CN114147218A - Gap-filled amorphous nanocrystalline insulating finished product powder and preparation method thereof - Google Patents
Gap-filled amorphous nanocrystalline insulating finished product powder and preparation method thereof Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 176
- 238000002360 preparation method Methods 0.000 title claims description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000011812 mixed powder Substances 0.000 claims abstract description 24
- 238000011049 filling Methods 0.000 claims abstract description 22
- XEVZIAVUCQDJFL-UHFFFAOYSA-N [Cr].[Fe].[Si] Chemical compound [Cr].[Fe].[Si] XEVZIAVUCQDJFL-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims abstract description 7
- 229910045601 alloy Inorganic materials 0.000 claims description 51
- 239000000956 alloy Substances 0.000 claims description 51
- 239000011651 chromium Substances 0.000 claims description 44
- 238000003723 Smelting Methods 0.000 claims description 34
- 238000000034 method Methods 0.000 claims description 34
- 239000000203 mixture Substances 0.000 claims description 24
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 238000000576 coating method Methods 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 14
- 239000011248 coating agent Substances 0.000 claims description 13
- 239000002159 nanocrystal Substances 0.000 claims description 13
- 238000000137 annealing Methods 0.000 claims description 12
- 238000009413 insulation Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000000889 atomisation Methods 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 4
- 230000008025 crystallization Effects 0.000 claims description 4
- 239000000945 filler Substances 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- 238000002161 passivation Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 5
- 239000000047 product Substances 0.000 description 47
- 239000011572 manganese Substances 0.000 description 28
- 230000008569 process Effects 0.000 description 19
- 238000000465 moulding Methods 0.000 description 14
- 238000011156 evaluation Methods 0.000 description 13
- 238000012360 testing method Methods 0.000 description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 12
- 239000000463 material Substances 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- 239000006247 magnetic powder Substances 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 239000011230 binding agent Substances 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 230000006835 compression Effects 0.000 description 5
- 238000007906 compression Methods 0.000 description 5
- 238000009689 gas atomisation Methods 0.000 description 4
- 238000009702 powder compression Methods 0.000 description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- 229910001141 Ductile iron Inorganic materials 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000000748 compression moulding Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000003085 diluting agent Substances 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000000314 lubricant Substances 0.000 description 3
- 229910052755 nonmetal Inorganic materials 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000012669 compression test Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 2
- 238000001132 ultrasonic dispersion Methods 0.000 description 2
- 238000009692 water atomization Methods 0.000 description 2
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 2
- 229910000976 Electrical steel Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
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- 238000013461 design Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
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- 230000006872 improvement Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 235000019359 magnesium stearate Nutrition 0.000 description 1
- 229910001004 magnetic alloy Inorganic materials 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 229910000889 permalloy Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910000859 α-Fe Inorganic materials 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
- H01F1/33—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 mixtures of metallic and non-metallic particles; metallic particles having oxide skin
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- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
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- C22C—ALLOYS
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- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/20—Ferrous alloys, e.g. steel alloys containing chromium with copper
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- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/22—Ferrous alloys, e.g. steel alloys containing chromium with molybdenum or tungsten
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- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/32—Ferrous alloys, e.g. steel alloys containing chromium with boron
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- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/34—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of silicon
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- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/54—Ferrous alloys, e.g. steel alloys containing chromium with nickel with boron
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/58—Ferrous alloys, e.g. steel alloys containing chromium with nickel with more than 1.5% by weight of manganese
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- C22C45/00—Amorphous alloys
- C22C45/02—Amorphous alloys with iron as the major constituent
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- 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
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Abstract
The invention provides amorphous nanocrystalline insulating finished product powder, which comprises amorphous nanocrystalline mixed powder and an insulating layer coated on the outer layer of the amorphous nanocrystalline mixed powder, wherein the amorphous nanocrystalline mixed powder comprises spherical amorphous nanocrystalline atomized powder and filling powder filled in gaps of the amorphous nanocrystalline atomized powder, and the filling powder comprises iron-silicon-chromium powder and/or carbonyl iron powder; according to the amorphous nanocrystalline insulating finished product powder filled in the gaps, the filling powder is used for filling and matching the amorphous nanocrystalline atomized powder, and all or part of the filling powder is arranged among the amorphous nanocrystalline atomized powder, so that the bonding strength among the mixed powder particles is effectively increased; and the amorphous nanocrystalline product prepared by the amorphous nanocrystalline insulating finished product powder has the technical effects of high product density and improved performance.
