CN118866496B - Amorphous soft magnetic composite material and preparation method thereof - Google Patents
Amorphous soft magnetic composite material and preparation method thereof Download PDFInfo
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- CN118866496B CN118866496B CN202411333443.2A CN202411333443A CN118866496B CN 118866496 B CN118866496 B CN 118866496B CN 202411333443 A CN202411333443 A CN 202411333443A CN 118866496 B CN118866496 B CN 118866496B
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- 239000002131 composite material Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 130
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 74
- 238000011282 treatment Methods 0.000 claims abstract description 44
- 239000011812 mixed powder Substances 0.000 claims abstract description 35
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 claims abstract description 29
- JIYIUPFAJUGHNL-UHFFFAOYSA-N [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] JIYIUPFAJUGHNL-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910002555 FeNi Inorganic materials 0.000 claims abstract description 24
- 238000002161 passivation Methods 0.000 claims abstract description 22
- 238000003825 pressing Methods 0.000 claims abstract description 22
- 239000011248 coating agent Substances 0.000 claims abstract description 20
- 238000000576 coating method Methods 0.000 claims abstract description 20
- 238000000137 annealing Methods 0.000 claims abstract description 17
- 239000000725 suspension Substances 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000000314 lubricant Substances 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims description 19
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 18
- 229920005989 resin Polymers 0.000 claims description 18
- 239000011347 resin Substances 0.000 claims description 18
- 229910052710 silicon Inorganic materials 0.000 claims description 18
- 239000010703 silicon Substances 0.000 claims description 18
- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical group [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000035699 permeability Effects 0.000 abstract description 11
- 239000000696 magnetic material Substances 0.000 abstract description 4
- 229920002050 silicone resin Polymers 0.000 abstract 1
- 239000000463 material Substances 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 19
- 239000006247 magnetic powder Substances 0.000 description 7
- 229910000859 α-Fe Inorganic materials 0.000 description 6
- 238000005253 cladding Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 238000005056 compaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 239000006249 magnetic particle Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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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
- H01F1/344—Ferrites, e.g. having a cubic spinel structure (X2+O)(Y23+O3), e.g. magnetite Fe3O4
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/14708—Fe-Ni based alloys
- H01F1/14733—Fe-Ni based alloys in the form of particles
- H01F1/14741—Fe-Ni based alloys in the form of particles pressed, sintered or bonded together
- H01F1/1475—Fe-Ni based alloys in the form of particles pressed, sintered or bonded together the particles being insulated
- H01F1/14758—Fe-Ni based alloys in the form of particles pressed, sintered or bonded together the particles being insulated by macromolecular organic substances
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- 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
- H01F1/153—Amorphous metallic alloys, e.g. glassy metals
- H01F1/15308—Amorphous metallic alloys, e.g. glassy metals based on Fe/Ni
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
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- 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
- H01F1/153—Amorphous metallic alloys, e.g. glassy metals
- H01F1/15341—Preparation processes therefor
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- 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
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- 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
- H01F1/26—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 by macromolecular organic substances
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- 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
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Abstract
本发明属于非晶软磁材料技术领域，具体涉及一种非晶软磁复合材料及其制备方法，包括如下步骤：（1）将FeSiBCCr非晶粉末置于锰锌铁氧体和乙醇的悬浊液中钝化处理，得到钝化后的FeSiBCCr非晶粉末；（2）将FeNi粉末和钝化后的FeSiBCCr非晶粉末按比例混合并置于有机硅树脂与乙醇的混合溶液中进行包覆处理，充分搅拌并烘干后得到混合粉末；（3）在混合粉末中加入润滑剂，混合均匀后置于模具中，温压压制，经去应力退火后，得到具有高磁导率、高直流叠加和低损耗特性的非晶软磁复合材料。
The present invention belongs to the technical field of amorphous soft magnetic materials, and specifically relates to an amorphous soft magnetic composite material and a preparation method thereof, comprising the following steps: (1) placing FeSiBCCr amorphous powder in a suspension of manganese zinc ferrite and ethanol for passivation treatment to obtain passivated FeSiBCCr amorphous powder; (2) mixing FeNi powder and passivated FeSiBCCr amorphous powder in proportion and placing them in a mixed solution of organic silicone resin and ethanol for coating treatment, and obtaining a mixed powder after sufficient stirring and drying; (3) adding a lubricant to the mixed powder, mixing evenly, placing it in a mold, pressing it at temperature, and performing stress relief annealing to obtain an amorphous soft magnetic composite material with high magnetic permeability, high DC superposition and low loss characteristics.
