization, small dielectric loss and oneThe excellent performance of the magnetic permeability of the insulating material is not influenced while the insulating capability is fixed.)
1. An iron-based amorphous soft magnetic alloy core material, characterized in that said core material has the following molecular formula: feaSibMcBdPeCfThe a + b + c + d + f is 100, the M element is one or more of Co, Zr, Nb and Cu, and NiCo is also arranged outside the magnetic core material2O4A nanowire layer of said nano NiCo2O4And a polyaniline film with the thickness of 5-10 mu m is deposited outside the nanowire layer by adopting chemical vapor deposition.
2. According to the claimsThe Fe-based amorphous magnetically soft alloy magnetic core material of claim 1, wherein said NiCo2O4NiCo in nanowire layer2O4The diameter of the nano wire is 50 nm-100 nm.
3. An iron-based amorphous soft magnetic alloy core material according to claim 1, wherein said NiCo2O4The thickness of the nanowire layer is 3 mm-8 mm.
4. The iron-nickel based amorphous soft magnetic alloy magnetic powder core material as claimed in claim 1, wherein the atomic percentage of Fe is 70 ≤ a ≤ 80.
5. The iron-nickel based amorphous soft magnetic alloy magnetic powder core material as claimed in claim 1, wherein the percentage of Si atoms is 10 ≤ a ≤ 15.
6. The iron-nickel based amorphous soft magnetic alloy magnetic powder core material as claimed in claim 1, wherein the atomic percentage of M is 5 ≤ a ≤ 10.
7. The iron-nickel based amorphous soft magnetic alloy magnetic powder core material as claimed in claim 1, wherein the atomic percentage of B is 3 ≤ a ≤ 7.
8. The iron-nickel based amorphous soft magnetic alloy magnetic powder core material as claimed in claim 1, wherein the atomic percentage of P is 0.5 ≤ a ≤ 2.
9. The iron-nickel based amorphous soft magnetic alloy magnetic powder core material as claimed in claim 1, wherein the atomic percentage of C is 1 ≤ e ≤ 3.
10. The method for preparing an iron-nickel based amorphous soft magnetic alloy magnetic powder core material according to any one of claims 1 to 9, comprising the steps of:
1) according to said formula FeaSibMcBdPeCfThe iron-based amorphous soft magnetic alloy magnetic core components are proportioned, the proportioned mixture is smelted into molten steel, the temperature of the molten steel is adjusted to 160-320 ℃, and the liquid level height of the molten steel is 600-700 mm;
2) carrying out spraying and rapid quenching on the molten steel obtained in the step 1) by adopting a single copper roller at the speed of 30-45 m/s to cool the molten steel to obtain the iron-based amorphous alloy thin strip, wherein the distance between a nozzle used for spraying and the single copper roller is 250-280 microns;
3) heating the iron-based amorphous alloy thin strip obtained in the step 2) to 250-350 ℃, and then mixing with the NiCo2O4Wrapping the nanowires on the surface of the heated iron-based amorphous alloy thin strip, and limiting the NiCo by adopting a mold2O4The thickness of the nanowire layer by layer is obtained to obtain the NiCo nanowire2O4A magnetic core material of the nanowire layer;
4) the NiCo with the NiCo obtained in the step 3)2O4The magnetic core material of the nanowire layer is coupled by adopting ethyl orthosilicate coupling agent, and then a polyaniline film with the thickness of 5-10 mu m is deposited by adopting a chemical vapor deposition method to form the NiCo coated with the polyaniline conductive insulating film2O4And the iron-based amorphous soft magnetic alloy magnetic powder core material of the nanowire layer.
Technical Field
The invention belongs to the technical field of magnetic materials, and particularly relates to an iron-based amorphous soft magnetic alloy magnetic core material and a preparation method thereof.