Description
Technical Field
The invention relates to the technical field of soft magnetic alloy metallurgy, in particular to gap-filled amorphous nanocrystalline insulating finished product powder and a preparation method thereof.
Background
The amorphous material has high saturation magnetic induction, high magnetic conductivity, low coercive force, low high-frequency loss, good strong hardness, wear resistance, corrosion resistance, good temperature and environmental stability and the like, has excellent comprehensive performance, replaces permalloy, silicon steel and ferrite, is applied to power electronic technology, shows the characteristics of small volume, high efficiency, energy conservation and the like, and has the optimal cost performance ratio in all metal soft magnetic materials.
In the prior art, carbonyl iron powder and iron-silicon-chromium powder are mainly used as raw materials for preparing an integrally formed inductor, but the two kinds of powder have larger hysteresis loss, and the powder body resistivity is lower, so that the product application process has larger eddy current loss, and the product application has the problems of higher loss, product heating, energy efficiency reduction and the like.
The term "amorphous nanocrystal" refers to a concept of juxtaposition of amorphous and nanocrystal, and the term "amorphous nanocrystal" refers to a generic concept of alloy morphology of amorphous, nanocrystal and nanocrystal, which is defined and described in the art based on different alloy processing stages, in the conversion process from amorphous to nanocrystal, or in the presence of three forms of amorphous, amorphous and nanocrystal, and nanocrystal.
Disclosure of Invention
The invention aims to provide gap-filled amorphous nanocrystalline insulating finished product powder and a preparation method thereof to overcome the defects of the prior art.
The amorphous nanocrystalline insulating finished product powder comprises amorphous nanocrystalline mixed powder and an insulating layer coated on the outer layer of the amorphous nanocrystalline mixed powder, wherein the amorphous nanocrystalline mixed powder comprises spherical amorphous nanocrystalline atomized powder and filling powder filled in gaps of the amorphous nanocrystalline atomized powder.
Further, the amorphous nanocrystalline atomized powder component comprises Fe100-a-b-c-x-y-zSiaBbCcMnxCryXZWherein X is P, Cu,Any one of Mo and Ni, wherein a is more than or equal to 8 and less than or equal to 15, b is more than or equal to 6 and less than or equal to 12, c is more than or equal to 0.2 and less than or equal to 3.0, x is more than or equal to 0.1 and less than or equal to 3.5, y is more than or equal to 0.5 and less than or equal to 2.5, and Z is more than or equal to 0 and less than or equal to 4.0.
Furthermore, b is more than or equal to 6 and less than or equal to 9, and y is more than or equal to 0.3 and less than or equal to 2.5.
Further, the amorphous nanocrystalline atomized powder component comprises Fe75Si11B9C2.5Cr2.3Mn0.2。
Further, the amorphous nanocrystalline atomized powder component comprises Fe74.8Si11B9C1.5Cr2.5Mn0.2P1Or Fe74.8Si11B9C0.5Cr1.5Mn0.2P2Or Fe73.8Si11B9C1.5Cr1.5Mn0.2P2Or Fe79Si11B7C0.5Cr0.3Mn0.2P2Or Fe79Si9B6.2C0.5Cr0.3Mn1P4。
Further, the amorphous nanocrystalline atomized powder component comprises Fe74.8Si11B9C1.5Cr2.5Mn0.2Mo1Or Fe76.8Si11B9C0.5Cr1.5Mn0.2Mo1Or Fe73.8Si11B9C1.5Cr1.5Mn1.2Mo1Or Fe78Si11B7C0.5Cr0.5Mn1Mo2。
Further, the amorphous nanocrystalline atomized powder component comprises Fe74.8Si11B9C1.5Cr2.5Mn0.2Ni1Or Fe74.8Si11B9C0.5Cr1.5Mn0.2Ni2Or Fe74.8Si11B7C1.5Cr1.5Mn0.2Ni3Or Fe76.8Si11B7C0.5Cr0.5Mn0.2Ni4。
Furthermore, in the amorphous nanocrystal mixed powder, the granularity range of the amorphous nanocrystal atomized powder is-325 to +500 meshes, and the granularity range of the filling powder is-600 to +800 meshes; the filling powder comprises iron-silicon-chromium powder and/or carbonyl iron powder; the filling powder is added in a proportion of 2-15% relative to the whole amorphous nanocrystalline mixed powder.