Description
Technical Field
The invention belongs to the technical field of magnetic materials, and particularly relates to an amorphous soft magnetic composite material and a preparation method thereof.
Background
With the progress of chip vertical power supply technology, chip power supply modules are developing toward miniaturization and high-current power supply demands, which provide serious challenges for the performance of soft magnetic materials for inductors. Compared with the traditional Mn-Zn ferrite and crystalline metal soft magnetic material, the amorphous soft magnetic composite material is formed by compounding a plurality of materials, so that the advantages of the amorphous soft magnetic composite material are complementary, the high saturation magnetic induction intensity, the high magnetic permeability, the low loss and the high direct current superposition characteristic of the amorphous soft magnetic composite material are realized, and the application requirements of high frequency, miniaturization and integration of magnetic devices can be met.
At present, the preparation process of the iron-based amorphous alloy magnetic powder core generally comprises the steps of powder mixing, passivation treatment, cladding treatment, compression molding, annealing heat treatment and the like, wherein the cladding treatment is an important link for determining the comprehensive performance of the magnetic powder core in order to realize a good insulating effect among magnetic particles. However, the common insulating coating materials such as epoxy resin, phenolic resin, phosphate and the like are all non-magnetic substances, and the reduction of magnetic permeability and saturation induction caused by the magnetic dilution effect is a main problem faced by the common insulating coating materials. The patent with publication number CN117542648A discloses a preparation method of high-density amorphous powder core, which adopts phosphoric acid to coat amorphous magnetic powder, and the loss of the obtained magnetic powder core is high and exceeds 250mW/cm 3 after warm pressing. In addition, the amorphous alloy has larger hardness, difficult low-pressure forming, larger air gap between powders, higher magnetic saturation, higher magnetic permeability reduction rate, poorer direct current superposition performance, and higher pressure, which is easy to cause the rupture of an insulating layer, and the increase of internal stress of the magnetic powder core and the increase of loss. Patent publication No. CN107967976A discloses a preparation method of amorphous magnetic powder cores, wherein amorphous powder coated by ferrite and adhesive is pressed and molded under the pressure of 18t/cm 3 at normal temperature to obtain the amorphous magnetic powder cores. The loss under the conditions of 50kHz and 0.1T is high due to high pressure during pressing, and is 711mW/cm 3. Therefore, it is necessary to develop an amorphous soft magnetic composite material which can be molded at a low pressure with high density and has excellent characteristics of high magnetic permeability, low eddy current loss and high dc superposition.
Disclosure of Invention
In order to solve the problems, the invention aims to provide an amorphous soft magnetic composite material and a preparation method thereof, which can be molded under a low pressure condition, improve magnetic permeability and direct current superposition characteristics, and effectively inhibit eddy current loss, and adopts the following technical scheme:
An amorphous soft magnetic composite material mainly comprises FeSiBCCr amorphous powder, feNi powder and manganese zinc ferrite powder, wherein the particle size of the FeSiBCCr amorphous powder is 10-20 mu m, the particle size of the FeNi powder is 1-10 mu m, and the particle size of the manganese zinc ferrite powder is 0.5-5 mu m;
Wherein FeSiBCCr amorphous powder is placed in suspension of manganese-zinc ferrite powder and ethanol for passivation treatment, and the total mass of FeSiBCCr amorphous powder and manganese-zinc ferrite powder is calculated as the basis, the manganese-zinc ferrite powder accounts for 0.5-3wt% and the ethanol accounts for 5-10wt%;
wherein, based on the total mass of FeNi powder and FeSiBCCr amorphous powder after passivation, the mass ratio of FeSiBCCr amorphous powder after passivation is 50-80wt%, and the mass ratio of FeNi powder is 20-50wt%;
Wherein, feNi powder and FeSiBCCr amorphous powder after passivation need to be mixed, and then the amorphous soft magnetic composite material is obtained after cladding treatment, warm compaction forming and annealing;
Wherein the temperature of the warm-pressing treatment is 180-230 ℃, the time of the warm-pressing treatment is 10-60s, and the pressure of the press forming is 300-700MPa.
Preferably, feSiBCCr amorphous powder is formed into Fe 73Si10B10C5Cr2 according to the component of atomic percent of each element.