Background
Compared with the traditional soft magnetic material, the iron-based amorphous nanocrystalline alloy has more excellent soft magnetic performance and is widely applied to high and new technical fields of electric power, electronics, information, energy and the like. With the progress of high and new technical fields and the development of times, new requirements of high frequency, micro size, integration, low cost, energy conservation, environmental protection and the like are put forward for soft magnetic materials. To meet these demands, it is aimed to research fe-based amorphous alloys with relatively simple components and preparation process, low cost and excellent performance, and to improve the magnetic properties of commercial fe-based amorphous nanocrystalline alloys through a simple heat treatment process, and to design and prepare a magnetic source using the heat-treated commercial amorphous ribbon. However, the prior art lacks a base amorphous soft magnetic alloy magnetic core material with high saturation magnetic induction and low dielectric loss.
Disclosure of Invention
Aiming at the defects, the invention provides the iron-based amorphous soft magnetic alloy magnetic core material which has high saturation magnetic induction intensity, smaller dielectric loss, certain insulating capability and no influence on magnetic conductivity and the preparation method thereof.
The invention provides the following technical scheme: an iron-based amorphous soft magnetic alloy core material, said core material having the formula: feaSibMcBdPeCfThe a + b + c + d + f is 100, the M element is one or more of Co, Zr, Nb and Cu, and NiCo is also arranged outside the magnetic core material2O4A nanowire layer of said nano NiCo2O4And a polyaniline film with the thickness of 5-10 mu m is deposited outside the nanowire layer by adopting chemical vapor deposition.
Further, the NiCo2O4NiCo in nanowire layer2O4The diameter of the nano wire is 50 nm-100 nm.
Further, the NiCo2O4The thickness of the nanowire layer is 3 mm-8 mm.
Furthermore, the percentage content of the Fe atom is more than or equal to 70 and less than or equal to 80.
Furthermore, the percentage content of the Si atoms is more than or equal to 10 and less than or equal to 15.
Furthermore, the percentage content of the M atoms is more than or equal to 5 and less than or equal to 10.
Furthermore, the percentage content of the B atoms is more than or equal to 3 and less than or equal to 7.
Furthermore, the percentage content of the P atoms is more than or equal to 0.5 and less than or equal to 2.
Furthermore, the atomic percentage content of C is more than or equal to 1 and less than or equal to 3.
The invention also provides a preparation method of the iron-nickel-based amorphous soft magnetic alloy magnetic powder core material, which comprises the following steps:
1) according to said formula FeaSibMcBdPeCfThe iron-based amorphous soft magnetic alloy magnetic core components are proportioned, the proportioned mixture is smelted into molten steel, the temperature of the molten steel is adjusted to 160-320 ℃, and the liquid level height of the molten steel is 600-700 mm;
2) carrying out spraying and rapid quenching on the molten steel obtained in the step 1) by adopting a single copper roller at the speed of 30-45 m/s to cool the molten steel to obtain the iron-based amorphous alloy thin strip, wherein the distance between a nozzle used for spraying and the single copper roller is 250-280 microns;
3) heating the iron-based amorphous alloy thin strip obtained in the step 2) to 250-350 ℃, and then mixing with the NiCo2O4Wrapping the nanowires on the surface of the heated iron-based amorphous alloy thin strip, and limiting the NiCo by adopting a mold2O4The thickness of the nanowire layer by layer is obtained to obtain the NiCo nanowire2O4A magnetic core material of the nanowire layer;
4) the NiCo with the NiCo obtained in the step 3)2O4The magnetic core material of the nanowire layer is coupled by adopting ethyl orthosilicate coupling agent, and then a polyaniline film with the thickness of 5-10 mu m is deposited by adopting a chemical vapor deposition method to form the NiCo coated with the polyaniline conductive insulating film2O4And the iron-based amorphous soft magnetic alloy magnetic powder core material of the nanowire layer.
The invention has the beneficial effects that:
1. the invention provides a molecular formulaIs FeaSibMcBdPeCfThe iron-based amorphous soft magnetic alloy magnetic powder core material ensures that the atomic percentage of iron is 70-80 and the atomic percentage of Si is 10-15, so that the content of iron and silicon is increased, and the finally obtained soft magnetic alloy magnetic powder core material has the saturated magnetic induction strength of 1.54-1.65T and lower resistivity, and further has high magnetic conductivity and small dielectric loss.