The preparation method of the amorphous nanocrystalline insulating finished product powder comprises the following steps:
s1, blending and smelting the raw materials according to preset component molecular formulas to prepare a master alloy;
s2, preparing powder from the obtained master alloy by an atomization powder preparation method to obtain amorphous nanocrystalline atomized powder;
s3, filling the obtained amorphous nanocrystalline atomized powder with filling powder, and fully and uniformly stirring to form amorphous nanocrystalline mixed powder;
s4, carrying out insulation coating treatment on the obtained amorphous nanocrystalline mixed powder to obtain coated powder;
and S5, forming the coated powder to obtain the amorphous nanocrystalline insulating finished product powder.
In step S4, the insulation coating process includes the following steps:
s4-1, mixing the obtained amorphous nanocrystalline mixed powder with a nitric acid solution and an acetone solution, placing the obtained mixture in a closed container, heating in a water bath at constant temperature, and performing heat preservation treatment;
and S4-2, after the mixture fully reacts, opening the closed container to volatilize acetone in the closed container, and obtaining the coated powder.
Further, between the steps S4 and S5, the method further includes the following steps: s4-1, carrying out pre-annealing treatment on the obtained coated powder to promote the insulation passivation reaction of the coated powder; the annealing temperature range of the pre-annealing treatment is Tx-100 to Tx +80 ℃, and Tx is the crystallization temperature of the amorphous nanocrystal.
The invention has the beneficial effects that:
according to the amorphous nanocrystalline insulating finished product powder filled in the gaps, the filling powder is used for filling and matching the amorphous nanocrystalline atomized powder, and all or part of the filling powder is arranged among the amorphous nanocrystalline atomized powder, so that the bonding strength among the mixed powder particles is effectively increased; and the amorphous nanocrystalline product prepared by the amorphous nanocrystalline insulating finished product powder has the technical effects of high product density and improved performance.
Detailed Description
In order to make the technical solution, objects and advantages of the present invention more apparent, the following examples further illustrate the present invention.
The preparation method of the inductor specifically comprises the following steps:
s1, blending and smelting the raw materials according to a preset component formula to prepare a master alloy;
s2, preparing powder of the obtained master alloy by a conventional belt-making crushing powder-making method or an atomization powder-making method in the prior art to obtain amorphous nanocrystalline powder, wherein the powder obtained by the belt-making crushing powder-making method is irregular and flaky; the powder prepared by the atomization powder preparation method is in a sphere-like shape;
s3, carrying out insulation coating treatment on the obtained amorphous nanocrystalline powder to obtain coated powder;
s4, molding the obtained coated powder to enable the corresponding powder to be granular so as to obtain amorphous nanocrystalline insulating finished product powder;
wherein the molding treatment process comprises adding binder into the coated powder for secondary coating treatment to obtain semi-finished powder; then, adding a lubricant into the semi-finished product powder, stirring and mixing to enable the corresponding powder to be granular, and obtaining the insulated finished product powder;
and S5, carrying out compression molding and baking solidification on the obtained insulating finished product powder, and carrying out subsequent treatment to obtain the inductor.
Example 1:
in the application based on step S1, the alloy composition prepared according to the predetermined composition formula of the present invention includes Fe100-a-b-c-x-y-zSiaBbCcMnxCryXZWherein X is any one of P, Cu, Mo and Ni, wherein a is more than or equal to 8 and less than or equal to 15, b is more than or equal to 6 and less than or equal to 12, c is more than or equal to 0.2 and less than or equal to 3.0, X is more than or equal to 0.1 and less than or equal to 3.5, y is more than or equal to 0.5 and less than or equal to 2.5, and Z is more than or equal to 0 and less than or equal to 4.0. Preferably, 6. ltoreq. b.ltoreq.9, 0.3. ltoreq. y.ltoreq.2.5.
The alloy components of the master alloy are arranged, so that the powder prepared subsequently has high amorphous forming capability, strong corrosion resistance, high saturation magnetic induction intensity and low coercive force, and the application of the master alloy has good application prospect.