Preferably, feSiBCCr amorphous powder has a particle size of 12-17 μm, feNi powder has a particle size of 3-8 μm, and Mn-Zn ferrite powder has a particle size of 1-3 μm;
Preferably, feSiBCCr amorphous powder has a particle size of 13-15 μm, feNi powder has a particle size of 5-7 μm, and Mn-Zn ferrite powder has a particle size of 1.5-2.5 μm.
Preferably, feSiBCCr amorphous powder is required to be placed in suspension of manganese-zinc ferrite and ethanol for passivation treatment, and the mass ratio of the manganese-zinc ferrite powder is 1-2.5wt% and the mass ratio of the ethanol is 6-9wt% based on the total mass of FeSiBCCr amorphous powder and manganese-zinc ferrite powder;
preferably, feSiBCCr amorphous powder is required to be placed in a suspension of manganese-zinc ferrite and ethanol for passivation treatment, and the mass ratio of the manganese-zinc ferrite powder is 1.5-2wt% and the mass ratio of the ethanol is 7-8wt% based on the total mass of FeSiBCCr amorphous powder and manganese-zinc ferrite powder.
Preferably, the temperature of the warm-pressing treatment is 200-220 ℃, the time of the warm-pressing treatment is 20-50s, and the pressure of the press forming is 400-600MPa;
Preferably, the temperature of the warm-pressing treatment is 205-215 ℃, the time of the warm-pressing treatment is 30-40s, and the pressure of the press forming is 450-550MPa.
The preparation method of the amorphous soft magnetic composite material comprises the following steps:
(1) Placing FeSiBCCr amorphous powder into suspension of manganese zinc ferrite powder and ethanol for passivation treatment to obtain passivated FeSiBCCr amorphous powder;
(2) Mixing the passivated FeSiBCCr amorphous powder and FeNi powder, placing the mixture into a mixed solution of organic silicon resin and an organic solvent for insulating coating treatment, fully stirring and drying to obtain mixed powder;
(3) Adding lubricant into the mixed powder, uniformly mixing, putting into a die, warm-pressing, and annealing to obtain the amorphous soft magnetic composite material.
Preferably, in the step 2, the mass ratio of the organic silicon resin is 2-5wt% based on the total mass of FeNi powder and the passivated FeSiBCCr amorphous powder, the organic solvent is ethanol, and the mass ratio of the ethanol is 5-10wt%;
Preferably, in the step 2, the mass ratio of the organic silicon resin is 3-4wt% based on the total mass of the FeNi powder and the FeSiBCCr amorphous powder after passivation, the organic solvent is ethanol, and the mass ratio of the ethanol is 7-9wt%.
Preferably, in the step 3, the lubricant is barium stearate, and the amount of the lubricant is 0.2-0.4wt% of the mass of the mixed powder;
Preferably, in step 3, the lubricant is barium stearate and the lubricant is used in an amount of 0.25 to 0.35wt% based on the mass of the mixed powder.
Preferably, in the step 3, the annealing temperature is 350-450 ℃, the heat preservation time is 50-150min, the heating rate is 8-12 ℃ per min, and the annealing temperature is cooled along with the furnace;
Preferably, in the step 3, the annealing temperature is 380-420 ℃, the heat preservation time is 80-120min, the heating rate is 9-10 ℃ per min, and the annealing temperature is cooled along with the furnace.
The invention has the following beneficial effects:
The Mn-Zn ferrite powder insulating coating material adopted by the invention has high resistivity and high magnetic conductivity, and is coated on the surface of amorphous powder, so that the magnetic conductivity of the amorphous soft magnetic composite material can be improved, and the eddy current loss can be reduced;
in the preparation method of the amorphous soft magnetic composite material, a warm compaction process is adopted to improve the fluidity between powders, reduce the internal stress of material compaction, and improve the density of the material and achieve the purpose of improving the magnetic conductivity while forming under the low pressure condition;
The invention adds small-grain FeNi powder into the amorphous soft magnetic composite material, wherein the FeNi powder has better plasticity and good forming effect in the pressing process, and can make up the defect of poor forming capability of the amorphous powder. In addition, the FeNi powder with small particle size fills the gaps among the amorphous powder, thereby improving the compactness of the composite material, enhancing the coupling effect among the magnetic particles, further improving the magnetic permeability of the composite material, reducing the magnetic loss, and forming discrete distributed air gaps after filling the gaps among the amorphous powder, delaying the magnetic saturation and improving the direct current superposition performance.