2. The application is provided by NiCo wrapped outside a magnetic powder core material2O4Nano NiCo in nanowire layer2O4Is a strong dielectric compound material, which contains two kinds of magnetic elements of Ni and Co, the magnetism of the compound material is closely related to the valence state and the site of the Ni and Co, and the tetrahedron position is composed of magnetic Co2+And nonmagnetic Co3+Occupying the octahedral sites by magnetic Ni3+And nonmagnetic Ni2+Therefore, the magnetic energy storage device has good magnetic performance and can play a certain magnetic energy storage performance, so that the magnetic energy storage device has smaller magnetic loss rate and dielectric loss.
3. According to the invention, the outermost layer is wrapped with the polyaniline conductive insulating layer, and polyaniline which is used as a conductive polymer has low production cost, low density, better processing performance and higher mechanical flexibility, so that the mechanical capability of the finally formed magnetic core material is improved, and the resistivity of the finally formed magnetic core material is reduced.
Detailed description of the preferred embodiments
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The iron-based amorphous soft magnetic alloy magnetic core material provided by the embodiment has the following molecular formula: fe80Si10Co5B3PC, the magnetic core material is also provided with oneNiCo with a layer thickness of 3mm2O4Nanowire layer, NiCo2O4NiCo in nanowire layer2O4The diameter of the nano wire is 50nm, and the nano NiCo2O4And a layer of polyaniline film with the thickness of 5 mu m is deposited outside the nanowire layer by adopting chemical vapor deposition.
The invention also provides a preparation method of the iron-nickel-based amorphous soft magnetic alloy magnetic powder core material, which comprises the following steps:
1) according to said formula Fe80Si10Co5B3Preparing the components of the iron-based amorphous soft magnetic alloy magnetic core of the PC, smelting the prepared mixture into molten steel, and adjusting the temperature of the molten steel to 160 ℃ to ensure that the liquid level height of the molten steel is 600 mm;
2) cooling the molten steel obtained in the step 1) by adopting a single copper roller to carry out spraying and rapid quenching at the speed of 30m/s to obtain an iron-based amorphous alloy thin strip, wherein the distance between a nozzle used for spraying and the single copper roller is 250 mu m;
3) heating the iron-based amorphous alloy ribbon obtained in the step 2) to 250 ℃, and then mixing with NiCo2O4Wrapping the nanowires on the surface of the heated iron-based amorphous alloy thin strip, and limiting the NiCo by adopting a mold2O4The thickness of the nanowire layer by layer is 3mm, and NiCo is obtained2O4A magnetic core material of the nanowire layer;
4) the NiCo with the NiCo obtained in the step 3)2O4The magnetic core material of the nanowire layer is coupled by adopting tetraethoxysilane coupling agent, and then a polyaniline film with the thickness of 5 mu m is deposited by adopting a chemical vapor deposition method to form the NiCo coated with the polyaniline conductive insulating film2O4And the iron-based amorphous soft magnetic alloy magnetic powder core material of the nanowire layer.
Through tests, the magnetic powder core material provided by the embodiment has the saturation magnetic induction intensity of 1.54T and the resistivity of 1105 multiplied by 10-8Omega · m, permeability loss of 3.88%, dielectric loss of 0.3487%.
Example 2
An iron-based amorphous soft magnetic alloy magnetic core material, and the magnetic coreThe material has the following molecular formula: fe75Si12(Zr0.5Cu0.5)5B5P2C, a layer of NiCo with the thickness of 8mm is arranged outside the magnetic core material2O4Nanowire layer, NiCo2O4NiCo in nanowire layer2O4The diameter of the nano wire is 100nm, and the nano NiCo2O4And a polyaniline film with the thickness of 10 mu m is deposited outside the nanowire layer by adopting chemical vapor deposition.