The preferable application of the alloy composition scheme is Fe74.8Si11B9C1.5Cr2.5Mn0.2P1Or Fe74.8Si11B9C0.5Cr1.5Mn0.2P2Or Fe73.8Si11B9C1.5Cr1.5Mn0.2P2Or Fe79Si11B7C0.5Cr0.3Mn0.2P2Or Fe79Si9B6.2C0.5Cr0.3Mn1P4。
Specifically, the smelting process of the master alloy is as follows:
s1-1, selecting metal raw materials including industrial pure iron, nodular iron, electrolytic chromium, metal manganese and the like, and putting the metal raw materials into a smelting furnace for smelting, wherein the smelting temperature is 1350-1550 ℃, and the smelting time is 1.5-3.5 h;
s1-2, after the materials are completely melted, sequentially adding alloy raw materials such as ferroboron, ferrophosphorus, industrial silicon and the like and non-metal raw materials for secondary smelting;
s1-3, after the materials are completely melted in the secondary smelting, keeping the temperature for 10 min;
s1-4, after the molten metal is cooled to 1350 ℃, starting the smelting furnace, and performing surface impurity removal treatment on the molten alloy;
and S1-5, pouring the alloy melt with the surface impurities removed into a steel ingot mold, and then cooling and molding to obtain the master alloy.
Wherein the adopted smelting furnace is preferably a vacuum smelting furnace, and the charging amount of the smelting furnace is 15-35 kg.
In the application based on step S2, the master alloy with specific alloy components can be used to prepare corresponding amorphous nanocrystalline strip products, flaky amorphous nanocrystalline crushed powder products and spheroidal amorphous nanocrystalline atomized powder products.
The strip made from the master alloy will have the following performance characteristics, as shown in attached table 1.
Attached table 1 (different component amorphous nanocrystalline strip test performance)
As shown in the attached Table 2, the strip made of the master alloy is crushed into powder, and the magnetic powder core prepared by the method has the following performance characteristics through the preparation method of the magnetic powder core in the prior art.
Attached table 2 (magnetic powder core test performance prepared from amorphous nanocrystalline crushing powder with different components)
As shown in the attached Table 3, the master alloy is used in the gas atomization or water atomization combined method based on the prior art
The performance of the atomized powder is evaluated by a compression ring mode, and the performance evaluation result has the following performance characteristics.
Attached table 3 (comparison of performance of amorphous nanocrystalline atomized powder and conventional powder compression ring test)
As shown in the attached Table 4, the performance evaluation results of the atomized powders prepared from different components based on the application of the alloy components have the following performance characteristics.
Attached table 4 (comparison of performance of different components amorphous nanocrystalline atomized powder compression ring test)
Example 2:
this example differs from example 1 above in that the alloy composition scheme is preferably applied as Fe74.8Si11B9C1.5Cr2.5Mn0.2Mo1Or Fe76.8Si11B9C0.5Cr1.5Mn0.2Mo1Or Fe73.8Si11B9C1.5Cr1.5Mn1.2Mo1Or Fe78Si11B7C0.5Cr0.5Mn1Mo2。
Specifically, the smelting process of the master alloy is as follows:
s1-1, selecting metal raw materials such as industrial pure iron, nodular iron, electrolytic chromium, metal manganese, electrolytic molybdenum and the like, and putting the metal raw materials into a smelting furnace for smelting, wherein the smelting temperature is 1350-1550 ℃, and the smelting time is 1.5-3.5 hours;
s1-2, after the materials are completely melted, sequentially adding alloy raw materials such as ferroboron, industrial silicon and the like and non-metal raw materials for secondary smelting;
s1-3, after the materials are completely melted in the secondary smelting, keeping the temperature for 10 min;
s1-4, after the molten metal is cooled to 1350 ℃, starting the smelting furnace, and performing surface impurity removal treatment on the molten alloy;
and S1-5, pouring the alloy melt with the surface impurities removed into a steel ingot mold, and then cooling and molding to obtain the master alloy.
Wherein the adopted smelting furnace is preferably a vacuum smelting furnace, and the charging amount of the smelting furnace is 15-35 kg.
In the application based on step S2, the master alloy with specific alloy components can be used to prepare corresponding amorphous nanocrystalline strip products, flaky amorphous nanocrystalline crushed powder products and spheroidal amorphous nanocrystalline atomized powder products.