Drawings
FIG. 1 is a graph showing the relationship between permeability and frequency of examples 1 to 4 and comparative examples 1 to 4;
FIG. 2 is a graph of the variation in loss versus frequency for examples 1-4 and comparative examples 1-4 under 20mT test conditions;
FIG. 3 is a graph of the loss of examples 1-4 and comparative examples 1-4 under 100mT, 50kHz test conditions;
FIG. 4 is a graph of the loss of examples 1-4 and comparative examples 1-4 under 50mT, 100kHz test conditions.
Detailed Description
In order to make the purposes, technical schemes and advantages of the invention more clear, the amorphous soft magnetic composite material and the preparation method thereof provided by the invention are further described in detail through the following examples and with reference to the accompanying drawings.
The invention provides an amorphous soft magnetic composite material, which is prepared from FeSiBCCr amorphous powder with the particle size of 10-20 mu m, feNi powder with the particle size of 1-10 mu m and manganese zinc ferrite powder with the particle size of 0.5-5 mu m, wherein FeSiBCCr amorphous powder is placed in suspension of manganese zinc ferrite powder and ethanol for passivation treatment, and the quality of the FeNi powder and the quality of the passivated FeSiBCCr amorphous powder are shown in table 1.
Table 1 shows the powder masses of examples 1 to 4
Example 1 is as follows:
the preparation method of the amorphous soft magnetic composite material comprises the following specific steps:
(1) Weighing 99.5g FeSiBCCr amorphous powder, and placing the amorphous powder into a suspension of 0.5g of manganese zinc ferrite powder and 7g of ethanol for passivation treatment to obtain passivated FeSiBCCr amorphous powder;
(2) Mixing the passivated FeSiBCCr amorphous powder and FeNi powder according to the proportion shown in table 1 to obtain mixed powder;
(3) Placing the mixed powder into a mixed solution of organic silicon resin and ethanol for insulating coating, wherein the organic silicon resin used for insulating coating accounts for 3wt% of the total mass of the mixed powder, the ethanol accounts for 8wt% of the total mass of the mixed powder, fully stirring and drying, adding barium stearate accounts for 0.3wt% of the total mass of the mixed powder, maintaining the pressure at 550MPa for 30s at 200 ℃ to obtain an annular material with the outer diameter of 14mm and the inner diameter of 8mm, and carrying out stress relief annealing treatment on the material at 450 ℃ for 120min to obtain the amorphous soft magnetic composite material.
Example 2 is as follows:
the preparation method of the amorphous soft magnetic composite material comprises the following specific steps:
(1) Weighing 98g FeSiBCCr amorphous powder, and placing the amorphous powder into a suspension of 2g of manganese zinc ferrite powder and 8g of ethanol for passivation treatment to obtain passivated FeSiBCCr amorphous powder;
(2) Mixing the passivated FeSiBCCr amorphous powder and FeNi powder according to the proportion shown in table 1 to obtain mixed powder;
(3) Placing the mixed powder into a mixed solution of organic silicon resin and ethanol for insulating coating, wherein the organic silicon resin used for insulating coating accounts for 1wt% of the total mass of the mixed powder, the ethanol accounts for 10wt% of the total mass of the mixed powder, fully stirring and drying, adding barium stearate accounts for 0.4wt% of the total mass of the mixed powder, maintaining the pressure at the temperature of 220 ℃ under the pressure of 700MPa for 20s to obtain an annular material with the outer diameter of 14mm and the inner diameter of 8mm, and carrying out stress relief annealing treatment on the material at the temperature of 350 ℃ for 60min to obtain the amorphous soft magnetic composite material.
Example 3 is as follows:
the preparation method of the amorphous soft magnetic composite material comprises the following specific steps:
(1) Weighing 99g FeSiBCCr amorphous powder, and placing the amorphous powder into a suspension of 1g of manganese zinc ferrite powder and 6g of ethanol for passivation treatment to obtain passivated FeSiBCCr amorphous powder;
(2) Mixing the passivated FeSiBCCr amorphous powder and FeNi powder according to the proportion shown in table 1 to obtain mixed powder;
(3) Placing the mixed powder into a mixed solution of organic silicon resin and ethanol for insulating coating, wherein the organic silicon resin used for insulating coating accounts for 2wt% of the total mass of the mixed powder, the ethanol accounts for 12wt% of the total mass of the mixed powder, fully stirring and drying, adding barium stearate accounts for 0.2wt% of the total mass of the mixed powder, maintaining the pressure at 700MPa for 15s at 180 ℃ to obtain an annular material with the outer diameter of 14mm and the inner diameter of 8mm, and carrying out stress relief annealing treatment on the material at 300 ℃ for 80min to obtain the amorphous soft magnetic composite material.
