CN116825467A - MnZn ferrite combined coated FeSiAl magnetic powder core and preparation method thereof - Google Patents
MnZn ferrite combined coated FeSiAl magnetic powder core and preparation method thereof Download PDFInfo
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- 239000006247 magnetic powder Substances 0.000 title claims abstract description 69
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000011248 coating agent Substances 0.000 claims abstract description 25
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 23
- 238000000576 coating method Methods 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 18
- 239000011247 coating layer Substances 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims description 40
- 238000000137 annealing Methods 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 19
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 11
- 229910045601 alloy Inorganic materials 0.000 claims description 10
- 239000000956 alloy Substances 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 239000012298 atmosphere Substances 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 239000011701 zinc Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 4
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 4
- GEYXPJBPASPPLI-UHFFFAOYSA-N manganese(III) oxide Inorganic materials O=[Mn]O[Mn]=O GEYXPJBPASPPLI-UHFFFAOYSA-N 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 239000011787 zinc oxide Substances 0.000 claims description 4
- 238000005253 cladding Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000000748 compression moulding Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 229920002050 silicone resin Polymers 0.000 claims description 2
- 230000035699 permeability Effects 0.000 abstract description 25
- 239000002131 composite material Substances 0.000 abstract description 13
- 239000000696 magnetic material Substances 0.000 abstract description 8
- 239000011162 core material Substances 0.000 description 41
- 230000005415 magnetization Effects 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 10
- 238000012360 testing method Methods 0.000 description 8
- 239000000126 substance Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 238000009740 moulding (composite fabrication) Methods 0.000 description 5
- 238000003825 pressing Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000000975 co-precipitation Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229920001296 polysiloxane Polymers 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000002490 spark plasma sintering Methods 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000005347 demagnetization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
Classifications
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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
- H01F1/34—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 non-metallic substances, e.g. ferrites
- H01F1/342—Oxides
-
- 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
- H01F1/14791—Fe-Si-Al based alloys, e.g. Sendust
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/20—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder
- H01F1/22—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
- H01F1/24—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
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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
- H01F1/34—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 non-metallic substances, e.g. ferrites
- H01F1/36—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 non-metallic substances, e.g. ferrites in the form of particles
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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
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
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- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
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- Manufacturing & Machinery (AREA)
- Soft Magnetic Materials (AREA)
Abstract
A MnZn ferrite combined coated FeSiAl magnetic powder core and a preparation method thereof relate to magnetic materials. The MnZn ferrite combined coating FeSiAl magnetic powder core comprises FeSiAl magnetic powder and a coating layer coated on the surface of the FeSiAl magnetic powder, and is characterized in that the material of the coating layer comprises SiO 2 And MnZn ferrite, based on the mass of FeSiAl magnetic powder, siO 2 The content of the ferrite is 0.2 to 1 weight percent, and the content of the ferrite of MnZn is 0.2 to 1 weight percent. The invention can make the composite magnetic powder core have higher magnetic permeability and low loss characteristic.
Description
Technical Field
The invention relates to a magnetic material, in particular to a magnetic powder core material and a preparation technology thereof.
Background
Due to the rapid increase in the global consumer electronics market demand, various devices are evolving toward miniaturization and weight reduction. Aiming at the daily and lunar demands of magnetic materials, the soft magnetic materials are widely applied to various electronic devices because of the characteristics of easy magnetization and easy demagnetization. The metal magnetic powder core is a soft magnetic material obtained by selecting proper insulating substances to coat alloy powder, pressing and forming and annealing, wherein the FeSiAl magnetic powder core has the characteristics of high saturation magnetic induction intensity, high cost performance and the like, and is more and more paid attention to by various companies. However, feSiAl materials are easy to generate eddy current loss in a high-frequency application environment, and limit the application scenes of the FeSiAl materials. With respect to the characteristic, the FeSiAl alloy powder needs to be modified by using a proper coating substance, so that the FeSiAl can adapt to a new application scene.