Then strips made from the master alloy will have the following performance characteristics, as shown in attached table 5.
Attached table 5 (different components amorphous nanocrystalline strip test performance)
As shown in the attached Table 6, the strip made of the master alloy is crushed into powder, and the magnetic powder core made of the strip by the method for preparing the magnetic powder core in the prior art has the following performance characteristics.
Attached table 6 (magnetic powder core test performance prepared by amorphous nanocrystalline crushing powder with different components)
As shown in the attached Table 7, the performance of the atomized powder made of the master alloy is evaluated by a pressure ring method based on the gas atomization or water-gas atomization combined method in the prior art, and the performance evaluation result has the following performance characteristics.
Attached table 7 (comparison of performance of amorphous nanocrystalline atomized powder and conventional powder compression ring test)
As shown in the attached Table 8, based on the application of the alloy components, the performance evaluation results of the atomized powders prepared from different components are evaluated according to an integrally formed inductance evaluation mode, and the atomized powders have the following performance characteristics.
Attached table 8 (Performance comparison of amorphous nanocrystalline powders of different compositions according to the Integrated inductance evaluation mode)
Example 3:
this example differs from example 1 above in that the alloy composition scheme is preferably applied as follows: fe74.8Si11B9C1.5Cr2.5Mn0.2Ni1Or Fe75.8Si11B9C0.5Cr1.5Mn0.2Ni2Or Fe75.8Si11B7C1.5Cr1.5Mn0.2Ni3Or Fe76.8Si11B7C0.5Cr0.5Mn0.2Ni4。
Specifically, the smelting process of the master alloy is as follows:
s1-1, selecting metal raw materials such as industrial pure iron, nodular iron, electrolytic chromium, metal manganese, electrolytic nickel and the like, and smelting in a smelting furnace at 1350-1550 ℃ for 1.5-3.5 h;
s1-2, after the materials are completely melted, sequentially adding alloy raw materials such as ferroboron, industrial silicon and the like and non-metal raw materials for secondary smelting;
s1-3, after the materials are completely melted in the secondary smelting, keeping the temperature for 10 min;
s1-4, after the molten metal is cooled to 1350 ℃, starting the smelting furnace, and performing surface impurity removal treatment on the molten alloy;
and S1-5, pouring the alloy melt with the surface impurities removed into a steel ingot mold, and then cooling and molding to obtain the master alloy.
Wherein the adopted smelting furnace is preferably a vacuum smelting furnace, and the charging amount of the smelting furnace is 15-35 kg.
In the application based on step S2, the master alloy with specific alloy components can be used to prepare corresponding amorphous nanocrystalline strip products, flaky amorphous nanocrystalline crushed powder products and spheroidal amorphous nanocrystalline atomized powder products.
Then strips made from the master alloy will have the following performance characteristics, as shown in attached table 9.
Attached table 9 (different components amorphous nanocrystalline strip test performance)
As shown in the attached Table 10, the strip made of the master alloy is crushed into powder, and the magnetic powder core made by the method has the following performance characteristics.
Attached table 10 (magnetic powder core test performance prepared by amorphous nanocrystalline crushing powder with different components)
As shown in the attached table 11, based on the gas atomization or water atomization combination method in the prior art, the performance of the atomized powder made of the master alloy is evaluated by a compression ring method, and the performance evaluation result has the following performance characteristics.
Attached table 11 (comparison of performance of amorphous nanocrystalline atomized powder and conventional powder compression ring test)
As shown in the attached Table 12, based on the application of the alloy components, the performance evaluation results of the atomized powders prepared from different components are evaluated in an integrated molding inductance evaluation mode, and the performance evaluation results have the following performance characteristics.
Attached table 12 (Performance comparison of amorphous nanocrystalline powders of different compositions according to the Integrated inductance evaluation mode)
Example 4:
based on the application cases of the above examples 1 to 3, in order to optimize the powder flowability and the bulk density, the atomized powder prepared in the step S2 can be dried and classified to be applied in different mesh levels. In a preferred embodiment, the atomized powder is classified into three grades of-800 mesh, -500 mesh and-325 mesh; the proportion of the adopted powder is preferably-800: -500: -325 ═ 1:3: 6; the powder is mixed and prepared in a mixing mode of preferably ultrasonic dispersion; the loose density of the powder is 3.2-4.5 g/cm 3.