Example 4 is as follows:
the preparation method of the amorphous soft magnetic composite material comprises the following specific steps:
(1) Weighing 97g FeSiBCCr amorphous powder, and placing the amorphous powder into a suspension of 3g of manganese zinc ferrite powder and 10g of ethanol for passivation treatment to obtain passivated FeSiBCCr amorphous powder;
(2) Mixing the passivated FeSiBCCr amorphous powder and FeNi powder according to the proportion shown in table 1 to obtain mixed powder;
(3) Placing the mixed powder into a mixed solution of organic silicon resin and ethanol for insulating coating, wherein the organic silicon resin used for insulating coating accounts for 4wt% of the total mass of the mixed powder, the ethanol accounts for 6wt% of the total mass of the mixed powder, fully stirring and drying, adding barium stearate accounts for 0.25wt% of the total mass of the mixed powder, maintaining the pressure at 350MPa for 40s at 150 ℃ to obtain an annular material with the outer diameter of 14mm and the inner diameter of 8mm, and carrying out stress relief annealing treatment on the material at 400 ℃ for 140min to obtain the amorphous soft magnetic composite material.
Comparative example 1 is as follows:
this comparative example differs from example 1 in that the pressing temperature is 25 ℃.
Comparative example 2 is as follows:
The preparation method of the amorphous composite material comprises the following specific steps:
(1) Mixing 80g FeSiBCCr amorphous powder and 20g FeNi powder to form mixed powder, placing the mixed powder in a mixed solution of organic silicon resin and ethanol for insulating coating treatment, wherein the organic silicon resin used for the insulating coating treatment accounts for 4wt% of the total mass of the mixed powder, the ethanol accounts for 6wt% of the total mass of the mixed powder, and fully stirring and drying;
(2) The added barium stearate accounts for 0.25 weight percent of the total mass of the mixed powder, and the pressure is maintained for 40s at the temperature of 150 ℃ and the pressure of 350MPa to prepare an annular material with the outer diameter of 14mm and the inner diameter of 8 mm;
(3) And carrying out stress relief annealing treatment on the material at 400 ℃ for 140min to obtain the amorphous composite material.
Comparative example 3 is as follows:
this comparative example differs from example 2 in that the finished powder was not doped with FeNi powder.
Comparative example 4 is as follows:
The preparation method of the amorphous material comprises the following specific steps:
(1) Placing 100g FeSiBCCr amorphous powder into a mixed solution of organic silicon resin and ethanol for insulating coating treatment, wherein the organic silicon resin used for the insulating coating treatment accounts for 3wt% of the total mass of the amorphous powder, the ethanol accounts for 10wt% of the total mass of the amorphous powder, and fully stirring and drying;
(2) The added barium stearate accounts for 0.4 weight percent of the total mass of the amorphous powder, and the pressure is maintained for 10s at the temperature of 25 ℃ under the pressure of 1200MPa, so that the annular material with the outer diameter of 14mm and the inner diameter of 8mm is prepared;
(3) And carrying out stress relief annealing treatment on the material at 480 ℃ for 120min to obtain the amorphous material.
Comparing example 1 with comparative example 1, it was found that the amorphous composite material performance can be significantly improved, the effective permeability improved, and the magnetic loss reduced by using an elevated pressing temperature and ferrite cladding process.
The change between the effective permeability and frequency of examples 1 to 4 and comparative examples 1 to 4 was detected, as shown in FIG. 1, and the effective permeability of examples was significantly higher than that of comparative examples in the range of 100 to 1000kHz, the change between the magnetic losses and frequency of examples 1 to 4 and comparative examples 1 to 4 under the test condition of 20mT was detected, as shown in FIG. 2, and the magnetic losses of examples were significantly lower than that of comparative examples as the frequency was increased, the magnetic losses of examples 1 to 4 and comparative examples under the test condition of 100mT and 50kHz were detected, as shown in FIG. 3, the magnetic losses of examples were significantly lower than that of comparative examples 1 to 4 under the test condition of 50mT and 100kHz were detected, as shown in FIG. 4, and the DC superposition properties of examples 1 to 4 and comparative examples 1 to 4 were detected, as shown in Table 2, and the DC superposition capability of examples was maintained at 90% or more.