Chinese patent publication No. CN106373697A discloses a preparation method of FeSiAl/Mn-Zn ferrite composite magnetic powder core, wherein MnZn ferrite is added by a coprecipitation method for ball milling, mixing and coating, and the obtained composite magnetic powder core has stable magnetic permeability which is close to 80. But MnZn ferrite has only high conductivity, and the resistivity is generally lower than 10 2 Omega.m. The magnetic powder core prepared by the method has the power loss larger than 46W/kg under the test conditions of 100kHz and 300mT, and the coating agent only plays a role in stabilizing magnetic permeability. And the coprecipitation method is not beneficial to large-scale industrial production.
The Chinese patent publication No. CN115101322A discloses a preparation method of composite magnetic powder cores, which selects ferrite as a coating agent and uniformly mixes metal soft magnetic powder and ferrite soft magnetic powder by using a ball milling mixing method. Then, ferrite powder and metal powder are sequentially brought into a molten state by Spark Plasma Sintering (SPS) to obtain the metal-ferrite alloy. Then crushing, ball milling and sieving, then carrying out secondary coating on the magnetic powder by using a coupling agent and silicone resin, pressing, forming and annealing treatment. The magnetic permeability is 60-80. The method needs to carry out secondary insulating coating, and needs to use SPS to carry out specific melting procedures, so that the process is complex, and the method is not beneficial to popularization and application in market.
Chinese patent publication No. CN112185641A discloses a method for coating magnetic powder core with phosphoric acid and nano calcium carbonate, which comprises the steps of phosphating magnetic powder to generate Fe (H) on the surface of the magnetic powder 2 PO 4 ) 2 Then the nano calcium carbonate is continuously reacted to generate Ca (H) 2 PO 4 ) 2 And a secondary coating layer. The method adopts two chemical reactions, so that the magnetic powder has a uniform coating layer, but non-magnetic substances are introduced in the two reactions, so that the magnetic core power loss of the magnetic powder cannot be reduced, and meanwhile, the magnetic properties such as magnetic conductivity and the like of the material are effectively improved.
Aiming at the MnZn ferrite coated FeSiAl alloy, the Chinese university of metering (Journal of Magnetism and Magnetic Materials,2017, 426:132-136) discloses a research on a metal magnetic powder core material, and the MnZn ferrite is coated by using a chemical coprecipitation method. Composite magnetic powder core performance index with MnZn ferrite addition amount of 3 wt%: permeability of magnetic material>85, power loss under the test conditions of 25kHz and 10mT>760mW/cm 3 . The MnZn ferrite effectively improves the magnetic permeability of the composite magnetic powder core, but the effect of reducing the low-frequency power loss is not obvious. The test results of specific saturation magnetization and high-frequency power loss are not published.
For SiO 2 The FeSiAl alloy coated by non-magnetic substances, the university of Wuhan technology (Materials Science and Engineering:B,2015, 201:79-86) discloses a research on a metal magnetic powder core material, and the modified material is adoptedMethod combines high-temperature sintering process to synthesize FeSiAl/SiO 2 Core-shell particles and Fe 3 Si/Al 2 O 3 And (3) a composite magnetic powder core. Power loss of composite magnetic powder core under 50kHz and 50mT test condition>480W/kg, but the permeability is poor in high-frequency stability, and the permeability is obviously reduced along with the increase of the frequency; meanwhile, the addition of SiO2 makes the composite magnetic powder core have stronger saturation magnetizationDegree sigma s Has obvious decrease, the TEOS addition amount is 10ml, and the sigma of the composite magnetic powder core s 116.6emu/g.
Disclosure of Invention
The invention aims to solve the technical problem of providing a MnZn ferrite combined coated FeSiAl magnetic powder core and a preparation method thereof, which can stabilize or improve the magnetic permeability performance of a magnetic powder core material and stabilize the magnetic powder core-to-saturation magnetization strength under the condition of meeting the low-loss application requirement.