The invention also provides a preparation method of the iron-nickel-based amorphous soft magnetic alloy magnetic powder core material, which comprises the following steps:
1) according to said formula Fe75Si12(Zr0.5Cu0.5)5B5P2C, preparing the iron-based amorphous soft magnetic alloy magnetic core component, smelting the prepared mixture into molten steel, and adjusting the temperature of the molten steel to 320 ℃ to ensure that the liquid level height of the molten steel is 700 mm;
2) carrying out spraying and rapid quenching on the molten steel obtained in the step 1) by adopting a single copper roller at the speed of 45m/s to obtain an iron-based amorphous alloy thin strip, wherein the distance between a spray nozzle used for spraying and the single copper roller is 280 microns;
3) heating the iron-based amorphous alloy ribbon obtained in the step 2) to 350 ℃, and then mixing with NiCo2O4Wrapping the nanowires on the surface of the heated iron-based amorphous alloy thin strip, and limiting the NiCo by adopting a mold2O4The thickness of the nanowire layer by layer is 8mm, and NiCo is obtained2O4A magnetic core material of the nanowire layer;
4) the NiCo with the NiCo obtained in the step 3)2O4The magnetic core material of the nanowire layer is coupled by adopting ethyl orthosilicate coupling agent, and then a polyaniline film with the thickness of 10 mu m is deposited by adopting a chemical vapor deposition method to form the NiCo coated with the polyaniline conductive insulating film2O4And the iron-based amorphous soft magnetic alloy magnetic powder core material of the nanowire layer.
Through tests, the magnetic powder core material provided by the embodiment has the saturation induction density of 1.62T and the resistivity of 115 multiplied by 10-8Omega m, magnetic conductanceThe loss ratio was 2.9% and the dielectric loss was 0.2956%.
Example 3
The iron-based amorphous soft magnetic alloy magnetic core material provided by the embodiment has the following molecular formula: fe70Si15Nb6B4P2C3The magnetic core material is also provided with a layer of NiCo with the thickness of 5.5mm2O4Nanowire layer, NiCo2O4NiCo in nanowire layer2O4The diameter of the nano-wire is 75nm, and the nano NiCo2O4And a polyaniline film with the thickness of 7.5 mu m is deposited outside the nanowire layer by adopting chemical vapor deposition.
The invention also provides a preparation method of the iron-nickel-based amorphous soft magnetic alloy magnetic powder core material, which comprises the following steps:
1) according to said formula FeaSibMcBdPeCfThe iron-based amorphous soft magnetic alloy magnetic core components are proportioned, the proportioned mixture is smelted into molten steel, the temperature of the molten steel is adjusted to 240 ℃, and the liquid level height of the molten steel is enabled to be 650 mm;
2) carrying out spraying and rapid quenching on the molten steel obtained in the step 1) by adopting a single copper roller at the speed of 32.5m/s to obtain an iron-based amorphous alloy thin strip, wherein the distance between a nozzle used for spraying and the single copper roller is 360 mu m;
3) heating the iron-based amorphous alloy ribbon obtained in the step 2) to 300 ℃, and then mixing with the NiCo2O4Wrapping the nanowires on the surface of the heated iron-based amorphous alloy thin strip, and limiting the NiCo by adopting a mold2O4The nanowire layer had a thickness of 5.5mm, resulting in a nanowire with NiCo2O4A magnetic core material of the nanowire layer;
4) the NiCo with the NiCo obtained in the step 3)2O4The magnetic core material of the nanowire layer is coupled by adopting tetraethoxysilane coupling agent, and then a polyaniline film with the thickness of 7.5 mu m is deposited by adopting a chemical vapor deposition method to form the NiCo-coated conducting insulation film with polyaniline2O4Iron-based amorphous nanowire layerSoft magnetic alloy magnetic powder core material.
Through tests, the magnetic powder core material provided by the embodiment has the saturation induction density of 1.65T and the resistivity of 107 multiplied by 10-8Ω · m, permeability loss rate of 3.0%, and dielectric loss of 0.3015%.
The above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Furthermore, those skilled in the art will appreciate that while some embodiments herein include some features included in other embodiments, rather than other features, combinations of features of different embodiments are meant to be within the scope of the invention and form different embodiments. For example, in the claims above, any of the claimed embodiments may be used in any combination. The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
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