In the following attached table 13, evaluation was performed in the integrated molding inductance evaluation manner, and the effect of distinguishing the properties of different powder ratios will be shown.
Attached table 13 (comparison of different powder ratio compression test performance)
However, in the case of the atomized powder preparation application of the present invention, since the shape of the atomized powder is in the form of a sphere, there will be many gaps between the powder or the powder; then the inductor product is directly produced, and the product performance still has limitation.
In this embodiment, in step S3, before the atomized amorphous nanocrystalline powder is subjected to insulation coating, filler powder is added to fully stir and mix; the filling powder is selected from iron-silicon-chromium and/or carbonyl iron powder, and gaps among the atomized amorphous nanocrystalline powder are filled to form amorphous nanocrystalline mixed powder through mixing, so that the bonding strength among the powder particles is effectively increased, the density of subsequent products is effectively improved, and the effect of improving the product performance is achieved.
In the case of application of the amorphous nanocrystalline mixed powder, the particle size range of the atomized powder used is-325 to +500 mesh, the particle size range of the filler powder is-600 to 800 mesh, and the addition ratio of the filler powder to the entire amorphous nanocrystalline mixed powder is 2 to 15%.
In the following attached tables 14 and 15, the results of comparing the performance of the compression ring test under different proportions of the amorphous nanocrystalline powder, iron silicon chromium powder, carbonyl iron powder and the like are shown.
Attached table 14 (amorphous nanocrystalline powder and iron silicon chromium powder matching compression ring test performance comparison)
Attached table 15 (amorphous nanocrystalline powder and carbonyl iron powder ratio compression test performance contrast)
Example 5:
in the application based on step S3, the present invention further provides an insulation coating processing method to meet the preparation requirement of the coating powder, wherein the specific process steps are as follows:
a1, mixing the obtained amorphous nanocrystalline powder with a nitric acid solution and an acetone solution, placing the obtained mixture in a closed container, heating in a water bath at constant temperature, and performing heat preservation treatment; the heating temperature of the constant-temperature heating of the water bath is preferably 45 ℃; the heat preservation treatment time is preferably 30 min.
A2, stirring the mixture in the closed container to make the mixture fully react; the stirring treatment mode can be selected to fully stir the mixture in the closed container by a magnetic stirrer or output the mixture in the closed container by ultrasonic waves so as to make the mixture subjected to ultrasonic dispersion mixing; a uniform oxide film is generated on the surface of the amorphous nanocrystalline powder based on the application of nitric acid solution as a passivating agent, and a coating powder is formed.
A3, after full reaction, opening the closed container to volatilize the acetone; and taking out the coated powder.
Wherein, as a preferred embodiment, the mass ratio of the nitric acid solution to the amorphous nanocrystalline powder is 1.2-2.4 wt% based on the mass of the amorphous nanocrystalline powder, and the nitric acid solution can be concentrated nitric acid with a concentration of 68%; the acetone solution accounts for 30-40 wt% of the amorphous nanocrystalline powder. No corresponding nitric acid reaction waste liquid is generated in the process, and no environmental pollution is caused.
In the above process, the binder material used in the process is formed by mixing organic silicon resin, epoxy resin and curing agent, and the mixture ratio is, in parts by mass, organic silicon resin: epoxy resin: the curing agent was 14.5:3: 1. The mass ratio of the binder material to the amorphous nanocrystalline powder is 1.0-5 wt%.
In the above process, the lubricant selected is zinc stearate.
In the above process, the pressure of the press molding is controlled at 500-800 MPa.
Example 6:
after the coating powder is obtained, the invention is applied in a pre-annealing treatment mode to effectively promote the insulating coating effect of the powder, effectively remove the stress generated in the powder preparation process, the insulating stirring process and other processes, and volatilize harmful substances introduced in the insulating coating process.
The obtained coating powder is subjected to pre-annealing treatment, so that the annealing temperature of the pre-annealing treatment ranges from Tx-100 to Tx +80 ℃, and Tx is the crystallization temperature of the amorphous nanocrystal.