The invention solves the technical problems by adopting the technical proposal that the MnZn ferrite is jointly coated with FeSiAl magnetic powder core, which comprises FeSiAl magnetic powder and a coating layer coated on the surface of the FeSiAl magnetic powder, and is characterized in that the material of the coating layer comprises SiO 2 And MnZn ferrite, based on the mass of FeSiAl magnetic powder, siO 2 The content of the ferrite is 0.2 to 1 weight percent, and the content of the ferrite of MnZn is 0.2 to 1 weight percent.
Further, siO 2 The content of (C) is 0.25wt%, and the content of MnZn ferrite is 0.25wt%.
The invention also provides a preparation method of the MnZn ferrite combined coated FeSiAl magnetic powder core, which comprises the following steps:
(1) Raw material selection: the raw materials comprise FeSiAl alloy powder and SiO 2 And MnZn ferrite;
(2) Coating: weighing FeSiAl powder and 0.2-1wt% SiO based on the mass of the FeSiAl powder 2 And 0.2-1wt% MnZn ferrite powder, adding the three powders into acetone solution, adding binder, continuously stirring, sieving and drying;
(3) Compression molding;
(4) Annealing: and (3) annealing the pressed green part under the protective atmosphere, wherein the annealing temperature is 700-900 ℃, and the heat preservation time is 1-3 h.
In the step (1), feSiAl powder is subjected to heat treatment at 650 ℃ and has the particle size of 20-40 mu m.
The MnZn ferrite is prepared by the following steps:
(a) Ferric oxide, manganic oxide and zinc oxide according to the molecular formula Mn x Zn 1-x Fe 2 O 4 Proportioning and mixing (x=0.5-0.6), and presintering at 800-900 ℃ to obtain a presintering material;
(b) Adding 0.01-0.05wt% of calcium carbonate, 0.01-0.05wt% of titanium oxide and 0.05-0.20wt% of bismuth oxide into the presintering material, performing ball milling for the first time, then sintering at 1350-1420 ℃, adopting air atmosphere in the sintering temperature raising stage, adopting nitrogen atmosphere in the heat preservation and cooling stage, and keeping oxygen partial pressure and oxygen content at 0.1-5.0%;
(c) And ball milling for the second time to obtain ferrite powder with the particle size of 1.2-2.5 mu m.
In step (2), the binder comprises 0.5wt% PVB and 0.5wt% silicone based on the mass of FeSiAl powder.
The numerical range expressed in "-" of the present invention includes the end values, and for example, the range of 0.01 to 0.05wt% includes 0.01wt% and 0.05wt%.
The invention provides a simple and effective combined coating scheme with less SiO addition 2 And MnZn ferrite, fully utilizing the characteristic advantages of high resistivity, high magnetic permeability and high specific saturation magnetization, and simultaneously utilizing SiO 2 The characteristics of the space net structure can enable the composite magnetic powder core to have higher magnetic permeability and low loss characteristics; the preparation process of the magnetic powder core is simple and quick, does not need long-time chemical reaction or SPS, and is favorable for large-scale popularization in market.
Drawings
Fig. 1 is a magnetic permeability bar graph of the magnetic powder core materials of comparative examples 1 to 5 and example 1.
Fig. 2 is a bar graph of the ratio saturation magnetization of the magnetic powder core materials of comparative examples 1 to 5 and example 1.
FIG. 3 shows the power loss P of the magnetic powder core materials of comparative examples 1, 4 and examples 1, 4, 5 cv (50 mT,10-500 kHz) frequency profile.
FIG. 4 shows hysteresis loss P of the magnetic powder core material of comparative examples 1, 4, and 5 h Frequency characteristic diagram.
FIG. 5 shows eddy current loss P of the magnetic powder core material of comparative examples 1, 4, and 5 e (50 mT,10-500 kHz) frequency profile.