Table 2 shows the DC superposition performance results of the examples and comparative examples
The foregoing embodiments have been described in some detail for purposes of clarity of understanding, it will be apparent that the invention is not limited thereto, and that any modifications, additions, or equivalent substitutions made within the principles of the invention are intended to be included within the scope of the invention.
Claims (9)
1. An amorphous soft magnetic composite material is characterized by mainly comprising FeSiBCCr amorphous powder, feNi powder and manganese zinc ferrite powder, wherein the particle size of FeSiBCCr amorphous powder is 10-20 mu m, the particle size of FeNi powder is 1-10 mu m, and the particle size of manganese zinc ferrite powder is 0.5-5 mu m;
Wherein FeSiBCCr amorphous powder is placed in suspension of manganese-zinc ferrite powder and ethanol for passivation treatment, and the total mass of FeSiBCCr amorphous powder and manganese-zinc ferrite powder is calculated as the basis, the manganese-zinc ferrite powder accounts for 0.5-3wt% and the ethanol accounts for 5-10wt%;
Wherein, based on the total mass of FeNi powder and FeSiBCCr amorphous powder after passivation, the mass ratio of FeSiBCCr amorphous powder after passivation is 50-80wt%, and the mass ratio of FeNi powder is 20-50wt%;
Wherein, after FeNi powder and FeSiBCCr amorphous powder after passivation are mixed, the mixture is put into a mixed solution of organic silicon resin and organic solvent for insulating coating treatment, the mass ratio of the organic silicon resin is 2-5wt% based on the total mass of FeNi powder and FeSiBCCr amorphous powder after passivation, the organic solvent is ethanol, and the mass ratio of the ethanol is 5-10wt%;
and fully stirring and drying the mixed powder subjected to the insulating coating treatment, and then performing warm-pressing forming and annealing to obtain the amorphous soft magnetic composite material, wherein the temperature of the warm-pressing treatment is 180-230 ℃, the time of the warm-pressing treatment is 10-60s, and the pressure of the pressing forming is 300-700MPa.
2. An amorphous soft magnetic composite material as claimed in claim 1, wherein FeSiBCCr the amorphous powder is formed as Fe 73Si10B10C5Cr2 in terms of atomic percent of each element.
3. An amorphous soft magnetic composite material according to claim 1, wherein the FeSiBCCr amorphous powder has a particle size of 12-17 μm, the FeNi powder has a particle size of 3-8 μm, and the manganese zinc ferrite powder has a particle size of 1-3 μm.
4. The amorphous soft magnetic composite material according to claim 1, wherein FeSiBCCr amorphous powder is subjected to passivation treatment in a suspension of manganese-zinc ferrite and ethanol, and the mass ratio of manganese-zinc ferrite powder is 1-2.5wt% and the mass ratio of ethanol is 6-9wt%, based on the total mass of FeSiBCCr amorphous powder and manganese-zinc ferrite powder.
5. An amorphous soft magnetic composite material according to claim 1, wherein the temperature of the warm-pressing treatment is 200-220 ℃, the time of the warm-pressing treatment is 20-50s, and the press forming pressure is 400-600MPa.
6. An amorphous soft magnetic composite material according to claim 1, wherein the temperature of the warm-pressing treatment is 205-215 ℃, the time of the warm-pressing treatment is 30-40s, and the press forming pressure is 450-550MPa.
7. A method for producing an amorphous soft magnetic composite material according to any one of claims 1 to 6, comprising the steps of:
Step 1, placing FeSiBCCr amorphous powder into a suspension of manganese zinc ferrite powder and ethanol for passivation treatment to obtain passivated FeSiBCCr amorphous powder;
step 2, mixing the passivated FeSiBCCr amorphous powder and FeNi powder, placing the mixture into a mixed solution of organic silicon resin and organic solvent for insulating coating treatment, fully stirring and drying to obtain mixed powder;
and step 3, adding a lubricant into the mixed powder, uniformly mixing, putting into a die, performing warm pressing, and annealing to obtain the amorphous soft magnetic composite material.
8. The method for preparing an amorphous soft magnetic composite material according to claim 7, wherein in the step 3, the lubricant is barium stearate, and the lubricant is used in an amount of 0.2-0.4wt% based on the mass of the mixed powder.
9. The method for preparing an amorphous soft magnetic composite material according to claim 7, wherein in the step 3, the annealing temperature is 350-450 ℃, the heat preservation time is 50-150min, the heating rate is 8-12 ℃ per min, and the amorphous soft magnetic composite material is cooled along with a furnace.
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