For the nanocrystalline powder, the formation of ultrafine crystals of the powder can be realized, the crystallization treatment is realized, the selected pre-annealing temperature is 420-570 ℃, and the annealing time is 30-80 min.
The pre-annealed coating powder is subjected to forming treatment to obtain insulating finished product powder; specifically, in the secondary coating treatment process, the adopted binder is epoxy resin, silicon resin, inorganic silicon and the like, and the diluent can be selected from acetone, ethanol, purified water and the like; the proportion of the binder is 0.5-5.0%, the proportion of the diluent is 0.5-10%, preferably the proportion of the binder is 1.2-3.0%, and the proportion of the diluent is 3-10%. The uniform mixing process can adopt normal temperature and heating state mixing, and the heating temperature is preferably 50-120 ℃.
The lubricant can be selected from paraffin, zinc stearate, magnesium stearate and the like, the adding proportion is 0.2-1.5%, and the insulating finished product powder is obtained after uniform mixing.
Example 7:
in the application process of step S5, in order to simplify the press forming process of the inductor, the present invention is directed to a structural form of integrally formed inductor to make an improvement of the press forming process therein.
Specifically, the obtained amorphous nanocrystalline insulating finished product powder is heated and further stirred and mixed, so that the obtained amorphous nanocrystalline insulating finished product powder is separated and uniformly heated; the amorphous nanocrystalline insulating finished product powder is heated to 100-250 ℃ integrally and then is kept warm for later use.
Preparing a corresponding molding die cavity, designing a prefabricated coil for the inductor, putting the prefabricated coil into the molding die cavity, filling the amorphous nanocrystalline insulating finished product powder subjected to heating treatment into the molding die cavity, and performing compression molding on the inductor by conventional cold pressing equipment to obtain an integrated inductor blank. In the compression molding process, the pressure range is 400-800 Mpa.
The following additional table 16 shows the performance differences of the amorphous nanocrystalline insulating finished product powder cold-pressed by cold pressing equipment under different heating temperatures.
Attached table 16 (different powder temperature compression ring test performance comparison)
Then, baking the obtained integrated inductor blank at the temperature of 150-220 ℃ for 1-2.5 h; and bending the pin part of the inductor according to the design requirement of a specific product to obtain the inductor.
Furthermore, in order to improve the magnetic permeability of the product and reduce the deformation of the coil, a step-by-step molding combination mode can be selected for preparing the inductor.
For example, for an inductor product which is formed by combining a T-shaped prefabricated magnet and a U-shaped prefabricated magnet, a corresponding T-shaped molding die cavity and a corresponding U-shaped molding die cavity can be arranged according to the structural characteristics; filling the heated amorphous nanocrystalline insulating finished product powder into the corresponding forming die cavity so as to prepare the T-shaped prefabricated magnet and the U-shaped prefabricated magnet firstly. Then, a coil is placed in the gap between the T-shaped prefabricated magnet and the U-shaped prefabricated magnet, and further, powder is filled for secondary pressing, so that a corresponding inductor product is obtained.
And on the other hand, after the coil is placed in the gap between the T-shaped prefabricated magnet and the U-shaped prefabricated magnet, or the contact boundary between the T-shaped prefabricated magnet and the U-shaped prefabricated magnet can be bonded by adopting magnetic glue, and the gap in the product can be filled by adopting the bonding, so that the required inductor product is obtained.
Based on the concept definition of "amorphous nanocrystalline", the above-mentioned related amorphous nanocrystalline alloy product may be considered as an application for selecting a corresponding amorphous alloy product, amorphous and nanocrystalline alloy product, or nanocrystalline alloy product.
The above description is only a preferred embodiment of the present invention, and those skilled in the art may still modify the described embodiment without departing from the implementation principle of the present invention, and the corresponding modifications should also be regarded as the protection scope of the present invention.
Claims (10)
1. The amorphous nanocrystalline insulation finished product powder filled in the gap is characterized by comprising amorphous nanocrystalline mixed powder and an insulation layer coated on the outer layer of the amorphous nanocrystalline mixed powder, wherein the amorphous nanocrystalline mixed powder comprises spherical amorphous nanocrystalline atomized powder and filling powder filled in the gap of the amorphous nanocrystalline atomized powder.