Detailed Description
The core idea of the invention is that the application requirement of the magnetic powder core on the aspects of high frequency and improvement of magnetic permeability is met by adopting a combined coating mode. The MnZn ferrite material is spinel structure, belongs to equiaxial crystal system, has high magnetic permeability, and has high magnetic permeability up to 15000 by adjusting Zn element in the formula, and simultaneously has higher saturation magnetization as magnetic material>75emu/g, but resistivity<10Ω·m；SiO 2 The material has a regular tetrahedral space network structure, has strong stability and high resistivity, and is SiO 2 Resistivity of (2)>10 13 Omega.m, can obviously improve the whole resistivity of magnetic powder core, reduce the power loss. Coating FeSiAl and SiO simultaneously 2 The space network structure of (2) forms a coating layer which effectively reduces the high-frequency eddy current loss on the surface of FeSiAl particles, and the space network structure with larger coverage area is formed by combination. And MnZn ferrite depends on a mesh-shaped structure coating layer and SiO 2 And alternately cladding FeSiAl alloy. The MnZn ferrite and FeSiAl are both cubic crystal systems, have similar anisotropism, and simultaneously have the characteristics of high magnetic permeability and high specific saturation magnetization of the MnZn ferrite, so that the integral magnetic permeability and the stable specific saturation magnetization of the FeSiAl magnetic powder core can be improved, and the requirements of improving the magnetic property of the magnetic powder core are met. Meanwhile, in order to achieve a good coating effect, the particle size ratio of the coating agent to the metal alloy powder needs to be controlled, so that the effect of alternate coating is achieved.
The method comprises the following steps:
1. preparing raw materials
The raw materials comprise FeSiAl alloy powder and a coating agent. The FeSiAl powder is heat treated at 650 ℃ and has the particle size of 20-40 mu m. The coating agent is MnZn ferrite and commercially available SiO 2 。SiO 2 Powder having a particle size of 0.5 μm was selected. The MnZn ferrite is prepared as follows:
ferric oxide, manganic oxide and zinc oxide according to the molecular formula Mn x Zn 1-x Fe 2 O 4 (x=0.5-0.6) and placing the mixture in a bell jar furnace at 800-900 DEG CPresintering. Adding 0.01 to 0.05 weight percent of calcium carbonate, 0.01 to 0.05 weight percent of titanium oxide and 0.05 to 0.20 weight percent of bismuth oxide, and ball milling for 1 to 2 hours by a planetary ball mill. And sintering the powder in a tube furnace at 1350-1420 deg.c. An air atmosphere is adopted in the sintering heating stage; the nitrogen atmosphere is adopted in the temperature-reducing stage, a certain oxygen partial pressure is maintained, and the oxygen content is 0.1-5.0%. Ball milling the sintered powder for 20h by using a planetary ball mill, wherein the particle size is 1.2-2.5 mu m. The magnetic permeability of the MnZn ferrite reaches about 10000, the resistivity is 3.72 omega-m, and the specific saturation magnetization is 77.8emu/g.
2. Coating
Weighing a proper amount of FeSiAl powder and 0.2 to 1 weight percent of SiO 2 And 0.2 to 1wt% of MnZn ferrite powder, adding the three powders into an acetone solution, adding a commercially available binder at the same time, and stirring and mixing. Stirring until acetone is volatilized basically, sieving with a 40-mesh sieve, and drying the obtained granulated powder until acetone is volatilized completely. Wherein the binder is 0.5wt% PVB and 0.5wt% silicone.
3. Shaping
And pressing the powder subjected to the coating treatment by using a hydraulic press to form a green part, wherein the forming pressure is 1800-2600 MPa.
4. Annealing
And (3) placing the pressed green blank in an atmosphere sintering device for annealing treatment, wherein the annealing temperature is 700-900 ℃, and the heat preservation time is 1-3 h. And adopting a vacuum argon annealing mode.