2. The amorphous nanocrystalline insulated finished powder of claim 1, wherein the amorphous nanocrystalline atomized powder composition includes Fe100-a-b-c-x-y-zSiaBbCcMnxCryXZWherein X is any one of P, Cu, Mo and Ni, wherein a is more than or equal to 8 and less than or equal to 15, b is more than or equal to 6 and less than or equal to 12, c is more than or equal to 0.2 and less than or equal to 3.0, X is more than or equal to 0.1 and less than or equal to 3.5, y is more than or equal to 0.5 and less than or equal to 2.5, and Z is more than or equal to 0 and less than or equal to 4.0.
3. The amorphous nanocrystalline insulated finished powder of claim 2, wherein b is 6. ltoreq. b.ltoreq.9, y is 0.3. ltoreq. y.ltoreq.2.5.
4. The amorphous nanocrystalline insulated finished powder of claim 3, wherein the amorphous nanocrystalline atomized powder composition includes Fe75Si11B9C2.5Cr2.3Mn0.2。
5. The amorphous nanocrystalline insulated finished powder of claim 3, wherein the amorphous nanocrystalline atomized powder composition includes Fe74.8Si11B9C1.5Cr2.5Mn0.2P1Or Fe74.8Si11B9C0.5Cr1.5Mn0.2P2Or Fe73.8Si11B9C1.5Cr1.5Mn0.2P2Or Fe79Si11B7C0.5Cr0.3Mn0.2P2Or Fe79Si9B6.2C0.5Cr0.3Mn1P4。
6. The amorphous nanocrystalline insulated finished powder of claim 3, wherein the amorphous nanocrystalline atomized powder composition includes Fe74.8Si11B9C1.5Cr2.5Mn0.2Mo1Or Fe76.8Si11B9C0.5Cr1.5Mn0.2Mo1Or Fe73.8Si11B9C1.5Cr1.5Mn1.2Mo1Or Fe78Si11B7C0.5Cr0.5Mn1Mo2。
7. The amorphous nanocrystalline insulated finished powder of claim 3, wherein the amorphous nanocrystalline atomized powder composition includes Fe74.8Si11B9C1.5Cr2.5Mn0.2Ni1Or Fe74.8Si11B9C0.5Cr1.5Mn0.2Ni2Or Fe74.8Si11B7C1.5Cr1.5Mn0.2Ni3Or Fe76.8Si11B7C0.5Cr0.5Mn0.2Ni4。
8. The amorphous nanocrystalline insulated finished powder of any one of claims 1 to 7, wherein in the amorphous nanocrystalline mixed powder, the amorphous nanocrystalline atomized powder has a particle size range of-325 to +500 mesh, and the filler powder has a particle size range of-600 to +800 mesh; the filling powder comprises iron-silicon-chromium powder and/or carbonyl iron powder; the filling powder is added in a proportion of 2-15% relative to the whole amorphous nanocrystalline mixed powder.
9. The method for preparing an amorphous nanocrystalline insulating finished powder according to any one of claims 1 to 7, characterized by comprising the following steps:
s1, blending and smelting the raw materials according to preset component molecular formulas to prepare a master alloy;
s2, preparing powder from the obtained master alloy by an atomization powder preparation method to obtain amorphous nanocrystalline atomized powder;
s3, filling the obtained amorphous nanocrystalline atomized powder with filling powder, and fully and uniformly stirring to form amorphous nanocrystalline mixed powder;
s4, carrying out insulation coating treatment on the obtained amorphous nanocrystalline mixed powder to obtain coated powder;
and S5, forming the coated powder to obtain the amorphous nanocrystalline insulating finished product powder.
In step S4, the insulation coating process includes the following steps:
s4-1, mixing the obtained amorphous nanocrystalline mixed powder with a nitric acid solution and an acetone solution, placing the obtained mixture in a closed container, heating in a water bath at constant temperature, and performing heat preservation treatment;
and S4-2, after the mixture fully reacts, opening the closed container to volatilize acetone in the closed container, and obtaining the coated powder.
10. The method of claim 9, further comprising, between steps S4 and S5, the steps of: s4-1, carrying out pre-annealing treatment on the obtained coated powder to promote the insulation passivation reaction of the coated powder; the annealing temperature range of the pre-annealing treatment is Tx-100 to Tx +80 ℃, and Tx is the crystallization temperature of the amorphous nanocrystal.
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