The final technical indexes of the FeSiAl composite magnetic powder core material prepared by the invention are as follows: the magnetic permeability is 71.1, the resistivity is 89.83 Ω & m, the specific saturation magnetization is 124.1emu/g, and the power loss is 43.05mW/cm under the test conditions of 50kHz and 50mT 3 The power loss is 191.93mW/cm under the test conditions of 50kHz and 100mT 3 。
Examples
Embodiments include the following steps:
1. raw materials
The raw materials comprise FeSiAl alloy powder and a coating agent. The FeSiAl powder is heat treated at 650 ℃ and has the particle size of 20-40 mu m. The coating agent is MnZn ferrite and commercially available SiO 2 。SiO 2 Selecting particle sizeIs 0.5 μm in size. The MnZn ferrite is prepared as follows:
ferric oxide, manganic oxide and zinc oxide according to the molecular formula Mn x Zn 1-x Fe 2 O 4 (x=0.5-0.6), and placing the mixture in a bell jar furnace for presintering at 800-900 ℃. Adding 0.01 to 0.05 weight percent of calcium carbonate, 0.01 to 0.05 weight percent of titanium oxide and 0.05 to 0.20 weight percent of bismuth oxide, and ball milling for 1 to 2 hours by a planetary ball mill. And sintering the powder in a tube furnace at 1350-1420 deg.c. An air atmosphere is adopted in the sintering heating stage; the nitrogen atmosphere is adopted in the temperature-reducing stage, a certain oxygen partial pressure is maintained, and the oxygen content is 0.1-5.0%. Ball milling the sintered powder for 20h by using a planetary ball mill, wherein the particle size is 1.2-2.5 mu m. The magnetic permeability of the MnZn ferrite reaches about 10000, the resistivity is 3.72 omega-m, and the specific saturation magnetization is 77.8emu/g.
2. Coating
Weighing a proper amount of FeSiAl powder and 0.25 to 1 weight percent of SiO 2 And 0.25 to 1wt% MnZn ferrite powder, three kinds of powders are added to an acetone solution, and a commercially available binder is added at the same time, and stirred and mixed using a stirrer. Stirring until acetone is volatilized basically, sieving with 40 mesh sieve twice, and oven drying the obtained granulated powder until acetone is volatilized completely. Wherein the binder is 0.5wt% PVB and 0.5wt% silicone.
3. Shaping
And (3) pressing and forming the coated powder into a green part by using a hydraulic press, wherein the pressure maintaining time is 20s, and the forming pressure is 1800-2600 MPa.
4. Annealing
And (3) placing the pressed green body in a tube furnace for annealing treatment, wherein the annealing temperature is 700-900 ℃, and the heat preservation time is 1-3 h. And adopting a vacuum argon annealing mode. Vacuum argon annealing is divided into:
(1) Vacuumizing for 40min, and introducing argon gas until the pressure gauge approaches 0MPa;
(2) Vacuumizing for 30min, and introducing argon until the pressure gauge is close to minus 0.05MPa;
(3) Starting annealing;
(4) And (3) carrying out the step (2) at the temperature of 500 ℃ in the furnace.
5. Testing
And (3) testing the magnetic property of the sample prepared in the step (4).
The permeability of the material is tested by adopting a TH2826 high-frequency LCR digital bridge of Henkel electronics limited company, the specific saturation magnetization intensity of the material is tested by adopting a 8604 vibration sample magnetometer of LakeShore company, the power loss of the material is tested by adopting a SY-8218BH analyzer of IWATCU company, and the hysteresis loss and the eddy current loss of the material are obtained by adopting a Jordan loss separation method.
For comparison, 5 sets of examples, 5 sets of comparative examples, were set forth below:
| comparative example number | SiO 2 (wt％.) | MnZn ferrite (wt%) |
| 1 | 0 | 0 |
| 2 | 0.25 | 0 |
| 3 | 0.50 | 0 |
| 4 | 0 | 0.25 |
| 5 | 0 | 0.50 |
In examples 1 to 5, 2200M molding pressure was used in each of comparative examples 1 to 5, and the annealing temperature was 750 ℃.
The composite magnetic powder cores were prepared by the above process, and the performance parameters of examples 1 to 5 were as follows:
the performance parameters of comparative examples 1 to 5 are as follows:
referring to FIG. 1, a non-magnetic substance SiO 2 The addition of (2) can greatly reduce the magnetic permeability of the magnetic powder core, the MnZn ferrite can effectively improve the magnetic permeability of the magnetic powder core, and the magnetic permeability of comparative example 5>80, and the magnetic permeability of the magnetic powder core subjected to the combined coating treatment can be kept above 70;
referring to fig. 2, the addition of sio2 greatly reduces the specific saturation magnetization of the magnetic powder core, and MnZn ferrite can stabilize this property. The magnetic powder core ratio saturation magnetization intensity of the combined coating treatment can be close to 124.1emu/g;
referring to FIG. 3, the addition amount of MnZn ferrite is kept constant along with SiO 2 With a significant reduction in power consumption;
referring to fig. 4 and 5, the addition amount of mnzn ferrite is kept unchanged, and thenSiO-adhered to 2 Has obviously reduced eddy current loss and SiO 2 The high resistivity characteristic of the (C) effectively improves the resistance between FeSiAl magnetic powder.
Claims (8)
- The MnZn ferrite combined coated FeSiAl magnetic powder core comprises FeSiAl magnetic powder and a coating layer coated on the surface of the FeSiAl magnetic powder, and is characterized in that the material of the coating layer comprises SiO 2 And MnZn ferrite, based on the mass of FeSiAl magnetic powder, siO 2 The content of the ferrite is 0.2 to 1 weight percent, and the content of the ferrite of MnZn is 0.2 to 1 weight percent.
- 2. The MnZn ferrite joint cladding fesai magnetic powder core according to claim 1, wherein SiO 2 The content of the ferrite is 0.25 to 1 weight percent, and the content of the ferrite of MnZn is 0.25 to 1 weight percent.
- 3. The MnZn ferrite joint cladding fesai magnetic powder core according to claim 1, wherein SiO 2 The content of (C) is 0.25wt%, and the content of MnZn ferrite is 0.25wt%.
- The preparation method of the MnZn ferrite combined coated FeSiAl magnetic powder core is characterized by comprising the following steps of:(1) Raw material selection: the raw materials comprise FeSiAl alloy powder and SiO 2 And MnZn ferrite;(2) Coating: weighing FeSiAl powder and 0.2-1wt% SiO based on the mass of the FeSiAl powder 2 And 0.2-1wt% MnZn ferrite powder, adding the three powders into acetone solution, adding binder, continuously stirring, sieving and drying;(3) Compression molding;(4) Annealing: and (3) annealing the pressed green part under the protective atmosphere, wherein the annealing temperature is 700-900 ℃, and the heat preservation time is 1-3 h.
- 5. The method for preparing the MnZn ferrite combined coated FeSiAl magnetic powder core according to claim 4, wherein in the step (1), the FeSiAl powder is subjected to heat treatment at 650 ℃ and has a particle size of 20-40 μm.
- 6. The method for preparing the MnZn ferrite combined coated FeSiAl magnetic powder core according to claim 4, wherein the MnZn ferrite is prepared by the following steps:(a) Ferric oxide, manganic oxide and zinc oxide according to the molecular formula Mn x Zn 1-x Fe 2 O 4 Proportioning and mixing (x=0.5-0.6), and presintering at 800-900 ℃ to obtain a presintering material;(b) Adding 0.01-0.05wt% of calcium carbonate, 0.01-0.05wt% of titanium oxide and 0.05-0.20wt% of bismuth oxide into the presintering material, performing ball milling for the first time, then sintering at 1350-1420 ℃, adopting air atmosphere in the sintering temperature raising stage, adopting nitrogen atmosphere in the heat preservation and cooling stage, and keeping oxygen partial pressure and oxygen content at 0.1-5.0%;(c) And ball milling for the second time to obtain ferrite powder with the particle size of 1.2-2.5 mu m.
- 7. The method for preparing the MnZn ferrite combined coated fesai magnetic powder core according to claim 4, wherein in the step (2), the binder comprises 0.5wt% of PVB and 0.5wt% of silicone resin based on the mass of the fesai powder.
- 8. The method for preparing the MnZn ferrite combined coated FeSiAl magnetic powder core according to claim 4, wherein in the step (4), vacuum argon annealing is adopted.
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